Phương Phap Phan Tich PH Nguyên T

PHM LUN
PHNG PHAP PHAN TICH

PH NGUYN T
(In Ln th 2 c sa cha v b sung)
NH XUT BN I HC QUC GIA H NI
LI M U
Php o ph pht x v hp th nguyn t l nhng k thut phn tch ha l, v ang

c pht trin v ng dng rng ri trong nhiu ngnh khoa hc k thut, trong sn xut cng
nghip, nng nghip, y dc, a cht, ha hc. c bit cc nc pht trin, phng php
phn tch ph pht x nguyn t tr thnh mt trong cc phng php dng phn tch
lng vt cc kim loi trong nhiu i tng khc nhau nh t, nc, khng kh, thc phm,
v.v... Hin nay trong cng tc nghin cu bo v mi trng, phng php phn tch ny l
mt cng c c lc xc nh cc kim loi nng c hi.
nc ta, k thut phn tch theo ph pht x v hp th nguyn t cng c pht
trin v ng dng trong khong hn hai chc nm nay. Mt s phng th nghim c
trang b my o ph pht x v hp th nguyn t, hoc do Nh nc ta u t, hoc do s
vin tr ca cc t chc nc ngoi theo cc chng trnh khc nhau. Mt s cn b khoa hc
ca ta c c ra nc ngoi hc tp, nghin cu v o to.Song i
s khng ciu kin
,nhng
licn sdng k thut phn tch
ny cho cng vic phn tch ca h. Hu ht cc ti liu hay sch khoa hc v k thut ny li
bng ting Anh. Mt khc, chng ta li cha c mt cun sch hoc cc ti liu c s l thuyt
bng ting Vit v k thut phn tch ny.
Do thc th , ng gp cho cng tc o to sinh vin trn lnh vc k thut phn
tch ny ca Khoa Ha hc, Trng i hc Khoa hc T nhin - i hc Quc gia H Ni,
cng nh to iu kin cho mt s cn b khoa hc, cng nhn vin phn tch ca cc phng
th nghim khc c ti liu tham kho, chng ti mnh dn bin son cun sch ny. N c
coi nh l gio trnh c s l thuyt v Phng php phn tch ph nguyn t. y cng l ni
dung nhm phc v o to cao hc v k thut phn tch ny.
y l gio trnh ting Vit u tin v k thut phn tch hin i ny nn khng th
trnh khi nhng hn ch v thiu st nht nh. V th rt mong s ng gp thm kin ca
cc bn b ng nghip v cc c gi quan tnm, tc gi c iu kin b sung cho hon
chnh hn.
Nhn dp ny chng ti xin chn thnh cm n GS. TS. J.F.M. Maessen, GS. TS. J.
Kragton, GS. TS. Ban, TS. J.C. Kraak, cc k s H. Balker v J.W. Elgersma (khoa Ha,
trng i hc tng hp Amsterdam, H Lan), GS. TSKH. Trnh Xun Gin (Vin Ha), TS.
Nguyn Hong (HQGHN), PGS. TS. Phm Gia Hu (H Dc) v cc ng nghip B mn
Ha Phn tch khoa Ha hc c nhiu kin ng gp cho ni dung ca gio trnh ny.
Phm Lun
PHN I
Chng 1
I CNG V PHNG PHP AES
1.1 S phn loi ph

Phn tch quang ph l tn gi chung cho mt h cc phng php phn tch quang hc
da trn c s ng dng nhng tnh cht quang hc ca nguyn t, Ion, phn t v nhm phn t.
V d, tnh cht pht x hay hp th quang ca nguyn t, tinh cht hp th quang ca phn
t, v.v... V vy ty theo quan nim, da theo nhng iu kin kch thch ph, phng tin thu
ghi v quan st ph, cng nh bn cht ca qu trnh sinh ra ph m ngi ta c mt s cch
phn chia thnh nhng php o khc nhau, nh php o ph pht x nguyn t, hp th
nguyn t, php o ph hng ngoi,... Tuy th, nhng c hai cch phn chia sau y l ph
hp hn:
1.1.1S phn chia theo c trng ca ph
Theo cch ny ngi ta c nhng phng php phn tch quang hc sau:
Phng php phn tch ph nguyn t, gm c:
a) Ph php x nguyn t
b) Ph hp th nguyn t
c) Ph hunh quang nguyn t
y l ph do s chuyn mc nng lng ca cc in t ha tr ca nguyn t trng
thi kh (hi) t do, khi b kch thch m sinh ra.
Phng php phn tch ph phn t, gm c:
a) Ph hp th phn t trong vng UV-VIS
b) Ph hng ngoi (IR v NIR)
c) Ph tn x Raman
Ph ny c quyt nh bi cc in t ha tr ca nguyn t trong phn t, l
nhng in t ha tr nm trong lin kt hay mt cp cn t do, chuyn mc nng lng khi b
kch thch.
Ph Rn-ghen (tia X), l ph ca in t ni ca nguyn t, gm c:
+ Ph pht x tia X
+ Ph hunh quang tia X
+ Ph nhiu x tia X
Trn
l hng
hai cch
Phy
cng
t,phn
gm:chia chnh cn hay c dng. Tt nhin cn c mt s cch
phn chia khc. Nhng c nhiu nhc im v t c s dng, nn khng cp n y.
a) Cng hng t in t (ERMS).
S phn chia ny c tnh cht gii thiu chung ton b vng ph. Song, trong gio trnh
b) ch
Cng
proton
nhn: NRMS))
ny chng ti
hng
cp ntph
pht(ht
x nguyn
t, v phng php phn tch ng dng tnh
Phng
php phn
khi
lng
cc
cht pht
x ca nguyn
t tch
trng
thiph:
hi Ph
cny
gic
l Kquyt
thut nh
phn bi
tch khi
ph pht
xca
nguyn
Ion
t. phn t hay cc mnh Ion ca cht phn tch b ct ra (t s m/z).
cchph
phn
chia
c stdng rng ri v c coi nh l hp l nht v tng
1.2 Sy
xutlhin
pht
x nguyn
ng
ngay
php
c th..
1.2.1vi
Tm
tttng
v cu
too
nguyn
t
1.1.2 Hng
Phn ngy
chia theo
tadi
sng quen vi nhng tn gi, st (Fe), ng (Cu) ch (Pb), bc
chng
thng
Nh chng
ta (Aj),
bit, bc
in t
mi nguyn
bc sng,
t hc.
sngn
di nay
hngngi
ngntamt
(Ao), vng
(Au), nhm
kmx
(Zn),...
c
l
nhng
t ha
n
ngnnguyn
vi micromet
hay khc
nanomet.
ph
in
ythuyt
phi
ht
bit sng
trn 110
t ha hc
nhau.Do
Nhng
v ca
mtbc
hax
hc
v t
theo
cacha
alton,
tt
c cc
sngbao
.gm
Nhng
trong
thc t
c mt
cnguyn
quang hc
c t
thnh
c
nguyn
t vng
ha hc
nhng
nguyn
t khng
ca cng
mt dng
loi v
t lno
phn
kh
thu c
nhn,tnh
phncht
li hay
c ton
vng ph
nhmi
th.nguyn
V th t
ngi
chia
nhtnng
cn gi
hapht
hc hin
ca nguyn
t. b
Nguyn
t ca
ha ta
hc
c
ph
inkhc
t thnh
min c
(vng
l nguyn
tc cht
ca cch
th hc
hai
cu to
nhau nhiu
nn chng
tnhph)
cht khc
khc nhau.
nhau.
Quyt
nh tnh
vt lchia
v ha
ny
(bng 1.1).
ca chng
l cu to ca lp v electron trong nguyn t, c bit l cc in t ha tr.
Bng
Nguyn t ca mi nguyn t ha hc
u1.1
c xy dng t mt ht nhn nguyn t v
S
chia(in
ph theo
di nguyn
sng t, ht nhn gia, cc in t chuyn ng xung quanh
ccphn
electron
t). Trong
ht nhn theo nhng qu o (orbital) tng i. Ht nhn chim th tch rt nh trong khng
Tn vngth
phtch nguyn t), nhng
di li
sng
gian ca nguynSTT
t (khong 1/10.000
chim hu nh ton b
khi lng ca nguyn t. Nu coi ng knh nguyn t l 10-8cm, th ng knh ht nhn
gama (lp
Y) v ca nguyn
< 0,1 nm
ch chim khong110-12cm. NhTia
vy,
t
ngoiht
nhnTia
l rtrng,
n chnh l khng gian0,1+ 5 nm
2
X
chuyn ng ca in t. S chuyn ng ca in t trong khng gian ny rt phc tp. N
3
T ngoi
80 + 400 nm
va tun theo quy lut ca chuyn ng sng, li va tun theo quy lut chuyn ng ca cc
4
Kh
kin
400 i,
+ 800
nm ta vn tha nhn
ht vi m. Song trong
mt iu
kin
nht nh v mt cch tng
ngi
cc in t chuyn
khngngoi
gian ca nguyn t theo ccqu
5 ng trongHng
1+ 400o.
p,m Nhng theo quan
my electron.
7 nguyn
Trong lp v
im hini cac lng

t th l cc m
Sng ngn
400 + 1000 p,m
Sng
t, Raa
in tphn b
0,1+lp
1 cm
thnh tng
ng
vi s lng t
chnh ca nguyn8t (n). Trong

tngcc
lpngn
li c nhiu qu o ng
Sng
0,1 -vi
50 s
cmlng t ph 1 ca
nguyn t. l cc phn lp. Nhng theo nguyn l vng bn th in t bao gi cng chim
9
Tivi - FM
1 +10 m
v lm y nhng qu o c mc nng lng thp trc. Sau mi n nhng qu o c
10
Sng raio
10+ 1500m
mc nng lng cao hn. Th t sp xp l: ls, 2s, 2p, 3s, 3p, 4s, 3d, 4p, 5s, 4d, 5p, 6s, 4f,
5d, 6p, 7s, 5f, 6d, 7p, v.v... (hnh 1.1a).
Trong bng 1.1, vng ph t 3 n 5 l vng ph quang hc. Cc ph ny xut hin do
s chuyn mc nng lng ca cc in t ha tr ca nguyn t v phn t, khi b kch thch.
Vic phn chia theo cch ny cng c nhng im cha r rng, nh trong vng t ngoi v
kh kin th c c ph ca nguyn t v phn t, m bn cht ca hai loi ph v s kch
thch ca hai loi li rt khc nhau.
4
Hnh 1.1a
S phn b nng lng trong nguyn t
(1)-cu to nguyn t: (2)-phn b nng lng trong lp v nguyn t.
Qu trnh pht x v hp th ca mt nguyn t.

E0: Nng lng trng thi c bn; cm: Nng lng trng thi kch thch; + hv v +
AE: Nng lng kch thch; - hv: Tia pht x.
(n = 5)
(n = 4)
(n = 3)
(n = 2)
Hnh 1.1 b
S phn b nng lng trong nguyn t v sinh ph
1.2.2 S xut hin ph pht x
Trong iu kin bnh thng, cc in t chuyn ng trn cc qu o ng vi mc
nng lng thp nht. Khi nguyn t trng thi bn vng, trng thi c bn. trng thi
ny nguyn t khng thu v cng khng pht nng lng. Nhng nu cungcp nng lng cho
nguyn t th trng thi khng tn ti na. Theo quan im ca thuyt lng t, khi trng
thi kh, in t chuyn ng trong khng gian ca nguyn t, c bit l cc in t ha tr,
nu chng nhn c nng lng bn
7
ngoi (in nng, nhit nng, ha nng,...) th in t s chuyn ln mc nng lng cao hn.
Khi nguyn t b kch thch. N tn ti trng thi kch thch. Nhng trng thi ny
khng bn vng. Nguyn t ch lu li trng thi ny nhiu nht l 10 8 giy. Sau n lun
lun c xu hng tr v trng thi c bn ban u bn vng. Ngha l gii phng nng lng
m chng hp th c trong qu trnh trn di dng ca cc bc x quang hc. Bc x
ny chnh l ph pht x ca nguyn t, n c tn s c tnh theo cng thc:
AE = (En - Eo) = hv
(1.1)
hay: AE =
X
trong :
En v E0 l nng lng ca nguyn t trng thi c bn v trng thi kch thch n;
h l hng s Plank (6,626.10 -7 erk.s) hay h = 4,1.10-15 eV.s;
c l tc nh sng (3.108 m/gy) - 2,99793.108 m/gy;
v l tn s ca bc x ;
X l bc sng ca bc x .
Trong biu thc trn, nu gi tr AE l nm ta c qu trnh hp th v khi gi tr AE
dng ta c qu trnh pht x ca nguyn t.
Nhng trong nguyn t, s chuyn mc ca in t t mc nng lng E n khng phi
ch v mc E0, m c rt nhiu s chuyn mc t E n v cc mc khc E 01, E02, E03_ cng vi
mc E0. Ngha l c rt nhiu s chuyn mc ca in t c lng t ha, v ng vi
mi bc chuyn mc ta c 1 tia bc x, tc l mt vch ph. Chnh v th m mt nguyn
t khi b kch thch thng c th pht ra rt nhiu vch ph pht x. Nguyn t no c nhiu
in t v c cu to phc tp ca cc lp in t ha tr th cng c nhiu vch ph pht x.
Mt cch tng trng ta c th m t qu trnh kch thch v pht x ca nguyn t theo m
hnh trong hnh 1.2.
Nu dng my quang ph thu chm ra pht x , phn li v ghi li cc chm tia pht
x do nguyn t pht ra ta s c mt di ph t sng ngn n sng di. l ph pht x
ca nguyn t ca cc nguyn t v n l ph vch. Nh vy, ph pht x nguyn t l sn
phm sinh ra do s tng tc vt cht, m y l cc nguyn t t do trng thi kh
vi
mt ngun
nng
lng nhit,in... nhtnh ph hp.
Nhng trong ngun sng, khng phi ch c nguyn t t do b kch thch, m c c Ion, phn
t, nhm phn t. Cc phn t ny cng b kch thch v pht ra ph pht x ca n. Tt nhin
l trong mc khc nhau ty thuc vo kh nng kch thch ca ngun nng lng. V vy,
ph pht x ca vt mu lun bao gm ba thnh phn:
1.
Nhm ph vch. l ph ca nguyn t v con. Nhm ph vch ny ca cc
nguyn t ha hc hu nh thng nm trong vng ph t 190-1000nm (vng UV- VIS). Ch
c mt vi nguyn t kim hay kim loi kim mi c mt s vch ph nm ngoi vng ny.
2.
Nhm ph m. l ph pht x ca cc phn t v nhm phn t. V d
ph ca phn t MeO, CO v nhm phn t CN. Cc m ph ny xut hin thng c mt

u m v mt u nht. u m pha sng di v nht pha sng ngn. Trong vng t
ngoi th ph ny xut hin rt yu v nhiu khi khng thy. Nhng trong vng kh kin th
xut hin rt m, v lm kh khn cho php phn tch quang ph v nhiu vch phn tch ca
cc nguyn t khc b cc m ph ny che lp.
3. Ph nn lin tc. y l ph ca vt rn b t nng pht ra, ph ca nh sng trng
v ph do s bc x ring ca in t. Ph ny to thnh mt nn m lin tc trn ton di
ph ca mu. Nhng nht sng ngn v m dn v pha sng di. Ph ny nu qu m th
cng s cn tr php phn tch.
Ba loi ph trn xut hin ng thi khi kch thch mu phn tch v trong phn tch
quang ph pht x nguyn t ngi ta phi tm cch loi bt ph m v ph nn. l hai
yu t nhiu.
1.3 Nguyn tc ca php o ph pht x (AES)
T vic nghin cu nguyn nhn xut hin ph pht x, chng ta c th khi qut
phng php phn tch da trn c s o ph pht x ca nguyn t phi bao gm cc bc
nh sau:
1. Trc ht mu phn tch cn c chuyn thnh hi (kh) ca nguyn t hay Ion t
do trong mi trng kch thch. l qu trnh ha hi v nguyn t ha mu. Sau dng
ngun nng lng ph hp kch thch m hi chng pht x. y l qu trnh kch
thch ph ca mu.
2.Thu, phn 1i v ghi ton b ph pht x ca vt mu nh my quang ph. Trc y,
ph c ghi ln knh nh hay phim nh. Chnh my quang ph s lm nhim v ny. Nhng
nhng trang b hin i ngy nay c th thu v ghi trc tip cc tn hiu cng pht x ca
mt vch ph di dng cc lc trn bng giy hay ch ra cc sng cng vch ph trn
my in (printer), ghi li vo a t ca my tnh.
3. nh gi ph ghi v mt nh tnh v nh lng theo nhng yu cu t ra.
y l cng vic cui cng ca php o.
Chnh v vy, ng vi cc nhim v v nguyn tc ny, thc hin mt php phn tch
da theo ph pht x ca nguyn t ngi ta phi cn mt h thng trang b cng gm ba phn
tng ng nh th.
A. Trang b c bn (ti thiu phi c):
Phn 1: Ngun nng lng ha hi, nguyn t ha mu v kch thch ph ca mu
phn tch, c ph ca nguyn t phn tch.
Phn 2: My quang ph thu, phn li v ghi li ph pht x ca mu phn tch theo
vng ph ta mong mun.
Phn 3: H thng trang b nh gi nh tnh, nh lng v ch th hay biu th cc
kt qu.
Mt cch tng qut, ta c th m t nguyn tc ny theo s hnh 1.3.
Ion Mg+
Si
ng
let
Tr
ip
let
Hnh
1.2b
S
vch
ph
pht
x
ca
nguy
n t
Mg
B. Trang b hon chnh:

C thm cc b phn sau:
1. B t ng bm hay a mu vo o.
11
2. H my tnh v phn mm ca n.
Mu phn tch
Ngun E
Ha hi, nguyn t ha v
kch thch ph pht x
Ngn la
H quang
Tia
in
ICP(AES)
Thu, phn li, ghi bc x
plasma
N
n
g
(theo ba cch khc nhau)

Cch I
Cch II
Ghi ph ln knh nh
(Spectrograph)
Quan st trc tip

nh tnh v nh lng
(Spectroscop)
Knh nh cha ph mu p.t.
nh gi nh tnh v
bn nh lng
(Spectroprojector)
nh gi nh tnh, nh lng
(theo hai cch)
r
o en trc tip
bng vi quang k
Cch III
My t ghi I ca
vch ln bng giy
Thu, phn li, ghi trc tip ph mu p.t.

(Spectrometer, mt hay nhiu knh)
Chn, khuch i tn hiu, b chnh
My tnh (Microcomputer) x l kt qu
Hin s" kt qu
In kt qu
T ghi cng
Hnh 1.3
S nguyn l ca qu trnh phn tch AES
Hnh 1.4
Vng nng phn tch ca cc phng php ph
13
12
1.4 i tng ca phng php phn tch ph pht x

Bn cnh mc ch nghin cu vt l quang ph nguyn t, php o ph pht x nguyn
t l mt phng php phn tch vt l da trn tnh cht pht x ca nguyn t trng thi
hi xc nh thnh phn ha hc ca cc nguyn t, cc cht trong mu phn tch. V vy
n c tn phn tch quang ph ha hc. Phng php ny c s dng phn tch nh tnh
v nh lng cc nguyn t ha hc, ch yu l cc kim loi trong mi i tng mu khc
nhau, nh a cht, ha hc, luyn kim, ha du, nng nghip, thc phm, y dc, mi
trng... thuc cc loi mu rn, mu dung dch, mu bt, mu qung, mu kh. Tuy phn tch
nhiu i tng, nhng thc cht l xc nh cc kim loi l chnh, ngha l cc nguyn t c
ph pht x nhy, khi c kch thch bng mt ngun nng lng thch hp; sau l mt
vi kim nh Si, P, C. V vy, i tng chnh ca phng php phn tch da theo php o
ph pht x ca nguyn t l cc kim loi nng nh trong cc loi mu khc nhau. Vi i
tng kim th phng php ny c nhiu nhc im v hn ch v nhy, cng nh
nhng trang b thu, ghi ph ca chng, v ph ca hu ht cc kim li nm ngoi vng t
ngoi v kh kin, ngha l phi c thm nhng trang b phc tp mi c th phn tch c
cc kim.
1.5 Cc u im v nhc im
Phng php phn tch quang ph pht x nguyn t s d c pht trin rt nhanh v
c s dng trong nhiu lnh vc ca khoa hc, k thut cng nghip, nng nghip v i
sng v n c nhng u im rt c bn:
a)Phng php ny c nhy rt cao. Bng phng php ny nhiu nguyn t c th
c xc nh t n nhy t n.10 3 n n.104 %. Nhng vi nhng trang b hin i v vi
nhng ngun kch thch ph mi (ICP) ngi ta c th t n nhy t n.10 -5 n n.10-6 %
i. Vi nhiu nguyn t m khng cn phi lm giu mu phn tch (bng 1). V th n l
phng php kim tra, nh gi tinh khit ca nhiu ha cht v nguyn liu tinh khit
cao, phn tch lng vt cc kim loi nng c hi trong i tng thc phm, nc gii kht,
mi trng. Trong khi vi nhng i tng ny th phng php ha hc khng th no t
c.
b) Phng php ny gip chng ta c th tin hnh phn tch
ng thi nhiu
nguyn t trong mt mu, m khng cn tch ring chng ra khi nhau. Mt khc, li khng
tn nhiu thi gian, c bit l phn tch nh tnh v bn nh lng.
c) Vi nhng tin b ca k thut hin nay v vi nhng trang b hin nay t c,
th phng php phn tch theo ph pht x nguyn t l mt php o chnh xc tng i
cao. Trong nhiu trng hp, vi nng nh (c ppm) m sai s ca php o l di 10%.
Tt nhin vi nhng trang b v my mc c in th
th ln
hn. Song thc t n b nhng trang b hin i y li.
14
sai
sc
d) Phng php phn tch theo ph pht x l mt phng php phn tch tiu tn t
mu, ch cn t 1 n vi chc miligam mu l . c bit l k thut ph pht x.
e) Phng php phn tch ny c th kim tra c ng nht v thnh phn ca vt
mu nhng v tr (ch) khc nhau. V th cng c ng dng kim tra ng nht ca
b mt vt liu.
f)Trong nhiu trng hp, ph ca mu nghin cu thng c ghi li trn phim nh,
knh nh hay trn bng giy. N l nhng ti liu lu tr v khi cn thit c th nh gi hay
xem xt li m khng cn phi c mu phn tch.
Bn cnh nhng u im nu, phng php ny cng c mt s nhc im v hn
ch nht nh. Trc ht phi ni n l: Phng php ny ch cho chng ta bit c thnh
phn nguyn t ca mu phn tch, m khng ch ra c trng thi lin kt ca n trong
mu. chnh xc ca php phn tch ph thuc vo nng chnh xc ca thnh phn ca
dy mu u v cc kt qu nh lng u phi da theo cc ng chun ca cc dy mu
u c ch to sn trc.
Mc du c mt s nhc im v hn ch, nhng phng php phn tch quang ph
pht x nguyn t ngy cng c pht trin v ng dng rng ri trong nhiu lnh vc khc
nhau xc nh lng vt cc nguyn t trong cc i tng mu khc nhau. l mt
phng php phn tch nhanh, c chnh xc bo m v nhy kh cao, c bit thch
hp cho phn tch t him, cc loi nc, khng kh, v.v.
1.6 Kh nng v phm vi ng dng
Phng php phn tch quang ph pht x nguyn t ngy nay gi vai tr quan trng
trong ha hc phn tch. Cng vi s pht trin mnh m ca cc ngnh khoa hc k thut,
c bit l vt l v ha hc, s pht trin ca k thut o v ghi tn hiu, lm tng kh nng
ng dng to ln ca n. Bng phng php ny ngi ta c th xc nh nh tnh, bn nh
lng v nh lng c hn nm chc kim loi v gn mt chc nguyn t kim trong cc
i tng mu khc nhau (v c v hu c). Phng php phn tch ny tr thnh cng c
phn tch nguyn t c lc ch nhiu lnh vc, nht l sau khi c ngun kch thch ICP.
a) Phn tch quang ph pht x trong ngnh ha v cng nghip ha hc. N l cng c
cc nh ha hc xc nh thnh phn nh tnh v nh lng ca nhiu cht, kim tra
tinh khit ca cc ha phm, nguyn liu v nh gi cht lng ca chng. N cng l mt
phng php xc nh cc ng v phng x v nghin cu cu trc nguyn t.
b) Phn tch quang ph pht x nguyn t trong a cht. Ngay t khi mi ra i, phng
php ny c cc nh a cht s dng phn tch cc mu qung phc v cho cng vic
thm d a cht v tm ti nguyn khong sn. V th ngnh a cht ca tt c cc nc u
c phng phn tch quang ph pht x rt hin i v hon chnh.
15
c) Phn tch quang ph pht x trong luyn kim. Luyn kim cng l mt ngnh s dng
phng php phn tch quang ph pht x u tin vo mc ch ca mnh trc c ngnh
ha. Chnh tnh cht nhanh chng v nhy ca phng php ny l mt iu rt cn thit
i vi ngnh luyn kim. N c th l cng c gip cc nh luyn kim xc nh ngay c
thnh phn ca cc cht ang nng chy trong l luyn kim; qua m h c th iu chnh
nguyn liu a vo ch to c nhng hp kim c thnh phn mong mun, kim tra
thnh phn, kim tra nguyn liu.
d) Phn tch quang ph pht x trong tiu ch un hc. Trc y con ngi tng rng
kh c th hiu bit c thnh phn ha hc ca cc hnh tinh xung quanh tri t chng ta.
Nhng phng php phn tch quang ph pht x ra i m rng tm vi cho con ngi.
Bng phng php ph pht x v kt hp vi mt s knh thin vn, cc nh thin vn c th
quan st c thnh phn ca cc nguyn t ha hc ca cc hnh tinh khc nh mt trng,
cc v sao. Chnh nhng kt qu phn tch thnh phn ca cc mu t do v tinh ly t mt
trng v ni ln ngha ca php o ph pht x trong lnh vc nghin cu thin vn. V
nhng kt qu phn tch thc t cc mu l rt ph hp vi nhng s liu thu c trc y
qua phn tch tia sng t mt trng bng h thng my quang ph v knh thin vn.
e)Phn tch quang ph pht x trong nng nghip, y v sinh hc. y l nhng ngnh khoa
hc s dng phng php ny cm li nhiu kt qu rc r, c bit l trong vic nghin cu
th nhng, nghin cu cc nguyn t vi lng trong t trng, trong cy trng, trong phn
bn ca nng nghip, hay nghin cu thnh phn thc n phc v chn nui, phn tch nguyn
t vi lng trong mu, serum, nc tiu, phc v cha bnh.
f) Phn tch quang ph trong cc lnh vc khc. Ngoi nhng lnh vc nu, phng
php phn tch quang ph pht x nguyn t cn c mt s ngnh khc s dng nh l mt
cng c phn tch. V d nh trong ngnh dc kim tra mt s kim loi c hi trong cc
dc phm (Pb, Cu, Zn, Hg,...). Ngnh nghin cu c s, cng an, to n, ngoi thng, cng
l nhng ni s dng phng php phn tch quang ph trong cc lnh vc nghin cu v
nng php o ph nguyn t ln ngang tm ca thi i.
Hnh 1.5
S phn chia cc loi ph theo di sng
16
Chng 2
S KCH THCH PH PHT X NGUYN T
Yu cu v nhim v ca ngun kch thch

Trong phn tch quang ph pht x nguyn t, ngun sng c gi l ngun kch thch
ph v c mt vai tr ht sc quan trng. V nh ngun nng lng kch thch ngi ta c th
chuyn vt liu mu phn tch thnh trng thi hi ca cc nguyn t v kch thch m hi
pht sng (pht x), ngha l ngun nng lng nh hng trc tip n kt qu ca php
phn tch. V vy ngun nng lng mun dng c vo mc ch phn tch quang ph pht
x nguyn t cn phi thc hin c hai nhim v sau y:
Trc ht ngun nng lng phi ha hi, nguyn t ha v chuyn c hon ton cc
nguyn liu mu phn tch vo vng phng in (plasma). C nh th thnh phn ca m hi
trong plasma mi ng nht vi thnh phn ca vt mu. ng thi ngun nng lng phi c
nng lng ln (nhit ) c th kch thch c tt nht cc nguyn t ca nguyn t
cn phn tch i n pht x ra ph ca n.
Song nh th vn cha hon ton . V mt phng php phn tch ch c gi tr khi n
c nhy v lp li cao. Chnh v th, ngoi hai nhim v trn mt ngun sng mun dng
c lm ngun kch thch ph pht x n cn cn phi tha mn mt s yu cu nht nh
sau y:
Trc ht ngun sng phi m bo cho php phn tch c nhy cao v cng ca
vch ph phi nhy vi s bin thin nng ca nguyn t phn tch; nhng li khng nhy
vi s dao ng ca iu kin lm vic.
Ngun nng lng phi n nh v bn vng theo thi gian, m bo cho phng
php phn tch c lp li v n nh cao. Ngha l cc thng s ca ngun sng chn
nht thit phi duy tr v lp li c.
Ngun nng lng phi khng a thm ph ph vo lm ln vi ph ca mu nghin
cu. Nu khng s lm kh khn thm cng vic nh gi nh tnh v nh lng v c khi
lm sai lc c kt qu phn tch.
Ngun kch thch phi c s cu to khng qu phc tp; nhng li c kh nng thay
i c nhiu thng s, c th chn c nhng iu kin ph hp theo tng i tng
phn tch hay tng nguyn t.
Yu cu cui cng l ngun nng lng kch thch phi lm tiu hao t mu phn tch v
trong mt s trng hp phi khng lm h hi mu phn tch, nh trong
17
kim tra thnh phm.

Trn y l nhng yu cu chung, nu ngun sng tha mn c y cc yu cu
l mt iu rt l tng. Song trong thc t khng c c iu kin l tng nh th. V vy,
mi ngi lm phn tch quang ph pht x cn phi hiu bit tng tn v ty theo tng
trng hp c th m xem yu cu no cn c ch nghim ngt trc ht v yu cu no
c th chnm chc c.
Cc loi ngun kch thch ph pht x
Do nhng yu cu nu trn, nn ch c mt vi loi ngun nng lng c dng
lm ngun kch thch cho phng php phn tch quang ph pht x. l: Ngn la n kh;
H quang in dng xoay chiu v mt chiu; Tia la in; Tia lc; Plasma cao tn cm ng
(ICP); tia X.
Trong cc loi ngun nng lng ny, ngn la n kh, h quang v tia la in
c dng t lu, nhng c nhy khng cao (ngun sng c in). Tia lc v ICP l
nhng ngun nng lng cho nhy cao. Nhng tia lc t c dng. V c c tia
lc ph hp cho mc ch phn tch phi c nhng trang b phc tp, tn km. Ring ICP l
ngun nng lng hin ang c ng dng ph bin v c nhiu u vit. N l ngun sng
mi c pht trin trong vng hn chc nm li y. Li khng t nh ngun lc. V
nhy ca cc ngun nng lng ny chng ta c th xem trong hnh 1.4 v bng ph lc A.
Ngn la n kh
Cu to v c im ngn la n kh
Ngn la n kh l ngun nng lng u tin c dng trong phn tch quang ph
pht x nguyn t, ngay t khi phng php ny ra i. Bunsen v Kirschoff l nhng ngi
u tin dng ngun sng ny phn tch cc kim loi kim v kim th. Nhng do s n
gin, n nh, nhy tng i v r tin, nn ngy nay n vn c s dng ph bin.
c im. Ngn la n kh c nhit khng cao (1700 - 3200 0C), c cu to n gin,
nhng n nh v d lp li c cc iu kin lm vic. Do c nhit thp, nn ngn la
n kh ch kch thch c cc kim loi kim v kim th. V ng vi loi ngun sng ny
ngi ta c mt phng php phn tch ring. l phng php phn tch quang ph ngn
la (Flame Spectrophotometry). Song v bn cht n vn l ph pht x ca nguyn t trong
ngn la. Cc cht kh t to ra ngn la ca n kh thng l mt hn hp ca hai kh
(1 kh oxy ha v 1 kh nhin liu) c trn vi nhau theo mt t l nht nh. Bn cht v
thnh phn ca hn hp kh quyt nh nhit ca ngn la v hnh dng cu to ca ngn la.
Di y l mt vi hn hp kh c s dng to ra ngn la trong php o ph pht
x:
18
Bng 2.1
n nguyn t ho mu (burner head)
Nhitb ca
kh hn hp kh
L
phnmts loi
t n
chy
to ra ngn STT
la. Tuy c nhiu
Loikiu
hnn
hp khc
kh t
nhau, nhng u c nguyn tc cu to
Axetylen
v loxy
ging nhau1 (hnh 2.4 v
2.5).
h thng
nguyn t ha mu. Song bt k mt loi
2
Butan v oxy
n no mun dng c cho php phn
t yu
v oxy
tch quang3 ph, ngoi Kh
nhng
cu nu
Nhit (oC)
2400-3100
2000-2550
2200-2500
(mc 1) n cn phi m bo trn u hn

4
Hydro v oxy
hp kh trc khi t v ngn la phi chy
2100-2300
ngoi ming
5 n.
2000-2450
Axetylen v khng kh
Hnh 2.4.
n vCu
h thng
NTH
mudng
ca hng
to. V
hnh
cu to v s phn b nhit ca ngn la, n kh gm
ba phn nh sau (hnh 2.3 v 2.4):
Philips
Phn
(a). tPhn
cng
st bo
ming
n(3)
l ng
phn ti
Trong
(1)
n mt
nguyn
ha trong
mu; (2)
Mng
him;
thi(a).
phn
mu phn
tha; ny
(4)
cht tdn
ccht
trnoxy
v nung
nngng
chun
t vo
chybung
phnaerosol
hai (b).ha;
Nhit(6)ng
trong dn cht
ng
ha; (S)
dnbmu
phn C
ny
700-1200
).
chy
; (7) (di
Vin bi
to bi 0C
aersol.
2H2thp
Phn
(b) lt
liha
camu
ngnbao
la.
Hhai
nguyn
gm:
Trong phn ny xy ra cc phn ng t chy
+ Bung ht mu v to th si kh (1)
cht kh. N khng mu hay c mu xanh
+ n
hanht.
mu (2)
nht v
nhitnguyn
ltcao
Chnh nh b l
ch c nhit cao nht ca ngn la. Nu
(2)
t bng hn hp kh axtylen v oxy hay

khng kh nn th nhit ca ngn la c
cung cp nh phn ng:
2C2H2 + 2O2 = 4CO + 2H2 + Q
Phn th ba (c) l v ca ngn la.
Trong phn ny thng xy ra cc phn ng
th cp, c mu vng v nhit thp. N to
thnh ui v v ca ngn la.
Hnh 2.5
H thng nbiulai theo k thut pneumatic
Do s phn b nhit ca ngn la nh vy, nn kh phn tch phi a mu vo vng
K: Kh mang (oxy ha); S: ng dn mu; F: Kh chy; Q: Cnh qut quay u; G:
tnm c nhit cao nht. l vng b ca ngn la v trong vng ny cc qu trnh s n
Mng bo him; A: ng dn th aetosol ln n nguyn t ha.
nh, v hiu sut kch thch ph s cao nht.
Qu trnh kch thch ph trong ngn la
Trong phn tch quang ph pht x, nu dng ngn la lm ngun kch thch th mu
phn tch phi chun b dng dung dch. Sau nh mt h thng phun
20
19
(Nebulizer system) a dung dch ny vo ngn la di dng th sng m (th si kh aersol) cng vi hn hp kh t. Khi vo ngn la, di tc dng ca nhit , trc ht
dung mi bay hi, li cc ht bt mu mn ca cc cht phn tch, ri n c t nng v
chuyn thnh hi ca nguyn t v phn t. Trong ngn la cc phn t hi ny chuyn ng,
va chm vo nhau, trao i nng lng cho nhau,... Kt qu ca cc qu trnh lm cc phn
t b phn li thnh nguyn t, b Ion ha v b kch thch. Nh vy trong ngn la tn ti c
nguyn t t do, phn t, Ion, nhm phn t v cc in t. Trong tp hp ch yu ch cc
nguyn t t do b kch thch v pht x. V th ph pht x ngn la l ph ca nguyn t
trung ha. Nguyn nhn gy ra s kch thch ph y l s va chm ca cc nguyn t vi
cc in t c ng nng ln trong ngn la. V th nhit ngn la cng cao th cc in t
c ng nng cng ln. V th n l s kch thch nhit. Do c ch ca qu trnh kch
thch trong ngn la l:
Trc ht l dung mi bay hi, li cc ht mu dng bt. Tip theo l bt mu b
nung nng, nng chy. Sau l cc qu trnh nhit ha ca cht mu xy ra theo tnh cht
ca n, v gm c.
Hai qu trnh chnh:
Nu
Eh < Ent th
mu
s ha hi, nguyn t ha to
ra cc nguyn
t t do,
chng b kch thch v pht x ^ c ph pht x (AES).

Men Xm(r).Th. ^ Men Xm(k) ^ mMe(k) + nX(k)
Me(k) + E ^ Me(k)* ^ Me O + n(Hv)
Nng lng K Chm tia pht x
C ch ny (c ch 1) cho nhy v n nh cao ca s pht x. Cc hp cht mui
halogen (tr F), axetat, mt s nitrat, sunphat... ca kim loi thng theo c ch ny.
Nu Eh > Ent th mu s b nguyn t ha trc, sau ha hi thnh nguyn t, ri b
kch thch ph ^ sinh ra ph pht x (AES).
MenXm(r) ^ Mn(r) + Xm(r) ^ mMe(k) + nX(k)
Me(k) + E ^ Me(k)* ^ Me O + n(Hv)
Nng lng K.Th. Chm tia pht x
C ch ny (c ch 2) cho nhy v n nh km so vi c ch 1 ca s pht x.
Cc hp cht mui SIO 2-3, PO3-4, F", mt s nitrat, sunphat,.. ca kim loi thng theo
c ch ny.
Do c im ca 2 c ch chnh , nn trong phn tch ngi ta thng to iu
21
kin s kch thch ph xy ra theo c ch 1 c li. iu gii thch ti sao ngi ta hay
dng cc mui halogen, v axetat ca kim loi kim lm nn, hay cht ph gia cho mu phn
tch.
Qu trnh ph
Trong ngn la thng c cc qu trnh ph km theo hai qu trnh chnh, cc qu trnh
ny ty iu kin ca ngn la m xut hin trong mc khc nhau, v n u khng c li,
nn cn c loi tr trong phn tch. Cc qu trnh l:
To ra cc hp cht bn nhit, ch yu l cc monoxit (dng Me O).
S Ion ha to ra cc Ion, ch yu l s Ion ha bc 1.
S hp th bc x ca nguyn t (qu trnh t o).
S pht x ph nn lin tc ca ht rn v electron b nung nng.
Ni chung, cc qu trnh ny u khng c li. Ngi ta phi tm bin php loi tr. V
d:
+ hn ch s hnh thnh hp cht bn nhit kiu Me O, ngi ta thm vo mu mui
Clorua ca kim loi kim (nh KCI, CsCL) lm nn, kch thch ph theo c ch
hoc kch thch ph trong mi trng kh tr argon.
+ Hay loi tr s Ion ha ca nguyn t phn tch, ngi ta thm vo mu cht ph
gia l mui halogen kim loi kim c th Ion ha thp hn th Ion ha ca nguyn t phn
tch. Nh th nguyn t phn tch s khng b Ion ha na.
So vi cc loi ngun kch thch khc, ngn la l ngun kch thch n gin, nhy
trung bnh (0,1 - 10p,g) v tng i n nh. Nhng cng ca vch ph cng b nh
hng bi mt s yu t nht nh, nh:
+ Trc ht l dng lin kt ca cc nguyn t trong cht mu.
+ Th hai l nh hng ca cc gc axit. Ni chung, cc axit d bay hi th nh hng
ny l nh.
+ Th ba l cht nn hay thnh phn ca dung dch mu, v vy dung dch phn tch v
dung dch mu chun u phi c cng thnh phn vt l v ha hc, nht l cht nn phi
cng loi.
+ nh hng th t l cc phn ng ha hc xy ra trong ngn la. c bit l nh
hng ca cc phn ng to ra cc hp cht bn nhit. Cc hp cht ny thng lm gim
cng ca vch ph, ngha l lm gim nhy ca phng php phn tch. l khi
qut chung, tt nhin cc yu t trn khng phi bao gi cng xut hin ng thi v tc dng
nh nhau trong mi trng hp, m ty tng trng hp yu t no l ni bt v cn c ch
. Song mt iu cn nh l nhit ngn la l yu t quan trng nht, n quyt nh cc
qu trnh xy ra trong khi kch thch ph.
22
H
in
binquang
tr ph
R2 tht ln (R2 >> Ri) hn ch s thay i cng dng in trong mch v
c
vn
tnhnh.
cht
gi cho
him
quang
H
ngun
c nng lng trung bnh v cng l ngun kch thch vn
Cuquang
to vlhot
ngkch
ca thch
h quang
nng. Tuy
N c
nng
c mu
dn
innhng
v khng
dn in.
ckh
nhiu
loikch
mythch
phtc
h quang
khc
nhau,
v nguyn
tcTy
cu thuc
to, ttvo
c cc
cc
thng
s (A,
C, R) u
ca my
h quang
my pht
h quang
gm pht
hai phn
chnh.v loi in cc ta chn m h quang c nhit
0C
t 3 5 00 - 60 00 Vi nhit ny nhiu nguyn t t cc nguyn liu mu khc nhau c th
Phn 1 l mch pht h quang (mch chnh), n c nhim v cung cp nng lng
c ha hi, nguyn t ha v kch thch ph pht x. Nhit ca h quang ph thuc rt
ha hi, nguyn t ha mu v kch thch m hi i n pht x. Nu h quang mt chiu
nhiu vo bn cht ca nguyn liu lm in cc. V th trong mt iu kin nh nhau, h
th l mch ca dng in mt chiu (hnh 2.6). Nu l h quang xoay chiu, th l dng
quang in cc than (graphite) c nhit cao nht (bng 2.2). Cng dng in trong
in xoay chiu.
mch h quang l yu t quyt nh nhit ca h quang.
Phn 2 l mch ch huy (mch iu khin), c nhim v ch huy phn mch chnh hot
H quang l ngun kch thch cho nhy tng i cao, v trong h quang mu phn
ng theo nhng thng s c chn cho mt mc ch phn tch nht nh. Theo s
tch c ha hi tng i d dng hn trong cc loi ngun nng lng khc, c bit l h
hnh 2.6, nu cng tc K c ng v tr AA, ta c h quang dng xoay chiu. Cn khi v
quang dng mt chiu. Nhng cng do tnh cht ny m php phn tch dng h quang c
tr BB' ta c h quang dng mt chiu. S hot ng ca h quang din ra nh s (s hnh
n nh v lp li km ngn la v tia in. y h quang dng xoay chiu cho kt qu
2.6):
n nh hn h quang dng mt chiu, v th h quang dng xoay chiu c s dng nhiu
hn. Khi ng cng tc K', ngha l a in vo my, qua h thng bin tr R; ta chn c
th lm vic ph hp a vo bin th Tr 1 tng th. Khi th hai u cun th cp ca
Bng 2.2
bin th ny t n hng ngn vn (2000-7000V). Hai u cun ny c ni vi cun cm
Th
haCvvnhit
h
mt
loi tch in v khi t n th Vf chn
Li, tIon
in
khong
nquang
ph E.ca
Lc
s
t kim
C c
1
th c mt tia in c nh qua khong E, nh th lp tc trn mch dao ng L 1c1 xut

hin mt dao ng cao tn. Do mch dao ng L 2C2 cng ghp vi mch dao ng L lC1, nn
trn mch
L2Ct
xut hin
ng ca
cao tn cm
ca L 2
2 cng
Nguyn
lm in
Th mt
Iondaoha
Nhitsvng
ca h
Dngng
innh
h th. Nhng
l ln hn nhiu
trn hai
ct ca t C 2 cng
s (A)
ln hn C 1. Th quang
ny li(oxut
ccL1s nn th
nguyn
t (eV)
C) hin
quang
tc khc khi cCtia in nh E v
iu khin s phng in
hai in cc
11,30
10 qua khong F ca
6000
h quang. NhZn
th mt chu k phng9,40
in th nht c thc
li tip din
10 hin v kt thc, ri
5200
n chu k phng in th hai, th ba,... v c th din ra cho n khi no ta ngt cng tc K',
Fe
7,80
10
4800
tc l ngng s phng in ca h quang.
Cr
6,90
10
4400
Al
5,67
10
4000
H quang l ngun kch thch c s mch tng i n gin, nhng li c nhiu

thng s c th iu chnh c chn c mt nhit tng i ph hp cho php phn
tch mi cht.
H quang l s phng in gia hai in cc c th thp (di 260V) v dng cao (t 8
- 20A). Th v dng ca mch h quang c lin h vi nhau theo cng thc:
,B
_
U
U _ A + v I _ --------
Im R + R2
m
Trong A v B l cc hng s, Ri l in tr plasma h quang. Cng thc ny gii

Hnh 2.6
thch ti sao h quang
km bn vng. V th phi a vo mch h quang mt
S nguyn tc cu to ca my pht h quang
24
23
Khi h quang lm vic, in cc F s c t nng v di tc dng ca in

trng cc in t bt ra khi b mt in cc nm, chng c gia tc v chuyn ng v cc
dng. Nhng in t ny c ng nng rt ln, v khi chuyn ng trong plasma gia hai
in cc, cc in t va chm vo cc phn t khc (nguyn t, Ion, phn t...) trong plasma
F, n truyn nng lng cho nhng phn t . Khi trong plasma c phn t b Ion ha, b
phn li v b kch thch. Kt qu li c thm in t t do na cng vi mt s nguyn t, Ion,
phn t b kch thch. Nh vy chnh cc phn t mang in tch dng v nm duy tr dng
in qua ct kh ca plasma. Gia hai in cc F cc phn t b kch thch s sinh ra ph
pht x ca n. Trong h quang mt chiu in t lun lun p vo in cc dng, nn in
cc dng nng hn in cc nm. Cn ngc li, trong h quang dng xoay chiu, hai
in cc li c t nng nh nhau.
H quang dng mt chiu thng xut hin s st th hai u ca in cc. Hiu ng
ny xut hin rt r rng trong thi gian u ca s phng in v h quang c dng thp
(di 5A). Nhng sau c nng lng ca ngun kch thch b vo th s st th s
gim i. Nguyn nhn ca s st th ny l do s xut hin lp in kp hai u ca in
cc v lp in kp ny c t trng ngc vi t trng chnh ca h quang. Vi h quang
xoay chiu, do dng in lun lun i chiu, nn s st th xut hin khng r rng v rt
t c tc dng. chnh l l do gii thch ti sao s kch thch ph pht x bng h quang
dng in xoay chiu lun lun n nh hn s kch ph trong h quang dng in mt chiu.
Nhit ca plasma h quang
Yu t th nht, yu t chnh quyt nh nhit ca h quang l cng dng in
trong mch h quang chnh. Trong mt khong nht nh ca nhit , khi tng cng ca
dng in th nhit ca h quang cng tng theo. Ngha l ta c:
T = k. I (2.2)
Trong k l h s t l, T l nhit ca h quang ( OC). Nhng n mt gi tr nht
nh ca cng dng in I 0, th nhit h quang tng rt chm theo s tng nhit
(hnh 2.7). Gi tr I 0 c gi l dng in gii hn ca h quang. Nhng cng dng in
trong mch h quang thay i tng i mnh. V ct kh ca plasma lun thay i c v
di v b rng, do im phng in trn b mt in cc lun lun di ng. l nhc im
ca h quang. Do ngi ta phi dng in cc i c hnh nn ct.
V vy, mun cho cng dng in I trong mch h quang n nh (t thay i)
ngi ta phi mc trong mch h quang h in tr R 2 tht ln, s thay i ca R1 do ct
kh gy ra t b nh hng n I. V th trong cc my pht h quang ngi ta thng lm mt
h in tr ni R2 rt ln v cng dng in c tnh theo cng thc:
25
_+R
(2.3)
trong :
R1: in tr ct kh ca plasma gia hai in cc.
R2: in tr ni ca my pht h quang.
U: Th ca ngun in ca my pht t ln hai u in cc F.
Yu t th hai quyt nh nhit ca h quang l bn cht ca nguyn liu
lm in cc. Ni chung, nguyn liu no kh bay hi v cu to t nhng nguyn t
ha hc c th Ion ha cng cao, th h quang dng in cc nguyn t s cho nhit
cng cao. V th h quang in cc than (graphite) s c nhit cao nht so vi
cc h quang in nguyn liu khc trong cng mt iu kin dng in th nghim
(bng 2.2).
Yu t th ba l th Ion ha ca cc cht c trong mu phn tch, ch yu l
cht nn v nhng cht c nng ln. Ni chung, nguyn t no (nht l cht nn ca
mu) c th Ion ha cng nh th cng lm gim nhiu nhit ca h quang, ngha l
cc kim loi kim c tc dng mnh nht, sau n cc kim loi kim th. Chnh v
th th ngi ta thng thm cc mui halogen ca kim loi kim vo mu gp
phn iu chnh nhit ca plasma ca h quang cho s kch thch ph ca cc
nguyn t phn tch. Bn cnh th Ion ha, th nng ca cc nguyn t cng c nh
hng n nhit ca h quang, c bit l cc nguyn t c th Ion ha thp s lm
gim nhit ca h quang cng nhiu, khi nng ca n trong plasma cng ln.
Trong
plasma
ca
quang thng lun lun xy ra

cc phn ng ha hc v vt l.
l qu trnh phn li, Ion ha,
t hp phn t v s kch thch
ph.
Nhng
qu
trnh
ny
thng l cc qu trnh nhit

ng
hc
hi
trong
plasma cng c mt nhit

nht nh ng vi nhng thng
s xc nh ca my pht h
quang c chn. Nhit
m bo cho plasma c mt
p lc in t xc nh duy
tr s kch thch ph.
26
S kch thch ph trong plasma h quang in

Trong plasma ca h quang, s kch thch ph pht x c th xy ra theo cc qu trnh
sau:
Nu l mu dung dch, th trc ht l dung mi bay hi,
licc ht bt
mu. Ri cc cht (c mu bt v b ca mu dung dch cn
li), bt mu b nung
nng, nng chy. Sau l cc qu trnh nhit ha ca cht mu xy ra theo tnh cht ca n.
C th l cc ht mu s bay hi hay chuyn khi vo plasma gia 2 in cc. Ti y s xy
ra cc qu trnh chnh v ph khc nhau, ty thuc vo thnh phn v bn cht ca cht mu.
Nu
mul dng bt c nhi vo trong l in cc
trnh trong in cc mang mu l:
mang th c cc qu
+ S nung nng v nng chy,

+ S chuyn ng nhit khuch tn v i lu ca cc ht trong l in cc,
+ Cc phn ng ha hc phn hy ca cc cht mu km bn nhit,
+ S bay hi ca cc phn t cht mu vo plasma,
+ S vn chuyn ca cc ht mu cha ha hi vo plasm.
Bn cht v thnh phn ca mu trong l in cc v nhit ca in cc l yu t
quyt nh s din bin ca cc qu trnh trn.
Sau l cc qu trnh trong plasma. Gm c 2 qu trnh chnh sinh ra ph pht x
nguyn t (AES) v mt s qu trnh ph nh sau:
A- Hai qu trnh chnh:
Nu Eh < Ent th mu s ha hi, nguyn t ha to ra cc nguyn t t do, chng b
kch thch v pht x ^ c ph pht x (AES)
Men Xm(r) ^ Men Xm(k) ^ mMe(k) + nX(k)
Me(k) + E ^ Me(k)* ^ Me O + n(hv)
Nng lng K.Th.
Chm tia pht x
C ch 2 ny cho nhy v n nh cao ca s pht x. Cc hp cht mui halogen

(tr F), axetat, mt s nitrat, sunphat,... ca kim loi thng theo c ch ny.
Nu Eh > Ent th phn t ca cht mu s b nguyn t ha trc, sau ha hi thnh
cc nguyn t t do, ri mi b kch thch ph ^ sinh ra ph pht x (AES).
Men Xm(r) ^ Men (r) + Xm(r) ^ mMe(k) + nX(k)
Me(k) + E ^ Me(k)* ^ Me O + n(hv)
Nng lng K.Th.
Chm tia pht x
C ch 2 ny cho nhy v n nh km so vi c ch 1 ca s pht x. Cc
27
hp cht mui SiO3, PO4, F, mt s nitrat, sunphat... kim loi thng theo c ch ny.
Do c im ca 2 c ch chnh , nn trong phn tch ngi ta thng to diu kin

s kch thch ph xy ra theo c ch 1 c li. iu gii thch ti sao ngi ta hay dng
cc mui halogen, v xetat ca kim loi kim lm nn, hay cht ph gia cho mu phn tch v
mu chun, bin i nn mu gc sang nn nhn to tt hn v li cn loi tr c cc
yu t nh hng, ng thi c khi cn tng c c nhy ln hng chc ln.
B- Cc qu trnh ph:
Trong plasma ca h quang thng c:
S hnh thnh hp cht bn nhit, ch yu l cc monoxit (dng Me O).
S pht x ph nn lin tc.
Bn cht ca cht mu, thnh phn ca mu, cht ph gia trong l in cc v nhit
ca in cc l yu t quyt nh din bin ca cc qu trnh trn.
Ni chung cc qu trnh ny u khng c li, ngi ta tm bin php loi tr.
V d:
+ hn ch s hnh thnh hp cht bn nhit kiu Me O, ngi ta thm vo mu mui Clorua
ca kim loi kim (nh KCI, CsCl,) lm nn, kch thch ph theo c ch
gia mui
halogen kim loi kim c th Ion ha thp
hn th Ion ha ca
nguyn t phn tch. Nh th nguyn t phn tch s khng b Ion ha na.
Cc loi my pht h quang
My pht h quang c rt nhiu, c nhiu hng cung cp, song xt v c ch mch
in ca mch h quang chnh, th c th chia thnh hai loi:
+ My pht h quang dng mt chiu.
+ My pht h quang dng xoay chiu.
Tuy l hai loi, nhng u c nguyn tc cu to nh nhau (hnh 2.6). Trong mi loi h
quang li c nhiu ch khc nhau. Thng thng c mt ch lin tc v nhiu ch
gin on. Chnh v th m chng ta c th chn c nhng gi tr nng lng khc nhau cho
tng mc ch phn tch c th.
Tia la in
c im v tnh cht
Tia la in l ngun kch thch ph c nng lng tng i cao. Ty theo cc thng
s ca my pht tia la in (C, L, R, T) chn, ta c th t c nhit
28
tnm plasma tia la in t 4000 - 6000 OC. V th tia la in c gi l ngun kch thch
cng (giu nng lng). Nn ph pht x ca tia la in ch yu l ph ca cc Ion bc 1 ca
cc kim loi.
Tia la in l ngun kch thch tng i n nh v c lp li cao. Nhng v
nhy li km h quang in. Do thi gian ghi ph cn phi di hn h quang.
v bn cht ca s phng in, tia in l s phng in gia hai in cc c th hiu
rt cao (10.000 - 20.000kV) v dng in rt thp (<1A). N l s phng in gin on t 50
- 300 chu k trong mt giy, ty thuc vo cc thng s ca my pht tia la in c
chn. Do in cc khng b t nng . Do c im ny m tia la in l ngun kch
thch ph hp i vi php phn tch cc mu thp, hp kim v dung dch, nhng li khng
ph hp cho vic phn tch cc mu qung, t v bt v khng ha hi tt cc mu loi
ny.
Trong tia la in qu trnh chuyn vt cht mu t in cc vo plasma l gin on
theo tng chu k phng in gia hai in cc.
Nhit ca plasma tia la in
Yu t quyt nh nhit plasma ca tia la in khng phi l cng dng in
nh trong h quang m l mt dng lc xy ra s phng tia in gia hai in cc. Nhng
mt dng in li thay i theo s phng in. N t c gi tr ln nht ti lc bt u
c tia in xy ra gia hai in cc v sau li gim v l nh nht ti thi im ngh nh
in. Qu trnh tip din mt cch tun hon theo nhng thng s ca my pht tia la in
c chn. Ni chung, trong mt gii hn nht nh, nhit plasma ca tia la in ph
thuc vo mt dng in (hnh 2.8), ngha l n mt gi tr mt dng j 0 no th nhit
ca tia in khng tng theo mt ca mt dng in na. Song mt dng in li
ph thuc vo ba thng s chnh ca my pht gia la in Vf, C, L (th, in dung, t
cm). Cho nn nhit ca tia la in cng ph thuc vo cc thng s . Ni chung n t
l thun vi
f v C v t l nghch vi t cm L. Trong ba thng s th Vf l yu t quan trong nht
v Vf li ph thuc vo:
Khong cch gia hai in cc.
Trng thi b mt ca in cc chnh v ph.
Cc thng s ca mch in nh V, C, L, I, S.
29
V vy, mun m bo cho qu

trnh phng in n nh, th phi gi
cc iu kin lm vic tht n nh.
Nhng cng khng nn chn cc
thng s mt dng t gi tr
gii hn j 0 v mt dng in ny
s phng in km bn vng v
khng n nh, tc l lm cho nhit
ca tia in dao ng nhiu. Mt
cch gn ng, trong plasma tia la
in ta c tn s phng in:
f = V LC
2n
Cng dng in:
V mt dng:
I = V14CL
j = hay a =
S
Vf4cTL
S
S kch thch ph trong plasma ca tia la in

Trong plasma ca tia la in s kch thch ph pht x xy ra cng tng t nh trong
h quang in. Nhng vi mu bt th s ha hi din ra rt km v khng n nh. Nhng do
nhit ca plasma cao nn s hnh thnh cc hp cht bn nhit, t gp hn trong h quang.
Mt khc, tia la in dng ch yu phn tch mu thp, hp kim (mu rn) v mu dung
dch. Nn cc qu trnh xy ra ch yu ch trn b mt in cc mang. C th l:
Nu l mu dung dch, th trc ht dung mi bay hi, li cc ht bt mu.
Ri cc cht
(c mu
bt v b ca mu dung
dch cn li), bt mu b nung
C th l cc ht mu s bay hi hay chuyn khi vo plasma gia 2 in cc. Ti s xy ra
cc qu trnh chnh v ph khc nhau, ty thuc vo thnh phn v bn cht ca cht mu.
Nu mu l dng rn, mu l chnh in cc mang, th c cc qu trnh trong in cc
mang mu l:
+ S nung nng b mt v b bn ph,
+ S vn chuyn ca cc ht mu cha ha hi vo plasma,
Bn cht ca mu, thnh phn ca mu, th phng in, v nhit b mt ca
30
in cc l cc yu t quyt nh din bin ca cc qu trnh trn.

Sau l cc qu trnh trong plasma. Gm c 2 qu trnh chnh sinh ra ph pht
x nguyn t (AES) v mt s qu trnh ph nh sau:
A- Hai qu trnh chnh
A1- Khi mu l dung dch nh ln in cc
kch thch v pht x ^ c ph pht x (AES).
Men Xm(r) ^Men Xm(k) ^ mMe(k) + nX(k)
Me(k) + E ^ Me(k)* ^ Me O + n(hv)
C ch 1 ny cho nhy v n nh cao ca s pht x. Cc hp cht mui
halogen (tr F), axetat, mt s nitrat, sunphat,.. ca kim loi thng theo c ch ny. Nu Eh
> Ent th phn t ca cht mu s b nguyn t ha trc, sau ha hi thnh cc nguyn t
t do, ri mi b kch thch ph ^ sinh ra ph pht x (AES).
Men Xm(r) ^Men (r) + Xm (r)^ mMe(k) + nX(k)
Me(k) + E ^ Me(k)* ^ Me O + n(hv)
C ch 2 ny cho nhy v n nh km so vi c ch 1 ca s pht x. Cc hp
cht mui SiO3, PO4, F, mt s nitrat, sunphat,... kim loi thng theo c ch ny.
Do c im ca 2 c ch chnh , nn trong phn tch ngi ta thng to iu kin
cc mui halogen v axetat ca kim loi kim lm nn, hay cht ph gia cho mu phn tch v
yu t nh hng ng thi c khi cn tng c c nhy ln hng chc ln.
A2- Khi mu l thanh kim loi lm in mang
+ Lp
cc nguyn t trn b
mt in
cc, di tc dng ca lc
in trng
in mnh (v th phng in rt cao gia 2 in cc, 15- 20 kV), nn cc nguyn t b bt ra

khi mt in cc v bay vo plasma, hoc l dng hi, hay l dng ht rn. Sau c cc qu
trnh sau:
Ha hi ca ht rn:
Men) + E1 ^ Me(k)
Nguyn t b kch thch:
Me(k) + E2 ^ Me(k)*
Nguyn t b Ion ha:
Me(k) + E3 ^ Me(k)+
Ion b kch thch:
Me(k)+ + E4 ^ Me(k)+*
31
Pht x ca nguyn t:
Me(k)* ^ Me(k) + n(hv)
Pht x ca Ion:
Me(k)+* ^ Me(k) + n(hv)
Trong : n(hv) l chm tia pht x ca nguyn t hay Ion b kch thch.
Cn El, E2,.. l nng lng nhit do plasma tia in cung cp.
B- Cc qu trnh ph
Trong plasma gm c:
S hnh thnh hp cht bn nhit, ch yu l cc monoixtit (dng Me O).
ca in cc l yu t quyt nh s din bin ca cc qu trnh trn.
Song qu trnh ph trong plasma tia in khng mnh nh trong ngn la v trong h
quang, ch c s Ion ha l ng k. V th cc kim loi kim phi o theo cc vch Ion bc 1.
d vi mu dung dch:
Clorua ca kim loi kim (nh KCI, CsCL,) lm nn, kch thch ph theo c ch
Vy, loi tr s Ion ha ca nguyn t phn tch, ngi ta thm vo mu cht ph gia
mui halogen kim loi kim c th Ion ha thp hn th Ion ha ca nguyn t phn tch. Nh
th, nguyn t phn tch s khng b Ion ha na.
Cc loi my pht tia in
V nguyn tc cu to, my pht tia la in cng c hai loi: my pht tia la in c
ch huy v my pht tia la in khng ch huy. Song trong mc ch phn tch quang ph
pht x, ngi ta ch dng my pht tia in c ch huy. Trong loi my pht ny, vic ch huy
(iu khin) cng theo hai nguyn tc v ng vi hai cch iu khin ny ngi ta ch to hai
loi my pht tia in khc nhau:
+ My pht tia in dng hai tia in, tia in chnh, tia in ph (hnh 2.9), tng t
nh my h quang.
+ My pht tia in dng ngt in ng b (hnh 2.10), ngha l iu khin bng m t
ng b.
My pht tia in dng hai tia din (hnh 2.9)
32
Trong my ny c mt tia in chnh v mt tia in ch huy. Theo s hnh

2.9, khi ng mch in K, bin th Tr c np in v tng th ln hng ngn vn
(V). Lc h t in C c tch in v th hai ct ca t C l th ca khong n
gia hai qu cu E. Lc ny trn mch in LC khng c dng in, t C c tch
in cho n khi t c th V f (th phng in gia hai qu cu E) th tia in s
nh qua hai qu cu E, t C phng in qua E lm cho trn mch dao ng LC xut
hin tc khc mt dao ng cao tn, dao ng ny khng qua c L 2 (hay Ri); do
bt buc phi nh qua khong n F (khong cch gia hai in cc chnh). Nh vy,
h c mt dao ng v mt tia in nh E, th cng c mt tia in phng qua F,
ngha l tia
in
E iu khin
trnh
c th tip
tia
in F. Sau
qu
din cho
n khi ta ngt cng tc K.

Mun cho qu trnh phng in
c n nh th hai qu cu E phi c
kch thc xc nh, khong cch
khng i v b mt phi nhn. C
nh th in th Vf mi c nhng gi
tr xc nh ng vi tng cp thng s
ca my pht tia in c chn,
m bo cho qu trnh phng in
F n nh v mt nng lng, v c
hai tia in xy ra ng thi, nn nng
lng phi chia i hai khong n E
b
b
^
,
7
v F. V th mun c nng lng ln
Hrnh 2 9
My pht tiain dng hia tia in
(nhit cao) th th Vf phi rt ln.

My pht dng ngt in ng b (hnh 2.10).
My pht loi ny ch to
theo s ca Fressner. y s
phng in c ch huy nh mt
m t ng b c gn b ngt in
mc ngay trn mch ca my pht
tia in. My pht gm bin th Tr
tng th, mch dao ng LC,
khong
phng
in
chnh
F, hai
cun cm Li5 L2 ngn khng cho

dao ng cao tn tr v bin th Tr
v m t ng b M ng v
m mch in ca qu trnh phng Hnh 2.10
in gia 2 in cc F
.
My pht
tia
in dng ngt in
33
Khi cho in vo my, bin th Tr tng in, t C c tch in dn, m t M quay u

c mang theo hai tip im A v A, cng quay, khi n v tr B v B1 mch in trong my
c ng, lc th t C cng t cc i, khin cho tia in phi phng qua F, sau tia
in li tt. Nhng v m t M quay u lin tip, nn tia in cng nh u n lin tip qua
F theo s quay ca mt M tun hon n v tr B v B1 ln lt theo thi gian chu k
c chn, cho n khi no ta ngt cng tc K. Nh vy, chnh m t ng b M iu
khin s phng in theo cc thng s c chn.
Plasma cao tn cm ng ICP
c im v tnh cht
y l ngun nng lng mi c s dng trong php phn tch quang ph pht x
nguyn t khong 10 nm li y; song li c s dng rng ri v c hiu qu cao v n c
nhng c im sau y:
Ngun nng lng ny c nhit cao. Thng thng tnm ca plasma c th t c
nhit t 5000 - 10000 OC nn ha hi v nguyn t ha c ht mi trng thi ca vt liu
mu vi hiu sut cao. Vi plasma ny, mi nguyn t kim loi u b kch thch to ra ph
pht x ca n. Cc hp cht bn nhit cng b ha hi v phn li thnh nguyn t t do,
nhng trong ngun nng lng ny ph pht x ca Ion l ch yu.
ICP (Inductivity Coupled Plasma) l ngun nng lng kch thch ph pht x m bo
cho php phn tch c nhy rt cao. Ni chung c th t t n.10 -4: n.106% (0,l - 5) ngng
i vi hu ht cc nguyn t. Tt nhin nhy ca php phn tch y ph thuc nhiu
vo cng sut ca my pht cao tn HF to ra plasma ICP (hnh
2.11).
ICP l ngun kch thch ph khng nhng c nhy cao, m cn c n nh cao.
N hn hn h quang v tia in. V th php phn tch dng ngun nng lng ny cho sai s
rt nh; ni chung l nh hn 10% trong vng nng t n.10 -3- n.10-5%.
34
kW
12
Hnh 2.11
S ph thuc ca cng vch ph vo cng sut my pht cao tn ICP
Tuy c nhit cao nhng s kch thch ph pht x trong ngun nng lng ny li rt
m du. N tng t nh s kch thch ph trong ngn la n kh. Chnh v th m phng
php phn tch t n nh cao v sai s nh.
Vi ngun nng lng ny, ngi ta c th nh lng c ng thi nhiu nguyn t
mt lc, nn tc phn tch rt cao (t 40 - 120 mu/gi). Mt khc, khi dng ngun nng
lng ICP, vng tuyn tnh ca phng php nh lng l rt rng (t 1 - 10.000 ln).
c im cui cng l rt t xut hin nh hng ca cht nn (matrix effect).
l im hn hn cc ngun nng lng c in nu.
Chnh do nhng c im v u vit ca ngun nng lng ICP nh th, nn n

nhanh chng c ng dng rng ri v thay th cho ngun nng lng c in: tia in v h
quang. Tt nhin, trang b to ra ngun nng lng ny t hn. Nhng trong iu kin
ngy nay v do tnh cht u vit ca n nn cc phng phn tch quang ph pht x u c
trang b loi ngun nng lng ny.
Cu to ca h thng 1CP
V nguyn tc, h thng thit b to ra ngun nng lng ICP gm hai phn chnh:
my pht cao tn HF v h thng to th si kh v n nguyn t ha kch thch ph ca mu
phn tch.
My pht cao tn HF
Cc my ny lm vic tn s rt cao nhng ph bin l hai tn s 27,12 MHZ v 450
MHZ. Trong my trung tn s 27,12 MHZ c s dng nhiu hn. l tn s sng
mang rai. My pht cao tn HF c nhim v pht tn s cao cung cp nng lng cho
cun cm cao tn u ming n nguyn t ha mu, to ra plasma nhit cao cho s ha
hi mu, nguyn t ha v kch thch ph (hnh 12a).
35
Phn th hai ca h thng ICP l b phn nguyn t ha mu, bao gm b phn to soi
kh mu v n nguyn t ha mu (nebulizer system v khch bumer). B phn burner c
ch to bng thch anh chu nhit. N gm ba ng lng vo nhau, gn chc vo nhau phn
y, v mi ng u c ng dn kh vo (hnh 2.12a). Trong , ng trong cng l mt ng
mao dn dn mu vo plasma nh kh mang; ng th hai l ng to ra kh plasma. Cn
ng th ba l ng to kh lm lnh cho n nguyn t ha. Pha ngoi ng th ba v ngay
u c cun cm cao tn bng ng. Cun cm ny c ni vi my pht cao tn HF v lun
c lm lnh bng dng nc chy qua khi lm vic. ng thi chnh cng sut lm vic
ca cun cm ny s quyt nh nhit ca plasma kch thch ph. Cn h thng nebulizer,
v nguyn tc, hon ton tng t nh trong ngn la n kh nu trn.
Kh dng trong plasma ca ICP l cc kh tr nh argon, hli, nit. Trong argon l u
vit nht. y ngi ta c th dng kh mang v kh plasma l argon, cn dng nit lm
lnh. Hoc c th dng ch mt kh Ar cng c. Trong tng lng kh cho c ba dng l
t 13 - 18 lt/pht v c phn chia nh nhau:
Kh mang: 0,7 - 1,0 l/pht.
Kh plasma: 6 - 8 l/pht.
Kh lm lnh: 5 - 9 l/pht.
Nhng ngy nay, ngi ta ci tin v dng loi mini - ICP nn ch cn n 1/3 lng kh
so vi loi thng thng nu.
Hnh 2.12a
H thng ngun ca ICP-AES
Nhit ca plasma ICP
ICP l ngun nng lng kch thch ph c nhit cao, nhng li n nh hn so vi
cc loi ngun kch thch khc, nh h quang, tia la in. Nhit ca plasma ca ngun
ny c quyt nh bi dng in cm ng trong cun cm A u ca n nguyn t ha,
tc l nng lng cao tn ca my pht HF. V vy, ng vi nhng thng s nht nh ca
my pht HF th plasma ny c mt nhit xc nh. Trong cc thng s ca my pht HF,
cng sut v tn s cm ng l hai thng s quan trng
36
nht. Song mi my pht thng ch dng mt tn s cm ng nht nh 27,12 MHZ hay 450
MHZ, nn cng sut ca my pht ng vai tr chnh. V th cng ca vch ph ph
thuc vo cng sut ca my pht HF (hnh 2.11).
Tt nhin, bn cnh cn c nhng yu t khc nh hng n nhit ca plasma
ICP. Trc ht l tnh cht ca kh plasma, kh mang v tc chy ca chng vo plasma.
Sau l thnh phn ca hn hp mu c dn vo plasma kch thch ph. Ni chung
dng lin kt, th Ion ha ca cc nguyn t cng c nh hng n nhit ca plasma.
Nhng cc yu t ny khng mnh nh trong h quang v tia in. Yu t matrix effect cng
c tc dng, nhng cng khng ln nh trong ngn la n kh v trong h quang in. Cc
yu t trn nh hng n nhit ca plasma, tc l nh hng n cng ca vch ph.
Nhng khi chn c cng sut ln ph hp, th nh hng ny s rt nh, hay khng cn
na.
S kch thch ph pht trongplasma ICP
Khi ta ng mch in ca my pht cao tn HF th cun cm A u n s xut hin
tc khc dng in cao tn cm ng c nng lng ln. Nng lng ny c quyt nh bi
cc thng s ca my pht HF c chn. ng thi tia la K cng c bt, hn hp
kh v mu c t chy, plasma nhit cao xut hin, ngha l ngn la hnh thnh. Trong
ngn la nhit cao ny, trc ht dung mi bay hi ( phn trong, phn ti ca ngn la),
li cht mu dng ht bt mn. Ri cc bt mu ny b nung nng, nng chy, c ha
hi, phn li, b nguyn t ha v Ion ha to ra trong plasma c phn t, nguyn t, Ion,
in t trng thi kh. Trong ch yu l cc nguyn t, Ion v in t. Sau cc phn t
kh ny c trong plasma s b kch thch v sinh ra ph pht x. Bn cht s kch thch ph
y l s kch thch nhit, n ging nh s kch thch ph pht x trong ngn la n kh.
Nhng v plasma c nhit cao (nng lng ln) nn hiu sut nguyn t ha v kch thch
ph cao v ph ca ngun nng lng ny vi cc kim loi kim v kim th ch yu l ph
ca cc Ion bc 1. C ch ca qu trnh trong plasma ICP c th tm tt theo s sau:
37
Hnh 2.12b
Hai loi my o ph pht x ICP (ICP-AES)
HF: My pht cao tn; Pm: H thng nguyn t ha mu; L: Thu knh; T: Khe sng; G:
Cch t; PM: H nhn quang in; >>: H in t; Mr: My tnh; Sig: B ch th kt qu o;
AB: Cung mt phng tiu; M h M2: cc gng chun trc v hi t.
Trc ht l dung mi bay hi, li cc ht bt mu. Tip theo l bt mu b nung
Ba qu trnh chnh: Cc qu trnh chnh y cng tng t nh trong ngn la n kh.
Nhng c khc ngn la n kh l hiu qu ha hi, nguyn t ha v kch thch ph cao hn
nhiu.
Nu Eh < Ent, th mu s ha hi, nguyn t ha to ra cc nguyn t t do, chng b
38
Me(k) + E ^ Me(k)* ^ MeO + n(hv)

Nng lng K.Th.
Chm tia pht x

(tr F), axetat, mt s nitrat, sunphat,.. ca kim loi thng theo c ch ny.
Nu Eh > Ent, th phn t ca cht mu s b nguyn t ha trc, sau ha hi thnh
Men Xm(r) ^ Men(k) + Xm(k) ^ mMe(k) + nX(k)
Me(k) + E ^ Me(k)* ^ Me O + n(hv)
Nng lng K.Th.
Chm tia pht x

cht mui SiO3-2, PO4-3, F, mt s nitrat, sunphat... ca kim loi thng theo c ch ny.
S Ion ha sinh Ion, sau cc Ion b kch thch v sinh ra ph ca n.
C th l:
Me(k) + Ei ^ Me(k)+ + e Me(k) + E ^ Me(k)+* ^ Me O + n(hv)
V trong ngun ICP c nhit cao, nn cc kim loi c th Ion ha thp s din ra theo
c ch ny, v d cc kim loi kim, kim th.
Qu trnh ph gm c:
+ To ra cc hp cht bn nhit, ch yu l cc monoxit (dng Me O). Nhng trong
plasma ca ngun ICP th cc qu trnh ny xy ra khng ng k. chnh l u vit ca
ICP.
+ S hp th bc x ca nguyn t (qu trnh t o).
+ S pht x nn (nhng cng nh).
+ S
Ion habc hai ca nguyn t
kim loi kim v cc nguyn t c
th Ion
ha bc hai thp.
39
Ht mu
Ha hi
Nguyn t ha
Ion ha
Kch thch ph
(nu E hh < Engt )
Hnh 2.13 S qu trnh nguyn t ha

mu
Nguyn tc v cch chn ngun kch thch ph
Cc iu kin kch thch ph l nhng yu t c nh hng trc tip n cng ca
vch ph v nhy ca phng php phn tch. V th chn ng cc iu kin kch thch
ph l mt m bo cho phng php phn tch t kt qu chnh xc, tin cy v nhy
cao. Mt khc, qua vic chn c iu kin kch thch ph ph hp ta c th loi tr c
mt suyn t nh hng, nh matrix effect, nng cao nhy. Do chn c nhng iu
kin, ngun kch thch ph ph hp cho mt i tng phn tch no chng ta phi da
theo mt s nguyn tc c bn sau y:
Phi xut pht t i tng phn tch thuc dng mu no (mu bt, mu rn, mu dung
dch hay hp kim), cng nh nhng tnh cht c l ca tng loi mu thuc loi mu d bay
hi hay kh bay hi, dn in hay khng dn in. V d khi phn tch mu bt (qung, t
,...) th h quang c dng trn 10A l thun li. Song khi phn tch mu hp kim th tia in
li u vit. Mu dung dch dng ICP.
Phi da theo tnh cht v c trng s kch thch ph ca mi nguyn t cn xc nh
m chn ngun nng lng kch thch v cc thng s ca ngun kch thch. V d phn tch
kim loi kim th nn dng ngn la n kh hay h quang gin on.
V th kch thch ph pht x ca cc kim loi kim l khng ln (3 - 5eV).
40
Ngc li, vi cc nguyn t V, Zn, W,... hp cht bn nhit, li phi chn ngun kch thch c
nng lng cao, h quang in dng ln hay ngun ICP.
Khi chn ngun kch thch phi m bo cho php phn tch c nhy cao, n nh,
c th d dng phn tch c cc nguyn t c nng nh.
Chn ngun kch thch phi m bo cho php phn tch tiu tn t mu v khi cn phi
khng ph hy mu. Yu t ny trong mt s trng hp khng yu cu, bt buc nh ba yu
t trn.
Cng vch ph pht x nguyn t
Cng vch ph :
Trong ngun pht sng hay trong plasma, nguyn t (A o) ca mt nguyn t c kch
thch t trng thi nng lng thp Eo, ln trng thi nng lng cao. Cm c biu din theo
phng trnh:
Ao + XE = A* (a)
Vi mu phn tch c nng xc nh ca A o th qu trnh ny lc u tng nhanh, sau
chm dn v ti mt thi im nht nh th khng tng na. Ngha l s nguyn t A o b
kch thch l khng i, ng vi mt nhit xc nh ca plasma. ng thi vi qu trnh
trn l qu trnh ngc li, tc l nguyn t b kch thch A* gii phng nng lng m n
nhn c di dng cc tia pht x n(hvi) tr v trng thi nng lng thp bn vng
ban u. Chnh qu trnh ny l qu trnh pht x ca nguyn t v sinh ra ph pht x ca
nguyn t, c th c biu din theo phng trnh:
A* = hv + Ao (b)
Qu trnh ny lc u chm, sau tng dn theo s nguyn t A* b kch thch v
n mt thi im nht nh th cng khng tng na ng vi mt nhit nht nh ca
plasma. Ngha l sau mt thi gian nht nh ca s kch thch ph, th hai qu trnh trn (a)
v (b) s t n trng thi cn bng. l hai cn bng ng hc thun nghch. Cn bng
ny ch ph thuc ch yu vo nhit ca plasma, ngha l s nguyn t A* b kch thch v
pht x l khng i, ng vi mt nhit xc nh ca plasma.
Nu gi Nm l s nguyn t ca nguyn t Ao b kch thch n trng thi nng lng
cao cm, th theo quy lut Bolzmans ta c:
N = N gme(-Ev )/Kt
m
a _
m'
g0
go v gm l trng lng thng k
ca nguyn t
A trng thi ban u, nng
lng Eo v trng thi kch thch nng lng cm;

Na l s nguyn t ca nguyn t Ao c trong plasma (trng thi hi);
41
Em l nng lng kch thch nguyn t o t trng thi Eo ln trng thi cm;
T l nhit ca plasma (oK);
k l hng s Bolzmans.
Nu gi Ia l cng ca vch ph do qu trnh kch thch ph ni trn sinh ra,
th trong mt gii hn nht nh ca nhit plasma v nng ca nguyn t Ao trong
plasma, ngi ta thy Ia ph thuc vo:
S nguyn t Ao b kch thch ln trng thi A*, (N m).
Thi gian tn ti ca nguyn t A* trng thi kch thch, (trn).
Nng
lng kch thch nguyn
t A t
trng
thi c
bn n
trng thi kch

thch, (Em).
Xc sut chuyn mc ca nguyn t A t trng thi kch thch nng lng C m v trng
thi ban u nng lng Eo, (Amo).
V mi quan h ny c th biu din theo cng thc sau:
Ia = f. f .Amo A . ^-hv.e-(E)/kT
tg
m
o
Nhng i vi mt loi nguyn t v trong mt iu kin th nghim nht nh ca
plasma (ch yu nhit plasma) th cc yu t tri Amo, go, gm, cm, hv l nhng hng s.
Cho nncng
nguyn
vch ph Ia ch cn
ph
thuc vo
kch
thch Na m thi. Nh vy ta c:
I =KN
a
Vi
k = f. t-. A .A . ^ .hv.e-(E)/
t
a
mo
(2.6)
kT
oo
l cng vch ph ca nguyn t.

Song cng thc (2.6) mi ch cho ta bit mi quan h gia cng vch ph I a v
nng ca nguyn t trng thi hi trong plasma, m cha ch cho ta c mi quan h
gia cng vch ph v nng ca nguyn t trong mu phn tch. Mun th ta phi xt
mi quan h gia nng C trong mu v s nguyn t N a trong plasma. Ni chung, mi quan
h ny l phc tp, n ph thuc vo nhiu yu t, nh:
Kh nng ha hi, bn cht ca cht mu, cht nn;
Thnh phn ca mu, cht ph gia thm vo;
Trng thi lin kt, tn ti ca cht mu;
Cc iu kin ha hi, nguyn t ha mu, kch thch ph;
Mi trng kch thch ph, v.v...
42
Tuy nhin ngi ta thy t thc nghim, trong mt phm vi nht nh ca nng
C th ta lun lun c:
Na = k2.Cb (2.7)
Nh vy, cng vch ph s l:
Ia = a.Cb (2.8)
Trong : a: k1.k2 v a c gi l hng s thc nghim. N ph thuc vo tt c cc
iu kin thc nghim ha hi, nguyn t ha v kch thch ph mt nguyn t. V th trong
mt php phn tch phi gi cho cc iu kin thc nghim n nh, m bo a thc s l
hng s ca php o. Cn b l hng s bn cht, n ph thuc vo bn cht ca tng loi
nguyn t, b ch nhn nhng gi tr bng 1 v nh hn 1, nhng ln hn 0. Gi tr ca b nh
hn 1 khi nng C ln, cn khi C nh th b lun lun bng
Khi b nh hn 1 l lc qu trnh t hp th xy ra. Qu trnh t hp th xy ra cng nhiu
(mnh) th b cng nh xa 1, tc l chnh hng s b l c trng cho qu trnh t o ca mi
loi nguyn t. Do , ng vi mi nguyn t v vi mi mt vch ph pht x v trong
nhng iu kin nht nh, ta lun c mt gi tr nng Co, m:
+ Khi vi mi Cx < Co th b lun lun bng 1.
+ Khi vi mi Cx > Co th b nh dn xa 1 (hnh 2.14).
Trn y cp n cng ca vch ph nguyn t trung ha nhng trong plasma
cn c c cc Ion. Chng cng b kch thch v sinh ra ph pht x. Qu trnh kch thch v
pht x cng ging nh cc nguyn
tvcng tnh ton hon ton
tng t nn chng ta c cng vch ph Ion l:

li = Al. Cb (2.9)
Hnh 2.14
Quan h gia cng vch ph v nng
c
Do , mt cch tng qut, ta c th vit cng vch ph pht x: I =
a.Cb
(2.10)
43
Cng thc (2.10) l phng trnh c bn ca phng php phn tch nh lng theo
ph pht x nguyn t. Phng trnh ny do Lmakins (Nga) v Saiber (c) tm ra, nn gi
l phng trnh Lmakins-saiber.
Cng vch ph v nhit plasma
Nh trn chng ta bit, cng vch ph pht x ca nguyn t c tnh theo biu
thc sau: Ia = Pa.N(l-x)e
V vch Ion:
Ii = Pi.N.x.e
(2.12)
l
g
Trong , vi:
P = Aa .hv
t
g
-E(m)/kT
-Em/kT
am
oo
iu ny cho thy cng ca vch ph ph thuc vo nhit ca plasma.

Nhng, tt nhin, s ph thuc ny i vi vch nguyn t v vch Ion l khc nhau v
khng n iu, m theo hm s m (e -Em/kT). Chnh hai cng thc trn d dng cho ta thy
rng, nhit no ca plasma to ra c s nguyn t N(1 - x) trong cng thc tnh cng
vch nguyn t v s phn t (N.x) trong cng thc vch ph ln l ln nht, th lc s
c c cng ca vch ph ln nht. l nhit ti u ca s kch thch ph.
100
200
300
100
200
Ca: 4226,70 /nn Al 20 3; Ca: 4226,70 /nn Si0 2 AI: 3093,00 ; Mg: 2852,19 ;
Si 2516,00 A;Sn: 2355,00 .
Hnh 2.15
S ph thuc ca cng vch ph vo nhit trung tm plasma
44
300
400
Vi mt vch ph ca mt nguyn t, thc t ch c mt nhit to ra c cng I

cc i. Nhit ny c gi l nhit ti hn ca vch ph v c k
l
To. Ttnhin
hiu
i vi mivch th nhit To ny khc nhau (hnh
2.15a,b,c). Ngay i vi vch ph ca mt nguyn t, nu n tn ti trong cc nn mu khc

nhau (matric khc nhau) th nhit T o ny cng khc nhau (hnh 2.15c). iu c ngha l,
ngoi
bncht ca chtphn tch, nhit
To cn phthuc vo
thnh phn v nn ca mu phn tch.

Tnh cht ny c ngha thc t rt ln khi xc nh lng nh cc nguyn t trong mu
phn tch. V trong nhng trng hp ny ta cn phi chn nhng iu kin lm vic v iu
kin kch thch ph sao cho thu c vch ph c cng ln nht, tc l chn cc iu kin
kch thch ph c c nhit ca plasma gn vi nhit T o ca vch ph cn o, hoc
bng ng c To l l tng. Tt nhin bng c l trng hp rt him, ta ch c th lm
cho nhit ca plasma cng gn vi nhit To th cng tt.
Hin tng t hp th (t o)
trng thi hi trong plasma, hin tng mt nguyn t c kh nng hp th tia bc x
do chnh mt nguyn t khc cng loi ca chng pht ra c gi l hin tng t hp th
(hay t o). Hin tng ny xy ra theo nh lut Kirschhoff. Ngha l mt nguyn t ch hp
th nhng tia bc x m chnh n c th pht ra c trong qu trnh pht x. Hin tng ny
thng xy ra mnh v ch yu i vi cc vch cng hng, vch
ph pht
x ca mtnguyn t, v
cuicng
ca
nng cng
ln, th hin tng ny xy ra cng mnh. Chnh do hin tng ny, m a n kt qu lm

cho cng vch ph pht x I khng ph thuc tuyn tnh vo C, khi nng C tng gi
tr Cx > Co, Gi tr Co c gi l nng gii hn, cn c quan h gia I v C l tuyn tnh.
Vi mi vch ph, C o l khc nhau. Vch cng nhy th C o cng nh. ng thi, trong qu
trnh pht x, cng sut pht x ca mt vch ph c tnh theo cng thc:
W = f.Wo
(2.13)
vi f l h s hot ng pht x ca vch ph v n nhn gi tr: 0 < f < 1.
Khi khng c hin tng t o, ngha l nng Cx nh hn Co th f = 1, tc l W =
Wo. Cn mi trng hp khc, khi c hin tng t o th lun lun c W < W o. Trong :
o
= j A .N .hv.e- m )dv
m
kT
(2.14)
0
y: Na l s nguyn t trong n v th tch V ca plasma.
Amo l xc sut chuyn mc;
Cm l nng lng kch thch trng thi mi T
l nhit ca plasma (oK);
45
hv l lng t sng c bc x ra; k

l hng s Bolzmans.
V ngha thc t, khi hin tng t hp th xut hin, ni chung u khng c li cho
php phn tch ph pht x nguyn t. iu c ngha l trong phn tch khng nn xc nh
mt nguyn t vng nng bt u xut hin hin tng t o, tc l nm ngoi vng
tuyn tnh, phi pha long mu kt qu s chnh xc hn.
Bc x nn trong ph pht x
Khi kch thch mu phn tch ta thu c ph pht x ca n. Ph ny gm c ph vch
ca nguyn t v Ion, ph m ca phn t v nhm phn t. Sau n ph nn hay gi l bc
x nn. Bc x nn thng l ph lin tc. N to thnh mt di en m trn ton b vng
ph ca mu phn tch. en ca di ph nn ny mi vng ph l khc nhau. Thng
thng vng sng di m hn vng sng ngn. Nhn chung, n tng dn t vng sng
ngn sang vng sng di, n th hin r rt vng kh kin (360 - 500 mm). Cn vng t
ngoi (UY) th ph nn thng rt nh.
Trong mt mc va th bc x nn l c li v n lm nn cho vch ph xut
hin ln trn m hn, ngha l lm tng cng ca vch ph. Do , trong mt s
trng hp nn qu yu ngi ta thng phi chiu sng ph knh nh bng nh sngtrng vi
mt thi gian phhp. Song trong nhiu
trng hp
ph nn
thng qu mnh, c bit l trong vng kh kin v khi dng h quang. Lc ny n che lp
mt vch ph ca nguyn t phn tch, nht l nng nh. Trong trng hp ny ngi ta
phi tm cch kh bt bc x nn. Vy nguyn nhn no gy ra bc x nn ?
T nhng kt qu nghin cu ngi ta thy c cc yu t sau y to ra bc x nn (ph
nn):
S pht sng ca ht vt rn c t nng trong plasma.
Tc dng ca nh sng trng.
S bc x ca in t trong plasma nhit cao.
Do in cc b t nng sng v pht x (vt rn pht sng nhit cao).
Trong ba yu t ny, yu t th ba th hin khng r nt bng hai yu t u. loi tr
bc x nn ngi ta c th p dng nhiu bin php khc nhau. V d vi nguyn nhn th
nht, ngi ta dng mn chn trc khe sng khng cho nh sng do hai u in cc c
t nng chiu vo khe my quang ph. Hoc cng c th thm cht ph gia vo mu phn
tch kh bt mt phn cng nn, lm cho nn ca ph khng qu en. Nhng tt nht
l kch thch ph trong mi trng kh tr Ar (argon) hay hn hp ca kh tr Ar v oxy theo
nhng t l ph hp. Bin php ny loi tr c c ph nn v ph xm ca nhm CN v ph
phn t H2O, mt khc li cn tng c cng vch ph, ngha l tng c nhy ca
phng php phn tch. l u vit ca mi trng kh tr trong s kch thch ph pht x
nguyn t.
46
Chng 3
MY QUANG PH V S PHN LI CHM SNG
Nguyn tc cu to ca my quang ph pht x

My quang ph l mt dng c dng thu, phn li v ghi li ph ca mt vng ph
quang hc nht nh. Vng ph ny l mt i ph ca vt mu nghin cu t sng ngn n
sng di. Ty theo b phn dng phn li nh sng trong my da theo hin tng vt l no
(khc x hay nhiu x) m ngi ta chia cc my quang ph thnh hai loi.
My quang ph lng knh. l nhng my quang ph m h tn sc ca chng c
ch to t 1 hay 2 hoc 3 lng knh. S phn li nh sng y da theo hin tng khc x ca
nh sng qua hai mi trng c chit sut khc nhau (khng kh v thy tinh hay khng kh v
thch anh).
My quang ph cch t. L nhng my quang ph m h tn sc l mt cch t phng
hay lm phn x. Bn cht ca s tn sc nh sng y l s nhiu x ca tia sng qua cc
khe hp.
Tuy c 2 loi my quang ph khc nhau, nhng v nguyn tc cu to th u nh nhau,
u gm 3 phn chnh. l h chun trc, h phn li v h hi t chm sng (hnh 3.1).
H chun trc v phn u ca my quang ph. N gm mt hay mt h
thng thu knh ghp vi nhau hay h gng hi t v mt khe hp (khe vo ca chm sng
v c th iu chnh c) t tiu c ca h thu knh ny. H chun trc c nhim v nhn
v to ra chm sng song song hng vo h tn sc phn li thnh ph.
Htn
sc. lmth thng
lng knh hay mt
tm cch t. H ny c
nhim v phn li (tn sc) chm sng a sc thnh cc tia n sc, tc l phn li mt ngun
sng phc tp nhiu bc sng khc nhau thnh mt di ph ca chng theo tng sng ring
bit lch i nhng gc khc nhau. Nu h tn sc c ch to bng lng knh th chng ta c
my quang ph lng knh. V ngc li, nu h tn sc l cch t ta c my quang ph cch
t. Trong my lng knh, tia sng ngn s b lch nhiu, sng di lch t, cn trong my cch
t th ngc li.
47
-1^
<D
H bung nh. l mt h thng thu knh hay mt h gng hi t v mt

mt phng tiu ca cc chm sng. H ny c nhim v hi t cc tia sng c cng
bc sng sau khi i qua h phn li li vi nhau to ra nh ca khe my trn mt
phng tiu. chnh l cc vch ph.
Thm vo l mt s b phn ph khc my quang ph c th hot ng
c chnh xc, d dng v c hiu qu cao hn. V d nh:
H thng gng hay thu knh chiu sng khe my.
H thng gi in cc.
Cc loi chn sng v lc sng trc khe my.
B phn t ng a mu.
My tnh v phn mm iu khin v x l s liu.
Cc loi my quang ph pht x
Lng knh v my quang ph lng knh
Lng knh v my quang ph
Lng knh l mt b phn quan
trng ca my quang ph lng knh.
N
quyt
nh
kh
nng,
tnh
cht
phn li nh sng ca my quang ph.

Lng
knh
sut,
ng
nht
mt
mi
trirng
trong
ng
hng
trong
mt vng ph nht nh. N c gii

hn bi 5 mt phng, nh trong hnh B
ta c: ABC v A,B'C' l hai mt Hj h32
tit din ca lng knh, n song song
vi nhau.
Cu to ca mt lng knh ______________________
BB'CC' l mt y ca lng knh. Cc mt ABB'A, v AAICC' l hai mt bn ca lng

knh. Cnh AA, gi l cnh nh ca lng knh. Gc i din vi mt y gi l gc nh ca
lng knh. Mt lng knh thng
chnh. l gc nh A (hay cnh y) v chit sut
c c trng
bi hai i lng
n ca vt liu lm lng
knh. Nu
ta chiu mt chm sng Si vo mt mt bn ca lng knh th hin tng khc x s xy ra

nh trong hnh 3.3.
Trong :
Si l tia ti; KH l tia l.
l gc ti v i' l gc l ca tia sng;
50
D l gc lch ca chm sng sau khi qua lng knh;

ABC l tit din chnh ca lng knh;
Di l gc lch ti thiu;
y ta c cng thc c trng cho 1 lng knh l:
Sin (A + D) = n. sin(A / 2)
(3.1)
dD dn .
2 sin( A / 2)
= .sin .- ==y== / __
d d
- n2 sin2(A/2)
(3.2)
Chnh hai i lng ni trn c nh hng trc tip n s phn li chm sng,
ngha l quyt nh gc lch D ca chm sng. Chnh v th khi ch to lng knh
ngi ta phi chn nhng vt liu c chit sut ln v ch to gc nh ca lng knh
c ln cho ph hp.
Vt
liu
lm
lng
knh cng phi trong sut,

ng nht v ng hng
trong mt vng ph nht
nh.
phi
bn
vi
nhit v nh sng.
Chit sut phi hu nh
khng ph thuc vo nhit
v m.
Trong vng kh kin, ch to lng knh ngi ta thng dng mt vi loi thy tinh,
nh thy tinh flin nng, flin nh, thy tinh krau. Trong vng t ngoi ngi ta thng dng
thch anh. Nu c vng ph (UY + VIS) phi dng thy tinh c bit.
Cc c trung ca my quang ph lng knh
nh gi cht lng, hiu qu v kh nng s dng ca mt my quang ph, ngi
ta thng dng ba thng s c trng c bn l tn sc gc, tn sc di v phn gii.
tn sc gc.
Trong mi my quang ph, s bin thin ca gc lch D theo di sng ca tia sng l
mt c trng quan trng. N ni ln kh nng tn sc gc ca mt my quang ph v c
gi l tn sc gc ca my quang ph .
Trong cc my quang ph lng knh, lng knh thng c t v tr cc tiu i vi
tia sng trung tnm ca mt vng ph ca my. V th tn sc gc s c
51
tnh theo cng thc:

^ Dd .
2sin(A/2)
Dg --.sin --------=====
dX
dn
X----
(3.3)
-n sin2(A/2) dX
Nu gc nh A ca lng knh bng 60 th cng thc trn s l:

-2 xdn
Vl - n
(3.4)
dX
Nu my quang ph c m lng knh nh nhau trong h tn sc, th tn sc ca my

s bng m ln ca my l lng knh. Cn nu cc lng knh c gc nh A khc nhau, th tn
sc chung s l tng ca tn sc tng lng knh theo cch b tr. Ngha l tn sc gc
chung bng tng tn sc gc ca tng lng knh c trong h tn sc ca my quang ph.
Nh vy, theo cc biu thc trn, chng ta thy tn sc gc ca mt my quang ph
lng knh ph thuc vo cc yu t sau:
S lng knh c trong h tn sc.
Gc nh A ca lng knh.
Chit sut ca vt liu lm lng knh.
Bin thin theo bc sng (sng ngn lch nhiu, sng di lch t).
V th, mun tng tn sc gc ca mt my quang ph lng knh ngi ta phi ch
to h tn sc c nhiu lng knh ghp li vi nhau. Trong thc t ngi ta thng ghp hai
hoc ba lng knh. Bin php th hai l chn nhng vt liu c chit sut ln ch to lng
knh v ch to cc lng knh c gc nh A ln. Nhng bin php ch to gc A ln cng ch
thc hin c trong mt mc nht nh, thng thng n 90 l ln nht. V khi tng gc
nh A ca lng knh th hin tng phn x ton phn mt bn ca lng knh s nhanh
chng xut hin, lm mt phn chm sng s khng ra khi lng knh, v ta b mt chm tia
.
tn sc di. tn sc gc ch cho bit s khc nhau v gc lch ca 2 tia sng,
ngha l tia sng b lch i ni gc ln bao nhiu sau khi phn li, m cha ch ra c
hai vch ph gn nhau s cch nhau l bao nhiu trn mt phng tiu (hay knh nh). Do ,
trong thc t, nh gi kh nng tn sc ca mt my quang ph ngi ta cn phi s dng
thm c tn sc di. Nhng tn sc di ph thuc vo tn sc gc v tiu c ca thu
knh bung nh f2, v n c tnh theo cng thc:
D1 - d_ -_f^xdD
d sin E d
(3.5)
Trong di l khong cch gia hi vch ph trn mn nh (mt phng tiu); E l gc

nghing ca hp nh vi quang trc bung nh ca my v do hiu s di sng ca 2 vch
ph, tc l : dX = (1 - X2) v X = (X2 + 1)/2.
52
Theo cng thc trn, mun tng tn sc di ca mt my quang ph lng knh

ngi ta phi:
Tng tn sc gc ca n.
Tng tiu c ca thu knh bung nh f 2. Nhng bin php ny ch t c
trong mt gii hn nht nh. V khi f2 cng ln th cng sng ca vch ph cng
gim, ngha l c v tn sc th mt v cng (hai yu t ny t l nghch vi
nhau). Do , trong thc t, ngi ta phi tnh ton v chn gi tr f 2 cho ph hp
sao cho c tn sc ln, m cng vch ph vn m bo cn trn 80%.
Tuy nhin, d nh gi v so snh tn sc di ca cc my quang ph vi
nhau, trong thc t ngi ta li thng dng gi tr nghch o ca tn sc di,
ngha l thay biu thc dl/d, bng biu thc dl/d. Nh vy, i lng mi quy c
ny cho ta bit c trn n v di ca knh nh (mm) hay mt phng tiu c cha
bao nhiu n v di sng (amstrong hay nm), ngha l my quang ph no c gi
tr d/dl cng ln th c tn sc di cng nh. V d hai my quang ph Q l v Q2,
m Qi c dl bng 4 A/mm v Q 2 c d/dl bng 2 A/mm, th my Q 2 c tn sc di
gp i tn sc di ca my Q1.
tn sc di ca mt my quang ph c lin quan trc tip n di ca vng
ph m my thu nhn c. Vi mt vng ph nht nh tn sc di cng ln th
vng ph ca my cng ri ra trn mt khong rng, ngha l mt phng tiu ln, nh
th trn mt knh nh c chiu di nht nh th ch thu c mt phn ca ton vng
ph ca my, nu my c tn sc ln. Nh trong v d trn ca hai my quang
ph Ql v Q2, i vi vng ph t 2000 - 4000 A th ton b vng ph thu c ca
my Q2 chim di gp i ca my Ql.
Do vi nhng my c tn
D (/mm)
sc ln, ngi ta khng th thu c

ton b vng ph ca chng ln mt
knh nh, v phi cn mt knh nh
qu di. Cho nn ngi ta phi ghi
tng phn ca ton b vng ph ca
my ln mt knh nh c di nht
nh (24 hay 30 cm), ngha l i vi
nhng my quang ph c tn sc
ln ngi ta phi c b phn quay v
hng vng ph cn nghin cu vo
Hnh 3.4
mn nh thu ghi.
ng cong tn sc ca 2 my quang ph
(I) - My lng knh Q24; (II) - My cch l PGS-
Trong my quang ph lng knh, tn sc ca chng gim theo s tng ca di

2
sng, ngha l trong mt my, th vng sng di c tn sc nh hn vng sng ngn (hnh
3.4).
53
Nng sut phn li.

Nng sut phn li (kh nng phn gii) ca mt my quang ph trong mt vng no
c biu th bng t s:
R - hay R -A
(3.6)
dX
Trong 1 v 2 l di sng ca hai vch ph gn nhau m cn c th tch ra thnh

hai vch r rt trn hnh nh (mt phng tiu); A hay d l hiu s ca 1 v 2.
Hnh 3.6a
Hnh 3.6b
Nhng my quang ph c nng sut phn gii R cng ln th hai vch ph c di
Tch
thnh
tch thnh hai vch
sng v ny
cng
nmhai
xavch
nhau trn knh nh Khng
(hnh 3.5).
1
V vy, nu chn cc thng s trn cho ph hp khi ch to lng knh v ch to my

Nhng gi tr d phi bng bao nhiu hai vch ph 1 v 2 cn c th tch ra r rt
quang
ph ta s thu c kh nng phn gii tt nht ca mt my quang ph.
thnh hai vch trn knh nh? Nghin cu vn ny v t nhng kt qu thc nghim
Nhng ng knh ca thu knh bung nh li c tnh theo cng thc:
Rayley nu ra quy tc: Hai tia sng c bc sng gn nhau i v 2 ch tch
d
ra
2=2 (A/2) w1 - n 2sin2( A /2)]

sin( Avch
/ 2)
Fe3057,45
thnh hai
(3 8)
^2
ph r
rng,
cc di
tiu
trong
bnu
l chiu
cnh y ca lng knh.
Fe3059,l
nhiu x th nht ca vch
Nh vy, nng sut phn gii ca my quang ph lng knh s l:
ny trng vi cc i
d
k
(3.9)
nhiu x th nht R
ca= m.b.(dn/d)
vch
Trn my Q24
kia.
l nhng
khongyu
cch
Ngoi
t tini, nng sut phn li ca mt my quang ph cn Trn
b nh
hng
my PGS-2
thiu
ca
2
vch
ph
(hnh
bi mt s yu t khc nh:
3.6).Trn c s , nng
Tnh cht v mn (c ht) ca lp nh tng trn knh nh, nu ph c ghi ln
sut phn li ca mt my Hnh 3 5
knh nh. Vi yu t ny, nhng kt qu thc nghim cho thy rng, lp nh tng trn knh
Khong cch ca hai vch ph trn cc my c nn
quang
phnhy
lngth
knh
3 sut
Phn vch
gii khc
tnhnhng
theo cng
nh cng
nhc
hng cng nhiu n kh nng phn
li ca
ph. V
knh
thc:
nh c nhy cao thng c lp nh tng cha cc ht AgBr bt nh sng c kch thc
ln. Nhng trong nhng h thng my mi ca th h th ba, yu t ny hon ton c loi
Nu my quang ph c h tn sc gm m lng knh nh nhau th R t=
tr, v ph c ghi trc tip ln bng giy hoc o trc tip m khng phi ghi ln knh nh
mRi
(3.7).
na.
Cng
thc
cho hng
ta thyn
nng
sut
phn
li lica
quang
Mt yu
t ny
na nh
nng
sut
phn
camt
mymy
quang
phph
l lng
rngknh
ca ph
khe
thuc
vo vo
nhiu
yu
t, nh:
my (khe
ca
chm
sng). Ni chung, vic tng rng ca khe my s a n kt qu
lm gim nng sut phn li ca my v rng ca khe my cng ln th rng ca vch
+ S lng knh trong h tn sc (m);
ph cng cng ln.
+
Chit
sut
calivt
liurng
lmkhe
lngmy
knh (n);
Nng
sut
phn
v
+
Sin ca
gclinh
(A/2)
Nng
sut1/2
phn
ca ca
mt lng
myknh
quang
ph nhn chung ph thuc vo rng ca khe
my. Khe my cng rng th nng sut phn li ca my cng gim. Nhng mi quan h ny l
+ ng knh ca thu knh bung nh (d 2);
khng n gin. V th chng ta c th xt trng hp c th sau y: Nu gi a l rng
+ S bin thin ca chit sut theo bc sng (dn/d)
ca khe my quang ph; f1 v f2 l tiu c ca thu knh chun
54
55
trc v thu knh bung nh; d l ng knh ca cc thu knh th rng hnh hc ca
vch ph s c tnh theo cng thc sau:
a, = a.(2/f1)
(3.10)
Trong ts f2/fl c gi l phng ica my quang ph. Ni chung trong

cc my quang ph ngi ta c gng ch to t s ny bng 1. Nh vy, vch ph l nh
khng phng i ca khe my, ngha l a, = a. V cho vch ph r nt th s phn b cng
phi tha mn iu kin:
a, < 2s
(3.11a)
s = X.(f2/d)
(3.11b)
trong
s l na
rng hnh hc
ca cc i th nht
ca vn nhiu x. Do trong
iu kin ti thiu ta phi c:

a, = 2fd)
(3.12)
Hay t cng thc (3.10) v (3.12) chng ta c:

a = 2fd)
(3.13)
Gi tr rng ca a theo cng thc (3.13) ny c gi l rng tiu chun ca khe my

quang ph v k hiu l ao, ngha l lc ny ta c:
ao = 2X (fl/d)
Nh vy rng tiu chun ao ph thuc vo:
di sng X ca tia sng.
Tiu c f1 ca thu knh chun trc.
T l nghch vi ng knh d ca thu knh.
L thuyt v thc nghim chng minh rng rng tiu chun a o ca khe my, nng
sut phn gii ca mt my quang ph thc s ch bng 90 phn trm theo l thuyt. V th,
mun c nng sut phn gii cao ta phi m khe my nh hn ao mt cht (10%). Nhng
m khe my nh hn gi trao ta mt v cng vch ph,
khi
trong mt gii hnnht nh, th rng khe my quang ph v cng
vch ph l
t l nghch vi nhau. Bng 3.1 l vi v d v rng ca khe my quang ph pht x. Cho

nn tt nht vn l chn rng khe my ng bng a o hay ln hn mt t c v cng
trong phn tch nh lng.
56
Bng 3.1
Nu knh nh c t vung gc vi quang trc ca h thng thu knh bung nh th
rng
phkhe
s l:
Quan
hvch
rng
my v nng sut phn gii - cng vch ph
Khe my
s = a, +Cng
2X(f2/d)
vch ph (%) (3.16a)Nng sut phn gii (%)
50v
0,50 ao
0,90 ao
s = 2Xv.(f2/)
75
98
(3.16b)
96
cho
cao
hai trng hp nu trn,
E = 1.
0,95
82 v trong trng hp ny sin 94
Cng
vch
1,00
ao ph v rng khe my 90
90
Trong phn tch quang ph nh tnh v nh lng, c bit l phn tch hm lng vt
1,20 ao
95
80
ca cc nguyn t, mt yu cu quan trng l phi thu c vch ph c cng ln nht,
ao
98ngun pht x qua khe my quang
75
ngha l phi 1,50
bit c
s truyn nh sng t
ph n vt
thu cng 2,00
vchao
ph (knh nh, etector) l99nh th no.
60
Nu gi2,20
Io laocng ca chm sng100
pht x ca tia sng X th quang
50thng tng cng
i vo h chun trc s l:
V khi khe my rng tiu
n chun th ch c cc i th_ nht ca vn nhiu x lt
=
Q/o
=
4.(d
f1)2 B.al
(3.17)
vo c h thng chun trc cho nn /trong
cc php phn tch
khng c chn khe my
nh hn rng tiu chun a o. Thng thng, theo kinh nghim thc t ngi ta hay chn khe
Hay l
my c rng t 1a o n 1,5ao l ph hp (phn tch T chn: 0,9 - 1a^ Phn tch L chn
t: 1,0 - 1,5ao).
OQ
rng ca vch ph
trongkhe
:my quang ph c rng l th rng ca vch ph bng rng hnh hc
Nu
ca khe
my
vi
x chnh
a v
l lcng
rng
v rng
chiuca
di vn
ca nhiu
khe my
quanggia,
ph; ngha l ta c:
B l huy ca chm sng c gc y l Q.
5 = a'+2 f
(3.14)
Khi chm sng Io i qua h quang
hcEca my quang ph th quang thng thc t tc
d .sin
dng ln
Nuknh
khenh
my(hay
rt vt
hp,thu)
th s
l:
rng ca vch ph ch l rng ca vn nhiu x chnh
gia, ngha l ta c: = a.o = a (d / f1)2 B.a.l
(3.18a)
5
(3.15)
k Ba
d.
sin
E
O' =a.kB.a.l ^ Io = ' .
(3.18b)
aQ
Hai biu thc trn cho thy, rng ca mt vch ph c lin quan trc tip rng
my
y avlnng
h ssut
mtphn
mt gii
nngca
lng
chm
hph
quang
cathmy
quang
ca khe
myca
quang
ph.sng
Khiqua
vch
cnghc
rng
nng
sut
ph,
Trong
hpcn
l tng
th avo:
bng 1, cn mi trng hp
phn nh
gii thu
cng knh,
gim.lng
ngknh...
thi
rngtrng
vch ph
ph thuc
khc u
ln c
hn
1. thu
Quang
thng
O' ny
+ Tiu
ca
knh
bung
nh.s tc dng ln knh nh vi ri l:
0
+ T l nghch vi
ca hp nh.
=ng
= -01knh ca thu knh v sin gc nghing
(3.19a)
S a''
+ T l thun vi di sng ca vch ph, ngha l cc bc sng di th vch ph
tronghn,
Smc
l din
ca vch
phkhe
v ta
c:bng a.
cng rng
du tch
c cng
rng
sng
58
57
S = a,.l'
vi
a,= a.f2/(fi.sins) v l' = l.(f 2/fl)
Nn din tch ca vch ph s l:

S = a.l.(f2/fl)2.(l/sin s)
(3.19b)
Do , nu nh sng l n sc v b qua hin tng nhiu x, khc x, tn x, khi

chm sng Io qua h quang hc ca my quang ph th ri ca chm sng s l:
' _ na d2
E = - = . \sins
S 4 (f 2
,
(3.20)
v
'
y l trng hp l tng, n gin v gi tr ri E trong trng hp ny c k

hiu l Eo. Nh vy, chm sng Io tc dng ln knh nh to ra vch ph c cng l:
I = E t ^4^ (d / f,)2.t.sins
(3.21)
Ngha l nu vch ph hon ton n sc th cng IM ca vch ph t l vi bnh

phng khu t i ca thu knh bung nh v sin ca gc nghing ca hp nh s, cng
nh thi gian t m ri E o ca chm sng tc dng ln knh nh hay vo khe o ca nhn
quang in.
Trn y l trng hp n gin, nhng thc t th phc tp hn, v nh sng vo my
quang ph khng phi khng c cc hin tng nhiu x, tn x, cc sai st ca h thng
quang hc, l nhng yu t thc t khng th loi tr c hon ton. Chnh v th m vch
ph trn knh nh thng rng hn mt cht ( 10%) so vi trng hp tnh ton trn y.
Nu gi mt cch tng qut, Aa 1, Aa2, Aa3..., l rng do cc hin tng nhiu x, tn
x, tnh khng tuyt i n sc ca vch ph gy ra, th rng thc t ca vch ph phi l:
f
1
a' = .(a.^- + Aa1, Aa2, Aa3,...)
sins
/2
(3 22)
v ri thc t lc ny s l:
E
= =
L (d / f2)2sins
(3.23)
[a + (Aa1, Aa2, Aa3...,)(f1/ /2)]
hay l:
E = E0T
59
Nh vy nu a >> (a1 + a2 + Aa3).(f1/f2) th chng ta li c E - E o, ngha l tr

i trng hp c bit trn. Tc l cng vch ph khng ph thuc vo rng ca khe
sng. Cn tt c cc trng hp khc th rng ca vch ph t hoc nhiu u c b nh
hng bi rng ca khe sng. V cng vch ph trong cc trng hp lun lun
phi tnh theo cng thc:
IX= E.t = Etj--------------------- a------------------
[a + ([ + a2 + a3).(f / f2)]
(3.25)
Cho nn khi khe my thay i th rng ca vch ph cng thay i theo. Nhng mi
quan h ny khng n iu v cng khng tuyn tnh. V vy, trong mt php phn tch bt
buc phi gi cho khe sng c rng khng i trong mt php o.
Mt khc, cng thc (3.23) v (3.25) cn cho thy, ngoi rng ca khe sng, cng
ca vch ph cn ph thuc vo c khu ca my quang ph, tc l t s d/f 2. Cng
vch ph s ln, nu my quang ph c khu ln. Ngha l tiu c thu knh bung nh
phi nh. Nhng nu tiu c thu knh bung nh f 2 nh, th li mt v tn sc di. Chnh
v th trong ch to my quang ph ngi ta phi tnh tm c gi tr khu sao cho ph
hp nht, nhm bo m c tn sc m cng ca vch ph cn ln c th o
c v pht hin c d dng.
Nu ly gi tr nghch o ca khu th ta c t s f 2/d. T s ny gi l m ca
thu knh bung nh. Trong thc t khi ch to cc my quang ph ngi ta thng hay chn
t s ny c gi tr t 10 n 20. Tri li, khi m ln hn 20, vch ph c cng ln,
nhng tn sc ca my li qu km.
sng ca vch ph pht x
Nu ta pht hin v o trc tip cng ca vch ph bng mt nhn quang in, th
sng ca vch ph l yu t quan trng. sng ca vch ph ph thuc vo cng ca
chm sng i vo my quang ph v cng ca chm sng sau khi qua my quang ph
vo nhn quang in. V th cu to, tnh cht ca h quang hc ca my u c nh hng
n sng ca vch ph. Mt cch gn ng v theo thc nghim, sng ca vch ph c
th c tnh theo cng thc:
L = (d2/f2)2
(3.26)
Trong d2 v f2 l ng knh v tiu c ca thu knh bung nh. Nh vy, sng

ca vch ph t l thun vi bnh phng ng knh ca thu knh bung nh d 2 v t l
nghch vi bnh phng ca tiu c bung nh f 2, ngha l ph thuc vo m ca thu knh
bung nh (t l f 2/d2). Nu tiu c f 2 cng ln th sng L ca vch ph cng gim, tc l
mt v cng v ngc li.
S quang hc mt s my quang ph lng knh
V d v cc s h quang hc ca mt s my quang ph pht x c ch ra trong
hnh 3.7.
60
s
e) My KC - 55 (Nga)
Hnh 3.7
S quang hc ca mt s my o ph pht x
P: Lng knh; G: Cch t; M, Mi, M 2: Cc h gng; L: Thu knh; E: Hp nh ghi ph;
T: Khe sng; S: Ngun pht x.
Cch t v my quang ph cch t
Gii thiu v cch t
Cch t l h gm nhiu khe hp (vch) song song vi nhau v cch u nhau.
Mi khe nh l mt chn sng, cn ch khng c vch nh l mt khe sng. Cch t c
tc dng phn li nh sng nh lng knh. Nhng bn cht s phn li nh sng cch t khc
lng knh. S phn li nh sng ca cch t l do hin tng nhiu
61
x ca chm sng qua khe hp. Khi s phn li nh sng ca lng knh l theo hin tng khc
x ca nh sng qua hai mi trng c chit sut khc nhau. Cch t c hai loi:
Cch t phn x v 2. Cch t truyn x.
ch to my quang ph ngi ta thng dng cch t phn x, v dng cch t
truyn x s b mt nhiu nng lng khi chm sng i qua cch t.
Trong mi loi trn li c cch t phng v cch t lm. T thc t chng ta s ch
cp n cu to v bn cht ca cch t phn x l chnh (hnh 3.8a v 3.8b).
Hnh 3.8a
Hnh 3.8b
Dch t phng
Cch t lm phn
x
Cc i lng c trng cho mt cch t l hai thng s chnh sau y:

Chu k ca cch t: L khong cch gia hai vch trn cch t v c k hiu l d (hnh
3.8a).
Hng s cacch t: L s vch trn mt n v
hiu l k, tc l s vch c
di ca cch t v c k
khc trn 1mm.
Nh vy, gia chu k v hng s ca cch t lin quan vi nhau theo biu thc: d. k =
1
(3.27)
Nu gi L l chiu di ca cch t, th tng s vch trn mt cch t s l:

N = k. L
(3.28)
v cu to th cch t phn x gm c hai phn. l b v mt cch t. B l tm

thu tinh hay thch anh dy t 1,5 n 2 cm, c hai mt song song vi nhau v thng c din
tch t 4 x 4 hay 4 x 6 n 8 x 12cm. Mt cch t l lp kim loi nhm (Al) tinh khit (99,999
%) v dy t 0,2 - 0,5 mm. Lp kim loi ny c a ln b bng con ng in phn
c bit trong mi trng tr. Mt lp kim loi nhn bng v c khc ln nhiu vch
song song v cch u nhau. S vch c khc ln lp kim loi ny thng l t 650 - 3600
vch/mm. S vch trn 1 mm cng nhiu th kh nng phn li nh sng ca cch t cng ln.
62
Nh th, nu chng ta chiu mt chm sng song song khng n sc vo mt cch t

theo mt gc ti a no th ch c vch trn cch t nh mt chn sng, ch khng c vch
nh mt khe sng v di tc dng ca hin tng nhiu x trn b mt cch t th chm sng
a sc s c phn li thnh ph. Nu gi p l gc l ca tia sng, di sng l X th ta lun
lun c biu thc:
sina + swinp = m.k.X
(3.29)
Biu thc ny c gi l cng thc c bn ca cch t. Cng thc ny gii thch cho ta
nguyn nhn s tn sc ca cch t, v t cng thc (3.29) ta c:
sinp = m.k.X + sina
(3.30)
y a l gc ti ca chm sng, m v k l khng i i vi mt cch t. Nn ng vi

mi bc sng X ta s c mt gi tr sinp tc l c 1 gi tr p. iu c ngha l cch t
phn li chm sng a sc thnh tng tia n sc lch i theo tng gc 13 khc nhau. Nhng
y sng di b lch nhiu, cn sng ngn b lch t hn. ng thi cch t cho ta ph c
nhiu bc, ng vi cc gi tr m ca cng mt di sng X S m c gi l bc ca ph
cch t.
Nu tia ti vung gc vi mt cch t, tc l gc ti a - 0 th cng thc (3.30) s c
dng l:
sinp = m.k.X
(3.31)
Trong trng hp ny gc phn x ca cc tia sng khng ph thuc vo gc ti a m

ch ph thuc vo hng s k ca cch t v di sng ca tia sng m thi. Trong thc t
ngi ta hay t cch t v tr ny trong my quang ph.
Nu gc ti a= 13 th cng thc (3.30) s l:
sinp = (mk/2).X
(3.32)
y chnh l tia sng X c gc ti a tc dng ng vo gia knh nh ca mt vng ph

ca hp nh. V th cng thc ny c s dng tnh
gc ti a khichn
vng ph cho mt php phn tch. cng l v tr cc tiu ca tia
sng trungtnm ca
vng ph cn chn trong my.

Mt khc, cng chnh do hin tng nhiu x qua khe hp to ra ph ca cch t cho
nn khong cch t v tr cc i cc vn sng n tnm hnh nhiu x c tnh theo cng
thc:
xt = m.f 0.(X/k)
(3.33)
ngha l:
Cc i th 1 cch tnm mt on x t1 = (1.f2,X)/k
Cc i th 2 cch tnm mt on xt2 = (2.f2.X )/k
63
Cc i th 3 cch tnm mt on x t3 = (3.f2)/k
Cc i th m cch tnm mt on x tm = (m.f2)/k.

iu ny gii thch cho ta ti sao tn sc di ca cch t bc th m gp m ln bc
th 1, ngha l c tn sc bc th m l:
DDM =
(3.34)
m
Vi m l s nguyn v m > 1.
My quang ph cch t
My quang ph cch t, v nguyn tc, cng c cu to nh my quang ph lng knh.
Nhng y h tn sc l mt cch t, v cng dng ba i lng c trng nh trong my
quang ph lng knh nh gi cht lng ca mt my quang ph cch t. C th l:
tn sc gc
T cng thc c bn ca cch t (3.29), nu xt s bin thin ca gc lch p theo di
sng X th ta c:
cosp.dp = (m.k).dX
hay l:
Dg = Dr
D cos p
<3-35)
Biu thc ny chnh l cng thc tnh tn sc gc ca my quang ph cch t.

Nh vy, tn sc gc ca mt my quang ph cch t s:
+ T l thun vi hng s k ca cch t v bc m ca ph cch t.
+ T l nghch vi cos ca gc phn x p.
Ngha l mt cch t th vi cc bc ph cng cao tn sc gc ca my cng ln.
V d:
Nu m bng 1 ta c dp/dX = 1.k/cosP
v.v...
Mt cch tng qut, ngha l tn sc bc m th ln gp m ln tn sc gc bc
1:
64
D
V
m
Nhng cc bc ph ca cch t li xut hin ng thi, ph ca cc bc cng cao th

cng cng yu. Gn n 70% nng lng l tp trung bc 1 (vn nhiu x th nht).
Chnh v th khi ghi ph phi dng knh lc ph hp loi b nhng bc ph khng cn
thit. Cho nn tnh cht a bc ca ph cch t va l u im, nhng cng va l nhc im
ca my quang ph cch t, v ph ca cc bc cao ta c v tn sc,nhng
mt vcng. Nn trong
thc t, ngi ta ch
dng ph bc
li
1,
hay i khi n bc 2 m thi.

tn sc di
i vi my quang
ph cch t, ngi ta cng
gi t sdl/d, l tn
sc di
ca n v c tnh theo cng thc:

(3.36)
Nh vy, tn sc di ca my quang ph cch t t l thun vi tn sc gc ca n
v tiu c f2 ca h bung nh. Hay ni mt cch khc, tn sc di l:
T l thun vi hng s ca cch t, tiu c ca bung nh, v s bc ca ph cch t,
v
Thay i trong quan h t l nghch vi cos ca gc phn x ca tia sng. V d t cng
thc trn chng ta c:
+ Nu m = 1 th dp/d, = (1 .k.f 2)/cosP;
+ Nu m = 2 th dp/d, = (2.k.f 2)/cosP;
+ Nu m = 3 th dp/d, = (3.k.f 2)/cosP;
Ngha l di tn sc bc th m th
cnggp mln tn
sc di bc 1
(cng thc 3.34).

Nhng trong thc t, d so snh, ngi ta cng dng gi tr nghch o ca i lng ni
trn, nh quy c trong my quang ph lng knh. Nh vy chng ta s c:
_ cos p
D
dm
mkf
(3.37)
Cng thc (3.37) ny l tn sc di nghch o ca my quang ph cch t bc th

m v ti im chnh gia ca vng ph. Cn tn sc di ti mt im X no cch tnm
knh nh mt khong x s c tnh theo cng thc:
Ddm = Ddm 0,00016.^3X
(3.38)
65
T biu
thy mt
tn
quang
cch
t hutng
nh vch
ph thuc
vch ph
1 vthc
%2ny
khctanhau
gisc
tr di
X ca
sau my
y s
cph
phn
li thnh
ring
rt t vo di sng ca tia sng (bng 3.2). Cng thc trn nhn du (-) khi i t tnm knh
bit:
nh theo chiu di sng tng dn v nhn du (+) theo chiu ngc li.
Nu m = 1, ta s c x = 0,02 ,
Bng 3.2
Nu m = 2, ta s c x = 0,01 ,
So snh tn sc ca hai my
Nu m = 4, ta s c x = 0,005 ,
Vng ph ()
tn sc di nghch o trong my
Ngha l bc m=1, hai vch 1 v %2 mun tch thnh hai vch r rng th phi khc
nhau mt gi tr di sng ti Cch
thiu t
l PGS-2,
0,02 . bc
Khi1 bc 2, hai
vch
ch cn khc
Lng
knhny
q 24
nhau mt gi tr2000
x = 0,01 l tch
thnh
hai vch ring bit. Nhng
7,390
/mm
4,00 trong
/mmthc t ngi
ta t dng ph bc cao ca cch t. Ngi ta thng hay dng ph bc I v bc II, v n 70%

2500
- nhng cch t
nng lng l tp
trung bc I. Cho nn7,380
trong- thc t hin nay ngi ta7,80
dng
c hng s k rt3000
ln (k:2400-3600) ch
to- nhng my quang ph c
kh-nng phn gii
7,370
13,00
cao. Hnh 3.1a, b l s quang hc ca mt s k my ph cch t.
3500
7,356 18,00 Vng lm vic ca
my quang ph
y cng l
mt ai lng nh7,340
gi mt
4000
- my quang ph.
31,00 -
Do tnh cht quang hc ca vt liu dng ch to h tn sc l trong sut v ng

nht trong mt min nht nh, nn mi my quang ph ch c th thu, phn li v ghi nhn
3. Nng
phn
giinh ca ton b gii ph quang hc. Vng ph ny c gi l
c mt
vngsut
sng
nht
vng lm
vic
mtgii
my
quang
vic
ca my
Nng
sutca
phn
R ca
mtph.
myVng
quangph
phlm
cch
t c
nhquang
ngha ph
nh lng
sau: knh l
do trong sut v tnh cht ca vt liu lm lng knh quyt nh v ph thuc vo cch b
tr (cu to) ca my quang ph y. V d: Cc my quang ph lng knh thch anh thng c
d
vng ph lm vic l min t ngoi gn (2000-4000 ). Cc my quang ph lng knh thu
tinh cVi
vng
l min kh kin (36007800
), theo
v thch
chsau:
trong sut trong vng
X tnh
dXlm
= (Xvic
cnganh
thc
2 - X1), X = (X2 - X 1)/2 v c
t ngoi; cn thy tinh ti trong sut trong vng kh kin (nhn thy). My quang ph cch t
R = xd
thng c vng lm vic rng hn my quang
ph lng knh. Vng lm vic ca mt my
dp dX
quang ph cch t l cu to, tnh cht, di sng blanz b) v s bc ca cch t quyt
nh. Ni
my quang ph cch t thng c vng lm vic rng hn my quang ph
hay chung,
l
lng knh.
R = m.k.L
V
Vi
phphn
cchgii
t PGS-2
lpquang
cch ph
t c
k:650
b = vi:
2700 , c
Nhd:
vy,
r my
rng quang
nng sut
mt my
cch
t tv
l thun
vng lm vic l: bc 1: 2000 - 7800 v bc 2: 2000 - 4000 ...
Hng s k ca cch t, ngha l k ln th tn sc ln
Nh vy, vi my cch t th vng lm vic bc ph th m hp hn bc 1 l m ln,
Chiu di ca cch t L, v
ngha l chng ta lun lun c:
S bc ph ca cch t, m. Bc ph cao th phn gii cao.
m = 1/m
Do , mun tng kh nng phn gii
ca mt my quang ph cch t phi s
Vng lm vic ca mt my quang ph c lin quan cht ch n di ca c di ph
dng nhng cch t c hng s k ln v chiu di L ln. Nhng vic tng chiu di L ch c
m n thu c. Cc my c tn sc cng ln th di ca di ph cng ln. V th
gii hn (di nht l 15 cm). Nn ch yu l tng hng s k ca cch t, ngha l phi ch to
nhng my quang ph c tn sc ln, vi mt tm knh nh c
nhng cch t c nhiu vch trn 1 mm di. ng thi phi s dng ph nhng bc cao,
nh bc m=2. Song cc bc cao ca ph th cng vch ph li
Vd: ng vicch
66
tc k
bng
nh.
1800, th trong vng sng 3000 hai

67
di nht nh (v d 24 hay 30 cm), chng ta ch c th ghi c mt phn ca vng ph

lm vic ca my . T thc t , trong cc my quang ph c tn sc ln ngi ta phi
cb phn
quay cch t hng phn
ph cn nghin
cu vo knh
nh, ngha l vng ph lm vic ca my cn phi c ghi ln nhiu tm knh. V d: Vi

my Q 24 vng ph lm vic ca n ch cn ghi trn mt tm knh nh di 24 cm. Khi
vng ph ny my PGS-2 ta phi cn hai tm knh 24 cm mi c th ghi ht c vi ph
bc I.
Trang b ca h thng my quang ph pht x
T nhng nghin cu c cp trn, chng ta c th minh ha tm tt trang b
ca mt h thng my quang ph pht x gm nhng phn sau y:
Trang b chnh, c bn ti thiu: Gm ba phn
Ngun cung cp nng lng ha hi mu, nguyn t ha v kch thch m hi
pht x. l ngn la n kh, h quang in, tia la in, ICP.
My quang ph c nhim v thu, phn li v ghi li vng ph cn nghin cu.
Nh cc my quang ph lng knh Q-24, ISP-28, ISP-30, KSAI,... v cc my cch t
PGS-2, D0-3, D0-13.
Cc trang b nh gi nh tnh (my chiu ph) v nh lng (my o en).
H trang b hon chnh, c thm:
+ B phn t ng dn mu vo bung
o, pha long t ng.
+ H my tnh v phn chng trnh iu khin, x l kt qu o.

Trang b ph thm, Cn c:
+ H thng chiu sng khe my quangph. N l mt h thng thu knh hi
t v hng chm sng pht x ca mu phn tch vo my quang ph vi hiu sut cao v
ph hp cho tng mc ch phn tch.
+ Cc lc sng v chn sng c nhim v chn v a vng ph cn thit vo khe my
quang ph cng v phm vi nht nh theo yu cu ca php phn tch.
Tt nhin cc th ph tr ny c th khng c cng c.
Trang b pht hin v thu nhn ph
Cho n nay, thu nhn ph pht x ca vt mu c hai loi trang b. l loi:
Knh nh hay phim nh (k thut c in) v 2. Cc loi nhn quang in kiu ng
(photomultiplier tube detector), hin nay l cc mng git (diode array).
Knh nh quang ph
Knh nh quang ph c nhiu loi, nhng v cu to, n gm hai phn: Phn v phn
lp nh tng bt nh sng. l tm thy tinh trong sut v ng nht, c dy u n,
thng t 1 n 2 mm, din tch 6 x 12 cm, 9 X 24 cm hay 9 x 30 cm.
68
Lp nh tng bt nh sn l lp glatin c dy t 0,1 n 0,05 mm, nhng phi ng nht

v u n trn mt tm thy tinh. Lp glatin ny c cha cc ht AgBr mn. nhy ca
knh nh ph thuc vo cc ht AgBr trong lp glatin ny. nhy l mt thng s c trng
cho mi loi knh nh v mi loi knh nh cng ch nhy trong mt vng ph nht nh (hnh
3.9). c trng ny do qu trnh sn xut quyt nh, theo loi nguyn vt liu v thnh phn
ca chng, cng nh iu kin ch to knh nh. V th mi loi c nhy khc nhau trong
cc vng ph khc nhau.
10
12
xiooo
Hnh 3.9
nhy ph ca cc loi knh nh
(1): Vng 1800-4000 , (2): Vng 3600-7800 v (3): Vng 7000-10000 .
Thng thng knh nh c nhy cao thng c nh hng n phn gii ca vch
ph, v cc knh nh nhy chng c ht AgBr kch thch ln. Do , tng nhy ca knh
nh ngi ta thng thm vo mt cht kch hot quang hc, vn dng lp nh tng c
ht AgBr kch thc nh m knh nh t c nhy cao.
Khi ta chiu chm sng cng I ln tm knh nh th ch b nh sng tc dng vo s
ha en. Nu gi en ti im b nh sng tc dng vo l S, th ta c:.
S = ylog I
y Y l h s nh tng (tng phn) ca knh nh, v chnh cu to v bn cht ca
lp glatin quyt nh h s nh tng Y. H s Y ny cng ph thuc vo di sng X ca
vch ph, nhng rt khc nhau trong mi vng ph (hnh 3.10a). Khi b nh sng tc dng th
c mt lng t sng hv s gii phng ra mt ht Ag kim loi theo phn ng sau:
AgBr + hv = Ago + Br
Cc ht Ag nguyn t t do ny nm n tng trong lp glatin ta cha nhn thy.
V th, mun c nh thc v gi li c chng ta phi x l knh nh c nh sng
tc dng qua dung dch hin hnh v dung dch nh hnh. Sau y l thnh phn ca cc dung
dch .
69
Dung dch hin v dung dch hm knh nh

Dung dch hin hnh
Dung dch nh hnh
Mentol: 1g.
Natri thiosunphat: 250g.
Natri sunfit khan: 26g.
Natri cacbonat khan: 25g.
Hydroqu Ione: 5g.
CH3COOH 99%: 8,5 mm.
Pha trong mt lt.

s
t(gy)
to
Hnh 3.10a
Hnh 3.10b
3 ph thuc ca h s Y v X.
Quan h gia en
s v thi gian hin t.
Ngoi nhy, thi gian chiu sng cng l yu t quan trng nh hng n en ca
vch ph. Ni chung, chiu sng cng lu th en cng ln. Song, tt nhin cng ch trong
mt thi gian nht nh ph hp. Cn nhiu hn na th ch lm gim phn gii ca vch
ph, v thi gian qu di s lm m rng chiu ngang ca vch ph m khng lm tng
en S vch ph.
Thi gian hin cng nh hng n cng vch ph. Mi quan h ny c thy trong
hnh 3.10b.
Ni chung, vi nhiu loi knh nh, thi gian hin ph hp l t 2 n 4 pht v thi
gian hm (nh hnh) l t 4 n 8 pht. Nhit thch hp l t 18 n 20 0C.
o en Sx ca vch ph trn knh nh
Nu chiu chm sng cng I o vo knh nh th ch c vch ph v khng c vch
ph, chm sng i qua s c cng l I v Io. Do en ca vch ph s l:
S = log(Io/I)
h ay S = log(ao/a)
Trong ao v a l lch ca in k ng vi chm sng cng I o v I. Do ,
thang o en S ch c gi tr t 0 - 2. Nhng vng en va phi (vng m mi quan h
gia S v C l tuyn tnh) ch nm trong khong t 0,3 - 1,7 (hnh 3.11). Cn khi S nh hn
0,3 l vng non, khi S ln hn 1,7 l vng gi. Trong 2 vng ny kt qu o l khng chnh
xc. V th phi chn iu kin ghi ph ph hp en
70
ca vch cn o ri vo vng tuyn tnh (0,3 - l,7).

Nhng
trong
phn
tch
lng vt th en ca vch
ph li c th nh hn 0,3 n v
S. V th ngi ta m rng
thang o en S v pha cng
nh. y c 2 cch bin i
en ca vch ph, v tng
ng n l hai thang o mi W v
P.
Theo thang W th en
vch ph c tnh theo cng
thc:
W = log.( -1)
a
V theo thang P th en vch ph li c tnh theo cng thc:
S + W P =
Do thc t nn hin nay cc my o en u c c ba thang o en S, W v

P. Vi thang W en c th m rng c n 0,1. Cn vi thang P th c th n gi tr
-0,3 n v S. V th trong phn tch lng vt ngi ta hay dng thang P. Tt nhin t cc gi
tr ca P ngi ta cng d dng tm c cc gi tr ca S hay W tng ng, nh mt bng
chuyn i en c sn (xem ph lc).
ng nhn quang in (Photomultiplier tubes)
Trong cc my quang ph hin nay, ngi ta c th pht hin v o trc tip cng
ca cc vch ph bng cc nhn quang in, m khng cn ghi ph ln knh nh. Do loi
tr c sai s do knh nh gy ra.
Nhn quang in kiu ng hay detector tubes l mt loi dng c quang hc thu nhn
v pht hin tn hiu quang hc (tc l o cng chm sng) theo hiu ng quang in ca
n. Vi s pht trin ca khoa hc v k thut, ngy nay ngi ta ch to c nhiu loi
nhn quang in kiu ng (photomultiplier tubes) thu nhn tn hiu quang hc v khuch
i ln hng ngn, n hng triu ln, lm cho cc my quang ph c th phn tch c nhiu
nguyn t nng rt nh (t ^g n ng). Hnh 3.12 l s nguyn tc cu to ca nhn
quang in v vng ph lm vic ca n. Nhn quang in l mt dng c vn nng thu
nhn tn hiu quang hc. N c nhy v chn lc cao. Vng ph lm vic ca nhiu loi
nhn quang in thng l t 190 n 900 nm, cho vng ph t ngoi v kh kin. Tt nhin,
vng ph
71
lm vic ca mt loi nhn quang in ph thuc vo bn cht kim loi dng ch to bn

catot ca nhn quang in (hnh 3.12). Cc kim loi ch to catot ca nhn quang in kiu
ny thng l Na-Cs-K-Li-Sb. H s khuch i ca cc nhn quang in thng l t 10+5
n 10+6, i khi c th n 10+7 ln.
Nguyn tc cu to ca nhn quang in kiu ng
72
73
X,
Hnh 3.14
Mt on ph ghi trn bng giy
Ph ICP-AES ca AI, Cr, Fe, Ni (200 ppm) ghi trn giy)
74
Chng 4
CC YU T NH HNG TRONG AES
Khi qut chung

Cc yu t nh hng n kt qu phn tch trong php o ph pht x nguyn t l rt
a dng v phc tp, c khi xut hin v cng c khi khng xut hin, c nh hng hay
khng c l ty thuc vo thnh phn ca mu phn tch v cht nn (matrix). Nhng
nghin cu mt cch ton din, chng ta im qua tt c cc yu t nh hng c th c trong
php o ny. Cc yu t c th c chia thnh 6 nhm nh sau:
Nhm 1. Cc thng s ca h my o ph.
Cc thng s
ny cn c kho st
v chn cho tng trng hp c th. Thc hincng vic ny chnh l qu trnh ti
ha cc thng s ca my o cho mt i tng phn tch.

Nhm 2. Cc iu kin ha hi, nguyn t ha mu v kch thch ph. Cc yu t ny
th hin rt khc nhau ty thuc vo k thut c chn thc hin qu trnh ha hi,
nguyn t ha, kch thch ph v n c nghin cu k trong chng 2.
Nhm 3. K thut v phng php c chn x l mu. Trong cng vic ny nu
lm khng cn thn s c th lm mt hay lm nhim bn thm nguyn t phn tch vo mu.
Do kt qu phn tch thu c s khng ng vi thc t ca mu. V th, vi mi mt loi
mu ta phi nghin cu v phi chn mt quy trnh x l ph hp nht, c c ng thnh
phn ca mu v khng lm nhim bn mu. Vn ny s c nghin cu trong mt
chng ring.
Nhm 4. Cc nh hng v ph.
Nhm 5. Cc yu t nh hng vt l.
Nhm 6. Cc yu t ha hc.
Trong chng ny chng ta s nghin cu k cc yu t thuc cc nhm 4, 5 v 6.
Mt s nh hng trong php o AES
Cc yu t v ph
S pht x ph nn
Yu t ny c trng hp xut hin r rng, nhng cng nhiu trng hp khng xut
hin. iu ny ph thuc vo vng ph v vch ph c chn o nm trong vng ph
no. Ni chung, trong vng kh kin th yu t ny th hin r rng, cn trong vng t ngoi
nh hng ny t xut hin, v ph nn trong vng t ngoi thng yu. Hn na, s pht x
nn cn ph thuc rt nhiu vo thnh phn ca mu phn
75
tch, c
bit
l matrix ca mu,
ngha l nguyn t c s ca mu, v ngun nng
lng kch thch ph.

V d: Khi xc nh
Pb trong mu
sinh hc
bng php o ngn la th
I)x
s hp th nn l khng
ng k. Nhng khi xc
nh Pb trong nc bin
(nn 2,9% NaCl) th nh
hng ny li l v cng
ln v bt buc phi b
chnh
loi
4.1).
Do
tr
(hnh
trong mi
trng hp c th phi
xem xt tm bin loi
(nm)
tr. loi tr pho nn,

ngy
nay
ngi
ta
lp
thm vo my quang ph
nguyn
thng
chnh nn. Hoc a vo
Hnh 4.1
nh hng ca s pht x ph nn a)
Khng b chnh nn; b) C b chnh nn
mu cc cht lm gim s
pht x nn.
S chen ln ca cc vch ph gn nhau
Yu t ny thng thy khi cc nguyn t th ba trong mu phn tch c nng ln
v thng l nguyn t c s ca mu. Tuy nguyn t ny c cc vch ph khng nhy,
nhng do nng ln, nn cc vch ny vn xut hin vi rng ln, nu n li nm cnh
cc vch phn tch (bng 4.1), th cc vch ph ny s chen ln cc vch phn tch, lm cho
vic o cng vch ph phn tch rt kh khn v thiu chnh xc, nht l i vi cc my
c phn gii khng cao. V th trong mi mc ch phn tch c th cn phi nghin cu v
chn nhng vch phn tch ph hp loi tr s chen ln ca cc vch ph ca nguyn t
khc. Nu bng cch ny m khng loi tr c nh hng th bt buc phi tch b bt
nguyn t c vch ph chen ln ra khi mu phn tch trong mt chng mc nht nh, cc
vch chen ln khng xut hin na. Tt nhin vic ny l hn hu.
76
Nhng
o vchtheo
ph Ion F(ml/ph)
th yu t ny li l cn thit v ta phi chn iu kin
o
v
xcnu nh
Bng 4.1
phng
quchen
trnhln
Ion
php
thm
hiu
tiu
sutca
caocc
vnguyn
n nhtnht, c c nng ln ca nguyn t cn
S
vha
s t
trng
vch
chun,
xc nh (phn tch) cao nht.
Nguyn t c vch chen ln
Nguyn t v vch phn
Pha
mu qu trnh Ion ha thng ch c ngha i vi cc kim loi
Thc t long
cho thy rng,
tch (nm)
bng
mt
mikimhay
kim v
sau dung
l cc
loi kim th, cn i vi cc nguyn t khc s Ion ha l khng
Vch chen ln
Nng xut hin nguyn t chen
mt nn ph hp,
ng k trong mi trng ca ngn la n kh v h quang in. loi tr s Ion ha mt
ln (ppm)
Thm
muchngcht
nguyn tvo
phn tch
ta c th dng cc bin php sau y:
m cAl-308,215
nng ln,
V- 308,211
>800
+ Chn iu kin nguyn t ha c nhit thp, m trong iu kin nguyn t phn
Dng Cu-324,754
bm
y TI Eu-324,753
>254
tch hu nh khng b Ion ha. 2
4
6
8
10
mu vi mt tc xc
Fe-271,903
Pt-271,904
>054
vo mu
phn tchHnh
mt4.2cht m cho s Ion ha. l cc mui halogen ca
nh +
mThm
chng
ta mong
Pr-411,848
Fe-411,854
>050
hng
nhtha
nca
tc
dn mu
cc kim
loi kim c th Ion hanh
thp
hnca
thIon
nguyn
t phn
tch vi mt nng
mun.
Mn-403,307
Ga-403,298
ln
Nhcht
vyphn
trongtch
iu kin
nguyn t phn tch s khng>025
b Ion ha na.
Sph
Ionhp.
ha ca
>200
Zn-213,856
Fe-213,850
Hin
otrung
(t hp
vch phng
Nu
otng
vchtph
hath)
caca
nguyn
t, y l yu t vt l th ba nh hng n kt
Hintch,
tng
nytrnh
thng
hingim
trongsvng
ngoi
l r rt
nht tch,
hay khi
qu phn
v qu
Ion xut
ha lm
nguyn
t ca
t doplasma
ca nguyn
t phn
do
lmgim
cng
vch
phvng
pht ny
x ca
trung
ha,
nguyn
phn
b
nng
chtS
phn
ln.
c nguyn
nhit tthp,
nn
cckhi
nguyn
t t
ca
chttch
phn
4.2.1:3
bc tch
x ca
ccVht
rn
Ion
cngth
nhiu. Nhng
b
ha ca mi
nguyn
t l khc
v v
ph thuc
tch ha
li
hp
tiapht
phtmc
x c
m
ccIon
nguyn
li ca
lanhau,
sinh
ra,
Trong
michnh
trng
x,
bit
l trong t
ngntrong
la n
kh,ngn
h quang,
nhiu
khith
cnlm
c
vo
nhit
ca
mi
trng
pht
x.
Trong
mt
iu
kin
nht
nh,
ni
chung
cc
nguyn
t
mt bt
cng
phn
tch.
iuhi
nyvcng
gp t
phn
cha
c i
ccmt
htphn
rn rt
nh
li tipht
ca x
vtca
chtcht
mu
cha
b ha
nguyn
ha,gii
haythch
cc
c
th
Ioncacbon
ha cng thp
thliu
cngcha
b Ion hat
nhiu.
Vi
mt nguyn
t, loi
khi nhitthng
ca mi
ht
mui
chy
hon
ti sao
nng ca
lnnhin
th mi
quan hc
gia cng
vchton.
ph Cc
phtht
x I^vny
nng C xcca
trng
phtngn
x cng cao
thcng
nguyn
t cng b Ion ha nhiu hn. Bng 4.2 l mt v d v
lp
v n
chtv
l ca
khng cnla
tuyn
tnh
na.b kch thch pht x ra ph nn, do cng gy kh khn cho
iu
vic ny.
quan st hay o cng vch ph phn tch. Yu t ny th hin rt r khi chn khng
Trn y l mt s yu t vt l c th xut hin trong php o AES v c th nh hng
Bng
ng 4.2
chiu cao ca n nguyn t ha mu v cc iu kin ca ngun kch thch ph khng
n kt
qu phn tch. Nhng mc xy ra l rt khc nhau trong mi trng hp c th, c
ph
hp.
Mc
Ion ha ca mt s nguyn t
khi c,
Mc ny xut hin ln hay nh ph thuc vo:
Cc
yuctkhi
vtkhng.
l
+ Nhitvloi
cayu
plasma,
Thuc
t vt l ny thng c:
nht
v sc
mt
ca dung
mu
N.t
Thb
Ion
ha(eV)
% x,
b Ion ha nhit ( oC):
+ Cc
iu
kincng
ca
mi
trng
kchdch
thch
phS
pht
Trong php o ICP-AES, hay vi k thut nguyn t ha mu trong ngn la, nu mu l
+ Tnh cht ca nguyn t phn tch v hp cht ca n,
4000
dung dch, yu t ny nh hng nhiu n tc 2000
dn mu vo 3000
bung aerosol ha
v hiu
sut aerosol
m
nhca
hng
n
kttch.
qu phn 05,00
tch. Ni chung,26,00
tc dn
+ Cht
nnca
camu
muv
vtthnh
phn
mu00,30
phn
Naha
5,21
ngDo
chun
phiphi
c cng
axit,
loiphp
axit loi
v thnh
phn
ha xut
hc, hin,
vt l theo
ca tt
c loi
cc
cn
xem nng
xt tm
bin
tr khi
chng
tng
02,10
22,00
K
4,32
82,00
nguyn t khc, nht l cht nn ca mu. Yu t ny thng th hin nhiu trong php o
mu c th.
AES dngRb
ngun ngn la4,16
v h quang in. 09,00
loi tr nh hng
34,00
ny chng ta c
90,00
th dng
Cc
yu
t
ha
hc
cc bin php sau y:
Cs
3,87
28,00
70,00
96,00
Trong s
php
o nhau
ph pht
x nguyn
t loi
cc nh
hacht
hc nn
cngca
rt mu,
a dng
v phc
Chnh
khc
v nng
axit,
axit,hng
nng
thnh
phn
00,12
Mg
7,54
00,50
05,60
tp. cc
N cht
xut c
hin
cng
rt khc
nhau nguyn
trong mi
trng
c nhau
th v
nhiu
hp
ca
trong
dung
dch mu,
nhn
gy rahp
khc
vcng
nht
catrng
dung dch
mu.
thCa
trongCc
minh
quhng
trnh phn
tchthng
mt nguyn
nht
phi
cho mu
6,11
00,20
khngVxut
hin.
ha hc
c tht,
dn
nthit
kt01,50
qu m bo sao
15,00
phn tch v cc mu u lpmu t l nghch vi nht ca dung dch mu (hnh 4.2)..
Sr
5,69
00,50
02,35
18,70
Ba
78
5,31
01,00
06,00
23,00
79
77
theo bn hng sau y:

Lm gim cng ca vch ph ca nguyn t phn tch, do s to thnh cc hp cht
bn nhit, kh ha hi v kh nguyn t ha. V d nh nh hng ca cc Ion silicat, sunfat,
photphat, florua.
Lm tng cng ca vch ph, do s to thnh cc hp cht d ha hi v d
nguyn t ha, hay do hn ch c nh hng ca s Ion ha ca nguyn t phn tch.
chnh l tc dng ca mt s hp cht, ch yu l mui halogen ca kim loi kim v kim
th hay lantan Clorua.
S tng cng vch ph khi nguyn t phn tch tn ti trong nn ca mu l nhng
hp cht d ha hi. Lc cc cht nn ny c tc dng nh l mt cht mang cho s ha
hi ca nguyn t phn tch v lm n c ha hi vi hiu sut cao hn. S gim cng
ca vch ph khi nguyn t phn tch tn ti trong nn mu l nhng hp cht bn nhit, kh
ha hi. Lc ny cc nguyn t nn km hm s ha hi ca nguyn t phn tch. Cc cht
nn ny thng l nhng hp cht bn nhit ca cc nguyn t, nh Al, t him, silicat, v.v...
V th vic nghin cu cc nh hng ha hc c trnh by trong chng ny c tnh
cht khi qut chung tt c cc loi c th c chng ta lu khi ng dng php o ph pht
x nguyn t, vi mc ch bit v loi tr cc nh hng ha hc, nu chng xut hin.
Cc nh hng ha hc c th c sp xp theo cc loi sau y:
Nng axit v loi axit trong dung dch mu
Ni chung nng axit trong dung dch mu lun lun c nh hng n cng ca
vch ph ca nguyn t phn tch v nh hng ny thng gn lin vi loi Anion ca axit.
Cc axit cng kh bay hi thng cng lm gim nhiu cng vch ph. Ngc li, cc
axit d bay hi gy nh hng nh (hnh 4.3). iu ny c th thy r rng khi xc nh Ca o
vch ph Ca-422,7 nm trong cc mi trng ca cc axit HClO 4, CH3COOH, HCl, HNO3,
H2SO4, H3PO4, HF vi cng mt nng l 2% (hnh 4.4).
Ni chung, cc axit lm gim cng vch ph theo th t: HClO 4 < HCl < HNO3 <
H2SO4 < H3PO4 < HF, ngha l axit HClO 4, HCl v HNO3 gy nh hng nh nht. Chnh v
th trong thc t phn tch ca php o ph pht x nguyn t (AES) ngi ta thng dng
mi trng l axit HCl hai HNO 3 1 hay 2%, v nng ny nh hng ca hai axit ny l
khng ng k (nh hn 5%).
80
Hnh 4.4
nh hng ca loi axit n cng vch ph.
V d vch ph Ca - 422,7 nm trong php o F - AES (khng kh + C 2H2)
v nh hng ca cc Cation khc trong mu

Dung dch mu phn tch, ngoi nguyn t cn xc nh, cn cha cc nguyn t khc. Cc
nguyn t ny tn ti di dng cc Cation hay Anion tan trong dung dch
81
mu. Cc Ion ny c th lm tng, cng c th lm gim, hoc cng c th khng gy nh

hng g n cng vch ph ca nguyn t phn tch. Khi c nh hng th mc nh
hng ca miIon cng rtkhc nhau trong
tngtrng hp c
th.
Nhng mt cch tng qut th chng ta c th quy nh hng ca cc Cation theo 7 loi nh
trong hnh 4.5 d xem xt.
Loi 1, khi nng ca Ion gy nh hng ln hn C 2 th n khng lm tng cng
vch ph ca nguyn t phn tch na, nh hng ny c s dng tng nhy ca
phng php phn tch mt nguyn t, khi thm vo mu nguyn t nh hng c nng
ln hn C2 (xem ng 1, hnh 4.5).
Loi 2, th ti nng Cl ca nguyn t gy nh hng cng vch ph ca nguyn
t phn tch t gi tr cc i. V th nh hng ny cng c dng tng nhy ca
phng php phn tch. Nhng phi gi (khng ch) nng ca nguyn t gy nh hng
gi tr khng i Cl (ng 2, hnh 4.5).
Loi 3. Trong trng hp ny cng vch ph gim lin tc theo ng cong li khi
nng nguyn t nh hng tng dn u (ng 3 trong hnh 4.5).
Loi 4. Cc Cation ch gy nh hng n cng vch ph ca nguyn t phn tch
khi nng ca n ln hn gi tr C 4. Do vy, nu nng ca cc Cation trong mu
nh hn gi tr C4 th khng phi quan tnm n tm bin php loi tr (ng 4, hnh 4.5).
Loi 5. Trong trng hp ny cng vch ph ca nguyn t phn tch li b gim
lin tc theo ng cong lm, khi nng Cation gy nh hng trong dung dch mu tng
dn v y nht thit phi tm bin php loi tr nh hng ny (ng 5, hnh 4.5).
Loi 6. Khi nng ca cc Cation khc trong mu ln hn gi tr C 5 th chng khng
lm gim cng vch ph ca nguyn t phn tch. Do nu khng tm c bin php
loi tr ph hp, th chng ta thm vo mu Cation gy nh hng vi nng ln hn gi tr
C6, a nh hng gim thnh mt gi tr hng s cho tt c cc mu phn tch v mu
chun. Nh th cng loi b c nh hng ny. Nhng tt nhin l ta lm gim nhy ca
phng php phn tch i mt t.
Loi 7. y cc Cation l lm gim lin tc cng vch ph ca nguyn t phn
tch theo chiu tng dn nng ca n mt cch tuyn tnh (ng 7, hnh 4.5). Do cng
cn phi tm bin php ph hp loi tr nh hng ny, hoc gi cho cc Cation l c nng
nht nh v khng i trong tt c cc mu chun v cc mu phn tch.
nh hng ca cc Cation c trong mu n cng vch ph ca nguyn t phn
tch trong php o ph nguyn t cng rt khc nhau. V d: Ion La(III) trong php o F-AAS
l yu t loi tr nh hng ca cc Ion l c trong mu khi xc nh Ca, Mg, Mn, Al, Fe.
Nhng chnh La(III) li l Ion nh hng v lm gim cng
82
vch ph ca chnh Ca, Mg, Al, Fe rt ln trong php o F-AES. iu c ngha l mi

Cation trong tng trng hp c th v trong mi php li c tc dng khc nhau, m
chnh n trong php o ny th nh hng, nhng trong php o khc li khng gy nh
hng.
Nh vy, nh hng ca cc Cation n cng vch ph ca nguyn t phn tch c
th c hiu ng dng, hiu ng nm v cng c th c hiu ng va nm va tng i vi
mt Ion, khi n cc nng khc nhau. minh ho v nh hng ca cc Cation i vi
vch ph ca nguyn t phn tch chng ta c th xem xt mt s v d trong cc hnh t 4.6 4.8.
Hnh 4.5
Khi qut v nh hng cc ion kim
loi
loi tr nh hng ca cc Cation n cng vch ph ca nguyn t phn tch

chng ta c th s dng mt s bin php sau y hoc ring bit, hoc t hp ca chng vi
nhau, ty tng trng hp c th, v d c th:
+ Thm cht ph gia kh nh hng;
+ Thay i nn ca mu loi tr nh hng;
+ Pha long mu bng cht ph gia lm gim thiu nh hng,
+ Thay i iu kin ha hi, nguyn t ha v kch thch ph;
83
+ Thay i mi trng kh quyn kch thch ph, dng kh tr argon, v.v.
12
16
20
24
28
HEIGHT ABOVE LOAD COIL (mml
Hnh 4.6
nh hng ca chiu cao o n cng vch ph
Nguyn t phn tch: (A) - Fe, (B) - Ca, v (C) -AI
200
Hlnh 4.7
nh hng ca T n Ba (1), Sr(2), v Ca (3)
(nh hng loi 6)
84
400
ng/mL.
nh hng ca cc Anion
Cng vi cc Cation, cc Anion cng nh hng n cng vch ph ca nguyn t
phn tch, v nh hng ny cng tng t nh nh hng ca cc loi axit. Ni chung, cc
Anion ca cc axit d bay hi thng lm gim t cng vch ph. Ch ring c hai Anion
ClO- 4 v CH 3CPPOO-, l gy hiu ng dng (lm tng), tc l lm tng cng vch ph
ca nguyn t phn tch trong mt s trng hp mt
85
vng nng nht nh. Cc Anion khc thng gy hiu ng nm (lm gim) theo th t
Cl-,ON3,CO3,SO4,PO4,SiO3. Trong Anion SiO3c nh hng ln nht, cn t
nht l hai Ion Cl- v NO-3. ng thi khi nng ca cc Anion tng th tc dng nh hng
cng tng theo (hnh 4.9). Do thc t nn trong mi php o phi gi cho nng ca cc
Anion trong mu phn tch v mu chun l nh nhau v mt gi tr nht nh khng i.
Mt khc, cng khng nn chn axit H 2SO4 lm mi trng ca mu cho php o AES m ch
nn dng axit HCl hay HNO 3 vi nng di 2%.
cr
Br'
NO;
so^
PO^
CAII
0,2
0,4
Hnh 4.9
Khi qut v nh hng ca cc anion
Thnh phn nn ca mu
Yu t nh hng ny ngi ta quen gi l matrix effect. Nhng khng phi lc no n
cng xut hin, m ch thy trong mt s trng hp nht nh. Thng thng l cc mu
c cha cc nguyn t nn di dng cc hp cht bn nhit, kh bay hi v kh nguyn t
ha. V d: Khi xc nh cc tp cht lng vt trong cc mu oxit t him, oxit kim loi
kim th, oxit nhm, oxit zircon, cc mu mui NaCl, th cc nn ny s kh cng ca
vch ph ca nguyn t phn tch; qua lm gim nhy ca phng php phn tch.
Trong nhiu trng hp, yu t ny lm gim hng chc ln, thm ch c trng hp lm gim
hng trm ln cng ca vch ph (bng 4.4). Nguyn nhn chnh ca nh hng ny l s
tn ti ca cc hp cht bn nhit trong mi trng pht x. Cc hp cht ny lm kh khn,
cn tr qu trnh ha hi v nguyn t ha ca cc nguyn t phn tch.
loi tr nh hng ca thnh phn nn ca mu phn tch ngi ta c th dng cc
bin php khc nhau, nh:
86
Tng nhit ca plasma kch thch ph;

Chng 5
mu cc
chtPHT
ph gia
cNH
nng
ph hp;
PHNThm
TCHvo
QUANG
PH
X
TNH
Thay i nn ca mu sang nn khc;
Tch loi b nguyn t nn cn tr, khi ba bin php trn khng t kt qu. Tt
nhin
php ny l hn hu.
Nguyn
tc bin
chung
Bng 4.4
Nh chng ta bit, khi cung cp nng lng ha hi, nguyn t ha mu phn tch
v kch thch m hi nguyn t i n pht x th chng ta s thu c ph pht x ca
nh hng ca thnh phn nn ca mu phn tch
mu phn tch. Ph gm ba thnh phn:
Ph vch ca nguyn t v Ion.
Cht nn ca mu
Ph m ca phn t v nhm phn t.
Cng vch ph C=30 ppb php o
AES
Mg-202,60 nm
Ca-422,70 nm
Trong ba thnh phn , th ph vch l thnh phn chnh c trng cho nguyn t v
1. Dung
dchtHCl
Ion trng
thi hi
do, 1%
khi chng b kch thch, ngha l0,220
trng thi hi. Khi 0,250
b kch thch,
Ph nn lin tc.
2. Nh
thm
0,005
cc nguyn
t v1,Ion
s 2%
phtLaCl
ra mt
chm bc x quang hc0,008
gm nhiu tia c bc
sng khc
3
nhau nm trong di ph quang hc (190-1100nm). Nu thu, phn li v ghi chm sng li ta
3. Nh 1, thm 0,5% LaCl 3
0,050
0,060
s c mt di ph gm cc vch pht x ca nguyn t v Ion ca cc nguyn t c trong
3. Nh
2, thm
1% NH
4NO
mu. Trong
tp hp
cc vch
ph
,3+LiBO
th mi2 loi nguyn0,210
t hay Ion li c mt0,245
s vch c
trng ring cho n. Cc vch ph c gi l cc vch ph pht x c trng ca loi nguyn
t y. V d khi b kch thch: Nguyn t Al pht ra vch c trng trong vng UV: 308,215;
309,271nm.
Cu pht
vchphp
c trng
trong
vngchUV:
324,754;
327,396nm.
- M
Trong Nguyn
cc bintphp
trn,rabin
th nht
cng
thc
hin c
trong nhng
pht ramc
vchnht
c nh,
trng v
trong
vng
UV: 259,373;
chng
chng
ta khng
th tng260,570nm.
nhit nguyn t ha ln cao mi c, do
s hnNguyn
ch cattrang
thitrab,
bnc
cht
ca trong
khi t,
hn
na khi nhit
nguyn t ha qu
m pht
vch
trng
vng
UV:279,553;
280,270nm.
cao thChnh
li xut
catrng
s Ionny
ha.
Chotann
php bit
hai v
ba s
l thng
nhhin
cc nh
vchhng
ph c
ngi
c bin
th nhn
c
c mtdng
hay
nht.
ph gia
thng
hay
c
dng
trong
php
F-AES,
ICP-AES
l LaCl
SrCl
2,
vng Cc
mt cht
ca mt
nguyn
t no
trong
mu
phn
tchoqua
vic quan
st ph
pht3,x
ca
LiCl,
KCl,tch,
AlClv
dngc
nhiu
nht
, NH4NO
ca
3 v
3 hay
mu phn
tmcht
xemph
c gia
cc c
vch ph
trng
calnLiBO
hay 2khng,
ngha
lhn
da hp
vo cc
hai
hp.
vchcht
phny
phtvi
xmt
c nng
trng
caph
tng
nguyn t nhn bit chng. l nguyn tc ca phng
php phn tch quang ph pht x inh tnh.
T c s vt l chng ta c th khi qut qu trnh phn tch quang ph pht x nh
tnh gm cc giai on sau y:
Cung cp nng lng ha hi, nguyn t ha mu phn tch to ra m hi nguyn t
t do v kch thch m hi pht ra ph pht x ca chng.
Thu chm sng pht x , phn li v ghi ph pht x ca mu phn tch.
Quan st ph thu c ca mu phn tch theo cc vch c trng ca cc
88
87
nguyn t pht hin chng.

Cc giai on ny c thc hin nh mt h thng my quang ph pht x. H thng
my ny cng gm ba phn chnh tng ng vi ba nhim v nu trn. l:
Phn 1.
Ngun nng
lng ha hi,
nguyn t
ha v kch thch m hi
nguyn t ca mu n pht x.
Phn 2. My quang ph thu, phn li v ghi ph pht x ca mu.
Phn 3. H thng trang b quan st nh tnh v nh lng.
Trong phn tch nh tnh, khi quan st khng thy vch ph pht x c trng ca mt
nguyn t trong ph ca mu phn tch, iu c th xy ra hai kh nng: 1hoc l hon
ton thc t khng c nguyn t trong mu phn tch, 2. Hoc l nguyn t c trong
mu phn tch, nhng nng ca n nh hn nhy pht hin ca phng php phn tch.
V th khng xut hin vch ph pht x c trng ca n. V d: Nu dng 2 loi ngun HQ
v ICP kch thch ph pht x th:
+ Vi ngun HQ: 2 vch Cu nu trn xut hin nng C > 0,0004%
+ Vi ngun
ICP: Cng 2 vch Cu ny,
nhng xut hin nng
C >
00004%. Do vic kt lun kt qu phn tch phi theo phng php phn tch v cc iu
kin trang b dng thu ghi ph ca mu phn tch v nhy ca phng php s
dng.
l hin tng thc t, song ngi ta thng hay quy c v coi nh l khng c
nguyn t trong mu phn tch, khi khng tm c cc vch c trng (2 vch ph) ca
nguyn t trong ph pht x ca mu phn tch, theo k thut dng nh tnh.
Vch chng minh nh tnh v cch chn
Mun xc nhn s c mt hay khng c mt ca mt nguyn t no trong mu phn
tch, ngi ta phi tm mt s vch ph c trng ca nguyn t trong ph ca mu phn
tch xem c hay khng, t m kt lun c n hay khng c n trong mu phn tch.
Nhng vch ph c trng c chn c gi l vch chng minh ca nguyn t y. Ni
chung, pht hin mt nguyn t t kt qu chnh xc v chc chn, ngi ta phi chn t nht
hai vch chng minh khi quan st ph ca mu phn tch. Cc vch ph ny phi tha mn mt
s iu kin sau y:
Nhng vch ph ny phi r rng v khng trng ln vi cc vch ca nguyn t khc,
nht l nguyn t nng ln.
N phi l nhng vch ph nhy, c th pht hin c cc nguyn t trong mu vi
nng nh (phn tch lng vt).
Vic
chn cc vch
ph chng minh cho
mtnguyn
t phi xut pht
ngun nng lng dng kch thch ph ca mu phn tch, v trong ngun kch
89
thch c nng lng thp
th ph ca nguyn t l ch yu v vch nguyn t ca n
thng l nhng vch nhy. Ngc li, trong ngun kch thch giu nng lng (ICP) th ph
ca Ion l ch yu. Cho nn phi ty thuc vo ngun nng lng dng kch thch ph
m chn vch chng minh l vch nguyn t hay vch Ion cho ph hp.
Phi cn c vo my quang ph c th thu, phn li v ghi c trong vng sng no m
chn vch chng minh cho mt nguyn t nht nh. V d chng minh Na, nu ph mu
c ghi trn my Q-24 (vng ph 200-400 no th ta phi chn hai vch Na 330,30 v Na
330,27 nm. Ngc li, nu ghi trn my lng knh thy tinh (vng ph 360-780 nm.), th li
phi chn hai vch Na 589,60 v 589,00 nm.
Nu
dng my cch t PGS-2 (vng ph 200- 1100 nm) th chn 4 vch trn u c.
nhy ph v kh nng pht hin
Trong phn tch quang ph pht x nguyn t ngi ta thng s dng hai khi nim v
nhy. l nhy tuyt i v nhy tng i xem xt hay nh gi kh nng phn
tch ca mt phng php.
nhy tuyt i (cn gi l nhy khi lng)
nhy tuyt i l lng gam nh nht ca mt nguyn t cn phi a vo kch thch
ph trong plasma cn pht hin c t nht hai vch ph c trng ca nguyn t y trong
mt iu kin nht nh chn, ngha l cn chng minh c nguyn t y. V d, ch c
th pht hin c cc nguyn t:
+ Pb khi trong plasma h quang kch thch ph phi c 0,000007 g Pb.
+ Al khi trong plasma h quang kch thch ph phi c 0,0000055 g Al.
Cn cc gi tr nh hn th khng th pht hin c Pb v Al. Cc gi tr (lng
gam) 0,000007 g v 0,0000055 g c gi l nhy tuyt i ca Pb v Al trong php phn
tch . Nh vy, mi nguyn t khc nhau c nhy tuyt i khc nhau v ph thuc vo
mi nguyn t, cc iu kin kch thch v ghi ph ca mu (bng 5.1).
nhy tng i (cn gi l nhy nng )
nhy tng i l nng nh nht ca mt nguyn t phi c trong mu phn tch
cn c th pht hin c t nht hai vch ph c trng ca n, trong cc iu kin thc
nghim nht nh chn. Cn nu nh hn nng th ta khng th tm c mt vch
c trng no ca n trong ph ca mu phn tch. V d: pht hin c hai vch ph c
trng ca cc nguyn t sau trong ngun h quang, phi c:
90
+ Pb vi nng trong mu l => 0,0008 %

+ Al vi nng trong mu l => 0,0004 %
+ Cu vi nng trong mu l => 0,0005 %
Cc gi tr 0,0008; 0,0004; 0,0005 % c gi l nhy tng i ca Pb, Al v Cu
trong php phn tch ny. l nng nh nht cn pht hin c cc nguyn t theo
2 vch ph pht x ca n trong mt iu kin nht nh chn .
Cng nh khi nim trn, mi nguyn t khc nhau
cng c
khc nhau. Ni chung, cc nguyn t c t vch ph thng

Trong phn tch
nhy tng i
c nhy cao (bng 5.1).
ngi ta hay dng khinim nhy tng i v ch i khi cn
thit mi dng khi nim nhy tuyt i, v dng khi nim nhy nng chng ta d
so snh nhy ca cc nguyn t vi nhau hn. Nh vy, kh nng chng minh ca mt
nguyn t ph thuc vo nhy ph ca nguyn t . Nguyn t no cng nhy ph th
cng c th pht hin c n ngay nng rt nh (tt nhin l nng ny phi cn ln
hn nhy tng i).
Ngoi nhy ph ca mt nguyn t, kh nng chng minh ca nguyn t cn ph
thuc vo mt s yu t khc, nh:
+ Cc iu kin thc nghim ha hi, nguyn t ha mu, kch thch cc nguyn t
v iu kin trang b ghi o ph ca mu phn tch.
+ Cht lng ca h thng quang hc ca my quang ph;
+ Cu to, thnh phn vt l v ha hc ca mu phn tch;
+ Mi trng kch thch ph;
+ Trng thi tn ti ca nguyn t trong mu;
+ Cht ph gia thm vo mu phn tch.
Nhng trong mt iu kin th nghim nht nh ph hp c chn, vi h thng
trang b nh nhau v cng mt loi mu, th kh nng chng minh ca mt nguyn t ch cn
ph thuc vo nhy ph ca nguyn t phn tch v trang b thu nhn ph m thi.
V th mun nh gi, so snh kh nng chng minh ca mt nguyn t bng ph pht
x nguyn t, chng ta phi nghin cu chng trong nhng iu kin nht nh nh nhau v
ph hp, nh ngun nng lng ha hi, nguyn t ha v kch thch ph, cng nh cc
iu kin ghi ph ca chng.
Bng 5.1
91
Vch
c trng
cacch
mtloi
s nguyn
t
S trng
vch v
tr
Ph phttx ca mt
t thng c
rt nhiu
khi
n
hng
ngn
Nguyn
Vchnguyn
ph (nm)
Cng
vch, c
Nng
xut
hin
(%)vch.
Cc vch ny phn b t vng sng ngn n sng di ca di ph quang hc (190-1100 nm).
Nguyn t no c cu toI lp
v in t cng phc
tp, nht l s in t0,0001
ha tr cng nhiu,
328,068
5500R
th ph pht
x ca chng cng c nhiu vch, v d nh Fe. V th, ph pht x ca mu phn
A
g
I 338,289
2800R
0,0006
tch, nht l cc mu a kim loi, th ph pht x ca n tt nhin cng c nhiu vch. Trong
di ph tt nhin c thI 520,907
c hai nguyn t khc 100R
nhau, nhng chng li c0,02
th pht ra tia bc
546,549
100Rnm. Trong trng hp
0,025
x cng di sng, hocI khc
nhau khng n 0,01
ny vch ph ca
hai nguyn t l trngInhau
hon ton hoc l 48R
chng ln nhau mt phn,
ngha l c hin
257,510
0,08
tng trng vch, hin tng quy ri v chen ln ca cc vch ph ca cc nguyn t vi
0,001
I 308,216
320R
nhau.
Al
I 309,271
650R
0,0005
Vch ph trng
I 396,153
900R
0,0003
Vch ph trng l cc vch ph ca cc nguyn t khc nhau, nhng c cng mt gi tr
I 249,678
420R
0,005La 412,323nm
di sng. V th trn knh
nh ta ch thy c mt
vch duy nht. V d vch
trng vi Ba
vch ph Er 412,823nm (khng nhy). Nn khi nh tnh khng c chn vch La
I 249,773
480R
0,003
412,323nm chng minh
nguyn
t
La,
mc
du
l
mt
vch
nhy
ca
La.
0,02
II 233,527
55R
Vch quyBari v chen ln
II 234,758
16R
0,05
Vch quy ri v chen
ln l vch ph ca 6500R
cc nguyn t khc nhau,0,0005
nhng chng c
II 455,404
i sng xp x bng nhau m my quang ph khng phn gii c thnh cc vch ring r.
0,001
II 493,409
2000R
V th trn knh nh hai vch ph ny nm k nhau v c mt phn chng ln nhau. Do khi
650R
quan st ta cng ch thy II
c553,555
mt vch rng. Song c
trng hp hai vch c0,006
th tch ra c
20trong hai nguyn t c
315,887
0,05
nng nh ca c hai II
nguyn
t, nhng khi mt
nng ln, tt
nhin l vch ca nguynIIt317,933

c nng ln s ln 50
t vch ca nguyn t c
nng nh.
0,02
l s quy ri v chen ln ca cc vch ph ca cc nguyn t. V th, chng minh nh
Ca
II 393,367
4420R
0,0005
tnh mt nguyn t chng ta cng phi loi tr nhng vch ph c hin tng .
0,001
II 396,847
2200R
Ph m
II 422,673
1100R
0,003
Bn cnh s trng vch v s quy ri ca cc vch ph ca cc nguyn t khc nhau,
I 2824,34
50
0,05
th ph m ca cc phn t v nhm phn t cng l mt yu t gy kh khn cho php phn
I 3247,54
5000R
0,0004
tch nh tnh, v trong nhiu
trng hp th ph m
ca cc phn t che lp
mt cc vch c
Cu
trng ca cc nguyn t khc.
iu ny th hin rt
r trong vng kh kin0,001
(380-780 nm), nu
I 3273,96
2500R
ta kch thch ph ca mu Iphn
tch trong mi trng
5105,54
40 khng kh, hay trong cc
0,06my quang ph
c phn gii khng Iln.
0,001
248,328
280rh
l nhng kh nng c th xy ra khi quan st bt k mt bng vch ph no ca cc
200
I 259,941
0,003
nguyn t ha hc. Song khng phi v th m khng chng minh nh tnh c mt nguyn
0,001
Fe
I 302,065
280R
t theo ph pht x ca n. Bng thc t, ngy nay ngi ta c rt nhiu cch khc nhau
I 358,120
600R
0,0005
loi tr cc yu t nh hng . V d: Trong iu kin kch
I 371,994
700R
0,00045
I 373,448
92
700r
0,0005
93
thch ph thng thng th tt nhin khng th xut hin cc vch ph ca cc cht kh nh

oxy, halogen, nit,... Hoc khi phn tch cc mu thng thng tt nhin khng th c kh
nng
trng
vch vi cc nguyn t
phng x, t him, nguyn t qu,...
Mt khc cn c vo cng ca cc vch ph hay nng xut hin ca cc vch ph khc

nhau ca cc nguyn t, chng ta cng c th d on c trong iu kin c th th vch
ph c xut hin hay khng, ngha l trong mi trng hp c th cn phi lun lun ch
n nhng kh nng trng vch, s quy ri v chen ln ca cc vch ph vi nhau. Song
cng t cc trng hp c th m tm cch khc phc cho ph hp.
Sau y
lmt s v d
v mt vi phng php loi tr
mt s yu t nh
hng nu.
Li dng tnh cht bay hi khc nhau ca cc nguyn t theo thi gian chn thi gian
ghi ph cho thch hp (theo ng cong bay hi). T c th loi tr c s quy ri ca
cc nguyn t khc i vi nguyn t phn tch.
Chn iu kin v ngun nng lng kch thch ph ph hp, to ra s kch thch ph
c u tin v chn lc i vi mt vi nguyn t chng ta cn kho st, phn tch.
Chn mi trng kch thch ph cho ph hp. V d: Khng kch thch ph trong khng
kh m kch thch chng trong mi trng ca mt kh tr hay hn hp ca kh tr vi oxy.
Trong trng hp ny ngi ta c th loi tr c hon ton nh hng ca ph m ca cc
phn t v nhm phn t CN. Chnh v th hin nay trong phn tch quang ph pht x, ngi
ta thng kch thch ph ca mu phn tch trong mi trng ca kh tr Al v hn hp ca
argon vi oxy.
Thm vo mu nhng cht ph gia thch hp c th loi tr cc hp phn sinh ra ph
quy ri khng c li, nh to ra s bay hi chn lc, s bay hi phn on ca cc nguyn t
khc nhau.
Chn my quang ph c phn gii ln v vng ph ph hp thu, phn li v ghi
ph ca mu phn tch. Trong thc t phn tch, th bin php ny trong nhiu trng hp
c kh nng loi tr hon ton cc yu t nh hng nu.
Nu tt c cc bin php trn s dng m vn cha loi tr c nh hng, th phi
dng phng php tch chit no loi cc nguyn t cn tr ra khi mu phn tch. Tt
nhin y l bin php cui cng v thc t hu nh rt t khi phi s dng n.
Cc phng php phn tch nh tnh
Mc ch ca phn tch quang ph pht x nh tnh l pht hin cc nguyn t, ch yu
l cc kim loi trong cc mu phn tch, n gm c hai loi yu cu, do cng c 2 kiu
nh tnh:
94
Phn tch nh tnh tng phn v

Phn tch nh tnh ton din.
Phn tch nh tnh (T) tng phn tc l kim tra xem trong mu phn tch c cha
nhng nguyn t m ngi ta cn quan tnm n hay khng, cn cc nguyn t khc th khng
cn bit n. V d ngi a mu yu cu tm xem trong mu ny c Pb hay khng?
y l phn tch T tng phn, v ch cn tm nguyn t Pb trong mu. - Ngc li,
phn tch nh tnh ton din l phi xc nh xem trong mu phn tch cha bao nhiu nguyn
t c thy. V d ngi a mu yu cu tm xem trong mu ny c bao nhiu kim loi c
thy? y l phn tch T ton din.
Chnh t thc t m ngi ta cng c mt s
cch quan st nh tnh khc
nhau, da theo ph pht x ca mu.

Phng php quan st trc tip trn mn nh
Nguyn tc ca phng php ny l trn mn nh ca my quang ph (mt phng tiu)
ngi ta t mt mng m, trn mng m ny c nh du v tr cc vch c trng ca mt
s nguyn t nht nh. ng thi b tr mt h thng thu knh lp phng i quan st
trc tip mn nh .
Nh vy, mun nh tnh mt mu no , ta thu ph ca mu phn tch, khi kch thch
chng bng mt ngun nng lng ph hp v quan st ph mt cch trc tip trn mn nh
ca my nh h thng knh lp phng i.
Khi da theo cc vch ph c trng nh du trn mng m m kt lun c mt
hay khng c mt nguyn t trong mu phn tch.
Phng php ny nhanh, n gin. Nhng ch gii hn trong nhng mu n gin v
nhng nguyn t cn phn tch c nh du cc vch ph c trng
ca
trn mng m ca my quang ph.

N ch yu phc v cho phn tch luyn kim, kim tra nhanh mt vi nguyn t cn
thit, nh Mn, Cr, Si, C, Al,...V cng v th m c mt loi my quang ph chuyn dng cho
mc ch ny. l cc loi my Styloscop. My quang ph ny phc v cho ni dung phn
tch nh tnh tng phn ca ngnh luyn kim l ch yu.
Phng php so snh ph
y l phng php n gin, chnh xc, nhng cng ch phc v cho mc ch phn
tch nh tnh tng phn.
Nguyn tc ca phng php ny l: Mun nh tnh mt nguyn t X no ,
95
chng ta phi ghi ph ca nguyn t X nguyn cht k vi ph ca mu phn tch. Ri tm mt

nhm vch c trng ca nguyn t X trong mu nguyn cht v so snh nhm vch ph
vi ph ca mu phn tch xem c nhng vch ph c trng hay khng trong ph ca mu
phn tch.
Trn c s m kt lun c mt hay khng c mt ca nguyn t X trong mu phn
tch. Phng php ny tuy n gin, nhng vi mi nguyn t cn tm ta li phi ghi mt ph
ca nguyn t nguyn cht.
V th chng nhng tn km knh nh, in cc v thi gian, m nhiu khi cn khng c
ca nguyn t X tinh khit lm ph so snh. Do n cng b hn ch v khng c
ng dng nhiu trong thc t.
Phng php ph chun (Dng bn atlas)
Ph chun hay cn gi l bn atlas ph l cc bng vch ph ca Fe theo mt my
quang ph nht nh. N c xem nh l mt thang di sng phc v cho vic nh du
v tr cc vch ph c trng ca cc nguyn t. N c cu to gm 2 phn.
Phn trn l mt dy cc vch ph ca Fe trong mt vng ph nht nh ca my quang
ph. Phn di, tc l k vi ph ca Fe, l v tr cc vch ph c trng ca cc nguyn t
khc v trn cng l thang s sng (hnh 5.1).
Nh vy, mun nh tnh mt mu no , ta cn phi ghi ph ca Fe v k l ghi
ph ca mu phn tch.
Sau nh my chiu ph v bn atlas ta c th nhn bit c trong mu phn tch c
cha nhng nguyn t no khi quan st ph ca mu phn tch theo cc vch ph c trng
ca tng nguyn t, bng cch em ph ca Fe trn knh nh lm trng vi ph ca Fe trn
bn atlas.
V th, nh tnh bao gi cng phi ghi ph theo tng cp, mt ph ca Fe v k l
ph ca mu phn tch, ngha l c bao nhiu mu phn tch th c by nhiu cp ph tng
ng.
Phng php ny ph hp cho c hai mc ch phn tch nh tnh tng phn v nh
tnh ton din. Nhng mi my quang ph cn phi c mt b atlas hon chnh cho n i vi
tt c mi nguyn t cn nghin cu.
V th ngy nay hu ht cc phng th nghim ch dng phng php ny cho c hai
mc ch phn tch nh tnh. Cc hng bn my quang ph cng cung cp cc bng
atlats cho cc my ca h.
Hnh 5.1 l v d v mt on ca bn atlas ca my quang ph.
96
47
VM
97
98
Chng 6
PHN TCH PH PHT X NH LNG
Nhng vn chung
Phng trnh c bn v nguyn tc
Phng php phn tch quang ph pht x nguyn t nh lng da trn c s gia
nng ca nguyn t cn phi xc nh v cng ca vch ph pht x do n pht ra, khi
b kch thch trong nhng iu kin thch hp, c mi lin h tuyn tnh v n tr theo hm
s.
I. = f (C)
( 6. 1)
trong mt gii hn nht nh ca nng C ca nguyn t phn tch, trong I. l

cng ca vch ph pht x ca nguyn t , cn C l nng ca nguyn t trong
mu phn tch.
Bng l thuyt v thc nghim ngi ta tm c mi lin h v c m t theo
phng trnh Lmaskin - Schraib nh trnh by trong chng II trn l:
I. = a.Cb
( 6. 2)
Theo phng trnh ny, nu c mt s mu u (mu chun) c nng C bit chnh

xc, v d C1, C2, ... Cn v xc nh c cng ca 1 vch ph pht x
tng ng ca chng, th ta c th dng c ng chun I - C, ri t c th d dng tm
c nng Cx cha bit.
Nhng trc y (trc 1965), do khng xc nh trc tip c gi tr cng pht
x I. ca mt vch ph, m ngi ta phi chiu chm sng pht x cng I. ln knh nh.
Sau xc nh cng hay en ca chng trn knh nh ti ch b chm sng I. tc
dng ln. en S. ny c tnh theo cng thc:
S. = y.log.I.
trong Y l h s
(6.3)
nh tng ca knh nh.Nh vy, ta c phng trnh h qu
nh sau, vi k = y.log a:
S. = Y b.log.C + k
(6.3)
T thc t , hin nay chng ta c hai phng trnh c bn ca php phn tch nh lng
theo ph pht x ca nguyn t. Nu cc my cho php xc nh trc tip
99
Vch
v cch
chn
c phn
gi trtch
cng
Ix
th chng ta tnh ton theo phng trnh (6.2). Nu cc my quang
ph phi
xc tr
nhph
gin

Ix en
qua Svic
en S, th phi tnhtch,
tonngi
theo
loi
nntip
khicng
xc nh
ca xc
vchnh
ph
phn
phng trnh (6.4), ngha l phng trnh th nht c dng y = ax, cn phng trnh
ta th hai
th c dng
= axtheo
+ b,mt
song
chng
phng trnh ca mt ng thng. Nhng nu o
thng
thc yhin
trong
hai u
cchlsau:
theo phng trnh en S, chng ta phi loi en ca ph nn. V th trong trng hp
Cch 1: o hiu s en gia vch ph phn tch v ph nn, tc l tnh gi tr S
ny phng trnh thc nghim s phi l:
trong phng trnh (6.4) theo cng thc S = (S v - Sn). Trong Sv v Sn l en ca vch
ASo=(hnh
Y.b.logC
+k
(6.5)
v en ca nn bn vch
6.1). o
Do , phng trnh (6.3) v phng trnh (6.5) c gi l phng trnh c bn ca
Cch 2: o hiu s en gia mt vch phn tch Spt v mt vch ph so snh S ss
phng php phn tch quang ph pht x nguyn t nh lng. ng biu din cc phng
(hnh 6.1), ngha l c S = (S pt - Sss). Trong :
trnh ny c m t trong hnh 6.1.
+ Vch phn tch l nhng vch ph ca nguyn t cn phi xc nh c chn xc
Ix n trong mu phn tch. N c chn ra t nhng
/
cvch c trng ca
nh nng ca
y
/ .
0,4Khi cn xc nh nhng
(A)
Jtr
nguyn t y.
nng nh thBphi chn/ nhng
vch c nhy cao.
+ Vch so snh l nhng vch ph ca mt nguyn t no c chn o en

phc v cho0,3
vic b chnh nn theo phng php 2 vch ph. Nguyn t cung cp cho vch so
snh ny c gi l nguyn t so snh. N phi c nng khng i trong c mu u v
0,2
mu phn tch.
1 N c th l nguyn t c s ca mu phn tch hay l mt nguyn t khc
c thm vo vi nng ph hp v khng i tt c mu v cng ca n phi nm
0,1 - 25 %
A en ca vng tuyn tnh.
trong vng 10
Nh vy, vch ph phn tch v vch ph so snh to thnh mt cp vch phn tch. Do
0 kt qu chnh xc trong cp vch phn tch th vch so snh v vch
c*
, c c
phn tch
cn phi tha
mn
, * mt s iu kin
c2 nht nhc3nh sau:c4
0,5
c5
Chng phi l hai vch cng loi, hoc l hai vch nguyn t,
s
2 vch
0,4
ln cng bc Ion ha.
hoc l
(B)
Th kch thch ca hai vch ny phi gn bng nhau. Nu bng nhau l iu l tng.
0,3
Tt nhin trng hp bng nhau l iu him c, do cn chn bi vch c th kch thch

ph cng gn bng nhau th cng tt. V nh th s loi b c nh hng ca s dao ng
0,2
ca nhit plasma.
Hai vch phi khng xa nhau qu 10 mm trn knh nh (mt phng tiu), v ch trong
iu kin h s nh tng knh nh Y mi thc s l hng s, ngha l hu nh khng ph
0,1
logC
thuc vo di sng ca cc vch ph.
Hai vch phi nt, r rng v gi tr S ca chng phi thay i nhy vi s bin
0
logC,t phn
logC
logCmu, nhng
logC
logC nhy vi nhng dao ng
thin nng ca nguyn
tch trong
li khng
2
ca iu kin thc nghim.

Hnh 6.1
Gi tr S phi khng qu ln, m cng phi khng qu nh. N phi nm trong vng
Mi quan h gia cng vch ph v nng cht.
gi tr en tuyn tnh ng cong, c trng ca knh nh ghi ph.
(A): Mi quan h I-Cx; (B): Mi quan h S-logCx
100
101
Trong mt s trng hp c th khng nn chn vch phn tch l nhng vch d xut
hin hin tng t o (t hp th), v khi phm vi tuyn tnh ca ng chun s b hp.
Tt nhin yu t ny l khng bt buc cho mi trng hp. N ch l mt iu ch thm
trong nhng trng hp cn thit, khi xc nh vng nng khng qu nh.
Nhng hin nay, vi cc my quang ph th h mi, o trc tip cng vch pht x
I. v trong my c sn h thng b chnh nn ca vch phn tch, th ngi ta ch cn o mt
vch phn tch l .
Cch biu din nng trong phn tch quang ph
Trong phn tch quang ph nh lng ngi ta thng dng v biu din nng theo
cc khi nim sau:
Nng phn trm (%).
Nng phn triu (ppm) v cc n v c s ca n.
Nng microgam (p,g/mL) v cc n v c s ca n.
Nng phn trm
Trong phn tch quang ph ngi ta thng hay biu din nng phn trm (%) theo
hai cch:
Nng phn trm tuyt i: Ch cho ta s phn trm ca nguyn t phn tch so vi
tng khi lng m ca mu phn tch, ngha l c tnh theo cng thc:
m
%Cxt = m 100
m
( 6. 6)
trong mx l s g ca nguyn t phn tch c trong khi lng mu mg.

Nng phn trm tng i: Ch cho ta bit s phn trm ca nguyn t phn tch so
vi khi lng m ca nguyn t c s (nguyn t c thnh phn > 90%) ca mu phn tch.
N c tnh theo cng thc:
%C
Trong hai cch
xd =
m
^ 100
m
g
(6.7)
biu
din
ny
th
cch
biu
din
th
nht
c
ng
dng
nhiu
hn, cn cch th hai ch dng khi so snh nng ca nguyn t phn tch vi nguyn t c
s ca mu. Trong thc t, ngi ta quy c rng, khi ni nng phn trm th ngi ta hiu
l nng phn trm tuyt i. Ngc li mun dng cch th hai ngi ta phi ni v ghi
y l nng phn trm tng i.C ,m
%Cxt =^m
( 6. 8)
m
102
Nng phn triu (ppm) v cc n v sau n

i lng nng ppm (phu pa mill Ion) l n v nng c tnh theo n v l
mt phn triu ( 1/1.000.000) theo n v khi lng hay mt phn triu theo n v th tch
ca mu phn tch (cho mu lng). Nn theo khi nim n v ny, mt nguyn t phn tch
c nng 10-6g trong 1 gam mu, th gi tr ny c gi l 1 ppm. Nh th, nu vit theo
khi lng: 1g/T, hay 1 mg/kg, hay 1^g/g, hay theo th tch 1 pl/mL; hay 1 mL/L; hay 1 L/m 3,
th u tng ng 1 ppm.
Cn cc n v nh hn sau ppm l:
ppb v 1 ppb bng 0,001 ppm
ppp v 1 ppp l bng 0,001 ppb = 0,000001 ppm
ppf v 1 ppj l bng 0,001 ppp = 0,000001 ppb = 0,0000000001 ppp
Cc n v ny hn km nhau 1000 ln. Trong phn tch vi lng v siu vi lng, h
n v ny c dng ph bin nht.
Nng microgam
Loi nng ny c biu th theo hai cch, c th l:
Theo th tch mu (khi lng th tch)
A1. Microgam/L: S microgam ca cht phn tch c trong mt lt dung dch mu, k
hiu l 0.g/l. V d, nu vit nng ca Pb l Cpb: 1,2 0.tg/l th c ngha l c trong 1 lt
dung dch mu s c 1,2 microgam ca Pb.
A2. Microgam/ml: S microgam cht phn tch c trong mt mnh dung dch mu, k
hiu l p,g/mL. Nu t trng ca dung dch d = 1, th n v ny tng ng ppm. V d nu
vit Cpb: 1,2 p,g/mL th c ngha l trong 1 mun dung dch mu s c
microgam ca Pb.
Theo khi lng mu (khi lng/khi lng)
B1. Microgam/gam: S microgam ca cht phn tch c trong mt gam mu v k hiu
l pg/g. V d, nu vit Cpb: 2,5 p,g/g, th c ngha l c trong 1 gam mu s c
microgam ca Pb.
Cng hon ton tng t nh trn chng ta cng c cc n v biu din nng theo
khi lng mu l: p,g/g; mg/kg; g/T. Cc n v ny u l tng ng ppm.
B2. Microgam/ml: S microgam ca cht phn tch c trong mt ml dung dch mu v
k hiu l p,g/mL. V d, nu vit Cpb = 2,5 p,g/mL, th c ngha l c trong 1 ml dung dch
mu s c 2,5 microgam ca Pb.
Cc n v c s ca ug
l nanogam (ng), picrgam (pa). Do cng c cc khi nim tng ng l:
103
cc mu
u
phipg/g.
bn Cc
vngn
theo
ngha
chun
b
ng/L, Thnh
ng/mL,phn
pg/L,ca
pg/mL
vagng/g
v thi
nnggian,
sau
p,g ll:sau
ng khi
v pg
chng
- hay
attogam;
xong
chng
khng
thay
v mi
mt,quan
t nng
nc
trngch
thiralin
ktbng
v cu
u km
nhau
1000
lni
v mi
tng
ca chng
trong
6.1,trc.
6.2, v 6.3.
pa - picogam.
Khi mu
u
v mu
phn tch
Mu chun
trong
phn
tch quang
phtha
phtmn
x nhng iu kin trn, ngha l mu u v mu
fg
femtogam;
phnTrong
tch ph
hptch
vi quang
nhau vph
minh
mtlng,
th cc
cdng
trngmt
v ph
ca chun
mu phn
l tng
t nhau.
phn
ng
tch ca
mt
V
d:
ngmc
- nanogam.
nguyn t no phc v cho
ch xc nh n trong mt i tng nht nh, hay
+ Nn
nhau,
xc nh
cc ca
hngph
s l
vtnh
l ca
p,gphng trnh
- c bn, ngi ta phi dng mt dy mu chun
(mu u).
Thnh
phn,
ca
dy mu
quyt
nhcdng
chnh
xc
+ ng
cong
baytnh
hicht
ca v
ccnng
nguyn
t trong
muu
uny
v s
mu
chun
ging
microgam.
v
ng n ca kt qu phn tch. V vy, m bo cho php phn tch t kt qu tt th
nhau,
ppm:
phnkin
triusau:
(part per mil Ion)
dy mu u ny phi tho mn
mtmt
s iu
+ Thnh phn ph vch ca nguyn t l nh nhau, c bit l nguyn t c s phi
Bng
6.3 ng nht trong cc mu,
hon ton
+ Thi gian kch thch ph ca cc mu l nh nhau.
Bng 6.1
Nng u c
Chuyn sang nng th hai
Chnh
trng
c s
Mi quan
h nh
gianhng
cc loic
n
v nng
ny ca ph mu m ngi ta c th pht hin c
Nng
H s phi nhn vo
xem mu phn tch v cc mu u c ch luyn c ng nht hay khng. Mu chun v
1 ppm
g/L
0,01 p
mu phn tch c th dng bt, rn hay dung dch l ty thuc vo nguyn t phn tch,
p
1 v
ppm
cc trang b
iu kin kch thch php,g/L
no cho kt qu tt nht.
n v gc
Tng ng vi (*)
Tng ng vi (*)
1 ppmminh v khong xc nh
Mol/L (M)
0,0001 p.A
Gii hn chng
1000 ppm
1 mg/mL
10"3 g/mL
Cng1 nh
phng php phn tch
quang ph pht x
0,0001
ppm cc phng php phn
% tch
trngkhc,
lng
6
ppmc mt gii hn nht
1 p,g/mL
nh lng1cng
nh i vi mi nguyn t10"
trongg/mL
mt i tng nht
1 Mg/L
ppm
1/p
nh. l1 mt
nguyn t cn kho st (xc
nh)
m php o nh
9
ppb khong nng ca
1 ng/mL
10"
g/mL
Mg/L
lng
/10000
lng cn 1cho
kt qu tin cy, ngha l%ctrng
mt cn
trn v cn di ca 1mt
php.pxc nh i
1
ppp
1 pg/mL
10"12 g/mL
vi mt nguyn
gia gii hn trn v gii hn di
p c gi l
1
ppd t. Vng nng nm
ng/mL
15
ppf ca phng php phn
1 fg/mL
" ca
g/mL
khong xc1nh
tch. Tt nhin khong xc 10
nh
mt phng php
i vi mi1nguyn
t l khc nhau1v
ngay mt nguyn t, nu o10nh
lng theo cc vch
ppa
ag/mL
"18 g/mL
ph khc nhau th khong xc nh ca n cng khc nhau. Vch ph no cng nhy th
trong :
khong xc nh cng hp v n nm trong vng nng cng nh (bng 6.4). Gii hn
T trng
ca dung
chngp:minh
v khong
xcdch
nh ca mt nguyn t c th c xc nh theo hai cch:
Bng 6.2
Phng
php
thc hay
nghim.
A:
Nguyn
t gam
phn t gam ca cht phn tch.
Mi quan h gia cc loi n v nng
Mu
uphp
phi ton
c thnh
Phng
thngphn
k. ha hc v vt l ging nh mu phn tch, ngha l trong
mu phn
tch
c t
cha
nguyn
txc
nonh
v tn
ti
trngcn
thi hp cht no th cc mu
Trong
thc
canhng
phn tch,
vic
vvi
m
rng
n
v gc
Tng
ng
cc
n v di ca mt phng php
u
chun)
cng
c thnh
nh
nht
l cht
mu.
Ccc
nh
th mi
phn(mu
tch lun
lun
c phi
ngha
ln, vphn
n rt
cnth,
thit
trong
cngnn
vicca
phn
tch
nguyn
t
10-3
1
mg
loi
b
c
nh
hng
ca
sai
khc
v
thnh
phn
n
kt
qu
phn
tch.
vi lng v siu vi lng, ngha l nng gii hn di pht hin c ca phng php
-6
-3
1
10phn
10trng
^g v
u
mu
phi
c hp
x lcvth
chbluyn
tronggiai
cngon
mtlm
iugiu
kinsnh
phn Mu
tch cng
nh,
th
trongtch
nhiu
qua c
b
nhau
v cng
mtm
trng
thi.xc nh
mu cn
phn
ta-9vn
10
10-6 c. 10-3
1 ngtch,
Nng1
tch
-9 trong cc-6mu u phi
10-12 t phn10
10
10-3 tht chnh xc. Khong nng
pg ca nguyn
ca c dy mu u phi phn b ri u trn ton b phn vng tuyn tnh ca ng
10-15
10-12
10-9
10-6
10-3
1 pf
chun.
10-18
10-15
10-12
10-9
10'6
10-3
1 ag
trong :
106
104
105
Trong phn tch quang ph, gii hn di ca phng php nh lng mt nguyn t
c biu th bng nng Cmin' m ng vi cc nng C x ca cht phn tch m nh hn
Cmin th vch phn tch ca nguyn t bin mt vo nn ca ph (khng xut hin), v ta
khng quan st c n na. Ngc li, ng vi cc nng C x no ln hn Cmin th vch
phn tch cn xut hin r rng, php o cho kt qu tin cy V th khi khng thy vch phn
tch ca mt nguyn t trong ph ca mu phn tch, th c th xy ra theo hai trng hp. C
th nng ca nguyn t trong mu l thc t bng 0, tc l khng c nguyn t . Hoc
cng c th l c nguyn t trong mu phn tch, nhng nng ca n trong mu l nh
hn nng gii hn di ca phng php phn tch (C min).
Theo Kaiser gii hn di (cn di) ca phng php phn tch quang ph mt nguyn
t theo 1 vch ph nht nh c tnh theo cng thc sau:
(n) = 3(Iv - In)
(6.9)
trong : I(v) l cng pht x ca vch phn tch ng vi nng C min;

I(n) l cng ca nn; l s dao ng ca gi tr en ca nn.
Trong phng php phn tch quang ph, ngi ta phn bit cn di (gii hn di)
thnh hai khi nim:
Gii hn pht hin: L nng nh nht ca mt nguyn t trong mu phn tch
cn pht hin c cc vch ph ca n (t nht hai vch nhy) theo cc iu kin thc
nghim chn.
Gii hn xc nh (nh lng): L nng nh nht ca mt nguyn t trong mu
phn tch cn c th nh lng c nguyn t cho kt qu tin cy, chc chn v chnh
xc (95%). Nu gi gii hn pht hin l C h v gii hn xc nh l C th chng ta lun c:
Cd > Ch
(6.10)
Khng nhng ch gii hn di, m gii hn trn (cn trn ca mi nguyn t trong mt
php o cng khc nhau. Trong mt nguyn t, nhng vch ph no cng nhy thnng gii
hn trn l nh.Nhng vch khng nhy
th nng gii hn
trn l tng i ln (bng 6.4).

Cn trn ca mt phng php phn tch quang ph cng c xc nh bng thc
nghim. l gi tr nng C max m t nhng nng C x ln hn, th mi quan h gia
cng pht x Ix v nng C ca nguyn t trong mu phn tch khng tuyn tnh na.
Ngha l ng chun biu th mi quan h bt u gc xung trc honh k t gi tr nng
Cmax.
Gii hn xc nh, khong xc nh ca mt phng php phn tch khng nhng ph
thuc vo chnh tng nguyn t, vo tng vch ph c chn o nh lng, m cn ph
thuc vo mt s yu t khc, nh:
107
pht x ca nguyn t, Ion, phn t ca cc cht mu. Trong cc qu trnh ti in cc

+ iu kin ha hi, nguyn t ha v kch thch ph ca mu phn tch. +
v plasma th s bay hi, nguyn t ha ca mu v s kch thch m hi l qu
b
ghi ph
ca mu.
trnhTrang
chnh.thit
Song
ithu
vivmi
nguyn
t v i vi mi loi mu phn tch th cc qu
trnh ny rt khc nhau. Ngha l c nguyn t d ha hi, c nguyn t kh ha hi,
+ K thut v phng php nh gi nh tnh v nh lng.
c nguyn t bay hi nhanh, c nguyn t bay hi chm. V th cn phi nghin cu
mi 6.4
quan h gia cng pht x ca mt vch ph ca mt nguyn t vi thi gian
Bng
bay hi ca n vo vng kch thch ph (plasma). ng cong biu din mi quan h
V d v gii hn xc nh v khong xc nh
ny c gi l ng cong bay hi cua nguyn t . Ni cch khc, ng biu din
s bin thin cng pht x ca mt vch ph ca mt nguyn t theo thi gian bay
hi ca mu c gi l ng
bay hin
hi. (%)
V d: Khi nghin cu s bay hi v
Giicong
hn pht
Nguyn t Vch
Khong xc nh (%) (Gii
pht x ca cc nguyn t trong nn
oxitnhy
t him ta thu c cc ng biu din nh
trong hnh 6.2.ph(nm)
l cc ng cong bay hi ca cc nguyn
Mn, Mg, Si, Ce...
hn trntvFe,
di)
Al 236,706
0,03
0,05 - 0,4
T nhng ng cong bay hi ny chng ta thy c nguyn t bay hi nhanh, c
nguyn t bay 237,208
hi chm. Cng chnh t cc0,1
ng cong bay hi ny0,15
chng
- 2,0ta d dng
chn c thi gian ghi ph ph hp cho qu trnh phn tch nh lng tng nguyn
0,001
309,271
0,003 - 0,15
t. Cng nh trong trng hp no v i vi nguyn t no th cn chn thi gian
5 nhng nguyn t no0,0003
0,05
khi phng v 396,
i 1vi
th phi0,0005ghi ph
ngay t lc bt u kch
0,1nguyn t Fe, Mn, Mg,...
thch ph. Nh
v d (hnh 6.2), i vi cc
ta - phi
Bi 240,088
0,15
0,9 ghi ph
ngay t u cho ti giy th 150 l , ngc li, vi Ce ta c th b 100 giy u tin

262,791
0,03
0,04 - 0,5
v ghi ph bt u t giy th 100 cho n giy th 250 l thch hp. Chnh nh chn
0,003 ta
0,005
c thi gian289,798
ghi ph ph hp nh th chng
lm- 0,2
cho ph thu c ca mu
phn tch phc tp v d quan st nh tnh cng nh nh lng. l ngha
0,001
Fe 238,204
0,002 - 0,25
thc tin ca vic nghin cu ng cong bay hi ca mi nguyn t trong cc i
259,940
0,00030,1c ng
tng khc nhau,
v trong thc t, khng 0,0002
nhng cc nguyn t khc
nhau
cong bay hi khc
nhau, m ngay mt nguyn
t, khi0,0004chng0,15
tn ti trong cc loi mu
259,957
0,0003
khc nhau, th cng c ng cong bay hi khc nhau. iu c ngha l dng ca
Si 230,302
0,3
0,4 - 2,0
cong bay hi ca cc nguyn
t ph thuc 250,690
vo thnh phn
0,001
nn ca mu phn tch, trng

251,612
thi lin kt vt l, ha hc ca
0,0003
mu, cu trc tinh th ca hp

Mg
278,142
280,270
cht mu, dng hp cht m
nguyn285,213
t tn ti trong
0,003 - 0,3
0,0005- 0,15
0,03
0,05 - 0,25 0,002 - 0,10
0,001
0,0005- 0,05
mu,... Nhn chung trong cc
0,0003
hpVcht
ha
hc,
kh
nng
th, mun nng cao nhy ca mt php phn tch, ngi ta c th chn nhng iu
bay hi ca chngkin
theothc
thnghim
t
no, ph hp nht i vi tng nguyn t cn xc nh.
MeX > Me(NO3)2 > MeO >
SMe
bay
hi v ng cong bay hi
x(PO4)y > MeSO 4 > MexSy
Hnh 6.2
ng cong bay hi ca cc nguyn t' Fe, Mn, Mg, Ce trong nn

t him
>
Mecxphn
v.v...tch quang ph, mu phn tch c a vo ngun sng kch thch ph v khi
Trong
Chnh v
vi
loingun
mu, nht
nghin
dngtiang
th
n i
cng
trmi
thnh
pht thit
sng,phi
tc l
nguncu,
phtxy
ra cc
ph
108
109
cong bay hi cho tng nguyn t v ch trn c s mi c th chn c thi gian

ghi ph ph hp.
6.1.7. Kh quyn kim tra
Mi trng kch thch ph c nh hng trc tip n thnh phn ph ca mu
Mi trng kch thch ph pht x phn tch. Nhiu trng hp chnh mi trng kch
thch ph lm cho ph ca mu phc tp thm v kh quan st; c khi khng th thc
hin c php nh tnh cng nh nh lng. V d: Khi kch thch ph trong mi
trng khng kh th ph ca mu lun c cc bng CN. l ph m ca nhm
phn t CN.
Ph ny che lp nhiu
vch phn tch ca nhiu
nguyn t v n th hin rt
r trong vng kh kin.
Nhng chnh trong vng ph
ny li c nhiu vch c
trng
nhy
ca
nhiu
nguyn t. V th ngi ta
thng khng kch thch ph
trong mi trng khng kh,
m
trong
mi
trng
kh
quyn kim tra c. l

mi trng kh tr, hay kh
tr c thm oxy.
Khi nim v kh quyn kim tra
Vi tn gi l kh quyn tr hay kh quyn kim tra, ngi ta hiu l mt mi trng
kch thch ph pht x ca mu phn tch c th iu khin v kim tra c Mi trng
ny khng cha nit (N2) nh khng kh bnh thng. N c th ch l mt kh tr thc s
nh: He, Ne, hay l hn hp ca mt kh tr vi oxy theo mt t l nht nh. V d nh hn
hp ca (Ar + O2) hay (He + O2) ... Mi trng cng c th l CO 2 hay hn hp ca(CO2 +
O2). Nhng trong
ttc cc loi th u vit nht
c s dng nhiu nht vn l hn hp ca argon v oxy, bi v nu ch dng kh tr lm mi

trng kch thch ph th mu kh bay hi v thi gian kch thch ph qu di. Nhng nu
thm vo kh tr mt lng oxy ph hp th li to iu kin thun li cho mu bay hi v qu
trnh kch thch ph d dng hn. Thnh phn kh ca mi trng ny cn phi c khng
ch v kim tra theo mt nhim v phn tch. Chnh v th m xut hin khi nim S kch
thch ph trong mi trng kh quyn kim tra. Mun kch thch ph trong mi trng kh quyn
tr, ngi ta phi thc hin trong mt bung kn. Kh tr v oxy dn vo theo mt thnh phn
nht nh, ph hp v phi gi
110
khng i sut trong qu trnh kch thch ph. Hn hp kh cn c trn u trc khi dn
vo bung kch thch ph. C nh th mi m bo cho qu trnh kch thch ph n nh.
Vai tr v tc dng ca kh quyn kim tra
Trong phn tch quang ph pht x nguyn t, a mu vo vng phng in v kch
thch ph, ngi ta phi dng in cc than hay graphit tinh khit, v nguyn liu ny tha
mn c nhng yu cu ca nguyn liu lm in cc. Nhng khi dng nguyn liu ny lm
in cc kch thch ph trong mi trng khng kh, tt nhin s c nhiu ph m trong
ph ca mu phn tch. Trong ch yu l ph m ca nhm phn t CN, MeO. Ph m
ny che lp nhiu vch phn tch ca nhiu nguyn t lm kh khn cho cng vic quan st
nh tnh v nh lng; c khi khng th no thc hin c. V th nht thit phi loi tr
ph m CN. loi tr hay hn ch s xut hin ca ph m ca cc phn t v nhm phn
t CN, MeO,.. ngi ta nghin cu v nu ra nhiu bin php khc nhau. Song chng ta c
th khi qut theo ba hng sau y:
Cch l: Khng dng in cc than hay graphit a mu vo phng in v kch thch
ph, v mu phn tch khng trn vi bt than quang ph, m dng in cc kim loi. Nhng
in cc kim loi thng kh ch to thnh dng ph hp cho qu trnh kch thch ph. Mt
khc kim loi thng nng chy nhit cao. Nn khng th dng h quang kch thch
ph. M h quang li l ngun kch thch tt cho phn tch mu bt. ng thi khi phn tch
cc mu qung, oxit, t ,... nu khng trn thm bt than quang ph vo mu phn tch lm
cht m th vic ha hi nguyn t ha mu rt kh khn v khng n nh, nhit ca
plasma li thp. Cho nn in cc kim loi vn khng c th thay th cho in cc than c,
m ch c th dng c trong mt vi trng hp phn tch dung dch. V th bin php ny
khng thch hp cho tt c v t c s dng.
Cch 2: Theo cch ny, ngi ta vn dng in cc than, nhng thm vo mu phn tch
nhng cht ph gia thch hp hn ch s xut hin ca ph m v ph bng (CN, MeO),
v d thm mui halogen ca kim loi kim CsCL, CsF, LiF,... Nhng bin php ny cng
khng trit , v n ch hn ch bt, ch khng loi tr hon ton ph m ca CN, MeO.
Mt khc, mun loi tr c mt phn ph m, chng ta phi thm mt lng ln cht ph
gia. Nh th trong nhiu trng hp li lm gim cng vch ph. iu ny khng ph
hp vi yu cu ca php phn tch lng vt, ngha l trong nhiu trng hp khng dng
c bin php ny.
Cch 3: Cch th ba l kch thch ph trong mi trng kh quyn kim tra khng c
nit. Nh th s c kh nng loi tr c hon ton ph m ca nhm phn t CN m vn
dng c in cc than v bt than quang ph lm cht m. y l phng php tt nht.
N chng nhng loi tr c cc bng CN m cn c nhiu tc dng tch cc khc. Ngy nay
phng php ny c s dng rt ph bin v
111
6.1.8 Cht
mgvphi
chtnghi
ph gia
phn
ph
x n. S d nh vy l v vic kch
khng
c iu
ngtrong
na v
tctch
dng
cpht
li ca
Trong
phn
quang
phttr
x,ny
mu
nghim
d nh
dng
thch ph
trong
mitch
trng
khph
quyn
c th
nhng
u vit
sau:rn, dung dch hay bt
cng Ph
u c
lm phn
bay hi
mti
ngun
nhcngn
quang
in,
tia
ca mu
tchtrong
l tuyt
sch,sng,
khng
ph la
mn
cakh,
cch
phn
t v
nhm
in, t
ICP,...
l mu
phn
tch vch
cca
chuyn
thnh
trng
tc dng
ca nng
phn
CN, ngha
m thun
khit
l ph
nguyn
t v
Ion.thi
Dohi
di
vic quan
st nh
tnh
lng
kh
cc khn,
nguyn
Ion,lv
c phn
trng
thi hi
c th
v
nhnhit.
lngTrong
khng
ct,bit
trong
vngtph
kh kin.
V cng
d: Khi
xcc
nh kch
Gdthch npht
sng ton
v cng
ca
phNhng
pht xnu
do kch
cc nguyn
t
pht
ra trng
c dng
4184,26
th hon
b bng
CN vch
che lp.
thch ph
trong
mi
kh
xckim
nh tra
nng
ca ca Gd l mt vch nhy,
quyn
cahn hp Al (80%) v oxy (20%) th vch ph
r nt v rt thch hp cho phn tch Gd trong nn t him. n
trong
u im th hai l khi kch thch ph trong mi trng kh quyn kim tra, trong nhiu
mu
phn
trng hp cng ca vch ph c tng ln r rng. y chnh l mt bin php tng
tch, v
nhy ca phng php phn tch. Vic xc nh Sm, Eu l mt v d v ngha ny (bng
cng vch pht x ca mt nguyn t ph thuc
vo
6.5).
nng
ca
Bng 6.5
trong
So snh kt qu trong hai mi trng kch thch ph

phn tch.
mu
Nhng trong nhiu trng hp cng vch ph ca mt nguyn t trong mu phn

Nguyn t
Mi trng khng kh
Mi trng kh quyn kim tra
tch khng nhng ch ph thuc vo nng ca n, m cn b nh hng bi nng ca
cc hp phn khc c trong mu
phn
l khi trong h
c cha
nguyn
Cng
tch. Nht
nhy
Cng
nhiu
nhy t v
thnh phn phc tp m nguyn t cn xc nh li l nguyn t vt. l yu t nh hng
120 vo mu 0
Eucc
4435,60
0,0004%
,0001
%mt
tng h gia
hp phn trong67mu phn tch.
c bit l khi thm
phn
tch
s hp cht Sm
ph4424,34
no th ngi65
ta c th lm 0,0008%
thay i cng vch
nguyn t.
104 ph ca cc
0,0003%
Cc cht thm vo c gi l cht ph gia. Nhng cht khi thm vo mu lm thay
i thnh
phn thch
ca mu,
quami
lm
nhkh
hng
phnthng
ca ph
ca
Khi kch
ph v
trong
trng
tr n
ph thnh
ca mu
c v
nncng
sng,
nhiu
vch yu
ph.li
Cc
chtmt,
phkhng
gia cxut
th lm
hayph
cng
th lm
vch
bin
hin.gim
Do
thucc
catng
mucng
thngtvch
vchph
hnca
so
mttrng
nguynhp
t. kch
S dthch
nh trong
vy lkhng
v s thay
vi
kh. i thnh phn ha hc ca mu thng nh hng
n mi
qunhiu
trnh trong
kch
thch
nh:
Trong
trngkhi
hp
vic
kchph,
thch
ph ca mu phn tch trong mi trng kh tr
li toS
ra thay
s bay
chn
thun li i vi nguyn t phn tch. iu ny rt c ngha
ihi
nhit
lc
plasma,
khi phn tch nhng mu c thnh phn phc tp, cng nh thch hp.
Thay i nng in t (Pe) trong plasma,
Mt u im na l vic kch thch ph trong mi trng kh quyn kim tra trong nhiu
S khuch tn v chuyn vn ca cc phn t,
trng hp cn c kh nng loi tr c nh hng ca nguyn t c s ca mu (matrix
phn
ng
hanhng
hc kt
in
cc
v plasma,
effect).Cc
ng
thi
theo
qu
nghin
cu ca V. F. Fassel th vic kch thch ph trong
mi trng
kh quyn
cn
c mu,
tc dng hn ch c c hin tng t o ca nhiu vch
Qu trnh
ha hitrca
cht
ph nhy. V th vng tuyn tnh rng hn. Tt nhin bn cnh nhng u im th vic kch
S bay hi v nguyn t ha cht mu,
thch ph trong mi trng kh kim tra cng c nhng kh khn nht nh, nh cn c kh
Thi
tncao
ti (>99,99%),
ca cc phn
t c
trong
plasma,
tr, oxy
tinhgian
khit
cn
nhng
trang b ph tr. V th, ngy nay trong php
do phS
pht
hin
ICP-AES,
ph
pht x ca mu lun c kch thch trong mi trng
Ionxha,
si
phn
li ca cc
cht,
kh tr argon.
S kch thch ph ca cc phn t trong plasma.
Trong tt c cc thay i th s thay i p lc in t (Pe) v nhit ca plasma l
112
113
Nhm 1: Cc mui halogen ca kim loi kim v kim th: Lia, LiF, NaCl, NaF, CsF,
CsCL, AgCl, CaF2, CaCL2, MgCl2,... v mt vi kim loi nng Ti, Sb, Sn, Ga,...
Nhm 2: Mt s oxit kim loi, nh oxit ca Ga, Sb, Sn, Ti, Mg, Al, Fe,...
Nhm 3: Mt s mui cacbonat, borat ca kim loi kim v kim th, nh Na 2CO3,
Li2CO3, LiBO2, BaCO3,...
Nhm 4: Mt s halogen ca hp cht hu c, nh CF4,.
Nhm 5: Cc n cht v hp cht ca lu hunh: S. CaSO 4, SrSO4,.
Nhm 6: Cc hp cht ca Si: SiO2, Na2Sio3,...
Cc cht ph gia ny c th lm tng hoc lm gim cng ca vch ph ca mt
nguyn t. Song mt cht ph gia c th c mt hay nhiu chc nng khc nhau khi chng
c thm vo mu phn tch. N c th l cht m, cht mang mu, cht chy, cht pha
long, cht tr lc cho s ha hi v bay hi ca mu,... ngha l ty tng trng hp c th
m nhng vai tr no l ch yu.
Cht m. L nhng cht khi thm vo mu c tc dng n nh mt iu kin nay mt
qu trnh no trong s kch thch ph. V d m cho nhit plasma, m cho p lc in
t trong plasma. in hnh cho loi cht m l bt than quang ph. Bt than quang ph
khng nhng c tc dng m nhit cho plasma, m cn lm cho s bay hi ca mu c
d dng v n nh. Mt khc n cn gi cho plasma c nhit cao thch hp i vi s kch
thch ph ca nhiu nguyn t. V th n rt cn v quan trng i vi php phn tch cc mu
bt v mu khng dn in. V d: Khi phn tch cc mu qung, t , oxit,... ngi ta
thng nghin chng thnh bt v sau trn vi bt than quang ph theo mt t l thch hp.
Ngoi bt than, mt s mui halogen ca cc kim loi kim cng l cc cht m quang ph,
nh CsCl, CsF, LiF, LiCl,... Nhng cht ny c tc dng m cho p lc in t (P) trong
plasma t thay i trong qu trnh kch thch ph. Tt nhin ngoi tc dng m, cc halogen
ca cc kim loi kim v kim th cn c tc dng duy tr v n nh dng in qua ct kh
ca plasma.
Cht mang. Trong nhiu trng hp khi thm cht ph gia vo mu th s ha hi v
nguyn t ha ca cc hp phn trong mu li d dng hn, nhanh hn, hoc n nh hn.
Nhng cht ph gia c tc dng nh th c gi l nhng cht mang. N thng l nhng
cht d ha kh, d bay hi. V th khi vo trong mu, n bay hi c th ko theo c cc hp
phn mu bay hi, hoc tc dng vi cc hp phn ca mu to thnh nhng hp cht mi d
ha hi. Chnh v th m mu bay hi tt hn. Tiu biu cho cc loi cht ny l cc mui
halogen v cacbonat ca cc kim loi kim v mt vi kim loi kim th nh CsF, CsCl, LiF,
LiCl, NaF, NaCl, Li2Coa, Na2CO 3, CaCO3, SrCO3, BaCO3. ng thi c bt than quang ph
cng c tc dng ny rt r rt khi phn tch cc mu khng dn in. Ngoi ra, mt s oxit d
bay hi ca mt s nguyn t nh Ga, Sb, cng l nhng cht mang. Cc cht mang ny trong
nhiu trng hp cn c tc dng lm tng cng vch ph.
114
Cht tr lc cho s t chy, ha hi mu. Thng thng khi phn tch cc

mu bt, c bit l cc mu khng dn in, nh cc mu qung, t , khong st, thng
c
hin tng kh t chy mu, kh ha hi v t bay
hi thng khng n
nh. Khi cng vic phn tch gp kh khn v kt qu thu c khng lp li tt Lc ny

ngi ta thng thm vo mu nhng cht lm cho s chy, s ha hi v nguyn t ha ca
mu c d dng hn. Nhng cht nh th c gi l cht tr lc cho s bay hi ca mu.
Cht in hnh cho loi ny li l bt than quang ph hay bt graphit quang ph. Sau l bt
lu hunh, bt oxit nhm. Nhng bt lu hunh v bt xit nhm khng th dng ring mt
mnh, m phi lun lun dng cng vi bt than. V th ngi ta gi bt than quang ph l
mt cht ph gia vn nng.
Cht dn in. Khi phn tch cc mu khng dn in, vn n nh dng
in qua ct kh ca plasma h quang hay tia la in l mt yu t rt quan trng. V nu
khng, s phng in khng n nh v iu ny s a n nhng kt qu phn tch khng
tt. Nguyn nhn chnh l do trong nhng trng hp trong plasma khng c nng
ln v n nh ca cc phn t mang in tch dng v nm ( Ion dng v in t). V th
ngi ta thng thm vo mu phn tch nhng hp cht d bay hi ca cc kim loi d b Ion
ha (c th Ion ha thp). Nhng cht c gi l nhng cht dn in. i din cho nhm
cht ny l cc mui halogen ca cc kim loi kim nh CsF, CsCl, LiF,... Nh c nhng cht
ny dng in qua ct kh c n nh, v qua cnglm chos phngin,
kch thch
ph trong plasmacng
c n nh. S d nh vy l v nhng cht ny cung cp cho plasma mt nng ln

ca Ion dng v in t, m yu t khc (s b sung khc) v in tch nm v dng l
khng ng k, ngha l duy tr dng in n nh qua ct kh ca plasma.
Cht pha long. L nhng cht khi thm vo mu phn tch c tc dng lm long nng
ca cc hp phn trong mu, nhng li khng nh hng n cng vch ph ca
nguyn t phn tch, ngc li c khi cn lm tng cng vch ph phn tch. Thc t
chng minh rng, trong hu ht cc trng hp phn tch cc mu qung, khi pha long mu
bng bt than quang ph, mui halogen kim loi kim, th cng vch ph ca cc nguyn
t cn xc nh ch c tng hoc khng i. Ngoi bt than quang ph th mt s mui
cacbonat, halogen ca kim loi kim v kim th, mt s mui sunfat kim loi kim th, mt
vi oxit, v d nh Li 2COa, Na2CO3, LiF, LiCl, BaCO3, CaCO3, CaSO4, SrSO4, SiO2,... cng
thng c dng cng vi bt than quang ph theo nhng t l thch hp. Tc dng ca cht
pha long l lm cho ph ca mu n gin hn v d quan st. Trong mt s trng hp cht
ny c tc dng kh bt ph ca nguyn t c s, lm tng cng vch ph ca nguyn t
phn tch (bng 6).
Cht chy. L nhng cht d nng chy, c tc dng lm cho mu d nng chy v d
ha hi. V d nh LiBO2, cc mui hydropyrosunphat ca kim loi K v Na hay Li. i vi
mt s mu c thnh phn phc tp, nh cc mu qung a kim
115
loi
kimvthng
cha nhng
gy ra nguyn
s bay hi
t chn
dnglc
hpca
cht
nhng
bn nhit,
nguyn
khtbay
vt hi
trong
ngi
mutacphi
khthm
nng vo
to
mu
vi cc
phn
halogen
tch cc
nhng
chthp
chy
cht
theo
d nhng
bay hi.
t Trong
l ph nhng
hp vi
trng
mc hp
chny
h thp
thng
nhit
ko
theo
nng
s
chy
tng cng
ca mu
v
calm
vch
muph.
d bay
l
hi.
iu
Ngoi
kintc
thun
dngliy,trong
nhng
php
chtphn
chytch
c nguyn
nhiu trng
t vi
hp
lng.
cn
lm
cng
tng
l cng
u im
ca
vch
cht
ph
ph
ca
gia.
nguyn t cn nghin cu. V d nh LiBO2 trong
bng 6Hng
. 6.
II. Ngi ta s dng cht ph gia nhm mc ch lm thay i cc qu trnh
chnh
trong s phng in v kch thch ph ca mu. V d: S ha hi, s kch thch ph ca
Bng 6.6
mt
hpca
phn
plasmamu
vi mc ch c th lm tng hay gim mnh cng vch ph
Vai tr
chttrong
pha long
ca mt nguyn t. Nhng kt qu nghin cu n nay chng minh rng, nhng yu t gy
ra cc thay i trn phi l cc phn ng ha hc trong in cc v trong s bay hi ca mu
STT
Mu + cht pha long t l: (gng)
Cng vch ph
khi c mt ca cht ph gia.
Mu
Bt than
nm th c
Trong cc cht ph gia
th cc halogen
ca kim loiLiBO2
kim v mt sFe-248,30
kim loi kim
1 vi mc ch1ny, bi v s 0
0 ln v ph 0,140
ngha ln i
c mt mt lng
hp ca cht ph
gia nh th trong
cc v trong s
2 mu phn tch
1 lm thay1i tt c cc qu
1 trnh trong in
0,230
kch thch ph3 ca mu.
0 280
Trong
nh cc yu t
4 nhit v p1lc in t trong
3 plasma l cc1yu t chnh, quyt
0,260
khc. Nhng thay i cui cng dn n s thay i cng ca vch ph.
Cht kh nn. Trong mt s trng hp phn tch quang ph pht x, nh cc mu
Tc dng ny c th l dng v cng c th l nm, ty thuc vo tng trng hp c
qung, th ph thu c thng c nn ph lin tc rt en, nht l khi kch thch ph bng h
th. Tt nhin trong thc t phn tch ngi ta lun lun chn tc dng no c li cho cng
quang. C khi nn ny che lp mt c nhng vch phn tch c cng nh. Trong nhng
vic phn tch, nh lm tng cng vch ph ca nguyn t phn tch v lm gim cng
trng hp nh vy ngi ta phi thm vo mu nhng cht c tc dng lm gim bt nn ca
vch ph ca nguyn t nn.
ph lin tc. Nhng cht c tc dng nh th c gi l cht kh nn. Cht thuc loi ny
V mt ha hc, khi thm cht ph gia vo mu phn tch tt nhin c nhiu phn ng
thng l mt s mui sunphat ca kim loi kim th v mt vi oxit: CaSO 4, BaSO4, SrSO4,
ha hc khc nhau xy ra, c phn ng chnh, c phn ng ph. Nhng c th tm chia thnh
SiO2, Al2O3. Nhng cht ny c th dng ring bit hay ng hn hp ca hai cht vi nhau,
my loi phn ng sau:
nhng chng cng phi c ng cng vi bt than quang ph. V d: Khi xc nh V v Ni
ngngi
oxy ha;
trong Phn
du m,
ta thng dng SiO 2 hay SrSO4 thm vo mu khi tro ha mu du.
NhngPhn
chtng
nysunfua
va cha;
tc dng l cht gp, cht bo v hay l n nh qu trnh tro ha trnh
mt mt, mt khc li chnh l cht kh bt nn khi ghi ph ca mu tro du .
Phn ng cacbua ha;
Trn y l mt s tc dng quan trng ca cht ph gia, nhng s trnh by v phn
Phn
loi nh thng
ch halogen
l tngha;
i, v trong thc t mt cht ph gia c th biu l ng thi nhiu
chc nng
dng
cng
mthy
lc.
Trong
ct,...
chc nng chnh, c chc nng ph. V d
Phn v
ngtc
phn
li v
phn
ca
cc phn
nh bt
thancc
quang
cht
cht mang.
tc dng
ca
n l
Trong
loi ph
phnva
ngl
th m,
phn va
ng l
halogen
ha lNhng
quan trng
nhtm
v c
ngha
chnh.t V
th v
ngi
thng
phmu
l cht
mhi,
quang
thc
nht,
nh ta
phn
ng gi
nybt
ccthan
hp quang
phn ca
d ha
cph.
bit l cc hp phn
phgialm
ctng
nhiu
tc dng
khc
nhau,
nn khi tsphn
dngtch
n v
ngi
thng
lng Cht
vt, qua
cng
vch
ph
ca nguyn
lm ta
gim
cngxut
pht t
nhng
mc ch
khc
Nhng c th khi qut theo hai hng chnh:
vch
ph
ca nguyn
t c
s nhau.
v nn.
Hng
I. gia
S dng
nhm
mc
ch gy
s loi
bay kim
hi chn
lc s
cakim
mtloi
s
Cht
ph
to racht
phnph
nggia
ny
l cc
halogen
carakim
v mt
hp phn
kim
th. trong mu m bo cho php phn tch thc hin d dng v t kt qu tt. V
d: Vic
thmlicc
ph
giahalogen
l cc mui
cc kim
Ngc
vicht
phn
ng
ha, halogen
phn ngca
sunfua
ha loi
v carbua ha thng
116
117
to ra cc hp cht bn nhit, kh bay hi, kh nguyn t ha, ngha l gim qu trnh bay hi
v nguyn t ha ca cc hp phn v cui cng lm gim cng vch ph.
V th phn ng ny c s dng kh bt ph ca nguyn t c s.
Xut pht t nhng nghin cu nu, ngy nay trong phn tch quang ph pht x
ngi ta thng s dng cht ph gia khc nhau thm vo mu phn tch vi nhng mc ch
sau:
To iu kin lm cho qu trnh ho hi, nguyn t ha mu, kch thch ph n nh,
m bo cho php phn tch t chnh xc v lp li cao, ngha l thu c kt qu tt.
Tng cng vch ph ca nguyn t nghin cu, ngha l tng nhy ca phng
php phn tch c th xc nh c nhng nng nh m khng phi lm giu mu
phn tch (bng 6.7 v hnh 6.4).
Loi tr bt nhng nh hng ca cc hp phn cn tr, nh ph nn lin tc, nh
hng ca nguyn t c s, nguyn t th ba.
0
c ((ig/mL)
Pha long mu phn tch loi b nh hng ca hin tng t o, hoc lm n gin
Hinh 6.4
ph ca mu phn tch
d quan st nh tnh v nh lng.
nh hng ca cht ph gia n cng vch ph ca Eu
4435,60
iu chnh s bay hi ca mt s hp phn trong mu theo nhng xu hng c li cho

qu trnh phn tch mt hay vi nguyn t.
Phn tch quang ph pht x bn nh lng
Bng 6.7
Phng php phn tch quang ph bn nh lng l php phn tch nh gi gn ng
nh hng ca cht ph gia n cng vch ph
hm lng (nng ) ca mt nguyn t trong mu phn tch da theo s quan st v so snh
en S hay cng IM ca vch ph phn tch.
Php phn tch quang ph bn nh lng c nhiu phng php khc nhau. Song trong
cun sch ny ch nu hai phng php chnh cn ang c s dng nhiu.
Phng php so snh
Nguyn t
Cng vch ph trong iu kin
Nguyn tc ca phng php ny l mun phn tch bn nh lng mt nguyn t X
Khng ph gia
C cht ph gia thm vo:
no , trc ht phi chun b mt dy mu u ca n c nng t nh n ln.
CsCl
(2%) t phn tch X
LiF
V d: Dy mu u (mu chun) c nng ca
nguyn
l (2%)
Cl,
C2, Ca, C4, C5, C8.
4424,34 Sm
115
138
134
ng thi cng chun b mu phn tch C x trong cng iu kin. Sau tin hnh ghi
4435,60 Eu
120
148
145
ph ca tt c dy mu cng mu phn tch trong mt iu kin ph hp c chn cho
4262,10
Gd
90
105
110
nguyn t
X.
Nhng vic quan st v nh gi d dng chng ta nn b tr ph theo th t:
Cl, Cx, C2, Cx, C3, Cx, C4, Cx, C5,...
Trn y l khi qut chung
v tc dng ca cc loi cht ph gia khc nhau.
thu c
knh
nh taph
chn
tch
nguyn
t mu
X vqung
so snh
Song Sau
thc khi
t phn
tch rt
l phong
vmt
phcvch
tp, phn
nht l
khica
phn
tch cc
c
cng
ca
chng
tt vn
c cc

xemnghin
nng
khong
x nm
thnh phn
phc
tp,trn
nhiu
nng
cn phi
c
cuCv
bntrong
bc thm
theo nhng kt
qu nghin cu tip tc hin nay v sau ny na, c bit l qu trnh kch thch ph pht x
trong ngun nng lng mi ICP ca php o ICP-AES.
118
119
Bng 6.8
no
mu
ca ca
vchcc
ph,
cnu.
phng trnh (b) l trng hp o en S ca vch ph trn knh nh.
Ri t cc cp gi tr (As/log C)
V d Nu
v xc
nh
Pb
phng
php
hin
vch
Nh
vy,
mun
xc nh
nng
C vch
t Xtatrong
S, theo
hay
cng
ca
ph nguyn
phn tch,
quanmt
st mu
nm no
gia,
trc
en
x ca mt
hay (VC)
ta en
dng
ng
chun
theo
ca
vch
nng
vdy
Cghi
th
ta ni
nngnguyn
Cx t
lnX hn
C2 nhng
hn
2 ph
3mu
ht ta
chng
taS phi
chun
bCmt
u
c cha
vi nng
Ci, li
C 2, nh
Ca, C
4,..
h

- log
C
(nu
trn
Nna
Ph (%)
S vch xut hin tna n 2 (Ao)
C
3, ngha
l
th vit:
knh
ta
cccmy
quang ph thcc
h
.V
Cnh
phn ;tch.
Song dng 1 ng chun, trong
x trong
Cicng
0,001mt iu kin nh
2614,20 mu
; 2802,00
2933,06
C2 < C x < C3
1thc
v nghim,
2) hay Ix
- C. cn
ng
nyu.
chnh l
t nht
ba mu
C
Ba
vch
trn r, c thm vch 2663,17 (m)
2 0,005
cc ng
chun
lysnh.
l ni
dung(hay
ca ng
phngcong
php so
V th phng php ny gi l phng php ba mu u, tc l s mu u cn thit
mu) Phng
Cxc
nh ny
nng
CBn
cha
x d
php
ngin,
thctrn
hin.
Nhng
mi 2873,30
khi phn tch mt mu li
3 0,01
vch
r, c
thm vch
dng
mt
ng
chun.
Nhng
trong
thc t, ngi ta hay dng 5 mu u, cng v th
bit
ca
nguyn
t
phn
tch
X.
Mun
phi ghi ph ca mt dy mu u, nh th cng tn nhiu mu chun, in cc v
C4 cm
0,05c
Nm
vch
r nt.
phng
ny
gitrmt
chung
l trn
phng
php ng
chun.
th
tath
chphp
cn
cc php
gi
AStn
hay
x thng
mt
gi.
Phng
ny
c
ng dng
phn tch
cc mu dung dch. V
c
t
ln
trcbtrong
tung
v
u
knc
d,xc
nh
loi
khong,
trnhin
(hnh
6.5).
Ckim
5chun
0,1
Nm
vch
nt v
thm
vch
Sau
khi
xongnc
cc t
mu
vtrn
mu
phn
tch,
tin
hnh2474,38
ha hi, nguyn t ha,
ng
song
song
vi
trc
honh,
n
Phng
php
hin
kch thch
ph,
v vch
ghi ph ca ccSu
mu
trn
theor,
nhng
kin (cn
ph hp
C6 0,5
vch
thmiu
2393,61
m) c chn (theo
ct ng chun
ti im A, t im
Nguyn
tc ca
phng php ny da trn c s s vch ph ca mt nguyn t
mt quy
trnh phn
tch).
A ny hC7ng
vung
gc vi
trc u to, nhe, thm 2401,95; 2443,86
1,0nhiu khi nng
Ba
xut hin cng
vch
ca nguyn
t trong mu cng ln, ngha l ng
Tip
chn
mt
cp
vch
phn
tch o en S hay chn vch phn tch o
honh, th ta c c Cx (nu o I)
vi mi mtC8nng
nht nhBath
c u
mtnhe,
s vch
ph sau
xutm.
hin trong iu kin th
1,5 o
vch
cc vch
hay
l
logC
S) ri
suy ra
C
x (nu
x
cng
I
theo
mt
trong
hai
phng
trnh
c
bn
trn
ty
thuc
vo
ca
nghim c chn ph hp i vi mt nguyn t trong mt h
ithng
tngtrang
mub nht
cn tm (hnh 6.6).
phng th nghim. Tnh cc gi tr trung bnh ca cng vch ph I, hay en S tng
nh.
T ng chun trn, ngoi vic
V tng
d: nng
nng
ca Pb mu, v nu kch thch ph trong iu kin h
ng vi
.
Nh0,001%
th ta c:
hin: 2614,20; 2802,00; 2933,06;2633,17.
xc nh Cx
Cx chng ta cng c Xut
th xc
quang dng 10A th ch c ba vch ca Pb: 2614,20; 2802,00; 2833,06 A o xut hin.
nh c h s a trong phng trnh
V
vy
mun
phn
tch
mt
v h s k cng nh y; h s b
Phng
php
ny
n
gin,
d
thc
hin
v c ng dng rt rng ri, c bit l trong
nguyn
,catrc
Bng 6.9.tDyno
chun
phnght
phpngi
ng ta
chun
trong phng trnh (b). C th l:
Mu
Nng
cng
phicht,
chun
b cn
mtlpdy
uvch ph xut hin
ngnh a
v ta ch
bngmu
ph cc
u tin, sau c th
Ci ln0,0005%
Cht
Dy
chun
Theo
hnh
6.6a ta
cha
nguyn
tc:
X phn
tch
vi nguyn
nng
, trong
v cc ln sau, m khng phi ghi ph li ca
s dng
bng ny
c*
C(6.11)
C2, Ca, C4, C5, C6, C7,...V
1
ad:
= tga
c2 th phng
0,001% php hin vch
mu
u.
Trong
hai phng php bn nhHnh
lng
trnh by,
6.6
2 c*
3
4
5
Cctheo
mu
tch Cx 1, Cx2, 0trong 1
V
hnh phn
6.6b ta c:
c s dng rng ri, nht l trong nghnhng
a cht,
phng
php
d thc hin v c
chunv
phn
tch nh
lng
cng
kin.
Sau ghi phCoca Ci
Y.biu
= tga tch
v
kXl on
Cht
phn
C2c3
C0,005%
3
C4
C5
(a)- Tho quan h I - C;c*(b)- Theo quan h AS - logC
nhiu
u
im.
cc mu trong
iu
kin chn.
OD
(6.12)
C4
0,01%
Cc st
cht ph
khc (nn,
mi trng)
tt c
cc mu
Quan
thupht
c
ca lng
tt c cc Nh nhau trong
Phn tch
quang ph
x dinh
c*
Phng php ny rt thun li khi phn tch hng lot mu ca cng mt i tng, v
nng xem mi nng c bao
c5
0,05%
I
I
ch
Phng
cnlxmt
phpng
ngchun
chunl c th xc nh
c rtIinhiu mu
c nng
o
Io
2
3 Cx cha
I4 bit.I5
c*
nhiu vch ph ca nguyn t phn
c6 ca php
0,1% o ph pht x nh
Phng
phpphn
ng
dabng
theo
phng
trnh c bn
tch Nhng
xut hin
v
lpchun
hin
mu
tch
vmt
mu
u
phi
cng
mtS3
iu kinS4v trnScng
o Sx
So ghi ph
Si[ trong S2
5
c,
vch
ca
ng
nng
ch
ra chng
trong
chng
IItng
l:
mt
knh
nh. V
thvi
nu
phn
tch.
nhiu i tng 1
m mi i
ch mt hoc hai mu
c7 tng
0,2%
...........
Bng
phn
th tnny
muc
u,dng
knh
nh,
thitch
gian,...
chnhl im
cha u vit ca
I = a.Cb (a)
X (Cu 3247,54 )
nguyn
t
sau
ny.
Bng
6.8
l
mt
(Vchthphan
tch) i.Song trong nhng
phng php ny. V th xut hin phng
php
khng
hay
S
=
y.
b.log
C
+
k
(b)
v dkin
v xc
nh
Pbth
trong
qungvn
theo
iu
nht
nh
n cng
l mt phng php c ng dng ph bin v c nhiu
Hnh 6.5
phng
phpiu
ny.kin b: 1, th y l phng trnh ca ng thng c dng: y= a.x v y: a.x
Trong
u
vit.
Xc nh Cu trong nc khong
+ b.
theo phng php so snh
Phng trnh (a) l i vi nhng my o c trc tip cng pht x IM
122
120
121
123
Phng php th chun khng i

Nguyn tc ca phng php ny l mun xc nh mt nguyn t no , trc ht
ngi ta cng phi dng mt ng chun nh trong phng php ba mu u.
ng chun ny c gi l ng chun c nh (ng chun khng i). Nhng c
khc l ph ca cc mu u dng ng chun c ghi trn mt knh nh ring, gi l
knh nh c s; cn ph ca cc mu phn tch li c ghi trn mt knh nh khc, knh nh
th hai - knh nh phn tch. Nh vy, mun xc nh c nng C x cha bit, ta phi
chuyn cc gi tr S xl tng ng v cc gi tr S xo ca knh nh c s th mi chiu ln
th chun xc nh C x hay loa Cx c. gii quyt vn ny ngi ta c hai cch
khc nhau:
Cch th nht: Xc nh h s chuyn k theo cng thc:
S
xo k-Sxl
(6.13)
y k c gi l h s chuyn ca gi tr en ca vch ph gia hai knh nh

(knh nh c s v knh nh phn tch) trong cng mt iu kin th nghim.
Mun th trn knh nh phn tch ta ghi li ph ca mt mu u, v d nng Ca.
Nh th trn knh nh c s ta c Sxo-3, v trn knh nh phn tch ta cng c S xl-3 v
h s chuyn k s c tnh theo cng thc:
(6.14)
Sau khi c h s k ta em n nhn vi cc gi tr en Sxl trn knh nh phn tch ta
s thu c cc gi tr en tng ng trn knh nh c s dng ng chun. By gi
ch chiu cc gi tr vo ng chun c nh l tm c loa Cx> Ri t suy ra C x.
Cch th hai: T thc t phn tch
khi nghin cu cc ng chun ngi ta thy
I;
rng, trong cng mt iu kin th nghim, i

vi mt nguyn t khi o trn mt cp vch
phn tch, th ng chun dng c t dy
ph ca cc mu u ghi trn cc ln khc nhau
ca mt loi knh nh, u l nhng ng thng
song song vi nhau hoc trng nhau (hnh 6.7),
ngha l cc ng c cng h s gc.
c
Phng php th khng i rt ph hp
i vi php phn tch hng lot mu t ngy
ny qua ngy khc, v trong mi ngy
124
Hnh 6.7
Cc ng chun ca dy mu u theo mi
ngy o
phn Trong
tch chng
cc ta
gikhng
tr C1phi
, C2,ghi
C3ph
, C4lil nng dc thm vo ca nguyn t phn
h
ca X
ton
bdng
dy mt
muhp
u,cht
nnctit
kim
tch
di
dng
lin c
kt ph hp nh trong mu
(I) phn
tch v theo cp
thicng.
gian, in cc, mu chun v knh nh,
s
ngha Sau
l
c cng
tnh tin
kinhhnh
t ghi
hnph
phng
(n) ph hp, chn mt
ca dyphp
mu theo nhng iu Vkin
ng
Tuyenth,
nhng
php
cp vchchun.
o
S hay
gi trphng
cng
I c tng ng. Nh vy ng vi mi nng ta
ng chun (Ba mu u) hay phng
cng s c c nh trong bng trn.
php ng chun c nh u ging nhau
n y chng ta dng phng php ngoi suy xc nh nng C x cha bit trong
ch u phi chun b mt dy mu u c
mu phn tch. Theo phng php ny, xc nh C x chng ta phi dng ng chun theo
iu kin ca mu u trong php phn
h to Ix - C. Nh vy, nu cng vch ph Ix c o trc tip th cng vic s n
tch quang ph nh lng. iu ny nhiu
gin,
ta dngthc
ngayhin
cc.
ngc
chun
- Cvi
t nhng gi tr Ix o c. Nhng nu
c o
khi khng
bitIx i
theo
gi tr S
chng
ta tnh
nhngcctrng
hp thmu
phn
tchcchuyn
thnhcc gi tr S thnh gi tr Ix tng ng
Hnh 6.8
theo
phn cng
phcthc:
tp m chng ta cha th bit
ng chun c nh (I) v ng chun phn
c chnh xc.
tch (II)
.log.I = S
(6.15)
V th
th chun
b c
mt dy
u- c
thnh
phn ha
hcva
v vt
l
Ri
saucng
khng
cng dng
ng
chun
nhmu
trn Ix
C.
ng
chun
dng
ng l
nht
mu thng.
phn tch.
trc
l tung
thc ti
t v
trong
nhng
hp gi
th
nhxc
hng
c
mtvi
ng
N ct
im
c ta
(Itrng
mun
nh
x, Cx). By
nguyn
c s
nguyn
th ba
kt nng
qu phn
tchng
l rt r.
iuny
ny
khi
Cx ta chtvic
kovdi
ngtchun
n
pha
nh,
chun
sth
ct hin
trc r
honh
xc
nhim
cc nguyn
vi lng.
ny
chng
ta phi
hoc l
thay i nn ca mu (modify
ti mt
Cx.. t
chnh
l gi Lc
tr nng
C x cn
tm (hnh
6.9).
matrix)
cch
qu,
dngkhc,
phng
php
tiu
Tanu
cng
cny
th c
xchiu
nh
C x hay
theolcch
ngha
l thm
t gc
tochun.
chng ta k ng
Phng
php
thm
tiu
chun
song song vi ng chun v t gi tr I X chng ta k ng song song vi trc honh; hai
ngNguyn
ny ct tc
nhau
im B.
T thm
B k l
ng
gc mt
vi nguyn
trc honh,
n ct
honh
catiphng
php
munvung
xc nh
t phn
tchtrc
X no
ti
C
.
chnh
l
gi
tr
nng
C
cn
tm.
x
trongx mu phn tch, ngi ta dng ngay
mu phn tch lm nn chun b mt dy mu u
bng cch ly mt lng chnh xc mu phn tch v thm vo nhng lng ph hp v
theo tng bc ca nguyn t X. Nu gi mu phn tch c nng l C x th dy mu chun
s l (bng 6.10):
Bng 6.10
Dy chun ca phng php thm
Cht
Co
C1
C2
C3
C4
C5
Cht PT X
Cx
Cx
Cx
Cx
Cx
Cx
X thm vo
AC1
AC1
AC1
AC1
AC1
Cht khc
0 AC, AC2 AC3 AC4 c (ppm)
cx
Nh nhau tt c
Hnh 6.9
2
I3
I4
I5
D th chun ca phng php thm - Xc nh y: Nguyn tc da theo hai mu
Hay o Sx
So
S1
S2
S3
S4
S5
o c Ix
Io
I1
chun bit chnh xc nng v

126
125
d: C1,C2 (C2 > C1).

Nh vy ta c:
S2 = y.b log C2 + k (a)

S1 = y.b.log C1 + k (b)
Ly (a) tr (b) ta c:
(S2 - S1) = Y.b(log C2 - log C1)
(S2 -S1)
Do ta suy ra: Y - _r
"
'
log(C2 / C1)
v b = 1
Phng php theo 1 mu chun
Khi c mu chun
Trong nhng trng hp n gin, chng ta khng cn pha mt dy chun dng
th chun, m c th tnh ngay gi tr Cx nh mt mu chun Cl ca cht phn tch, ngha l
chng ta c:
Vi mu phn tch:
Ix = a.Cx
(a)
Vi mu u:
I1 = a.C1
(b)
Do em (a) chia cho (b) chng ta c:

Cx = (Ix/Io).C1
(6.17)
Nh vy khi o c gi tr I x v I1 ta c t s ca chng, v ch vic nhn n vi gi tr

Cl l chng ta c gi tr nng C x phi tm theo biu thc (6.17).
Nhng cn phi nh rng, nu o S trc ht phi tnh chuyn cc gi tr S sang cc
gi tr cng I tng ng ri mi ng dng c phng php ny, gi tr nng chun
Cl v c nng cht phn tch phi nm trong vng tuyn tnh ca php o xc nh cht
m chng ta bit r trc.
Khi khng c mu chun
Trong trng hp ny, chng ta cng khng cn pha mt dy chun dng th
chun, m dng ngay 1 mu phn tch lm nn chun b mt mu phn tch v 1 mu thm
chun theo phng php thm v tnh ngay gi tr Cx nh mt lng chun C 1 ca cht phn
tch c thm vo. Ngha l chng ta c:
Vi mu phn tch khng thm chun:
Ix = a.Cx
(a)
Vi mu u phn tch c thm chun:
Itch = a(Cx + C1)
(b)

Cng = [Ix/(Itch - Ix)]C1
(6.18)
127
Nh vy khi o c gi tr Ix v Itch ta c tnh c nng Cx phi tm theo biu thc

(6.18).
Nhng cn phi nh rng, nu o S trc ht phi tnh chuyn cc gi tr AS sang cc
gi tr cng I tng ng ri mi ng dng c phng php ny v gi tr nng
chun Cl v c nng cht phn tch phi nm trong vng tuyn tnh ca php o xc nh
cht chng ta bit.
Trn y l cc phng php nh lng ch yu hay c s dng. Tt nhin mi
phng
php u c nhng
u im v nhc im nht
nh ca n, v ngi
dng tu iu kin m p dng cho thch hp.

Cc phng php xc nh gin tip bng AES
Nguyn tc
xc nh gin tip cc cht khng c ph pht x nguyn t theo php o ph pht
x nguyn t, ngi ta thng da theo mt trong hai nguyn tc sau y v ng vi mi loi
nguyn tc ngi ta c mt kiu xc nh ring nht nh theo bn cht ca cht phn tch.
Cch 1: Cho cht cn phn tch X (cn xc nh) tc dng vi mt thuc th l mui ca
mt kim loi c ph pht x nguyn t trong nhng iu kin thch hp v phn ng ny c
tnh cht nh lng hon ton. V d: xc nh Ion Cl, ngi ta cho mu c Ion Cl tc
dng vi dung dch AgNO 3 trong mi trng axit HNO 3 2%, sinh ra kt ta AgCl theo
phn ng:
C- + Ag+ = AgCl T
Sau lc hay li tnm ly kt ta AgCl, ho tan n trong dung dch NH 4OH 5% v xc
nh hm ljng Ag trong dung dch ny, ri suy ra nng ln C -, v theo phn ng trn, 1 Ion
Cl s tng tc vi 1 Ion Ag+.
Cch 2: Da theo hiu ng ca cht cn xc nh trong mt vng nng nht nh, n
lm gim hay lm tng cng vch ph pht x ca mt kim loi mt cch tuyn tnh. V
d: xc nh Anion F1- ta o ph pht x ca nguyn t Mg nng
ppm, v trong vng nng Anion F 1- t 2 - 20 ppm, th cng vch ph pht x Mg 285,20 nm s b gim mt cch tuyn tnh theo s tng nng F.
Cc phng php phn tch gin tip
Theo nguyn tc th nht
Theo phn ng to kt ta khng tan
Theo loi phn ng ny, ngi ta c th thc hin cc phn ng ha hc c tnh cht
nh lng bit, nh:
To kt ta l mui khng tan
128
Cc phn ng kt ta nh lng trong ha hc th c rt nhiu, v d nh phn ng to

kt ta: AgCl, AgBr, AgI, PbSO 4, BaSO4, v.v...Theo cch ny, ngi ta ly mt lng nht
nh cht mu (theo Vml hay a mg) cho tc dng vi mt thuc th thch hp v d, trong
iu kin nht nh phn ng kt ta xy ra hon ton. Sau li tnm hay lc tch kt ta
khi dung dch, ri thc hin xc nh kim loi theo mt trong hai cch sau:
+ Ho tan kt ta v xc nh kim loi trong kt ta, ri suy ra hm lng cht phn tch
X.
+ Xc nh lng kim loi thuc th d sau khi kt ta ht cht phn tch cn li.
T suy ra lng kim loi phn ng vi cht phn tch X, v tnh hm lng cht
phn tch X.
Cch ny thng c s dng xc nh cc mui: Halgen (F, Cl, Br, I), sunphat
2-
(SO4 ), photphat (PO43-), oxalat (C2O42-), v.v... Sau y l cc phn ng .

C- + Ag+ ^ AgCl xc nh Anion Cl Br + Ag+ ^ AgBr xc nh Anion Br I- + Ag+ ^ AgI xc nh Anion r
C2O42- + Ca2+ ^ CaC2O4 xc nh Anion C 2O42PO4 + Ca2+ ^ Ca3(PO4)2 xc nh Anion PO 4
SO42- + Ba2+ ^ BaSO4 xc nh Anion SO42SO42- + Pb2+ ^ PbSO4 xc nh Anion SO42PO43- + Mg2+ + NH4+ ^ MgNH4PO4 xc nh Anion PO 4
V d: xc nh hm lng Anion Cl - trong nc, ngi ta ly 100 ml mu nc,
thm 5 ml HNO 3 65%, thm 2 ml dung dch AgNO 3 5 mg/mL Ag (lng Ag thm vo l 10
mg), lc u, sinh ra kt ta AgCl theo phn ng:
C- + Ag+ -^AgCl
Lm mui kt ta, sau lc hay li tnm ly kt ta AgCl, ra sch kt ta bng 10ml
HNO3 1%, thu nc lc v nc ra nh mc thnh 100 ml bng dung dch HNO 3 1%, v
xc nh lng Ag d trong dung dch ny bng php o ph pht x ca nguyn t Ag. Nh
th ta tnh c lng Ag, v suy ra lng Ag phn ng vi mun Cl, sau tnh hm
lng mun Cr trong mu nc, v theo phn ng trn, 1 Ion Cl s tng tc vi 1 Ion Ag+.
To kt ta l sunphua khng tan
Mt s cht, v d cc hp cht hu c, dc phm thuc h thioo (c cha Ion S 2-,
trong nhng iu kin thch hp c th tc dng vi mt s Ion kim loi to ra hp
129
cht sunphua khng tan, v cng c s dng xc nh cc cht hu c .

V d: xc nh vitamin B 1 (trong 1 phn t B 1c 1 Ion S2-), ngi ta ly a mg mu
c B1 cho tc dng vi b mg NaPbO 2 trong mi trng KOH nng chy trong ng nghim,
phn ng sinh ra PbS rt nh lng l c 1 phn t B 1, th bao gi cng to ra 1 phn t PbS.
1 phn t vitamin Bl + NaPbO2 ^ PbS
Sau ho tan hn hp phn ng trong 20ml dung dch NH 4C11%, lc v ra kt ta
PbS, ho tan kt ta PbS trong 15 ml HNO 3 1/1, nh mc thnh 25 mg v xc nh Pb trong
dung dch ny. Sau suy ra hm lng vitamin Bi trong mu a mg. theo phn ng trn.
Phn ng ny trc y c dng xc nh vitamin B 1, cng nh hm lng
penicillin trong thuc, hay trong cc sn phm thc phm, bng phng php khi lng, nn
ch xc nh c hm lng ln, v tin hnh rt lu cc thao tc kt ta, sy kh, cn kt
qu. Hin nay nh php o ph AES hay AAS, xc nh c c hm lng nh, m li
nhanh.
Theo phn ng kh mui kim loi
y chnh l phn ng trng gng, phn ng kh Ion Ag v Ag + kim loi, dng thuc
th Tulen, l phn ng xc nh cc cht andehit. V th phn ng ny ch yu c dng
xc nh hm lng cc cht c chc andehit trong phn t. Trong phn ng ny, c 1
nhm chc andehit - CHO trong phn t cht, th lun gii phng ra 1 nguyn t Ag.
R- (CHO)n + n(Ag+) ^ nAgo
V th cch ny hin nay c s dng xc nh cc hp cht hu c c cha andehit
dng R-(CHO)n, ch yu l theo phn ng trng gng.
V d: xc nh hm lng andehit fomic, ta ly V ml mu cho tc dng vi
ml thuc th Tulen, khi un nng nh, qu trnh kh Ion Ag+ xy ra theo phn ng:
HCHO + Ag+ ^ A go
Nh vy, kim loi Ag c gii phng v bm vo thnh ng nghim. Sau loi b
dung dch, ho tan kt ta Ag kim loi bng 10 ml axit HNO 3 1/1 nng, un nh cho tan ht,
nh mc thnh 25 ml, v xc nh Ag trong dung dch ny. Theo kt qu nng Ag, ta suy
ra hm lng andehit trong V ml mu theo phn ng trn.
Theo phn ng ho tan mt kim loi
Mt s cht, m ch yu y l cc axit hu c c kh nng ho tan cc kim loi hot
ng nh Cd, hay Zn rt nh lng, nn cng c s dng xc nh n, theo phn ng
to ra mui tan nh sau:
2R-(COOH) + Zn ^ (R-COO) 2Zn
130
Sau li tnm ly dung dch mui ny v xc nh nng Zn bng php o ph pht x

ca Zn, ri suy ra nng (hm lng) axit R-COOH tc dng vi Zn kim loi sinh ra
dung dch mui Zn(R-COO) 2.
Theo phn ng to hp cht phc bn chit c
Cch ny dng xc nh mt s Anion, hay cht hu c, ngha l cc Anion no c
th tc dng c vi mt Ion kim loi to ra c mt hp cht phc bn trong mt iu
kin nht nh v chit ra c khi dung dch mu, th u c th s dng xc nh cc
Anion .
V d: Xc nh Anion CNS -1 qua phn ng ca Anion ny vi dung dch mui FeCla
trong mi trng pH=1, theo phn ng:
Fe3+ + CNS ^ Fe(CNS)
Sau chit phc Fe(CNS) vo dung mi etyl e v xc nh Fe trong dch chit ny
(c th gii chit phc vo dung dch HCI 2M, v xc nh Fe trong dung dch gii chit ny).
Sau ta cng tnh c nng ln CNS trong mu phn tch.
Theo phn ng to hp cht d a
Cch ny thng c dng xc nh P, Si, qua thuc th molipdic trong mi trng
axit nc c 6M, sinh ra hp cht d a ca P vi Mo, m chng ta dng trong phn
tch ha hc xc nh P trong t trng bng phng php trung ha. Cch lm cng hon
ton tng t nh th, nhng y sau khi c c hp cht kt ta d a ca P, ngi ta ho
tan n trong kim 0,5 M v xc nh hm lng ca nguyn t molipden, bng ph pht x
ca Mo, sau suy ra hm lng P trong mu phn tch, theo phn ng sau.
PO4 + NH4+ + MoO42- + HNO3 ^ (NH4)3 [P(Mo3 O10H]
Hp cht d a ca P
Phn ng kh hp cht c nhm Nitro (-NO 2)
Mt s hp cht Nitro trong mi trng pH thch hp c th b kh v amin (R- NO 2 ^
R-NH2) bng kim loi hot ng, v d nh Cd, Zn,... rt nh lng, v phn ng ny
c s dng xc nh mt s hp cht hu c c nhm nitro, v d nh xc nh
Chloramphenicol, qua chun lng Ion Cd(II) sinh ra trong phn ng hay o ph pht x
nguyn t (AES hay ICP-OES) ca dung dch Ion kim loi Cd(II). V d trong mi trng axit
long (HCl 0,05M), bt kim loi xp Cd kh nhm -NO 2 v NH2 hon ton nh lng theo
phn ng sau.
3Cd + R-NO2 + 6HCl ^ 3CdCl2 + H2O + R-NH2 Chloramphenicol
Nh vy sau khi phn ng kt thc, ly tnm ly dung dch Anion CdCl 2 v xc nh Cd
bng php o AES v suy ra hm lng Chloramphenicol theo phn ng trn.
131
Vi cch ny c th xc nh c Chloramphenicol n nhy 0,005 ppm.

Hon ton tng t, nhiu hp cht hu c nitro u c th xc nh gin tip theo php
o ph hp th nguyn t.
Theo phn ng to hp cht hydrua bay hi
y l phn ng ca mt s Anion ca mt s nguyn t vi nguyn t hydro mi sinh
to ra hp cht kh hydrua dng MeHn (vi n = 3,4,5, v 6). V d: HgH 2, AsHa, ASH5, SbH3,
SbH5, SeH4, SeH8, TeHi, TeH3, v.v... Phn ng ny rt nh lng, trong nhng iu kin ph
hp cho mi cht. V th n cng c s dng xc nh cc nguyn t Hg, As, Se, Te..
trong cc i tng khc nhau, nh trong qung, trong nc, trong thc phm,.. bng php o
ph pht x v hp th nguyn t. Song trc ht l mu phn tch cn c x l a cc
nguyn t ny v dng mui ca Ion tan trong dung dch nc mi trng axit, v d HgCl 2,
SbCl5, SnCl4, Na3AsO4, Na2SeO0, Na2TeO4. Sau thc hin theo cc phn ng sau:
+ Vi Hg:
HgCl2 + Na2BH4 + HCl ^ HgH
+ Vi As:
ASO43- + Na2BH4 + HCl ^ AsH3

ASO43- + Na2BH4 + HCl ^ ASH5
+ Vi
Se SeO43- + Na2BH4 + HCl ^ SeH

SeO43- + NA2BH4 + HCl ^ SeH6
+ Vi
Te: TeO43- + Na2BH4 + HCl ^ TeH4

TeO43- + Na2BH4 + HCl ^ TeHs
Cc kh hydrua sinh ra trong cc phn ng trn c kh argon dn vo h thng nguyn

t ha mu ca my v o ph ca cc nguyn t theo cc iu kin thch hp cho mi
nguyn t.
Theo k
thut ny, hin nay
ngi ta c ring mt h phng php ha hi
nguyn t ha lnh qua vic to hp cht kh hydrua d b phn hu phc v vic tch v xc
nh cc nguyn t ni trn. Phng php ny c nhy rt cao, c 1-5 ng. Cc hng sn
sut my o AES v AAS u c bn b trang b cho k thut ny vi cc kiu khc nhau, t
n gin n hon chnh v t ng.
Theo nguyn tc hai
Theo tc dng lm gim cng vch ph
Theo cch ny, ngi ta cho cht phn tch X (cn xc nh) tc dng vi dung dch
mui ca mt kim loi c ph pht x nhy mt nng nht nh ph hp v khng i
to thnh hp cht bn, v hp cht ny s lm gim cng vch ph pht x ca kim loi
mt cch tuyn tnh trong mt vng nng nht nh ca cht cn xc nh X, ngha l y
chng ta c cng vch ph (lc ph) c gi tr
132
Phn II
Trongmu
dchta dng
th ph
pht
x ca
hay Cavkhi
mtph
ca
nm.V V
d d:
xc nh
Aniondung
F - ngi
Mg c
nng
2 ppm (2Zr,^g/mL)
oc
vch
-4
-5
glucose,
amino
axit, haynm.
protein,
v.v.lng
trong Fvng
tphp
n. 10
- n.10
mol/l
c c
tng
pht x ca
Mg-285,20
v nh
theonng
phng
ng
chun.
Dyschun
theo
tuyn
tnh.sau.
Tnh cht ny c s dng xc nh glucose trong cc i tng mu
pha theo
bng
sinh hc (hnh 6.11).
Bng 6.11
Bng 6.11
Dy chun xc nh nng Anion F Dy chun xc nh nng Protein
Chng 7
NHNG VN CHUNG CA PHP O ASS
Cc cht
Co
Ci
Cc cht
Ng Mg(ppm)
2
Co
C1
Ng. F (ppm)
0
S xut hin
phhp
th nguyn t2
Nng
Ca(ppm)
C2
C3
Dy chun
C2
2
4
2
C3
2
C4
2
C4
C5
Cx
2
C5
2
Cx
10
2
Cx
2
Nh chng
ta
bit,vt0cht 0,02
c cu
to bi
cc nguyn
t 0,10
v nguyn
t l
0,06
0,08
Cx
HClProtein
(%) (mm)
1
1 0,041
1
1
1
1
phn t c bn nh nht cn gi c tnh cht ca nguyn t ha hc. Nguyn t li bao gm
HCl
1khc(khong
nh
1 nhau
1
ht nhn nguyn
t(%)
nm gia v1chim 1mt th 1Cc
tch cht
rt nh
1/10.000
th 1tch ca
nguyn t) Cc
v cc
t (electron)Nh
chuyn
ng
xung
ht nhn
trong phn khng gian
I quanh
yuin
t khc
tt c,
nh
cht
o Ix (Mg285,20
nm)
Io nhau Ii
2 mi trng,
I3
I4 m,I5v.v. Ix
ln ca nguyn t. Trong iu kin bnh thng nguyn
t khng thu v cng khng pht ra
I
Io
I
2
I3
I4
I5
Ix
o Idi
nng lng
dng ccnm)
bc x. Lc ny nguyn t tn ti trng thi c bn. l trng
x (Ca-422,70
Sau
dng ng chun v pht hin nng ln F trong mu phn tch Cx
thi bn vng v ngho nng lng nht ca nguyn t. Nhng khi nguyn t trng thi hi
(hnh 6.10).
t do, nu ta chiu mt chm tia sng c nhng bc sng (tn si xc nh vo m hi
nguyn t , th cc nguyn t t do s hp th cc bc x c bc sng nht nh ng
ng vi nhng tia bc x m n c th pht ra c trong qu trnh pht x ca n. Lc ny
nguyn t nhn nng lng ca cc tia bc x chiu vo n v n chuyn ln trng tha
kch thch c nng lng cao hn trng thi c bn. l tnh cht c trng ca nguyn t
trng thi hi. Qu trnh c gi l qu trnh hp th nng lng ca nguyn t t do
trng thi hi v to ra ph nguyn t ca nguyn t . Ph sinh ra trong qu trnh ny c
gi l ph hp th nguyn t.
Nu gi nng lng ca tia sng b nguyn t hp th l XE th chng ta c:
AE = (Cm - Eo) = hv
(7.1)
hay l.
AE = h.c / X
(7.2)
c0 C
C2
c3 c4 c5
trong Eo v Cm l nng lng ca nguyn t trng thi c bn v trng thi kch

Hnh6.11b
thch m;Hnh
h l6.11a
hng s Plank; c l tc ca nh sng
trong chn khng; X l di sng ca
Cc pic ph
ng chun phn tch
vch ph hp th.
Theo tc dng lm tng cng vch ph
Nh vy,
vitng
mi gi
tr nng
lng
t hp
th ta
Cng
honng
ton
t nh
nguyn
tc AE;
ca m
cchnguyn
trn, nhng
c khc
l s
khiccmt
mtvch
ca
ph hp
viX
sng
i vch
c trng
cho nguyn
qu trnh
l ph
hp
thtuyn
ca nguyn
t
cht
phnth
tch
thdi
cng
ph ca
t ,
kimngha
loi li
c
tng
tnh theo
cng
l nng
ph vch.
s
tng
ca cht phn tch X c trong mu vi mt vng nht nh.
134
135
133
Nhng nguyn t khng hp th tt c cc bc x m n c th pht ra c trong qu

trnh pht x. Qu trnh hp th ch xy ra i vi cc vch ph nhy, cc vch ph c trng v
cc vch cui cng ca cc nguyn t.
Cho nni vi cc
vch ph qu trnh hp th v pht x l hai qu trnh ngc
nhau (hnh
7.1). Theo
phng trnh (7.1), nu gi tr nng lng AE l dng ta c qu trnh pht x; ngc li khi
gi tr AE l nm ta c qu trnh hp th. Chnh v th, ty theo tng iu kin c th ca ngun
nng lng dng nguyn t ha mu v kch thch nguyn t m qu trnh no xy ra l
chnh, ngha l nu kch thch nguyn t:
+ Bng nng lng Cm ta c ph pht x nguyn t,
+ Bng chm tia n sc ta c ph hp th nguyn t.
Trong php o ph hp th nguyn t m hi nguyn t ca mu trong ngn la hay
trong cuvet graphit l mi trng hp th bc x (hp th nng lng ca tia bc x) Phn t
hp th nng lng ca tia bc x hv l cc nguyn t t do trong m hi . Do , mun
c ph hp th nguyn t trc ht phi to ra c m hi nguyn t t do, v sau chiu
vo n mt chm tia sng c nhng bc sng nht nh ng ng vi cc tia pht x nhy ca
nguyn t cn nghin cu. Khi cc nguyn t t do s hp th nng lng ca chm tia
v to ra ph hp th nguyn t ca n.
Qu trnh pht x v hp th ca mt
nguyn t Eo: Mc nng lng trng
thi c bn; cm: Mc nng lng trng
thi kch thch; AE: Nng lng nhn vo
(kch thch);
+ hv: Photon kch thch;
+ hv: Photon pht x.
136
Hnh 7.1
Cng ca vch ph hp th nguyn t
Nghin cu s ph thuc ca cng mt vch ph hp th ca mt nguyn t vo
nng C ca nguyn t trong mu phn tch, l thuyt v thc nghim cho thy rng,
trong mt vng nng C nh ca cht phn tch, mi quan h gia cng vch ph
th v nng N ca nguyn t
trongm
hp
hicngtun theo
nh lut Lambe Bear, ngha l nu chiu mt chm sng cng ban u l I o qua m hi
nguyn t t do ca nguyn t phn tch nng l N v b dy l L cm, th chng ta c:
KN .L
(7.3)
trong Kv l h s hp th nguyn t ca vch ph tn s v v K v l c trng ring

cho tng vch ph hp th ca mi nguyn t v n c tnh theo cng thc:
( )2
K=Ke2
__A_
v-Vo
RT
( )2
V
(7.4)
Ko l h s hp th ti tnm ca vch ph ng vi tn s v o. A l
nguyn t lng ca nguyn t hp th bc x.
137
R l hng s kh.
T l nhit ca mi trng hp th ( oK).
Nu gi
Ax l cng ca vch ph hp
th nguynt,
t cng thc (7.3)
chng ta c:
A =
hay l:
= 2,303.K .N.L
Ax = 2,303.KV.N.L
(7.5)
y A chnh l tt nguyn t ca chm tia sng cng I o sau khi qua mi trng
hp th. A ph thuc vo nng nguyn t N trong mi trng hp th v ph thuc c vo
b dy L ca lp hp th (b dy chm sng i qua). Nhng trong my o ph hp th nguyn
t, th chiu di ca n nguyn t ha hay cuvet graphit l khng i, ngha l L khng i,
nn gi tr A ch cn ph thuc vo s nguyn t N c trong mi trng hp th. Nh vy
cng ca vch ph hp th s l:
Ax = k.L
(7.6)
vi k = 2,303.Kv.L
trong K l h s thc nghim, n ph thuc vo cc yu t.
H s hp th nguyn t Kv ca vch ph hp th,
Nhit ca mi trng hp th, v
B dy ca mi trng hp th L.
Song cng thc (7.6) cha cho ta bit mi quan h gia cng vch ph v nng
C ca nguyn t phn tch trong mu. Tc l qua h gia N v C. y chnh l qu trnh ha
hi v nguyn t ha mu phn tch. Nghin cu qu trnh ny, l thuyt v thc nghim ch ra
rng, mi quan h gia nng N v nng C trong mu phn tch c tnh theo biu thc
sau:
N = 3.1012xFW's'nR C
QT n
(7.7)
y l cng thc tng qut tnh gi tr N trong ngn la nguyn t ha mu theo

Winefordner v Vicker. Trong :
F l tc dn mu vo h thng nguyn t ha (ml/pht),
W l hiu sut aerosol ha mu,
s l hiu sut nguyn t ha,
nR l s phn t kh nhit ban u (ambient), T o(oK), nT l s
phn t kh nhit T(oK) ca ngn la nguyn t ha,
138
Q l tc ca dng kh mang mu vo bung aerosol ha (lt/pht),

C l nng ca nguyn t phn tch c trong dung dch mu.
Phng trnh (7.6) cho ta bit mi quan h gia A v N, phng trnh (7.7) cho
ta bit mi quan h gia N v C. Mi quan h ny rt phc tp, n ph thuc vo tt c
cc iu kin nguyn t ha mu, ph thuc vo thnh phn vt l, ha hc, trng thi
tn ti ca nguyn t trong mu. Nhng nhiu kt qu thc nghim ch ra rng, trong
mt gii hn nht nh ca nng C, th mi quan h gia N v C c th c biu
th theo cng thc:
N = Ka.Cb
(7.8)
trong Ka l hng s thc nhim, ph thuc vo tt c cc iu kin ha hi v

nguyn t ha mu; cn b c gi l hng s bn cht, ph thuc vo tng vch ph
ca tng nguyn t, b c gi tr bng 1 v nh hn 1, tc l 0 < b <=l. Gi tr b = 1 khi
nng C nh v ng vi mi vch ph ca mi nguyn t phn tch, ta lun lun tm
c mt gi tr C = Co b bt u nh hn 1, ngha l ng vi:
+ Vng nng C x < Co, th lun lun c b = 1, ngha l mi quan h gia
cng vch ph v nng Cx ca cht phn tch l tuyn tnh c dng ca phng
trnh y = ax.
+ Vng nng C x > Co th
b lun nh hn 1, tc l b tin v
tt nhin l khng bng 0. Nh
vy trong vng ny mi quan h
gia cng vch ph v nng
Cx ca cht phn tch l khng
tuyn tnh.
Nn Co c gi l gii hn
trn ca vng tuyn tnh.
n
kt
hp
phng
trnh (7.6) v (7.8) chng ta c:

Ax = a.Cb
(7.9)
c (ng/mL)
Hnh 7.2
Mi quan h gia cng vch ph A\ v nng cht cx
AB: Vng tuyn tnh(b=1), BC:Vng khng tuyn tnh
trong a = K.Ka v c gi l hng s thc nghim, ph thuc vo tt c cc iu

(b<1).
kin thc nghim ha hi v nguyn t ha mu, nh trnh by trn. Chnh do thc t

ny m trong mt php o nh lng xc nh mt nguyn t phi gi cho cc iu kin ha
hi, nguyn t ha mu n nh v khng i. Phng trnh (7.9) c gi l phng trnh c
s ca php o inh lng cc nguyn t theo ph hp th nguyn t ca n. ng biu din
ca phng trnh ny c 2 on, mt on thng (trong on ny b = 1), v quan h gia Ax.
v C l tuyn tnh) v mt on cong, trong on ny b < 1 (hnh 7.2).
139
Cu trc
vch
thHiu
nguyn
tny t
Stark
ca
ca
cu
rng
trc
kp,ph
nguyn
Hdhp
" khc
t.
vi
ngrng
cng
nhin,
gp
phn
rng
lmkp
tnglic
rng quyt
ca vch
nhph
bihp
s
Cc
vch
ph
hp
th
nguyn
t
cng
c
cu
trc
nht
nh
nh
cc
vch
ph
chuyn ng nhit
camt
nguyn
do
trong
mi trng
hp thth
theo
hng
th.
Do ,
cch t
yt,
rngca
vch phhp
nguyn
t cng
phi chiu hay
l:
pht
tng
vi ng
n. Nhng
vchtrong
ph mi
hp trng
th thng
n sc
nh thuc
vch
ngcxchiu
ving
chuyn
ca phtn
. V khng
th rng
ny ph
Ht = (Hn + Hd + Hl + Hc)
(7.13)
ph
iu
l
hp th
lnc
hn tnh
rng
nhiupht
vox.
nhit

cac
mingha
trng
hprng
th. ca
Mt vch
cch ph
gn ng,
thng
rng kp
theo
y
l
cng
thc
tng
qut
y
ca
ph pht x tng ng (hnh 7.3).
cngvch
thc:
cho
rngrngcavch
vch ph
hp
th-5th
hp
Hph
= 1,76.10
.v Vt/A
(7.11)
nguyn t. Nhng trong thc t ca
c xc nh bi nhiu yu t v
php o
phT hp
th nguyn
y,
l nhit
t,
cakhi
mi trng hp th
(oK), A l nguyn t lng ca
n l tng nhiu rng ring phn
khng
tcth
dng
cav t
trng
nguyn c
t hp
bc x
v o l
tn s trung tnm ca vch ph hp th.
ca cc
ngoi
v yu
vi t
cckhc
mynhau,
quangmt
phcch
c
Nh
vy,
rngton
kp ph
thuc
vo ba yu t T, A v v o. Ni chung, rng ny ca
tng
qut,
rng
phn
ca
tn sc nh hn 2 /mm, th l
hu ht
cc vch
phgm
hp cc
th
nguyn t thng nm trong khong t n.10 -3 n n.10-1 cm-1
vch
ph
bao
thuyt
v hp
thcth
nghim
ch ra rng,
(bng
7.2).
rng
chung
ca mt
rng
t nhin,
H n.vch ph hp th
Bng
ch
do7.2
ba thnh phn u (chim trn
rng
kp,biu
Hd. thc (7.13) quyt
95%) ca
rng kp ca mt s vch ph hp th
nh; rng Lorenz, HL.
Hnh7.3
~ , ,
TT
rng ca vch ph pht x (w1) v hp th (w2)
ngha l chng ta c:
rng cu trc tinh vi, H c.
= (Hn + Hd + Hl)
(7.14)
Vch ph (nm) Nguyn Ht
t lng
rng Hd cc nhit khc nhau ( oK).10-2 cm-1
Tc l:
iu ny hon ton ng i vi hu ht cc vch ph cng hng trong iu
Ht
= (Hn
+ Hd -+ 3500
HL +oCHcv) p sut l 1 atm. y, phn
kin mi trng hp th c nhit
t 1600
2500oC
3000oC
3500oC
Trong
t Htrn,
rng t nhin Hn c
n.
trung
tnmrng
ca vchtnhin,H
ph l do
rngbn
t yu
nhin
nh, quyt
phn
n v rng kp H d quyt
nh
bi
hiuquyt
s ca
bc
chuyn
nng lng ca 9,10
nguyn t trng22,00
thi c bn
rng
Lorenz
nh
(hnh
Li-670,80
7 7.4). gia hai mc
5,70
v trng thi kch thch. rng ny ph thuc vo thi gian lu ca nguyn t trng thi
B -249,80
11 ,
1,20
22,00
48,00
Trong tng rng
kch thch, v c tnh theo cng thc:
rng
Hn chim 45- 50 % 133
cn li l
Cs 825,10
1,00
1,60
4,00
ca rng Hd (25%) v Hi
H
(7 10)
=
'
(20%).Cn
rngH L:HL
thng
c yu
rng
Lorenz,
t th ba gp phn m rng rng ca vch ph hp th.
khng
ng
k,
ch nh
c lu
trong
tm n
lquyt
thi
gian
ca
nguyn
trng
thi t
kch
m. ami
s trng
cc trng
rng
nyc
bingha
s tng
tctca
cc phn
khthch
c trong
hp
-3
-1
khi
nguyn
t
c
t
trong
mt
hp,
rng
t
nhin
ca
vch
ph
hp
th
thng
khng
vt
qu
1.10
cm
(bng
7.1).
th vi s chuyn mc nng lng ca nguyn t hp th bc x trong mi trng .
t
trng
Bng
rng
Lorenz
7.1 mnh.
HL c tnh theo cng thc:
Ngoi
ph hp th
rngnhng
t nhinnghin
ca mtcu
mt trn,
s vch
HL = 12,40.1023.Po 2J^-( + )
L
so snh rng
ca cc vch
\RTph
AM
(7.12)
v
'
hp th vi nhau ngi ta thng

P.o na
laf p
lc rng
kh vca
M l phn t lng ca kh trong mi trng hp th
dng trong
i lng
-4
2
Vchva
ph
hp hiu
th ng.t
t
rng
Ni
(cm
) t kh tc dng
n() ph
l tit
din
chm
dng gia nguyn
hpHth
bc
x1.10
v phn
vch
(Wl/2).
vi n trong mi trng hp th. V cu trc hnh hc th rng Lorenz cng c dng ging
l 130Hg-253,70
rng ca vch
nm ph hp th v tr ng vi
0,50mt na (1/2) ca h s hp th
nh rng t nhin.
cc i Kmax (hnh 7.5). Gi tr ny ca vch ph hp th lun lun ln hn ca vch ph pht
Trn y l ba yu t chnh
quyt nh rng ca vch ph hp th. Ngoi ra cn c
x tng ng, tc Na-589,90
l vch phnm
hp th c rng ln hn 3,50
vch ph pht x nguyn t tng
cc yu t khc, nh s m rng rng do cu trc tinh vi ca lp v in t ca nguyn t.
ng vi n, v vch ph pht x, rng t nhin Hn quyt nh n 90% tng rng
V d, khi m hiCd-228,80
nguyn tnm
hp th nng lng c t2,70
trong mt t trng hay trong mt
chung ca vch ph.
in trng, th yu t ny mi th hin r. l hiu ng
142
140
141
Nguyn tc v trang b ca php o AAS

Phng php phn tch da trn c s o ph hp th nguyn t ca mt nguyn t
c gi l php o ph hp th nguyn t (php o AAS). Nh trong mc 7.1. chng ta
nghin cu, c s l thuyt ca php o ny l s hp th nng lng (bc x n sc) ca
nguyn t t do trong trng thi hi (kh) khi chiu chm tia bc x qua m hi ca
nguyn t y trong mi trng hp th. V th mun thc hin c php o ph hp th
nguyn t ca mt nguyn t cn thc hin cc qu trnh sau y:
Chn cc iu kin v mt loi trang b ph hp chuyn mu phn tch t trng thi
ban u (rn hay dung dch) thnh trng thi hi ca cc nguyn t t do. l qu trnh ha
hi v nguyn t ha mu. Nhng trang b thc hin qu trnh ny c gi l h thng
nguyn t ha mu (dng c nguyn t ha mu). Nh chng ta c c m hi ca
cc nguyn t t do ca cc nguyn t trong mu phn tch. m hi chnh l mi trng hp
th bc x v sinh ra ph hp th nguyn t.
Chiu chm tia sng bc x c trng ca nguyn t cn phn tch qua m hi nguyn
t va iu ch c trn. Cc nguyn t ca nguyn t cn xc nh trong m hi s
hp th nhng tia bc x nht nh v to ra ph hp th ca n. y, phn cng ca
chm tia sng b mt loi nguyn t hp th l ph thuc vo nng ca n mi trng
hp th. Ngun cung cp chm tia sng pht x ca nguyn t cn nghin cu gi l ngun
pht bc x n sc hay bc x cng hng.
Tip , nh mt h thng my quang ph ngi ta thu ton b chm sng, phn li v
chn mt vch ph hp th ca nguyn t cn nghin cu o cng ca n. Cng
chnh l tn hiu hp th ca vch ph hp th nguyn t. Trong mt gii hn nht nh ca
nng C, gi tr cng ny ph thuc tuyn tnh vo nng C ca nguyn t trong
mu phn tch theo phng trnh (7.9).
Ba qu trnh trn chnh l nguyn tc ca php o ph hp th nguyn t. V vy, mun
thc hin php o ph hp th nguyn t, h thng my o ph hp th nguyn t phi bao
gm cc phn c bn sau y:
Phn 1. Ngun pht tia pht x cng hng ca nguyn t phn tch (vch ph pht x
c trng ca nguyn t cn phn tch), chiu vo mi trng hp th cha cc nguyn t
t do ca nguyn t. l cc n canh rng (HCL), cc n phng in khng in cc
(EDL), hay ngun pht bc x lin tc c bin iu (xem mc 9.1. chng 9).
Phn 2. H thng nguyn t ha mu phn tch. H thng ny c ch to theo hai loi
k thut nguyn t ha mu. l k thut nguyn t ha bng ngn la n kh (lc ny ta c
php o F-AAS) v k thut nguyn t ha khng ngn la (lc ny ta c php o ETAAAS).
Trong k thut nguyn t ha bng ngn la, h thng ny bao gm:
143
+ B phn dn mu vo bung aerosol ha v thc hin qu trnh aerosol ha mu (to

th sol kh).
+ n
nguyn t ha
mu (Burner head)
t chy hn hp kh c
cha
mu th huyn ph sol kh (hnh 7.6).

Ngc li, khi nguyn t ha mu bng k thut khng ngn la, ngi ta thng dng
mt l nung nh bng graphit (cuvet graphit) hay thuyn Tangtan (Ta) nguyn t ha mu
nh ngun nng lng in c th thp (nh hn 12 V) nhng n c dng rt cao (50-800 A).
Hnh 7.6
H thng nguyn t ha mu trong ngn la
(1) n nguyn t ha mu, (2) Mng bo him, (3) ng thi phn mu tha, (4)
ng dn cht oxi ha, (5) ng dn mu vo bung aerosol ha, (6) ng dn cht chy
C2H2, (7) Vin bi to bi aerosol.
Phn 3. H thng my quang ph hp th, n l b n sc, c nhim v thu, phn li v
chn tia sng (vch ph) cn o hng vo nhn quang in pht hin tn hiu hp th AAS
ca vch ph.
Phn 4.
Hthng ch th tn hiu hp th ca vch ph (tc l cng
vch ph hp th hay nng nguyn t phn tch). H thng c th l cc trang b:

+ n gin nht l mt in k ch nng lng hp th (E) ca vch ph,
+ Mt my t ghi lc ca vch ph,
+ Hoc b hin s digital,
+ Hay b my tnh v my in (printer).
+ Hoc my phn tch (lntergrator).
144
ca
Vi cc my hin i cn c thm mt microcomputer hay microprocessor, v h thng

phn mm. Loi trang b ny c nhim v iu khin qu trnh o v x l cc kt qu o c,
v th, tnh nng ca mu phn tch, v.v... Mt cch tm tt, chng ta c th minh ho
mt h thng my o ph hp th nguyn t nh s trong hnh 7.7.
H gng
H gng
b)
B pht hin
=Q
Ngun
H gng
H gng
a)
_______________________________________________________________________________
Hnh 7.7
S nguyn tc cu to h thng my AAS.
a) H 1 chm tia; b) H 2 chm tia
1- Ngun pht tia bc x n sc; 2- H thng nguyn t ha mu; 3- H thng n sc
v detetctor; 4- B khuch i v ch th kt qu o; 5- Microcomputer.
Nhng u v nhc im ca php do AAS
Cng nh cc phng php phn tch khc, phng php phn tch ph hp th nguyn
t cng c nhng u im v nhc im nht nh. Cc u im v nhc im l:
Php o ph hp th nguyn t c nhy v chn lc tng i cao. Gn 60
nguyn t ha hc c th c xc nh bng phng php ny vi nhy t 1.10 -4
145
l mt
u5im
ln bit,
ca php
odng
ph hp
th nguyn
n
1.10"
%. c
nu s
k thut
nguynt.
t ha khng ngn la th c th t n
-7
nhy
(bng
7.3).phng
Chnh php
v c ny
nhy
nntc
phng
phpnh
phn
tch ny
un.10
im%th
ba ca
l cccao,
ng
thc hin
nhng.
Cc
ktc
qu
s
dng
ri trong
xcgin
nh
lng
vt gi
cc li
kimsau
loi
cCng
bit vi
l trong
phn
tchrtlirng
c th
ghi linhiu
trn lnh
bngvc
giyhay
lu
ny.
cc
phn
tch
cc
nguyn
t
vi
lng
trong
cc
i
tng
mu
y
hc,
sinh
hc,
nng
nghip,
kim
trang thit b hin nay ngi ta c th xc nh ng thi hay lin tip nhiu nguyn t trong
tra
ha Cc
cht kt
c
khit
mtcc
mu.
qutinh
phn
tchcao.
li rt n nh, sai s nh. Trong nhiu trng hp sai s
Bng
7.3
khng qu 15% vi vng nng c 1 - 2 ppm. Hn na, bng s ghp ni vi my tnh c
nhnnhy
(PC)ca
vcc
ccnguvn
phn mm
c php
hp qu
trnh o v x l kt qu s nhanh v d dng, lu li
t theo
o AAS
ng chun cho cc ln sau.
Bn
u im, php o ph F-AAS
hp th nguyn t cng c mt
s hn ch v
No cnh nhng
ETA-AAS
Nguyn t
nhc im nht nh. iu hn ch
trc ht
l mun
thc hin php o
ny
cn(ng/mL)
phi c mt
Flame
nhy (p,g/mL)
nhy
(nm)
h thng my AAS tng i t tin. Do nhiu c s nh khng iu kin xy dng
01
Ag-328,10
AA
0,05
0,10
phng th nghim v mua sm my mc.
02
Al-309,30
NA
0,10
0,50
Mt khc, cng chnh do php o c nhy cao, cho nn s nhim bn rt c ngha
03
Au-242,80
AA
0,05
0,05
i vi kt qu phn tch hm lng vt. V th mi trng khng kh phng th nghim phi
04
Ba-553,50
NA
0,10
0,50
khng c bi. Cc dng c, ha cht dng trong php o phi c tinh khit cao. cng l
05
Be-234,90
NA
0,10
0,30
mt kh khn khi ng dng phng php phn tch ny. Mt khc, cng v php o c
06 nn ccBi-223,10
1,00c k s c
nhy cao
trang thit b myAA
mc kh tinh vi 0,10
v phc tp. Do cn phi
Ca-422,70
0,05 phn tch cng c thnh
0,05tho vn
trnh 07cao bo
dng v chmAA
sc, cn cn b lm
08 NhngCd-228,80
0,03cng tc chun b v o
0,04
hnh my.
yu t ny c th AA
khc phc c qua
to cn b.
09
AA
1,00
Nhc
imCo-240,70
chnh ca phng
php phn tch 0,10
ny l ch cho ta bit thnh
phn nguyn
10 trong
Cr-357,50
AA khng ch ra trng
0,10 thi lin kt ca nguyn
0,80 t trong
t ca cht
mu phn tch m
AA tch thnh phn
0,04ha hc ca nguyn t 0,05
mu. V11th n chCu-324,70
l phng php phn
m thi.
12 v phm
Fe-248,30
0,08
0,10
i tng
vi ng dng caAA
AAS
i
ca phngAA
php phn tch theo
l phn tch
13 tng chnh
K-766,50
0,05 ph hp th nguyn 0t10
lng nh
vt) cc kim loiAA
trong cc loi mu
v c v hu
14 (lngMg-285,20
0,03khc nhau ca cc cht0,10
c. Vi15
cc trang Mn-279,50
b v k thut hinAA
nay, bng phng0,05
php phn tch ny ngi0,06
ta c th nh
lng c
cc kim loi (khong
hn nng
16 hu ht
Na-589,60
AA 65 nguyn t)
0,03v mt s kim n gii
0,05
c ppm (micrgam) bng k thut F-AAS, v n nng ppb (nanogam) bng k thut ETA17
Ni-232,00
AA
0,10
0,10
AAS vi sai s khng ln hn 15%.
18
Pb-283,30
AA
0,10
0,20
Trong khong 10 nm tr li y, phng php phn tch ph hp th nguyn t
19
Sr-466,70
AA
0,08
0,20
c s dng xc nh cc kim loi trong cc mu qung, t, , nc khong, cc mu
20
Si-251,60
NA
0,30
1,00
ca y hc, sinh
hc,cc sn phm nng nghip, rau qu, thc phm, nc
21
Zn-213,90
AA
0,03
0,10
ung, cc nguyn t vi lng trong phn bn, trong thc n gia sc, v.v... nhiu nc trn
th gii,
ccNgn
ncla
pht
trin,kh
phng
php phn
phlahp
thNnguyn
t tr
Ghinht
ch: l
AA:
(Khng
+ Axetylen),
NA:tch
Ngn
(Khi
2O + Axetylen)
thnh mt phng php tiu chun nh lng nhiu kim loi.
ng thi cng do c nhy cao nn trong nhiu trng hp khng phi lm giu
cc nh
kim loi,
kim
nh
S, Se,
Te cngliu
c
xc tn
nht thi gian,
nguynBn
t cnh
cn xc
trcmt
khivi
phn
tch.
DoSi,P,tn
t nguyn
mu,
khng cn phi dng nhiu ha cht tinh khit cao khi lm giu mu. Mt khc cng trnh
c s nhim bn mu khi x l qua cc giai on phc tp. cng
146
147
bng phng php phn tch ny. Cc kim khc nh C, Cl, O, N, khng xc nh trc tip
c bng phng php ny, v cc vch phn tch ca cc kim ny thng nm ngoi vng
ph ca cc my hp th nguyn t thng ng (190 - 900nm). V d C- 165,701 N-134,70;
O-130,20; Cl-134,78; S-180,70 nm. Do mun phn tch cc kim ny cn phi c cc b
n sc c bit. Cho nn n nay, theo phng php phn tch trc tip, i tng chnh ca
phng php phn tch theo ph hp th nguyn t vn l phn tch lng nh v lng vt
cc kim loi. Cn cc Anion, cc kim, cc cht hu c khng c ph hp th nguyn t phi
xc nh theo cch gin tip thng qua mt kim loi c ph hp th nguyn t nhy nh mt
phn ng ha hc trung gian c tnh cht nh lng, nh phn ng to kt ta khng tan, to
phc, y kim loi, hay ho tan kim loi, v.v... gia kim loi o ph v cht cn phn tch.
y l mt i tng mi, phong ph ang c nghin cu v pht trin.
Vi i tng , khong chc nm tr li y php o ph hp th nguyn t v
ang c pht trin rt nhanh, khng nhng phn tch cc kim loi m phng hng
ang pht trin nht hin nay l nghin cu xc nh cc cht hu c, nh cc hp cht hu c
halogen, lu hunh, photpho. N cng v ang c s dng nh l mt cng c phn tch
c lc cho nhiu ngnh khoa hc v kinh t. Nhiu phng th nghim v php o ph hp th
nguyn t c xy dng. Cc hng trn th gii ch to nhiu my mi c nhiu tnh
nng u vit. Cc vin nghin cu khoa hc quc gia, cc vin nghin cu nng nghip, vin
a cht, cc ngnh a cht, cng nghip luyn kim, cng nghip ha hc, cng nghip ha
du, cng nghip thc phm, ngnh y, bnh vin, cc trng i hc u c cc phng th
nghim v php o ph hp th nguyn t. C th ni n nay, hu ht cc lnh vc ca khoa
hc k thut v kinh t u s dng phng php phn tch ph hp th nguyn t. Ring
nc ta, tuy mi tip thu k thut ny trong vng 5 nm, nhng n nay trong ton quc chng
ta cng c gn ba chc phng th nghim v h thng my o ph hp th nguyn t.
148
Chng 8
CC K THUT NGUYN T HA MU
Mc ch v nhim v
Nguyn t ha mu phn tch l mt cng vic ht sc quan trng ca php o ph hp
th nguyn t, bi v ch c cc nguyn t t do trng thi hi mi cho ph hp th nguyn
t, ngha l s nguyn t t do trong trng thi hi l yu t quyt nh cng vch ph hp
th v qu trnh nguyn t ha mu thc hin tt hay khng tt u c nh hng trc tip n
kt qu phn tch mt nguyn t. Chnh v th ngi ta thng v qu trnh nguyn t ha mu
l hot ng tri tim ca php o ph hp th nguyn t.
Mc ch ca qu trnh ny l to ra c m hi cc nguyn t t do t mu phn tch
vi hiu sut cao v n nh php o t kt qu chnh xc v c lp li cao. p ng
mc ch , nguyn t ha mu phn tch, ngy nay ngi ta thng dng hai k thut.
Th nht l k thut nguyn t ha mu trong ngn la n kh. K thut ny ra i u tin
cng vi s ra i ca php o ph hp th nguyn t. Nhng k thut ny c nhy khng
cao, thng l trong vng 0,05 - 1 ppm (bng
. Sau l k thut nguyn t ha khng ngn la. K thut ny ra i sau, nhng li c
nhy rt cao t n 0,1ng (bng 7.3) v hin nay li c ng dng nhiu hn k thut
nguyn t ha mu bng ngn la. Chnh v c hai k thut nguyn t ha mu khc nhau nn
chng ta cng c hai php o tng ng. l php o ph hp th nguyn t trong ngn la
(F-AAS: Flame Atomic Absorpt Ion Spectrophotometry) v php
ph hpthnguyn t khngngn
la(Electro-Thermal Atomizat Ion
Atomic Absorpt Ion Spectrophotometry: ETA- AAS).

K thut nguyn t ha mu bng ngn la
Theo k thut ny ngi ta dng nng lng nhit ca ngn la n kh ha hi v
nguyn t ha mu phn tch. V th mi qu trnh xy ra trong khi nguyn t ha mu ph
thuc vo cc c trng v tnh cht ca ngn la n kh, nhng ch yu l nhit ca ngn
la. l yu t quyt nh hiu sut nguyn t ha mu phn tch, v mi yu t nh hng
n nhit ca ngn la n kh u nh hng n kt qu.
Yu cu v nhim v ca ngn la
Trong php o
ph hp th nguyn t, ngn la
l mi trng hp th. N c
149
nhim v ha hi v nguyn t ha mu phn tch, to ra m hi ca cc nguyn t t do c

kh nng hp th bc x n sc to ra ph hp th nguyn t. V th ngn la n kh
mun dng vo mc ch ha hi v nguyn t ha mu phn tch cn phi tho mn mt
s yu cu nht nh sau y:
Ngn la n kh phi lm nng u c mu phn tch, ha hi v nguyn t ha mu
phn tch vi hiu sut cao, bo m cho php phn tch t chnh xc v nhy cao.
Nng lng (nhit ) ca ngn la phi ln v c th iu chnh c ty theo
tng mc ch phn tch mi nguyn t. ng thi li phi n nh theo thi gian v c th
lp li c trong cc ln phn tch khc nhau m bo cho php phn tch t kt qu
ng n. Yu cu ny c lc khng c tha mn, v nhit cao nht ca ngn la cng
ch n 3300oC Do vi nhng nguyn t to thnh hp cht bn nhit th hiu sut nguyn
t ha ca ngn la l km.
Yu cu th ba l ngn la phi thun khit, ngha l khng sinh ra cc vch ph ph
lm kh khn cho php o hay to ra ph nn qu ln quy ri php o. Qu trnh Ion ha v
pht x phi khng ng k v qu trnh ny lm mt cc nguyn t t do to ra ph hp th
nguyn t.
Mt yu
cuna l
ngn la phi c b dy ln c c lp hp th
dy lm tng nhy ca php o. ng thi b dy ca lp hp th li c th thay i c

khi cn thit, o nng ln. Trong cc my hin nay, b dy ny c th thay i c
t 2 ci n 10 cm.
Tiu tn t mu phn tch.
to ra ngn la, ngi ta c th t chy nhiu hn hp kh khc nhau, bao gm mt
kh oxy ha v mt kh chy, trong cc n kh thch hp. Nhng vi nhng yu cu ni
trn th ch c mt vi loi n kh l to ra c ngn la tng i ph hp cho php o ph
hp th nguyn t. l nhng mi trng nguyn t ha mu tng i bn vng v kinh t
(bng 8.1). c bit c ng dng nhiu nht trong php o AAS l ngn la ca n kh
c t bng hn hp kh: (axetylen v khng kh nn) hay ngn la ca n kh (N 2O v
axetylen), hay (hydro v axetylen).
Bng 8.1a v 8.1b l mt s v d v nhit ca ngn la mt s n kh c dng
trong php o AAS (Ox: cht oxy ha; K.K: khng kh.).
Bng 8.1b
Quan h gia nhit v loi kh t
150
t nng cng vi cc ht sol kh (th aerosol) ca mu phn tch. Phn ny c nhit

thp (700-1200oC). Dung mi ha tan mu s bay hi trong phn ny v mu c
Loi kh
T l kh (l/ph)
Nhit (oC)
sy nng.
Phn K.K
b: L vng trung tm
ca ngn la. Phn
cao, nht l
Propan
6/1,4 ny c nhit 2200
nh b, v thng khng c mu hoc c mu xanh rt nht. Trong phn ny hn hp
K.K
Axetylen
4,2/1,2
2450
kh c t chy tt nht v khng c phn ng th cp. V th trong php o ph
K.K
Hydro
4/3
2050
hp th nguyn t ngi ta phi a mu vo phn ny nguyn t ha v thc hin
Oxyl ngun n scAxetylen
1/1ca ngn la.
3000
php o, ngha
phi chiu qua phn ny
2900
Phn Nc:2OL v v ui Axetylen
ca ngn la. Vng 2/1,8
ny c nhit thp,
ngn la c
mu vng v thng xy ra nhiu phn ng th cp khng c li cho php o ph hp
Bng
8.1b t.
th nguyn
Thnh phn
nhit
ngnv
lacu to nn trong mi php phn tch cn phi kho
Chnhkhdovcc
cim
st chn c cc iu kin ph hp, nh thnh phn v tc ca hn hp kh
chy K.K
to ra ngn la, Axetylen
chiu cao ca ngn la, v
4,2/0,7
.v...
Trang b nguyn t ha mu
K.K
Axetylen
4,2/0,9
Mun thc hin php o ph hp th
K.K
Axetylen
4,2/1,1
nguyn t (F-AAS), trc ht phi chun b
1800
2000
2300
mu K.K
phn tch trng
thi dung dch. Sau 4,2/1,2
Axetylen
dn dung dch mu vo ngn la n kh
K.K
Axetylen
4,2/1,5
ha hi v nguyn t ha mu phn tch v
2450
thc K.K
hin php o. Axetylen
Qu trnh nguyn t ha4,2/1,6
trong ngn la gm hai bc k tip nhau.
c
im
v cu
to ca dung
ngn la
kh phn tch
Bc
mt
l chuyn
dchn
mu
2300
thnh
th cc
Nhit
l
vi
kh
mang
c trng ca
2400
ht nh
nh s
sng m trn u
mt
thng
v
kh la
chy.n
l cc ht sol
ngn
kh Nhit
(th aerosol).
kh.
ngnQulatrnh
ca ny c gi l
quloi
trnh
hayrtnebulize ha. K
mt
naerosol
kh phha
thuc
thut vo
thc bn
hin cht
qu
nhiu
n nh
phn
cahng
cht trc
kh
o AAS.
chy
to
ra
trnh
ny v hiu sut ca
v thnh
tip
cn
tkt qu ca php
ngn
la,
ngha lSaung
mi hp
mtaerosol
hn cng hn hp kh t vo n (burner head) nguyn t
vi
dn hn
hp
s hai
c kh t chy to ra ngn la. Thng thng ngi ta hay
ha.kh
Khchy,
mang ngn
l mtla
trong
mt
ha
xc (khng
nh v
dngnhit
kh oxy
khkhi
nn hay kh N 2O). Hai giai on trn c thc hin bng mt
thnh
phntrang
kh chy
thay i
h thng
b nguyn
t ha mu (hnh 7.6). H thng ny gi l Nebulizer System, gm
thhainhit
ngn la cng b thay i (bng 8.1a v 8.1b). Ngoi yu t trn, tc
phn
chnh:
dn ca hn hp kh vo n t chy cng nh hng n nhit ca ngn la v
qua m nh hng n cng ca vch ph (hnh 8.1).
n nguyn t ha mu (burner head). Cc n ny thng c hai dng khc nhau, hoc
Xt v cu to, ngn la n kh gm ba phn chnh (hnh 8.2):
hnh trn c nhiu l hay hnh mt khe hp c rng t 0,5 - 1,0 mm v 152
Phn a: L phn ti ca ngn la. Trong phn ny hn hp kh c trn u v
151
chiu di 5 cm hay 10 cm.

Loi khe di 10 cm cho hn hp kh t axetylen v khng kh nn; loi khe di
5 cm l cho hn hp kh t axetylen v kh N 2O (hnh 8.3). Cn loi ming trn ch
thch hp cho php o ph pht x.
Phn hai l bung aerosol
ha mu. l bung iu ch
cc ht sol kh ca mu vi kh
mang. thc hin cng vic ny
ngi ta p dng hai k thut theo
nguyn l khc nhau. l k thut
pneumatic-mao dn (phun kh) v
k thut ultrasonic (siu nm). Do
n NTH
ca Perkin Elmer
cng c hai loi h trang b khc
nhau (hnh 8.4 v 8.5) iu ch

sol kh ca mu.
, Hnh 8.3
n NTH
ca Phillips
Cc loi n nguyn t ha mu
Aerosol ha mu theo k thutpneumatic-mao dn.

Theo cch ny ngi ta dng h thng nebulize v kh mang to ra th si kh ca
mu phn tch nh hin tng mao dn (hnh 8.4).
Trc ht nh ng mao dn S v dng kh mang K m dung dch mu c dn vo
bung aerosol ha. Trong bung ny, dung dch mu c nh tung thnh th bi (cc ht rt
nh) nh qu bi E v cnh qut Q, ri c trn u vi hn hp kh t v c dn ln n
nguyn t ha (burner head).
Khi hn hp kh t chy burner head s to ra ngn la, di tc dng ca nhit ca
ngn la cc phn t mu th si kh s b ha hi v nguyn t ha to ra cc nguyn t t
do ca cc nguyn t c trong mu phn tch.
l nhng phn t hp th nng lng v to ph hp
th
nguyn
ca
nguyn t cn nghin cu.
Nhng cn ch rng, ngoi nh hng ca thnh phn kh t v tc dn hn hp
kh n cng vch ph, th tc dn dung dch mu vo bung aerosol ha cng nh
hng ng k n cng vch ph (bng 8.2).
Tc dn mu ph thuc vo nhiu yu t v c tnh gn
ng theocng
thc:
153
(1)
___________________1________________________A.
Hnh 8.4
H thng to soi kh (nebulize) theo k thut pneumatic
K: Kh mang (oxy ha); S- ng dn mu; F- Kh chy; Q: Cnh qut quay u; GMng bo him; A: ng dn th aeresol ln n nguyn t ha.
nrP
V (ml / ph) = nLP
(81)
8Ln
trong :
r- bn knh ca ng mao dn dn mu;
P- chnh lch p sut gia hai u ng mao dn;
L- chiu di ng mao dn;
n- nht ca dung dch mu (g.cm.s).
Bng 8.2
nh hng ca tc dn mu n cng vch ph Cu - 324,70mm
Tc kh (lt/pht)
Cng vch ph
1,00
0,150 '
2,00
0,180
3,00
0,206
4,00
0,225
5,00
0,235
6,00
0,230
Ngha l tc dn mu V ph thuc vo cc tham s r, P, L v n Nhng trong mt h

thng my th r v L thng l c nh, P c gi khng i, cho nn V ch
154
cn ph thuc ch yu vo nht n ca dung dch mu (hnh 8.5).

Aerosol ha mu bng siu nm.
Theo
thut
ny,
aerosol
ha mu phn tch ngi ta dng

h thng siu nm c tn s t 1-4,5
MHz. Lc siu nm c th c
truyn qua tng rn (hnh 8.6a)
hay qua th lng (hnh 8.6b) n
dung dch mu thc hin vic
aerosol ha mu, ngha l di tc
dng ca lc siu nm, mu dung
dch cng c phn tn (nh ti)
thnh nhng ht rt nh v trn u
vi hn hp kh dn ln n (burner head) nguyn t ha. y ng knh (d)
ca
cc ht sol kh c tnh theo cng thc:

d = yj (n.s / 4.Di.F2)
(8.2)
trong :
s: sc cng b mt ca dung dch mu;
Di: t trng ca dung dch mu;
F: tn s ca my pht siu nm.
Nh
vy,
mun
cc
ht aerosol nh th phi s
dng tn s siu nm cao.
Tn s v cng sut ca my
pht siu nm u nh hng
n
kch
thc
ca
ht
aerosol (hnh) Trong hai k

thut
aerosol
ha,
th
thut pneumatic l n gin,

trang b r tin, khng phc
tp nh k thut siu nm.
Nhng k thut siu nm c
u im cho nhy cao
hn. V kch thc cc ht
sol kh kh nh, hiu sut
to sol kh cao v qu trnh aerosol t ph thuc vo kh mang v qu trnh dn mu. c bit l
vic aerosol ha cc dung dch mu c nng mui cao th n u vit hn
155
(cc
mui
ca cc cht)
trongsngn
la,ha
v n
c
vocho
vng
ngn(bng
la.
k thut
pneumatic.
Mt khc,
aerosol
bng
siudn
nm tip
thng
trung
lp litnm
tt hn
Tip
8.3). s nung nng, nng chy, cc qu trnh ha hi v nguyn t ha ca cc ht mu bt
kh
Bng.
8.3 y cc cht s c cc qu trnh chnh sinh ra ph v qu trnh ph khng sinh ra
ph din bin theo tnh cht nhit ha ca cht mu.
nhy theo hai k thut aerosol ha mu
Cc qu trnh chnh: Xy ra thng theo hai c ch chnh:
Nu nng lng (nhit ) ha hi (E h) ca cc hp phn c trong mu nh hn nng
lng nguyn
t hat(E a) ca n, tc lPneumatic
E h<Ea, th trc ht cc hp phn
ny s ha hi
Nguyn
Ultrasonic
dng phn t. Sau
b phn li (nguyn t ha) thnh
Cu cc phn t kh ny mi
0,05
0,03cc nguyn t
t do (c ch I).Fe
Hoc cng c th chng khng
t t do, nu
0,0 b phn li thnh cc nguyn0,03
l cc hp cht bn
Mg nhit.
0,05
0,03
Pbh< Ea):
C ch I: (E
Ni
Cr
0,10
0,10
MnAm (l) ^ MnAm (k) ^ n.M(k) + m.A(k)
0,10
M(k) + n(hv)
0,10 ^ Ph AAS
0,08
0,06
0,08
Co
0,07
Ni chung,
mui axetat, mt s mui nitrat,
Mncc mui halogen (tr F),
0,05
0,03 mt s mui
sunphat ca kimZnloi thng xy ra theo c
0,03ch ny. V d: Cc hp cht:
0,02CuCl 2, ZnCl2,
FeCl3, Cu(Ac)2, Zn(Ac)2. v.v... theo c ch 1 ny. C ch ny cho php o AAS c nhy
cao v n nh.
Ngc li, nu nng lng phn li Ea ca cc hp phn ca mu nh hn nng lng
ha hi Eh ca chnh n, th trc ht cc hp phn s b phn li thnh cc nguyn t t
do, ri sau mi ha hi (c ch II).
C ch II (Eh > Eo):
MnAm (l) ^ n.M(r,l) + mA(l.r) ^ n.M(k)
M(k) + n(hv) ^Ph AAS
Cc loi hp cht mui ca kim loi vi -sunphat, -photphat, -silicat, flo, thng theo
c ch II. C ch ny khng n nh, nn php o AAS km n nh, v nhy km hn c
ch 1. V th ngi ta thng thm vo mu cc mui halogen, hay axetat ca kim loi kim
lm nn mu hng cc qu trnh chnh xy ra theo c ch 1 u vit v c li hn.
l hai c ch ca qu trnh nguyn t ha mu phn tch (qu trnh chnh) trong
ngn la n kh. N l nhng qu trnh chnh to ra cc nguyn t t do quyt nh cng
ca vch ph hp th nguyn t ca nguyn t phn tch. Yu t quyt nh cc qu trnh
Nhng qu trnh xy ra trong ngn la
ny l:
Ngn la l mi trng nguyn t ha mu ca php o ph hp th nguyn t (F+ Nhit ca ngn la;
AAS). Trong ngn la c nhiu qu trnh ng thi xy ra: c qu trnh chnh v cng c qu
+ Bn
caTrong
cht mu
v thnh
phn
cala
mu;
trnh ph
(thcht
cp).
nhit
ca
ngn
l yu t quyt nh mi din bin ca cc
qu trnh
.dng nh hng ca cht ph gia thm vo mu.
+ Tc
Trc
ht,
khiph:
mu th si kh c dn ln n nguyn t ha, di tc dng nhit
Cc qu
trnh
ca ngn la, ming n, l s bay hi ca dung mi ho tan mu v cc cht hu c (nu
c) trong th si kh. Nh vy mu cn li l cc ht bt mu rt nh mn
156
157
0C
Bng
8.5 hi,
cng
chotrnh
chng
ta thy
rng,
trong
nhit cn
di
3 0 s
00 qu
thtrnh
kh
Bn Ha
cnh
cc nguyn
qu
trong
ngn
langn
n la
kh c
thng
c mt
t chnh,
ha.
ph.
quthch
trnhph
phpht
ny x
thng
nh ln
hng
n c
cng
phtr
trong
nng Cc
b kch
l khng
v nu
cng
chvch
gi vai
quannhng
trng mc
i vi
MeA(r) ^ MeA(l) ^ MeA(k)
khc
nhau,
lmm
gim
cc kim
loinh
kim
thi.cng ca vch ph, n xy ra nh th no l ty thuc vo nhit
S
phn
li,
kch
thch,
th,vIon
ha, pht x.
caS
ngn
thnh
cahp
mu,
hpla
thvca
phnphn
t: Trong
ngn d
la,nh:
ngoi cc nguyn t t do cng cn c c cc
o Qu trnh ny xy ra d dng i vi cc nguyn t
Ionphn
ha t
ca nguyn
t phn
tch.
1 Me
+phn
A (phn
li) ty theo tnh cht ca n v cng ty
Ion vScc
trng thi
hi.
Cc
t ny
c
th vo
Ion ha
v mc
b Ion
hao catamt
loi
tc
l s
tyhp
thuc
nhit
ca
thuc
nhitthp
ca
ngnla,
vng
quan
st,nguyn
m x)
cn
thvo
nng
lng,
s
1 Meph
+ vh (hp
th
bc
ngn
la
v
th
Ion
ha
ca
nguyn
t
.
Nu
th
Ion
ha
cng
nh,
th
n
b
Ion
ha
cng
Ion ha hay s kch thch ph ca chnh cc phn t . Nhng qu trnh ny, tuy l qu trnh
MeAny
^ c ngha
1 Meo +ln
E (kch
thch)
nhiu.
V th
quc
trnh
i vi
cc
kim
loiph
kim
sau tlphn
cc kim
ph nhng
cng
trng hp
c nh rt
hng n
cng
vch
cavnguyn
tch.
o
th
(bng
Memu
- e (rn
Ioncha
ha)b ha hi. Yu t ny gi l s hp th
Thm
vo8.4).
l s hp th ca cc1ht
gi. 8.4
Bng
1 Meo +......
Bng
8.5b Ion ha ca cc nguyn t theo nhit ngn la v th Ion ha ca n
Mc
S kh oxy ca oxit bi cacbon.
Mc b kch thch ph pht x ca cc nguyn t - ng vi nhit khc nhau
NguyMeO + CTh
Ion+ha
S % b Ion ha nhit 0C
^ Me
CO(eV)
2500
Nguyn
t ng ha
Thhc
kch
thch
(Nhng)
nhitMe
+( 0C).3000
Cc phn
ph
khc (hp2000
chtT
bnsnhit
monoxit):
Na
5,21 (ev)
1,00
15,0
26,0
Vch ph(nm)
2000
3000
4000
O ^ Meo
K
4,32
10,0
30,5
80,5
-4
-3
-2
Cs-852,10
1,48
4,40.10
7,20.10
3,00.10
Me
+
C
^
MeC
x
Rb
4,06
14,0
44,0
89,0
Na-589,00
Cs
3,872,11
-5
1,00.10
30,0
-4
5,90.10
70,0
-3
4,40.10
95,0
Ca
Ca-422,70
Ba
Zn-213,90
6,102,95
5,505,89
2,00 -6
1 20.10
3,00 -13
7,50.10
10,0-5
3,70.10
17,0-10
5,60.10
16,0-4
6,00.10
33,0-8
1,50.10
Al
6,60
0,60
1,00
09,0
Mgthnh hp cht7,60
0,30 la n kh, 0,60
S to
bn nhit. Trong ngn
mt s kim loi 05,0
c th hnh
thnh cc hp
kiu monoxit dng MeO, nh AlO, Bao,
Be cht bn nhit9,30
0,30 MgO, Beo, ZrO,...
01,0 Loi
hp cht ny rt bn, khi hnh thnh th kh phn li thnh cc nguyn t t do trong ngn
Nh vy, qu trnh Ion ha l lm gim s nguyn t t do trong ngn la, c ngha l
la n kh. V th lm gim nhy ca php o.
lm gim cng ca vch ph hp th. V th cn phi hn ch nh hng ny, bng cch
Cc qu trnh ph tuy c mc khc nhau, nhng trong mt mi tng quan nht nh
chn cc iu kin ph hp gi cho nhit ca ngn la n nh v khng qu ln xy ra
trong ngn la, c bit l nhit ngn la, th tt c cc qu trnh u c th xy ra cng
s Ion ha nguyn t phn tch; hoc thm vo mu Anion ca mt nguyn t kim loi c th
vi cc qu trnh chnh ca php o F-AAS. Do iu quan trng i vi chng ta l phi
Ion ha thp hn th Ion ha ca nguyn t phn tch hn ch qu trnh Ion ha ca nguyn
chn cc iu kin ph hp hn ch n mc nh nht cc qu trnh ph v gi cho n
t phn tch.
khng i sut trong mt php o xc nh mt nguyn t. lmt phn cacng vic ti
S pht x: ng thi vi qu trnh Ion ha, cn c s kch thch ph pht x ca cc
uha cciukin cho phpo ph
hp th
nguyn
tt do ca nguyn t phn tch di tc dng nhit ca ngn la. S
nguyn t trong ngn la.
nguyn t b kch thch v mc b kch thch ph pht x cng ph thuc vo nng lng
kch thch ph pht x ca tng nguyn t. Nguyn t no c nng lng kch thch ph pht
Bng
8.6nh th s b kch thch cng nhiu (bng 8.5). Nhit ca ngn la cng cao th
x
cng
cng
thch
cng
t
loi
yu t nh hng ny, ngi ta cng thm vo mu
Tm b
tt kch
cc qu
trnh
khinhiu.
nguyn
hatrmu
Anion ca cc nguyn t kim loi c th kch thch ph pht x thp hn nguyn t phn tch,
Dn mu vo bung aerosol ha.
qu trnh ny ch xy ra vi nguyn t thm vo .
Qu trnh aerosol ha mu to ra th sol kh.
158 160
159
Hnh 8.8
S cc qu trnh trong ngn la
M1: Kim loi phn tch; M2: Cc kim loi khc trong mu; A: Anion khng oxy; AxOz: Anion
c oxy; Mo: Kim loi t do trng thi hi; x, y v z nhn gi tr 1,2,3,4,...
161
a) Cc qu trnh trong ngn la ca CaCl 2 khng c PO4
162
cc qu trnh trong ngn la ca CaCl 2 khi c Al Hnh

8.9
V d v cc qu trnh trong ngn la n kh (a, b, c).
Ti u ha cc iu kin nguyn t ha mu
Nh trn chng ta xc nh, nguyn t ha mu l cng vic quan trng nht ca php
o F-AAS. Qu trnh ny thc hin khng tt s nh hng trc tip n kt qu ca php o.
Do mun t c kt qu chnh xc v ng n, chng ta phi kho st, pht hin v
chn cc iu kin nguyn t ha mu ph hp nht cho tng nguyn t cn phn tch trong
mi loi mu c th. Cc iu kin c th l: Thnh phn v tc ca hn hp kh t to
ra ngn la. y l yu t quyt nh nhit ca ngn la. V th qua vic thay i thnh
phn v tc ca hn hp kh t to ra ngn la chng ta c th chn c nhit ph
hp ha hi v nguyn t ha nguyn t cn nghin cu (hnh 8.1 v hnh 8.10) v (bng
8.1).
Tc dn dung dch mu vo h thng nguyn t ha. Ni chung, trong nhiu trng
hp tc dn mu ph hp nm trong khong t 4-5 ml/pht vi php o ca nhiu nguyn
t (hnh 8.11).
Chiu cao ca n nguyn t ha. Yu t ny cng nh hng trong mt mc nht
nh v ty thuc vo tng nguyn t (hnh 8.12), nn chn chiu cao ca burner head sao cho
c c cng vch ph ln nht v n nh nht ...
163
C0H2l/niin
C2H2l/min
Hnh 8.10
nh hng ca tc kh chy n cng vch ph
Hnh 8.11
nh hng ca tc dn mu
n cng vch ph
Hnh 8.12
nh hng ca chiu cao quan st
n cng ca vch ph
B dy ca mi trng hp th L: Khi thay i b dy ca lp hp th (mi trng hp

th) chng ta c th tng hay gim nhy ca php o. Ngha l ty theo nng ln hay
nh ca nguyn t phn tch m chng ta thay i gc nghing ca n nguyn t ha mu
(burner head) c c b dy L ca lp hp th ph hp nht. Khi L ln nht ta s c
nhy cao nht, lm gim L th nhy gim theo, ngha l khi o nng ln th ta phi quay
n nguyn t ha mt gc cho ph hp m khng cn pha long, nhng sau cn phi gi
khng i sut trong qu trnh o.
Tn s my siu m: Nu to soil kh mu phn tch trong h thng aerosol ha bng
siu nm th tn s v cng sut ca h thng siu nm cng cn c chn cho ph hp. Yu t
ny cng nh hng n hiu sut nguyn t ha mu (hnh 8.7). Tip l tc dn mu
vo bung siu nm cng cn c chn cho ph hp.
nht ca dung dch mu: Tip theo cc yu t trn l nht ca dung dch mu. Yu
t ny nh hng rt nhiu n hiu sut nguyn t ha thng qua qu trnh aerosol ha mu
theo k thut pneumatic (hnh 8.5) v (bng 8.2). Do mu phn tch
164
v cc mu chun dng ng chun cn phi c chun b trong cng mt iu kin,

phi c cng thnh phn ha hc, vt l, c bit l thnh phn ca cht nn ca mu, axit,
loi axit dng lm mi trng chng c cng nht.
Trn y l cc yu t c nh hng n qu trnh nguyn t ha mu, ngha l nh
hng n kt qu ca php o F-AAS. Tt nhin mi yu t c nh hng trong mc
khc nhau, c trng hp xut hin, song cng c trng hp khng xut hin r rt. Trong
yu t u tin, nhit ngn la l quan trng nht, n quyt nh hiu sut ca qu trnh
nguyn t ha mu. Cc yu t khc cn li nh hng n yu t th nht v qua m gy
nh hng n kt qu ca php o.
Do , vic nghin cu pht hin v chn cc thng s cho ph hp nht i vi mc
ch phn tch nh lng mt nguyn t vi lng trong mi i tng mu l mt cng vic
ht sc cn thit v quan trng cho k thut phn tch F-AAS, chn v xy dng mt quy
trnh chun.
Mt khc, nu chn c cc iu kin nguyn t ha mu ph hp, th trong nhiu
trng hp li loi tr c mt s yu t nh hng nht nh, nh nh hng ca ph nn,
s Ion ha, s pht x hay cc qu trnh th cp trong ngn la khng c li cho php o.
Thc hin cc cng vic trn chnh l tiu chun ha xy dng mt quy trnh phn tch mt
nguyn t bng php o ph hp th nguyn t ca n.
K thut nguyn t ha khng ngn la
c im v nguyn tc
K thut nguyn t ha khng ngn la ra i sau k thut nguyn t ha trong ngn la.
Nhng k thut ny c pht trin rt nhanh v hin nay ang c ng dng rt ph bin, v
k thut ny cung cp cho php o AAS c nhy rt cao (mc nanogam ppb); c khi gp
hng trm n hng nghn ln php o trong ngn la (bng
. y l u im chnh ca k thut nguyn t ha khng ngn la. Do , khi phn tch
lng vt cc kim loi trong nhiu trng hp khng cn thit phi lm giu s b cc nguyn
t cn xc nh. c bit l khi xc nh cc nguyn t vi lng trong cc loi mu ca y hc,
sinh hc, dc phm, thc phm, nc gii kht, mu, srum.
Tuy c
nhy
ca php
caonhng trongmt strng hp,
n nh
khng ngn la thng km php o trong ngn la, nh hng ca ph nn thng rt ln.
l c im v cng l nhc im ca php o ny. Song vi s pht trin ca vt l v
ca k thut o hin i, ngy nay ngi ta c th khc phc c nhc im ny khng kh
khn lm. V th cc h thng my o ph hp th theo k thut khng ngn la ca nhng
nm 1980 lun lun c km theo h thng b chnh nn v n nh ca n cng khng km
cc h thng ca php o trong ngn la v m bo nhy cao c ppb i vi nhiu
nguyn t.
c im na ca php o khng ngn la l i hi mt lng mu tng i
165
nh. Thng thng mi ln o ch cn lng mu t 20 n 50 p,L. Do khng cn nhiu

lng mu phn tch, vic chun b mu cng d dng v khng tn nhiu ha cht cng nh
cc dung mi tinh khit cao t tin.
V nguyn tc, k thut nguyn t ha khng ngn la l qu trnh nguyn t ha tc
khc trong thi gian rt ngn nh nng lng ca dng in cng sut ln v trong mi trng
kh tr. Qu trnh nguyn t ha xy ra theo ba giai on k tip nhau: sy kh, tro ha luyn
mu, nguyn t ha o ph hp th v cui cng l lm sch cuvet. Trong hai giai on
u l chun b cho giai on nguyn t ha t kt qu tt. Nhit trong cuvet graphit l
yu t chnh quyt nh mi s din bin ca qu trnh nguyn t ha mu.
Cc yu cu h thng nguyn t ha mu
H thng nguyn t ha phi ha hi v nguyn t ha mu phn tch vi hiu sut cao
v n nh, m bo cho php o c nhy cao v lp li tt.
Phi cung cp c nng lng (nhit cao) ln, c th nguyn t ha c
nhiu loi mu v phn tch c nhiu nguyn t.
Cuvet cha mu nguyn t ha phi c tinh khit cao. Khng lm nhim bn mu,
khng c ph ph gy kh khn cho php o nguyn t cn phn tch.
Hn ch, c t hay khng c cc qu trnh ph trong qu trnh nguyn t ha mu thc
hin php o.
Tiu tn t mu.
l nhng yu cu ti thiu cn thit i vi mt h thng trang b nguyn t ha mu
trong php o khng ngn la. Trn c s cc yu cu ny, mi hng ch to my ph hp th
nguyn t u c nhng h trang b ring cho cc my ca h. Song v nguyn tc v cc
bc ca qu trnh nguyn t ha th u nh nhau.
Nguyn tc v cc giai on ca qu trnh nguyn t ha mu
Nguyn tc v cch thc hin ca k thut nguyn t ha khng ngn la l hon ton
khc vi k thut nguyn t ha trong ngn la. y ngi ta thng dng nng lng nhit
ca mt ngun nng lng ph hp nung nng, ha hi v nguyn t ha mu phn tch
trong ng cuvet graphit hay trong thuyn tng tan (Ta) nh. Ngun nng lng thng c
dng hin nay l dng in c cng dng rt cao (t 50 - 600 A) v th thp (di 12 V)
hay l nng lng ca dng in cao tn cm ng.
Di tc dng ca cc ngun nng lng ny, cuvet cha mu phn tch s c nung
nng tc khc v mu s c ha hi v nguyn t ha to ra cc nguyn t t do
trng thi hi c kh nng hp th bc x n sc, to ra ph
hp
th
nguyn t ca n. Dng c nguyn t ha mu theo k thut ny hin
nay c rt
nhiu loi khc nhau c ch to ty thuc theo tng hng v tng phng th nghim. Nhng
c th khi qut theo cc nhm chnh di y:
166
+ Cc loi cuvet graphit;

+ Cc loi cc graphit;
+ Cc loi thuyn kim loi chu nhit, nh Ta.
Trong cc loi trn, c dng ph bin nht l cc cuvet graphit, v n tho mn c
nhng yu cu chnh ca php do khng ngn la. v cuvet graphit, mi hng ch to my
quang ph hp th nguyn t u c cuvet graphit ring cho cc my ca h v h thng
nguyn t ha khng ngn la tng ng.
H thng nguyn t ha mu theo k thut khng ngn la gm c:
+ Bung nguyn t ha v cuvet graphit cha mu phn tch thc hin qu trnh
nguyn t ha;
+ Ngun nng lng nung nng l graphit n nhit nguyn t ha mu v b
iu khin hay b chng trnh (programer) t chng trnh v ch huy qu trnh nguyn
t ha mu theo cc giai on nht nh. V d: Hng Perkin Elmer c h thng khng ngn
la HGA-70, HGA-400, HGA-5001 Hng Philips'pye Unicam c SP9- 041.
Tuy mi hng c nhng dng c khc nhau, nhng qu trnh nguyn t ha trong cc
dng c u xy ra theo 4 giai on k tip nhau trong thi gian tng cng t 80 - 60 giy.
Cc giai on l:
Sy kh mu
y l giai on u tin ca qu trnh nguyn t ha mu. N l rt cn thit m
bo cho dung mi ho tan mu bay hi nh nhng v hon ton, nhng khng lm bn mu,
mt mu. V nu khng thc hin sy tt, mu s b bn lm sai lch kt qu phn tch.
thc hin qu trnh sy tt, i vi mi mt loi mu cn phi tin hnh nghin cu, pht hin
v chn nhit v thi gian sy cho ph hp. Nhit v thi gian sy kh ca mi loi
mu ph thuc vo bn cht ca cc cht trong mu v dung mi ho tan n. Thc nghim
cho thy rng, khng nn sy mu nhit cao v sy kh nhanh. Ni chung nhit sy
kh ph hp i vi ba s cc mu v c trong dung mi nc nm trong khong t 100 150oC trong thi gian t 25-40 giy vi lng mu c bm vo cuvet nh hn 100 pl Tt
nhin qu trnh sy kh chm nhit thp bao gi cng cho kt qu n nh. Vic tng
nhit khi sy, t nhit phng n nhit sy mong mun cng cn c thc hin t
t, vi tc tng nhit t 8 n 5 0C trong mt giy l ph hp.
i vi cc
mu c cha
cc cht hu c hay ho tan trong dung mi
hu c,
thng phi sy nhit thp hn v tc tng nhit phi chm hn dung mi nc.
Vi loi mu ny, nhit sy thng l di 100 0C. Hnh 8.13 l mt v d v qu trnh sy
kh mu. Trong T 8 l nhit sy ti a (ti hn) v trong 6 tc tng mhit sy, th
ch c qu trnh theo ng s 5 v 6 l cho kt qu tt. ng
167
thi trong quan h t l gia thi gian Ramp (thi gian tng nhit ) v thi gian sy
thng nm trong t l t 3/4 - 2/4 l
phhpcho nhiu nguyn t.
nguyn t cng c mt nhit sy ti a cho
(bng 8.6),
Mt khc, mi
ngha l nu sy mu
nhit cao hn nhit th kt qu phn tch km n nh v s mc sai s rt ln.

Tro ho luyn mu
y l giai on th hai ca qu
trnh nguyn t ha mu. Mc ch
l tro ha (t chy) cc hp cht
hu c v mn c trong mu sau
khi sy kh, ng thi nung
luyn mt nhit thun li cho
giai on nguyn t ha tip theo
t hiu sut cao v n nh. Giai
on ny c nh hng rt nhiu
n kt qu phn tch, nu chn
nhit tro ha khng u ho th
mt s hp cht c th b phn hu mt trong giai on ny, nu nhit tro ha l
qu cao. L thuyt v cc kt qu thc nghim xc nhn rng, tro ha mu t t v
nhit thp hn nhit gii hn th php o lun lun cho
kt qun nh, v
mi
nguyn t u c mt nhit tro ha luyn mu gii hn (T r.) trong

php oETAAAS.
Nhit tro ha gii hn l nhit m s tro ha mu nhit v nh
hn n, th cng vch ph hp th l khng i (hnh 8.14). Cn nu tro ha mu
nhit ln hn nhit th cng vch ph b gim v khng n nh. Nhit
tro ha gii hn ca mi nguyn t
rt khc nhau,n ph thuc vo bn
mi nguyn t v ph thuc vo dng
hp cht mnguyn t
matrix (cht nn) ca mu (hnh 8.14).

Ni
chung,
mt
ha
hc, cc nguyn t bn nhit v

tn ti trong cc dng hp cht
bn nhit thng phi tro ha
luyn mu nhit tng i
cao. Nh v d trong hnh 8.14,
Si c nhit tro ha gii hn
l 1100oC, Ni l 1000oC, cn Pb
l 600oC. Ngay i vi mt
nguyn t nhit tro ha gii
hn Tr cng c th khc nhau,
khi chng tn ti trong cc cht
168
tn
cht ca
ti,cng
nh
khc nhau
Khi Nn
nghin
cuca mu
k (matrix
qu effect), nht l cc cht nn bn nhit. Hnh 8.18 l mt
v d v
ny
khi o
ph hp
trnh
trovnha
luyn
mu
ca th nguyn t ca Mg trong cc nn khc nhau.
nhiu Ngha
nguyn
t, trong
ngiccta cht
thynn khc nhau c nhit tro ha gii hn l T1, T2, T 3 v
l Mg
rng,
quan
hvgia
T4 (tcmi
l 600,
1000
1100oCnhit
).
trong
ha thi
luynquamu
v cng
chng
ta thy ngha ca cht ph gia c thm vo mu phn
ca
vch
ph
hp
th
tch.
nguyn t ca cc nguyn t
thng tun theo mt trong ba
Bng 8.6
loi nh trong hnh 8.14. Loi
l tiu biu cho cc nguyn
t Pb, Zn, Co, Mg. Loi (2) l
Mt s v d v nhit sy, tro ha luyn mu, nguyn t ha mu gii hn ca mt s
Ni, Cu. Loi (3) l Si, Ca, Al.
nguyn t (theo W. Fuller)
Mt
khc Nguyn
cc t kt
qu
Nhit ti hn ca qu trnh (oC)
thc nghim cng ch ra rng,
khng nn tro ha luyn mu Sy
nhitmu
qu gii hn,
v nh th vic
luyn
Tro ha
Nguyn
t mu
ha chun
b cho giai on nguyn t ha s khng tt.
Al
130
1100
2850
Ch nn tro ha nhit cao nht l bng hay thp hn nhit tro ha gii hn mt t
(khong 30 - 50oCBa
).
150
1100
2900
Ngoi yu t nhit th tc tng nhit trong qu trnh tro ha cng c nh hng

Be
130
1100
2750
n n nh ca cng vch ph. Ni chung, tc tng nhit qu ln thng lm
Ca chm bao gi cng
130 cho kt qu tt 1100
2800hin tro ha
bn mu. Vic tng
hn, ngha l phi thc
luyn mu trong mt thi gian khng qu ngn. Thng thng l t 30 - 60 giy, vi lng
Cu
120
0650
2650
mu a vo cuvet nh hn 100 ^L. Trong tng thi gian tro ha, thng dnh 1/3 cho vic
tng nhit t Fe
nhit sy n nhit
l tc tng nhit
nm trong
120 tro ha, ngha
1000
2700
vng t 60-100 trong 1 giy l thch hp. Sau thi gian cn li 2/3 l gi nhit khng
Pb
100
0600
2500
i chn luyn mu.
170
Mg
150
1100
2850
Mn
130
1000
2700
Si
150
1200
2850
Na
139
0800
2200
Sr
130
1100
2800
Zn
110
0600
2500
Co
110
1100
2750
Cr
110
1100
2750
169
i vi cc mu c cht hu c hay trong dung mi hu c th giai on ny cng phi

cn thn v nhit chn tro ha phi thp hn dung mi l nc, trnh s bay hi
trc ca nguyn t phn tch dng hp cht c kim. Do , vi mi loi mu, trong mi
loi dung mi, chng ta cn kho st pht hin c nhit tro ha ph hp cho n.
Nguyn t ho
y l giai on cui cng ca qu trnh nguyn t ha mu, nhng li l giai on
quyt nh cng ca vch ph. Song n li b nh hng bi hai giai on trn. Giai on
ny c thc hin trong thi gian rt ngn, thng thng t 3 n 6 giy, rt t khi n 8-10
giy.
Nhng tc
tng nhit li l rt ln t ngay tc khc
n nhit
nguyn t ha v thc hin php o cng vch ph. Tc tng nhit thng l t
1800 - 2500oC/giy, thng thng ngi ta s dng tc ti a. nguyn t ha ca mt
nguyn t rt khc nhau (hnh 8.17).
ng thi mi nguyn t cng c mt nhit nguyn t ha gii hn Ta ca n. Nhit
Ta ny ph thuc vo bn cht ca mi nguyn t v cng ph thuc trong mc nht
nh vo trng thi v thnh phn ca mu m n tn ti, nht l cht nn ca mu (hnh 8.18).
2600 2800
Hnh 8.17
Quan h gia nhit nguyn t ha v cng vch ph ca cc nguyn t
171
2000
2400
2800
Hnh 8.18
nh hng thnh phn nn ca mu n nhit nguyn t ha mt nguyn t
Khi nghin cu qu trnh nguyn t ha ca nhiu nguyn t trong cc iu kin khc

nhau, ngi ta thy s din bin ca nhit nguyn t ha ca mt nguyn t v cng
vch ph ca n thng theo hai loi nh trong hnh 8.19. Cc nguyn t theo loi (1) c nhit
nguyn t ha gii hn l Ta1, ngc li, cc nguyn t theo loi (2) c nhit nguyn t
ha gii hn l Ta2.
Tiu biu cho loi (1) l cc nguyn t Zn, Fe, Pb, Cu v Mo, tiu biu cho loi
l cc nguyn t, Si. Sn, Mg, Ca (hnh 8.17). Cc gi tr nhit Ta1 v Ta2 l nhit
nguyn t ha gii hn ca mi loi. Khi nguyn t ha mu o cng vch ph ca
mt nguyn t nhit cao hn nhit gii hn ny thng khng c li thm v cng
, m kt qu thc nghim cho thy cc kt qu o thng khng n nh v thng lm
hng nhanh cuvet graphit.
172
Ngoi vic
chn
nhit
trong
giai on
Cc
yu ,
t nh
hng
ny cn cn phi chn
Cng
vi
cc
thi gian nguyn t ha
iu kin sy, tro
cho ph hp lm sao m
ha v nguyn t
bo cc lc cng vch
ha mu nh
ph thu c phi gn v
trnh by trn, qu
ch c mt nh. Nh v
trnh nguyn t ha
d trong hnh 8.20 ch c
mu theo k thut
trng hp (a) l tt.
khng ngn la cn
b
nh
hng
bi
mt s yu t khc
na. Cc yu t ny
nh
hng
khc
"t------ - ! _ ... 1
i.......i... :
........- .............................
nhau
nguyn
vi
'
mi
cng
>
J-----------
1-------
u
- - -----f- l|
4
-------------
---------------!_
c khi li
khng gy
4
nh hng.
----------r
-T .
H---------------4
41
i
T.
-!
:!
----------p
----1
----
T
~
=
=t
~ ---- =4
Trc ht l mi trng kh tr thc hin qu

r t ha.ri
t trnh nguyn
t hcho qu trnh nguyn
___
Kh tr thng c dng lm mi trng
t
=f
i
.....
-4
---------H
.......7
-----------------
-----------------
i-t '
--------
-i_-
t-
-tr-
-----------
ir
r-
1
I
(Ar), nit (N2) v hai
(He),
ngha l qu
;ri
>
.. .
-1 3
-----
-4.
'
T-
,4-
1 T T
trnh nguyn
------5
kiH _______u
____
!....
ha l argon
----1---
-----------j-------
^---------
r hin
""
t ha -1
thc--
trong mi
__
-1
=4=
....c oxy. Do khng xut^1

trng khng
hin hp cht bn nhit loi MeO hay MeOX.
L
-i
b
d graphit
Nhng abn cht, thnh phn
v tc dn kh ctr vo trong cuvet
nh
hng
cng
ca
nhit
vtrong
graphit t
(hnh 8.22).
Hnh
8.20n
Quan
h gia
hnhvch
dngph
lcv
vch
ph
thi cuvet
gian nguyn
ha
Trong ba loi kh tr ni
trn, th Ar l kh tt nht, sau
nCa-422,7nm.
N2. nga: 3thi
giy,khi
b: 4 giy, c: 6 giy v d: 8 giy
tng tcn
y
dnchng
kh vo
ta ccuvet
th khi qut ton b qu trnh nguyn t ha mu theo k thut
graphit
th
cng
vch
ph
khng ngn la nh trong hnh 8.21. Trong : (1) l giai on sy mu; (2) l giai on tro
lun
lun mu;
gim(3)vl giai
mcon
nguyn t ha o cng vch ph v (4) l giai on lm
ha luyn
gim
cng graphit.
khc nhau
sch cuvet
oni
R lvi
thi gian tng nhit ca hai giai on u (thi gian Ramp).
mi nguyn t (hnh 8.22a).
Do trong phn tch, khi o
cng vch ph bt buc
phi
gi
cho
tc
dn
khng i, hoc c th tt kh
Q | -----------------1 --------------- 1---------------- 1----------------1 ---------------1----------------1 ------------------
100
200
400
(ml/ph)
Hlnh 8.22a
nh hng ca tc kh tr n cng vch ph
mi trng trong giai on nguyn t ha o cng vch ph.
174
173
Yu
th
hai
l cng sut t nng

cuvet. Nhn chung, khi
tng
cng
sut
nng cuvet th cng

vch ph tng theo
(hnh 8.23). Nhng s
ph
thuc
ny
cng
ch trong mt gii hn
nht
nh,
sut
khi
cng
nng
cuvet
nh hn 6 KW.
Cn khi t nng cuvet cng sut ln hn 7 KW th hu nh cng vch ph
khng tng na (hnh 8.23).
Yu t th ba l tc t nng cuvet. Tc t nng cuvet v thi gian nguyn t ha
t l nghch vi nhau. Nu o din tch ca lc th yu t ny hu nh khng nh hng,
nhng nu o chiu cao ca lc th li rt khc nhau (hnh 8.24). Ni chung chiu cao ca lc
t l vi tc t nng cuvet.
175
Hnh 8.24 l cc lc vch ph

ca qu trnh nguyn t ha 10 ppb
Pb vi cc tc t nng cuvet: 1)
2300; 2) 1600; 3) 1000 v 4)
800oC/giy. y chng ta thy vi
tc t nng 1, vch ph c
chiu cao ln nht, sau n tc
2 v cui cng l tc 4.
Nhng vn chnh l ch, khi
Hnh 8.24
nguyn t ha vi tc t nng
nh hng ca tc t nng cuvet n cng vch Pb
cuvet thp, ta thng phi nguyn

t ha thi gian di, do trng
hp dn n lc ca vch ph khng nhng c chiu cao thp, m cn c nhiu nh
v dng phc tp gy kh khn cho vic nh gi nh lng.
Yu t th t l loi cuvet graphit dng nguyn t ha mu, ngha l cc loi nguyn
liu graphit khc nhau cng nh hng n cng vch ph v thi gian nguyn t ha
mu (hnh 8.25).
Ni chung, cc
loi graphit hot ha ton phn thng
cho kt qu tt nht,
nhy cao, n nh.

Hnh 8.25 l mt v d v vn
ny. l vic nguyn t ha
Cr v Al vi ba
loi cuvet khc nhau. Pic 1 l vi cuvetgraphit c hot ha nhitton phn; tc 2 l

cuvet graphit
chc hot
hot
ha.
176
ha b mt v tc
3 l cuvet graphit thng khng
Cc qu trnh trong cuvet graphit

Cc qu trnh xy ra trong cuvet graphit v c ch ca qu trnh nguyn t ha mu l
nhng vn ht sc phc tp, nhng li quyt nh cng ca vch ph. Mun hiu bit
c ch ca vn ny, chng ta phi xem xt tt c cc yu t ng hc, nhit ng hc v
cc phn ng ha hc c th xy ra trong cuvet, v cc qu trnh l xy ra ng thi v c
tc ng qua li ln nhau. Nhng khi nghin cu mt yu t ny, thng thng ngi ta phi
c lp hay gi cho cc yu t khc khng i. Song thc cht khng phi nh th, cc qu
trnh xy ra trong cuvet graphit khng c lp v tch bit ln nhau, m chng gn cht vi
nhau v c tc ng qua li nh hng ln nhau nhng mc nht nh di tc dng
quyt nh ca nhit trong cuvet graphit. V th vic xem xt mt yu t trong khi cc yu
t khc c gi khng i ch l tng i trong mt iu kin nht nh dt ra, theo
di s thay i ca mt yu t.
Nhiu tc gi nghin cu cc qu trnh xy ra trong cuvet graphit, song cho n nay cng
ch c nhng kt qu bc u trong mt vi trng hp c th. Chnh v th cha th nu
mt c ch chung ca qu trnh nguyn t ha mu trong cuvet graphit, do chng ti ch
mun cp n mt vi vn chnh c th chp nhn
177
c theo quan im ng hc v nhit ng hc ha hc nhit cao, theo trt t ca qu

trnh nguyn t ha mu.
Qu trnh nguyn t ha mu xy ra theo ba giai on k tip nhau, nh hng ln nhau.
Trong hai giai on u l chun b cho giai on th ba nguyn t ha mu o cng
vch ph. l mt tng th lin tip din bin ca nhiu qu trnh. Nhng d hiu chng
ta c th tch ring v khi qut theo nhng vn sau y:
S bay hi ca dung mi. y l qu trnh vt l n gin, n xy ra trong giai on u
(sy mu) ca qu trnh nguyn t ha mu v nhit l yu t quyt nh s din bin ca
qu trnh ny. Nhng thnh phn ca mu, cc cht hu c c mt trong mu cng nh hng
n qu trnh ny. Sau khi dung mi bay hi s li cc ht mu l bt mn ca cc mui
kh trong cuvet.
S tro ha (t chy) cc cht hu c v mn. Qu trnh ny xy ra trong giai on th
hai ca qu trnh nguyn t ha. Khi cc cht hu c b tro ha, s to ra cc cht kh (CO,
CO2, H2O) bay i v li phn b v c ca mu. l cc mui hay cc oxit ca cc cht
mu. Tip b ny c nung nng, nng chy hay b phn hy ty theo nhit tro ha
chn v ty thuc vo bn cht ca hp cht mu tn ti trong cuvet sau khi sy kh. Lc ny
mu c luyn thnh th nng chy ng nht. ng thi y cng c s phn hu ca
mt s mui khng bn thnh oxit hay mui hay oxit n gin. V d, nu trong mu c
CaCO3 th c th c phn ng phn hy nh sau:
CaCO3 (r) ^ Cao(r) + Co2(k)
S ha hi ca cc hp phn mu dng phn t. Nu nhit ha hi (nng
lng ha hi) ca cc hp phn mu nh hn nhit phn li ca chng th cc hp phn mu
ny s ha hi dng phn t, sau chng b phn li thnh cc nguyn t t do. l c
ch ha hi ca cc phn t c p sut ha hi cao v nhit ha hi thp hn nhit phn li (Eh
< Ea). Tiu biu cho cc hp cht thuc loi ny l cc oxit Sb 2O3, Ga2O3,
halogen ca cc kim
loi nh SbCl5, SnCl4,
cc
mui
SnBr4, AlCl3,
TiCl4, GaCl3, cc mui axetat, Clorat ca kim loi, v.v... C ch din bin ca cc hp cht
loi ny c th minh ho theo hai kiu s sau y
C ch chnh 1:
MxXy(r,l) > MxXy(k) > xM(k) + X
MxOy (r,l) > MxOy(k) > xM(k) + O 2
M(k) + n(hv) ^ ph AAS
Qu trnh (a) xy ra i vi cc mui halogen kim loi v qu trnh (b) l i vi cc
oxit kim loi d ha hi. Nh cc hp cht ZnCl 2, CuCl2, FeCl3, CdCl2,...Cn qu trnh (c) l
s hp th bc x ca nguyn t, to ra ph.
178
Sau y l vi v d v c ch ny:
CdCl2(r,l) ^ CdCl 2(k) ^ Cd(k)
CuCh(r,l) ^ CuCl2(k) ^ Cu(k)
SbCl5(r,l) ^ SbCl5(k) ^ Sb(k)
Nhng ring mui AlCl 3 ngoi qu trnh chnh theo c ch (a) th cn qu trnh ph
sinh ra hp cht monooxit bn nhit dng AlO nh sau:
AlCl3 (r,l) ^ Al3(k) + Cl 2
Alo(k) ^ A(k) + O2
Qu trnh ph ny ph thuc vo s c mt ca oxy v nhit ca cuvet. nhit
nh hn 2500oC th qu trnh (e) hu nh khng xy ra c. V th n lm mt nguyn t t
do Al, qua lm gim cng vch ph. Do phi tm cch ngn cn khng cho hnh
thnh AlO, tc l phi hn ch qu trnh (d) xy ra khi nguyn t ha mu. kh b qu
trnh (d), ngi ta phi nguyn t ha mu trong mi trng kh tr hay thm vo mu nhng
cht ph gia thch hp.
S phn li ca cc phn t cht mu trc khi ha hi. Khuynh hng ny thng xy ra
i vi cc phn t c p sut ha hi thp v nhit phn li nh hn nhit ha hi phn t ca
chnh n Eh > Ed. Cc phn t thuc loi ny, di tc dng ca nhit trong cuvet graphit,
trc ht chng b phn li thnh cc monooxit hoc thnh cc nguyn t t do trng thi rn,
hay lng, ri sau mi c chuyn thnh th hi theo cc tnh cht ring ca sn phm va
c hnh thnh. Din bin ca qu trnh thuc loi ny c th minh ho theo cc s di
y:
C ch chnh 2:
MxXy (r,l) ^ Mx(r,l) + yX(k)
_______________^ xM(k)
MxXy (r,l) ^ xMO(r,l) + yX(k)
_______________xM(k)
MxOy(r,l) ^ mX(r,l) ^ xM(K)
MxOy(r,l) ^ xMO(r,l) ^xM(r,l) ^ xM(k)
Sau l qu trnh hp th bc x ca cc nguyn t M(k).
M(k) + n(vh) ^ Ph AAS
Cc qu trnh (f) v (g) ny l i vi cc mui ca kim loi vi nitrat, cacbonat, sun
pht, phtpht, ngha l cc mui c oxy. Cc qu trnh (h) v (i) l i vi cc hp cht oxit.
Cc qu trnh theo cc c ch ny thng km n nh v cho kt qu nhy thp hn cc
qu trnh ca cc mui halogen trn. Tiu biu cho s din bin
179
theo kiu ny l cc hp cht, cc mui cacbonat, sunphat v photphat ca kim th Ca, Ba,
Si. V d:
FeCl3(r,l) ^ Fe(r,l) ^ Fe(k)
Mn(NO3)2(r) ^ Mno(r,l) ^ Mn(k)
CaO(r) ^ Ca(r) ^ Ca(k)
V2O5(r) ^VO(r) ^ V(k)
Nh vy, cc qu trnh ny xy ra trong cuvet nh th no ty thuc vo:
+ iu kin nguyn t ha mu (ch yu l nhit ).
+ Tnh cht nhit ha ca cc hp cht mu ,
+ nh hng thnh phn nn ca mu, v
+ Mi trng tin hnh nguyn t ha mu.
+ Cht nn ca mu, cht ph gia thm vo.
S to thnh hp cht cacbua kim loi.
Trong cuvet graphit s xut hin hp ht cacbua kim loi l iu tt nhin, nhng mc
rt khc nhau i vi mi kim loi. Ch yu l cc kim loi bn nhit nh kim th, t
him. Phn ng ny thng may xy ra gia cc monooxit kim loi vi cacbon ca cuvet
graphit hay ca kim loi th lng v rn vi cacbon:
(k) M + xC ^ MCx
(l) MO + xC ^ MCx + O2
trong x c th l 1,2,3,4.
Sau cc hp cht cacbua va hnh thnh s ha hi v b nguyn t ha theo tnh
cht, c trng nhit ha ca n. Tt nhin qu trnh ha hi v nguyn t ha ca cc hp
cht loi ny tng i kh khn v phi nhit kh cao, v n l cc hp cht bn nhit.
V th phi ngn nga khng cho cc qu trnh (k) v (l) xy ra. Mc hnh thnh cc hp
cht loi ny rt khc nhau i vi tng kim loi v ph thuc vo nhiu yu t nh:
+ Tnh cht ca mi kim loi;
+ iu kin nguyn t ha mu, nhit nguyn t ha;
+ Thnh phn ha hc ca mu;
+ Loi cuvet graphit nguyn t ha mu.
Ni chung, cc cuvet graphit hot ha nhit ton phn (pyrolitic coated graphit)
thng hn ch xu hng to thnh hp cht cacbua kim loi. Ngc li, cc loi cuvet
graphit thng (standard graphit cuvet) kh nng hnh thnh cc hp cht
180
cacbua kim loi l rt ln. Hin tng ny th hin rt r rng khi phn tch cc kim loi kim
th, nhm v cc t him. c bit khi cc nguyn t ny l nn ca mu, th s xut hin
cc hp cht cacbua kim loi c th lm gim nhy ca phng php phn tch hng trm
ln, thm ch c khi n ngn ln.
V th trong nhiu trng hp ngi ta phi chn nhng iu kin nguyn t ha mu
ph hp loi tr s xut hin cc hp cht cacbua, hoc thm vo mu cc cht chy nh
NH4NO3, LiBO2 Vi nng thch hp hn ch vic tip xc ca cht mu vi cacbon,
hoc tin hnh cacbua ha b mt cuvet graphit trc bng mt hp cht cacbua bn, sau
mi a mu vo nguyn t ha hoc t mu trong thuyn Ta trong cuvet.
f. S kh xit kim loi bi cacbon. Trong cuvet graphit, di tc dng ca nhit, mt s
hp cht mu cng c th b kh bi cacbon ca cuvet. Phn ng ny rt phc tp v n cng
ph thuc vo cc yu t nh trong qu trnh hnh thnh cc hp cht cacbua kimloi.
thi
tc ca
phn
ngkh ny cn
ng
phthucvo p sut
ring phn ca nguyn t cacbon trong cuvet v kh tr lm mi trng nguyn t ha mu.

Phn ng ny thng din bin theo hai loi:
(m) MxOy(r,l) + C(r) ^ Mx(r,l) + CO
(n) MxOy(k) + C(k) ^ xM(k) + CO
Trong hai loi phn ng ny, loi qu trnh (m) thng d xy ra v chim u th hn v
trong nhng trng hp ca cc oxit bn nhit, th qu trnh ny li lm cho vic nguyn t
ha mu c th tt hn. Sau y l mt vi v d v cc phn ng kh cc oxit:
NiO(4) + C ^ Ni(r,l)
--------------------- Ni(k)
PbO(r) + C Pb(r,l) +OC
--------------------->Pb(k)
Cc hp cht oxit CaO, Cr 2O3, MoO3, ZnO, CdO, CuO,.. thng xy ra theo kiu c ch
ny.
Trn y l minh ho cc qu trnh c th xy ra trong cuvet graphit. Tt nhin l c tnh
cht khi qut, nn khng phi lc no, trong mi loi mu u c cc qu trnh , m
trong thc t din ra cuvet graphit c s chn lc, c s tng tc ln nhau v ng thi
cng c s loi tr nhau. Trong , qu trnh chim u th hn l ph thuc vo nhiu yu t,
nh:
+ Nhit t nng cuvet (y l yu t quyt nh);
+ Bn cht ca nguyn t v hp cht m n tn ti trong cuvetl
181
+ Thnh phn ca mu phn tch, c bit l nguyn t c s (nn);

+ Trng thi b mt v loi cuvet graphit;
+ Mi trng kh tr tin hnh nguyn t ha mu;
+ Cui cng l cht ph gia c thm vo mu.
Chnh do c nhng quan h ph thuc ny, m chng ta c th iu chnh v
khng ch cho mt qu trnh no u vit s xy ra, cn qu trnh no khng c li
s c hn ch hay loi tr.
H thng trang b nguyn t ha mu theo k thut khng ngn la bao gm
hai phn chnh:
B
phn
ng
mu
nguyn t ha. chnh l

cc loi cuvet graphit, cc
graphit,
hay
thuyn
tantan,
hay l cc loi filamen cha

mu.
Trong
cc
loi
ny,
cuvet graphit c dng ph

bin nht v tt nht l cuvet
graphit
hot
ha
nhit luyn ton phn. V loi

ny th mi hng ch to my
o ph hp th nguyn t
cng c nhng loi c hnh
dng v kch thc ring cho
my ca h (hnh 8.26).
Phn th hai l ngun nng lng nung nng cuvet v gi cuvet.
Phn ny bao gm b chng trnh iu khin theo bn giai on (bn phase) sy, tro
ha, nguyn t ha v lm sch cuvet theo nguyn l ca php o v ngun nng lng c
cng sut cc i l c 3,5 - 7,5 KVA cung cp nng lng cho qu trnh nguyn t ha
mu.
N thng l ngun
nng lng in c dng rt cao (thay
600 A), nhng th rt thp (di 12 V).
182
i c t 50 n
Hnh 8.26b
H thng nguyn t ha mu trong ngn la (Philips Pye Unicam)
Ti u ha cc diu kin cho php o khng ngn la mu.

N c nghin cu k trn. Do y ch nu li mt s iu cn ch . C th
vi php o ETA-AAS bao gm nhng iu kin:
Cc iu kin nguyn t ha mu:
+ Thi gian, nhit nung nng cuvet ca cc giai on sy mu, tro ha luyn mu v
nguyn t ha o cng vch ph,
183
+ Kh mi trng cho qu trnh nguyn t ha mu (tc , loi khi)

+ Cng sut, tc t nng cuvet graphit nguyn t ha mu;
+ iu kin lm sch cuvet graphit;
+ Lng mu v cch a vo cuvet nguyn t ha cho php o.
Cht nn ca mu phn tch v cc mu chun cn phi c pha ch v chun cho ng
nht.
Mi trng axit v loi axit pha ch mu v lm mi trng cho dung dch mu chun
v mu phn tch.
Cc yu t nh hng sau y cng cn c xem xt.
Trong mt php o c th cc yu t nh hng cn phi xem xt l:
+ Cc nh hng v ph;
+ Cc nh hng v vt l;
+ Cc nh hng ha hc ca cc Cation v Anion c trong mu;
+ V nh hng ca thnh phn nn ca mu.
184
Chng 9
TRANG B CA PHP O ASS
Ngun pht bc x n sc
Mun thc hin c php o ph hp th nguyn t ngi ta cn phi c mt ngun
pht tia bc x n sc (tia pht x cng hng) ca nguyn t cn phn tch chiu qua mi
trng hp th. Ngun pht tia bc x n sc trong php o ph hp th nguyn t thng l
cc n canh rng (HCL), cc n phng in khng in cc (EDL) v cc n ph lin tc
c bin iu ( c n sc ha). Nhng d l loi no, ngun pht tia bc x n sc trong
php o ph AAS cng phi tha mn c nhng yu cu ti thiu sau y mi c th chp
nhn c.
Ngun pht tia bc x n sc phi to ra c cc tia pht x nhy (cc vch pht x
nhy, c trng) ca nguyn t cn phn tch. Chm tia pht x phi c cng n nh,
phi lp li c trong nhiu ln o khc nhau trong cng iu kin, phi iu chnh c vi
cng mong mun cho mi php o.
Ngun pht tia bc x phi cung cp c mt chm tia pht x thun khit ch bao
gm mt s vch nhy c trng ca nguyn t phn tch. Ph nn ca n phi khng ng
k. C nh th mi hn ch c nhng nh hng v vt l v v ph cho php o AAS.
Chm tia pht x n sc do ngun cung cp phi c cng cao, nhng li phi
bn vng theo thi gian v phi khng b cc yu t vt l khc nhiu lon, t b nh hng bi
cc dao ng ca iu kin lm vic.
Ngun pht tia bc x n sc phi bn lu, khng qu t tin v khng qu phc tp
cho ngi s dng.
Tt nhin trong 4 yu cu trn th 3 yu cu u tin l quan trng nht v bt buc phi
tha mn, cho php o t kt qu chnh xc, n nh v tin tng. Ring yu cu th 4 th
c th chnm chc c trong nhng trng hp c th nht nh.
Xut pht t nhng nhim v v yu cu phi tha mn, hin nay trong php o ph hp
th nguyn t, ngi ta thng dng ch yu ba loi ngun pht tia bc x n sc. l:
+ n catot rng (HCL - Hollow Cathode Lamp),
185
+ n phng in khng in cc (EDL- Electrodeless Discharge Lamp),

+ n pht ph lin tc c bin iu (D 2-lamp, W-lamp).
+ Cc loi ngun n sc khc.
Trong ba loi , n HCL c dng ph bin nht. n pht ph lin tc mi c
pht trin v s dng trong vi nm nay, nhng li c nhiu u vit trong cc my nhiu knh
v qu trnh phn tch t ng lin tip nhiu nguyn t, tuy nhin gi thnh cn t v
nhy cn km nn cha c dng ph bin.
n catot rng (HCL)
n pht tia bc x n sc c dng sm nht v ph bin nht trong php o S l
n catot rng (HCL). n ny ch pht ra nhng tia pht x nhy ca nguyn t kim loi lm
catot rng. Cc vch pht x nhy ca mt nguyn t thng l cc vch cng hng. V th
n catot rng cng c gi l ngun pht tia bc x cng hng. N l ph pht x ca cc
nguyn t trong mi trng kh km.
V cu to, n catot rng gm c ba phn chnh:
Phn 1 l thn n v ca s,
Phn 2 l cc in cc catot v anot, v
Phn 3 l kh cha trong n. l kh tr He, Ar hay N 2.
Thn v v. Thn n gm c v n, ca s v b cc in cc anot v catot. B
bng nha PVC. Thn v v n bng thu tinh hay thch anh. V n c hai dng (hnh 9.1).
Ca s S ca n c th l thu tinh hay thch anh trong sut trong vng UY hay VIS l
ty thuc vo loi n ca tng nguyn t pht ra chm tia pht x nm trong vng ph no.
Ngha l vch pht x cng hng o ph hp th vng no th nguyn liu lm ca s S
phi trong sut vng .
in cc. in cc ca n l catot v anot. Anot c ch to bng kim loi tr v bn
nhit nh W hay Pt. Catot c ch to c dng hnh xylanh hay hnh ng rng c ng knh
t 3 - 5 mm, di 5 -6 mm v chnh bng kim loi cn phn tch vi tinh khit cao (t nht
99,9 %).
Dy dn ca catot cng l kim loi W hay Pt. C hai in cc c gn cht trn b
ca thn n v cc catot phi nm ng trc xuyn tnm ca n (hnh 9.1). Anot t bn
cnh catot hay l mt vng bao quanh catot. Hai u ca hai in cc c ni ra hai cc gn
cht trn n, cm vo ngun in nui cho n lm vic. Ngun nui l ngun 1 chiu c
th 220-240 V.
Kh trong n. Trong n phi ht ht khng kh v np thay vo l mt kh tr vi p
sut t 5 - 15 mHg. Kh tr l argon, heli hay nit nhng phi c sch
186
cao hn 99,99 %. Kh np vo n khng c pht ra ph lm nh hng n chm

tia pht x ca n v khi lm vic trong mt iu kin nht nh th t s gia cc
nguyn t b Ion ha v cc nguyn t trung ho phi l khng i. C nh th n
lm vic mi n nh.
Ngun nui n. n c t nng pht ra chm tia pht x cng hng
nh ngun in mt chiu n nh. Th lm vic ca n HCL thng l t 250 220V ty thuc vo tng loi n ca tng hng ch to v ty thuc vo tng nguyn
t kim loi lm catot rng.
Cng lm vic ca cc n catot rng thng l t 3- 50 ma v cng ty
thuc vo mi loi n HCL ca mi nguyn t do mi hng ch to ra n.
Th v cng dng in lm vic ca n HCL c lin quan cht ch vi cng
tch kim loi ra khi b mt catot rng to ra hi kim loi sinh ra chm tia pht
x ca n HCL.
Dng in qua n
HCL ca mi nguyn t
rt khc nhau. Mi n
HCL u c dng in
gii hn cc i m n
c th chu ng c v
gi
v
tr
n.
ny
Tt
nhin
c
khi
ghi
s
Cu
trn
to
ca
Hnh
n
catot
9.1
rng
dng khng bao gi c

php dng n dng in cc i , m thch hp nht l trong vng t 65 - 85 % gi tr cc
i, v iu kin dng cc i n lm vic khng n nh v rt chng hng, ng thi
php o li c nhy v lp li km.
Theo l thuyt v thc nghim ca thc t phn tch theo k thut o ph hp th nguyn
t, tt nht ch nn dng cng dng trong vng t 60 - 85 % dng gii hn cc i ghi
trn n HCL.
Mun c nhy cao, nn s dng cng dng gn gii hn di. Mun c n
nh cao, nn dng cng dng gn gii hn trn. Nhng nn nh rng cng dng
lm vic ca n HCL v cng ca vch ph hp th c quan h cht ch vi nhau.
Ni chung, nhiu trng hp cng ca vch ph hp th l t l nghch vi cng
dng in lm vic ca n HCL (hnh 9.2), tuy nhin cng c vi trng hp khng tun
theo quy lut .
187
Quan h gia cng vch ph v cng dng in lm vic ca n HCL

(A) l trng hp ph bin (Cd-228,8 nm), Cu, Ca, Fe; (B) l ca Pb 283,3 nm, c
bit;
(C) l ca Al 309,3 nm, c bit.
Khi n lm vic, catot c nung , gia catot v anot xy ra s phng in lin tc.
Do s phng in m mt s phn t kh b Ion ha. Cc Ion va c sinh ra s tn cng
vo catot lm b mt catot nng v mt s nguyn t kim loi trn b mt catot b ha hi
v n tr thnh nhng nguyn t kim loi t do. Khi di tc dng ca nhit trong n
HCL ang c t nng , cc nguyn t kim loi ny b kch thch v pht ra ph pht x
ca n. chnh l ph vch ca chnh kim loi lm catot rng. Nhng v trong iu kin c
bit ca mi trng kh tr c p sut rt thp, nn ph pht x ch bao gm cc vch nhy
ca kim loi m thi. chnh l s pht x ca kim loi trong mi trng kh km. Chm
tia pht x ny l ngun tia n sc chiu qua mi trng hp th thc hin php o AAS.
Cc n catot rng c cu to nh m t trn l nhng n HCL n nguyn t,
ngha l mi n HCL ch phc v cho phn tch mt nguyn t. Ngy nay ngoi cc n
HCL n, ngi ta cng ch to c mt s n kp i, kp ba hay kp su nguyn t.
V d cc n kp i l (Ca+Mg), (Cu+Mn), (Cu+Cr), (Co+Ni), (K+Na), (Cu+Pb); cc n
kp ba nh (Cu+Pb+Zn) v n kp su l (Cu+Mn+Cr+Fe+Co+Ni).
ch to cc n kp ny, catot ca n HCL phi l hp kim ca cc nguyn t .
Hp kim ny phi c thnh phn ph hp, sao cho cng pht x ca cc nguyn t l
gn tng ng nhau; ngha l s pht x ca kim loi ny phi khng c ln t s pht x
ca nguyn t kia. Do phi ch to trong iu kin dung ha cho tt c cc nguyn t. V
d: n HCL kp su ca Cu, Mn, Cr, Fe, Co, v Ni th hp kim lm catot rng phi cha
25% Cu, cc nguyn t khc c thnh phn l 15%.
188
Xt
nhy,
ni thch
chunganh
ccchu
n nhit,
kp thng
cm,
nhy
km knh
hn cc
tng
Thnvn:
Mt ng
di 18c
- 15
ng
6 - 5n
cm.n
Mt
u
ng,n
hayEDL
tt nht
ch s
gnS.bng
Mt khc,
vqua
chcng
to li
khtrong
khnsut
hnvi
nchm
n.
ca
cngcng
c ca
Ca l
s cng.
cho chm
sng i
phi
V th.cng ch c mt s t n kp v cng ch c dng trong mt s trng hp khi vic
sng
thay i
n ng
c nh
hng
qu trnh
phn ng.
tch vCun
trongcm
cc c
my
nhiu
th n
HCL
Ngoi
thch
anh n
l cun
cm bng
cng
sutknh
t 800
- 400
W
kp
l
u
vit
hn
n
n.
ty loi n ca tng nguyn t, v c ni vi ngun nng lng cao tn HF ph hp
nn
HCL
lmlm
vic
ti (hnh
mi ch
Ngoi
dng nht
cho nhit.
chm sng pht x c cng
nui cho
EDL
vic
9.4).
cngnh
l vth
tschu
nht
nh.
Cht
trong n l vi miligam kim loi hay mui kim loi d bay hi ca nguyn t
Mi
s lm
dao sao
ngkhi
vton
dngbin
nh hi
hng
ca
phn tch,
chtlm
havic
hi ca
bo n
mu
cho lm
p sut
ca n
kimcng
loi trong
chm
tia sng
x
(hnh
9.2).
Do oCltrong
mitphp
o mmHg.
c th phi chn mt gi tr cng
n
iu
kinpht
nhit
t 800
- 550
khong
1 - 1,5
dng
in
phthay
hpcho
v gi
ctrong
nh trong
sut qu
trnh
o nh
mt nguyn
t.x ca
Cht
ny
catot
n HCL,
n l
ngun
cunglng
cp chm
tia pht
n phng
intch,
khng
ccb(EDL)
nguyn
t phn
khidin
chng
kch thch, trong qu trnh n EDL hot ng.
Kh trong
n EDL
ht ht khng kh v npthhai
thay vo
l mt
Ngun
phtn.
tia Trong bc
x cng
n phisc
cdng
kh
trphp
Al, He hay Nit c po
sutph
thp,hp
vi mmHg
trong
th khi u cho s lm vic ca n EDL.
nguyn
t l nui
n phng
in
khng
in
cc.lng cao tn nui n EDL lm vic c ch
Ngun
n lm
vic.
Ngun
nng
to theo
hain
tnny
s. Tn
sng
v tnv
s cung
sng cp
raiochm
27,12tiaMHz,
sut
Loi
cngsnh
nngn
HCL450
uMHz
c nhim
pht c
x cng
c trng
di
1 kW. t phn tch, c bit l cc kim, th n EDL cho nhy cao hn, n nh hn
ca nguyn
n HCL.
Bng 9.1
9.3lng
l nhng
d in
v iu
. hai tn s khc nhau nn n EDL
Do ngun
nuivlhnh
nng
cm vng
t vi
cng
Bng c
9.1 chia thnh hai loi: 1. n EDL sng ngn, ngun nui tn s 450 MHz, v 2. n
EDL
sng
sng
raio
MHz.
So snh
raio,
nhy ngun
v giinui
hn tn
phtshin
ca
n27,12
HCI v
EDL
Nguyn t
nhy (pl/mL)
Gii hn pht hin (pl/mL)
HCL
EDL
HCL
EDL
As-193,70
1,10
0,80
0,80
0,400
Cd-228,80
0,03
0,02
0,01
0,008
Pb-283,20
0,10
0,07
0,05
0,030
Hg-253,60
6,00
4,50
0,50
0,200
Sn-286,30
2,50
1,60
0,20
0,100
Zn-213,90
0,03
0,02
0,02
0,018
V cu to, n EDL thc cht cng l mt ng phng in trong mi trng kh km c

cha nguyn tcn phn tch vi mt nng nht
nh ph hp to ra
c chm tia pht x ch bao gm mt s vch ph nhy c trng ca nguyn t phn tch.
Hnh 9.3
n EDLn
cng
gmin
cckhng
b phn:
phng
in cc
190
189
191
Cng vch ph v vng tuyn tnh ca As-193,7 v Se-196,1 i vi hai loi n

HCL v EDL. Khi n lm vic, di tc dng ca nng lng cao tn cm ng n c nung
nng
, kimloi hay mui
kim loitrong
n c ha hi v b
nguyn t ha. Cc nguyn t t do c sinh ra s b kch thch v pht ra ph pht x ca

n trong iu kin kh km di tc dng nhit khi n lm vic. chnh l ph vch ca
kim loi cha trong n EDL.
Ngoi u im v nhy v gii hn pht hin, n EDL ca cc kim hay bn kim
thng c bn cao hn n HCL. ng thi vng tuyn tnh ca php o mt nguyn t
khi dng n EDL thng rng hn so vi vic dng n HCL (hnh 9.4).
Ngy nay cc hng sn xut my o ph hp th nguyn t sn xut c n 30 loi
n EDL cho 30 nguyn t. Nhng tt v c dng nhiu ch c 12 nguyn t kim v bn
kim l As, Bi, Cd, Hg, P, Pb, Se, Sn, Te, TI v Zn. Cc n EDL ca cc nguyn t ny u
c bn theo cc my ca hng. Nhng n EDL ca cc nguyn tkhc cnli t c
dng, v n khng
u vithn nHCL, m gi
thnh li t hn.
Ngoi n catot rng v n phng in khng in cc, ngi ta cng ch to ra
c nhiu loi n pht tia bc x n sc ca cc nguyn t, nh n catot rng cng
cao (trnh intensity cmiss Ion lamp - HIEL), n gradient nhit (controlled temperaturegradient lamp - CTGL), n phng in c chi sng cao (glow- discharge lamp - GDL).
Cc loi kin ny c u im hn n HCL mt cht v nhy, v vng tuyn tnh, v gii
hn pht hin. Nhng cc n loi ny li kh ch to v t tin, mt khc li km bn vng.
V th n t c dng v khng c bn ngoi th trng, ch yu ch c ng trong
nghin cu l thuyt v ph.
n ph lin tc c bin iu
Trong khong vi nm li y, mt loi ngun pht x ph lin tc cng c dng lm
ngun pht bc x cng hng cho php o AAS. l n hydrogen nng (D 2-lamp), cc
n xenon p sut cao (Xe-lamp), cc n hot ca kim loi W. l cc loi n pht ph
lin tc trong vng t ngoi v vng kh kin (UV-VIS). Cc tc
192
gi Fassel, Ivanop, Gibson, Mc G, Winerfordner l nhng ngi u tin nghin cu v s

dng cc loi n ny lm ngun pht bc x cng hng cho php o AAS.
n ny tuy pht ra ph lin tc, nhng nh h thng bin iu v h lc giao thoa, nn
chm sng pht x b bin iu v lng t ha thnh chm sng khng lin tc c ph
dng rng ca, mi rng ca cch nhau 0,2 nm, nn mi rng ca c coi nh l 1 tia n
sc. Hnh 9.5 l mt v d v h my o ph hp th nguyn t dng ngun sng bc x lin
tc. Trong ngun sng c t trc h thng bin iu v b lc giao thoa. Chm sng
ny khi i qua h thng bin iu v b lc giao thoa s b bin iu theo nhng di sng
nht nh dao ng vi bin nh nhau. Sau cng c chiu vo mi trng hp th l
ngn la hay cuvet graphit. Cc nguyn t t do trong mi trng hp th s hp th mt
phn nng lng ca chm sng ng vi mt di bin iu A, ca vng ph. Phn cn li s
i vo b n sc v detector pht hin v o cng sau khi qua b khuych i bng
sng theo di ph ca n nn li tn s. Tip cng vch ph hp th cng c o
v ch th theo cc cch bit, nh hin s digital, ghi pic trn recorder, hay dng printer in
ln bng giy.
Hnh 9.5
H thng my AAS dng ngun ph lin tc
1- Ngun ph lin tc; 2- H thng bin iu v lc giao thoa; 3- B phn nguyn t ha mu;
4- B n sc v detector; 5- B nn v khuych i tn hiu o
AAS.
Ngun pht ph lin tc c u im l d ch to, r tin v c bn tng i
193
cao, v ch cn mt n c th thc hin c php o AAS i vi nhiu nguyn t trong

mt vng ph UY hay VIS. Do n rt u vit i vi cc my ph hp th nhiu knh v
xc nh ng thi hay lin tip nhiu nguyn t trong cng mt mu phn tch, m khng
phi thay n HCL cho vic o ph mi nguyn t. Vi n ny, vng tuyn tnh rng, li
khng c hin tng t hp th ring (t o). Song v n sc v chn lc hay
nhy, th ni chung trong nhiu trng hp cn km cc n HCL hay n EDL nhng li u
vit v d dng i vi qu trnh phn tch t ng hng
ph hp
lot
trong cc my
thnhiuknh. Chnh v th
m trong
khong nm nm li y cc loi n ph lin tc c pht trin, ci tin v bt u

c s dng rt nhiu trong php o AAS v nhiu h thng my o ph hp th vi ngun
pht ph lin tc cng c bn trn th trng th gii.
Cc loi ngun n sc khc
Ngoi ba loi ngun pht bc x n sc ch yu c trnh by trn, trong php
o ph hp th nguyn t, ngi ta cng s dng mt vi loi ngun pht tia bc x n sc
khc na nh n catot rng c di cao, ng pht x c bit, tia laze. Nhng nhng loi
ny ch ch yu dng trong nghin cu l thuyt vt l.
nguyn t ha mu, trong php o ph hp th nguyn t ngi ta thng dng hai
k thut khc nhau. l k thut nguyn t ha bng ngn la ca n kh v k thut nguyn
t ha khng ngn la. ng vi hai k thut nguyn t ha c hai loi dng c nguyn
t ha mu.
K thut ngn
la. H thng
nguynt ha mu
bng ngn la
gm hai phn
chnh:
+ Bung aerosol ha (Nebulizer system), to th si kh mu,
+ n nguyn t ha mu (burner head).
Kh to ra ngn la nguyn t ha mu thng hay c dng l hn hp ca
cht kh (1 cht oxy ha v 1 cht chy), v d nh hn hp khng kh nn vi axetylen hay
kh N2O vi kh axetylen. i khi cng dng hn hp ca kh hydro vi axetylen hay khng
kh v kh propan.
H thng nguyn t ha khng ngn la. H thng ny gm ba phn chnh l:
+ Cuvet graphit hay thuyn Ta cha mu, nguyn t ha.
+ Ngun nng lng nung cuvet hay thuyn Ta.
+ B iu khin thc hin vic nguyn t ha mu theo cc giai on ca mt
chng trnh ph hp.
Nguyn l cu to, qu trnh hot ng ca cc loi trang b nguyn t ha mu
c m t chi tit trong chng 8 v k thut nguyn t ha mu.
194
H thng n sc v my quang ph hp th nguyn t

H thng n sc chnh l h thng thu, phn li, chn v pht hin vch ph hp th
cn phi o. Trong php o ph hp th nguyn t h thng n sc ny l mt my quang
ph c phn gii tng i cao c th l h my mt chm tia hay h my 2 chm tia. Cu
to ca n gm ba phn chnh:
H chun trc, chun trc chm tia sng vo;
H thng tn sc (phn li) phn li chm sng a sc thnh n sc;
H bung ti (bung nh) hi t, hi t cc tia cng bc sng li.
c trng cho h quang ca my AAS l cc thng s.
+ tn sc gc;
+ tn sc di;
+ phn gii (tn sc);
+ Vng ph lm vic ca h.
Bn thng
s
ca
ny
cng l cc
yu t xem xt cht
lng
mtmy quang
ph AAS.
Trc h chun trc l khe vo ca chm sng a sc v sau h bung nh l khe ra ca
chm tia n sc cn o. Hnh 3.6 l s quang hc, nguyn tc ca h thng my quang
ph hp th nguyn t. Theo s ny, chm tia pht x cng hng ca nguyn t cn
nghin cu c pht ra t n catot rng sau khi qua mi trng hp th, s c hng vo
khe my v vo h chun trc, ri vo b phn tn sc, vo h hi t chn 1 tia cn o.
Nh vy chm sng a sc c chun trc, c phn li v sau ch mt vch ph cn o
c chn v hng vo khe o tc dng vo nhn quang in (detector-photomultiveler)
pht hin v xc nh cng ca vch ph hp th .
Mun h thng
my quang ph hp thnguyn
t cho c kt qu tt th h
thng tn sc phi bo m c mt s yu cu bt buc sau y:

N phi c tn sc ln c th tch v c lp c tt cc vch ph
cn o, trnh s quy ri, s chen ln ca cc vch ph khc bn cnh. Trong cc my hin
nay, b phn ny thng l mt h ccht c hng s t 1200
n 2400
vch/mm.
Phi khng gy ra bt k mt hin tng sai lch no lm mt nng lng ca chm
sng trong my, nh s hp th, s tn x, s khuych tn ca cc b phn cu to thnh
my. c bit l cc h thng gng, cc thu knh, khe vo, khe ra ca chm sng. Cc thu
knh phi trong sut trong vng ph lm vic ca my.
Khe vo v khe ra ca my phi c m chnh xc v phi iu chnh c cho ph
hp vi tng vch ph v c lp li cao trong mi php o.
195
Detector pht hin cng vch ph phi c nhy cao. C nh th mi c th

pht hin c s thay i nh trong qu trnh hp th ca vch ph ca mi nguyn t. l
cc iu kin ti thiu ca h quang hc trong my ph hp th nguyn t. Vi s pht trin
ca khoa hc v k thut, ngy nay ngi ta c th tha mn c tt c cc yu cu . Chnh
v th hin nay c rt nhiu my o ph hp th nguyn t c cht lng cao c bn
trn th trng quc t. l cc my o ph hp th nguyn t ca hng Perkin Elmer,
Varian, Becman, Philips Pye Unicam, Wet Zeiss, Shimadu, Instr, Lad, Alpha,...
Hnh 9.6
S quang hc ca h thng my AAS
(1)- Loi 1 chm tia; (2)- Loi 2 chm tia; V d v 1 h my AAS ca hng
196
Perrkin Elmer
Trang b pht hin, Detector, Photomultivlier
Detector l mt loi dng c quang hc dng thu nhn v pht hin tn hiu quang
hc theo hiu ng quang in ca n. Trc y thu nhn cng ca chm sng ngi
ta thng dng knh nh hay phim nh sau l t bo quang in. l cc dng c c in
c nhy km, nht l knh nh, v knh nh c nhiu nhc im, nh kh bo qun, d b
nh hng bi m, nhit , thi tit. Mt khc, n li l mt dng c trung gian thu
nhn chm sng v sau phi x l tip mi c c cng vch ph. Tc l o en
ca knh nh b chm sng tc dng vo. Vi s pht trin ca khoa hc v k thut, ngy
nay ngi ta ch to ra c nhiu loi detector quang hc kiu ng c th khuych i tn
hiu o ln c n c triu ln. l cc ng nhn quang in (photomultivler tube). Hnh
9.7 l s ca mt nhn quang in kiu ng .
Nhn quang in kiu ng l mt loi dng c thu nhn tn hiu quang hc c tnh
cht vn nng, n c nhy v chn lc cao. Nhiu hng ch to c cc detector
loi ny. Vng ph hot ng ca cc detector kiu ng loi ny thng l t 190 - 900 nm,
c khi n 1100 nm. Tt nhin l thng s ny ph thuc vo bn cht ca nguyn liu ch
to bn catot ca n.
Hnh 9.7
H s khuch i ca loi detector ny thng n 106, i khi c loi n 107.
Nguyn liu ch to bn catot ca cc detector kiu ng l cc hp kim ca cc kim loi
kim vi Sb, Ga hay As, v d hp kim Cs-Sb; Ga-As; Na-K-Cs-S (hnh 9.8).
197
9.5 K thut o cng vch ph hp th

Cng ca cc vch ph hp th sau khi c detector pht hin v khuych
i s c a sang h thng ch th kt qu. y n c th c khuych i tip
v x l c c cng thc ca vch ph hp th. n nay ch th (biu th)
cng ca vch ph hp th nguyn t, c nhiu cch khc nhau t n gin n
tinh vi phc tp. Sau y l mt vi k thut v ang c s dng trn cc my o
ph hp th c bn trn th trng quc t.
Thang o mt quang (thang o
nng lng hp th ca vch ph).
y l mt phng php n gin
nht v c dng t khi my quang
ph hp th nguyn t mi ra i.
Theo cch ny, cng ca vch
ph hp th c biu th theo thang
o mt quang D. Thang o ny
c cu to v phn chia theo quy
lut ca thang logarit ca t s gia
cng tia sng i vo v i ra khi
mi trng hp th.
Nh vy, im gc ca thang o s c mt quang D = 0, ngha l khng c s hp
th. im cui ca thang o l im c hp th l 100%, ngha l D = 2. Trn tt c cc
my hin nay u c thang o ny. Cc gi tr D c c trc tip trn thang o theo lch
ca kim in k ch nng lng hp th E ca vch ph.
Phng php hin s (digital) ch hp th ca vch ph. y l mt k thut biu th
cng vch ph cng ang c dng hin nay. Cc s o hin trn mn digital ch trc
tip nng lng hp th ca vch ph cn o. Cng tng t nh thang o mt quang D,
cc s o ny cng t l vi nng ca nguyn t trong mu theo phng trnh c bn ca
php o AAS. Ngy nay tt c cc my o ph hp th nguyn t u c b phn ch th
cng vch ph theo nguyn tc ny. N c tn l b Readout. B Readout ca cc my
thng c 4 hng s l t 0 n + 9999.
Ghi cng vch ph dng pic. Cng ca vch ph hp th c th c a
sang my ghi (Recorder) ghi li di dng cc lc. S o cng vch ph lc ny c th
c tnh theo chiu cao ca lc hay din tch ca lc. V trong mt gii hn nht nh nng
C ca nguyn t phn tch chng ta lun lun c quan h:
H = kC
hay l
S = kC
Trong H l chiu cao v S l din tch ca lc. Cn k l mt h s t l. Hnh 9.9 l

mt v d v cc lc ca vch ph hp th vi cc nng khc nhau.
198
detector,
x lqua
theovic
cc o
yugi
cutrHthay
ra v
ta
chcng
theo mt
nht
nh ca
s o
Nhnvy,
S sau
chng
dngcch
c
ng
chun
v
cng
vch
nh
ghi bit
chiutheo
cao hay
lc,hp
hoc
hin s
trnCc
mnmy
vi deo.
xc nh
cph,
nng
printer,
C x cha
mt din
cchtch
ph
tng
ng.
o
V
yth
l k
thut vn
nngnay
nht.
phth
hp
nguyn
t hin
u c u sang my t ghi th o 0 - 10 mV v
a raTrn
b intergrator
0 - 1 V.
y l cc t
phng
php ang c dng ch th cng ca vch ph.
Phng
php
in my
trc
Hin
nay, cc
h thng
o ph hp th nguyn t bn trn th trng quc t u c
tipccgi
o bng
myphinnh th. Song chng ta c th s dng ng thi, hay chn
cchtro cng
vch
(printer).
mtthuc
k vo
thut
mt
k thuty
no l
l ty
mc trang b hin c ca tng phng th nghim v tng
hin i,
nhanh
v nhng
tin li.
cn thit nht nh cho ph hp. Nhng mun c c
ngi
nghin
cu c
yu cu
yqu
ccng
s n
o v
cng
kt
chnh
xc,vch
ngoi vic c c trang b hin i, cn phi c con ngi c
ph
hp
th
c
in
ngay
trn
kin thc v hiu bit chnh xc v php o AAS; Nh th mi lm ch c trang b phc v
bngcng
giy
nh
mycu
in ca
(printer)
cho
vic
nghin
mnh.
theo tng ln o v sau c
gi tr trung bnh ca n ln o.
y l k thut mi c pht
trin. Do ch nhng my o
ph hp th nguyn t hin i
mi c u a tn hiu ra
ch th theo cch ny. Bng 9.2
l mt v d v cch o ny.
Bng 9.2
V d v bng kt qu o ph ca mu (trch trong Report 09/20 - hng Philips)
Sample ID
Cu Abs
Cu Conc.
Fe Abs
Fe Conc.
Al Abs
Al Conc.
Saple 1
0.4583
2.9201
0.1523
2.1677
02085
29.6433
Saple 2
0.6738
4.3051
0.2003
2.8481
0 1128
16.0784
Saple 3
0.2856
1.8102
0.3589
5.0961
0 3789
53.7964
Saple 4
0.4126
2.6220
0.4126
5.8566
0 4055
57.5667
Saple 5
0.4933
3.1453
0.1855
2.6383
0 2369
33.6688
Saple 6
0.6337
4.0475
0.3333
4.7333
0 1278
18.2046
Saple 7
0.8568
5.4806
0.3725
5.2889
0 3014
42.8112
Microcomputer v mn video. y l mt k thut ch th s o hin i nht hin nay,

nhanh v tin li. Cc my o ph hp th nguyn t hin nay u c u ghp vi b
phn ny. Microcomputer l trung tnm ch huy ton b mi hot ng ca h thng my AAS,
iu khin mn video ch th cc thng s nghin cu v cc kt qu o c t ra theo
mt chng trnh nht nh. Microcomputer nhn s o t
200
199
Chng 10
CC YU T NH HNG TRONG AAS
Khi qut chung

Cc yu t nh hng n kt qu phn tch trong php do ph hp th nguyn t rt a
dng v phc tp, c khi xut hin v cng c khi khng xut hin, c nh hng hay khng
l ty thuc vo thnh phn ca mu phn tch v matrix ca n. Nhng nghin cu mt
cch ton din, chng ta im qua tt c cc yu t nh hng c th c trong php o ny.
Cc yu t c th c chia thnh 6 nhm sau:
Nhm l: Cc thng s ca h my o ph. Cc thng s ny cn c kho st v chn
cho tng trng hp c th. Thc hin cng vic ny chnh l qu trnh ti u ha cc thng
s ca my o cho mt i tng phn tch.
Nhm 2: Cc iu kin nguyn t ha
nhau ty thuc vo k thut c chn thc
mu. Cc yu t ny th hin rtkhc

hin qu trnhnguyn t ha mu v n
c nghin cu k trong chng II.

Nhm 3: K thut v phng php c chn x l mu. Trong cng vic ny nu
Do kt qu phn tch thu c khng ng vi thc t ca mu. V th, vi mi mt loi
chng ring.
Mt s nh hng trong php do AAS
Cc yu t v ph
S hp th nn
201
Yu t ny c trng hp xut hin r rng, nhng trong nhiu trng hp khng

xut hin. iu ny ph thuc vo vch ph c chn o nm trong vng ph no.
Ni
chung,
trong
vng
kh kin th yu t ny th
hin r rng. Cn trong vng
t ngoi th nh hng ny t
xut hin, v ph nn trong
vng t ngoi yu. Hn na,
s hp th nn cn ph thuc
rt nhiu vo thnh phn nn
ca mu phn tch, c bit l
matrix
ca
mu,
ngha
nguyn t c s ca mu. V
d: Khi xc nh Pb trong
mu sinh hc bng php o
ngn la th s hp th nn l
khng
ng k, nhng
khi xc nh Pb trong
nc
bin (nn
2,9% NaCl) th nh
hng ny l v cng ln (hnh 10.1).

Do , trong mi trng hp c th phi xem xt tm bin php loi tr.
loi tr ph nn, ngy nay ngi ta lp thm vo my quang ph hp th nguyn t h
thng b chnh nn.
Trong
ngi
ta
h
dng
thng
n
ny
hydro
nng (D2-lamp) b chnh

nn trong vng t ngoi v
dng n W (W-habit lamp)
cho vng kh kin. Do ,
trong mi php o xc
nh mt nguyn t chng ta
c th thc hin b chnh
nn hay khng l ty thuc
vo yu t c nh hng
hay khng. Hn na, ngy
nay ngi ta dng c hiu
ng
Zeeman
nn.
thut
b
ny
chnh
khng
nhng b chnh c nn c
hiu
qu
cao
hn
10.2b), nht trong cc mu
202
(hnh
nng
mui
nnln,
mgy
cnratng
csaisnhy
o cng
ln nhiu
hiuthc.
ng
hp th
gi, do
cng
nhng
cho ca
kt php
qu o
ln,
vchvph
Zeeman
dng
cng
khng
ca vch
phchiu
hp th
t ca
cc nguyn
K
Yu t c
nytcth
hinlm
rttng
r khi
chn
ng
caonguyn
ca n
nguyn
t ha t.
mu
thut
b hn
chnh
thkh
ba chy
l dng
n HCL
ng
chdo
thnh
k tip:
ch ca
dng
thp kh
(o
v khi
hp
khng
c hot
t chy
tt,haihay
phn
hn hp
tn
hiu
hp th
tng)
chhp
dng
caol(ch
hp th nn). Hiu gia 2 ln o
chy
khng
c
chnvph
(thng
quodcng
axetylen).
l tn hiu
hp
th
cat vch ph. Cch b chnh ny tuy c tin hn, v ch cn 1 n
10.2.2
Cc
yuthc
t vt
HCL, nhng n HCL li chng hng, do phi dng ch dng cao lin tc trong qu trnh
Thuc v loi yu t vt l ny thng c:
o ph.
chen
nhtln
v ca
sc vch
cng ph
b mt ca dung dch mu
S
Trong php o AAS, vi k

thut nguyn t ha mu
trong ngn la, yu t ny
nh hng nhiu n tc
cc vch phn tch (bng 10.1a), th cc vch ph ny s chen ln cc vch phn tch, lm cho
dn mu vo bung aerosol
ha v hiu sut aerosol ha
c phn gii khng cao. V th, trong mi mc ch phn tch c th cn phi nghin cu
ca mu v t m nh
v chn nhng vch phn tch ph hp loi tr s chenln ca
cc
vch
hng n kt qu phn tch.
phca nguyntkhc. Nubngcch ny m
Ni chung, tc dn mu t
khng loi tr c nh hng th bt buc phi tch b bt nguyn t c vch ph chen
l nghch vi nht ca
ln ra khi mu phn tch trong mt chng mc nht nh, cc vch chen ln khng xut
dung dch mu (hnh 10.3).
hin na.
Bng 10.1a
Chnh s khc nhau v nng axit, loi axit, nng cht nn ca mu, thnh phn
cachen
cc cht
cs
trong
dung
l nguyn
S
ln v
trng
vchdch
camu
cc nguyn
t nhn gy ra s khc nhau v nht ca dung
dch mu. V th, trong mi qu trnh phn tch mt nguyn t, nht thit phi m bo sao
cho mu phn Nguyn
tch v cc
chun phi
cngchen
nng
axit, loi axit v
t mu u lp ng Nguyn
t ccvch
ln(ppm)
thnh phn ha hc, vt l ca tt c cc nguyn t khc, nht l cht nn ca mu. Yu t ny
v vch
phn tch
(nm)
Vch
chen
Nng
xut
hin stachen
lndng
thng th
hin nhiu
trong
php o FAAS.
ln
loi tr nh
hng
ny chng
c th
/\
V-308,211
800
+ o v xc nh theo phng php thm tiu chun,
Cu-324,754
Eu-324,753
254
+ Pha long mu bng mt dung mi hay mt nn ph hp,
Fe-271,903
Pt-271,904
0,54
+ Thm vo mu mt cht m c nng ln, ng nht nht,
Mn-403,307
Ga-403,298
0,25
+ Dng bm y mu vi mt tc xc nh m chng ta mong mun.
Zn-213,856
Fe-213,850
200
Hiu ng 1u li
cc bin php Al-308,215

sau y:
Yu t ny th hin r rng c bit trong php o ph hp th khng ngn la v cng

Scht
hp phn
th ca
cccht
rn ln, ng thi cng ph thuc vo bn cht ca cc nguyn
ln khi
tch
nng
t, hp
Trong
cht mi
n tn
trng
ti trong
hp th,
mu,
ccng
bit nh
l trong
loi ngn
cuvetla
graphit
n kh,
cnhiu
dngkhi
cn
nguyn
c cha
t ha
c
mu.htNi
nguyn
t kh
baycha
hi v
cht bn
nhithay
lun
ra
cc
rnchung,
nh licc
ti ca
vt cht
mu
b d
hasinh
hiravhp
nguyn
t ha,
cclun
ht gy
mui
nh hng
t hon
graphit
Cc
hot ht
haloi
thng
hn chc
c
cacbon
ca ny.
nhinCc
liucuvet
chac
cch
t to
chy
ton.
ny thng
th hiu
c ng
lp
ny.ca
Hn
na,la.
b mt
ca cuvet
v
ngn
Cc bn
ht trong
ny hoc
hp th hoc chn ng i ca chm sng t n HCL
chiu vo mi trng hp th. Yu t ny c gi l s
204
203
Cayu
6,11
00,20
17,00
ha hi
ca
nguyn
t phn
tch.
Cc
cht
nn
nylthng
l
nhng
cht
bn
cng
lmt
ng
gp
vo
hiu
ng
ny,
ngha
bphn
mt 01,50
cng
mn hp
th
hng
cng
loi
trtnh
hng
ca
s
pht
x
ca
nguyn
t
tch
chng
ta nh
c
th
dngnhit
cc
ca
cc
nguyn
t,
nh
Al,
t
him,
v.v...
nh,
mt
cng
hng cng ln. Do
tnh cht ny m
khi nguyn thamu
bin b
php
sau
y:xp th nh
Ba
5,31
01,00
06,00
23,00 o
th
vic nghin
culngnh
cc nh hng ha hc c canguyn
trnh by trongtchng
ny
cngV
nhit
vchph
th mt
Chn
nguyn
t ha mu thp ph hp m ti nhit
s kch phn
thch ph
c tnh
chttkhi
tt c
ccIon
loiha
c thng
th c
chng
ta lu i
khi
Thc
cho qut
thy chung
rng,
qu
trnh
cv c
ngha
vi ng
cc dng
kim
tch
b nguyn
chng
c
li vi
trnnguyn
b mt ch
cuvet
phtkhng
x l khng
ngtkha,
hoc
khng
xylu
ra i
t
phn
tch.th tch t li qua mt
php
o
ph
hp
th
nguyn
t,
vi
mc
ch
bit
v
loi
tr
cc
nh
hng
ha
loilnkim
v t
sauha
mu.
l cc
kim n
loimt
kim
th,
cnthi
vibcc
nguyn
t theo
khcvsdoIon
s
nguyn
Nhng
ln
no
n
li
nguyn
t
ha
Thm
vo
mu
cc
cht
m
hn
ch
s
pht
x
ca
nguyn
t
phn
tch.
chnh
l
hc nu chng xut hin. Cc yu t nh hng v mt ha hc c th c sp xp
ha
khng
ng
k
trong
mi
trng
hp
th
ca
php
o
ph
hp
th
nguyn
t
(Fcc
mui
halogen
ca
cc
kim
loi
kim,
c
th
kch
thch
ph
pht
x
thp
hn
th
kch
thch
tora
docchcanguyn
t phn tch tng
t ngt
theo cc loi sau y,
dsnguynt
xem xt vt
tm
loi tr:
ph
pht
x
ca
nguyn
t
phn
tch.
AAS
hay
ETA-AAS).
loi
tr
s
Ion
ha
ca
mt
nguyn
t
phn
tch
chng
c
khngNng
theo
nng
l lm tng cng ca vch ph v dntan
axit
vca
loin
axittrong
trongmu,
dungngha
dch mu
Bng
th
dng
cc
bin
pht
sau
y:V th cn phi loi tr nh hng ny. loi tr nh hng
Nng
kt
axit
trong
lm
sai10.2
lc
qu
phn
tch.
dung
lun
ny chng
ta mu
ciu
thlun
theo
cch t
sau:ha c nhit thp ph hp, m trong iu kin
+dch
Chn
kin cc
nguyn
Mcnh
bhng
kch thch
pht x ca cc nguyn t trong cc nhit khc nhau No- S
c
nph
cng
nguyn
phn
tch
hu
khng
bnguyn
Ion ha.t
+ t
Lm
sch
cuvet
sau
habmu,
lmph
baypht
hix
ht cc cht cn li
nguyn
t
trung
ho
ban nh
u;
Ni -ln
S
nguyn
kch
thch
ca
vch
ph
cami
Nguyn
ttch phi
Tnhit
s Ni/No
nhittha nguyn t
trong +cuvet.
Ttvo
nhin
hin
nhitm
cao
nguyn
nguyn
t
phn
Thm
mu thng
phnthc
tchthch
mt(eV)
cht
cho hn
s Ion
ha.
l cc
mui halogen
Th
kch
oC
oC
qua
tc
dn
mu,
kh
phn
tch;
2000
3000
4000oC
ca cc kim loi kim c th Ion ha thp hn th Ion ha ca nguyn t phn
tch vi
nng ha hi v nguyn t
+ Dng
c vy
ch trong
to t iu
cc loi
c
hot
ha
ton
phn,
c
mt nng
cc
ln loi
ph cuvet
hp. Nh
kingraphit
t phn
tch3,00.10
s khng
b
-4 nguyn
-3
-2
4,00.107,10.10
ha caCs-852,10
cht mu. nh 1,76
b
mn;
Ionmt
hachc
na.v
Hnh
10.4
mt v d v tc dng ca cht m KCl v NaCl trong vic
hng
ny
thng
gnl lin
Na-589,00
2,12
1,00.10-5
6,00.10-4
4,00.10-3
loi loi
tr
s phn
Ion
ca o
haicc mu c nng nh trc;
vi
Anion
caha
axit.nn
+ Khi
tch
Ni
chung,
cc tch
axit Ba
cng
nguyn
t
phn
v 2,95
Ca-422,70
1,10.10-7
4,10.10-5
6,00.10-4
+
Thm
vo
mu
nhng
cht
m
c
nng
ph
hp;
kh bay hi v bn nhit,
Rb. Trong trng hp ny
Zn-213,90
5,86
7,00.10-13
6,00.10-8
1,10.10-6
+
Trng
b
mt
trong
ca
cuvet
graphit
bng
mt
lp
cc
hp
cht
bn
nhit.
nng ca kim loi m
Tt nhin
l nhng
nguyn tc chung. Cn trong thc t phi ty tng trng
phi thm
vo y
ti ch
thiu
l
Trn y l mt s yu t vt l c th c xut hin trong php o AAS v c th nh
hp
c
thgim
m
chn
cc
bin
php
ph
hp
nht.
cng
lm
nhiu
cng
vch
ph
hp
th
nguyn
t phn
250
^g/mL
hng
hng
n
ktth
qunh
phn
tch.
Nhng
mc
xyca
ra l
rt khc
nhautch.
trong mi trng hp c
th, c
c,
cca
khil
khng.
nynh
xut(hnh
hin10.5).
ln hay
nhny
l c
c th
phthy
thuc
ca
s
Ion
ha
khng
Skhi
Ion
ha
cht
phn
tch hng
Cc
axit
d
bay
hi
gy Mc
nh
iu
r vo
rngnhit
khi xc
ca
mi
trng
hp
th,
tnh
cht
ca
nguyn
t
phn
tch,
v
thnh
phn
ca
mu
phn
tch.
cn Ca
na.
khibaCa-422,7
nh
o tchung,
vch
ph
ccphn
mitch,
trng
ccIonaxit
4,
ylc
lNi
yu
vt
l th
nh hngnm
ntrong
kt qu
v quca
trnh
haHClO
thng
Do
cn
phi
xem
xt
tm
bin
php
loi
tr
khi
chng
xut
hin.
CH
COOH,
HCl, HNO
3, do
H2
SO4nguyn
, H3POt
4,phn
HF vi
mt
nong
lhp
2%th
(hnh
xc3gim
nhs nguyn
cc
nguyn
tca
lm
t t
tchcng
trong
mi
trng
to 10.6).
ra ph, do
Cc yu
t
ha
hc
Ni
chung,
cc
axit
lm
gim
cng
vch
ph
theo
th
t:
HClO
<
HCl:
4
kim
th ngi
lm th
gim cng
vchtaph hp th, nu nguyn t phn tch b Ion ha cng nhiu.
Trong php o ph hp th nguyn t cc nh hng ha hc cng rt a dng v phc
thng mc
dng KCl,
phn mi nguyn t l khc nhau, v cn ph thuc vo nhit ca
Nhng
b cng
Ionkhi
ha
tp, n xut
hin
rt ca
khc nhau trong mi trng hp c th v cng nhiu trng hp
Hnh 10.4
tch
cc
kim
loi
kim
mi
trng
mt iu
nht nh,
ni dn
chung
t bn
c th
Ion ha
khng
xut hp
hin.th.
CcTrong
nh hng
ha kin
hc thng
c th
ncc
ktnguyn
qu theo
hng
sau
Tc dng ca KCI v NaCI trong vic loi tr s ion ha ca Ba
ngi
ta
thng
thm
CsCl
y:
cng thp th cng b Ion ha nhiu. Vi mt nguyn t, th khi nhit ca mi trng hp
(10 ng/mL) v Rb (10 |ig/mL)
vo cng
mu
phn
tch
Lm
gim
cng
ca
phha
canhiu
nguyn
t Bng
phn 10.1b
tch, do
cht
th
cao,
nguyn
t
theo
cngvch
b Ion
hn.
l s
mttovthnh
d vcc
iuhp
ny.
bn
nhit,
kh
ha
hi
v
kh
nguyn
t
ha,
v
d
nh
nh
hng
ca
cc
Ion
silicat,
sunfat,
trong ph hp (500 Bng 10.1b
photphat,
florua.
1000
ppm).
Mc
Ion
ha cng
ca mtsca
nguyn
t do s to thnh cc hp cht d ha hi v d nguyn
Lm tng
vch ph,
Shay
phtdo
x hn
ca nguyn
t phn
t ha,
ch c
nh tch
hng ca s Ion ha v s kch thch ph pht x ca
nguyn
t t
phn
chnh
l tclm
dng
ca nng
mt s
ch yu t
l trung
mui halogen
ca
Yu
nytch.
xuthin
thng
gim
hp
cacht,
cc nguyn
ho c kh
kim
loi
kim
v
kim
th
hay
lantanClorua.
nng hp th bc x trong mi trng hp th, do cng lm gim cng o ca vch ph
Nguyn
t
Ion ph
ha khi
(eV)nguyn t phn tch
S %
Iontrong
ha nn
nhit
( C):
S
tngchung
cng
vch
tnbpht
ti
mu
nhng
hp
hp th.
Ni
cc
nguyn
t c th kch thch ph
x thp ca
thng
bl nh
hng
cht d ha hi. Lc cc cht nn ny c 20,00
tc dng nh l mt
cht
mang
cho
s
ha
hi
30,00
40,00
nhiu. ng thi mi trng hp th c nhit cng cao th nh
hng ny cng
ln (bng
ca nguyn t phn tch v lm cho n c ha hi hiu sut cao hn.
Na trong nhit 5,21
10.2). Nhng
ca php o AAS,00,30
th s kch thch 05,00
ph pht x thng26,00
ch xy ra
S gim cng ca vch ph khi nguyn t phn tch tn ti trong nn ca mu l
mnh
cc kh
kim
loihi.
kim
vny
sau
nguyn
l cc kim
th,
v hm
cc nguyn
t ny c
Kchti
4,32ha
02,10
22,00
nhngch
hpyu
bnvi
nhit,
Lc
cc
t nn
km
s 82,00
th kch thch
cc kim loi khc34,00
th s kch thch 90,00
ph pht x
Rb ph pht x tng
4,16 i thp. Cn09,00
l khng ng
Cs k (bng 10.2).
3,87
28,00
70,00
96,00
206
208
205
207
HN03 < H2S04 < HaP04

< HF, ngha l axit HCIO4 <
HC1 v HNO3 gy nh hng
nh nht trong vng nng

nh. Chnh v th trong thc t
phn tch ca php o ph hp
th nguyn t (AAS) ngi ta
thng dng mi trng l

axit HC1 hay HNO3 1 hay 2%.
V nng nh th nh
hng ca hai axit ny l
Hnh 10.6
10.2.3.2 v nh hng nh hng ca loi axit n cng vch ph

ca cc Cation c trong mu:
Ca-422,7nm trong php o F-AAS (kh.kh + C 2H 2 )_____________________
Dung dch mu phn tch, ngoi nguyn t cn xc nh, thng cn cha cc

nguyn t khc. Cc nguyn t ny tn ti di dng cc Cation hay Anion tan trong
dung dch mu. Cc Ion ny c th lm tng, cng c th lm gim, hoc cng c th
khng gy nh hng g n cng vch ph ca nguyn t phn tch. Khi c nh
hng th mc nh hng ca mi Ion cng rt khc nhau trong tng trng hp c
th. Nhng mt cch tng qut th chng ta c th quy nh hng ca cc Cation theo
7 loi nh trong hnh 10.7 d xem xt.
Nh vy nh hng ca cc Cation n cng vch ph ca nguyn t phn
tch c th c hiu ng dng, hiu ng nm v cng c th c hiu ng va nm va
dng i vi mt Ion, khi n cc nng khc nhau.
Khng c
4
76
3
C[
C5
Nng nguyn t nh hng
209
Hnh 10.7
Khi qut v nh hng ca Cation bao gm 7 loi
Loi 1: Khi C > C2 khng nh hng; Loi 2: nh hng cc i Ci ; Loi 3: Gim
lin tc theo ng cong li; Loi 4: Khi C < C 2 khng nh hng; Loi 5: Gim theo ng
cong lm; Loi 6: Khi C > C 2 khng nh hng na; Loi 7: Gim lin tc tuyn tnh, khi C
tng.
Loi l: Khi nng ca Ion gy nh hng ln hn C 2 th n khng lm tng cng
ln hn C2.
Loi 2: Ti nng C 1 ca nguyn t gy nh hng, cng vch ph ca nguyn t
phn tch t gi tr cc i. V th nh hng ny cng c dng tng nhy ca
gi tr khng i C1.
Loi 3: Trong trng hp ny cng vch ph gim lin tc theo ng cong li, khi
nng nguyn t nh hng tng dn u (xem v d ng 5 trong hnh 10.8).
Loi 4: Cc Cation ch gy nh hng n cng vch ph ca nguyn t phn tch
nh hn gi tr C2 th khng phi quan tnm n tm bin php loi tr.
Loi 5: Trong trng hp ny cng vch ph ca nguyn t phn tch li b gim
dn v y nht thit phi tm bin php loi tr nh hng ny (xem v d trong hnh
10.10a).
Loi 6: Khi nng ca cc Cation khc trong mu ln hn gi tr C 2 th chng khng
lm thay i cng vch ph ca nguyn t phn tch.
Do , nu khng tm c bin php loi tr ph hp th chng ta thm vo mu
Cation gy nh hng vi nng ln hn gi tr C 2, a nh hng gim thnh mt gi
tr hng s cho tt c cc mu phn tch v mu chun. Nh th cng loi b c nh hng
ny. Nhng tt nhin l ta lm gim nhy ca phng php phn tch i mt t.
Loi 7: y cc Cation l lm gim lin tc cng vch ph ca nguyn t phn
tch theo chiu tng dn nng ca n mt cch tuyn tnh (xem v d trong hnh 10.10b,
ng s 7).
Do cng cn phi tm bin php ph hp loi tr nh hng ny, hoc gi cho cc
Cation l c nng nht nh v khng i trong tt c cc mu chun v cc mu phn tch.
210
nh hng cc Cation trong dung dch mu n cng vch ph ca nguyn t phn

tch trong php o ph hp th nguyn t vi k thut nguyn t ha trong ngn la v khng
ngn la cng rt khc nhau.
V d. Ion La(III) trong php o F-AAS l yu t loi tr nh hng ca cc Ion l
khi xc nh Ca, Mg, Mn, Al, Fe. Nhng chnh La(III) li l Ion lm gim cng vch ph
ca chnh Ca, Mg, Al, Fe rt ln trong php o ETA-AAS. iu c ngha l mi Cation
trong tng trng hp c th v trong mi php li c tc dng khc nhau, m chnh n
trong php o ny th nh hng, nhng trong php o khc li khng gy nh hng.
minh ho v nh hng ca cc Cation l i vi vch ph ca nguyn t phn tch
chng ta c th xem xt mt s v d trong cc hnh t 10.8 - 10.11.
Hnh 10.8 l nhng v d v cc nh hng cc Cation thuc loi 1, 2 v 3. Cc ng
1, 2 v 3 l thuc loi 1. ng 4 v 6 thuc loi 2. ng 5 l thuc loi 3. Khi cc ng
trong hnh 10.7 l biu
din
cc nh hng cacc Cation thuc
loi 4. Trong hnh 10.10b, ng s 1, 2 v 3 m t cc nh hng thuc loi 6. Cui cng

ng s 5 m t cc nh hng thuc loi th 7 nh trnh by trn. Ngc li vi cc
nh hng trn, hnh 10.9 l m t nh hng tng hp ca cc Ion Mg(II), TI(IV), Al(III),
Fe(III), Si, P n cng vch ph ca nguyn t Ca 422,7 nm trong php o F-AAS vi
ngn la n kh nguyn t ha mu bao gm khng kh v axetylen, khi khng c mt v c
mt LaCl3 vi nng khc nhau.
y vi s c mt ca LaCla dung dch mu nng t 1 % tr ln th nh hng
ca cc Ion l nu l hon ton c loi tr. V th mui LaCla l mt cht ph gia c
dng loi nh hng ca cc Cation v Anion trong php o F-AAS vi hiu lc tt nht.
nhau:
211
Hnh 10.8
nh hng ca cc Cation thuc loi 1, 2 v 3
ng 1: Na/Rb 780 nm, n kh (khng kh + C 2H2);
ng 2: K/Ba 553,6 nm, n kh (N 2O + C2H2); ng 3:
K/Sr 460,7 nm, n kh (N2O + C2H2); ng 4: La/P
213,6 nm, n kh (ETA-AAS);
ng 5: Fe/Ca 422,7 nm, n kh (O 2 + C2H2); ng 6:
Sr/Ca 422,7 nm, n kh (N2O + C2H2).
212
10
100
1.000
10.000
(ng/mL)
Hnh 10.9
(-nt-
ng 4: Si/ca 422,6 nm. F-AAS

nh hng ca cc Cation : (thuc loi 4)
ng 5: Si/Mg 285,2 nm. F-AAS
(-nt- )
(khi c mt 1% LaCl 3)
ng
6: 283,3
Si/Ca,Mg,
F-AAS
Al, Fe, Ca
n Pb
nm, ETA-AAS;
Cu. Ni, Fe n As 193,7 nm, F-AAS (kh.kh +
(kh. kh + C2H2)
C2H2).
ng 7: Ti/Mg 285,2 nm, F-AAS
nh
hng
ccx
anlIon
c ph
tronghp
mu
+
Chn
iuca
kin
mu
loi cc nguyn t nh hng ra khi dung dch
Cngtch
vicc
mu phn
oCation,
ph. cc Anion cng nh hng n cng vch ph ca nguyn t
phn tch nh hng ny v tnh cht tng t nh nh hng ca cc loi axit. Ni chung,
+ Chn cc thng s ca my o thch hp.
cc Anion ca cc axit d bay hi thng gim t cng vch ph.
+ Thay i hay chn vch ph khc, c th km nhy mt cht.
Ch ring c hai Anion ClO - v CH3COO- l gy hiu ng dng (lm tng), tc l lm
+ Thm vo mu phn tch nhng cht ph gia ph hp chuyn mu sang cht nn
tng cng vch ph ca nguyn t phn tch trong mt s trng hp mt vng nng
khc ph hp nhm loi tr cc nh hng ca cc Cation, nh LaCl 3, SrCl2, AlCl
3 trong php
nht nh. Cc Anion khc thng gy hiu ng nm (lm gim) theo th t Cl - < NO- < CO- <
o -F-AAS
v LiBO2, NH 4NO3 hay hn hp (LiBO2 v NH 4NO3) trong php o ETA-AAS
SO < F- < PO4- < SIO^- v.v...Trong Anion
hay nhng
cht ph gia khc.
SIO^- c nh hng ln nht, cn t nht l Ion Cl. ng thi khi nng ca cc Anion tng
Tt nhin trong
mitrng hp c th cn phi nghin cu chn c loi
th tc dng nh hng cng tng theo (hnh 10.5).
cht v nng ph hp ca n.
Do thc t nn trong mi php o phi gi cho nng ca cc Anion trong mu
+
Chn
cc chun
iu kin
nguyn
mugi
thch
hp v
chn
lc.i.
phn tch
v mu
l nh
nhautvha
mt
tr nht
nh
khng
+ Vi tt c cc bin php trn m khng c, th bin php cui cng l bt buc
Mt khc cng khng nn chn axit H 2SO4 lm mi trng ca mu cho php o AAS
chng
phi
tchaxit
HCl
loi hay
b cc
Cation
c nh hng. Tt nhin bin php ny rt t khi phi
m chtann
dng
HNO
3 vi nng di 2% (hnh 10.12).
p dng.
1 Ax
------------------------------------6
Php o ETA-AAS
\ \\
\4
|ig/mL NaCl
100
Hnh 10.10a
200
C(jj.g/mL)
Hlnh 10.10b
nh hng ca nng NaCl/Pb-217,0 nm nh hng ca cc Cation loi 5, 6, 7
214
ng 1: Ti/Ca 422,7 nm, F-AAS
(kh. kh +
ng 2: Ti/Sr 460.7 nm, F-AAS
(-nt- )
ng 3: Ti/Ba 553,6 nm, F-AAS
(-nt- )
C2 H 2 )
213
2%
LaCl nhng
Trong bn bin php trn, bin php th nht cng ch thc
hin c trong
3
1,5% LaCl3
chng mc nht nh, v chng ta khng th tng nhit nguyn t ha ln cao mi c, do

1 % LaQ 3
s hn ch ca trang thit b, bn cht ca kh t, hn na khi nhit
nguyn t ha qu cao
0,5% LaCl
3
th li xut hin nh hng ca s tn ha v s pht x.

Cho nn bin php hai l thng dng nht. Cc cht -------0,1%
ph giaLaCl
thng hay c dng
3
trong php o F-AAS l LaCl 3, SrCl2, Li3, KCl, AlCl 3, ------------- y LaCl 3 c
s dng rng ri
0,05% Lad
3
nht, cc cht cn li ch cho mt s trng hp ring bit. Ngc li, trong php o ETA5)
AAS cht ph gia c dng nhiu nht l(Loi
LiBO2,
NH 4NO3 hay hn hp ca hai cht ny
trong mt nng ph hp. iu ny chng ta c th thy trong v d ca bng 10.4.

**
nh hng ca dung mi hu c
'
0% LaCl 3
C(ig/mL)
Trong php o ph hp th nguyn t, c bit l i vi k thut nguyn t ha mu

trong ngn la, s c mt ca dung mi hu c trn ln vi nc trong dung dch mu phn
tch, hay mu phn tch ha tan trong dung mi hu c thng lm tng cng ca vch
2,5
7,5
125
250
375
10 p
ph hp th nguyn t5 ca nhiu nguyn

t ln
10 5). y l mt phng
10
15 nhiu ln20(bng
Si
500 Al, Fe
php
tng nhy. V
tch cc
cTi nng rt nh st gii hn
Bng
10.4
25 th, khi phn
50
75 nguyn t100
20
40
60
di
ca php
chng
c th
vo mu
nh hng
cao,
thnh
phntann
cathm
mu phn
tch phn tch mt dung mi hu c c nng
ph hp th c th tng nhy ca phng php phn tch ln n hai hay i khi n ba ln
Hnh 10.11
so vi khi ch dng dung mi nc. Song dung mi hu c thm vo phi trn u c
Cht nn ca mu
vch
C=30
ppb php
nh
hng
hp
mtkhit
s nguyn
422.7nm
trongph
php
o F-AAS
khi o
c v
vi nc
v t
phi
c ca
tinh
cao. t n CaCng
ETA-AAS
khngNu
c mt
LaCl
dung
mi3 khng tinh khit cao th chng ta li lm nhim bn mu phn tch. Hoc
80 Mg
Thnh
phn
mutan trong nc th chng
nu dung
mi
hunn
c ca
khng
ta c th
nguyn t
Mg-202,60
nmchit
Ca-422,70
nmphn tch t
dung mi
dng
phc,
d cc
Me-APDC
trong
dungphi
mi lc
huno
c,
Yu nc
t nh
hnghp
nycht
ngi
ta v
quen
gi phc
l matrix
effect. vo
Nhng
khng
1
Dung
dch
HCl
1%
0,220
0,250
sau
o ph
ca nguyn
t phn
dung hp
mi hu
Thng thng l
cngxut
hin,hp
mth
thng
ch thy
trong tch
mttrong
s trng
nht c
nh.
dung
micc
MIBK
(Methyl
Izobutyl
l hp
dungcht
mibn
hunhit,
c in
chit
2.d
Nh
1,
thm
2%nguyn
LaCl
0,020
0,025
nhngV
mu
c
cha
diKetone)
dng cc
khhnh
bay
hi
v
3 t nn
cc
Me-APDC
kh phc
nguyn
t ha. cho php o F-AAS (Me: l cc Ion kim loi nng, APDC l Amonium
3. Nh
1, thm 0,5% LaCl
0,050
0,060
Pyrolydine
Dithio-carbamate.
Cc3 phc Me-APDC c
chit tt vo MIBK,
CHCl 3, CCl4
V d: Khi xc nh cc tp cht lng vt trong cc mu oxit t him, oxit kim loi
trong mi trng pH t 2 - 6).
kim th, 4.oxit
nhm,
oxit1%
zircon,
cc +LiBO2
mu mui NaCl, 0,210
th cc nn ny s kh
cng ca
Nh
2, thm
NH NO
0,245
Vic s dng dung mi hu4 c 3 y c hai cch:
vch ph ca nguyn t phn tch, qua lm gim nhy ca phng php phn tch.
Nu dung mi hu c tan trong nc th ngi ta thm vo dung dch mu phn tch
Trong
nhiu
trng hp,
yu
t phn
ny lm
hng
ln, nhiu
thm ch
trng
loi
tr nh
ca
thnh
nn gim
ngi
ta ca
c chc
th
dng
binc
php
khchp
mt nng
dung
mihng
hu c
thch
hp
tng
nhy
phng
php phn
tch.
hng
trm ln cng ca vch
ph (bng 10.4). Nguyn nhn chnh ca
nh
nhau:
Nu dung mi hu c khng tan trong nc th ngi ta chit cht phn tch dng hp
hng Tng
ny lnhit
s tn
ti ca cc
cht bn nhit trong mi trng hp th.
t hp
ha
cht phc ca
n
vinguyn
mt thuc
thmu.
thch hp vo dung mi hu c . Nh th va tng
Cc
hp
cht
ny
lm
kh
trqu
hi v
hacc
ca
cc
nhy, va
loi
tr
c
cc
Ion
cnkhn,
tr.ccn
Thm
vo
mu
cc
cht
ph
gia
nng
phtrnh
hp ha
ngn
cnnguyn
s xut t
hin
hp
nguyn
phn tch.
cht
bntnhit.
chuyn mu sang cht nn khc, y l 1 bin php c dng kh ph bin trong php
o AAS loi tr nh hng ca cht nn mu.
Tch b nguyn t nn, khi hai bin php trn khng t kt qu. Tt nhin bin php
ny l hn hu.
216
217
215
Bng 10.5
nh hng ca dung mi hu c n cng vch ph
STT
Dung mi hu c thm vo
Cng Cu-324,70
Chng 11
1
Dung dch HCl 0,1 M
PHN TCH NH LNG BNG PH AAS
2
Nh 1, thm 40% CH3OH
3
1,000
1,670
Nh 1, thm 40% C2H5OH
1,750
Nhng vn chung
Nhphp
1, thm
Phng trnh 4c bn ca
o 40% Axeton
2,000
Trong php
hp1,th
nguyn
t,Izobutanol
mi quan h gia cng ca mt vch
ph hp th ca
5 o ph
Nh
thm
20 %
2,400
mt nguyn t phn tch v nng ca n trong mi trng hp th cng tun theo nh lut hp th
6 Ngha
Nh
1, thm
% Axeton
2,500
quang Lamber-Bia.
l, nu
chiu 70
chm
tia sng n sc cng I o i qua mt mi
trng cha mt
loi nguyn t t do nng N v c
phncng
Nh 1, thm 50 % EAK
sng
dyl L cm, th mi quan

Itqqua mi
trng c8tnh theoNh

cng1,80
thc:% Ethyl Amine Ketone (EAK)
log10 K(Methyl
' N L Izobutyl Ketone)
(11. 1)
Trong MIBK
hgia Io
2,600
2,800
3,000
y i lng lgIo/I chnh l nng lng ca tia sng b mt i do s hp th ca cc nguyn t

t do trong mi trng . Nh vy, n chnh l cng ca vch ph hp th v chng ta c:
Ax = k'.N.L
(11. 2)
Cng thc ny cho chng ta bit mi quan h gia cng ca mt vch ph hp th v nng
ca nguyn t trng thi hi trong mi trng hp th. Nhng n cha cho bit mi quan h gia cng
ca vch ph v nng ca nguyn t trong mu phn tch. Nh vy, nu gi nng ca nguyn t
trong mu phn tch l C th chng ta cn phi tm mi quan h gia C v N v t s suy ra c mi
quan h gia C v A. M t nng C trong dung dch chuyn thnh nng N trng thi kh, c c
bi qu trnh ha hi v nguyn t ha mu phn tch. Nghin cu vn ny, nhiu kt qu thc nghim
ch ra rng, mi quan h ca s chuyn ha gia C v N l rt phc tp v n ph thuc vo nhiu yu t
nh:
+ Bn cht ha hc ca mi nguyn t, trng thi lin kt,
+ Tnh cht ca hp cht m cc nguyn t tn ti trong mu,
+ Thnh phn vt l v ha hc ca mu phn tch, c bit l cht nn,
+ Cc iu kin thc hin qu trnh nguyn t ha mu.
Tuy c phc tp, nhng t nhng kt qu thc nghim v trong mt phm vi nht
218
219
nh ca nng C ca nguyn t cn nghin cu trong mu phn tch, mt cch tng qut,

th mi quan h gia C v N c xc nh theo cng thc:
N = k.Cb
(11.3)
trong k l mt hng s thc nghim, n ph thuc vo tt c cc iu kin ha hi

v nguyn t ha mu v khng i trong nhng iu kin nht nh c chn cho mt
php o, c bit l nhit ca mi trng hp th.
Cn b l mt hng s, c gi l hng s bn cht, n ph thuc vo nng C, tnh
cht hp th ph ca mi nguyn t v tng vch ph ca nguyn t . Hng s b c gi tr
bng v nh hn 1 (0 < b < 1).
Khi nng C ca nguyn t phn tch nh th b lun lun bng 1. Khi C tng th b nh
dn xa gi tr 1, tin v 0, tt nhin khng bao gi bng 0. Nh th, vi mi mt vch ph ca
mt nguyn t phn tch, chng ta lun lun c mt gi tr nng Co, m vi mi gi tr:
+ Cx < Co th b lun lun bng 1, lc ny A ph thuc tuyn tnh vo C.
+ Cx > Co th b nh hn 1. A ph thuc vo C theo cng thc (11.4) - khng tuyn tnh.
Nh vy, t hai phng trnh (11.2) v (11.3) chng ta c:
Ax = K.L.Cb
(11.4)
trong K = k'.k v c gi l hng s thc nghim ca php o AAS. ng thi t

cng thc (11.4) ny chng ta thy, cng A ca mt vch ph hp th ph thuc vo ba
i lng (thng s K, L v C).
Nhng trong mt php o th K lun lun l hng s, L l chiu di ca ngn la trong
php o F-AAS hay chiu di ca cuvet graphit trong php o ETA-AAS, tc l b dy ca
mi trng hp th v nh th trong mt php o th n cng khng i. Do A ch cn ph
thuc vo nng C ca nguyn t cn xc nh trong mu phn tch. Do vy, mt cch
tng qut chng ta c:
Ax = a.Cb
(11.5 )
y chnh l phng trnh c s ca phng php phn tch nh lng da theo vic
o ph hp th ca mt nguyn t xc nh nng (hm lng) ca n v mi quan h
ny c minh ho trong hnh 11.1.
220
Nu b bng 1 th mi quan h gia A

v C l tuyn tnh theo phng trnh c
dng y = a.x. Khi ng biu din mi
quan h ny l mt ng thng i qua gc
to . Nhng thc nghim cho thy rng
trng hp ny l ch c trong mt vng
nng nh. y l trng hp l tng,
n ch c c i vi mt s vch ph
khng nhy ca mt vi nguyn t nh Fe,
Ni, Si (hnh 11.1b). Ph bin nht l trng
hp trong hnh 11.1a. l trng hp
chung cho hu ht cc vch ph hp th ca
cc nguyn t. N gm mt on tuyn tnh
(b=1) v mt on khng tuyn tnh (b<1).
Ni chung trong trng hp ny thng
lun lun c mt on thng ca ng biu
din mi quan h gia A v C vng nng
nh ca nguyn t phn tch. l on
OA. Vi cc vch ph cng nhy th on
OA ny cng ngn. Tc l vng nng
ng vi on tuyn tnh l hp. Vng nng
ng vi on tuyn tnh OA c gi l
vng tuyn tnh ca php o AAS.
i vi mi nguyn t v mi mt vch ph th vng ny l khc nhau r rng (bng
11.4). Trng hp th ba cn li (hnh 11.1c) l mt dng phc tp. Trong trng hp ny
mi quan h gia A v C l khng tuyn tnh trong bt k vng nng no. Song ch rt t
vch ph, c bit l cc vch ph rt nhy v c kh nng t o ln mi tun theo quan h
ny. Trong phn tch, nu gp phi trng hp ny cn phi ht sc ch khi lp ng
chun, ngha l phi dng nhiu mu u c nng gn nhau dng ng chun v ch
c nh th chng ta mi xc nh c chnh xc v tr ca ng chun. Vch ph hp th
Na-589,00 nm i din trng hp ny.
Mu chun trong php o AAS
Trong phng php phn tch nh lng theo ph hp th nguyn t, mu u (mu
chun) dng ng chun cng bt buc phi tha mn mt s iu kin nht nh. Cc
iu kin l:
Cc mu u phi c trng thi vt l v ha hc nh mu phn tch, ngha l mu phn
tch tn ti trng thi, dung mi, mi trng v dng lin kt no th mu u cng phi c
tnh cht ging nh th. C nh th mi loi tr c nh hng ca cht nn, ca thnh phn
ca mu n kt qu phn tch.
221
Cc mu u v mu phn tch phi c pha ch hay ch luyn, x t trong cng mt

iu kin nh nhau.
Cc mu u phi bn vng theo thi gian, ngha l khng b thay i thnh phn sau
khi ch luyn v bo qun s dng lu di, khng b sa lng, khng b phn hy to
thnh cc cht khc lm thay i thnh phn ca mu u. C nh th mi bo m c
thnh phn ca n nh tnh ton pha ch v s dng lu di.
Nng ca cc nguyn t cn phn tch trong cc mu u phi rt chnh xc theo yu
cu ca phng php phn tch. ng thi khong nng ca mt dy mu u phi phn
b u trong vng tuyn tnh hay trong ton b ng chun ca php o v bao trm nng
ca cc mu phn tch.
Ngha l nng cc mu phn tch phi trong vng tuyn tnh ca ng chun. Cn
nu khng, chng ta phi pha long mu phn tch cho ph hp.
Biu din nng trong php o AAS
Trong php o ph
hp thnguyn t, ngi ta thng biu din nng
ca
nguyn t phn tch theo cc cch sau y:

Nng phn trm (%)
y l khi nim thng thng, n c biu th bng s gam ca cht phn tch, c trong
100g mu em phn tch. Nng ny c tnh theo cng thc:
C (%) = ^ .100
m
(11.6)
trong mx l s gam cht phn tch c trong mu ly phn tch, cn m l s gam

mu phn tch.
V d, nu vit dung dch NaOH 0,1%, ngha l trong 100 gam dung dch c 0,1 gam
NaOH.
Nng microgam 1 ml hay microgam li
Loi nng
ny c c s dng ph bin
trong phn tch lng vt v
thng c biu th theo hai cch:

S microgam ca cht phn tch c trong mt lt dung dch mu (p,g/mL) hay s
microgam cht phn tch c trong mt mnh dung dch mu (p,g/mL).
V d, nu vit Cpb = 1,2 p,g/l th c ngha l c trong 1 lt dung dch mu s c
microgam ca Pb. Hay nu vit C pb: 1,2 p,g/mL th c ngha l trong mt minilit dung dch
S microgam ca cht phn tch c trong mt gam mu (p.g/g), hay s microgam cht
phn tch trong 1 kg mu (p,g/kg). V d, nu vit C pb = 2,5 p,g/g th c ngha l c trong 1
gam mu s c 2,5 microgam ca Pb.
222
Khi nim
Bng
11.2 v nhy
Bng
11.1
nhy l mt i lng ch ra kh nng ca mt phng php phn tch theo mt k thut o
Mi
quani
hgia
giacc
ccnng
loi n
Chuyn
v nng (d=1)
no c p dng cho phng php phn tch . Phng php phn tch c nhy cao tc l
nng gii hn di c th phn tch c l nh. Cng nh cc phng php phn tch khc,
Nng u c
Chuyn sang nng th 2
n vphp
gc phn tch theoTng
ng
vi (1) t cng phTng
ng
viyu
(1) t khc
nhy ca phng
ph hp
th nguyn
thuc vo
nhiu
Nng
nhau, nh.:
mpp
H s phi nhn vo
g/L
-3
0,001p
ppm
mg/mL
Trc1000
ht phi
k n cc c trng, 1
tnh
cht ca h thng my o, nh10hg/mL
quang hc, dng c
p
thu nhn v pht
hin
tn hiu cn o, h thng
khuch
i v ch th tn hiu 10
o.-6g/mL
chnh
l cc c
ppm
Mg/L
1 ppm
1 p,g/mL
trng k thut ca h thng
my quang ph.
m
1 ppbpp
1 n/mLmol/ (m)
10-90,000.1p.A
g/mL
Yu t th hai l cc iu kin v k thut thc hin nguyn t ha mu o ph ( nghin
ppm
% (trng lng)
0,0001
1
ppp 2). V th phng php1 pg/mL
10-12
cu k trong chng
nguyn t ha trong ngn la c
g/mL
nhy km phng
php nguyn t1ha

khng ngn la. Bng 11.3
v bng
ppf
1 fg/mL
p,g/mL
ppm
l nhng v d v vn
ny.
10-15g/mL
1/p
1 ppa
1 ag/mL
10-181/10000.p
g/mL
p,g/mL
% (trng
Yu t th
ba
l kh nng v tnh cht
hp
th bclng)
x ca mi vch ph,
ca
mi nguyn t.
Vch ph no, nguyn
mnh th php o theo vchP c nhy
ppbt no c kh nng hp th cng
ng/mL
n v gc
Tng ng vi cc n v sau
cng cao. Ngha l i vi mt nguyn t cc vch ph khc nhau cng s c nhy khc nhau
(bng 11.3, bng 11.4 v bng 11.5). V th, khi ni n nhy ca mt nguyn t phn tch l phi
^g
Ng
trong
: iu kin phn tch c th nht nh ca mt php o.
gn lin
vi nhng
1 mg
pa
fg
10-3
ba yuca
t dung
chnh,dch
tt nhin cn nhiu yu t khc cng nh hng n nhy ca mt
p: tltrng
1
-6
phng php phn
ca
mu, nguyn
t c s ca mu. V vy, nu lm tt, ngha l
^gtch, nh axit10
10-6
A: nguyn t gam hay phn t gam ca cht phn tch.
tiu chun ha c cc yu t nu,

chng ta -9s thu c-9 nhy tt nht ca mt php o. Nh
-9
ng Nu trong 110
10-6g cht phn tch th gi tr ny (10 -6g)
Vi mu1 rn:
gam mu 10
c cha 10
vy nhy l g? V vn ny, hin nay ngi ta c hai khi nim.
-12 l ppb, -12

-12 ppa. Cc n v ny km
c gi l 1ppm.
n v 10
ppm
1 pa Cc c s ca
10-12
10 ppp, ppf10v
nhy tuyt i. Trong php o AAS, nhy tuyt i l lng gam (khi lng nh
nhau 1000 ln (bng 11.1). V d: Hm lng Cu trong thp l 5 ppm, ngha l c 1 kg thp
-15
-15
nht ca nguyn
t cn phn tch phi
cn thu
cng ca
1 fg
10-15 c trong
10-15mi trng
10-15hp th10
10c
th c 5 mg Cu, hay 1 Tn thp c 5 gam Cu.
vch ph hp th chn chim 1% -18
ton bng-18hp th, hay
bng 3 ln
nn. Nh vy,
mi
-18 tn hiu-18
-5
ag Nu trong 110mL mu10c
10-18
10-18 ca
Vi mu1lng:
cha 10
g cht 10
phn tch10
v khi t trng
nguyn t v mi vch ph s c nhy tuyt i khc nhau (bng 11.4). Do , khi phn tch cc
dung dch mu bng 1 th i lng 10 -5g/mL mu cng c nh ngha l 1 ppm.

V d: Hm lng Fe trong nc l 2 ppm, ngha l c 1 lt nc th c 2 mg Fe.
nhy
tng
i.
tng i cn c gi l nhy nng . nhy ny
trong
: agattogram;
fg-nhy
femtogram;
Hai khi
nim
ny c
dng
tng t nh nhau. Khi mu phn tch l cht rn th
c nh ngha l nng nh nht ca nguyn t phn tch c trong mu cn c th pht
ngipata thng
dng
v l g(p,g/g),
picogram;
ng-n
nanogram
v p,g-kg(mg/kg),
microgram.hay tn(g/t); cn khi mu l cht lng th
hin c tn hiu hp th ca n theo mt vch ph nht nh chn v tn hiu ny phi bng
dng n v mu l m(p,g/mL), Lt(mg/L).
1% ca
bng
hpton
tontng
phn, t,
hayngi
bng 3taln
ng
nn.
nhy ny c dng
Cng
hon
cndao
dng
ccca
ngi
vtr
c
s Loi
ca p,g.
Nng
mol/lit
(M)
ph bin
php o(ng),
AASpicrogam
hn khi nim
i.khi
K c
cc nng
phng
tch
trong
l nanogam
(pa). v
Do
nhy
cngtuyt
c cc
nim
php
ng/L,phn
ng/mL,
Khi
nim
nng
ny
biu
th
s
phn
t
gam
cht
phn
tch
c
trong
mt
lt
dung
khc, th khi nim nhy ny cng c dng ph bin hn, v hm lng cc cht trong mu phn
ng/g, pg/L,pg/mL v pg/g. Cc n v p,g, ng v pa u km nhau 1000 ln v mi tng
dchhay
mu.
l khi
nim
thng
haDophn
tch so
(xem
trnhgia
Ha phn tch
tch
muN
chun
thng
c
biuthng
th theo trong
nng .
, vic
snhgio
nhy
quan ca chng c ch ra trong bng 11.1.
nh lng c s).
Nng
ppm
v c
V d
vit
NaOH
0,1sM,ca
thn
c ngha l c trong 1 lt dung dch NaOH th c 0,1 phn
nguyn t c nng nh phi chn cc vch c nhy cao o v ngc li.
Loi
nng ppm (part per mill Ion: mt phn triu) thng hay c dng trong phn
t gam
NaOH.
tch lng vt cc cht, v cng c biu th theo hai cch, da theo mu dng lng (theo
n v ml hay lt), hay dng rn, hay bt (theo n v g, hay kg.):
224
225
223
Mg
285,2
KKng
-vi
C 2H
0,005
0,001
Bng
11.5a
11.4
2
hn
pht
hincc
trong
AAS
cc
A Gii
vnguyn
C
l tuyn
t, gia
tnh,
vch
ng
ph
nhau
vi
phng
s d dng
trnh
v thun
(11.8).tin
Khong
hn. Bng
nng
11.3 l0,1
mt
C- 4vi
ca
Be
234,90
Bi
0,002
1.000
0,00003
3
v
nguyn
d
v
t
phn
nhy
tch
ca
ng
mt
ng
sv
nguyn
vi
phng
trnh
loi ta
theo
(11.8)
mt
ny
vi
c
vch
ph
lAAS
hp
khong
thgii
nguyn
xchn
nh
t-(hay
ca
Mn
279,5
KK
0,03
0,01
0,05
5 hin
2t
2kim
nhy,
gii
hn
pht
hin
khong
xc
nh
ca
cc
nguyn
tgi
theo
Bn
cnh
khi
nim
v
- C
nhy
ngi
cn
s
dng
khi
nim
v
pht
Gii
hn
pht
hin
ca
php
o
ETA
-HAAS
theo
cc
my
khc
nhau
(theo
VH2/2P)
n
l i
khong
trong
tuyn
iu
tnh)kin
ca
nguyn
nguyn
t
theo
nht phng
nh ca
php
ngn
la
nu.
n
Trong
kh.
khong
ypht
cc
nng
nguyn
ny
t c
vi
mt
nguyn
t khi
dng
mt
chng
minh
n.
Gii
hn
hin
cng
Hgnhng
253,7
KK -t
Cha
0,5
10
-
150
2H2vch ph 4,0
223,10 Ca 422,70
0,003
500.000
0,0002
20
khc
thhai
quan
nhau,
hnim
cc
giavch
A vph
Ctc
khc
dng
nhau
ca
cng
phng
cl
trnh
nhy
ton
khc
hc
nhau.
y (pa)
= trng
ax.
Nguyn
t
vch
ph no
khi
tng
nh
nhy.
gii
hn
pht
hin
tuyt
ii
v no,
tng
i.
Cc
c
ca
AAS
Nguyn
t
hin
tuyt
Mo
813,3
KK
- C2H
1,9
0,15
4 - 200
n
kh
2 Gii hn pht
Nguyn
t
Vch
c khThc
nng
hp
bc
xtng
mnh
th
php
o
theo
c
nhy
tng
i cao.
nghim
thy
khong
xc
nhvch
i
vismi
nguyn
l khc
nhau,
mi
nguyn
t
ha
Gii
hn th
phtcho
hin
i
nguyn
t theo
mt
vch
nht
nh
Cd
228,80
1.000
0,00001
0
Mo
313,3
Nrng
2O
-0,003
Cca
2Hmt
0,5
0,2phtKhong
- 100
Vch
o(nm)
HGA-74
CRA-63
A-3470
nhy
Gii
hn
pht
xc1 nh
oTrong
(nm) hai khi nim trn, trong php o ph AAS, nh ngha v nhy IL-355
tng
i
vch
ph
khclnhau
l
rt nh
khcnht
nhau (bng
11.4).t trong
cAg
th328,1
xem
nng
nguyn
muphn tch
cn
c th(
pht
(^g/mL)
(p,g/mL)
0,1- Cca
0,2 0,07 hin (p,g/mL)
4,0,2
Ni 232,0
KK
0,02
- 15
2 H2
nhy
nng )
lun
c
dnghpth
ph
bin
so snh
hay nh
ccs
phng
php
phn
tch
0,001
1.000
0,000001
1 nht
hin
ctn
hiu
n
theo
vch
ph
trong
mt
iu
kin
trong
mt
nguyn
t
th
ccca
vch
ph khc
nhaugi
cng
c khong
tnh
AlNgay
309,3
10,0
90,
1341,5
2 2,0
330,0
4 0,1
5 tuyn
Ni
KK
- C 2 H2
0,4
1
80
0,00005
cnh
th cho
tng i tng.
chn.
khcAu
nhau
(bng 11.6). Vch ph
c hp- th3.000
cng nhy 0,6
th 0,0001
c khong nng
242,8
10,0no
10, tuyn
Mg
285,20
0,003
10
Al
N2O -NC
2
H
2
1,0
0,2
2 -100
200- 4000
Nb309,3
334,9
O
C
H
25,0
50,0
2
2 2
Bng
11.3
Ngc
li
gii
hn
pht
hin
tuyt
i
ca
mt
nguyn
t
l
khi
lng
ti
thiu
ca
Cd
288,8
0,1
0,1
2,
tnh cng hp v ko v pha nng nh.
0,00002
Sb
217,6
KK
0,4
0,1
1
60
Os
290,9
NC2H2
1,5
0,5
2
250
2O - C2H 2
t mt
c trong
hpca
th
cn
c th
pht hin
tn
hiu hp
th
nguyn
nhy
ca
s
nguyn
tmi
CoV240,7
5,0 trng
4,0
40,php
th
khicn
nim
v khong
xc nh
mt
nguyn
t 8,0
trong
mt c
phng
phn
Mn 279,50
0,001
2.000
0,00003
2
193,7
Ar -KK
H2- nht
0,50,25
0,2
- 50
Pd
247,6trong mt iu
C2H2nh 2,0
0,1 vi v d1 v
1 -
40ny.
caAs
n
cng
kin
chn.
Bng 11.55,0
l mt
vn
357,9
10,0
tchCr
gn
lin vi mt vch ph
c chn o
v cc iu kin
th nghim 20,
c chn.
Mo
313,30
0,01
0,000001
3
As
193,7
KK
-2C2H2
1,210.000
2,0
10hin
-7,100
Pd
247,6
O
H2mi mt4,0
2,2 cng10,0
1,0 hn pht
5 - 200
Cu
324,7
2,0- C
Nh
nguyn
t2v
c
Bng
11.6
l vy,
mt mi
s vmt
d v
khong
xc nh cavch
mtph
s nguyn
tgii
theo cc vch
phkhc
ca nhau.
n
Fe
248,3
3,0
4,0
0,2
100,
Trong
mt
vch
no
hp th mnh
s c gii0,6
hn
pht- hin
Ba
553,6
Cph
0,30,02
0,20,01
- 60
K 766,6
0,04
4
2O.KK
2H-2 C
2H2 c kh nng
trong
php
o nguyn
AAS. t, N
Na
589,00
0,001 Tng i5.000
0,0001
0,1
Vch
ph
(nm)
(pg/l)
Tuyt
i
(pa)
Mg
285,2
0,1
0,06
3,0
0,1- 4
lng
hay nng Nnh
(bng
Be
234,9
C2H-2C11.5).
0,02 1,5
0,010,3
0,04
Ptnh
265,9
KK
5 - 300
2O 2 H2
B chnh
nn trong php o
AAS
Mn 275,9
0,2
0,5
5,
Nhng
ngoi ccKK
yu- Nt
trn, gii hn pht
hin mt nguyn
t theo php
hp th
223,1
0,310,0
0,20,00001
1 -o
50ph
Pt
265,9
8,0
25
- 2000
2O - C2H 2
Ti
sao phi b chnh
nnC2H2
CBi
357,90
0,001
100
1
Mo
313,3
3,0
13,0
20,0
nguyn t cn
thuc vo:
Agph
328,10
0,002
03,5
B
N2O -KK
C2H-2C2H2
12,0 0,5
10,00,1
25 - 1500
Rh249,7
343,5
1,100
hp th ca nguyn
t lun c ph nn
NiPh
232,0
10,0
10,0km theo. Ngha
10,0 l ti v tr vch
200,ph cng
+324,70
Tnh cht,
chtlng0,002
v cc c 0,010
trng
k thut ca
mi my
quang
ph ca
Cu
2.000
0,000002
238,30
07,5
228,8
KK vo.
- KK
C2H2
0,01
0,003
2th-0,2
Rb
780,0
- C2H2phn tch
0,05 nh (mc
0,03
10
c cng
nn cng thm
nng
ppm hay0,02ppb)
phn
PbCd
217,0
2,0Trong
3,0
3,0
10,0,1
tng hng sn xut my o ph hp th nguyn t (bng 11.5a).
Cs
852,1
KKph
- KK
C2H2
0,1
0,03
Ru
349,9
200,0
100,0
1,0
- 0,3 45,00,2 -- 10
2 - 150
ca Pt
ph
nn
cng
kh ln,
nn- C
ny
2H2l:
Al 309,30
0,04
Fe265,9
248,30
200.000
+ Cc iu kin thu nhn tn0,02
hiu cng
vch ph. Yu0,00003
t ny lin quan n h3 nhn
SnCa
235,5
9,0
200,0
100,
422,7
KK
- 100,0
C2H2
0,05
0,006
- 8 1,20
196,0 tc,
Ar -AAS
H2 chnh cn
0,2
0,2 60,0 0,1
+Se
Ph
che
vch
ph
o,
396,20
0,07
quang
inlin
v vng
ph.
VKCa
318,5
100,0
400,0
400,
766,50
2.000
0,000005
422,7
N2O -KK
C2-0,0002
HC2H
2 2
0,03 0,5
0,008
0,05 - 42 -0,3
Se
196,0
2,0
50
+ Tng
t sng ngn sang sng
di,
0,10
80,0 1,
Bng
11.5 dn 308,20
Zn 213,9
0,05
0,08
0,08
Cr
KK N
- C2H2
0,08 2,0
0,020,7
0,2 - 15
Si 357,9
251,6
2O - C 2H 2
4 - 400
Gii+hn
Pht
hin
t aufs,
theo AAS
Cng
phca
nncc
t nguyn
0 n 1,7
c khi
n 2,0 aufs.
394,40
1,20
120,0
Pb
217,00
0,01
20.000
0,00002
2
Cr
C
0,150,05CRA-63: 0,15
- 25
Ag357,9
328,1
KK
C2H2 Perkin Elmer,
0,006
0,1 - 10
2O 2H-2hng
Ghi
ch:
- HGA-74: NMy
ca
My
ca hng 0,4
VARIAN,
V th phi loi tr, nht l khi o nng nh trong vng VIS.
Cr 357,90
0,05
15,00,2 - 20
Co
240,7
KK -Shandon,
C2H2
0,1
0,02
589,0
KK
- C20,1
HUSA.
0,01
0 004
0,02200
-2
2
A-3470:
My
ca hng
PtNa
265,90
100,000
0,002
Cc
phng
php
b
chnh
nn
Cu
KK Instrumentat
- NC2H2
0,04
0,01
Sr 324,8
460,7
0,1
0,02 23,00,1 - 10
0,2 - 20
0,10
2O - C2H 2
IL-355:
My359,40
ca hng
Ion Lao.
Sb
250.000
10
Hin
nay c425,40
4 phng
tr) ph nn:0,1 0,0001
Ga
287,4
KK -php
1,0
Ta217,60
271,5
NC2H2
C0,04
H2 chnh (loi
12,0
4,0 45,02 - 150
30 - 2000
2O -
2b
0,20
Khong xcNguyn
nh trong
php
o
AAS
t
Theo php o F - AAS
Theo php ETA - AAS.
Ge
265,2
Nph.
C2H-2C2H2
1,5 0,5
0,4 0,2
3 - 200 80
Te
214,3
KK
2O Phng
php
2
vch
Khi
nim nygn lin vi
mt nguyn 50.000
t v mt vch
ph ca nguyn 1 - t
Se
196,00
0,2
0,0005
50
Vch o
Tng i
Tuyt i
Tng i
Tuyt i
Cu
324,80
0,008
27,0
Au
Ti
242,8
276,8
KK
KK
C
H
C
H
0,2
0,4
0,5
0,06
0,5
20
1
2
2
2
2
c s
dng php
phn
tch
n trong
mt tc
iu
nht nh chn. Trong php o ph80
hp
Phng
dng
ngun
sng lin
kin
b chnh.
(nm)
( a)
( a)
(p,g/mL)
p
(pg/mL)
p
th nguyn
Hf
Sn307,3
224,6
t, vic
nhNlng
2O -KK
Cmt
2-HC
2
nguyn
t da
15,0
vo
0,4phng trnh
10,0c
0,1bn 54,0
30 - 20001 - 60
2 H2
327,40
0,015
Sn
235,50php da theo hiu ng0,02
100.000
0,0001
10
Phng
Zeeman.
b
Ag 328,10
0,002
5.000
0,000001
1
In
KK
C2H2
0,4
0,2
1
100
Ax.
=
K.C
(11.7)
Sn303,9
224,6
N
O
C
H
2,4
0,6
5
300
2
2
2
216,50
0,050
162,0
Phng
php
dng
ngun
n
sc
hot
ng
theo
2
ch
dng.
Sr
0,00005
Ir
208,9
KK N
- cu
C2H2
1,010.000
2,5ch
- 20
200
Ti460,70
364,3
2O -0,002
Ctrn
2H2(mc 11.1.1),
2,0trong mi0,6
0,4h ny A
-1500
Nh
chng
ta nghin
quan
ph
thuc
Al
309,30
0,02
20.000
0,00002
25
Hin nayFecc
my AAS bn trn th trng0,005
thng thit k dng 2 phng
php b
248,30
20,0th vit:
tuyn tnh
vo C khi
b = 1,N2ngha
l khi nng C8,0
rt
nh. Khi 3,0
chng
Ir
ON
- 2CO
-300-20000
1500 20
W208,9
255,1
10,0
4,0 ta c 20
2H2- C 2H
As
193,70
0,15
25.000
0,0001
364,30
0,05
100.000
0,002
2000
chnhTinn.
l phng
php 2 v 3.
Ngi mua0,007
ty
yu cu m chn
loi35,0
no cho thch
hp.
248,80 KK
= -K.C
x2O
Fe
-A
0,1
0,2 - 20
U 248,3
358,5
NC2H2
C2H 2
150,0 (II.8) 0,02
80,0
2 - 150
Sau y lAu
nguyn
tc ca mi phng
php b chnh
nn (BC). 0,0001
242,80.
0,01
100,000
10
302,10
0,025
72,0h
Ngha
l
ch
trong
mt
khong
nng
C
nht
nh
th 2,0
mi
quan
V
318,50
0,05
20.000
0,001
PbV2318,4
1 7,0
KK - NC2H2
0,15 1,0 v nh,0,05
0,3gia
- 25
0,02100
-2
2O - C2H 2
Ba 553,50
0,01
20.000
0,0005
50
Pb
C2H2
0,30,01
0,07
0,7550
- 50
Zn283,3
213,9 252,30KK - KK
- C 2 H2
0,003 100,0
- 2000
0,030
Li
Zi670,8
360,1
230 228
226
232
KK - NC2H2
2O - C2H 2
0,0215,0
0,005
5,0
0,05 - 44 - 400
231
227229
Phng php 2 vch ph

Nguyn tc:
Chn 2 vch ph o, l:
+
vch
ca
nguyn
phn
tch (gi l vch PT- PT) ta c APT

+
vch
ca
nguyn
so
snh (vch so snh- ss) ta c Ass

+
Cng
thc
tnh
nh sau (hnh 11.2):

Ath = (APT - Ass)
iu kin:
+ Cng ca ASS nm trong vng tuyn tnh, nhng phi nh.
+ Nng ca cht so snh phi nh v khng i trong mi mu.
+ Vch so snh phi gn vch PT, phi cch nhau t hn 10 nm.
+ Vch XSS phi gn, v r rng.
u v nhc im:
+ n gin, khng cn trang b BC.
+ B chnh trit .
+ Nhng li lm gim mt nhy.
Phng php dng ngun sng lin tc
Nguyn tc:
+ V ph nn l lin tc,
+ Nn dng ph lin tc BC.
+ Ngun sng lin tc c dng:
n HQ Hydro (D2-lamp) cho vng t ngoi (UY: 190-3 60nm), n W-Halid
cho vng kh kin (VIS: 380-1000 nm).
Cch o ph:
+ Phi o cng ca vch ph phn tch 2 ln.
+ Trc tin o cng tng Atot (khi D2-lamp khng hot ng), o nn An, khi D2lamp hot ng (n HCL khng hot ng).
233
Nh vy cng thc s l: Am = (Atot - An)

iu kin:
+ D thc hin, nhanh
+ C trang b BC h n D 2+
B chnh
trit
, n(VIS),
ht c 2 aufs cng nn.
Lamp (UY)
v n
W-Halid
C b
mch
BChi(BC'++Thm
phnin
trang t
b BC
t tin:
Modul).
Phng php dng ngun n sc hot ng 2 ch dng
u v nhc im:
Nguyn tc:
+ Trang
BC khng
Da
theobhin
tng t,
t o ca vch ph cng hng (vch nhy) ca nguyn t
cng +D
n
HCL
rt ln. Lc ny vch ph b ch i, phn tnm vch ph ch cn nn.
thc
hin,
+ B
trit ,
ch cng n HCL bnh thng ta s c A tot,
Nh
vychnh
nu ta khng
o cng
lc u
c
hnln
1,3cng
aufs. cao (100-150 bnh thng) v o th ta ch c cng
sau
khi
chonn
nnh
HCL
ph nn.
Nh vy
cng
thc
ph Ath
l:
Phng
php
da theo
hiuca
ngvch
Zeeman
- Nguyn
tc:
+ Khi c hiu ng Zeeman, vch ph ca
nguyn t PT b phn thnh 2,4,... nhnh i
Ath = (Atot - An)
xng qua tnm vch (v tr o), cn ti v tr tnm
(1)
Hiul ng
Hieftje
Lan) pht hin. Nn phng php ny gi l phng
vch ch
nn ny
ca do
phSmith
lin tc
(hnh(H
11.4).
php BC Smith Hieftie.

+ Nh vy nu o ph khi c v khng
iung
kin:Zeeman th ta kh b c ph
c hiu
nn lin
tc.
+ C
mch BC theo nguyn.l Smith Hieftje.
iu kin:
+ C n HCL hot ng c dng rt cao.
+ C h thng in t iu khin BC
Cch o ph:
a+
(BC- Modul),
++Trc
tin o cng
hp
C trang
b ngun
cp th,
hiukhi
ngHCL dng bnh thng,
(1
+Zeeman.
o cng hp th, dng
~~
Hnh 11.4
cao ca-Cch
n HCL,
o:
Bchlnhni
Ath
Saunn
ly ta
hiu
2 ln
ta phn
+ BC
o s
ph
ca o,
vch
tch
c
cng
thc.
ti 2 thi
im:
X
0,00 5 run
(2)
a-
A
c hiu ng Zeeman
Dtot dng bnh thng
hiu ng Zeeman
theo hiu ng Zeeman

Dn dng cao
o cng
u v +
nhc
im: tng Atot, khi khng c hiu ng Zeeman,
+ Phng
php
BC trit
+ Sau
ny
o cng
.
nn An, khi c hiu ng Zeeman.
+ n Nh
HCLvy
dng
kh cao
l rtca vch ph Ath l:
cng
thc
Hnh
Ath =Hnh
(Atot
- An)
t (gp 3 ln n HCL thng).
11.5
u im v nhc im:
+ n HCL hot ng c dng
BC nn theo phng php Smith Hieftje
rt cao, rt chng hng.
234
235
11.1.8 Ti u ha cc iu kin cho php o AAS

Bng
11.6xc nh mt nguyn t theo mt k thut o no , chng ta cn phi c mt quy trnh
Mun
Vng
php.
o Ngha l phi c mt phng php phn tch n nh. C nh th
phn
tch tuyn
c th tnh
theoca
k thut
chng taNguyn
mi thutc
qu chnh xc.
Mun
nhng ngi Vng
lm phn
tchtnh
trc
ht phi tin
vchkt(nm)
nhyth,
(p,g/mL)
tuyn
(pg/mL)
hnh nhng nghin cu, th nghim ti u ha cc iu kin phn tch v xy dng mt quy trnh
phn tch c th theo k thut m mnh nh p dng cho mc ch ca mnh t ra. Cng vic ny
Al 309,3
bao gm nhng vn sau y cn c gii quyt:
396,2
Chn cc thng s ca my o ph
237,3
0,2
0,5 - 15,
0,5
1 - 20,
1,2
2 - 30,
Cc thng s ca h my o ph AAS thng bao gm cc yu t.
257,4
2,5
4, - 50,
VchBaph
o. Vch ph c chn xc nh nguyn
553,6
0,08 t mnh mong mun.
0,1 - 10,
Vch ph
ny phi tha mn iu kin:
455,4
0,1
0,5 - 15,
48,0 hay trng lp. 50 - 500,

+ Khng350,1
b cc vch khc quy ri, chen ln gy nhiu
Cr 357,9
+ Phi r rng v nt, c di sng chnh xc.
0,03
0,1 - 10,
0,06tnh vo nng 0,2

- 15, mt vng nng
+ Cng359,4
vch ph hp th A phi ph thuc tuyn
C trong
nht nh. 425,4
0,3
+ Vch 429,0
ph phi nm trn mt nn khng qu ti. 0,6
1 - 25,
1,2 - 30,
Fe 248,3
- 10,
Tt nhin
khi cn xc nh cc nng rt nh th0,05
phi chn vch ph 0,1
c
nhy cao v ngc
li, khi xc nh
cc nng khng nh th cn chn cc0,15
vch km nhy hn.0 3 - 15,
252,3
Cng271,9
dng lm vic ca n HCL. Cng0,25
dng in lm 0,5
vic- 25,
ca n catot rng
(HCL), ni chung
nn chn cng dng nm trong vng
so vi
cng cc i
372,0
0,5t 60% n 85% 0,8
- 30,
ghi trn n HCL. Khi cn nhy cao th chn cn di, cn khi cn n nh cao th chn cn trn.
Mg 279,5
0,02
0,1 - 6,
Khe o ca my quang ph. Khe o (khe vo v khe ra ca chm tia) c nh hng n
279,8
0,04
0,2 - 8,
nhy v vng tuyn tnh ca php o. Ni chung nhiu my quang ph hp th thng c khe o thay
280,1
0,1
0 4 - 15,
i c theo cc gi tr t 0,2 n 10 nm theo 5 hay 4 bc. V d 0,2; 0,4; 0,8; 1; 2 v 10 nm. Nhng
0,3 t 0,2 n 1 nm.

0,5 Do
- 20,
i vi nhiu 403,1
vch ph th khe o ph hp l nm trong vng
cn phi chn
- 10,
ch mt giNi
tr230,0
ph hp nht cho php o nh lng mt0,04
nguyn t theo vch0,1
ph
c chn, lm
sao ch cho va
vch ph cn o vo khe o l tt nht.0,1
331,1
0,2 - 16,
Burner234,6
Head Hight. Chiu cao n nguyn t 0,25
ha mu, nu chn khng
ng ra s khng
0,5 - 25,
0
,
3
-
nhng thu c
nhy km v tn hiu o khng n nh,
341,5
0,3 m ng thi li b nhiu yu t nh
hng.
Cu 324,7
0,01
0,1 - 5,
Thi
gian o. Thi gian o, s ln o cng vch ph. Yu t ny ph thuc vo c
327,4
0,02
0,3 - 8,
trng k thut ca tng my quang ph v ty thuc vo k thut nguyn t
217,9
0,5
0,8 - 20,
216,5
0,7
1 - 25,
Si 251,6
0,06
0,2 - 12,
250,7
1,2
2 - 25,
288,2
8,0
10 - 80,
237
236
ha mu. Vi php o F-AAS th l thi gian thu c tn hiu hp th n nh, vi php o ETAAAS th li l thi gian nguyn t ha mu (xem chng 8).
Lng mu. l tc dn mu, lng mu bm vo.

Vng
tuyn tnh ca vch ph c chn nh lng. Yu t ny cng cn c xc nh
chnh xc cho tng vch ph chn nh lng nguyn t phn tch. C nh th mi c th chun b
mt dy mu chun ph hp cho php o ca mnh. V cc kt qu thu c nm trong vng tuyn
tnh ca vch ph bao gi cng c chnh xc cao.
Phng tin ch th kt qu o. N c th l my t ghi lc cng vch ph, my hin

s digital, my printer hay my tnh ch trc tip hm lng (nng ) ca nguyn t phn tch. Tt
nhin chn phng tin no l ty thuc vo trang b m mnh hin c v l ph hp nht i vi
mnh trong iu kin thc t .
B chnh nn khi o. Yu t ny c thc hin hay khng l ph thuc vo vch ph c chn

o. Nu nn ca ph c nh hng th phi thc hin php o c b chnh nn loi tr nh
hng v ngc li, nu khng nh hng th khng cn thit. Trong php o ETA-AAS th yu t
ny rt quan trng, n nh hng rt ln n kt qu phn tch. Do cn phi ht sc cn thn trong
mi trng hp c th ca mi loi mu phn tch. V nn ca mu l mt nguyn nhn gy ra nh
H nhn quang in nhn tn hiu AAS. Yu t cui cng trong vn ny l th lm vic ca

nhn quang in. Yu t ny l thang nng lng hp th ca php o AAS. Trn cc my thang ny
c chia thnh 100 n v.
Trong vng t 70 n 100 l vng lm vic ph hp ca th nui nhn quang in cho cc my o
ph hp th nguyn t v vng ny c nh du mu xanh hay mu en. Trong cc php o phi iu
chnh nm GAIN kim ch thang nng lng nm trong vng ny v phi gi mt gi tr chn trong
sut qu trnh o nh lng mt nguyn t.
Cc iu kin nguyn t ha mu
Vn ny ty thuc vo k thut c chn nguyn t ha mu. N c nghin cu k
trong chng II. Do y nu li mt s iu cn ch . C th l:
Vi php o F-AAS. Cn phi chn cc thng s sau y:

Nhit ngn la, tc l chn thnh phn kh chy to ra ngn la c nhit ph hp.
+ Chiu cao ca n nguyn t ha mu (burner head).

+ Tc kh mang v tc dn mu vo bung aerosol ha.
+ B dy ca lp hp th, tc gc nghing n nguyn t ha mu (burner head).
Vi php ETA-AAS. Bao gm nhng iu kin:
238
Thi gian, nhit ca cc giai on sy mu, tro ha, luyn mu v thi gian nguyn
t ha o cng vch ph.
+ Kh mi trng cho qu trnh nguyn t ha mu.
+ Cng sut t nng cuvet graphit nguyn t ha mu.
+ Lm sch cuvet graphit.
+ Lng mu a vo cuvet nguyn t ha o ph.
Cc yu t nh hng
Cc nh hng v ph.
Cc nh hng v vt l.
Cc nh hng ha hc ca cc Cation v Anion c tng mu.
nh hng ca thnh phn nn ca mu.
Cc yu t ny c cp k trong chng 10. Tt nhin cc yu t ny cng ch c
trong mt s trng hp nht nh v nhiu trng hp l khng c. Nhng cng cn phi
bit chnh xc khi n xut hin th tm bin php loi tr ph hp.
Chn quy trnh x l mu ph hp
X l mu l cng vic u tin ca ngi lm phn tch. Nu x l mu khng tt th tt
nhin s c kt qu phn tch sai, hoc nh (lm mt), hoc ln (lm nhim bn thm).
Trong phn tch lng vt (vi lng), giai on x l mu l cc k quan trng i vi
c qu trnh phn tch. V trong giai on ny chng ta c th lm mt hay lm nhim bn
thm nguyn t cn xc nh c khi n hng chc, thm ch c khi n hng trm ln nu
chn quy trnh x l mu sai v cc ng tc trong qu trnh x l mu thc hin khng cn
thn.
Cc ngun gy sai trong qu trnh x l mu c th l:
+ Mi trng lm vic khng sch yu cu.
+ Dung mi, ha cht (axit) dng x l mu khng tinh khit.
+ Dng c ng, cha mu khi x l khng tt, khng sch.
+ Nc ct khng tinh khit.
Phng php chn x l mu khng tch chit c tt nht nguyn t cn phn tch
vo dung dch phn tch.
Cc cht chun khng t yu cu cao.
l cc vn cn c ch trong mi trng hp c th.Cc vn ny s
239
c trao i chi tit trong mt xemina ring.
Phng php chun ha nh lng

Ngoi 4 yu t trn, nhng nu phng php chun ha c chn nh lng khng ph
hp th cng cha thu c kt qu chnh xc v ph hp vi thc t. Vn ny ty thuc vo bn
cht v thnh phn vt l ha hc ca mu phn tch.
V th phi ty theo tng trng hp c th m chn phng php ng chun hay phng
php thm tiu chun xc nh nng ca nguyn t phn tch trong mt i tng mu nht
nh.
Trn y l tm tt cc vn cn thit trong qu trnh ti u ha cc iu kin th nghim
chn ra cc iu kin ph hp xy dng mt phng php theo mt k thut o nht nh.
Ngha l mun xut mt phng php phn tch th phi tr li c nhng vn mt
cch chnh xc v r rng.
chnh l cng vic nghin cu xy dng quy trnh ca cc nh phn tch. Cn khi c mt
quy trnh phn tch n nh ri th bt k k thut vin phn tch no cng c th tin hnh phn tch
c.
Cc phng php phn tch c th

xc nh nng (hm lng) ca mt nguyn t trong mu phn tch theo php o ph hp
th nguyn t ngi ta thng thc hin theo cc phng php sau y, da theo phng trnh nh
lng c bn ca php o ny qua vic o cng ca vch ph hp th ca nguyn t phn tch v
xc nh (hay pht hin) nng ca cht phn tch trong mu o ph theo mt trong cc phng
php chun ha sau:
Phng php ng chun;
Phng php thm tiu chun;
Phng php th khng i;
Phng php dng 1 mu chun.
Phng php th chun (ng chun)

Phng php ny cn c gi l phng php ba mu u. V nguyn tc ca phng php
ny l ngi ta da vo phng trnh c bn ca php o A - K.C v mt dy mu u (t nht l ba
mu u) dng mt ng chun v sau nh ng chun ny v gi tr A x xc nh nng
Cx ca nguyn t cn phn tch trong mu o ph, ri t tnh c nng ca n trong mu phn
tch.
240
Do trc ht ngi ta
phi chun b mt dy mu u,
dy mu chun (thng thng l
5 mu u) v cc mu phn tch
trong cng mt iu kin. V d
cc mu u c nng ca
nguyn t X cn xc nh l C i,
C2, C3, C4, C5 v mu phn tch l
Cx1, Cx2 , . . . Sau chn cc
iu kin ph hp v o cng
ca mt vch ph hp th ca
nguyn t phn tch trong tt c
cc mu u v mu phn tch
c chun b trn.
Hnh 11.6
V d ta thu c cc gi th chun ca phng php ng chun
tr cng tng ng vi cc
nng l Ai,
A
2, A3, A4, A5 v Ax1, Ax2
v.v... By gi trn h ta A - C
theo cc im c ta (C 1A1),
(C2A2), (C3A3), (C4A4), (C5A5)
ta s dng c mt ng biu
th mi quan h A - C. chnh
l ng chun ca phng php
ny (hnh 11.6).
Hnh 11.6
th chun ca phng php ng chun
Tip nh ng chun ny v cc gi tr A x chng ta d dng xc nh c nng C x.

Cng vic c th l em cc gi tr A x t ln trc tung A ca h ta , t k ng song song vi
trc honh C, ng ny s ct ng chun ti im M, t im M ta h ng vung gc vi trc
honh v n ct trc honh ti im C x, Cx y chnh l nng phi tm (hnh 11.6).
Phng php ny n gin, d thc hin v rt thch hp vi. mc ch phn tch hng lot mu
ca cng mt nguyn t, nh trong kim tra cht lng thnh phm, kim tra nguyn liu sn xut. V
mi khi dng mt ng chun chng ta c th xc
241

(Aoc
, O). Sau

xc
Ct
bithng
chng
ta lm
nhphn
sau: tch. l u im ca
x cha
nh
nng
canh
mtnng
nguyn
trong
trm
mu
phng
phpI. ny.
trong nhiu
hptri,
chng
chun
cCmt
dy
Cch
Ko Song
di ng
chuntrng
v pha
n tactkhng
trc th
honh
ti bim
x. on
muX chnh
u tha
cc
iu
tm
quy(hnh
nh11.7).
cho phng php ny ( trnh by trong mc
OC
bngmn
gi tr
nng
kin
C x cn
11.1.2)Cch
nn II.
khng
xccnh
xc
v tr ca ng chun v nh th tt nhin kt
Cng
thc
xc chnh
nh C
x bng cch t gc ta k mt ng song
qu phn
s mc
sai v
s ln.
NghaAlo khi
phn
tch song
c thnh
v chng
song
vi tch
ng
chun
t im
k mu
ng
song
vi phn
trc phc
honh,tphai
ng
ta cha
khng
th chun
c mt
dy gc
mu vi
u trc
nghonh,
n nnng
s b nh
ny
ct bit
nhauchnh
ti xc
imthM,
t im
M hb ng
vung
ny
hng
ca nn,
ca thnh
phn
caOAC
mu.
chnh
im
phng php ny.
ct
trc honh
ti im
C o, Chnh
on
x l
bng
gi trlCxnhc
phi tm
(hnhca
11.7).
Trong nhng trng hp nh th, tt nht l dng phng php thm tiu chun xc nh
Phng
php
ny
nng ca nguyn t phn tch trong mu, hay bin i ca mu sang nn t to ph hp
im l qu trnh chun b mu
cho c mu u v cc mu phn tch.
d dng, khng cn nhiu ha
Phng
thm
cht
tinhphp
khit
caotiuchun
chun b
dy
Trong
phn tch,
mu thc
u tnhn
to. c
Mtbit l xc nh lng vt cc kim loi, khi gp phi cc i
tng phn
tch ctrthnh
phnhon
phc tp v khng th chun b c mt dy mu u (mu
khc
li loi
c
chun)nh
ph hng
hp v v
thnh
phn phn
vi mu phn tch, th tt nht l dng phng php thm tiu
ton
thnh
chun.
Chcng
nh th
tr c
ca
mu
nhmi
culoitrc
vt yu t nh hng v thnh phn ca mu (matrix effect).
l ca cc
cht to
Nguyn
tcthnh
ca mu.
phng php ny l ngi ta dng ngay mu phn tch lm nn
Nhng
chmu
u,
rng,bng
nng
chun bphi
mt dy
cch ly mt lng mu phn tch nht nh v gia thm vo
thm lng
vo nht
ca nh
nguyn
t
nhng
ca nguyn
t cn xc nh theo tng bc nng (theo cp s
phn
tch
phi
theo
tng
bc
v
cng). V d lng thm vo l ACI, AC2, AC3, AC4, nh th chng ta s c mt dy mu
khong
cch
chun nh
trongca
bngcc
sau, bc
trong Cx l nng (hm lng) ca nguyn t cn xc nh
phi
xp phn
x bng
trong mu
tch. nng C x
phi tm.
Bng dy chun ca phng php thm tiu chun.

C nh th th phn ni suy tuyn tnh mi c ngha chnh xc.
Phng php ny c s dng rt nhiu trong phn tch lng vt v lng cc nh cc
nguyn t kim loi trong cc loi mu khc nhau, c bit l cc loi mu c thnh phn vt l v ha
hc phc tp, cc mu qung a kim. Co
ng
thi y cng l mt
Lng mu phn tch
phng php phn tch.
Cx
C2
C3
C4
phng php xc nh pht
AC1
AC2
Cx
Cx
hin ca
Cx
mt
<
Cx
C5
<
Cx
<
Lng
Phng
php thm
thvo
chun c nh 0
C1
5
C
4
C
3
C
Nguyn tc ca phng php ny l mun xc nh mt nguyn t no , trc ht ngi ta
Cht khc
Cc cht khc l nh nhau
cng phi dng mt ng chun nh trong phng php ba mu u, phng php ng chun.
Ax o c
Ao
Al
ng chun ny c gi l ng chun c nh (ng chun khng i) v ng chun

ny c dng lu di. Nh vy mun xc nh c nng C x cha bit, ta phi chuyn cc gi tr
Tip ng
vcng
kin chun
th nghim
phxchp
v mtvch
ph vn
ca
Axl tng
cc chn
gi trcc
A xoiu
ca ng
c nh
nh Cng.
gii quyt
nguyn
t phn
tin hnh
ghi cng hp th ca vch ph theo tt c dy mu u.
ny ngi
ta ctch,
hai cch
khc nhau:
V d chng ta thu c cc gi tr tng ng l Ao, A l3A2, A3, v A4.. By gi t cc gi tr
cng ny v ng vi cc nng thm vo ca nguyn t phn tch chng ta dng mt

ng chun theo h ta A - AC. chnh l ng chun ca phng php thm (hnh
11.7). ng chun ny ct trc tung A ti im c ta
242
243
y k c
xo kAxl
gil h s
(a)
chuyn ca gi tr cng A
ca vch
ph gia hai
ln o trong cng mt iu kin th nghim.

Mun th mi khi phn tch ta ghi li ph ca mt mu chun, v d thng dng nng Ca.
Nh th, ta c gi tr A xo-3 ca ng chun c nh, v hm nay ta li c gi tr A xl-3, do h
s chuyn k s c tnh theo cng thc:
k: A
xo-3/Axl-3
(b)
Sau khi c h s k ta em n nhn vi cc gi tr cng A xl ca ngy lm phn tch ta s thu

c cc gi tr cng tng ng vi ng chun c nh. By gi ch chiu cc gi tr vo
ng chun c nh l tm c cc nng C x.
Cch th hai: T thc t phn tch khi nghin cu cc ng chun ngi ta thy rng, trong
cng mt iu kin th nghim, i vi mt nguyn t khi o trn mt vch phn tch, nu ng
chun dng c t dy ph ca cc mu chun ghi trn cc ln khc nhau, th chng u l nhng
ng thng song song vi nhau hoc trng nhau (hnh 11.8a). Ngha l cc ng c cng h s
gc. T thc t ny c th suy ra cch dng ng chun phn tch mi ch nh mt mu chun m
khng phi tnh h s chuyn k nh trn. Mun th, khi ghi ph ca cc mu phn tch chng ta cng
ghi li ph ca mt mu chun dng dng ng chun c nh, v d nng Ca. Sau cng
chn mt vch phn tch dng dng ng chun c nh, o cc gi tr A x ca chng v gi tr
Ax-3 ng vi nng Ca. T cc gi tr A x-8 v nng Ca t ln h to dng ng chun
c nh chng ta c mt im A, ri qua im A ny ta v mt ng song song vi ng chun c
nh th ng ny chnh l ng chun phn tch. Dng n v cc gi tr A x ta s tm c cc nng
Cx ca mu phn tch (hnh 11.8b).
Trong thc t, nu my o tt, iu kin mi trng khng kh ( m, nhit ) khng i v
cc iu kin thc nghim tht n nh, th cc ng chun (I) v (II) hu nh trng nhau Trong hai
cch nu, th cch th hai c ng dng nhiu hn v n n gin v khng phi tnh ton phc
tp nh cch th nht.
Phng php th khng i rt ph hp i vi php phn tch hng lot mu t ngy ny
qua ngy khc. V trong mi ngy phn tch chng ta khng phi ghi ph li ca ton b dy mu u
nn tit kim c thi gian, mu chun, ngha l c tnh cht kinh t hn phng php ng chun.
Tuy th nhng phng php ng chun (ba mu u) hay phng php ng chun c nh
u ging nhau l u phi chun b mt dy mu chun c iu kin ca mu u trong php phn
tch quang ph nh lng. iu ny nhiu khi khng thc hin c. c bit i vi nhng trng
hp mu phn tch c thnh phn phc tp m chng ta cha th bit c chnh xc. V th cng
khng th chun b c mt dy mu u c thnh phn ha hc v vt l ng nht vi mu phn
tch. l
244
thc t v trong nhng trng hp th nh hng nguyn t c s v nguyn t th ba n

kt qu phn tch l rt r. iu ny th hin r khi xc nh cc nguyn t vi lng. Lc ny
chng ta phi hoc l thay i nn ca mu (Modify matrix) nu cch ny c hiu qu, hay l
dng phng php thm tiu chun.
Phng php mt mu chun

Khi c mu chun
Trong nhng trng hp n gin, chng ta cng khng cn pha mt dy chun dng
th chun, m c th tnh ngay gi tr C x nh mt mu chun Cl ca cht phn tch. Ngha
l chng ta c:
V i mu phn tch:
Ax = a. Cx (a)
Vi mu u:
Ao = a.Cl (b)

C: (Ax/Ao).Cl (11.6) Nh vy khi o c
v ch vic nhn n vi gi tr Ci l chng ta
gi tr Ax
vAo ta c t scachng,
c gi trnng Cx phi tm theo
biu
thc (11.6).
Khi khng c mu chun
chun theo phng php thm v tnh ngay gi tr Cx nh mt lng chun AC 1 ca cht phn
(a)
a C
. x
245

Atch= a.(Cx + ACl)
(b)
Do cm (a) chia cho (b) chng ta c:

C = [Ax/(Atch-Ax)]. AC1
(11.7)
Nh vy khi o c gi tr Ax v Atch ta c tnh c nng C x phi tm theo biu

thc (11.7).
Nhng mt iu phi ch l nng thm vo ACl v cc gi tr C x phi nm trong
vng tuyn tnh ca phng php.
Trn y
l cc phng
php
nh
lng ch
yuhay csdng. Tt
nhin
mi phng
php u c nhngu
im v nhc im nht nh ca
n, v ngi

Cc kiu phng php phn tch theo AAS
Trong php o ph hp th nguyn t xc nh mt nguyn t hay mt hp cht
ngi ta c th tin hnh phn tch ngay chnh cht theo ph hp th nguyn t ca n,
nh phn tch cc kim loi, hay qua vic o ph hp th nguyn t ca mt cht khc, khi
cht phn tch khng c tnh cht hp th nguyn t, nhng cht ny li c mt s tng tc
rt nh lng v mt ha hc theo mt phn ng ha hc nht nh vi mt kim loi c ph
hp th nguyn t nhy. Do xut hin hai loi phng php phn tch nh lng theo ph
hp th nguyn t, l:
Cc phng php phn tch trc tip, cho cht c ph AAS v
Cc phng php phn tch gin tip, cho cht khng c ph AAS.
Sau y chng ta s nghin cu mt cch tm tt v hai loi phng php phn tch ny.
Cc phng php xc nh trc tip
v nguyn tc
th tt c cc nguyn
tv cccht c
phhp
th
nguyn
chng ta u c th xc nh n mt cch trc tip theo ph hp th nguyn t ca n t dung
dch mu phn tch. Ngha l cc phng php xc nh trc tip ch ph hp cho vic xc
nh cc kim loi c vch ph hp th nguyn t. V cc kim loi u c ph hp th nguyn
t ca n trong nhng iu kin nht nh. Theo cch ny, ni chung trong nhiu trng hp,
mu phn tch trc ht c x l theo mt cch ph hp c dung dch mu c cha
cc Ion kim loi cn phn tch. Tip tin hnh nh lng n theo mt trong cc cch
chun ha bit (nh theo phng php ng chun, phng php thm, hay phng php
mt mu u,... c trnh by trong mc 11.2 trn). y l cc phng php phn tch
thng thng, v ang c dng rt ph bin, xc nh lng vt cc kim loi trong
cc i tng mu hu c v v c khc nhau theo ph hp th nguyn t ca n. V th
ngi ta gi i
246
tng ca cc phng php phn tch ny l phn tch kim loi trong cc loi mu v c v hu c. V
d cc mu v c l qung, t, , khong liu, mui, oxit, kim loi, hp kim, xi mng, nc, khng
kh v cc mu hu c l mu thc phm, ng, sa, hp, rau qu, ung, gii kht, mu, se
rum, nc tiu, cc mu cy v sinh hc.
Khi phn tch cc loi mu ny th nguyn tc chung l gm hai giai on.
Giai on I: X l mu a nguyn t kim loi cn xc nh c trong mu v trng thi dung
dch ca cc Cation theo mt k thut ph hp, chuyn c hon ton nguyn t cn xc nh vo
dung dch o ph.
Giai on II: Phn tch nguyn t cn thit theo ph hp th nguyn t ca n theo nhng iu
kin ph hp (mt quy trnh) c nghin cu v chn ra.
Tt nhin, y giai on I l cc k quan trng. V nu x l mu khng tt th c th lm mt
nguyn t cn phn tch hay lm nhim bn thm vo. Ngha l vic x l mu khng ng s l mt
ngun sai s rt ln cho kt qu phn tch, mc du phng php phn tch c chn l ph hp
nht. Vn ny c bit c ngha ln trong phn tch lng vt cc nguyn t.
Cc phng php phn tch trc tip ny l thch hp xc nh cc kim loi, m bn thn
chng c ph hp th nguyn t. Nhng trong khong nm nm li y, nhiu phng php phn tch
gin tip xut hin phn tch cc cht khng c ph hp th nguyn t, v d nh xc nh cc
Anion, cc nhm phn t, cc hp cht hu c, cc dc phm.
Cc phng php xc nh gin tip cc cht bng AAS

Nguyn tc chung
y l mt phm vi ng dng mi ca php o ph hp th nguyn t phn tch cc cht
khng c ph hp th nguyn t hay ph hp th nguyn t ca n km nhy. Cc phng php ny
hin nay ang c pht trin v ng dng phn tch cc Anion v cc cht hu c.
Ni chung cc phng php xc nh gin tip cc cht khng c ph hp th nguyn t bng
php o ph hp th nguyn t c da theo hai nguyn tc chnh sau y.
Nguyn tc th nht ca cc phng php ny l nh mt phn ng ha hc trung gian c tnh
cht nh lng ca cht ta cn nghin cu X (cht X cn xc nh) vi mt thuc th thch hp c
ph AAS trong mt iu kin nht nh.
Nguyn tc th hai l da theo hiu ng l khi cht phn tch X c mt trong mu vi mt vng
nng nht nh, th n lm gim hay lm tng cng , vch ph hp th nguyn t ca mt kim
loi mt cch tuyn tnh. Sau y l mt vi phng php c th.
247
11.3.12 Cc phng php phn tch gin tip Cc

phng php theo cc phn ng ho hc
Theo cch xc nh gin tip ny, ngi ta c cc phng php phn tch c th sau y
da theo mt s phn ng ha hc bit:
Phn ng to ra kt ta khng tan (mui hay sunphua)
Ni chung, cht no khi tc dng vi mt Ion kim loi trong dung dch to ra c mt
kt ta t tan, c tnh cht nh lng v c th tch ra c khi dung dch mu th phn ng
c th dng c cho php o ny. Theo nguyn tc ny ngi ta xy dng phng
php phn tch cc Ion SO 42-, Cl C2O42-, po43-, NH4 +. V d xc nh SO 42- ngi ta cho
Ion ny tc dng vi dung dch BaCl 2 hay Pb(NO3)2 c nng xc nh trong iu kin ph
hp to ra kt ta BaSO4 hay PbSO 4- lc tch kt ta khi dung dch. Sau xc nh Ba
hay Pb theo hai cch hoc l trong kt ta sau khi ha tan chng, hoc l xc nh lng Ba
hay Pb cn d c trong dung dch sau khi phn ng vi Ion sunphat. Nh vy t lng Ba
hay
Pb tiu tn
ta Ion SO42- chng ta d dng tnh c hm lng ca Ion sunphat c
kt
trong mu
phn tch. V d cc phn ng c s dng trong cch ny:

Cl- + Ag+ ^ AgCl ^ xc nh Anion Cl Br - + Ag+ ^ AgBr ^ xc nh Anion Br
+ Ag+ ^ AgI ^ xc nh Anion I C2O42- + Ca2+ ^ CaC2O4 ^ xc nh Anion C 2O42PO43- + Ca2+, Ca3(PO4)2 ^ xc nh Anion PO 43SO42- + Ba2+ ^ BaSO4 ^ xc nh Anion SO42SO42- + Pb2+ ^ PbSO4 ^ xc nh Anion SO42PO43- + Mg2+ + NH4+ ^ MgNH4PO4 ^ xc nh Anion PO 43Cng bng cch ny ngi ta tin hnh xc nh penicillin, vitamin B 1, v.v... theo
php
o AASbng cch cho muvitamin Bl
tc dng vi mt lng
xc nh
oC
NaPbO2 trong KOH nng chy 280 V trong iu kin ny, c mt phn t vitamin B 1 bao
gi cng to ra mt phn t PbS. Sau tch ly kt ta PbS, ra sch v ha tan n trong
axit nitric 6M v xc nh Pb. Ri t hm lng Pb ta tnh c hm lng ca vitamin B 1
trong mu phn tch.
Mt khc, y chng ta cng c th xc nh lng Pb trong phn NaPbO2 d khng
tc dng vi vitamin B 1, ri sau cng tnh c hm lng B 1.
Hin nay, theo cch ny, c nhiu hp cht hu c c cha S (lu hunh) c xc
nh bng php o ph hp th nguyn t, nu Ion S 2- trong phn t hu c tc dng c vi
mt Ion kim loi trong mt iu kin nht nh to ra c mt
248
sunphua kh tan c tnh cht nh lng. V th thuc vitamin B1 cc hp cht hu c kiu

diol cng c xc nh theo cch ny.
Penicillin + NaPbO2....................^ PbS
trong KOH nng chy, 280 oC
Vitamin B1 + NaPbO2..................^ Pbs
Theo phn ng to hp cht phc
Cht phn tch X phn ng vi thuc th l mt hp cht phc. Nguyn tc ca cch
ny l cho cht X cn xc nh tc dng vi mt phc cht thuc th kim loi to ra mt
hp cht phc bn c th chit tch ra c. Nhng phn ng ny phi c tnh cht nh
lng. Sau tch ly phc cht v xc nh hm lng kim loi trong phc cht , ri t
tnh ra hm lng ca cht cn phn tch X. V d axit phthalic hay cc mui phthalat c th
c xc nh qua phn ng ca n vi thuc th phc Cu(I)-Neocuproine to ra phc cht
mi l Cu(I)-(Neocuproine) 2 Phthalat. Sau chit ly phc cht ny vo mt dung mi hu
c ph hp, nh MIBK v xc nh hm lng Cu trong phc ny, t tnh ra hm lng
phthalic trong mu phn tch.
Cng tng t nh vy, ngi ta xc nh nng NO- qua phn ng ca Ion NO vi thuc th Cu(I)-Neocuproine to ra phc cht Cu(I)-(Neocuproine) 2_NO3_ chit c
vo MIBK. Sau xc nh Cu trong phc ny bng php o AAS, v sau suy ra hm
lng Anion NO- trong mu.
Cht phn tch X phn ng vi dung dch mui kim loi. Cch ny dng xc nh cc
Anion. Tt c cc Anion no c th tc dng c vi mt Ion kim loi to ra c mt hp
cht phc bn trong mt iu kin nht nh v chit ra c khi dung dch mu th u c
th s dng xc nh cc Anion .
V d xc nh Anion SCN qua phn ng ca Anion ny vi dung dch mui FeCl 3
Fe3+ + SCN
Fe(SCN)2+
Sau chit phc Fe(SCN) vo dung mi etyl ete v xc nh Fe trong dch chit ny
bng php o AAS (c th gii chit phc vo dung dch HCl 2M v xc nh Fe trong dung
dch gii chit ny). Sau ta cng tnh c nng ln SCN trong mu phn tch.
Qua phn ng to thnh hp cht d a axit
Theo cch ny, nhng kim loi, Ion hay hp cht c kh nng to thnh nhng hp cht
axit d a u c th xc nh c mt cch gin tip qua hp cht d a. V d nh photpho
(P), Anion photphat (PO 43-) hay ton silicat (SiO 32-),... c th c xc
249
nh bng cch cho n tc dng vi thuc th molipat trong mi trng axit HNO 3 a 6M,
to ra hp cht d a photpho-molipat kt ta, tch ly sn phm ny, ho tan n trong dung
dch kim 0,5M v xc nh Mo trong dung dch hp cht d a theo vch ph hp th nguyn
t Mo-313,0 nm. T tnh ra lng P c trong mu. Mui asenat v mt s hp cht alcaloit
cng c xc nh theo cch gin tip ny.
Cch ny c dng xc nh P, Si qua thuc th molipic trong mi trng axit
nc c 6M sinh ra hp cht d a ca P vi Mo theo phn ng:
PO4 3" + NH4+ + MoO42- + HNO3 ^ (NH4)3[P(Mo3O1o)4]
m chng ta c dng trong phn tch ha hc xc nh P trong t trng bng
phng php trung ha. Nhng y sau khi c c hp cht kt ta d a ca P, ngi ta
ho tan n trong kim 0,5 M v xc nh hm lng ca nguyn t molipden, bng ph hp
th nguyn t ca Mo, sau suy ra hm lng P trong mu phn tch.
Qua phn ng kh Ion kim loi v kim loi
Mt s cht hu c khi tc dng vi mt s mui kim loi trong nhng iu kin xc
nh, n kh cc kim loi v trng thi kim loi t do c tnh cht nh lng. V d nh phn
ng ca chc andehit vi mui AgNO 3 trong mi trng NH 3 (thuc th Tulene). Tnh cht
ny c ng dng phn tch cc cht hu c c nhm -CHO bng php o AAS. Cc
andehit c xc nh bng cch cho andehit tc dng vi mt lng d AgNO 3 ton b
andehit trong mu phn ng vi AgNO 3 , gii phng ra Ag kim loi, tch Ag kim loi, ha tan
n trong axit HNO 3 v xc nh Ag bng php o AAS theo vch ph Ag-328,1 nm, t
tnh ra hm lng andehit c trong mu phn tch. V trong iu kin ny c 1 nhm -CHO th
lun lun gii phng ra 1 nguyn t Ag kim loi theo phn ng sau:
R-(CHO)n + n(Ag+) ^ nAg o
V d vi andehit focmic (HCHO), th ta c:
HCHO + Ag+ ^ Ago
Phn ng th hay ph hu hp cht phc
Nguyn tc ca cch ny l cho cht phn tch X tc dng vi mt hp cht phc trong
mt iu kin xc nh, to ra sn phm mi bn hn phc ban u. Bng cch ny ngi
ta c th xc nh c cc Anion hay mt s kim loi khng nhy ph hp th qua mt kim
loi nhy ph hp th.
V d nh xc nh Anion F - khi cho n tc dng vi phc Fe(III)-SCN c nng xc
nh. Sau chit tch phn phc Fe(III)-SCN d v xc nh Fe trong phn phc d ny
theo
vch ph
hp
la nkh axetylen
khng kh.
250
thFe-248,3 nm trong
ngn
Bng cch ny La v Ce l cc nguyn t khng nhy ph hp th nguyn t trong ngn

la axetylen-khng kh (DL > 20 p,g/mL) li xc nh c n nhy l
5 - 1 pl/mL. Bng cch bm mu phn tch cha La hay Ce vo dng cht mang nn l dung
dch phc Fe(III)-tartat hay Fe(III)-EDTA. Khi chiu cao ca lc hp th ca vch ph Fe248,3 nm l ph thuc tuyn tnh vo nng ca La v Ce trong phm vi t 0,5 - 18 p,g/mL.
y chnh l mt hng mi phn tch lng vt t him bng php o F-AAS vi
nhy cao.
Phn ng kh hp cht c nhm Nitro (-NO2)
Chloramphenicol, qua chun lng ln Cd(II) sinh ra trong phn ng hay o ph hp th
nguyn t ngn la (F-AAS ) ca dung dch Ion kim loi Cd(II). V d trong mi
axit long (HCl 0,05M),
trng
bt kim loi xp Cd kh nhm -NO2
NH2 hon ton nh lng theo phn ng sau.

3Cd + R-NO2 + 6HCl ^ 3CdCl2 + H2O + R-NH2
Chloramphenicol
Nh vy sau khi phn ng kt thc, ly tnm ly dung dch mui CdCl2 v xc nh Cd
bng php o F-AAS v suy ra hm lng Chloramphenicol theo phn ng trn. Vi cch ny
c th xc nh c Chloramphenicol n nhy 0,1 ppm.
Hon ton
tng
t, nhiu hp cht hu cnitro u
c thxc nh gin
tip
theo php o ph hp th nguyn t [20].

Theo hiu ng tng hay gim cng vch ph AAS
Vic xc nh theo cch ny l da trn nguyn tc l cc cht cn xc nh trong mt
gii hn nng no n c kh nng lm tng hay gim tn hiu hp th (cng ) ca
mt vch ph ca mt nguyn t mt cch tuyn tnh. S tng tc ny c th theo ba cch
sau.
Tng tc an Ion-Cation
y Anion cn phn tch khi tc dng vi Ion kim loi s lm gim cng ca vch
ph hp th ca n, mt cch tuyn tnh, hay lm tng, khi Anion ny nm trong mt khong
nng nht nh. V d dung dch nn Mg 5 p,g/mL, Anion F - lm gim cng hp th
ca vch ph Mg-285,2 nm trong ngn la n kh axetylen- khng kh rt tuyn tnh, khi
nng ca Ion F- trong dung dch mu tng t 1-20. p,g/mL. V d, theo tc dng lm gim
cng vch ph, ngi ta cho cht phn tch X (cn xc nh) tc dng vi dung dch mui
ca mt kim loi c ph hp th nhy mt nng nht nh ph hp v khng i to
thnh hp cht bn v hp cht
251
nhng
ny s
li
cgim
tc
cng
lmmt
tng
vch
hay
ph
gim
ca
cng
kim
loi
mt
cath
cch
mt
vch
tuynph
hp
trong
th
mt
catrong
kim
vngloi
nng
mt
hp
th
nguyn
t
qua
kim
loi
nhy
ph
hp
nguyn
ttnh
hn.
V d
ngn
la
+lm
Vi
As:dng
cch
nht u
nhn,
ca khi
X.kh
Ngha
nng
ca
yn
chng
bin
tathin
c
trongAAS
mt
vch
khong
ph
nht
ph)
nh.
cnm
Do
gi tuyn
tr
nm.
ngy
axetylen-khng
Ionl
Ti(IV)
lm
tng
tn cng
hiu
ca
vch(pic
Fe-248,3
tnhnay
khi
3
ASO
4
"
+
Na
2
BH
4
+
HCl
^
AsH
3
ngi
dng
tnh
cht
nh
cht
c

bng
php(2
o|ug/mL)
AAS.
V
nng ta
TI(IV)
thay
i
t
2Anion
-ny
50
p,g/mL.
Cc
Ion
La(III),
lm
tng
tn
hiu
AAS
ca
V
dli
mun
xc
nh
F xc
ngi
tacc
dng
Mghu
cCe(IV)
nng
2 ppm
vd
o
3
glucoz
vpht
hp
hu
c
tcLa
dng
lm
tngphng
cng
vch
phchun
hp th
ASO
4cc
" +nm
Na
2cht
BH
4amino
+ HCl
^nm.
AsH
5c+nh
Vi
vch ph
Fe-248,3
cng
tuyn
tnh
khi
nng
v Ce
mu
i tphp
x
ca
Mg-285,20
lng
F - trong
theo
ng
dy
nguyn
t
ca
Ca,
Zr,...
tuyn
tnh
khi
nng
ca
cc
cht
bin
thin
trong
vng
nh
hn
5 n Se:
20
p,g/mL.
Tnhbng
chtsau.
ny hin ang c nghin cu ng dng xc nh Ti La, Ce v
chun
c
pha theo
-6
1.10
M.
mt sDy
nguyn
khc
hp thFtrong ngn la n kh axetylen-khng kh nn.
chunt
xckm
nhnhy
nngph
Anion
SeO43- + Na2 BH4 + HCl ^ SeH4
Dy
chun
xcto
nh
nng
d
protein
Theo
phn
ng
ra hp
cht
bay hi
3SeO4
+ Na
2 BH
4 hydrua
+ chun
HCl ^ SeH6
Theo phn
ng
hp
cht
Cc
chtsinh
Dy
Cc cht
Dy chun
Cch
xc nh
tCAs,
Ge,
Hg.
+ Viny
Te: ch yu c dngCo
C1 cc nguyn
C2
3 Bi, C
4 Pb, Sb,
C5 Sn, Te,Cx
Co
C
1
C
2
C
3
C
4
C
5
Cx
V n cho kt qu vi
nhy cao hn php o trc tip bnh thng hng chc n hng
TeO43 + Na2BH4 + HCl
Ng Ca(ppm)
2 ^ TeH
24
2
2
2
2
2
trm ln
(bng
sau).(ppm)
y ngi ta cho
Nng
Mg
2 Zn kim
2 loi tc
2 dng vi
2 cht 2phn tch
2 trong2mi
3
(mM)
0,02
0,08 v d0,10
Cx ,
TeO4
Na2kh
BH4NaBH
+0HCl4 ^
TeH8
trng Protein
axit HCl,
hay +cht
sinh ra 0,04
cc hp 0,06
cht hydrua,
AsH 3, SbH
3
Nng F (ppm)
0
2
4
6
8
10
Cx
PbH2 trong
Cc
mt
hydrua
h thng
sinh phn
ra trong
ng1cc
ng
phn
kn,
sau
trn
1c
nh kh
mt1argon
dng dn
kh
mang
htr
(v nguyn
d 1nh
HClkh
(%)
1ng
1 vo
1thng
HCI
(%)
1
1
1
1
1
1
1mi
khha
t
argon)
mumca
hp
my
chtvhydrit
o ph
nyca
c
ccdn
nguyn
vo mi
t theo
trng
hp
iu
thkin
nguyn
thch hp
t ha
chov
o
Cc
chtcc
khc
nh
nhau
ph hpt.
nguyn
th ca nguyn t trong hp cht hydrua
.ACc cht Akhc nhA nhau A
A
o Ax. (Ca-422,70 nm)
Ao
1
2
3
4
5
Ax
A phng php ha hi v nguyn t
Theo
ny, hinnh
nay ngi
o k
ANthut
(Mg-285,20
Aota c ring
A1 mt h
2
A3
A4
A5
Ax
ha lnh
qua
vic
to
hp
cht
kh
hydrua
d
b
phn
hu
phc
v
vic
tch
V d trong mu dung dch th vch ph hp th ca Ca-422,70nm, khi c mt ca
-5php ny c
v xcSau
nh
nguyn
ni
nhy
rtphn
cao,
ckhi
1Cng,
- 5 (hnh
ng.
glucoz,
trong
vng
nngt
ttrn.
n.10
- n.10
mol/l
tng
theo
tuyn
tnh,
thc
hin
cc
dng
ng
chun
v-4Phng
pht
hin
nngsc
ln F
trong
mu
tch
Nguyn t
nhy ca F-AAS (p.g/L)
php
trong
ngn
n
kho
l AES
khngvkh
nnu
v c
axetylen
11.9aov
11.9b).
Cc
hng
snla
sut
my
AAS
bn b(hnh
trang b cho k thut ny vi cc
10a
v
11.
10b).
Tnh
cht
ny
c
s
dng
xc
nh
mt Hydro
s glucoz hay amino axit
tip
Qua
kiu khc
t cng
n gin
n hon
chnh
v
ng.
Theonhau,
s tng
vch
phTrc
(tng
tc t
Cation-phn
t)
trong cc
i ng
tng
muhp
sinhcht
hc.
Sauvy
l dy chun xc nh glucoz qua ph AAS
. Phn
sinh
alkyl
Cng
honAs
tonratng
t nh
nguyn
tc ca cch trn,0,2
nhng c khc l khi c mt ca
140 cacbonyl
ca Ca.
cht phn
XSb
th cng
da
vch
ph
cang
nguyn
t kim
loi
theo
s
Theotch
cch
ny
ngi ta
vo
phn
ca Ion
kim0,1
loi li
vic
nhmtng
Co tuyn
hay gc
alkyl
30
tng
nng
tch Xhay
c trong
mu vi
mt
sinh
ra
mtca
hpcht
chtphn
cacbonyl
mt nhm
alkyl
cavng
kimnht
loi nh.
trong mt iu kin xc
Bi
29
0,2
nh v c tnh cht nh lng, m cc kim loi li khng c kh nng sinh ra cc hp
30
0,2
cht hydrua kim Se
loi.
V d Ni trong
c c th c xc nh
Sn cc hp cht hu
110
0,5qua vic iu ch hp cht Nicacbonyl, ri sau nh mt kh mang tr dn hp cht ny vo mi trng hp th ca php o
F-AASy
xc
nhng
Ni vi
nhy
c 1 ng.
l phn
ca
mt
s Anion
ca mt s nguyn t vi nguyn t hydro mi sinh
to raCng
hp cht
tngkht,hydrua
Pb cng
dng
c
MeHn
xc nh
(vi qua
n = phn
3, 4, ng
5 vca
6). Pb(II)
V d vi
nh:LiCH
HgH3 2
, ASH
sinh 3
ra,
ASH5 ,3)SbH
Pb(CH
sau
, SbH
5
dn
, SeH
hp4 ,cht
SeHs,
ch TeH
alkyl4 ,ny
TeHvo
mi trng
Phn ng
hp ny
th rt
o
nh
phlng,
ca Pb
trong
vi
4 v 3
6, v.v...
nhng
nhyiu
caokin
hn ph
nhiu
hp
lncho
so mi
vi php
cht. o
V bnh
th nthng
cng c
nguyn
s t
dng
haPbxc
trong
nhngn
cc la
nguyn
n
t Hg, As, Se, Te.. trong cc i tng khc nhau, nh trong qung, trong nc, trong thc
kh.
t c0 c, c2 c3 c4 c5
phm,...
o phng
ph phtphp
x v
hp tnh
th nguyn
Song
ht hng
l mumi
phnng
tchdng
cn
Nibng
tmphp
li cc
phn
gin tipt.hin
naytrc
l mt
c o
x ph
l hp
athcc
nguyn
ny
v
dng
mui
tan Anion
trong dung
mi
php
nguyn
t,tm
rng
phn
tchca
ccIon
kim,
v ccdch
hpnc
cht hu
Hnhaxit,
11.10a
11.10b
trng
vtch
d cc
nh kim
cc loi
mui:
SbCl
SnCl
ASOn
Na2SeO
Na2TeO
4, Na
4, qu
4, Sau
c, hay
phn
mHgCl2,
ph hp
th5,Hnh
nguyn
t 3ca
km4, nhy.
y
l mt
Cc
pic
ph
ng
chun
phn
tch
thc
hin
theo
ccc
phnpht
ng trin
sau. v s dng trong vi nm li y, nhng c nhiu trin vng.
hng
mi,
ang
Tng
Cation-Cation
+ Vitc
Hg:
Cchlny
c
xc
mt nguyn
kim nhiu
loi khng
nhy
y
hiuthng
ng ca
s dng
tng
ca^nh
Cation-phn
t. t
Trong
trng
hp,ph
mt s cht
HgCl2
+ Na2BH4
+tc
HCl
HgH
phn tch dng phn t, m bn thn n khng c ph hp th nguyn t,
252
254
253
255
c bit l trong vic phn tch cc cht hu c, cc sn phm dc v ha du cc nc

cng nghip pht trin, nh M, Php, CHLB c, Anh, Nht, H Lan,v.v... Theo hng ny mt
cun sch mang tn "Organic compound Analysis hy Atomic Absorpt Ion Spectrometry" c cng
b bi tc gi H. Hassan, 1988.
256
- Vch
ph
o
AAS:
Chiu
cao
Burner:
5Nol:
- ph
6 mm.
nhy
No
LOD
vch
Vch
0,1
(nm)
p,g/mL (ppm).
Ghi ch
Khe
o:
0,5
- 0,7
nm.
4.20.
Nguyn
Mc
nhyL/ph
ph(V/V).
km
Loi
Burner:
cm.
11.
Nguyn
t.
Nguyn
t.- la:
Khe
o:t.
0,5
0,710
nm.
No
Vch
ph
(nm)
Ghi ch
Kh
ngn
(N
C2H
l
5,5/4,2
2O +
2) vi t
Mc nhy ph km vch s
No
Vch
ph
(nm)
Ghi
ch
Kh
ngn
la:
(Khng
kh
+
C
H
)
vi
vi
t
l
5,2/1,3
5,211,3
L/ph
L/ph
(VN).
(V/V).
2
2
2
2
Khe
o:
0,7n
- 0,5
nm.-608,0
vchph
s 1km vch
Vng
tuyn
tnh:
0,5
p,g/mL.
Cng
HCL:
- 80%
I max Mc nhy
Chiu
cao
Burner:
585,4680.
- 6 mm.
Cng
n
HCL:
50-80%
I
max
1
137,3400.
Th
Ion
ho
I:
8,29
eV.
Nguyn
Nguyn
t
t
lng:
lng:
63,5460.
Th
Ion
ho
I:
7,72
4,18
eV
eV
nhy LOD vch Nol: 0,5 p,g/mL (ppm).
Ni-232,00
11LOD
Co-240,70
nhy
vch
Nol:
0,05
pg/mL
p,g/mL(ppm).
(ppm). 1s1 1
Cng
n (Khng
HCL:
60kh
- 0,025
80%
Nguyn
Kh
t.ngn
la:
+ C 2IHmax
2) vi t l 5,2/1,2 L/ph (V/V).
Loi
Burner:
10
cm.
Loi
Burner:
5
cm.
Ch
ph:
F-AES
(Phtth
xnguyn
ngn la).
Ch
ph:
F-AAS
t).
Vng
tnh:
1Ni-341,50
-Nol:
15(Hp
pglml.
2tuyn
Co-242,50
1,5ln
lnkm
km
2oo
2,5
Chng
12nhy
vch
0,05
p,g/mL (ppm).
1LOD
Ag-328,10
1
Loi
Burner:
10
cm.
Vng
tuyn
tnh:
0,1
5,0
8,0
p,g/mL.
pg/mL.
Nguyn
t
lng:
28,0860.
Th
Ion
ho
I:
8,15
eV
Chiu
cao
Burner:
5PH
-Ni-305,10
3cao
Co-241,20
2,5T
lnkm
km
Chiu
Burner:
56 -mm.
6 mm.TH NGUYN
CC
IU
KIN
O
HP
V
PHT
AAS:
Vch
ph
o
AAS:
Vch
3ph
o
F-AES:
4,5
ln
Vng
tnh: 0,1
- 68,0
p,g/mL.
Nguyn
t. 4tuyn
Chiu
cao
2 Burner:
5
Ag-328,30
mm.
2,5
ln
km
Co-252,10
8,5
ln
km
Ch
o
F-AAS
(Hp
th nguyn
t).
X
NGN
LA
CA
MT
S
NGUYN
No
Noph:
Vch
Vch
ph
(nm)
Ghi
Ghich
ch
Nguyn
t.
Kh
ngn
(Kh
N
+
C2(nm)
H+
lT
5,5/4,5
L/ph(V/V).
4la:
Ni-234,60
8 ln
km
2O ph
2) vi t
Mc
nhy
ph
km
nhy
ph
kmL/ph(VN).
vch
No
Vch
ph
(nm)
Ghi ch
Kh
ngn
la:
(Khng
kh
C 2H2)Mc
vi
t
l
5,2/1,25
Mc
nhy
ph
km
Nguyn
t
lng:
208,9806.
Th
Ion
ho
I:
7,29
eV
Kh
nhy
LODla:
vch
Nol: 0,5
p,g/mL
Nguyn
t.nhy
ngn
(Khng
kh0,025
+ C 2Hp,g/mL
vi t
l 5,2/1,3 U/ph (V/V).
2)(ppm).
LOD
vch
Nol:
(ppm).
Vch
pht
o
vch
s 1
s s
1eV
Khe
o:
0,7
--AAS:
0,5
nm.
Nguyn
lng:
65,3700.
39,1000.
Th g/mL
Ion ho
I:vch
9,39
4,34
Khe
o:
0,7
0,5
nm.
1
nhy
LOD
vch
Nol:
0,05
(ppm).
Khe
o:
0,5
0,7
nm.
Vng
tuyn
tnh:
2 -F-AAS
10
p,g/mL.
Ch
1o
ph:
(Hp
thIon
nguyn
Nguyn
t
lng:
24,3050.
Th
ho I:t).
7,64 1eV
Rb-780,00
1
Cu-324,76
Cng
HCL:
60
--LA
80%
IImax
Ch
Ch
o
on
ph:
ph:
F-AES
F-AAS
(Pht
(Hp
x
th
ngn
nguyn
la).t). 11
Vng
tuyn
tnh:
0,1
5,0
p,g/mL.
Phn I.Cng
PHP
O
PH
NGN
Cng
No
n
HCL:
Vch
ph
(nm)
80%
Ghi ch
max .
1
Ba-553,60
Vng
tuyn
tnh:
0,1
--60
5,0
g/mL.
n
HCL:
60
80%
Imax
Mc
nhy
ph
km
2o o
Rb-794,80
2,5 ln
km
Vchph
AAS:
Ch
ph:
F-AAS
(Hp
th
nguyn
t).
2 o F-AES:
Cu-327,40
2 ln km
Loi
Burner:
10
cm.
Vch
ph
2
Ba-455,40
6vch
ln km
s 1
Loi
Burner:
Khe
di
10 cm.
Loi
Burner:
10
cm.
3
Rb-420,20
100 ln km
Nguyn
t.
Vch ph
3 o AAS:Cu-217,90
4,5 ln km
1 o
Si-251,60
Chiu
Burner:
55 -- 66 mm.
3cao
Ba-350,10
20
ln1ln
km
Vch
AAS:
Chiu
cao
Burner:
mm.
Nguyn
t. ph
No
Vch
ph
(nm)
Ghi ch
4t Burner:
Rb-421,60
260
km
Chiu
cao
5
6
mm.
Nguyn
lng:
112,4000.
Th
Ion
ho
I;
6,12
eV
Mc
nhy
ph
km
22
ln
km
No42 t lng:
VchCu-222,60
ph
(nm)
Ghi ch
Nguyn
22,9898.
Th
Ion
ho
I:
5,14
eV
Si
250,70
3
ln
km
Mc
nhy
ph
km
vch
No la: (Khng
Vch ph
(nm)
Kh
ngn
kh
C 2H
t
l
5,2/1,25
L/ph (V/V). Ghi ch
2) vi
Mc
nhy
ph1 L/ph
km
Khngn
ngn
la:
(Khng
kh+++
H
vi
t
l
5,2/1,2
vch
s
2))vi
Kh
la:
(Khng
kh
CC
t
l5,98
5,2/1,30
L/ph(V/V).
(V/V).
22H
2nguyn
Nguyn
t
lng:
26,8915.
Th
Ion
ho
I:
eV.
Ch
o
ph:
F-AAS
(Hp
th
t).
Khe
o:
0,7
0,5
nm.
nhy
LOD
vch
Nol:
0,1
p,g/mL
(ppm).
Khe
o:
0,2
0,5
nm.
s
1
Si-251,40
4vch
ln km
Chnhy
31o
ph:
F-AES
(Pht
x
ngn
la).
s
1
Khe
o:
0,5
- 0,7
nm.
LOD
vch
Nol:
0,05
p,g/mL
(ppm).
Zn-213,90
K-766,50
1

nhy
vch
Nol:
0,05
1ph
Bi-223,10
1 (ppm).
Ch
ph:
F-AAS
(Hp
th
nguyn
t).
Vng
tuyn
tnh:
0,5
- 8,0
p,g/mL.
Cng
LOD
n
HCL:
60
- 80%
Ip,g/mL
Vch
o
AAS:
max
41o
Si-252,90
12 ln1 km
Loi
Burner:
10
cm.
Mg-285,20
Vngph
tuyn
tnh:
0,1
6,0
p,g/mL.
Vng
tuyn
0,1
--8,0
p,g/mL.
Cng
HCL:
60
- 80%
Imax
2 n
Zn-307,60
K-769,90
2000
3 ln
lnkm
km
Vch
otnh:
F-AES:
2
Bi-222,80
4 ln
kmkm
Vch
ph
o
AAS:
Loi
Burner:
5
cm.
2
Mg-202,60
40
ln
Chiu
5 - 6 mm.
3cao Burner:
200 ln km
10. Nguyn
t.
Loi
Burner:
10 cm.K-404,40
Nguyn
t.
Nguyn
t.o:
Khe
o:
0,5 nm.
-Bi-306,80
0,7 nm.
3 3 0,5
4,5
ln ln
kmkm
Khe
Mg-279,60
100
Chiu
cao
5K-407,70
- 6 kh
mm.+ C 2H2) vi t
4 Burner:
210
ln
kmL/ph (V/V).
Kh
ngn
la:
(Khng
l
5,2/1,2
Chiu
cao
5 - 6 mm.Th Ion ho
Vch
ph (nm)
Ghi ch
Nguyn
tBurner:
lng:
51,9960.
I:ln
6,76
eV
4
Bi-227,70
20
km
Mc
nhy
ph
km
vch
Cng
n
HCL:
50
80%
I
max
ngn
nhy
LOD
vch
Nol:
0,05
p,g/mL
(ppm).
No
Vch
ph
(nm)
Ghi ch
60
Nguyn
t
lng:
207,2000.
Th
Ion
ho
I:I:7,42
eV
Nguyn
t
lng:
196,9665.
Th
Ion
ho
9,22
eV.
max
Kh
la.
(N
O
+
C
H
)
vi
t
l
5,514,5
L/ph
(V/V).
2
2
2
Mc nhy ph km
Vch
(nm)
Ghi ch
Khengn
o:No
0,5
- 0,7
nm. ph
Mc
nhy
ph
km
Kh
la:
(Khng
kh
+
C
H
)
vi
t
l
5,2/1,2
L/ph
(V/V).
s
1
2
2
Khe
Ch
o:
o
0,2
ph:
- tnh:
0,5
F-AAS
nm.
(Hp
th nguyn
t).
nhy
LOD
vch
Nol:
0,5p,g/mL.
p,g/mL
(ppm).
Vng
0,1
- (Hp
5,0
Loi
Burner:
cm.
510vch
cm.
Ch
o
ph:
F-AAS
th
nguyn
t).
Ch
tuyn
o
ph:
F-AAS
(Hp
th
nguyn
t).
vch
max
nhy
LOD
Nol:
0,025
p,g/mL
(ppm).
vch s
s 11
Cng n HCL: 60-80% I
Khe Burner:
o:
-AAS:
0,5cm.
Loi
10
Vch
ph0,7
otnh:
Vng
tuyn
2nm.
- 18 p,g/mL.
Cd-228,80
1
Chiu
cao
Burner:
5 -- 64,0
mm.
Vch
AAS:
Vchph
ph
AAS:
Vng
tuyn
tnh:
0,1
p,g/mL.
11 o
Na-589,00
11
Nguyn
Loit.Burner:
10 cm.Al-309,30
Cngcao
Burner:
n HCL:
- 80% Imax
Chiu
5 -60
6 mm.
Kh
la: (N
(Khng
vi
t 2,5
lkm
5,2/1,2
L/ph (V/V).
2 Cd-326,90
Na-589,60
ln
km
Nguyn
t.ngn
2Ht
2)500
+ Ckh
)C
vi
l 5,5/4,5
L/ph
(V/V).
ln
2O
2H2+
2 tBurner:
Al-396,20
1,5
ln eV
km
No
Vch
ph
(nm)
Ghi
ch
Nguyn
lng:
121,7500.
Th
Ion
ho
I:
8,68
Chiu
cao
5
6
mm.
Nguyn
t.
No
Vch
ph
(nm)
Ghich
ch
Mc
nhy
ph
km
vch
nhy
vch
Nol:
0,02
p,g/mL
Loi
Burner:
cm.
Kh
ngn
No
la: 10
(Khng
Vch
ph
kh
(nm)
+ C 2H(ppm).
vi
t
l
5,2/1,25
L/ph
(V/V).
Ghi
2)Mc
nhy
ph
km
vch
3
Na-330,30
300
ln
km
Mc nhy ph km
nhy
LOD
vch
Nol:
0,5
p,g/mL
(ppm).
Nguyn
t
lng:
9,0122.
Th
Ion nguyn
ho
I: 9,32
eV
nhy
LOD
vch
Nol:
p,g/mL
ss1eV
Ch
3t
o
ph:
F-AAS
th
t).
Kh
ngn
la:
(K.kh
Al-308,20
C(Hp
H
l(ppm).
5,2/1,25
1,8
ln
km
(V/V).
20,05
2) vi
1L/ph
Nguyn
55,847.
Th
Iont
ho
I: 7,87
Vng
tnh:
-+2,5
p,g/mL.
Chiutuyn
cao lng:
Burner:
6p,g/mL.
mm.
vch
s
1
20,1
-520
nhy
LOD
vch
Nol:
0,02
p,g/mL
(ppm).
Khe
o:o
0,2ph:
- 0,5
0.5
nm. (Hp th nguyn t).
Ch
Khe
o:
-tnh:
F-AAS
nm.
Vng
0,1
- 8,0 p,g/mL.
1tuyn
Cr-357,90
1 1ln km
Vch
o
AAS:
40,7la:
Al-394,40
1ph
Pb-217,00
Ch
o
ph:
F-AAS
(Hp
1
Au-242,80
1
Kh
ngn
(Khng
kh
+ th
C 2Hnguyn
l3,5
5,2/1,3
L/ph (V/V).
2) vi tt).
Nguyn
t.
Vng
tuyn
tnh:
0,1 50
- 3,0
p,g/mL.
Loi
Burner:
10
cm.
Vch
Cng
ph
o
n
AAS:
HCL:
80%
I
max
t.nhy
Nol: 0,1 p,g/mL
(ppm).
2 LOD vch
Pb-283,30
lnkm
km
2ph
cr-359,40
2 2ln
Nguyn
Vch
o
AAS:
2 No
Au-267,60
2,5
lneV
km
Nguyn
t
lng:
91,2200.
Th
Ion
ho
I:
7,80
87,6200.
5,69
Vch
ph
(nm)
Ghi ch
Khe
0,7 - 0,5
nm.
Nguyn
t:o:
Mc
nhy
ph km
3
Pb-261,40
40
ln
km
Loi
Burner:
10
cm.
Vng
tuyn
tnh:
0,5
8
p,g/mL.
Chiu
cao
Burner:
5
6
mm.
3 t lng:
Cr-360,30
ln eV
km
Nguyn
6,9410. Th Ion ho 3,6
I: 5,39
Ch No
3
o ph:
F-AAS
th
nguyn
t).vch
Au-312,30
900
ln km
Vch
ph
(nm)
Ghi ch
s vch
1
Cng
HCL:
60
-(Hp
80%
I max
. ho
4 tn
Pb-368,40
100
lnkm
km
Mc
nhy
ph
Nguyn
lng:
54,9380.
Th
Ion
I:
7,43
eV
No
Vch
ph
(nm)
Chiu
cao
Burner:
5
6
mm.
4
Cr-429,00
10
ln
km
Mc
nhy
ph L/ph
km (V/V). Ghi ch
Nguyn
Kh
ngn
la:
kh
+ Cx
t l
5,2/1,2
Cht.
o
ph:(Khng
F-AES
(Pht
la).
2Hngn
2) vi
1
Sb-206,80
1
s 1
VchBurner:
ph o Khe
AAS:di- 5 cm.
Loi
Ch
ola:
ph:(Khng
F-AASkh
(Hp
vch
s 1 L/ph (V/V).
Kh ngn
+ Cth
) vi t t).
l
5,2/1,2
2H2nguyn
Nguyn
40,0800.
Th
Ion ho
I: 26,11
Vch
ph
olng:
F-AES:
2t
Sb-217,60
lneV
km
nhy
LOD
vch
Nol:
0,02
p,g/mL
(ppm).
1
Be-234,90
1
Khe o:
o:
0,5
- 0,7
0,7 nm.
nm.
1 0,5
Fe-248,30
1
Chiu
cao
Burner:
7
6
mm.
Khe
nhy
LOD
vch
Nol:
0,025
g/mL
(ppm).
Vng
tuyn
tnh:
0,05
- 2,0
p,g/mL.
Khe
0,7ph:
- 0,5
nm.
3o
Sb-231,20
8 ln
km
Ch
F-AAS
(Hp
th
nguyn
t).
No
Vch
ph
(nm)
Ghich
ch
2o:
Be-313,04
10nhy
ln
km
No
Vch
ph
(nm)
Ghi
Mc
ph
km
Mc
nhy
ph
kmvch
2
Fe-248,80
2,5
ln
km
Vng
tuyn
tnh:
0,1
2,5
g/mL.
Cng
n
HCL:
60
80%
I
Vch
ph
o
AAS:
max
Kh
ngn
la:
(N
C2-H80%
t l 5,5/4,5
L/ph
(V/V).
2O +60
2) viI max
Cng
n
HCL:
No
Vch 50
ph- 80%
(nm) Imax Mc
Ghi ch
3 ph
Be-332,14
80 ln
km
Cng
nAAS:
HCL:
nhy
ph
ss
1 1 km
Vch
o
vch
nhy
LOD
vch
No1:
0,2
p,g/mL (ppm).
No
Vch
ph
(nm)
Ghi
ch
3
Fe-271,90
3,5
ln
km
Nguyn
Khe
t.
o:
0,5
0,7
nm.
Mc nhy ph km
Loi
Burner: 10
10 cm.
cm.
Nguyn
t. Burner:
Loi
vch
s
1
1
sr-460,70
1
Loi tuyn
Burner:
10 1cm.
Zr-360,10
Vng
- 1260
p,g/m.
41 tnh:
Fe-372,00
12 ln1s
km
Cng
n HCL:
- 80%
IIon
max ho I:vch
Nguyn
t
lng:
58,7900.
Th
7,611eV
eV1
Chiu
cao
Burner:
5
6
mm.
Khe
o:
0,7
0,5
nm.
1
Li-670,80
Nguyn
t
lng:
58,9332.
Th
Ion
ho
I:
7,86
Chiu cao
Burner:
5
6
mm.
2
Sr-407,80
25
ln
No Burner:
Vch
Ghi ch
12cao
Mn1 km
Chiu
5 - 279,50
6 ph
mm.(nm)
Zr-303,10
2 ln
km
Mc
nhy
ph km
A Burner: 10 cm.
Loi
Nguyn
t.
g
Khe
o:
0,5
0,7
nm.
Kh
ngn
2
la:
(Khng
Li-323,30
kh
+
C
H
)
vi
t
330
l
5,2/1,3
ln
km
L/ph
(V/V).
2
2
Cng
n
HCL:
60kh
- 80%
I max
Ch ngn
2
ola:
ph:(Khng
F-AAS
(Hp
t).
Kh
+ Cth
) vi t 1,5
l 5,2/1,25
L/ph
(V/V).
2H
2nguyn
vch
sL/ph
1 (V/V).
Mn279,80
ln
km
Khnhy
ngn
3 0,5
la:
(Khng
Zr-352,00
kh0,1
+C
t l
2 ln
5,2/1,2
km
2H2) vi
LOD
vch
Nol:
p,g/mL
(ppm).
Khe
o:
nm.
nhy
LOD
vchLi-610,40
Nol:
p,g/mL
(ppm).
Chiu
cao
Burner:
560
- 6- 0,1
mm.
3
1400
lneV.
km
Cng
n
HCL:
80%
Ip,g/mL
max
Nguyn
lng:
107,8680.
Th
Ion ho
I:3 7,57
Loi
Burner:
5AAS:
cm.
nhy
1 LOD
vch
Nol:
Ca-422,70
0,05
(ppm).
1
Vch
ph
o
AAS:
3t
Mn280,10
ln km
Vch
ph
o
Vng
tuyn
tnh:
0,5
8,0
p,g/mL.
4
Zr-298,50
4
ln
km
Cng
n
HCL:
- 80%
Vng
tuyn
tnh:
0,5 60
- 8,0
p,g/mL.
Kh
ngn
la:
(Khng
+th
CImax
l 5,2/1,25 L/ph (V/V).
2H
2) vi t
Loi
Burner:
10
cm.
Ch
ph:
F-AAS
(Hp
nguyn
t).
Vng
tuyn
0,1
-6403,00
5kh
p,g/mL.
4o
Mn10150
ln ln
kmkm
Chiu
cao
Burner:
5 -Ca-239,90
mm.
Khe
o:
-tnh:
0,5
nm.
20,2
Loi Burner: 10 cm.
Ba
Cu
Rb
Si
Bi
Zn
K
Mg
Cd
Na
Al
Pb
AuCr
Sb
Be
Fe
Zr
Si
Li
Mn
Ca
Ni
Co
268
258
270
264
266
262
260
259
269
265
271263
267
257
261
Vng tuyn
- 50 ph
ng/mL.
Vch
ph
(nm)
(nm)
N
No tnh: 2Vch
oC
Mc
Mc
ph
phgian:
km 2vch
vch
Kh
+
B
iu
Khe
Giai
chnh
tr
o:
kin
on
mi
0,5
nn:
nguyn
trng:
lm
-o:
C
sch
nm.
BC
t
Argon.
ho:
Cuvt:
Nhit
2700nhy
, Thi
giy.
11.
8.
Nguyn
t.
t.
5. Nguyn
Khe
o:
0,7
-0,7
0,5
nm.
Khe
0,5
nm.
Loi
Cuvt
Graphit:
Hot
ho
ton:
phn.
Phn
II. PHP
22.
Nguyn
t. O KHNG NGN LA
s 1
oC
B
iu
+
Cng
Giai
chnh
nhy
kin
on
LOD
nn:
nguyn
n
sy:
C
vch
HCL:
Nhit
BC
tNol:
ho:
60
:
- 0,25
120
I-Ion
250
(ppb).
,II:max
Thi
gian:
max
Nguyn
Cng
t.
n
HCL:
60
-80%
80%
Nguyn
t
lng:
63,5460.
Th
ho
I:9,32
eV
Kh
tr
mi
trng:
Argon.
9,0122.
Th
Ion
ho
eV
Cng
n
HCL:
60ng/mL
-I max
80%
Nguyn
t
lng:
112,4000.
Th
Ion
ho
I:7,72
6,12
eV30 giy.
Cd
Cu
Be
V
Sb
1
Ghi
Ghi ch
ch
Ag-328,10
Si 251,60
Mo1
Nguyn t lng: 50,9441. Th Ion ho
I: 6,75 eV
oC oC
iu
Vng
+
Loi
Giai
Cuvt
kin
tuyn
on
nguyn
Graphit:
tnh:
sy:
tro
ho:
Nhit
2
t
Hot
Nhit
20
ho:
:
ng/mL.
ho
:
120
ton
550
200
phn.
700
,
Thi
,
Thi
gian:
gian:
30 giy.
30 giy.
Loi
Cuvt
Graphit:
Hot
ho
ton
phn.
Ch
o
ph:
F-AAS
(Hp
th
nguyn
t).
B
chnh
nn:
C
BC
Cuvt
Graphit:
hoho
ton
Ch
o
F-AAS
th
t).
2Loi
Ag-328,30
Si (Hp
250,70
Mo- Hot
2,5
2,6
Ln
ln
km
Nguyn
tph:
lng:
121,7500.
Thnguyn
Ion
I:phn.
8,68
eVkm
Ch o ph: F-AAS (Hp th nguyn
t).
oC oC
oC
Kh
tr
mi
trng:
Argon.
Vch
ph
o
AAS:
iu
kin
nguyn
t
ho:
+Kh
Giai
tr
on
mi
sy:
tro
trng:
NTH:
ho:
Nhit
Nhit
Argon.
Nhit
:
:
:
120
2550
450
- 200
-, 600
Thi
, Thi
,gian:
Thi
gian:
3gian:
giy.
30
giy.
20 giy.
Vch
ph
o
AAS:
mi
trng:
Argon.
3Kh
Si-251,40
Mo4Ln
ln
km
km
Vch
ph
otr
AAS:
Nguyn
t.
Ch
o
ph:
F-AAS
(Hp
th
nguyn
t).
Khet.
o:
0,7
-AAS:
0,5 nm.
Vch
ph
(nm)
Ghi
Vch
ph
oC oC
N
ooo
Nguyn
Vch
ph
(nm)
Ghi ch
ch
oC gian:
N
B
chnh
nn:
C
BC
+Giai
Giai
on
sy:
Nhit
:
120
- oC
200
, Thi
30
giy.
Mc
nhy
ph
km
vch
Vch
ph
(nm)
Ghi
ch
N
onn:
+
B
chnh
on
NTH:
tro
lm
C
ho:
sch
BC
Nhit
Nhit
Cuvt:
:
:
2300
Nhit
600
-:
, 800
Thi
2700
,gian:
Thi
,Ln
Thi
3ln
gian:
giy.
gian:
30
giy.
2 giy.
Mc
nhy
ph
km
vch
4B
Si
252,90
Mo10
km
km
chnh
nn:
C
BC
Mc
nhy
ph
km
vch
NguynNt
lng:
54,9380.
Th
Ion
ho
I:
7,43
eV
Vch
ph
(nm)
Ghi ch
o o
Cng
HCL:
50
- 80%
I max
s
11 km
Vch
ph
AAS:
Mc
ph
Nguyn
tn
lng:
26,8915.
Th
Ion
I:oC5,98
eV
s
iu
kin
nguyn
t
ho:
+Giai
Giai
on
tro
ho:
Nhit
:
500
700
,nhy
Thi
gian:
20 vch
giy.
oC -ho
oC
s
1
+
iu
nhy
kin
on
LOD
nguyn
NTH:
lm
vch
sch
t
Nhit
Nol:
ho:
Cuvt:
:
0,25
2600
Nhit
ng/mL
:
,
Thi
(ppb).
2500
gian:
,
Thi
3
giy.
gian:
2
giy.
kin nguyn(Hp
t ho:
Cho:
1iu
o
th nguyn t). s1 1
Khe
o:
0,5ph:
- 0,7F-AAS
nm.
Khe
0,5
nm.
Cu-324,76
Be-234,90
oC
Loi
Cuvt
Graphit:
Hot
ho
ton
phn.
Cd-228,80
NTH:
Nhit
:120
2550
,oCoC
Thi
gian:
311giy.
+ Giai
sy:
Nhit
:
- nguyn
200
, Thi
30 giy.
Ch
11Non
o
ph:
F-AAS
(Hp
th
t).
oC gian:
Vch
ph
(nm)
Ghi ch
o
oC
+
Vng
Giai
nhy
tuyn
on
LOD
lm
tnh:
sy:
vch
sch
Nhit
2,5sy:
Nol:
-Cuvt:
25
:
0,25
ng/mL.
120
Nhit
ng/mL
- 200
:
(ppb).
,2700
Thi
gian:
,, Thi
30gian:
giy.230
giy.
Mc
nhy
ph
km
vch
+
Giai
on
Nhit
:
120
200
Thi
gian:
giy.
1
V-318,50
1
2
Cu-327,40
2
ln
km
Vch
o
AAS:
Cngph
n
HCL:
60
80%
I
Cng
n
HCL:
60
80%
I
Be-313,04 max
8 ln
km
max
oC
oC 500
22on
Cd-326,90
ln
km20 giy.
B
chnh
nn:
Cho:
BC
lm
sch
Cuvt:
, Thi
2 giy.
+ Giai
tro
Nhit
:Nhit
400 -:
6002700
, Thi
gian:
ph
otnh:
AAS:
oC
s
1 gian:
oC
Vng
+Vch
Giai
nhy
tuyn
on
LOD
tro
vch
ho:
2,5
Nol:
Nhit
25
0,25
ng/mL.
:
ng/mL
550
800
(ppb).
,
Thi
gian:
20gian:
giy.20 giy. Ghi ch
2
V-306,60
3
ln
km
33N
+ oGiai on
Cu-217,90
tro ho:
Nhit : 450 - 100
700
4,5 ln
, Thi
km
Vch
ph
(nm)
Nguyn
t.
Be-332,14
ln
km
Loi
Cuvt
Graphit:
Hot
ho
ton oC
phn.
Loi
Cuvt
Graphit:
Hot
ho
ton
phn.
Mc gian:
nhy 3ph
km vch
1on
Sb-206,80
1giy.
Giai
nhy
vch
Nol:ph
0,5(nm)
ng/mL
+
NTH:
Nhit
:
2300
,(ppb).
Thi
Kh
tr
mi
trng:
Argon.
Vch
Ghi ch
NoLOD
oC
Khe
o:
-tnh:
0,5 nm.
V-437,90
5
ln
km
oC
Vng
+ Giai
tuyn
on
NTH:
2,5
Nhit
25
:
ng/mL.
2550
,
Thi
Mc
gian:
nhy
3
giy.
ph
km
vch
43+0,7
Cu
222,60
21
ln
km
Giai
on47,90.
NTH:Th
Nhit
:
2300
, Thi
gian:
3 giy.
s
1
Nguyn
t.
Nguyn
t
lng:
Ion
ho
I:
6,82
eV
oC
Kh
trtuyn
trng:
Argon.
Kh
tr
mi
Argon.
2mi
Sb-217,60
km
Vng
tnh:
2,5
-Cuvt:
25 ng/mL.
+
Giai
on
lm
sch
Nhit : 2500 2, ln
Thi
gian: 2 giy.
Khe
o:
-trng:
0,5
B
chnh
nn:
Cnm.
BC
1gian:
410,7
V-385,60
lns
Cng
n
HCL:
50Cuvt:
-279,50
80%Nhit
I max : 2700 oC7, Thi
Mn1km
oC
+ Giai
on
lm
sch
2 giy.
Khe
o:
0,5
0,7
nm.
+
Giai
on
lm
schTh
Cuvt:
Nhit
, Thi
gian: 2 giy.
Nguyn
t.
Nguyn
lng:
137,3400.
Ion(ppb).
ho t).
I::
8,29
eV1km
Ch
ph:
F-AAS
(Hp
nguyn
3o
Sb-231,20
32500
ln
B
chnh
nn:
C
BC
B
C
BC
1tnn:
Al-309,30
chnh
nhy
LOD
vch
Nol:
0,5th
ngi
Nguyn
t.
Cng
n
HCL:
60
80%
I
max
iu
kin
nguyn
t
ho:
2
Mn279,80
1,5
ln
km
Loi
Cuvt
Graphit:
Hot
hong/mL
ton
Kh tr mi trng: Argon.
nhy
LOD
vch
Nol:
0,5
(ppb).
Cng
n
HCL:
50vch
- 80%
I max phn.
Khe
o:
0,5
- AAS:
0,7
nm.
nhy
LOD
Nol:
ng/mL
(ppb).
Nguyn
t
lng:
207,2000.
Th
IonoC
ho t).
I: 7,42
Ch
o
ph:
F-AAS
(Hp
th 0,1
nguyn
Vch
ph
o
2
Al-396,20
1,5eV
ln km
iu
kin
nguyn
t
ho:
iu
kin
nguyn
t
ho:
Vng
tuyn
tnh:
4
40
ngi.
Khe
o:
0,5
0,7
nm.
Loi
Cuvt
Hot
ho
ton
phn.
lng:
51,9960.
Th
Ion
ho
I: 6,76
eV30
+Nguyn
Giai
on
sy:
Nhit
:
120
- 200
, Thi
gian:
giy.
3 tGraphit:
Mn280,10
3 ln
km
B
chnh
nn:
C
BC
Loi
Graphit:
Hot
ho- ton
phn.
VngCuvt
tuyn
tnh:
2Vch
-tnh:
25
ng/mL.
Cng
n
HCL:
60
80%
I
Vng
tuyn
0,5
10
maxng/mL.
3
Al-308,20
ph
(nm)
1,8
ln
km
Ghi ch
oC
oC
N
o
Ch
ph
ph:
(Hp
th--250
nguyn
t).nhy
+Ch
Giai
on
gy:F-AAS
Nhit
:
120
,Thi
Thi
gian:
30
giy.vch
+
Giai
on
sy:
Nhit
120
,Mc
gian:
30
giy.
oC t).
ph
km
Nguyn
t.
4ooAAS:
Mn10
tn
km
ph:
F-AAS
(Hp
nguyn
Kh
tr
mi
trng:
Argon.
Cng
n
60:
-403,00
80%
I max250
+Vch
Giai
on
troHCL:
ho:
Nhit
: th
500
- 800
, Thi
gian:
20 giy.
Kh
mi
trng:
iutr
kin
nguyn
tArgon.
ho:
Al-394,40
ln1 km
Loi
Graphit:
Hot
ho(nm)
ton phn. oCoC 3,5 s
Vch
ph
Ghi ch
N4ooo
Nguyn
t.Cuvt
Vch
ph
AAS:
+
Giai
on
tro
ho:
Nhit
:
600
900
, ,Thi
gian:
30
+
Giai
on
tro
ho:
Nhit
:
600
ThieV
gian:
30giy.
giy.
oC-- 1000
Vch
ph
AAS:
Mc
nhy
ph km
vch
B
chnh
nn:
C BC
Nguyn
t NTH:
lng:
40,0800.
Th
Ion
ho
I:
6,11
+
Giai
on
Nhit
:
2550
,
Thi
gian:
3
giy.
oC
Loi
Cuvt
Graphit:
Hot
ho
ton
phn
B
chnh
nn:
C
BC
Khe
o:
0,5
0,7
nm.
+ Giai on sy: Nhit : 120 - 200 , Thi gian: 30 giy.
Kh
tr N
mi
trng:24,3050.
Argon.
oC ho I: 7,64 eV
oC
Vch
ph
(nm)
Ghi ch
s
o0,7
lng:
Th
Ion
1t
Ti-3
64,30
1 1km vch
+Khe
Giai
on
NTH:
Nhit
;
2700
Thi
gian:
3ph
giy.
+Nguyn
Giai
on
NTH:
Nhit
:
,, Thi
gian:
giy.
o:
- 0,5sch
nm.
Ch
o
ph:
F-AAS
(Hp
th
nguyn
t).
oC 3
Mc
nhy
iu
kin
nguyn
t
ho:
Vch
ph2700
(nm)
Ghi ch
+
Giai
on
lm
Cuvt:
Nhit
2700
, Thi
gian:
2 vch
giy.
N
o
oC
iu
kin
nguyn
t
ho:
n
HCL:
50 - 80%
I max -:
nhy
ph
km
+Cng
Giai
on
tro
ho: Nhit
: 400
600Mc
, Thi
gian:
20
giy.
Kh
tr
mi
trng:
Argon.
B
chnh
nn:
CF-AAS
BCBa-553,60
oC
1
oC
1
s
1
Ch
o
ph:
(Hp
th
nguyn
t).
oC 2800
2 n
1,6
ln
km
+Cng
Giai on
on
lm
schTi-365,40
Cuvt:
Nhit
:
2800
Thi
giy.
Vch
ph
o
AAS:
lm
sch
Cuvt:
Nhit
:
,, Thi
HCL:
60
80%
I max
+
Giai
sy:
Nhit
:-0,25
120
250
Thi gian:
gian:
30gian:
giy.22 giy.
oC
s
1gian:
nhy
LOD
vch
Nol:
ng/mL
(ppb).
+
Giai
on
sy:
Nhit
:
120
-- 200
,, Thi
30
giy.
oC
Cuvt
Graphit:
Hot
ho
ton
phn.
+Loi
Giai
on
NTH:
Nhit
:
2200
,
Thi
gian:
3
giy.
1
Pb-217,00
1
B chnh
nn:
C t
BCBa-455,40
iu
kin
nguyn
ho:
231LOD
ln1km
km
oC
Vch
ph
o
AAS:
Cr-357,90
nhy
vch
Nol:
ng/mL
(ppb).
Ti-320,00
25ln
nhy
vch
Nol:
10,5
ng/mL
(ppb).
Loi
Cuvt
Graphit:
Hot
ho
ton
Vch
ph
(nm)
Ghi ch
oC , Thi
+
Giai
on
tro
ho:
Nhit
:
550
800
gian:
20
giy.
NLOD
o tro
+
Giai
on
ho:
Nhit
:
450
-- phn.
600
, Thi
gian:
20
giy.
Vng
tuyn
tnh:
1
20
ng/mL.
Mc
ph
km
oCnhy
2mi lm
Pb-283,30
2
ln
km
tron
trng:
+Kh
Giai
schArgon.
Cuvt:
Nhit :
2400
,
Thi
gian:
2 vch
giy.
oC
+iu
Giaikin
on
sy: Nhit
:
120
- 250
, Thi gian:
30km
giy.
ph
(nm)
Ghi ch
3mi
223 ln
N
Cr-359,40
n
t
ho:
oC
Vng
tuyn
tnh:
60
ng/mL.
tuyn
tnh:
55Vch
-- Ba-350,10
100
ng/mL.
Kh
trng:
Argon.
skm
1km vch
+Vng
Giaitr
on
NTH:
Nhit
:
2600oC
Thi
gian:
giy.
Mc
nhy
ph
42onguyn
Ti-399,00
521
+
Giai
on
NTH:
Nhit
:
2400
,, Thi
gian:
3ln
giy.
3
Pb-261,40
40
ln
km
Bt.
chnhLOD
nn: C BC
nhy
Nol:
0,05 ng/mL (ppb).
Nguyn
oC
31 trovch
Cr-360,30
3,6gian:
+ Giai
on
ho: Nhit
: 550 - 700
, Thi
20 giy.
Ca-422,70
11 km
sln
oC
oC
oC
+B
Giai
on
sy:
Nhit
:
120
180
,
Thi
gian:
30
giy.
chnh
nn:
C
BC
2700
giy
+
Giai
on
lm
sch
Cuvt:
Nhit
:
2500
, Thi
gian:
2 giy.
40,7 - 0,5 nm. Pb-368,40
100
ln
km
Nguyn
t.
Nguyn
Khe
t.
o:
iu
kin
nguyn
t -ho:
Vng
tuyn
tnh:
0,5
15 ng/mL.
Nguyn
t
lng:
196,9665.
Th
Ion
eV
oC ho I: 9,22
Khe
o:
0,5
0,7nm.
4
Cr-429,00
6
ln
km
2
Ca-239,90
150
ln
km
+ Giai on
NTH: Nhit
: 2700 , Thi gian: 3 giy.
1LOD
Mg-285,20
1
nhy
Nol:
0,5:
ngi
(ppb).
oC
iu
kin
nguyn
t
ho:0,2
ng/mL
+
Giai
on
trovch
ho:
Nhit
400
-(ppb).
600
,5,69
ThieV
gian: 30 giy.
Cng
n
HCL:
60
80%
I
Nguyn
t
lng:
58,7900.
Th
Ion
ho
oC I:
I:
7,61
eV
Nguyn
t
lng:
87,6200.
Th
Ion
ho
max
+
Giai
on
Nhit
:
120
200 , Thi
30 giy + Giai on
Khe
o:
0,5
-gy:
nm.
o
ph:
F-AAS
(Hp
th
nguyn
t).oCgian:
Cng
n
HCL:
60
- 80%
I-max
0,5
0,7
Khe
o:
-0,7
0,5
nm.
+Ch
Giai
on
lm
sch
Cuvt:
Nhit
:oC2800
, Thi
gian: 2 giy.
Nguyn
t.
2 0,7
40
ln30
km
Vng
tuyn
tnh:
- Mg-202,60
20 ng/mL.
ngi.
+ Giai
on
sy: 12Nhit
: 120 - 250
,
Thi
gian:
giy.
oC
Loi
Cuvt
Graphit:
Hot
ho
ton
phn.
oC
Ch
on
o
ph:
F-AAS
(Hp
th
nguyn
t).
Ch
o
ph:
F-AAS
th
nguyn
+
Giai
NTH:
Nhit
:
2400
,gian:
Thit).
gian:
3 giy.
tro
ho:
Nhit
:
500
-(Hp
700
, ton
Thi
20
giy.
Cng
n
HCL:
60
80%
I
Vch
Loi
Cuvt
ph
AAS:
Graphit:
Hot
ho
phn.
max
max
Cng
n
HCL:
60
80%
I
max ho
nhy3t
LOD
vch58,9332.
Nol: 0,5Th
ng/mL
(ppb).
Nguyn
lng:
Ion
I: 7,86
eVln km
100
+ t.
Giai on tro ho:Mg-279,60
Nhit : 600 - 800 oC, Thi
gian: 25 giy.
Nguyn
Kh
tr
mi
trng:
Argon.
oC
Vch
ph
o
AAS:
Vch
ph
o
AAS:
oC
Nguyn
t.tr
+
Giai
on
NTH:
Nhit
:
2450
, phn.
Thi
gian:, Thi
3 giy.
Loi
Cuvt
Graphit:
Hot
ho
tonphn.
lm
sch
Cuvt:
Nhit
:
2600
gian: 2 giy.
Loi
Cuvt
Graphit:
Hot
ho
ton
Kh
mi
trng:
Argon.
Vngtuyn
tnh:F-AAS
5Vch
- 80 (Hp
ng/mL.
ph (nm)
Ghi ch
N
Ch
ooph:
th nguyn
t).nhy ph km vch
oC
Mc
+
Giai
on
NTH:
Nhit
:
2650
,
Thi
gian:
3
giy.
Nguyn
t
lng:
55,847.
Th Ion ho I: 7,87oC eV
B
chnh
nn:
C
BC
Khe
o:
0,5
0,7
nm.
Nguyn
t
lng:
208,9806.
Th
Ion
ho
I:
7,29
eV
Kh
tr
mi
trng:
Argon.
+
lm
sch
Cuvt:
Nhit
2600 , Thi gian: 2 giy.
Vch
Vch
ph
ph
(nm)
Ghi
Ghi ch
ch
Kh
tron
N
N
mi
oLOD
trng:
B
chnh
nn:
C
BCArgon.
Giai
nhy
vch
Nol:
0,5(nm)
ng/mL:
(ppb).
Mc
Mc nhy
ph
ph
vch
s
1 km vch
Vch
o
AAS:
Nguyn
Ch
+ t.
Giai
ph
o
on
ph:
lm
F-AAS
sch Cuvt:
(Hp th
Nhit
nguyn
: 2800
t). oC, Thi gian: 2 giy
iu
kin
nguyn
tBC
ho:
Cng
n
HCL:
50(Hp
- 0,2
80%
I max
Ch
o
ph:
F-AAS
th
nguyn
Bchnh
chnh
nn:C
CBC
nhy
vch
Nol:
ngi
(ppb).t).
1 LOD
B
nn:
s1 1
iu
kin
nguyn
tAu-242,80
ho:
Vng
tuyn
tnh:
2,5
40
ng/mL.
Vch
ph
o
AAS:
Vch
ph0,5
(nm)
Ghi ch
Not
-
Nguyn
lng:
65,3700.
Th
Ion
ho
I:
9,39
nhy
LOD
vch
Nol:
ng/mL
(ppb).
oCMc nhy eV
ph
km
12 onguyn
Sr-460,70
Ni-232,00
130km
+
GiaiCuvt
on
sy;
Nhit
:
120ton
- 250phn.
, Thi gian:
giy.vch
Loi
Graphit:
Hot
ho
Au-267,60
ln
kin
ho:
Vch
ph
AAS:
Vng
tuyn
tnh:
1t-t
20
ngi.
iu
nguyn
ho:
+iu
Giaikin
on
sy:
Nhit
:
120 - 250 oC, Thi 2,5
gian:
30 giy.
s
1km
Vch
(nm)
Ghi
Ch
Vng
tuyn
o
tnh:
F-AAS
2,5
- ph
(Hp
25
th -nguyn
t).
N
oo ph:
oC oC
23mi
Sr-407,80
Ni-341,50
2,5
50
ln
ln
km
oC
Vch
ph
(nm)
Ghi ch
ch
N
Au-312,30
600
ln30
km
ph
km
vch
+Giai
Giai
on
sy:
Nhit
;ng/mL.
120
,oC
Thi
gian:
30
giy.
Nguyn
t.
+
tro
ho:
Nhit
:
600250
- 900
, nhy
Thi
gian:
30
giy.
Kh
tron
trng:
Argon.
:
,Thi
Thi
gian:
giy.
oCMc
Mc
nhy
ph
km
vch
+
Giai
on
sy:
Nhit
:
120
200
,
gian:
30
giy.
tro
ho:
Nhit
:
600
900
,
Thi
gian:
20
giy.
Co 240,70
1
Nguyn t. 13
Ni-305,10
ln
11km20 giy.
oC 4,5 s
Vch
phon
o AAS:
oC - 800 oC
+Giai
Giai
tro
Nhit
500
Thi
gian:
600
, ,Thi
gian:
20 giy.
+
on
NTH:
Nhit
::
2600
3sgiy.
B
chnh
nn:
Cho:
BC
Nguyn
t.
oC gian:
oC, Thi
Khe
o:on
0,5
nm.
+Nguyn
Giai
tro
ho:
Nhit
:
450
550
,
Thi
gian:
20 giy.
Khe
o:
0,7
0,5
nm.
t
lng:
28,0860.
Th
Ion
ho
l:
8,15
eV
NTH:
Nhit
:
2650
,
Thi
gian:
3
giy.
Co-242,50
1eV
5 ln
km
Fe-248,30
1
Nguyn1214t lng: 95,94.
Th Ion ho
I:
7,80
Ni-234,60
8
ln
km
Bi-223,10
1
oC
oC
oC
2600Ion
+Giai
Giai
on
NTH:
Nhit
:
2550
, Thi
3eV
giy.
Vch
ph
(nm)
Ghi ch
N
+
on
lm
sch
Cuvt:
Nhit
2700
, Thi
gian:
2 giy.
iu
kin
nguyn
t
ho:
lng:
107,8680.
Th
I:gian:
7,57
oC:ho
oC
Cng
HCL:
60
-- :
80%
II max
3 otn
Co
252,10
6,5
1nkm
Mc
nhy
ph
km vch
+Nguyn
Giai on
NTH:
Nhit
1900
,
Thi
gian:
3ln
giy.
Cng
n
HCL:
50
80%
lm
sch
Cuvt:
Nhit
:
2800
, Thi
gian:
2 giy.
max
2
Fe-248,80
km
ph: F-AAS
Bi-222,80
4
ln
km
Ch 2o ph:
(Hp th nguyn t).2,3
oC
oC
oC 2700 , Thi
+Giai
Giai
on
lm
sch
Cuvt:
Nhit
:
Khe
o:
0,5
-gy:
0,7
nm.
s 30
1 gian:
nhy
LOD
vch
Nol:
0,5
ng/mL
(ppb).
+
on
Nhit
:
120
- 250
, Thi
gian:
giy. 2 giy.
Ch
o
ph:
F-AAS
(Hp
th
nguyn
t).
oC3
Loi
Cuvt
Graphit:
Hot
ho
ton
phn.
3
Fe-271,90
ln
km
+
Giai
on
lm
sch
Cuvt:
Nhit
:
2200
,
Thi
gian:
2 giy.
Loi
Cuvt
Graphit:
Hot
ho
ton
phn
nhy
LOD
vch
Nol:
0,5
ng/mL
(ppb).
3
Bi-306,80
4,5
ln
km
Khe
0,7o- AAS:
0,5 nm.
Vcho:
ph
ph
1
Zn-213,90
1
nhy
LOD
vch
Nol:
0,5
ng/mL
(ppb).
nhy
LOD
vch
ng/mL
Cng
n
HCL:
60ng/mL.
-0,5
80%
I max -(ppb).
Vng
tuyn
tnh.4
- Nol:
40
+
Giai
on
tro
ho:
Nhit
:
600
900 oC, Thi
gian:
20 giy. + Giai
Vch
ph
otrng:
AAS:
44
10
km
Bi-227,70
35 ln
ln
km
Kh
trtuyn
mi
Argon.
Vng
tnh:
52-Fe-372,00
80
Vng
tuyn
tnh:
-60
20-ng/mL.
ng/mL.
Cng
n
HCL:
80%
I
max
2
2000 ln km
Vng tuyn
tnh: 2 Zn-307,60
- 30 ng/mL.
oC ton phn.
Loi Cuvt
Graphit:
on
NTH:
Nhit
:Hot
2600ho
, Thi gian: 3 giy.
B
chnh
nn:
C BC
Mn
Al
Ti
Ba
Pb
Cr
Ca
Mg
Au
Ni
Si
Co
Fe
Bi
Zn
Si
Mo
Ao
272
274
280
284
286
282
276 288
278
279
277
275
283
273
285
281
287
TI LIU THAM KHO
RiChard D. Beaty & Jack D. Kerber, 1979 & 1983, Concepts on Instrumentation and
Techniques in Atomic Emission Spectrophotometry, Perkin Elmer Company.
Hobart H. Willard, Lynne L. Merritt, John A. Dean & Frank A. Settle, 1993, Instrumental
Methods for Analysis, Wadsworth Pub. Company, 6th Edition.
E.L. Grove, 1978, Applied Atomic Spectroscopy, Plenum Press, New York.
M. Pinta, 1979, Atomic Absorption and Emission Spectrometry, Vol. I & II, London, Hilger.
Peter J. Whitesside, 1979 & 1985, Atomic Spectrometry Data Book, Pye Unicam, Ltd.
R.E. Stuegeon & C.L. Charrabarti, 1979 & 1985, Recent Advances in Atomic Emission
Spectrometry, Perkin Elmer.
Douglas A. Skoog & James J. Leary, 1995. Principles of Instrumental Analysis, Saunder8
College Pub., 4th Edit Ion, New York, London.
Perkin Elmer Company, 1985-90, Some Application Notes In AAS, Perkin Elmer Ltd.
S.S. M. Hassan, 1984, Organic Analysis Using Atomic Spectrometry, Amsterdam, Hilger,
London.
J.B. Dowson, 1989, Annual Reports on Analytical Atomic Spectroscopy, Vol. 7 & 8,
Amsterdam, London.
Daniel C. Harris, 1998, Quantitative Chemical Analysis, Fifth Edit Ion, W.H. Freeman &
Company, New York.
Douglas A. Skoog, Donald M. West & F. James Holler, 1995. Fundamentals of Instrumental
Analysis, 7th Edit Ion, New York, London, Amsterdam, Tokyo.
James D. Ingle, Jr. & Stanley R. Grouch, 1992, Spectro-chemical Analysis, Prentice Hall, Upper
Saddle River, New Jersey.
Geoge R. Harrison, 1979, Wavelength Tables, The M.I.T. Press, Cambridge, London.
R.M. Barnes, 1987, Application Inductively Coupled Plasma Emission Spectroscopy, Easten
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John H. Kennedy, 1990, Analytical Chemistry Principles, Saunders College Pub., 2nd Edit Ion,
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289
Nguyn Phng Tho, 2005, Lun n thc s, Trng H KHTN - HQG H Ni.
Jose A.C. Broekaet, 2002, Atomic Analytical Spectrophotometry, Wiley CH. Ltd., New York London - Amsterdam - Tokyo.
Shimadzu Company, 2002, AAS Cook Book, Shimadzu Company.
Phm Th Qunh Lng, 2002, Lun n thc s, Trng H KHTN - HQG H Ni.
290
MC LC
PHN 1..........................................................................................................................................................3
Chng 1: I CNG V PHNG PHP AES ..................................................................................3
S phn loi ph............................................................................................................................................3
S phn chia theo c trng ca ph ...................................................................................................3
Phn chia theo di sng...................................................................................................................4
S xut hin ph pht x nguyn t.........................................................................................................5
Tm tt v cu to nguyn t ...............................................................................................................5
S xut hin ph pht x......................................................................................................................7
Nguyn tc ca php o ph pht x (AES) ............................................................................................9
i tng ca phng php phn tch ph pht x .............................................................................. 14
Cc u im v nhc im...................................................................................................................14
Kh nng v phm vi ng dng..............................................................................................................15
Chng 2: S KCH THCH PH PHT X NGUYN T................................................................17
Yu cu v nhim v ca ngun kch thch...........................................................................................17
Cc loi ngun kch thch ph pht x ...................................................................................................18
Ngn la n kh................................................................................................................................ 18
H quang in.....................................................................................................................................23
Tia la in.........................................................................................................................................28
Plasma cao tn cm ng ICP ..............................................................................................................34
Nguyn tc v cch chn ngun kch thch ph ....................................................................................40
Cng vch ph pht x nguyn t ..................................................................................................41
Cng vch ph :.......................................................................................................................... 41
Cng vch ph v nhit plasma ............................................................................................ 44
Hin tng t hp th (t o) ...............................................................................................................45
Bc x nn trong ph pht x.................................................................................................................46
Chng 3: MY QUANG PH V S PHN LI CHM SNG.........................................................47
Nguyn tc cu to ca my quang ph pht x...................................................................................47
Cc loi my quang ph pht x............................................................................................................50
Lng knh v my quang ph lng knh ............................................................................................50
Cch t v my quang ph cch t....................................................................................................61
Vng lm vic ca my quang ph........................................................................................................67
Trang b ca h thng my quang ph pht x ......................................................................................68
Trang b pht hin v thu nhn ph ........................................................................................................68
Knh nh quang ph............................................................................................................................68
o en Sx ca vch ph trn knh nh........................................................................................70
ng nhn quang in (Photomultiplier tubes) ..................................................................................71
Chng 4: Cc yu t nh hng trong AES.............................................................................................75
Khi qut chung......................................................................................................................................75
291
4.2 Mt s nh hng trong php o AES .............................................................................................75

Cc yu t v ph................................................................................................................................75
Cc yu t vt l...................................................................................................................................77
Cc yu t ha hc..............................................................................................................................79
Chng 5: PHN TCH QUANG PH PHT X NH TNH............................................................88
Nguyn tc chung....................................................................................................................................88
Vch chng minh nh tnh v cch chn ..............................................................................................89
nhy ph v kh nng pht hin ....................................................................................................... 90
nhy tuyt i (cn gi l nhy khi lng) ..........................................................................90
nhy tng i (cn gi l nhy nng ) ..............................................................................90
S trng vch v cch loi tr ................................................................................................................93
Vch ph trng....................................................................................................................................93
Vch quy ri v chen ln ..................................................................................................................93
Ph m...............................................................................................................................................93
Cc phng php phn tch nh tnh .....................................................................................................94
Phng php quan st trc tip trn mn nh ................................................................................... 95
Phng php so snh ph...................................................................................................................95
Phng php ph chun (Dng bn atlas) .........................................................................................96
Chng 6: PHN TCH PH PHT X NH LNG ....................................................................... 99
Nhng vn chung................................................................................................................................99
Phng trnh c bn v nguyn tc....................................................................................................99
Vch phn tch v cch chn ............................................................................................................101
Cch biu din nng trong phn tch quang ph ........................................................................102
Mu chun trong phn tch quang ph pht x................................................................................104
Gii hn chng minh v khong xc nh .......................................................................................106
S bay hi v ng cong bay hi...................................................................................................108
6.1.7. Kh quyn kim tra.................................................................................................................110
Cht m v cht ph gia trong phn tch ph pht x...................................................................113
Phn tch quang ph pht x bn nh lng .......................................................................................119
Phng php so snh.........................................................................................................................119
Phng php hin vch.....................................................................................................................120
Phn tch quang ph pht x dinh lng ..............................................................................................121
Phng php ng chun ...............................................................................................................121
Phng php th chun khng i .............................................................................................. 124
Phng php thm tiu chun ..........................................................................................................125
Phng php theo 1 mu chun ....................................................................................................... 127
Cc phng php xc nh gin tip bng AES ...................................................................................128
Nguyn tc.........................................................................................................................................128
Cc phng php phn tch gin tip ...............................................................................................128
Phn II........................................................................................................................................................ 135
292
Chng 7: NHNG VN CHUNG CA PHP O ASS................................................................135

S xut hin ph hp th nguyn t......................................................................................................135
Cng ca vch ph hp th nguyn t ...........................................................................................137
Cu trc ca vch ph hp th nguyn t.............................................................................................140
Nguyn tc v trang b ca php o AAS .............................................................................................143
Nhng u v nhc im ca php do AAS........................................................................................145
i tng v phm vi ng dng ca AAS ............................................................................................147
Chng 8: Cc k thut nguyn t ha mu ......................................Error! Bookmark not dened.
Mc ch v nhim v...........................................................................................................................149
K thut nguyn t ha mu bng ngn la ..........................................................................................149
Yu cu v nhim v ca ngn la...................................................................................................149
c im v cu to ca ngn la n kh.......................................................................................151
Trang b nguyn t ha mu........................................................................................................ 152
Nhng qu trnh xy ra trong ngn la............................................................................................156
Ti u ha cc iu kin nguyn t ha mu...................................................................................163
K thut nguyn t ha khng ngn la................................................................................................165
c im v nguyn tc....................................................................................................................165
Cc yu cu h thng nguyn t ha mu ........................................................................................166
Nguyn tc v cc giai on ca qu trnh nguyn t ha mu ...................................................... 166
Cc yu t nh hng........................................................................................................................174
Cc qu trnh trong cuvet graphit ..................................................................................................... 177
Trang b nguyn t ha mu........................................................................................................ 182
Ti u ha cc diu kin cho php o khng ngn la mu...........................................................183
Chng 9: TRANG B CA PHP O ASS............................................................................................185
Ngun pht bc x n sc...................................................................................................................185
n catot rng (HCL) ....................................................................................................................... 186
n phng in khng din cc (EDL)............................................................................................189
n ph lin tc c bin iu........................................................................................................... 192
Cc loi ngun n sc khc .............................................................................................................194
Trang b nguyn t ha mu.............................................................................................................194
H thng n sc v my quang ph hp th nguyn t ......................................................................195
Trang b pht hin, Detector, Photomultivlier......................................................................................197
K thut o cng vch ph hp th................................................................................................198
Chng 10: Cc yu t nh hng trong AAS..........................................................................................201
Khi qut chung.....................................................................................................................................201
Mt s nh hng trong php do AAS ................................................................................................. 201
10.2.1 Cc yu t v ph...................................................................................................................201
10.2.3 Cc yu t ha hc.................................................................................................................207
Chng 11: Phn tch nh lng bng ph AAS.....................................................................................219
1 1 . 1 Nhng vn chung....................................................................................................................219
293
Phng trnh c bn ca php o....................................................................................................219

Mu chun trong php o AAS ........................................................................................................221
Biu din nng trong php o AAS ............................................................................................222
Khi nim v nhy.......................................................................................................................225
Gii hn pht hin trong AAS.........................................................................................................229
Khong xc nh trong php o AAS ..............................................................................................231
B chnh nn trong php o AAS ....................................................................................................232
Ti u ha cc iu kin cho php o AAS....................................................................................237
Cc phng php phn tch c th .......................................................................................................240
Phng php th chun (ng chun) ......................................................................................240
Phng php thm tiu chun ..........................................................................................................242
Phng php th chun c nh ..................................................................................................243
Phng php mt mu chun ...........................................................................................................245
Cc kiu phng php phn tch theo AAS .........................................................................................246
Cc phng php xc nh trc tip ................................................................................................246
Cc phng php xc nh gin tip cc cht bng AAS ...............................................................247
Chng 12: CC IU KIN O PH HP TH NGUYN T V PHT X
NGN LA CA MT S NGUYN T............................................................................................257
Phn I. PHP O PH NGN LA.......................................................................................................257
Phn II. PHP O KHNG NGN LA...............................................................................................272
TI LIU THAM KHO.........................................................................................................................289
294

16 Hng Chui - Hai B Trng - H Ni in thoi: (04) 9718312; (04) 7547936;
Fax: (04) 9714899 Email: nxb@vnu.edu.vn
***
Chu trch nhim xut bn:
Gim c: PHNG QUC BO Tng bin
tp: PHM THNH HNG Chu trch nhim ni dung:
Hi ng nghim thu gio trnh Trng
HKHTN - i hc Quc gia H Ni Ngi nhn xt:
GS. TSKH TRNH XUN GIN TS. NGUN
HONG
Bin tp:
H TH IP - QUC THNG Bin tp ti
bn:
INH QUC THNG
V hnh:
INH QUC THNG
Trnh by ba:
NGUYN NGC ANH
PHNG PHP PHN TCH PH NGUYN T

M s 1K-25 H2006
In 1000 cun, kh 19 x 27cm ti Xng in Tng cc Cng nghip Quc phng S
xut bn: 105 - 2006/CXB/62 - 08/HQGHN, ngy 10/02/2006.
Quyt nh xut bn s: 173 KH/XB In xong v np lu chiu qu 11 nm 2006.
295
PHM LUN
PHNG PHAP PHAN TICH

PH NGUYN T
LI M U
Php o ph pht x v hp th nguyn t l nhng k thut phn tch ha l, v

ang c pht trin v ng dng rng ri trong nhiu ngnh khoa hc k thut, trong sn
xut cng nghip, nng nghip, y dc, a cht, ha hc. c bit cc nc pht trin,
phng php phn tch ph pht x nguyn t tr thnh mt trong cc phng php dng
phn tch lng vt cc kim loi trong nhiu i tng khc nhau nh t, nc, khng
kh, thc phm, v.v... Hin nay trong cng tc nghin cu bo v mi trng, phng php
phn tch ny l mt cng c c lc xc nh cc kim loi nng c hi.
vin tr ca cc t chc nc ngoi theo cc chng trnh khc nhau. Mt s cn b khoa
hc ca ta c c ra nc ngoi hc tp, nghin cu v o to.
a skhng ciu kin
,nhng
Song i
ny cho cng vic phn tch ca h. Hu ht cc ti liu hay sch khoa hc v k thut ny
li bng ting Anh. Mt khc, chng ta li cha c mt cun sch hoc cc ti liu c s l
thuyt bng ting Vit v k thut phn tch ny.
trnh khi nhng hn ch v thiu st nht nh. V th rt mong s ng gp thm kin
ca cc bn b ng nghip v cc c gi quan tnm, tc gi c iu kin b sung cho
hon chnh hn.
Nguyn Hong (HQGHN), PGS. TS. Phm Gia Hu (H Dc) v cc ng nghip B
mn Ha Phn tch khoa Ha hc c nhiu kin ng gp cho ni dung ca gio trnh
ny.
Phm Lun
PHN I
Chng 1
S phn loi ph
Phn tch quang ph l tn gi chung cho mt h cc phng php phn tch quang hc da trn
c s ng dng nhng tnh cht quang hc ca nguyn t, Ion, phn t v nhm phn t. V d, tnh
cht pht x hay hp th quang ca nguyn t, tinh cht hp th quang ca phn t, v.v... V vy ty theo
quan nim, da theo nhng iu kin kch thch ph, phng tin thu ghi v quan st ph, cng nh bn
cht ca qu trnh sinh ra ph m ngi ta c mt s cch phn chia thnh nhng php o khc nhau, nh
php o ph pht x nguyn t, hp th nguyn t, php o ph hng ngoi,... Tuy th, nhng c hai cch
phn chia sau y l ph hp hn:
S phn chia theo c trng ca ph


Ph php x nguyn t
Ph hp th nguyn t
Ph hunh quang nguyn t
y l ph do s chuyn mc nng lng ca cc in t ha tr ca nguyn t trng thi kh
(hi) t do, khi b kch thch m sinh ra.

Ph hp th phn t trong vng UV-VIS
Ph hng ngoi (IR v NIR)
Ph tn x Raman
Ph ny c quyt nh bi cc in t ha tr ca nguyn t trong phn t, l nhng in t
ha tr nm trong lin kt hay mt cp cn t do, chuyn mc nng lng khi b kch thch.
+ Ph pht x tia X
+ Ph nhiu x tia X
Ph cng hng t, gm:

Cng hng t in t (ERMS).
Cng hng t proton (ht nhn: NRMS))
Phng php phn tch khi ph: Ph ny c quyt nh bi khi lng ca cc Ion
phn t hay cc mnh Ion ca cht phn tch b ct ra (t s m/z).
y l cch phn chia c s dng rng ri v c coi nh l hp l nht v tng
ng vi ngay tng php o c th..
Phn chia theo di sng
Nh chng ta bit, bc x in t c mi bc sng, t sng di hng ngn mt
n sng ngn vi micromet hay nanomet. Do ph ca bc x in t y phi cha
ht tt c cc vng sng . Nhng trong thc t khng c mt dng c quang hc no c th
c kh nng thu nhn, phn li hay pht hin c ton b vng ph nh th. V th ngi ta
chia ph in t thnh nhiu min (vng ph) khc nhau. l nguyn tc ca cch chia th
hai ny (bng 1.1).
Bng 1.1
S phn chia ph theo di sng
STT
Tn vng ph
di sng
Tia gama (Y)
< 0,1 nm
Tia X
0,1+ 5 nm
T ngoi
80 + 400 nm
Kh kin
400 + 800 nm
Hng ngoi
1+ 400 p,m
Sng ngn
400 + 1000 p,m
Sng Raa
0,1+ 1 cm
Sng cc ngn
0,1 - 50 cm
Tivi - FM
1 + 10 m
10
Sng raio
10+ 1500m

s chuyn mc nng lng ca cc in t ha tr ca nguyn t v phn t, khi b kch
thch. Vic phn chia theo cch ny cng c nhng im cha r rng, nh trong vng t
ngoi v kh kin th c c ph ca nguyn t v phn t, m bn cht ca hai loi ph v
s kch thch ca hai loi li rt khc nhau.
4
Table of Contents
Gas Management.........................................................1
Gas Types...........................................2
Gas Purification Systems....................4
Renewable Gas Purification System....6
Gas Traps............................................7
Universal/External Split Vent Trap.....13
Internal Split Vent Trap......................13
Flow Meters......................................14
Gas Leak Detector............................16
Low Gas Alarm System.....................18
Regulators........................................20
Tubing...............................................21
Sample Introduction..................................................23
Vials.................................................24
Electronic Crimpers and Decappers. .28
Syringes...........................................29
Autosampler Syringes.......................35
Manual Syringes...............................43
7693A Automatic Liquid Sampler Parts
& Supplies........................................52
Headspace Sampler..........................53
CTC Autosampler Supplies................56
Purge and Trap Supplies...................59
Markes Thermal Desorption..............61
Premium Non-Stick Septa..................64

Split/Splitless Liners..........................68
Direct Connect Liners........................73
Programmable Temperature Vaporizing
(PTV)
Liners..........74
Liner O-Rings....................................75
Ferrules.............................................76
Capillary Flow Technology Supplies. . .80
Inlet Systems....................................83
Multimode Inlet.................................86
Split/Splitless Inlets...........................89
Cool On-Column Inlets.......................96
Purged Packed Inlets.......................101
Programmed Temperature Vaporizer
(PTV) Inlets.....................................104
Detectors...................................................................109
Flame Ionization Detector (FID).......110
Electron Capture Detector (ECD).....117
Thermal Conductivity Detector (TCD)
.......................................................120
Flame Photometric Detector (FPD). .125
Nitrogen Phosphorus Detector (NPD)
.......................................................133
Nitrogen
and
Sulfur
Chemiluminescence Detectors........139
GC/MS Systems.....................................................141
Maintaining Mass Selective Detectors
(MSD)..............................................142
MSD Contamination........................143
Cleaning and Maintenance Supplies
.......................................................149
Ion Source.......................................151
Installing a Capillary Column in the
GC/MSD
Interface.....156
QuickSwap MS Interface Restrictors 158
Gas Management
Avoid column damage, improve detector life, and
achieve reliable, consistent results.
Gas management means more than just selecting
the appropriate carrier gas for your needs. It also
means taking steps to prevent contaminants like
oxygen, moisture, and hydrocarbons from damaging
your GC column.
As you read through the following pages, you will
find:
Practical advice about carrier gas types, impurities,
leak detection, and flow rates
Valuable techniques that can minimize the likelihood
Order online at
www.agilent.com/chem/store
DONG Bank
^m/ kry pAi' t/ ny hon/ ho/
n/
nn/em/t/duy/nAt/
Chc mng ngy Ph n Vit Nam 20/10!
A./*
PHM LUN
PHNG PHAP PHAN TICH

PH NGUYN T
LI M U
Php o ph pht x v hp th nguyn t l nhng k thut phn tch ha l, v ang

c pht trin v ng dng rng ri trong nhiu ngnh khoa hc k thut, trong sn xut cng
nghip, nng nghip, y dc, a cht, ha hc. c bit cc nc pht trin, phng php
phn tch ph pht x nguyn t tr thnh mt trong cc phng php dng phn tch
lng vt cc kim loi trong nhiu i tng khc nhau nh t, nc, khng kh, thc phm,
v.v... Hin nay trong cng tc nghin cu bo v mi trng, phng php phn tch ny l
mt cng c c lc xc nh cc kim loi nng c hi.
vin tr ca cc t chc nc ngoi theo cc chng trnh khc nhau. Mt s cn b khoa hc
ca ta c c ra nc ngoi hc tp, nghin cu v o to.Song i
s khng ciu kin
,nhng
ny cho cng vic phn tch ca h. Hu ht cc ti liu hay sch khoa hc v k thut ny li
bng ting Anh. Mt khc, chng ta li cha c mt cun sch hoc cc ti liu c s l thuyt
bng ting Vit v k thut phn tch ny.
trnh khi nhng hn ch v thiu st nht nh. V th rt mong s ng gp thm kin ca
cc bn b ng nghip v cc c gi quan tnm, tc gi c iu kin b sung cho hon
chnh hn.
Nguyn Hong (HQGHN), PGS. TS. Phm Gia Hu (H Dc) v cc ng nghip B mn
Ha Phn tch khoa Ha hc c nhiu kin ng gp cho ni dung ca gio trnh ny.
Phm Lun
PHN I
Chng 1
S phn loi ph
Phn tch quang ph l tn gi chung cho mt h cc phng php phn tch quang hc da trn c
s ng dng nhng tnh cht quang hc ca nguyn t, Ion, phn t v nhm phn t. V d, tnh
cht pht x hay hp th quang ca nguyn t, tinh cht hp th quang ca phn t, v.v... V vy ty theo
quan nim, da theo nhng iu kin kch thch ph, phng tin thu ghi v quan st ph, cng nh bn
cht ca qu trnh sinh ra ph m ngi ta c mt s cch phn chia thnh nhng php o khc nhau, nh
php o ph pht x nguyn t, hp th nguyn t, php o ph hng ngoi,... Tuy th, nhng c hai cch
phn chia sau y l ph hp hn:
S phn chia theo c trng ca ph


Ph php x nguyn t
Ph hp th nguyn t
Ph hunh quang nguyn t
y l ph do s chuyn mc nng lng ca cc in t ha tr ca nguyn t trng thi kh (hi)
t do, khi b kch thch m sinh ra.

Ph hp th phn t trong vng UV-VIS
Ph hng ngoi (IR v NIR)
Ph tn x Raman
Ph ny c quyt nh bi cc in t ha tr ca nguyn t trong phn t, l nhng in t
ha tr nm trong lin kt hay mt cp cn t do, chuyn mc nng lng khi b kch thch.
+ Ph pht x tia X
+ Ph nhiu x tia X
Trncng
y l
hai cch
phn chia chnh cn hay c dng. Tt nhin cn c mt s cch
Ph
hng
t, gm:
phn chia khc. Nhng c nhiu nhc im v t c s dng, nn khng cp n y.
Cng hng t in t (ERMS).
S phn chia ny c tnh cht gii thiu chung ton b vng ph. Song, trong gio trnh
Cng
proton
(ht x
nhn:
NRMS))
ny chng ti
ch hng
cp t
n
ph pht
nguyn
t, v phng php phn tch ng dng tnh
Phng
php
phnttch
khi ph:
Phc
ny c
nhphn
bi tch
khiph
lng
Ion
cht pht
x ca
nguyn
trng
thi hi
gi lquyt
K thut
phtca
x cc
nguyn
phn
t. t hay cc mnh Ion ca cht phn tch b ct ra (t s m/z).
y
l ph
cchpht
phn
cts dng rng ri v c coi nh l hp l nht v tng
S xut
hin
xchia
nguyn
ng
o t
c th..
Tmvi
tt ngay
v cutng
to php
nguyn
Phn chia
chng
di sng
Hngtheo
ngy
ta thng quen vi nhng tn gi, st (Fe), ng (Cu) ch (Pb), bc
Nh chng
ta (Aj),
bit, bc
in t
mi nguyn
bc sng,
t hc.
sngn
di nay
hngngi
ngntamt
(Ao), vng
(Au), nhm
kmx
(Zn),...
c
l
nhng
t ha
n
sng
ngn
vi
micromet
hay
nanomet.
Do
ph
ca
bc
x
in
t
y
phi
cha
ht
bit trn 110 nguyn t ha hc khc nhau. Nhng v mt ha hc v theo thuyt ca alton,
tt
c cc
sngbao
.gm
Nhng
trong
thc t
c mt
cnguyn
quang hc
c t
thnh
c
nguyn
t vng
ha hc
nhng
nguyn
t khng
ca cng
mt dng
loi v
t lno
phn
kh
thu c
nhn,tnh
phncht
li hay
c ton
vng ph
nhmi
th.nguyn
V th t
ngi
chia
nhtnng
cn gi
hapht
hc hin
ca nguyn
t. b
Nguyn
t ca
ha ta
hc
c
ph
inkhc
t thnh
min c
(vng
l nguyn
tc cht
ca cch
th hc
hai
cu to
nhau nhiu
nn chng
tnhph)
cht khc
khc nhau.
nhau.
Quyt
nh tnh
vt lchia
v ha
ny
(bng 1.1).
ca chng
l cu to ca lp v electron trong nguyn t, c bit l cc in t ha tr.
Bng
Nguyn t ca mi nguyn t ha hc
u1.1
c xy dng t mt ht nhn nguyn t v
S
chia(in
ph theo
di nguyn
sng t, ht nhn gia, cc in t chuyn ng xung quanh
ccphn
electron
t). Trong
ht nhn theo nhng qu o (orbital) tng i. Ht nhn chim th tch rt nh trong khng
Tn vngth
phtch nguyn t), nhng
di li
sng
gian ca nguynSTT
t (khong 1/10.000
chim hu nh ton b
khi lng ca nguyn t. Nu coi ng knh nguyn t l 10-8cm, th ng knh ht nhn
gama (lp
Y) v ca nguyn
< 0,1 nm
ch chim khong110-12cm. NhTia
vy,
t
ngoiht
nhnTia
l rtrng,
n chnh l khng gian0,1+ 5 nm
2
X
chuyn ng ca in t. S chuyn ng ca in t trong khng gian ny rt phc tp. N
3
T ngoi
80 + 400 nm
va tun theo quy lut ca chuyn ng sng, li va tun theo quy lut chuyn ng ca cc
4
Kh
kin
400 i,
+ 800
nm ta vn tha nhn
ht vi m. Song trong
mt iu
kin
nht nh v mt cch tng
ngi
cc in t chuyn
khngngoi
gian ca nguyn t theo ccqu
5 ng trongHng
1+ 400o.
p,m Nhng theo quan
my electron.
7 nguyn
Trong lp v
im hini cac lng

t th l cc m
Sng ngn
400 + 1000 p,m
Sng
t, Raa
in tphn b
0,1+lp
1 cm
thnh tng
ng
vi s lng t
chnh ca nguyn8t (n). Trong

tngcc
lpngn
li c nhiu qu o ng
Sng
0,1 -vi
50 s
cmlng t ph 1 ca
nguyn t. l cc phn lp. Nhng theo nguyn l vng bn th in t bao gi cng chim
9
Tivi - FM
1 + 10 m
v lm y nhng qu o c mc nng lng thp trc. Sau mi n nhng qu o c
10
Sng raio
10+ 1500m
mc nng lng cao hn. Th t sp xp l: ls, 2s, 2p, 3s, 3p, 4s, 3d, 4p, 5s, 4d, 5p, 6s, 4f,
5d, 6p, 7s, 5f, 6d, 7p, v.v... (hnh 1.1a).
s chuyn mc nng lng ca cc in t ha tr ca nguyn t v phn t, khi b kch thch.
Vic phn chia theo cch ny cng c nhng im cha r rng, nh trong vng t ngoi v
kh kin th c c ph ca nguyn t v phn t, m bn cht ca hai loi ph v s kch
thch ca hai loi li rt khc nhau.
4
Hnh 1.1a
(1 )-cu to nguyn t: (2 )-phn b nng lng trong lp v nguyn t.
Qu trnh pht x v hp th ca mt nguyn t.

E0: Nng lng trng thi c bn; cm: Nng lng trng thi kch thch; + hv v +
AE: Nng lng kch thch; - hv: Tia pht x.
(n = 5)
(n = 4)
(n = 3)
(n = 2)
Hnh 1.1 b
S phn b nng lng trong nguyn t v sinh ph
S xut hin ph pht x
Trong iu kin bnh thng, cc in t chuyn ng trn cc qu o ng vi mc
nng lng thp nht. Khi nguyn t trng thi bn vng, trng thi c bn. trng thi
ny nguyn t khng thu v cng khng pht nng lng. Nhng nu cungcp nng lng cho
nguyn t th trng thi khng tn ti na. Theo quan im ca thuyt lng t, khi trng
thi kh, in t chuyn ng trong khng gian ca nguyn t, c bit l cc in t ha tr,
nu chng nhn c nng lng bn
7
ngoi (in nng, nhit nng, ha nng,...) th in t s chuyn ln mc nng lng cao hn.
Khi nguyn t b kch thch. N tn ti trng thi kch thch. Nhng trng thi ny
khng bn vng. Nguyn t ch lu li trng thi ny nhiu nht l 10 8 giy. Sau n lun
lun c xu hng tr v trng thi c bn ban u bn vng. Ngha l gii phng nng lng
m chng hp th c trong qu trnh trn di dng ca cc bc x quang hc. Bc x
ny chnh l ph pht x ca nguyn t, n c tn s c tnh theo cng thc:
AE = (En - Eo) = hv
(1.1)
hay: AE =
X
trong :
En v E0 l nng lng ca nguyn t trng thi c bn v trng thi kch thch n;
h l hng s Plank (6,626.10 -7 erk.s) hay h = 4,1.10-15 eV.s;
c l tc nh sng (3.108 m/gy) - 2,99793.108 m/gy;
v l tn s ca bc x ;
X l bc sng ca bc x .
Trong biu thc trn, nu gi tr AE l nm ta c qu trnh hp th v khi gi tr AE
dng ta c qu trnh pht x ca nguyn t.
Nhng trong nguyn t, s chuyn mc ca in t t mc nng lng E n khng phi
ch v mc E0, m c rt nhiu s chuyn mc t E n v cc mc khc E 01, E02, E03_ cng vi
mc E0. Ngha l c rt nhiu s chuyn mc ca in t c lng t ha, v ng vi
mi bc chuyn mc ta c 1 tia bc x, tc l mt vch ph. Chnh v th m mt nguyn
t khi b kch thch thng c th pht ra rt nhiu vch ph pht x. Nguyn t no c nhiu
in t v c cu to phc tp ca cc lp in t ha tr th cng c nhiu vch ph pht x.
Mt cch tng trng ta c th m t qu trnh kch thch v pht x ca nguyn t theo m
hnh trong hnh 1.2.
Nu dng my quang ph thu chm ra pht x , phn li v ghi li cc chm tia pht
x do nguyn t pht ra ta s c mt di ph t sng ngn n sng di. l ph pht x
ca nguyn t ca cc nguyn t v n l ph vch. Nh vy, ph pht x nguyn t l sn
phm sinh ra do s tng tc vt cht, m y l cc nguyn t t do trng thi khvi
mt
ngun
nng
lng
nhit, in... nht nh ph hp.
Nhng trong ngun sng, khng phi ch c nguyn t t do b kch thch, m c c Ion, phn
t, nhm phn t. Cc phn t ny cng b kch thch v pht ra ph pht x ca n. Tt nhin
l trong mc khc nhau ty thuc vo kh nng kch thch ca ngun nng lng. V vy,
ph pht x ca vt mu lun bao gm ba thnh phn:
Nhm ph vch. l ph ca nguyn t v con. Nhm ph vch ny ca cc nguyn
t ha hc hu nh thng nm trong vng ph t 190-1000nm (vng UV- VIS). Ch c mt
vi nguyn t kim hay kim loi kim mi c mt s vch ph nm ngoi vng ny.
Nhm ph m. l ph pht x ca cc phn t v nhm phn t. V d
ph ca phn t MeO, CO v nhm phn t CN. Cc m ph ny xut hin thng c mt u m v

mt u nht. u m pha sng di v nht pha sng ngn. Trong vng t ngoi th ph ny xut
hin rt yu v nhiu khi khng thy. Nhng trong vng kh kin th xut hin rt m, v lm kh khn
cho php phn tch quang ph v nhiu vch phn tch ca cc nguyn t khc b cc m ph ny che lp.
3. Ph nn lin tc. y l ph ca vt rn b t nng pht ra, ph ca nh sng trng v ph do

s bc x ring ca in t. Ph ny to thnh mt nn m lin tc trn ton di ph ca mu. Nhng nht
sng ngn v m dn v pha sng di. Ph ny nu qu m th cng s cn tr php phn tch.
Ba loi ph trn xut hin ng thi khi kch thch mu phn tch v trong phn tch quang ph pht
x nguyn t ngi ta phi tm cch loi bt ph m v ph nn. l hai yu t nhiu.
Nguyn tc ca php o ph pht x (AES)

T vic nghin cu nguyn nhn xut hin ph pht x, chng ta c th khi qut phng php phn
tch da trn c s o ph pht x ca nguyn t phi bao gm cc bc nh sau:
Trc ht mu phn tch cn c chuyn thnh hi (kh) ca nguyn t hay Ion t do trong mi
trng kch thch. l qu trnh ha hi v nguyn t ha mu. Sau dng ngun nng lng ph hp
kch thch m hi chng pht x. y l qu trnh kch thch ph ca mu.
Thu, phn 1i v ghi ton b ph pht x ca vt mu nh my quang ph. Trc y, ph c ghi
ln knh nh hay phim nh. Chnh my quang ph s lm nhim v ny. Nhng nhng trang b hin i
ngy nay c th thu v ghi trc tip cc tn hiu cng pht x ca mt vch ph di dng cc lc trn
bng giy hay ch ra cc sng cng vch ph trn my in (printer), ghi li vo a t ca my tnh.
nh gi ph ghi v mt nh tnh v nh lng theo nhng yu cu t ra. y l cng vic
cui cng ca php o.
Chnh v vy, ng vi cc nhim v v nguyn tc ny, thc hin mt php phn tch da theo
ph pht x ca nguyn t ngi ta phi cn mt h thng trang b cng gm ba phn tng ng nh th.
Trang b c bn (ti thiu phi c):

Phn 1: Ngun nng lng ha hi, nguyn t ha mu v kch thch ph ca mu phn tch,
c ph ca nguyn t phn tch.
Phn 2: My quang ph thu, phn li v ghi li ph pht x ca mu phn tch theo vng ph ta
mong mun.
Phn 3: H thng trang b nh gi nh tnh, nh lng v ch th hay biu th cc kt qu.
Mt cch tng qut, ta c th m t nguyn tc ny theo s hnh 1.3.
Ion Mg+
Si
ng
let
Tr
ip
let
Hnh
1.2b
S
vch
ph
pht
x ca
nguy
n t
Mg
Trang b hon chnh:

C thm cc b phn sau:
B t ng bm hay a mu vo o.
11
H my tnh v phn mm ca n.
Mu phn tch
Ngun E
Ha hi, nguyn t ha v
kch thch ph pht x
Ngn la
H quang
Tia
in
ICP(AES)
Thu, phn li, ghi bc x
plasma
N
n
g
(theo ba cch khc nhau)

Cch I
Cch II
Ghi ph ln knh nh
(Spectrograph)
Quan st trc tip

nh tnh v nh lng
(Spectroscop)
Knh nh cha ph mu p.t.
nh gi nh tnh v
bn nh lng
(Spectroprojector)
nh gi nh tnh, nh lng
(theo hai cch)
r
o en trc tip
bng vi quang k
Cch III
My t ghi I ca
vch ln bng giy
Thu, phn li, ghi trc tip ph mu p.t.

(Spectrometer, mt hay nhiu knh)
Chn, khuch i tn hiu, b chnh
My tnh (Microcomputer) x l kt qu
Hin s" kt qu
In kt qu
T ghi cng
Hnh 1.3
S nguyn l ca qu trnh phn tch AES
Hnh 1.4
Vng nng phn tch ca cc phng php ph
13
12
i tng ca phng php phn tch ph pht x

Bn cnh mc ch nghin cu vt l quang ph nguyn t, php o ph pht x nguyn t l mt
phng php phn tch vt l da trn tnh cht pht x ca nguyn t trng thi hi xc nh thnh
phn ha hc ca cc nguyn t, cc cht trong mu phn tch. V vy n c tn phn tch quang ph ha
hc. Phng php ny c s dng phn tch nh tnh v nh lng cc nguyn t ha hc, ch yu
l cc kim loi trong mi i tng mu khc nhau, nh a cht, ha hc, luyn kim, ha du, nng
nghip, thc phm, y dc, mi trng... thuc cc loi mu rn, mu dung dch, mu bt, mu qung, mu
kh. Tuy phn tch nhiu i tng, nhng thc cht l xc nh cc kim loi l chnh, ngha l cc
nguyn t c ph pht x nhy, khi c kch thch bng mt ngun nng lng thch hp; sau l mt
vi kim nh Si, P, C. V vy, i tng chnh ca phng php phn tch da theo php o ph
pht x ca nguyn t l cc kim loi nng nh trong cc loi mu khc nhau. Vi i tng
kim th phng php ny c nhiu nhc im v hn ch v nhy, cng nh nhng trang b thu, ghi
ph ca chng, v ph ca hu ht cc kim li nm ngoi vng t ngoi v kh kin, ngha l phi c
thm nhng trang b phc tp mi c th phn tch c cc kim.
Cc u im v nhc im
Phng php phn tch quang ph pht x nguyn t s d c pht trin rt nhanh v c s
dng trong nhiu lnh vc ca khoa hc, k thut cng nghip, nng nghip v i sng v n c nhng u
im rt c bn:
Phng php ny c nhy rt cao. Bng phng php ny nhiu nguyn t c th c xc nh
t n nhy t n.103 n n.104 %. Nhng vi nhng trang b hin i v vi nhng ngun kch thch
ph mi (ICP) ngi ta c th t n nhy t n.10 - 5 n n.10- 6 % i. Vi nhiu nguyn t m khng
cn phi lm giu mu phn tch (bng 1). V th n l phng php kim tra, nh gi tinh khit ca
nhiu ha cht v nguyn liu tinh khit cao, phn tch lng vt cc kim loi nng c hi trong i tng
thc phm, nc gii kht, mi trng. Trong khi vi nhng i tng ny th phng php ha hc
khng th no t c.
Phng php ny gip chng ta c th tin hnh phn tch ng thi nhiu nguyn t trong mt
mu, m khng cn tch ring chng ra khi nhau. Mt khc, li khng tn nhiu thi gian, c bit l phn
tch nh tnh v bn nh lng.
Vi nhng tin b ca k thut hin nay v vi nhng trang b hin nay t c, th phng
php phn tch theo ph pht x nguyn t l mt php o chnh xc tng i cao. Trong nhiu trng
hp, vi nng nh (c ppm) m sai s ca php o l di 10%. Tt nhin vi nhng trang b v my
mc c in th sai s c th ln hn. Song thc t n b nhng trang b hin i y li.
14
Phng php phn tch theo ph pht x l mt phng php phn tch tiu tn t mu, ch cn t 1
n vi chc miligam mu l . c bit l k thut ph pht x.
Phng php phn tch ny c th kim tra c ng nht v thnh phn ca vt mu nhng
v tr (ch) khc nhau. V th cng c ng dng kim tra ng nht ca b mt vt liu.
Trong nhiu trng hp, ph ca mu nghin cu thng c ghi li trn phim nh, knh nh hay
trn bng giy. N l nhng ti liu lu tr v khi cn thit c th nh gi hay xem xt li m khng cn
phi c mu phn tch.
Bn cnh nhng u im nu, phng php ny cng c mt s nhc im v hn
nht nh. Trc
ht
phi
ni nl: Phng php ny
ch
ch
cho chng ta
bit c thnh phn nguyn t ca mu phn tch, m khng ch ra c trng thi lin kt ca n trong
mu. chnh xc ca php phn tch ph thuc vo nng chnh xc
phn
ca dy muu v cc
ktqu nh lng u
ca
phi
thnh
da
theo cc ng chun ca cc dy mu u c ch to sn trc.

Mc du c mt s nhc im v hn ch, nhng phng php phn tch quang ph pht x
nguyn t ngy cng c pht trin v ng dng rng ri trong nhiu lnh vc khc nhau xc nh
lng vt cc nguyn t trong cc i tng mu khc nhau. l mt phng php phn tch nhanh, c
chnh xc bo m v nhy kh cao, c bit thch hp cho phn tch t him, cc loi nc, khng
kh, v.v.
1.6 Kh nng v phm vi ng dng

Phng php phn tch quang ph pht x nguyn t ngy nay gi vai tr quan trng trong ha hc
phn tch. Cng vi s pht trin mnh m ca cc ngnh khoa hc k thut, c bit l vt l v ha hc,
s pht trin ca k thut o v ghi tn hiu, lm tng kh nng ng dng to ln ca n. Bng phng
php ny ngi ta c th xc nh nh tnh, bn nh lng v nh lng c hn nm chc kim loi v
gn mt chc nguyn t kim trong cc i tng mu khc nhau (v c v hu c). Phng php phn
tch ny tr thnh cng c phn tch nguyn t c lc ch nhiu lnh vc, nht l sau khi c ngun kch
thch ICP.
Phn tch quang ph pht x trong ngnh ha v cng nghip ha hc. N l cng c cc
nh ha hc xc nh thnh phn nh tnh v nh lng ca nhiu cht, kim tra tinh khit ca cc ha
phm, nguyn liu v nh gi cht lng ca chng. N cng l mt phng php xc nh cc ng
v phng x v nghin cu cu trc nguyn t.
Phn tch quang ph pht x nguyn t trong a cht. Ngay t khi mi ra i, phng php
ny c cc nh a cht s dng phn tch cc mu qung phc v cho cng vic thm d a cht v
tm ti nguyn khong sn. V th ngnh a cht ca tt c cc nc u c phng phn tch quang ph
pht x rt hin i v hon chnh.
15
Phn tch quang ph pht x trong luyn kim. Luyn kim cng l mt ngnh s dng phng
php phn tch quang ph pht x u tin vo mc ch ca mnh trc c ngnh ha. Chnh tnh cht
nhanh chng v nhy ca phng php ny l mt iu rt cn thit i vi ngnh luyn kim. N c th
l cng c gip cc nh luyn kim xc nh ngay c thnh phn ca cc cht ang nng chy trong l
luyn kim; qua m h c th iu chnh nguyn liu a vo ch to c nhng hp kim c thnh
phn mong mun, kim tra thnh phn, kim tra nguyn liu.
Phn tch quang ph pht x trong tiu ch un hc. Trc y con ngi tng rng kh c th
hiu bit c thnh phn ha hc ca cc hnh tinh xung quanh tri t chng ta. Nhng phng php
phn tch quang ph pht x ra i m rng tm vi cho con ngi. Bng phng php ph pht x v
kt hp vi mt s knh thin vn, cc nh thin vn c th quan st c thnh phn ca cc nguyn t
ha hc ca cc hnh tinh khc nh mt trng, cc v sao. Chnh nhng kt qu phn tch thnh phn ca
cc mu t do v tinh ly t mt trng v ni ln ngha ca php o ph pht x trong lnh vc nghin
cu thin vn. V nhng kt qu phn tch thc t cc mu l rt ph hp vi nhng s liu thu c trc
y qua phn tch tia sng t mt trng bng h thng my quang ph v knh thin vn.
Phn tch quang ph pht x trong nng nghip, y v sinh hc. y l nhng ngnh khoa hc
s dng phng php ny cm li nhiu kt qu rc r, c bit l trong vic nghin cu th nhng,
nghin cu cc nguyn t vi lng trong t trng, trong cy trng, trong phn bn ca nng nghip, hay
nghin cu thnh phn thc n phc v chn nui, phn tch nguyn t vi lng trong mu, serum, nc
tiu, phc v cha bnh.
Phn tch quang ph trong cc lnh vc khc. Ngoi nhng lnh vc nu, phng php phn
tch quang ph pht x nguyn t cn c mt s ngnh khc s dng nh l mt cng c phn tch. V
d nh trong ngnh dc kim tra mt s kim loi c hi trong cc dc phm (Pb, Cu, Zn, Hg,...).
Ngnh nghin cu c s, cng an, to n, ngoi thng, cng l nhng ni s dng phng php phn
tch quang ph trong cc lnh vc nghin cu v nng php o ph nguyn t ln ngang tm ca thi
i.
Hnh 1.5
S phn chia cc loi ph theo di sng
16
Chng 2
S KCH THCH PH PHT X NGUYN T
Yu cu v nhim v ca ngun kch thch

Trong phn tch quang ph pht x nguyn t, ngun sng c gi l ngun kch thch ph v c
mt vai tr ht sc quan trng. V nh ngun nng lng kch thch ngi ta c th chuyn vt liu mu
phn tch thnh trng thi hi ca cc nguyn t v kch thch m hi pht sng (pht x), ngha l ngun
nng lng nh hng trc tip n kt qu ca php phn tch. V vy ngun nng lng mun dng
c vo mc ch phn tch quang ph pht x nguyn t cn phi thc hin c hai nhim v sau y:
Trc ht ngun nng lng phi ha hi, nguyn t ha v chuyn c hon ton cc
nguyn liu mu phn tch vo vng phng in (plasma). C nh th thnh phn ca m hi trong
plasma mi ng nht vi thnh phn ca vt mu. ng thi ngun nng lng phi c nng lng
ln (nhit ) c th kch thch c tt nht cc nguyn t ca nguyn t cn phn tch i n pht
x ra ph ca n.
Song nh th vn cha hon ton . V mt phng php phn tch ch c gi tr khi n c
nhy v lp li cao. Chnh v th, ngoi hai nhim v trn mt ngun sng mun dng c lm
ngun kch thch ph pht x n cn cn phi tha mn mt s yu cu nht nh sau y:
Trc ht ngun sng phi m bo cho php phn tch c nhy cao v cng ca vch ph
phi nhy vi s bin thin nng ca nguyn t phn tch; nhng li khng nhy vi s dao ng ca
iu kin lm vic.
Ngun nng lng phi n nh v bn vng theo thi gian, m bo cho phng php phn tch
c lp li v n nh cao. Ngha l cc thng s ca ngun sng chn nht thit phi duy tr v lp
li c.
Ngun nng lng phi khng a thm ph ph vo lm ln vi ph ca mu nghin cu. Nu
khng s lm kh khn thm cng vic nh gi nh tnh v nh lng v c khi lm sai lc c kt qu
phn tch.
Ngun kch thch phi c s cu to khng qu phc tp; nhng li c kh nng thay i c
nhiu thng s, c th chn c nhng iu kin ph hp theo tng i tng phn tch hay tng
nguyn t.
Yu cu cui cng l ngun nng lng kch thch phi lm tiu hao t mu phn tch v trong mt
s trng hp phi khng lm h hi mu phn tch, nh trong
17
kim tra thnh phm.

Trn y l nhng yu cu chung, nu ngun sng tha mn c y cc yu cu l mt iu
rt l tng. Song trong thc t khng c c iu kin l tng nh th. V vy, mi ngi lm phn tch
quang ph pht x cn phi hiu bit tng tn v ty theo tng trng hp c th m xem yu cu no cn
c ch nghim ngt trc ht v yu cu no c th chnm chc c.
Cc loi ngun kch thch ph pht x

Do nhng yu cu nu trn, nn ch c mt vi loi ngun nng lng c dng lm ngun
kch thch cho phng php phn tch quang ph pht x. l: Ngn la n kh;
dng xoay chiu v
mt chiu;
Hquang
in
Tia la in; Tia
lc; Plasma cao tn cm ng (ICP); tia X.

Trong cc loi ngun nng lng ny, ngn la n kh, h quang v tia la in c dng t
lu, nhng c nhy khng cao (ngun sng c in). Tia lc v ICP l nhng ngun nng lng cho
nhy cao. Nhng tia lc t c dng. V c c tia lc ph hp cho mc ch phn tch phi c
nhng trang b phc tp, tn km. Ring ICP l ngun nng lng hin ang c ng dng ph bin v c
nhiu u vit. N l ngun sng mi c pht trin trong vng hn chc nm li y. Li khng t nh
ngun lc. V nhy ca cc ngun nng lng ny chng ta c th xem trong hnh 1.4 v bng ph lc
A.
Ngn la n kh
Cu to v c im ngn la n kh
Ngn la n kh l ngun nng lng u tin c dng trong phn tch quang ph pht x
nguyn t, ngay t khi phng php ny ra i. Bunsen v Kirschoff l nhng ngi u tin dng ngun
sng ny phn tch cc kim loi kim v kim th. Nhng do s n gin, n nh, nhy tng i v
r tin, nn ngy nay n vn c s dng ph bin.
c im. Ngn la n kh c nhit khng cao (1700 - 3200 0C), c cu to n gin, nhng n
nh v d lp li c cc iu kin lm vic. Do c nhit thp, nn ngn la n kh ch kch thch
c cc kim loi kim v kim th. V ng vi loi ngun sng ny ngi ta c mt phng php phn
tch ring. l phng php phn tch quang ph ngn la (Flame Spectrophotometry). Song v
bn cht n vn l ph pht x ca nguyn t trong ngn la. Cc cht kh t to ra ngn la ca n
kh thng l mt hn hp ca hai kh (1 kh oxy ha v 1 kh nhin liu) c trn vi nhau theo mt t l
nht nh. Bn cht v thnh phn ca hn hp kh quyt nh nhit ca ngn la v hnh dng
cu to ca ngn la. Di y l mt vi hn hp kh c s dng to ra ngn la trong php o

ph pht x:
18
2.2.1.2 n nguyn t ho mu (burner head)

L
Bngb2.1 phn
chy
hn
hp
kh
to ra ngn la. Tuy c nhiu kiu n khc
Nhit ca mt s loi n kh
nhau,
nhng u c nguyn tc cu to
STT 2.4 v 2.5).
Loilhnhhpthng
kh t
ging nhau (hnh
Nhit (oC)
nguyn t 1 ha mu. Song bt k mt loi

Axetylen v oxy
n no mun dng c cho php phn
2400-3100
oxy cu nu
tch quang 2 ph, ngoi Butan
nhngvyu
2000-2550
(mc
1)
n cn phi m bo trn u hn
3
Kh t v oxy
hp kh trc khi t v ngn la phi chy
2200-2500
ngoi ming
4 n.
Hydro v oxy
2100-2300
Hnh 2.4. 5
Axetylen v khng kh
2000-2450
n v h thng NTH mu ca hng

Philips
Cu to. V hnh dng cu to v s phn b nhit ca ngn la, n kh gm
(1) n nguyn t ha mu; (2) Mng bo him; (3) ng thi phn mu tha; (4) ng dn
ba phn nh sau (hnh 2.3 v 2.4):
cht oxy ha; (S) ng dn mu vo bung aerosol ha; ( 6 ) ng dn cht chy C2 H2; (7) Vin bi to
Phn mt (a). Phn trong cng st ming n l phn ti (a). Trong phn ny
bi aersol.
cht t c trn v nung nng chun b t chy phn hai (b). Nhit trong
Hthp
nguyn
t700-1200
ha mu 0C
bao
phn ny
(di
). gm:
+ Bung
htca
mu
v to
Phn hai
(b) l li
ngn
la.th si kh (1)
Trong +phn
ny xy
ra mu
cc (2)
phn ng t chy
n nguyn
t ha
cht kh. N khng mu hay c mu xanh
(2)
nht v nhit l cao nht. Chnh nh b l

ch c nhit cao nht ca ngn la. Nu
t
bng
hn
hp
kh
axtylen
oxy
hay
khng kh nn th nhit ca ngn la c

cung cp nh phn ng:
2C2 H2 + 2O2 = 4CO + 2H2 + Q
Phn th ba (c) l v ca ngn la.
Trong phn ny thng xy ra cc phn ng
th cp, c mu vng v nhit thp. N to
Hnh
2.5 v v ca ngn la.
thnh ui
H thng nbiulai theo k thut pneumatic
K: Kh mang (oxy ha); S: ng dn mu; F: Kh chy; Q: Cnh qut quay u; G: Mng bo
him; A:
dnbthnhit
aetosol
ln n
t ha.
Dong
s phn
ca
ngnnguyn
la nh
vy, nn kh phn tch phi a mu vo vng tnm c
trong
latrong vng ny cc qu trnh s n nh, v hiu sut kch
nhit Qu
caotrnh
nht. kch
lthch
vngph
b ca
ngnngn
la v
thch ph
s cao
nht.
Trong
phn
tch quang ph pht x, nu dng ngn la lm ngun kch thch th mu phn tch phi
chun b dng dung dch. Sau nh mt h thng phun
20
19
(Nebulizer system) a dung dch ny vo ngn la di dng th sng m (th si kh aersol) cng vi hn hp kh t. Khi vo ngn la, di tc dng ca nhit , trc ht
dung mi bay hi, li cc ht bt mu mn ca cc cht phn tch, ri n c t nng v
chuyn thnh hi ca nguyn t v phn t. Trong ngn la cc phn t hi ny chuyn ng,
va chm vo nhau, trao i nng lng cho nhau,... Kt qu ca cc qu trnh lm cc phn
t b phn li thnh nguyn t, b Ion ha v b kch thch. Nh vy trong ngn la tn ti c
nguyn t t do, phn t, Ion, nhm phn t v cc in t. Trong tp hp ch yu ch cc
nguyn t t do b kch thch v pht x. V th ph pht x ngn la l ph ca nguyn t
trung ha. Nguyn nhn gy ra s kch thch ph y l s va chm ca cc nguyn t vi
cc in t c ng nng ln trong ngn la. V th nhit ngn la cng cao th cc in t
c ng nng cng ln. V th n l s kch thch nhit. Do c ch ca qu trnh kch
thch trong ngn la l:
Trc ht l dung mi bay hi, li cc ht mu dng bt. Tip theo l bt mu b
nung nng, nng chy. Sau l cc qu trnh nhit ha ca cht mu xy ra theo tnh cht
ca n, v gm c.
Hai qu trnh chnh:
Nu
Eh < Ent th
mu
s ha hi, nguyn t ha to
ra cc nguyn
t t do,
chng b kch thch v pht x ^ c ph pht x (AES).

Men Xm(r).Th. ^ Men Xm(k) ^ mMe(k) + nX(k)
Me(k) + E ^ Me(k)* ^ Me O + n(Hv)
Nng lng K Chm tia pht x
C ch ny (c ch 1) cho nhy v n nh cao ca s pht x. Cc hp cht mui
halogen (tr F), axetat, mt s nitrat, sunphat... ca kim loi thng theo c ch ny.
Nu Eh > Ent th mu s b nguyn t ha trc, sau ha hi thnh nguyn t, ri b
kch thch ph ^ sinh ra ph pht x (AES).
MenXm(r) ^ Mn(r) + Xm(r) ^ mMe(k) + nX(k)
Me(k) + E ^ Me(k)* ^ Me O + n(Hv)
C ch ny (c ch 2) cho nhy v n nh km so vi c ch 1 ca s pht x.
Cc hp cht mui SIO 2-3, PO3-4, F", mt s nitrat, sunphat,.. ca kim loi thng theo
c ch ny.
Do c im ca 2 c ch chnh , nn trong phn tch ngi ta thng to iu
21
kin s kch thch ph xy ra theo c ch 1 c li. iu gii thch ti sao ngi ta hay dng cc mui
halogen, v axetat ca kim loi kim lm nn, hay cht ph gia cho mu phn tch.
Qu trnh ph
Trong ngn la thng c cc qu trnh ph km theo hai qu trnh chnh, cc qu trnh ny ty iu
kin ca ngn la m xut hin trong mc khc nhau, v n u khng c li, nn cn c loi tr
trong phn tch. Cc qu trnh l:
To ra cc hp cht bn nhit, ch yu l cc monoxit (dng MeO).
S pht x ph nn lin tc ca ht rn v electron b nung nng.
Ni chung, cc qu trnh ny u khng c li. Ngi ta phi tm bin php loi tr. V d:
+ hn ch s hnh thnh hp cht bn nhit kiu Me O, ngi ta thm vo mu mui Clorua ca
kim loi kim (nh KCI, CsCL) lm nn, kch thch ph theo c ch
+ Hay loi tr s Ion ha ca nguyn t phn tch, ngi ta thm vo mu cht ph gia l mui
halogen kim loi kim c th Ion ha thp hn th Ion ha ca nguyn t phn tch. Nh th nguyn t
phn tch s khng b Ion ha na.
So vi cc loi ngun kch thch khc, ngn la l ngun kch thch n gin, nhy trung bnh
(0,1 - 10p,g) v tng i n nh. Nhng cng ca vch ph cng b nh hng bi mt s yu t
nht nh, nh:
+ Trc ht l dng lin kt ca cc nguyn t trong cht mu.
+ Th hai l nh hng ca cc gc axit. Ni chung, cc axit d bay hi th nh hng ny l nh.
+ Th ba l cht nn hay thnh phn ca dung dch mu, v vy dung dch phn tch v dung dch
mu chun u phi c cng thnh phn vt l v ha hc, nht l cht nn phi cng loi.
+ nh hng th t l cc phn ng ha hc xy ra trong ngn la. c bit l nh hng ca cc
phn ng to ra cc hp cht bn nhit. Cc hp cht ny thng lm gim cng ca vch ph, ngha
l lm gim nhy ca phng php phn tch. l khi qut chung, tt nhin cc yu t trn khng
phi bao gi cng xut hin ng thi v tc dng nh nhau trong mi trng hp, m ty tng trng hp
yu t no l ni bt v cn c ch . Song mt iu cn nh l nhit ngn la l yu t quan trng
nht, n quyt nh cc qu trnh xy ra trong khi kch thch ph.
22
2.2.2
Hph
quang
inln (R >> Ri) hn ch s thay i cng dng in trong mch v
bin tr
R2 tht
2
gi cho
him
quang
c
v n
tnhnh.
cht
Cuquang
to v
H
l hot
ngunng
kchca
thchhcquang
nng lng trung bnh v cng l ngun kch thch vn nng. N c
kh nng
mupht
dn h
inquang
v khng
in.nhng
Ty thuc
vo cctc
thng
(A,tt
C, c
R) cc
ca
Tuykch
c thch
nhiuc
loic
my
khcdn
nhau,
v nguyn
custo,
my
vu
loi gm
in cc
chnchnh.
m h quang c nhit t 3 5 00 - 60 00 0C Vi nhit ny
my pht
phthhquang
quang
hai ta
phn
nhiu nguyn
cc nguyn
liuquang
mu khc
nhauchnh),
c th c
hi, nguyn
t ha
kch lng
thch ph
Phn 1tltmch
pht h
(mch
n cha
nhim
v cung
cpvnng
pht
x. Nhit
ca
h quang
ph
thuc
rt m
nhiuhi
vo
bnicht
liuh
lm
in cc.
th
ha hi,
nguyn
t ha
mu v
kch
thch
nca
phtnguyn
x. Nu
quang
mt V
chiu
trong
iu kin
nhau,
h mt
quang
in (hnh
cc than
(graphite)
cao
nht
(bngth
2.2).
th mt
l mch
canh
dng
in
chiu
2.6).
Nu lchnhit
quang
xoay
chiu,
Cng
l dng
dng
in trong
mch h quang l yu t quyt nh nhit ca h quang.
in xoay
chiu.
H
quang
ngunch
kchhuy
thch
cho iu
nhykhin),
tng i
v trong
h quang
mu phn
chot
ha
Phn
2 llmch
(mch
c cao,
nhim
v ch
huy phn
mchtch
chnh
hi
tng
d dng
hns
trong
cc loi
ngun
c bit
l nht
h quang
mt
ng
theoi
nhng
thng
c
chn
chonng
mtlng
mc khc,
ch phn
tch
nh.dng
Theo
schiu.

Nhng cng do tnh cht ny m php phn tch dng h quang c n nh v lp li km ngn la
hnh 2.6, nu cng tc K c ng v tr AA, ta c h quang dng xoay chiu. Cn khi v
v tia in. y h quang dng xoay chiu cho kt qu n nh hn h quang dng mt chiu, v th h
tr BB' ta c h quang dng mt chiu. S hot ng ca h quang din ra nh s (s hnh
quang dng xoay chiu c s dng nhiu hn.
2.6):
Bng 2.2
Khi ng cng tc K', ngha l a in vo my, qua h thng bin tr R; ta chn c
Th
Ion vic
ha v
hvo
quang
th lm
phnhit
hp
a
binca
thmt
Tr 1 s
kim
tngloi
th. Khi th hai u cun th cp ca
bin th ny t n hng ngn vn (2000-7000V). Hai u cun ny c ni vi cun cm
Li, t in C1 v khong n ph E. Lc t C 1 c tch in v khi t n th Vf chn
th c mt tia in c nh qua khong E, nh th lp tc trn mch dao ng L 1c1 xut
hin mt dao ng cao tn. Do mch dao ng L 2C2 cng ghp vi mch dao ng L lC1, nn
trn mch
L2t
C2lm
cng
xut
mtha
daoca
ng
cao tn Dng
cm ng
vng
ca L 2
Nguyn
in
cc hin
Th Ion
nguyn
Nhit sca
h quang
in nh
h th. Nhng
l ln hn nhiu L1s nn th
trn hai ct ca t C 2 cng
s(A)
ln hn C 1. Th ny(oli
t (eV)
C) xut hin
quang
10
tc khc khi cCtia in nh E v11,30
iu khin s phng in
qua khong F ca6000
hai in cc
h quang. NhZn
th mt chu k phng9,40
in th nht c thc
li tip din
10 hin v kt thc, ri
5200
n chu k phng in th hai, th ba,... v c th din ra cho n khi no ta ngt cng tc K',
Fe
7,80
10
4800
Cr
6,90
10
4400
Al
5,67
10
4000
tc l ngng s phng in ca h quang.
H quang l ngun kch thch c s mch tng i n gin, nhng li c nhiu thng s c th
iu chnh c chn c mt nhit tng i ph hp cho php phn tch mi cht.
H quang l s phng in gia hai in cc c th thp (di 260V) v dng cao (t
- 20A). Th
v dng ca mch h quang c lin h vi nhau theo cng thc:
,B
_ U
U _ A + v I _ --------
Im
R+R
m
Trong A v B l cc hng s, R 1 l in tr plasma h quang. Cng thc ny gii thch ti sao h

quang km bn vng. V th phi a vo mch h quang mt
Hnh 2.6
S nguyn tc cu to ca my pht h quang
24
23
Khi h quang lm vic, in cc F s c t nng v di tc dng ca in trng cc in t

bt ra khi b mt in cc nm, chng c gia tc v chuyn ng v cc dng. Nhng in t ny c
ng nng rt ln, v khi chuyn ng trong plasma gia hai in cc, cc in t va chm vo cc phn t
khc (nguyn t, Ion, phn t...) trong plasma F, n truyn nng lng cho nhng phn t . Khi trong
plasma c phn t b Ion ha, b phn li v b kch thch. Kt qu li c thm in t t do na cng vi
mt s nguyn t, Ion, phn t b kch thch. Nh vy chnh cc phn t mang in tch dng v nm duy
tr dng in qua ct kh ca plasma. Gia hai in cc F cc phn t b kch thch s sinh ra ph pht
x ca n. Trong h quang mt chiu in t lun lun p vo in cc dng, nn in cc dng nng
hn in cc nm. Cn ngc li, trong h quang dng xoay chiu, hai in cc li c t nng
nh nhau.
H quang dng mt chiu thng xut hin s st th hai u ca in cc. Hiu ng ny xut
hin rt r rng trong thi gian u ca s phng in v h quang c dng thp (di 5A). Nhng sau
c nng lng ca ngun kch thch b vo th s st th s gim i. Nguyn nhn ca s st th
ny l do s xut hin lp in kp hai u ca in cc v lp in kp ny c t trng ngc vi t
trng chnh ca h quang. Vi h quang xoay chiu, do dng in lun lun i chiu, nn s st th
xut hin khng r rng v rt t c tc dng. chnh l l do gii thch ti sao s kch thch ph pht x
bng h quang dng in xoay chiu lun lun n nh hn s kch ph trong h quang dng in mt
chiu.
Nhit ca plasma h quang

Yu t th nht, yu t chnh quyt nh nhit ca h quang l cng dng in trong
mch h quang chnh. Trong mt khong nht nh ca nhit , khi tng cng ca dng in th
nhit ca h quang cng tng theo. Ngha l ta c:
T = k. I (2.2)
Trong k l h s t l, T l nhit ca h quang ( OC). Nhng n mt gi tr nht nh ca
cng dng in I0, th nhit h quang tng rt chm theo s tng nhit (hnh 2.7). Gi tr I0 c
gi l dng in gii hn ca h quang. Nhng cng dng in trong mch h quang thay i tng
i mnh. V ct kh ca plasma lun thay i c v di v b rng, do im phng in trn b mt
in cc lun lun di ng. l nhc im ca h quang. Do ngi ta phi dng in cc i c
hnh nn ct.
V vy, mun cho cng dng in I trong mch h quang n nh (t thay i) ngi ta phi
mc trong mch h quang h in tr R 2 tht ln, s thay i ca R1 do ct kh gy ra t b nh hng
n I. V th trong cc my pht h quang ngi ta thng lm mt h in tr ni R 2 rt ln v cng
dng in c tnh theo cng thc:
25
I=+R
(2.3)
trong :
R1: in tr ct kh ca plasma gia hai in cc.
R2: in tr ni ca my pht h quang.
U: Th ca ngun in ca my pht t ln hai u in cc F.
Yu t th hai quyt nh nhit ca h quang l bn cht ca nguyn liu
lm in cc. Ni chung, nguyn liu no kh bay hi v cu to t nhng nguyn t

ha hc c th Ion ha cng cao, th h quang dng in cc nguyn t s cho nhit
cng cao. V th h quang in cc than (graphite) s c nhit cao nht so vi
cc h quang in nguyn liu khc trong cng mt iu kin dng in th nghim
(bng 2 .2 ).
Yu t th ba l th Ion ha ca cc cht c trong mu phn tch, ch yu l
cht nn v nhng cht c nng ln. Ni chung, nguyn t no (nht l cht nn ca
mu) c th Ion ha cng nh th cng lm gim nhiu nhit ca h quang, ngha l
cc kim loi kim c tc dng mnh nht, sau n cc kim loi kim th. Chnh v
th th ngi ta thng thm cc mui halogen ca kim loi kim vo mu gp
phn iu chnh nhit ca plasma ca h quang cho s kch thch ph ca cc
nguyn t phn tch. Bn cnh th Ion ha, th nng ca cc nguyn t cng c nh
hng n nhit ca h quang, c bit l cc nguyn t c th Ion ha thp s lm
gim nhit ca h quang cng nhiu, khi nng ca n trong plasma cng ln.
Trong
quang
plasma
thng
lun
ca
lun
xy
ra
cc phn ng ha hc v vt l.
l qu trnh phn li, Ion ha,
t hp phn t v s kch thch
ph.
Nhng
thng
ng
nht
xc
quang
trnh
nhit
hi
trong
ng
nh
ny
qu
cng
nh
trnh
cc
hc
plasma
s
qu
mt
vi
ca
nhit
nhng
my
chn.
thng
pht
Nhit
m bo cho plasma c mt
p lc in t xc nh duy
tr s kch thch ph.
26
S kch thch ph trong plasma h quang in
Trong plasma ca h quang, s kch thch ph pht x c th xy ra theo cc qu trnh

sau:
Nu l mu dung dch, th trc ht l dung mi bay hi,
licc ht bt
mu. Ri cc cht (c mu bt v b ca mu dung dch cn
li),bt mu b nung
C th l cc ht mu s bay hi hay chuyn khi vo plasma gia 2 in cc. Ti y s xy
ra cc qu trnh chnh v ph khc nhau, ty thuc vo thnh phn v bn cht ca cht mu.
Nu mu l dng bt c nhi vo trong l in cc mang th c cc qu trnh trong
in cc mang mu l:
+ S nung nng v nng chy,
+ S chuyn ng nhit khuch tn v i lu ca cc ht trong l in cc,
+ Cc phn ng ha hc phn hy ca cc cht mu km bn nhit,
+ S vn chuyn ca cc ht mu cha ha hi vo plasm.
Bn cht v thnh phn ca mu trong l in cc v nhit ca in cc l yu t
quyt nh s din bin ca cc qu trnh trn.
Sau l cc qu trnh trong plasma. Gm c 2 qu trnh chnh sinh ra ph pht x
nguyn t (AES) v mt s qu trnh ph nh sau:
A- Hai qu trnh chnh:
Nu Eh < Ent th mu s ha hi, nguyn t ha to ra cc nguyn t t do, chng b kch
thch v pht x ^ c ph pht x (AES)
Me(k) + E ^ Me(k)* ^ Me O + n(hv)
Nng lng K.Th.
Chm tia pht x

(tr F), axetat, mt s nitrat, sunphat,... ca kim loi thng theo c ch ny.
Nu Eh > Ent th phn t ca cht mu s b nguyn t ha trc, sau ha hi thnh
Men Xm(r) ^ Men (r) + Xm(r) ^ mMe(k) + nX(k)
Me(k) + E ^ Me(k)* ^ Me O + n(hv)
Nng lng K.Th.
Chm tia pht x
C ch 2 ny cho nhy v n nh km so vi c ch 1 ca s pht x. Cc
27
hp cht mui SiO3, PO4, F, mt s nitrat, sunphat... kim loi thng theo c ch ny.
Do c im ca 2 c ch chnh , nn trong phn tch ngi ta thng to diu kin s kch

thch ph xy ra theo c ch 1 c li. iu gii thch ti sao ngi ta hay dng cc mui halogen, v
xetat ca kim loi kim lm nn, hay cht ph gia cho mu phn tch v mu chun, bin i nn mu
gc sang nn nhn to tt hn v li cn loi tr c cc yu t nh hng, ng thi c khi cn tng
c c nhy ln hng chc ln.
B- Cc qu trnh ph:
Trong plasma ca h quang thng c:
S hnh thnh hp cht bn nhit, ch yu l cc monoxit (dng MeO).
Bn cht ca cht mu, thnh phn ca mu, cht ph gia trong l in cc v nhit ca in cc
l yu t quyt nh din bin ca cc qu trnh trn.
Ni chung cc qu trnh ny u khng c li, ngi ta tm bin php loi tr.
V d:
+ hn ch s hnh thnh hp cht bn nhit kiu MeO, ngi ta thm vo mu mui Clorua ca kim loi
kim (nh KCI, CsCl,) lm nn, kch thch ph theo c ch
halogen kim
loi kim
c thIon ha thp
hn th
gia mui
Ion ha ca
nguyn t phn tch. Nh th nguyn t phn tch s khng b Ion ha na.
Cc loi my pht h quang

My pht
v
h quang c
rt
nhiu, c
nhiu hng cung cp, song xt
c ch
mch in ca mch h quang chnh, th c th chia thnh hai loi:

+ My pht h quang dng mt chiu.
+ My pht h quang dng xoay chiu.
Tuy l hai loi, nhng u c nguyn tc cu to nh nhau (hnh 2.6). Trong mi loi h quang li
c nhiu ch khc nhau. Thng thng c mt ch lin tc v nhiu ch gin on. Chnh v th
m chng ta c th chn c nhng gi tr nng lng khc nhau cho tng mc ch phn tch c th.
Tia la in
c im v tnh cht
Tia la in l ngun kch thch ph c nng lng tng i cao. Ty theo cc thng s ca my
pht tia la in (C, L, R, T) chn, ta c th t c nhit
28
tnm plasma tia la in t 4000 - 6000 OC. V th tia la in c gi l ngun kch thch
cng (giu nng lng). Nn ph pht x ca tia la in ch yu l ph ca cc Ion bc 1 ca
cc kim loi.
Tia la in l ngun kch thch tng i n nh v c lp li cao. Nhng v
nhy li km h quang in. Do thi gian ghi ph cn phi di hn h quang.
V bn cht ca s phng in, tia in l s phng in gia hai in cc c th hiu
rt cao (10.000 - 20.000kV) v dng in rt thp (<1A). N l s phng in gin on t 50
- 300 chu k trong mt giy, ty thuc vo cc thng s ca my pht tia la in c
chn. Do in cc khng b t nng . Do c im ny m tia la in l ngun kch
thch ph hp i vi php phn tch cc mu thp, hp kim v dung dch, nhng li khng
ph hp cho vic phn tch cc mu qung, t v bt v khng ha hi tt cc mu loi
ny.
Trong tia la in qu trnh chuyn vt cht mu t in cc vo plasma l gin on
theo tng chu k phng in gia hai in cc.
Nhit ca plasma tia la in
Yu t quyt nh nhit plasma ca tia la in khng phi l cng dng in
nh trong h quang m l mt dng lc xy ra s phng tia in gia hai in cc. Nhng
mt dng in li thay i theo s phng in. N t c gi tr ln nht ti lc bt u
c tia in xy ra gia hai in cc v sau li gim v l nh nht ti thi im ngh nh
in. Qu trnh tip din mt cch tun hon theo nhng thng s ca my pht tia la in
c chn. Ni chung, trong mt gii hn nht nh, nhit plasma ca tia la in ph
thuc vo mt dng in (hnh 2.8), ngha l n mt gi tr mt dng j 0 no th nhit
ca tia in khng tng theo mt ca mt dng in na. Song mt dng in li
ph thuc vo ba thng s chnh ca my pht gia la in Vf, C, L (th, in dung, t
cm). Cho nn nhit ca tia la in cng ph thuc vo cc thng s . Ni chung n t
l thun vi
f v C v t l nghch vi t cm L. Trong ba thng s th Vf l yu t quan trong nht
v Vf li ph thuc vo:
Khong cch gia hai in cc.
Trng thi b mt ca in cc chnh v ph.
Cc thng s ca mch in nh V, C, L, I, S.
29
V vy, mun m bo cho qu trnh

phng in n nh, th phi gi cc iu
kin lm vic tht n nh. Nhng cng
khng nn chn cc thng s mt
dng t gi tr gii hn j0 v mt dng
in ny s phng in km bn vng v
khng n nh, tc l lm cho nhit ca
tia in dao ng nhiu. Mt cch gn
ng, trong plasma tia la in ta c tn s
phng in:
f = V LC 2n
I = V14CL
Cng dng in:
V mt dng:
j = hay a =
S
Vf4cTL
S
S kch thch ph trong plasma ca tia la in

Trong plasma ca tia la in s kch thch ph pht x xy ra cng tng t nh trong h quang
in. Nhng vi mu bt th s ha hi din ra rt km v khng n nh. Nhng do nhit ca plasma
cao nn s hnh thnh cc hp cht bn nhit, t gp hn trong h quang. Mt khc, tia la in dng ch
yu phn tch mu thp, hp kim (mu rn) v mu dung dch. Nn cc qu trnh xy ra ch yu ch trn
b mt in cc mang. C th l:
Nu l mu dung dch, th trc ht dung mi bay hi, li cc ht bt mu.
Ri cc
cht
(c mu
bt v b ca mu dung
dch cn li), bt mu
b nung
nng, nng chy. Sau l cc qu trnh nhit ha ca cht mu xy ra theo tnh cht ca n. C th l cc
ht mu s bay hi hay chuyn khi vo plasma gia 2 in cc. Ti s xy ra cc qu trnh chnh v
ph khc nhau, ty thuc vo thnh phn v bn cht ca cht mu.
Nu mu l dng rn, mu l chnh in cc mang, th c cc qu trnh trong in cc mang mu l:
+ S nung nng b mt v b bn ph,
+ S vn chuyn ca cc ht mu cha ha hi vo plasma,
Bn cht ca mu, thnh phn ca mu, th phng in, v nhit b mt ca
30
in cc l cc yu t quyt nh din bin ca cc qu trnh trn.

Sau l cc qu trnh trong plasma. Gm c 2 qu trnh chnh sinh ra ph pht
x nguyn t (AES) v mt s qu trnh ph nh sau:
A- Hai qu trnh chnh
A1- Khi mu l dung dch nh ln in cc
Men Xm(r) ^Men Xm(k) ^ mMe(k) + nX(k)
Me(k) + E ^ Me(k)* ^ Me O + n(hv)
C ch 1 ny cho nhy v n nh cao ca s pht x. Cc hp cht
mui
halogen (tr F), axetat, mt s nitrat, sunphat,.. ca kim loi thng theo c ch ny. Nu Eh
> Ent th phn t ca cht mu s b nguyn t ha trc, sau ha hi thnh cc nguyn t
t do, ri mi b kch thch ph ^ sinh ra ph pht x (AES).
Men Xm(r) ^Men (r) + Xm (r)^ mMe(k) + nX(k)
Me(k) + E ^ Me(k)* ^ Me O + n(hv)
cht mui SiO3, PO4, F, mt s nitrat, sunphat,... kim loi thng theo c ch ny.
Do c im ca 2 c ch chnh , nn trong phn tch ngi ta thng to iu kin
cc mui halogen v axetat ca kim loi kim lm nn, hay cht ph gia cho mu phn tch v
yu t nh hng ng thi c khi cn tng c c nhy ln hng chc ln.
A2- Khi mu l thanh kim loi lm in mang
+ Lp
cc nguyn t trn b
mt in cc, di tc dng ca lc
in trng
in mnh (v th phng in rt cao gia 2 in cc, 15- 20 kV), nn cc nguyn t b bt ra

khi mt in cc v bay vo plasma, hoc l dng hi, hay l dng ht rn. Sau c cc qu
trnh sau:
Ha hi ca ht rn:
Men) + E1 ^ Me(k)
Nguyn t b kch thch:
Me(k) + E2 ^ Me(k)*
Nguyn t b Ion ha:
Me(k) + E3 ^ Me(k)+
Ion b kch thch:
Me(k)+ + E4 ^ Me(k)+*
31
Pht x ca nguyn t:
Me(k)* ^ Me(k) + n(hv)
Pht x ca Ion:
Me(k)+* ^ Me(k) + n(hv)
Trong : n(hv) l chm tia pht x ca nguyn t hay Ion b kch thch.
Cn El, E2,.. l nng lng nhit do plasma tia in cung cp.
B- Cc qu trnh ph
Trong plasma gm c:
S hnh thnh hp cht bn nhit, ch yu l cc monoixtit (dng Me O).
ca in cc l yu t quyt nh s din bin ca cc qu trnh trn.
Song qu trnh ph trong plasma tia in khng mnh nh trong ngn la v trong h
quang, ch c s Ion ha l ng k. V th cc kim loi kim phi o theo cc vch Ion bc 1.
d vi mu dung dch:
Clorua ca kim loi kim (nh KCI, CsCL,) lm nn, kch thch ph theo c ch
Vy, loi tr s Ion ha ca nguyn t phn tch, ngi ta thm vo mu cht ph gia
mui halogen kim loi kim c th Ion ha thp hn th Ion ha ca nguyn t phn tch. Nh
th, nguyn t phn tch s khng b Ion ha na.
Cc loi my pht tia in
V nguyn tc cu to, my pht tia la in cng c hai loi: my pht tia la in c
ch huy v my pht tia la in khng ch huy. Song trong mc ch phn tch quang ph
pht x, ngi ta ch dng my pht tia in c ch huy. Trong loi my pht ny, vic ch huy
(iu khin) cng theo hai nguyn tc v ng vi hai cch iu khin ny ngi ta ch to hai
loi my pht tia in khc nhau:
+ My pht tia in dng hai tia in, tia in chnh, tia in ph (hnh 2.9), tng t
nh my h quang.
+ My pht tia in dng ngt in ng b (hnh 2.10), ngha l iu khin bng m t
ng b.
My pht tia in dng hai tia din (hnh 2.9)
32
Trong my ny c mt tia in chnh v mt tia in ch huy. Theo s hnh

2.9, khi ng mch in K, bin th Tr c np in v tng th ln hng ngn vn
(V). Lc h t in C c tch in v th hai ct ca t C l th ca khong n
gia hai qu cu E. Lc ny trn mch in LC khng c dng in, t C c tch
in cho n khi t c th Vf (th phng in gia hai qu cu E) th tia in s
nh qua hai qu cu E, t C phng in qua E lm cho trn mch dao ng LC xut
hin tc khc mt dao ng cao tn, dao ng ny khng qua c L 2 (hay R1); do
bt buc phi nh qua khong n F (khong cch gia hai in cc chnh). Nh vy,
h c mt dao ng v mt tia in nh E, th cng c mt tia in phng qua F,
ngha l tia in E iu khin tia in F. Sau qu trnh c th tip din cho
n khi ta ngt cng tc K.
Mun cho qu trnh phng in
c n nh th hai qu cu E phi c
kch thc xc nh, khong cch
khng i v b mt phi nhn. C
nh th in th Vf mi c nhng gi
tr xc nh ng vi tng cp thng s
ca my pht tia in c chn,
m bo cho qu trnh phng in
F n nh v mt nng lng, v c
hai tia in xy ra ng thi, nn nng
Hnh 2.9
lng phi chia i hai khong n E

b
My pht tiain dng hia tia in
v F. V th mun c nng lng ln

(nhit cao) th th Vf phi rt ln.
My pht dng ngt in ng b (hnh 2.10).

My
pht
loi
ny
ch
to
theo s ca Fressner. y s
phng
in
ch
huy
nh
mt
m t ng b c gn b ngt in
mc
ngay
trn
mch
ca
my
pht
tia in. My pht gm bin th Tr
tng
khong
cun
th,
phng
cm
L1 s
mch
in
L2
dao
ng
LC,
F,
hai
khng
cho
chnh
ngn
dao ng cao tn tr v bin th Tr

v m t ng b M ng v
m mch in ca qu trnh phng Hnh 2.10
in gia 2 in cc F
.
My pht tia in dng ngt in ng b

33
Khi cho in vo my, bin th Tr tng in, t C c tch in dn, m t M quay u c mang
theo hai tip im A v A, cng quay, khi n v tr B v B 1 mch in trong my c ng, lc th
t C cng t cc i, khin cho tia in phi phng qua F, sau tia in li tt. Nhng v m t M quay
u lin tip, nn tia in cng nh u n lin tip qua F theo s quay ca mt M tun hon n v tr
B v B1 ln lt theo thi gian chu k c chn, cho n khi no ta ngt cng tc K. Nh vy, chnh m
t ng b M iu khin s phng in theo cc thng s c chn.
Plasma cao tn cm ng ICP

c im v tnh cht
y l ngun nng lng mi c s dng trong php phn tch quang ph pht x nguyn t
khong
10
nm li y; song li c s dng rng ri v c hiu qu cao v n c nhng c im sau
y:
Ngun nng lng ny c nhit cao. Thng thng tnm ca plasma c th t c nhit t
5000 - 10000OC nn ha hi v nguyn t ha c ht mi trng thi ca vt liu mu vi hiu sut cao.
Vi plasma ny, mi nguyn t kim loi u b kch thch to ra ph pht x ca n. Cc hp cht bn
nhit cng b ha hi v phn li thnh nguyn t t do, nhng trong ngun nng lng ny ph pht x ca
Ion l ch yu.
ICP (Inductivity Coupled Plasma) l ngun nng lng kch thch ph pht x m bo cho php
phn tch c nhy rt cao. Ni chung c th t t n.10" 4: n.106% (0,l - 5) ngng i vi hu ht cc
nguyn t. Tt nhin nhy ca php phn tch y ph thuc nhiu vo cng sut ca my pht cao
tn HF to ra plasma ICP (hnh
2 .11 ).
ICP l ngun kch thch ph khng nhng c nhy cao, m cn c n nh cao. N hn hn h
quang v tia in. V th php phn tch dng ngun nng lng ny cho sai s rt nh; ni chung l nh
hn 10 % trong vng nng t n.10 -3- n.10 -5%.
34
kW
1
Hnh 2.11
S ph thuc ca cng vch ph vo cng sut my pht cao tn ICP
Tuy c nhit cao nhng s kch thch ph pht x trong ngun nng lng ny li rt m du. N
tng t nh s kch thch ph trong ngn la n kh. Chnh v th m phng php phn tch t n
nh cao v sai s nh.
Vi ngun nng lng ny, ngi ta c th nh lng c ng thi nhiu nguyn t mt lc, nn
tc phn tch rt cao (t 40 - 120 mu/gi). Mt khc, khi dng ngun nng lng ICP, vng tuyn tnh
ca phng php nh lng l rt rng (t 1 - 10. 000 ln).
c im cui cng l rt t xut hin nh hng ca cht nn (matrix effect).
l im hn hn cc ngun nng lng c in nu.
Chnh do nhng c im v u vit ca ngun nng lng ICP nh th, nn n nhanh chng
c ng dng rng ri v thay th cho ngun nng lng c in: tia in v h quang. Tt nhin, trang b
to ra ngun nng lng ny t hn. Nhng trong iu kin ngy nay v do tnh cht u vit ca n
nn cc phng phn tch quang ph pht x u c trang b loi ngun nng lng ny.
Cu to ca h thng 1CP
V nguyn tc, h thng thit b to ra ngun nng lng ICP gm hai phn chnh: my pht cao
tn HF v h thng to th si kh v n nguyn t ha kch thch ph ca mu phn tch.
My pht cao tn HF
Cc my ny lm vic tn s rt cao nhng ph bin l hai tn s 27,12 MHZ v 450 MHZ.
Trong my trung tn s 27,12 MHZ c s dng nhiu hn. l tn s sng mang rai. My pht
cao tn HF c nhim v pht tn s cao cung cp nng lng cho cun cm cao tn u ming n
nguyn t ha mu, to ra plasma nhit cao cho s ha hi mu, nguyn t ha v kch thch ph (hnh
12 a).
35
Phn th hai ca h thng ICP l b phn nguyn t ha mu, bao gm b phn to soi kh mu v
n nguyn t ha mu (nebulizer system v khch bumer). B phn burner c ch to bng thch anh
chu nhit. N gm ba ng lng vo nhau, gn chc vo nhau phn y, v mi ng u c ng dn kh
vo (hnh 2.12a). Trong , ng trong cng l mt ng mao dn dn mu vo plasma nh kh mang; ng
th hai l ng to ra kh plasma. Cn ng th ba l ng to kh lm lnh cho n nguyn t ha. Pha
ngoi ng th ba v ngay u c cun cm cao tn bng ng. Cun cm ny c ni vi my pht cao
tn HF v lun c lm lnh bng dng nc chy qua khi lm vic. ng thi chnh cng sut lm vic
ca cun cm ny s quyt nh nhit ca plasma kch thch ph. Cn h thng nebulizer, v nguyn
tc, hon ton tng t nh trong ngn la n kh nu trn.
Kh dng trong plasma ca ICP l cc kh tr nh argon, hli, nit. Trong argon l u vit nht.
y ngi ta c th dng kh mang v kh plasma l argon, cn dng nit lm lnh. Hoc c th dng
ch mt kh Ar cng c. Trong tng lng kh cho c ba dng l t 13 - 18 lt/pht v c phn chia
nh nhau:
Kh mang: 0,7 - 1,0 l/pht.
Kh plasma: 6 - 8 l/pht.
Kh lm lnh: 5 - 9 l/pht.
Nhng ngy nay, ngi ta ci tin v dng loi mini - ICP nn ch cn n 1/3 lng kh so vi loi
thng thng nu.
Hnh 2.12a
H thng ngun ca ICP-AES
Nhit ca plasma ICP
ICP l ngun nng lng kch thch ph c nhit cao, nhng li n nh hn so vi cc loi
ngun kch thch khc, nh h quang, tia la in. Nhit ca plasma ca ngun ny c quyt nh bi
dng in cm ng trong cun cm A u ca n nguyn t ha, tc l nng lng cao tn ca my pht
HF. V vy, ng vi nhng thng s nht nh ca my pht HF th plasma ny c mt nhit xc nh.
Trong cc thng s ca my pht HF, cng sut v tn s cm ng l hai thng s quan trng
36
nht. Song mi my pht thng ch dng mt tn s cm ng nht nh 27,12 MHZ hay 450 MHZ, nn
cng sut ca my pht ng vai tr chnh. V th cng ca vch ph ph thuc vo cng sut ca my
pht HF (hnh 2.11).
Tt nhin, bn cnh cn c nhng yu t khc nh hng n nhit ca plasma ICP. Trc ht
l tnh cht ca kh plasma, kh mang v tc chy ca chng vo plasma. Sau l thnh phn ca hn
hp mu c dn vo plasma kch thch ph. Ni chung dng lin kt, th Ion ha ca cc nguyn t
cng c nh hng n nhit ca plasma. Nhng cc yu t ny khng mnh nh trong h quang v tia
in. Yu t matrix effect cng c tc dng, nhng cng khng ln nh trong ngn la n kh v trong h
quang in. Cc yu t trn nh hng n nhit ca plasma, tc l nh hng n cng ca vch
ph. Nhng khi chn c cng sut ln ph hp, th nh hng ny s rt nh, hay khng cn na.
S kch thch ph pht trongplasma ICP

Khi ta ng mch in ca my pht cao tn HF th cun cm A u n s xut hin tc khc
dng in cao tn cm ng c nng lng ln. Nng lng ny c quyt nh bi cc thng s ca my
pht HF c chn. ng thi tia la K cng c bt, hn hp kh v mu c t chy, plasma
nhit cao xut hin, ngha l ngn la hnh thnh. Trong ngn la nhit cao ny, trc ht dung mi
bay hi ( phn trong, phn ti ca ngn la), li cht mu dng ht bt mn. Ri cc bt mu ny b
nung nng, nng chy, c ha hi, phn li, b nguyn t ha v Ion ha to ra trong plasma c
phn t, nguyn t, Ion, in t trng thi kh. Trong ch yu l cc nguyn t, Ion v in t. Sau
cc phn t kh ny c trong plasma s b kch thch v sinh ra ph pht x. Bn cht s kch thch ph
y l s kch thch nhit, n ging nh s kch thch ph pht x trong ngn la n kh. Nhng v plasma
c nhit cao (nng lng ln) nn hiu sut nguyn t ha v kch thch ph cao v ph ca ngun nng
lng ny vi cc kim loi kim v kim th ch yu l ph ca cc Ion bc 1 . C ch ca qu trnh trong
plasma ICP c th tm tt theo s sau:
37
Hnh 2.12b
Hai loi my o ph pht x ICP (ICP-AES)
HF: My pht cao tn; Pm: H thng nguyn t ha mu; L: Thu knh; T: Khe sng; G:
Cch t; PM: H nhn quang in; >>: H in t; Mr: My tnh; Sig: B ch th kt qu o;
AB: Cung mt phng tiu; M h M2: cc gng chun trc v hi t.
Trc ht l dung mi bay hi, li cc ht bt mu. Tip theo l bt mu b nung
Ba qu trnh chnh: Cc qu trnh chnh y cng tng t nh trong ngn la n kh.
Nhng c khc ngn la n kh l hiu qu ha hi, nguyn t ha v kch thch ph cao hn
nhiu.
Nu Eh < Ent, th mu s ha hi, nguyn t ha to ra cc nguyn t t do, chng b
38
Me(k) + E ^ Me(k)* ^ MeO + n(hv)

Nng lng K.Th.
Chm tia pht x

(tr F), axetat, mt s nitrat, sunphat,.. ca kim loi thng theo c ch ny.
Nu Eh > Ent, th phn t ca cht mu s b nguyn t ha trc, sau ha hi thnh
Men Xm(r) ^ Men(k) + Xm(k) ^ mMe(k) + nX(k)
Me(k) + E ^ Me(k)* ^ Me O + n(hv)
Nng lng K.Th.
Chm tia pht x

cht mui SiO3-2, PO4-3, F, mt s nitrat, sunphat... ca kim loi thng theo c ch ny.
S Ion ha sinh Ion, sau cc Ion b kch thch v sinh ra ph ca n.
C th l:
Me(k) + Ei ^ Me(k)+ + e Me(k) + E ^ Me(k)+* ^ Me O + n(hv)
V trong ngun ICP c nhit cao, nn cc kim loi c th Ion ha thp s din ra theo
c ch ny, v d cc kim loi kim, kim th.
Qu trnh ph gm c:
+ To ra cc hp cht bn nhit, ch yu l cc monoxit (dng Me O). Nhng trong
plasma ca ngun ICP th cc qu trnh ny xy ra khng ng k. chnh l u vit ca
ICP.
+ S hp th bc x ca nguyn t (qu trnh t o).
+ S pht x nn (nhng cng nh).
+ S
Ion habc hai ca nguyn t
kim loi kim v cc nguyn t c
th Ion
ha bc hai thp.
39
Ht mu
Ha hi
Nguyn t ha
Ion ha
Kch thch ph
(nu E hh < Engt )
Hnh 2.13 S qu trnh nguyn t ha

mu
Nguyn tc v cch chn ngun kch thch ph
Cc iu kin kch thch ph l nhng yu t c nh hng trc tip n cng ca vch ph v
nhy ca phng php phn tch. V th chn ng cc iu kin kch thch ph l mt m bo cho
phng php phn tch t kt qu chnh xc, tin cy v nhy cao. Mt khc, qua vic chn c
iu kin kch thch ph ph hp ta c th loi tr c mt suyn t nh hng, nh matrix effect, nng
cao nhy. Do chn c nhng iu kin, ngun kch thch ph ph hp cho mt i tng phn
tch no chng ta phi da theo mt s nguyn tc c bn sau y:
Phi xut pht t i tng phn tch thuc dng mu no (mu bt, mu rn, mu dung dch hay
hp kim), cng nh nhng tnh cht c l ca tng loi mu thuc loi mu d bay hi hay kh bay hi,
dn in hay khng dn in. V d khi phn tch mu bt (qung, t ,...) th h quang c dng trn 10A
l thun li. Song khi phn tch mu hp kim th tia in li u vit. Mu dung dch dng ICP.
Phi da theo tnh cht v c trng s kch thch ph ca mi nguyn t cn xc nh m chn
ngun nng lng kch thch v cc thng s ca ngun kch thch. V d phn tch kim loi kim th nn
dng ngn la n kh hay h quang gin on.
V th kch thch ph pht x ca cc kim loi kim l khng ln (3 - 5eV).
40
Ngc li, vi cc nguyn t V, Zn, W,... hp cht bn nhit, li phi chn ngun kch thch c nng lng
cao, h quang in dng ln hay ngun ICP.
Khi chn ngun kch thch phi m bo cho php phn tch c nhy cao, n nh, c th d
dng phn tch c cc nguyn t c nng nh.
Chn ngun kch thch phi m bo cho php phn tch tiu tn t mu v khi cn phi khng ph
hy mu. Yu t ny trong mt s trng hp khng yu cu, bt buc nh ba yu t trn.
Cng vch ph pht x nguyn t

Cng vch ph :
Trong ngun pht sng hay trong plasma, nguyn t (A o) ca mt nguyn t c kch thch t
trng thi nng lng thp Eo, ln trng thi nng lng cao. Cm c biu din theo phng trnh:
Ao + XE = A* (a)
Vi mu phn tch c nng xc nh ca A o th qu trnh ny lc u tng nhanh, sau chm
dn v ti mt thi im nht nh th khng tng na. Ngha l s nguyn t Ao b kch thch l khng i,
ng vi mt nhit xc nh ca plasma. ng thi vi qu trnh trn l qu trnh ngc li, tc l
nguyn t b kch thch A* gii phng nng lng m n nhn c di dng cc tia pht x n(hv i)
tr v trng thi nng lng thp bn vng ban u. Chnh qu trnh ny l qu trnh pht x ca nguyn
t v sinh ra ph pht x ca nguyn t, c th c biu din theo phng trnh:
A* = hv + Ao (b)
Qu trnh ny lc u chm, sau tng dn theo s nguyn t A * b kch thch v n mt thi
im nht nh th cng khng tng na ng vi mt nhit nht nh ca plasma. Ngha l sau mt thi
gian nht nh ca s kch thch ph, th hai qu trnh trn (a) v (b) s t n trng thi cn bng. l
hai cn bng ng hc thun nghch. Cn bng ny ch ph thuc ch yu vo nhit ca plasma, ngha
l s nguyn t A* b kch thch v pht x l khng i, ng vi mt nhit xc nh ca plasma.
Nu gi Nm l s nguyn t ca nguyn t Ao b kch thch n trng thi nng lng cao cm, th
theo quy lut Bolzmans ta c:
N = N gme(-Ev )/ Kt
m
a _
m'
g0
go v
gm l trng lng thng k
ca
nguyn t
A trng
thi ban u, nng
lng Eo v trng thi kch thch nng lng cm;

Na l s nguyn t ca nguyn t Ao c trong plasma (trng thi hi);
41
Em l nng lng kch thch nguyn t o t trng thi Eo ln trng thi cm;
T l nhit ca plasma (oK);
k l hng s Bolzmans.
Nu gi Ia l cng ca vch ph do qu trnh kch thch ph ni trn sinh ra, th trong mt
gii hn nht nh ca nhit plasma v nng ca nguyn t A o trong plasma, ngi ta thy Ia ph
thuc vo:
S nguyn t Ao b kch thch ln trng thi A*, (Nm).
Thi gian tn ti ca nguyn t A* trng thi kch thch, (trn).
Nng
lng kch thch nguyn
t A t
trng thi c
bn n
trng thi kch
thch, (Em).
Xc sut chuyn mc ca nguyn t A t trng thi kch thch nng lng C m v trng thi ban u
nng lng Eo, (Amo).
V mi quan h ny c th biu din theo cng thc sau:
a = f. f .Amo .Aa . ^.hv.e-(EE) / k T

tg
m
o
Nhng i vi mt loi nguyn t v trong mt iu kin th nghim nht nh ca plasma (ch yu
nhit plasma) th cc yu t tri Amo, go, gm, cm, hv l nhng hng s.
vch ph
Ia ch
cn
ph
Cho nn cng
thucvo s nguyn
t bkch
thch Na m thi. Nh vy ta c:
I
Vi
=KN
= f.
tg
m
(2.6)
.A
. ^ .hv.e-(E)/
l cng vch ph ca nguyn t.

Song cng thc (2.6) mi ch cho ta bit mi quan h gia cng vch ph I a v nng ca
nguyn t trng thi hi trong plasma, m cha ch cho ta c mi quan h gia cng vch ph v
nng ca nguyn t trong mu phn tch. Mun th ta phi xt mi quan h gia nng C trong mu
v s nguyn t Na trong plasma. Ni chung, mi quan h ny l phc tp, n ph thuc vo nhiu yu t,
nh:
Kh nng ha hi, bn cht ca cht mu, cht nn;
Thnh phn ca mu, cht ph gia thm vo;
Trng thi lin kt, tn ti ca cht mu;
Cc iu kin ha hi, nguyn t ha mu, kch thch ph;
Mi trng kch thch ph, v.v...
Tuy nhin ngi ta thy t thc nghim, trong mt phm vi nht nh ca nng
42
C th ta lun lun c:
Na = k2.Cb (2.7)
Nh vy, cng vch ph s l:
Ia = a.Cb (2 .8 )
Trong : a: k1.k2 v a c gi l hng s thc nghim. N ph thuc vo tt c cc iu kin thc
nghim ha hi, nguyn t ha v kch thch ph mt nguyn t. V th trong mt php phn tch phi gi
cho cc iu kin thc nghim n nh, m bo a thc s l hng s ca php o. Cn b l hng s bn
cht, n ph thuc vo bn cht ca tng loi nguyn t, b ch nhn nhng gi tr bng
v nh hn 1 ,
nhng ln hn 0. Gi tr ca b nh hn 1 khi nng C ln, cn khi C nh th b lun lun bng

Khi b nh hn 1 l lc qu trnh t hp th xy ra. Qu trnh t hp th xy ra cng nhiu (mnh) th b cng
nh xa 1 , tc l chnh hng s b l c trng cho qu trnh t o ca mi loi nguyn t. Do , ng vi
mi nguyn t v vi mi mt vch ph pht x v trong nhng iu kin nht nh, ta lun c mt gi tr
nng Co, m:
+ Khi vi mi Cx < Co th b lun lun bng 1.
+ Khi vi mi Cx > Co th b nh dn xa 1 (hnh 2.14).
Trn y cp n cng ca vch ph nguyn t trung ha nhng trong plasma cn c c
cc Ion. Chng cng b kch thch v sinh ra ph pht x. Qu trnh kch thch v pht x cng ging nh
cc nguyn
tvcng tnh ton hon ton
tng t nn chng ta c cng vch ph Ion l:

li = Al. Cb (2.9)
Hnh 2.14
Quan h gia cng vch ph v nng
Do , mt cch tng qut, ta c th vit cng vch ph pht x: I = a.C b

(2 .10 )
43
Cng thc (2.10) l phng trnh c bn ca phng php phn tch nh lng theo
ph pht x nguyn t. Phng trnh ny do Lmakins (Nga) v Saiber (c) tm ra, nn gi
l phng trnh Lmakins-saiber.
Cng vch ph v nhit plasma
Nh trn chng ta bit, cng vch ph pht x ca nguyn t c tnh theo biu
thc sau: Ia = Pa.N(l-x)e
V vch Ion:
Ii = Pi.N.x.e
(2.12)
lg
Trong , vi:
P
= .A
,hv
tg
E(m)/kT
-Em/kT
iu ny cho thy cng ca vch ph ph thuc vo nhit ca plasma.

Nhng, tt nhin, s ph thuc ny i vi vch nguyn t v vch Ion l khc nhau v
khng n iu, m theo hm s m (e -Em/kT). Chnh hai cng thc trn d dng cho ta thy
rng, nhit no ca plasma to ra c s nguyn t N(1 - x) trong cng thc tnh cng
vch nguyn t v s phn t (N.x) trong cng thc vch ph ln l ln nht, th lc s
c c cng ca vch ph ln nht. l nhit ti u ca s kch thch ph.
100
200
300
100
200
Ca: 4226,70 /nn Al203; Ca: 4226,70 /nn Si02 AI: 3093,00 ; Mg: 2852,19 ;
Si 2516,00 A;Sn: 2355,00 .
Hnh 2.15
S ph thuc ca cng vch ph vo nhit trung tm plasma
44
300
400
Vi mt vch ph ca mt nguyn t, thc t ch c mt nhit to ra c cng I

cc i. Nhit ny c gi l nhit ti hn ca vch ph v c k
l
To. Ttnhin
hiu
i vi mivch th nhit To ny khc nhau (hnh
2.15a,b,c). Ngay i vi vch ph ca mt nguyn t, nu n tn ti trong cc nn mu khc

nhau (matric khc nhau) th nhit T o ny cng khc nhau (hnh 2.15c). iu c ngha l,
ngoi
bncht ca chtphn tch, nhit
To cn phthuc vo
thnh phn v nn ca mu phn tch.

Tnh cht ny c ngha thc t rt ln khi xc nh lng nh cc nguyn t trong mu
phn tch. V trong nhng trng hp ny ta cn phi chn nhng iu kin lm vic v iu
kin kch thch ph sao cho thu c vch ph c cng ln nht, tc l chn cc iu kin
kch thch ph c c nhit ca plasma gn vi nhit T o ca vch ph cn o, hoc
bng ng c To l l tng. Tt nhin bng c l trng hp rt him, ta ch c th lm
cho nhit ca plasma cng gn vi nhit To th cng tt.
Hin tng t hp th (t o)
trng thi hi trong plasma, hin tng mt nguyn t c kh nng hp th tia bc x
do chnh mt nguyn t khc cng loi ca chng pht ra c gi l hin tng t hp th
(hay t o). Hin tng ny xy ra theo nh lut Kirschhoff. Ngha l mt nguyn t ch hp
th nhng tia bc x m chnh n c th pht ra c trong qu trnh pht x. Hin tng ny
thng xy ra mnh v ch yu i vi cc vch cng hng, vch
ph pht
x ca mtnguyn t, v
cuicng
ca
nng cng
ln, th hin tng ny xy ra cng mnh. Chnh do hin tng ny, m a n kt qu lm

cho cng vch ph pht x I khng ph thuc tuyn tnh vo C, khi nng C tng gi
tr Cx > Co, Gi tr Co c gi l nng gii hn, cn c quan h gia I v C l tuyn tnh.
Vi mi vch ph, C o l khc nhau. Vch cng nhy th C o cng nh. ng thi, trong qu
trnh pht x, cng sut pht x ca mt vch ph c tnh theo cng thc:
W = f.Wo
(2.13)
vi f l h s hot ng pht x ca vch ph v n nhn gi tr: 0 < f < 1.
Khi khng c hin tng t o, ngha l nng Cx nh hn Co th f = 1, tc l W =
Wo. Cn mi trng hp khc, khi c hin tng t o th lun lun c W < W o. Trong :
o
=jA
.N
.hv.e-
)dv
(2.14)
0
y: Na l s nguyn t trong n v th tch V ca plasma.
Amo l xc sut chuyn mc;
Cm l nng lng kch thch trng thi mi T
l nhit ca plasma (oK);
45
hv l lng t sng c bc x ra; k l

hng s Bolzmans.
V ngha thc t, khi hin tng t hp th xut hin, ni chung u khng c li cho php phn
tch ph pht x nguyn t. iu c ngha l trong phn tch khng nn xc nh mt nguyn t vng
nng bt u xut hin hin tng t o, tc l nm ngoi vng tuyn tnh, phi pha long mu kt
qu s chnh xc hn.
Bc x nn trong ph pht x
Khi kch thch mu phn tch ta thu c ph pht x ca n. Ph ny gm c ph vch ca nguyn
t v Ion, ph m ca phn t v nhm phn t. Sau n ph nn hay gi l bc x nn. Bc x nn
thng l ph lin tc. N to thnh mt di en m trn ton b vng ph ca mu phn tch. en ca
di ph nn ny mi vng ph l khc nhau. Thng thng vng sng di m hn vng sng ngn.
Nhn chung, n tng dn t vng sng ngn sang vng sng di, n th hin r rt vng kh kin (360 500 mm). Cn vng t ngoi (UY) th ph nn thng rt nh.
Trong mt mc va th bc x nn l c li v n lm nn cho vch ph xut hin ln trn
m hn, ngha l lm tng cng ca vch ph. Do , trong mt s trng hp nn qu yu ngi
ta thng phi chiu sng ph knh nh bng nh sng
gian phhp. Song trong nhiutrng
trng vi
mt thi
hp ph
nn
thng qu mnh, c bit l trong vng kh kin v khi dng h quang. Lc ny n che lp mt vch ph
ca nguyn t phn tch, nht l nng nh. Trong trng hp ny ngi ta phi tm cch kh bt bc
x nn. Vy nguyn nhn no gy ra bc x nn ?
T nhng kt qu nghin cu ngi ta thy c cc yu t sau y to ra bc x nn (ph nn):
S pht sng ca ht vt rn c t nng trong plasma.
Tc dng ca nh sng trng.
S bc x ca in t trong plasma nhit cao.
Do in cc b t nng sng v pht x (vt rn pht sng nhit cao).
Trong ba yu t ny, yu t th ba th hin khng r nt bng hai yu t u. loi tr bc x nn
ngi ta c th p dng nhiu bin php khc nhau. V d vi nguyn nhn th nht, ngi ta dng mn
chn trc khe sng khng cho nh sng do hai u in cc c t nng chiu vo khe my quang
ph. Hoc cng c th thm cht ph gia vo mu phn tch kh bt mt phn cng nn, lm cho
nn ca ph khng qu en. Nhng tt nht l kch thch ph trong mi trng kh tr Ar (argon) hay
hn hp ca
kh tr
Ar v oxy theo nhng t l
ph hp. Bin php ny
loi tr c c ph nn v ph xm ca nhm CN v ph phn t H 2 O, mt khc li cn tng c cng

vch ph, ngha l tng c nhy ca phng php phn tch. l u vit ca mi trng kh tr
trong s kch thch ph pht x nguyn t.
46
Chng 3
MY QUANG PH V S PHN LI CHM SNG
Nguyn tc cu to ca my quang ph pht x

My quang ph l mt dng c dng thu, phn li v ghi li ph ca mt vng ph quang hc nht
nh. Vng ph ny l mt i ph ca vt mu nghin cu t sng ngn n sng di. Ty theo b phn
dng phn li nh sng trong my da theo hin tng vt l no (khc x hay nhiu x) m ngi ta chia
cc my quang ph thnh hai loi.
My quang ph lng knh. l nhng my quang ph m h tn sc ca chng c ch to t 1
hay 2 hoc 3 lng knh. S phn li nh sng y da theo hin tng khc x ca nh sng qua hai
mi trng c chit sut khc nhau (khng kh v thy tinh hay khng kh v thch anh).
My quang ph cch t. L nhng my quang ph m h tn sc l mt cch t phng hay lm phn
x. Bn cht ca s tn sc nh sng y l s nhiu x ca tia sng qua cc khe hp.
Tuy c 2 loi my quang ph khc nhau, nhng v nguyn tc cu to th u nh nhau, u gm 3
phn chnh. l h chun trc, h phn li v h hi t chm sng (hnh 3.1).
H chun trc v phn u ca my quang ph . N gm mt hay mt h

thng thu knh ghp vi nhau hay h gng hi t v mt khe hp (khe vo ca chm sng v c th iu
chnh c) t tiu c ca h thu knh ny. H chun trc c nhim v nhn v to ra chm sng song
song hng vo h tn sc phn li thnh ph.
Htn
sc. l mt h thng lng knh hay mt tm cch
t. H ny c
nhim v phn li (tn sc) chm sng a sc thnh cc tia n sc, tc l phn li mt ngun sng phc tp
nhiu bc sng khc nhau thnh mt di ph ca chng theo tng sng ring bit lch i nhng gc khc
nhau. Nu h tn sc c ch to bng lng knh th chng ta c my quang ph lng knh. V ngc li,
nu h tn sc l cch t ta c my quang ph cch t. Trong my lng knh, tia sng ngn s b lch nhiu,
sng di lch t, cn trong my cch t th ngc li.
47
-1^
<D
H bung nh. l mt h thng thu knh hay mt h gng hi t v mt

mt phng tiu ca cc chm sng. H ny c nhim v hi t cc tia sng c cng
bc sng sau khi i qua h phn li li vi nhau to ra nh ca khe my trn mt
phng tiu. chnh l cc vch ph.
Thm vo l mt s b phn ph khc my quang ph c th hot ng
c chnh xc, d dng v c hiu qu cao hn. V d nh:
H thng gng hay thu knh chiu sng khe my.
H thng gi in cc.
Cc loi chn sng v lc sng trc khe my.
B phn t ng a mu.
My tnh v phn mm iu khin v x l s liu.
Cc loi my quang ph pht x

Lng knh v my quang ph lng knh
Lng knh v my quang ph
Lng knh l mt b phn quan
trng ca my quang ph lng knh.
N
quyt
nh
kh
nng,
tnh
cht
phn li nh sng ca my quang ph.

Lng
knh
sut,
ng
nht
mt
vng
ph
mt
v
nht
mi
trirng
trong
ng
hng
trong
nh.
gii
hn bi 5 mt phng, nh trong hnh B

ta c: ABC v A,B'C' l hai mt Hj h32
tit din ca lng knh, n song song
vi nhau.
Cu to ca
mt lng knh______________________
BB'CC' l mt y ca lng knh. Cc mt ABB'A, v AAICC' l hai mt bn ca lng knh. Cnh

AA, gi l cnh nh ca lng knh. Gc i din vi mt y gi l gc nh ca lng knh. Mt lng knh
thng
chnh. l gc nh A (hay cnh y) v chit sut
c c trng
bi hai i
n ca vt liu lm lng
lng
knh. Nu
ta chiu mt chm sng Si vo mt mt bn ca lng knh th hin tng khc x s xy ra nh trong hnh
3.3.
Trong :
Si l tia ti; KH l tia l.
l gc ti v i' l gc l ca tia sng;
50
D l gc lch ca chm sng sau khi qua lng knh;

ABC l tit din chnh ca lng knh;
Di l gc lch ti thiu;
y ta c cng thc c trng cho 1 lng knh l:
Sin (A + D) = n. sin(A / 2)
dD dn .
2 sin( A / 2)
= .sin .- ==y== / __
d d
- n2 sin2(A/2)
(3.1)
(3.2)
Chnh hai i lng ni trn c nh hng trc tip n s phn li chm sng,
ngha l quyt nh gc lch D ca chm sng. Chnh v th khi ch to lng knh
ngi ta phi chn nhng vt liu c chit sut ln v ch to gc nh ca lng knh
c ln cho ph hp.
Vt
liu
lm
lng
knh
cng
phi
trong
sut,
ng
nht
trong
mt
vng
ph
nht
nh.
phi
bn
vi
hu
nh
khng ph thuc vo
nhit
ng
hng
nhit v nh sng.
Chit
sut
phi
v m.
Trong vng kh kin, ch to lng knh ngi ta thng dng mt vi loi thy tinh, nh thy
tinh flin nng, flin nh, thy tinh krau. Trong vng t ngoi ngi ta thng dng thch anh. Nu c vng
ph (UY + VIS) phi dng thy tinh c bit.
Cc c trung ca my quang ph lng knh

nh gi cht lng, hiu qu v kh nng s dng ca mt my quang ph, ngi ta thng
dng ba thng s c trng c bn l tn sc gc, tn sc di v phn gii.
tn sc gc.
Trong mi my quang ph, s bin thin ca gc lch D theo di sng ca tia sng l mt c
trng quan trng. N ni ln kh nng tn sc gc ca mt my quang ph v c gi l tn sc gc
ca my quang ph .
Trong cc my quang ph lng knh, lng knh thng c t v tr cc tiu i vi tia sng
trung tnm ca mt vng ph ca my. V th tn sc gc s c
51
tnh theo cng thc:

^ Dd .
2sin(A/2)
D --7 -.sin ---------=====
dX
dn
X-:-
(3.3)
-n sin2(A/2) dX
Nu gc nh A ca lng knh bng 60 th cng thc trn s l:

-2 xdn
Vl - n
(3.4)
dX
Nu my quang ph c m lng knh nh nhau trong h tn sc, th tn sc ca my s bng m

ln ca my 1 lng knh. Cn nu cc lng knh c gc nh A khc nhau, th tn sc chung s l tng
ca tn sc tng lng knh theo cch b tr. Ngha l tn sc gc chung bng tng tn sc gc ca
tng lng knh c trong h tn sc ca my quang ph.
Nh vy, theo cc biu thc trn, chng ta thy tn sc gc ca mt my quang ph lng knh ph
thuc vo cc yu t sau:
S lng knh c trong h tn sc.
Gc nh A ca lng knh.
Chit sut ca vt liu lm lng knh.
Bin thin theo bc sng (sng ngn lch nhiu, sng di lch t).
V th, mun tng tn sc gc ca mt my quang ph lng knh ngi ta phi ch to h tn sc
c nhiu lng knh ghp li vi nhau. Trong thc t ngi ta thng ghp hai hoc ba lng knh. Bin php
th hai l chn nhng vt liu c chit sut ln ch to lng knh v ch to cc lng knh c gc nh A
ln. Nhng bin php ch to gc A ln cng ch thc hin c trong mt mc nht nh, thng
thng n 90 l ln nht. V khi tng gc nh A ca lng knh th hin tng phn x ton phn mt
bn ca lng knh s nhanh chng xut hin, lm mt phn chm sng s khng ra khi lng knh, v ta b
mt chm tia .
tn sc di. tn sc gc ch cho bit s khc nhau v gc lch ca 2 tia sng, ngha l tia
sng b lch i ni gc ln bao nhiu sau khi phn li, m cha ch ra c hai vch ph gn nhau s
cch nhau l bao nhiu trn mt phng tiu (hay knh nh). Do , trong thc t, nh gi kh nng tn
sc ca mt my quang ph ngi ta cn phi s dng thm c tn sc di. Nhng tn sc di ph
thuc vo tn sc gc v tiu c ca thu knh bung nh f2, v n c tnh theo cng thc:
D1 - dl -_f^xdD
d sin E d
(3.5)
Trong di l khong cch gia hi vch ph trn mn nh (mt phng tiu); E l gc nghing ca
hp nh vi quang trc bung nh ca my v do hiu s di sng ca 2 vch ph, tc l : d X = (1 -
X2) v X = (X2 + 1)/2.
52
Theo cng thc trn, mun tng tn sc di ca mt my quang ph lng knh

ngi ta phi:
Tng tn sc gc ca n.
Tng tiu c ca thu knh bung nh f 2. Nhng bin php ny ch t c
trong mt gii hn nht nh. V khi f 2 cng ln th cng sng ca vch ph cng
gim, ngha l c v tn sc th mt v cng (hai yu t ny t l nghch vi
nhau). Do , trong thc t, ngi ta phi tnh ton v chn gi tr f 2 cho ph hp
sao cho c tn sc ln, m cng vch ph vn m bo cn trn 80%.
Tuy nhin, d nh gi v so snh tn sc di ca cc my quang ph vi
nhau, trong thc t ngi ta li thng dng gi tr nghch o ca tn sc di,
ngha l thay biu thc dl/dX bng biu thc dl/dX. Nh vy, i lng mi quy c
ny cho ta bit c trn n v di ca knh nh (mm) hay mt phng tiu c cha
bao nhiu n v di sng (amstrong hay nm), ngha l my quang ph no c gi
tr dX/dl cng ln th c tn sc di cng nh. V d hai my quang ph Q l v Q2,
m Q1 c dl bng 4 A/mm v Q 2 c dX/dl bng 2 A/mm, th my Q 2 c tn sc di
gp i tn sc di ca my Q1.
tn sc di ca mt my quang ph c lin quan trc tip n di ca vng
ph m my thu nhn c. Vi mt vng ph nht nh tn sc di cng ln th
vng ph ca my cng ri ra trn mt khong rng, ngha l mt phng tiu ln, nh
th trn mt knh nh c chiu di nht nh th ch thu c mt phn ca ton vng
ph ca my, nu my c tn sc ln. Nh trong v d trn ca hai my quang
ph Ql v Q2, i vi vng ph t 2000 - 4000 A th ton b vng ph thu c ca
my Q2 chim di gp i ca my Ql.
Do vi nhng my c tn
sc ln, ngi ta khng th thu c
D (/mm)
ton b vng ph ca chng ln mt

knh nh, v phi cn mt knh nh
qu di. Cho nn ngi ta phi ghi
tng phn ca ton b vng ph ca
my ln mt knh nh c di nht
nh (24 hay 30 cm), ngha l i vi
nhng my quang ph c tn sc
ln ngi ta phi c b phn quay v
hng vng ph cn nghin cu vo
Hnh 3.4
mn nh thu ghi.
ng cong tn sc ca 2 my quang ph
(I) - My lng knh Q24; (II) - My cch l PGS-2
Trong my quang ph lng knh, tn sc ca chng gim theo s tng ca di

sng, ngha l trong mt my, th vng sng di c tn sc nh hn vng sng ngn (hnh
3.4).
53
3. Nng sut phn li.

Nng sut phn li (kh nng phn gii) ca mt my quang ph trong mt vng no
c biu th bng t s:
R = hay R = -
(3.6)
Trong 1 v 2 l di sng ca hai vch ph gn nhau m cn c th tch ra thnh

hai vch r rt trn hnh nh (mt phng tiu); A hay d l hiu s ca 1 v 2.
Hnh
Hnh
3.6b ln th hai vch ph c di
Nhng my quang
ph3.6a
c nng sut phn gii
R cng
sng 1 v 2 ny
cng
nmhai
xavch
nhau trn knh nh (hnh
3.5).
Tch
thnh
Khng
tch thnh hai vch
V vy, gi
nutrchn
ccbng
thngbao
s nhiu
trn cho
phvch
hp ph
khi ch
tolng
v tch
ch ra
tormy
Nhng
d phi
hai
1 v
c th
rt
2 cnknh
quang hai vchph
ta sknh
thunh?
cNghin
kh nng
phngii
mt
thnh
trn
cu vn
ny tt
v nht
t nhng ca
kt qu thc nghim
my
Rayley
nuquang
ra quyph.
tc: Hai tia sng c bc sng gn nhau i v 2 ch tch
Nhng ng knh ca thu knh bung nh li c tnh theo cng thc:
Fe3057,45
^2
ra c thnh hai vch
d
1 - n 2sin2( A /2)]
(3 8)
2=2 icc
(A/2)tiu
w
.
ph r rng, nu
Fe3059,l
sin( A / 2)
Trn my Q24
nhiu x th nht ca vch
b l chiu
cnh y ca lng knh.
ny trong
trng vi
cc dii
d
k2
nhiu Nh
x th
ca phn
vch gii ca my quang ph lng knh s l:
vy, nht
nng sut
kia. l khong cch ti
Trn my PGS-2
R = m.b.(dn/d)
(3.9)
thiu ca 2 vch ph (hnh
Ngoi
yu t ni, nng sut phn li ca mt my quang ph cn b nh hng
3.6).Trn
c nhng
s , nng
Hnh 3 5
bi mt
khc
nh:
sut
phnsliyu
cat
mt
my
cch ca hai vch ph trn cc my c nn
Tnhlng
chtknh
v
mnKhong
(c ht)
ca lp nh tng trn
knh
nh,
phtnh
c
ghicng
ln
quang ph
c
3 sut
Phn
giinu
khc
theo
knh nh. Vi yu t ny, nhng kt qu thc nghim cho thy rng, lp nh tng trn knh
thc:
nh cng nhy th nh hng cng nhiu n kh nng phn li ca vch ph. V nhng knh
my quang
ph cchlp
tnnh
sc gm
lng cc
knhht
nhAgBr
nhaubt
th nh
R t= sng c kch thc
nh cNu
nhy
cao thng
tngmcha
ln. Nhng trong nhng h thng
yu t ny hon ton c loi
mR i my mi ca th h th ba,
(3.7).
tr, v ph c ghi trc tip ln bng giy hoc o trc tip m khng phi ghi ln knh nh
Cng thc ny cho ta thy nng sut phn li ca mt my quang ph lng knh ph
na.
thuc vo nhiu yu t, nh:
Mt yu t na nh hng n nng sut phn li ca my quang ph l rng ca khe
+ S lng knh trong h tn sc (m);
my (khe vo ca chm sng). Ni chung, vic tng rng ca khe my s a n kt qu
lm gim
nng
sut
li ca
my
rng
+ Chit
sut
caphn
vt liu
lm
lngvknh
(n); ca khe my cng ln th rng ca vch
ph cng cng ln.
+ Sin ca 1/2 gc nh ca lng knh (A/2)
Nng sut phn li v rng khe my
+
ng
ca
knhmy
bung
nh (d
2); nhn chung ph thuc vo rng ca khe
Nng
sutknh
phn
li thu
ca mt
quang
ph
+ S bin thin ca chit sut theo bc sng (dn/d)
my. Khe my cng rng th nng sut phn li ca my cng gim. Nhng mi quan h ny l
khng n gin. V th chng ta c th xt trng hp c th sau y: Nu gi a l rng
ca khe my quang ph; f 1 v f2 l tiu c ca thu knh chun
54
55
trc v thu knh bung nh; d l ng knh ca cc thu knh th rng hnh hc ca
vch ph s c tnh theo cng thc sau:
a, = a.(2/fO
(3.10)
Trong ts f2/f c gi l phng ica my quang ph. Ni chung trong

cc my quang ph ngi ta c gng ch to t s ny bng 1. Nh vy, vch ph l nh
khng phng i ca khe my, ngha l a, = a. V cho vch ph r nt th s phn b cng
phi tha mn iu kin:
a, < 2s
(3.11a)
s = .(f2/d)
(3.11b)
trong
s l na
rng hnh hc ca cc
i th nht
ca vn nhiu x. Do trong
iu kin ti thiu ta phi c:

a, = 2(f2/d)
(3.12)
Hay t cng thc (3.10) v (3.12) chng ta c:

a = 2(f1/d)
(3.13)
Gi tr rng ca a theo cng thc (3.13) ny c gi l rng tiu chun ca khe my

quang ph v k hiu l ao, ngha l lc ny ta c:
ao = 2 (fl/d)
Nh vy rng tiu chun ao ph thuc vo:
di sng ca tia sng.
Tiu c f1 ca thu knh chun trc.
T l nghch vi ng knh d ca thu knh.
L thuyt v thc nghim chng minh rng rng tiu chun a o ca khe my, nng
sut phn gii ca mt my quang ph thc s ch bng 90 phn trm theo l thuyt. V th,
mun c nng sut phn gii cao ta phi m khe my nh hn ao mt cht (10%). Nhng
m khe my nh hn gi trao ta mt v cng vch ph,
khi
trong mt gii hnnht nh, th rng khe my quang ph v cng
vch ph l
t l nghch vi nhau. Bng 3.1 l vi v d v rng ca khe my quang ph pht x. Cho

nn tt nht vn l chn rng khe my ng bng a o hay ln hn mt t c v cng
trong phn tch nh lng.
56
Bng 3.1
Nu knh nh c t vung gc vi quang trc ca h thng thu knh bung nh th
rng
phkhe
s l:
Quan
hvch
rng
my v nng sut phn gii - cng vch ph
Khe my
s = a, +Cng
2X(f2/d)
vch ph (%) (3.16a)Nng sut phn gii (%)
v
50
0,50 ao
0,90 ao
s = 2Xv.(f2/)
75
98
(3.16b)
96
cho c hai trng hp nu trn, v trong trng hp ny sin E = 1.

0,95 ao
82
94
Cng vch ph v rng khe my
1,00 ao
90
90
Trong phn tch quang ph nh tnh v nh lng, c bit l phn tch hm lng vt
1,20 ao
95
80
ca cc nguyn t, mt yu cu quan trng l phi thu c vch ph c cng ln nht,
ao
98ngun pht x qua khe my quang
75
ngha l phi 1,50
bit c
s truyn nh sng t
ph n vt
thu cng 2,00
vchao
ph (knh nh, etector) l99nh th no.
60
Nu gi Io l cng ca chm sng pht x ca tia sng X th quang thng tng cng
2,20 ao
100
50
i vo h chun trc s l:
V khi khe my rng tiu
n chun th ch c cc i th_ nht ca vn nhiu x lt
2
0 = Q/o
4. (d
/ f1)cc
B.al
(3.17)
vo c h thng chun trc
cho =nn
trong
php phn tch
khng c chn khe my
nh hn rng tiu chun a o. Thng thng, theo kinh nghim thc t ngi ta hay chn khe
Hay l
my c rng t 1a o n 1,5ao l ph hp (phn tch T chn: 0,9 - 1a^ Phn tch L chn
t: 1,0 - 1,5ao).
OQ
rng ca vch ph
trongkhe
:my quang ph c rng l th rng ca vch ph bng rng hnh hc
Nu
ca khe
my
vi
x chnh
a v
l lcng
rng
v rng
chiuca
di vn
ca nhiu
khe my
quanggia,
ph; ngha l ta c:
B l huy ca chm sng c gc y l Q.
5 = a'+2 f
(3.14)
Khi chm sng Io i qua h quang
hcEca my quang ph th quang thng thc t tc
d .sin
dng ln
Nuknh
khenh
my(hay
rt vt
hp,thu)
th s
l:
rng ca vch ph ch l rng ca vn nhiu x chnh
gia, ngha l ta c:
= a.0 = a (d / f1)2 B.a.l
(3.18a)
(3.15)
d. sin kEB a 1
O' =a.kB.a.l ^ I = '
(3.18b)
aQ mt vch ph c lin quan trc tip rng
Hai biu thc trn cho thy, rng ca
o
my
y avlnng
h ssut
mtphn
mt gii
nngca
lng
chm
hph
quang
cathmy
quang
ca khe
myca
quang
ph.sng
Khiqua
vch
cnghc
rng
nng
sut
phn nh
gii thu
cng knh,
gim.lng
ngknh...
thi
rngtrng
vch ph
ph thuc
ph,
Trong
hpcn
l tng
th avo:
bng 1, cn mi trng hp
khc u
ln c
hn
1. thu
Quang
thng
O' ny
+ Tiu
ca
knh
bung
nh.s tc dng ln knh nh vi ri l:
+ T l nghch vi
ca hp nh.
0
E =ng
= -0-knh ca thu knh v sin gc nghing
(3.19a)
+ T l thun vi S
dia''sng ca vch ph, ngha l cc bc sng di th vch ph
tronghn,
Smc
l din
ca vch
phkhe
v ta
c:bng a.
cng rng
du tch
c cng
rng
sng
58
57
S = a,.l'
vi
a,= a.f2/(fi.sins) v l' = l.(f 2/fl)
Nn din tch ca vch ph s l:

S = a.l.(f2/fl)2.(l/sin s)
(3.19b)
Do , nu nh sng l n sc v b qua hin tng nhiu x, khc x, tn x, khi

chm sng Io qua h quang hc ca my quang ph th ri ca chm sng s l:
O' _ na d2
E = - = . \sins
S 4 (f2
(3.20)
v
'
y l trng hp l tng, n gin v gi tr ri E trong trng hp ny c k

hiu l Eo. Nh vy, chm sng Io tc dng ln knh nh to ra vch ph c cng l:
= E t ^4^ ( d / f,)2.t.sins
o
(3.21)
Ngha l nu vch ph hon ton n sc th cng IM ca vch ph t l vi bnh

phng khu t i ca thu knh bung nh v sin ca gc nghing ca hp nh s, cng
nh thi gian t m ri E o ca chm sng tc dng ln knh nh hay vo khe o ca nhn
quang in.
Trn y l trng hp n gin, nhng thc t th phc tp hn, v nh sng vo my
quang ph khng phi khng c cc hin tng nhiu x, tn x, cc sai st ca h thng
quang hc, l nhng yu t thc t khng th loi tr c hon ton. Chnh v th m vch
ph trn knh nh thng rng hn mt cht (10%) so vi trng hp tnh ton trn y.
Nu gi mt cch tng qut, Aa 1, Aa2, Aa3..., l rng do cc hin tng nhiu x, tn
x, tnh khng tuyt i n sc ca vch ph gy ra, th rng thc t ca vch ph phi l:
f
1
a' = .(a.^- + Aa1, Aa2, Aa3,...)
sins
/2
(3 22)
v ri thc t lc ny s l:
E = = anB (d / f2)2sins--------------------------------------
2
(3.23)
[a + ([, Aa2, Aa3...,)(f1/ /2)]
hay l:
E = E0T
(3.24)
59
Nh vy nu a >> (Aa1 + Aa2 + Aa3).(f1/f2) th chng ta li c E - Eo, ngha l tr

i trng hp c bit trn. Tc l cng vch ph khng ph thuc vo rng ca khe
sng. Cn tt c cc trng hp khc th rng ca vch ph t hoc nhiu u c b nh

hng bi rng ca khe sng. V cng vch ph trong cc trng hp lun lun phi
tnh theo cng thc:
I= E.t = E tT-------------------- a------------------
[a + ([ + Aa2 + Aa3).(/1 / /2)]
(3.25)
Cho nn khi khe my thay i th rng ca vch ph cng thay i theo. Nhng mi
quan h ny khng n iu v cng khng tuyn tnh. V vy, trong mt php phn tch b t
buc phi gi cho khe sng c rng khng i trong mt php o.
Mt khc, cng thc (3.23) v (3.25) cn cho th y, ngoi rng ca khe sng, cng
ca vch ph cn ph thuc vo c khu ca my quang ph , tc l t s d/f2. Cng
vch ph s ln, nu my quang ph c khu ln. Ngha l tiu c thu knh bung nh phi
nh. Nhng nu tiu c thu knh bung nh f2 nh, th li mt v tn sc di. Chnh v th
trong ch to my quang ph ngi ta phi tnh tm c gi tr khu sao cho ph hp
nht, nhm bo m c tn sc m cng ca vch ph cn ln c th o c v
pht hin c d dng.
Nu ly gi tr nghch o ca khu th ta c t s f2/d. T s ny gi l m ca thu
knh bung nh. Trong thc t khi ch to cc my quang ph ngi ta thng hay chn t s
ny c gi tr t 10 n 20. Tri li, khi m ln hn 20, vch ph c cng ln, nhng
tn sc ca my li qu km.
sng ca vch ph pht x
Nu ta pht hi n v o trc tip cng ca vch ph bng mt nhn quang in, th
sng ca vch ph l yu t quan trng. sng ca vch ph ph thuc vo cng ca
chm sng i vo my quang ph v cng ca chm sng sau khi qua my quang ph
vo nhn quang in. V th cu to, tnh cht ca h quang hc ca my u c nh hng n
sng ca vch ph. Mt cch gn ng v theo th c nghim, sng ca vch ph c th
c tnh theo cng thc:
L = (d2/f2)2
(3.26)
Trong d2 v f2 l ng knh v tiu c ca thu knh bung nh. Nh vy, sng

ca vch ph t l thun vi bnh phng ng knh ca thu knh bung nh d2 v t l
nghch vi bnh phng ca tiu c bung nh f2, ngha l ph thuc vo m ca thu knh
bung nh (t l f2/d2). Nu tiu c f2 cng ln th sng L ca vch ph cng gim, tc l mt
v cng v ngc li.
S quang hc mt s my quang ph lng knh
V d v cc s h quang hc ca mt s my quang ph pht x c ch ra trong
hnh 3.7.
60
s
e) My KC - 55 (Nga)
Hnh 3.7
S quang hc ca mt s my o ph pht x
P: Lng knh; G: Cch t; M, Mi, M 2: Cc h gng; L: Thu knh; E: Hp nh ghi ph;

T: Khe sng; S: Ngun pht x.
Cch t v my quang ph cch t
Gii thiu v cch t

Cch t l h gm nhiu khe hp (vch) song song vi nhau v cch u nhau.
Mi khe nh l mt chn sng, cn ch khng c vch nh l mt khe sng. Cch t c
tc dng phn li nh sng nh lng knh. Nhng bn cht s phn li nh sng cch t khc
lng knh. S phn li nh sng ca cch t l do hin tng nhiu
61
x ca chm sng qua khe hp. Khi s phn li nh sng ca lng knh l theo hin tng khc x
ca nh sng qua hai mi trng c chit sut khc nhau. Cch t c hai loi:
Cch t phn x v 2. Cch t truyn x.
ch to my quang ph ngi ta thng dng cch t phn x, v dng cch t truyn x s b
mt nhiu nng lng khi chm sng i qua cch t.
Trong mi loi trn li c cch t phng v cch t lm. T thc t chng ta s ch cp n
cu to v bn cht ca cch t phn x l chnh (hnh 3.8a v 3.8b).
Hnh 3.8a
Hnh 3.8b
Dch t phng
Cch t lm phn
x
Cc i lng c trng cho mt cch t l hai thng s chnh sau y:

Chu k ca cch t: L khong cch gia hai vch trn cch t v c k hiu l d (hnh 3.8a).
Hng s cacch t: L s vch trn mt n v
hiu l k, tc l s vch c
khc trn
di ca cch t v c k
1 mm.
Nh vy, gia chu k v hng s ca cch t lin quan vi nhau theo biu thc: d. k = 1
(3.27)
Nu gi L l chiu di ca cch t, th tng s vch trn mt cch t s l:
N = k. L
(3.28)
V cu to th cch t phn x gm c hai phn. l b v mt cch t. B l tm thu

tinh hay thch anh dy t 1,5 n 2 cm, c hai mt song song vi nhau v thng c din tch t 4 x 4 hay
4 x 6 n
x 12cm. Mt cch t l lp kim loi nhm (Al) tinh khit (99,999 %) v dy t 0,2 - 0,5 mm.
Lp kim loi ny c a ln b bng con ng in phn c bit trong mi trng tr. Mt lp kim
loi nhn bng v c khc ln nhiu vch song song v cch u nhau. S vch c khc ln lp
kim loi ny thng l t 650 - 3600 vch/mm. S vch trn 1 mm cng nhiu th kh nng phn li nh
sng ca cch t cng ln.
62
Nh th, nu chng ta chiu mt chm sng song song khng n sc vo mt cch t

theo mt gc ti a no th ch c vch trn cch t nh mt chn sng, ch khng c vch
nh mt khe sng v di tc dng ca hin tng nhiu x trn b mt cch t th chm sng
a sc s c phn li thnh ph. Nu gi p l gc l ca tia sng, di sng l X th ta lun
lun c biu thc:
sina + swinp = m.k.X
(3.29)
Biu thc ny c gi l cng thc c bn ca cch t. Cng thc ny gii thch cho ta
nguyn nhn s tn sc ca cch t, v t cng thc (3.29) ta c:
sinp = m.k.X + sina
(3.30)
y a l gc ti ca chm sng, m v k l khng i i vi mt cch t. Nn ng vi

mi bc sng X ta s c mt gi tr sinp tc l c 1 gi tr p. iu c ngha l cch t
phn li chm sng a sc thnh tng tia n sc lch i theo tng gc 13 khc nhau. Nhng
y sng di b lch nhiu, cn sng ngn b lch t hn. ng thi cch t cho ta ph c
nhiu bc, ng vi cc gi tr m ca cng mt di sng X S m c gi l bc ca ph
cch t.
Nu tia ti vung gc vi mt cch t, tc l gc ti a - 0 th cng thc (3.30) s c
dng l:
sinp = m.k.X
(3.31)
Trong trng hp ny gc phn x ca cc tia sng khng ph thuc vo gc ti a m

ch ph thuc vo hng s k ca cch t v di sng ca tia sng m thi. Trong thc t
ngi ta hay t cch t v tr ny trong my quang ph.
Nu gc ti a= 13 th cng thc (3.30) s l:
sinp = (mk/2).X
(3.32)
y chnh l tia sng X c gc ti a tc dng ng vo gia knh nh ca mt vng ph

ca hp nh. V th cng thc ny c s dng
tnhgc ti a khi chn
vng ph cho mt php phn tch. cng l v tr cc tiu
ca tia sng trung tnm ca
vng ph cn chn trong my.

Mt khc, cng chnh do hin tng nhiu x qua khe hp to ra ph ca cch t cho
nn khong cch t v tr cc i cc vn sng n tnm hnh nhiu x c tnh theo cng
thc:
xt = m.f 0.(X/k)
(3.33)
ngha l:
Cc i th 1 cch tnm mt on x t1 = (1.f2,X)/k
Cc i th 2 cch tnm mt on x t2 = (2.f2.X )/k
63
Cc i th 3 cch tnm mt on x t3 = (3.f2)/k
Cc i th m cch tnm mt on x tm = (m.f2)/k.

iu ny gii thch cho ta ti sao tn sc di ca cch t bc th m gp m ln bc
th 1, ngha l c tn sc bc th m l:
DDM = m
(3.34)
m
Vi m l s nguyn v m > 1.
My quang ph cch t
My quang ph cch t, v nguyn tc, cng c cu to nh my quang ph lng knh.
Nhng y h tn sc l mt cch t, v cng dng ba i lng c trng nh trong my
quang ph lng knh nh gi cht lng ca mt my quang ph cch t. C th l:
tn sc gc
T cng thc c bn ca cch t (3.29), nu xt s bin thin ca gc lch p theo di
sng X th ta c:
cosp.dp = (m.k).dX
hay l:
Dg =
DX cos p
<3-35)
Biu thc ny chnh l cng thc tnh tn sc gc ca my quang ph cch t.

Nh vy, tn sc gc ca mt my quang ph cch t s:
+ T l thun vi hng s k ca cch t v bc m ca ph cch t.
+ T l nghch vi cos ca gc phn x p.
Ngha l mt cch t th vi cc bc ph cng cao tn sc gc ca my cng ln.
V d:
v.v...
Mt cch tng qut, ngha l tn sc bc m th ln gp m ln tn sc gc bc
1:
64
mg
=L
m
g
Nhng cc bc ph ca cch t li xut hin ng thi, ph ca cc bc cng cao th cng cng

yu. Gn n 70% nng lng l tp trung bc 1 (vn nhiu x th nht). Chnh v th khi ghi ph phi
dng knh lc ph hp loi b nhng bc ph khng cn thit. Cho nn tnh cht a bc ca ph cch t
va l u im, nhng cng va l nhc im ca my quang ph cch t, v ph ca cc bc cao ta
c v tn sc,
ngi ta ch
nhngli mt vcng . Nn trong
dng
ph bc
thc t,
1,
hay i khi n bc 2 m thi.

tn sc di
i vi
my quang ph
cch t,
ngi ta cng
gi t s dl/d, l tn sc
di
ca n v c tnh theo cng thc:
= ^ m.k. f2
d cos J 3
(3.36)
v
'
Nh vy, tn sc di ca my quang ph cch t t l thun vi tn sc gc ca n v tiu c f 2

ca h bung nh. Hay ni mt cch khc, tn sc di l:
T l thun vi hng s ca cch t, tiu c ca bung nh, v s bc ca ph cch t, v
Thay i trong quan h t l nghch vi cos ca gc phn x ca tia sng. V d t cng thc trn
chng ta c:
+ Nu m =
1 th dp/d, =
(1 .k.f2)/cosP;
+ Nu m =
2 th dp/d, =
(2.k.f2)/cosP;
+ Nu m =
3 th dp/d, =
(3.k.f2)/cosP;
Ngha l di
tn sc bc th m th
cnggp m ln tn sc di
bc 1
(cng thc 3.34).

Nhng trong thc t, d so snh, ngi ta cng dng gi tr nghch o ca i lng ni trn,
nh quy c trong my quang ph lng knh. Nh vy chng ta s c:
= -co^
mk f
dm
.2
(3.37)
Cng thc (3.37) ny l tn sc di nghch o ca my quang ph cch t bc th m v ti

im chnh gia ca vng ph. Cn tn sc di ti mt im X no cch tnm knh nh mt khong x
s c tnh theo cng thc:
dm = dm 0,00016.103x
(3.38)
65
T biu
ny tanhau
thymt
tn
di ca
quang
cch
t hutng
nh vch
ph thuc
vch ph
X1 vthc
X2 khc
gi sc
tr X
sau my
y s
cph
phn
li thnh
ring
rt
t
vo
di
sng
ca
tia
sng
(bng
3.2).
Cng
thc
trn
nhn
du
(-)
khi
i
t
tnm
knh
bit:
nh theo chiu di sng tng dn v nhn du (+) theo chiu ngc li.
Nu m = 1, ta s c X = 0,02 ,
Bng 3.2
Nu m = 2, ta s c X = 0,01 ,
So snh tn sc ca hai my
Nu m = 4, ta s c X = 0,005 ,
Vng ph ()
tn sc di nghch o trong my
Ngha l bc m=1, hai vch X 1 v X2 mun tch thnh hai vch r rng th phi khc
Lng
knhny
q 24
nhau mt gi tr di sng ti Cch
thiu t
l PGS-2,
0,02 . bc
Khi1 bc 2, hai
vch
ch cn khc
nhau mt gi tr 2000
X = 0,01 l tch
thnh
hai vch ring bit. Nhng
7,390
/mm
4,00 trong
/mmthc t ngi
ta t dng ph bc cao ca cch t. Ngi ta thng hay dng ph bc I v bc II, v n 70%
2500
- nhng cch t
nng lng l tp
trung bc I. Cho nn7,380
trong- thc t hin nay ngi ta7,80
dng
c hng s k rt3000
ln (k:2400-3600) ch
to- nhng my quang ph c
kh-nng phn gii
7,370
13,00
cao. Hnh 3.1a, b l s quang hc ca mt s k my ph cch t.
7,356 18,00 Vng lm vic ca3500
my quang ph
y cng l
mt ai lng nh7,340
gi mt
4000
- my quang ph.
31,00 -
Do tnh cht quang hc ca vt liu dng ch to h tn sc l trong sut v ng

nht trong mt min nht nh, nn mi my quang ph ch c th thu, phn li v ghi nhn
3. Nng
sutsng
phn nht
gii nh ca ton b gii ph quang hc. Vng ph ny c gi l
c mt
vng
Nng
sutca
phn
R ca
mtph.
myVng
quangph
phlm
cch
t c
nhquang
ngha ph
nh lng
sau: knh l
vng lm
vic
mtgii
my
quang
vic
ca my
do trong sut v tnh cht ca vt liu lm lng knh quyt nh v ph thuc vo cch b
tr (cu to) ca my quang ph y. V d: Cc my quang ph lng knh thch anh thng c
d
vng ph lm vic l min t ngoi gn (2000-4000 ). Cc my quang ph lng knh thu
tinh cVi
vng
l1),min
kh2 -kin
(36007800
), theo
v thch
chsau:
trong sut trong vng
dXlm
= (Xvic
X = (X
1)/2
v c tnh
cnganh
thc
2 -
t ngoi; cn thy tinh ti trong sut trong vng kh kin (nhn thy). My quang ph cch t
R=xd
thng c vng lm vic rng hn my quang
ph lng knh. Vng lm vic ca mt my
quang ph cch t l cu to, tnh cht, ddi
p dsng
X blanz Xb) v s bc ca cch t quyt
nh. Ni chung, my quang ph cch t thng c vng lm vic rng hn my quang ph
hay l
lng knh.
R = m.k.L
V d: Vi my quang ph cch t PGS-2 lp cch t c k:650 v Xb = 2700 , c
Nhvic
vy,l:
rrng
sut- 7800
phn
gii
my
vng lm
bc nng
1: 2000
vmt
bc
2: quang
2000 - ph
4000cch
...t t l thun vi:
Hngvy,
s kvi
camy
cchcch
t, ngha
k lnlm
th
Nh
t thlvng
victn sc
bc ln
ph th m hp hn bc 1 l m ln,
ngha l
chng
lun
lun
Chiu
ditaca
cch
t c:
L, v
X
X
m =th
S bc ph ca cch t, m. Bc ph
cao
1/m
phn gii cao.
Do ,lm mun
tng
nng
phn
mtcht
my
quang
ph
phi
s
Vng
vic ca
mtkh
my
quang
phgii
c linca
quan
ch
n
dicch
ca t
c di
ph
dng
cchCc
t c
hng
lnsc
vcng
chiuln
dith
L ln.
Nhng
vic
tng
di LVch
m nnhng
thu c.
my
c s
ktn
di
ca di
ph
chiu
cng ln.
thc
gii hn
(diquang
nht l
15ccm).
Nnsc
chln,
yuvi
l mt
tng tm
hngknh
s knh
caccch t, ngha l phi ch to
nhng
my
ph
tn
nhng cch t c nhiu vch trn 1 mm di. ng thi phi s dng ph nhng bc cao,
nh bc m=2. Song cc bc cao ca ph th cng vch ph li
Vd: ng vicch
66
tc k
bng
nh.
1800, th trong vng sng 3000 hai

67
di nht nh (v d 24 hay 30 cm), chng ta ch c th ghi c mt phn ca vng ph

lm vic ca my . T thc t , trong cc my quang ph c tn sc ln ngi ta phi
c b phn
quay cch t
hng phn ph
cn nghin
cu
vo knh
nh, ngha l vng ph lm vic ca my cn phi c ghi ln nhiu tm knh. V d: Vi
my Q 24 vng ph lm vic ca n ch cn ghi trn mt tm knh nh di 24 cm. Khi
vng ph ny my PGS-2 ta phi cn hai tm knh 24 cm mi c th ghi ht c vi ph
bc I.
Trang b ca h thng my quang ph pht x
T nhng nghin cu c cp trn, chng ta c th minh ha tm tt trang b

ca mt h thng my quang ph pht x gm nhng phn sau y:
Trang b chnh, c bn ti thiu: Gm ba phn
Ngun cung cp nng lng ha hi mu, nguyn t ha v kch thch m hi

pht x. l ngn la n kh, h quang in, tia la in, ICP.
My quang ph c nhim v thu, phn li v ghi li vng ph cn nghin cu.
Nh cc my quang ph lng knh Q-24, ISP-28, ISP-30, KSAI,... v cc my cch t
PGS-2, D0-3, D0-13.
Cc trang b nh gi nh tnh (my chiu ph) v nh lng (my o en).
H trang b hon chnh, c thm:
+ B phn t ng dn mu vo bung o, pha long t ng.

+ H my tnh v phn chng trnh iu khin, x l kt qu o.
Trang b ph thm, Cn c:
+ H thng chiu sng khe my quang ph. N l mt h thng thu knh hi t v

hng chm sng pht x ca mu phn tch vo my quang ph vi hiu sut cao v ph hp
cho tng mc ch phn tch.
+ Cc lc sng v chn sng c nhim v chn v a vng ph cn thit vo khe my
quang ph cng v phm vi nht nh theo yu cu ca php phn tch.
Tt nhin cc th ph tr ny c th khng c cng c.
Trang b pht hin v thu nhn ph
Cho n nay, thu nhn ph pht x ca vt mu c hai loi trang b. l loi:

Knh nh hay phim nh (k thut c in) v 2. Cc loi nhn quang in kiu ng
(photomultiplier tube detector), hin nay l cc mng git (diode array).
Knh nh quang ph
Knh nh quang ph c nhiu loi, nhng v cu to, n gm hai phn: Phn v phn
lp nh tng bt nh sng. l tm thy tinh trong sut v ng nht, c dy u n,
thng t 1 n 2 mm, din tch 6 x 12 cm, 9 X 24 cm hay 9 x 30 cm.
68
Lp nh tng bt nh sn l lp glatin c dy t 0,1 n 0,05 mm, nhng phi ng nht v u n

trn mt tm thy tinh. Lp glatin ny c cha cc ht AgBr mn. nhy ca knh nh ph thuc vo
cc ht AgBr trong lp glatin ny. nhy l mt thng s c trng cho mi loi knh nh v mi loi
knh nh cng ch nhy trong mt vng ph nht nh (hnh 3.9). c trng ny do qu trnh sn xut quyt
nh, theo loi nguyn vt liu v thnh phn ca chng, cng nh iu kin ch to knh nh. V th mi
loi c nhy khc nhau trong cc vng ph khc nhau.
10
12
xiooo
Hnh 3.9
nhy ph ca cc loi knh nh
(1): Vng 1800-4000 , (2): Vng 3600-7800 v (3): Vng 7000-10000 .
Thng thng knh nh c nhy cao thng c nh hng n phn gii ca vch ph, v cc
knh nh nhy chng c ht AgBr kch thch ln. Do , tng nhy ca knh nh ngi ta thng
thm vo mt cht kch hot quang hc, vn dng lp nh tng c ht AgBr kch thc nh m knh
nh t c nhy cao.
Khi ta chiu chm sng cng I ln tm knh nh th ch b nh sng tc dng vo s ha en.
Nu gi en ti im b nh sng tc dng vo l S, th ta c:.
S = ylog I
y Y l h s nh tng (tng phn) ca knh nh, v chnh cu to v bn cht ca lp glatin
quyt nh h s nh tng Y. H s Y ny cng ph thuc vo di sng X ca vch ph, nhng rt
khc nhau trong mi vng ph (hnh 3.10a). Khi b nh sng tc dng th c mt lng t sng hv s gii
phng ra mt ht Ag kim loi theo phn ng sau:
AgBr + hv = Ago + Br
Cc ht Ag nguyn t t do ny nm n tng trong lp glatin ta cha nhn thy.
V th, mun c nh thc v gi li c chng ta phi x l knh nh c nh sng tc dng
qua dung dch hin hnh v dung dch nh hnh. Sau y l thnh phn ca cc dung dch .
69
Dung dch hin v dung dch hm knh nh

Dung dch hin hnh
Dung dch nh hnh
Mentol: 1g.
Natri thiosunphat: 250g.
Natri sunfit khan: 26g.
Hydroqu Ione: 5g.
CH3COOH 99%: 8,5 mm.
Pha trong mt lt.
t(gy)
to
Hnh 3.10a
Hnh 3.10b
3 ph thuc ca h s Y v X.
Quan h gia en s v thi gian hin t.
Ngoi nhy, thi gian chiu sng cng l yu t quan trng nh hng n en ca
vch ph. Ni chung, chiu sng cng lu th en cng ln. Song, tt nhin cng ch trong
mt thi gian nht nh ph hp. Cn nhiu hn na th ch lm gim phn gii ca vch
ph, v thi gian qu di s lm m rng chiu ngang ca vch ph m khng lm tng
en S vch ph.
Thi gian hin cng nh hng n cng vch ph. Mi quan h ny c thy trong
hnh 3.10b.
Ni chung, vi nhiu loi knh nh, thi gian hin ph hp l t 2 n 4 pht v thi
gian hm (nh hnh) l t 4 n 8 pht. Nhit thch hp l t 18 n 20 0C.
o en Sx ca vch ph trn knh nh
Nu chiu chm sng cng I o vo knh nh th ch c vch ph v khng c vch

ph, chm sng i qua s c cng l I v Io. Do en ca vch ph s l:
S = log(Io/I)
h a y S = log(ao/a)
Trong ao v a l lch ca in k ng vi chm sng cng I o v I. Do ,
thang o en S ch c gi tr t 0 - 2. Nhng vng en va phi (vng m mi quan h
gia S v C l tuyn tnh) ch nm trong khong t 0,3 - 1,7 (hnh 3.11). Cn khi S nh hn
0,3 l vng non, khi S ln hn 1,7 l vng gi. Trong 2 vng ny kt qu o l khng chnh
xc. V th phi chn iu kin ghi ph ph hp en
70
ca vch cn o ri vo vng tuyn tnh (0,3 - l,7).

Nhng
lng
vt
trong
th
phn
en
ca
tch
vch
ph li c th nh hn 0,3 n v
S. V th ngi ta m rng
thang o en S v pha cng
nh. y c
en
ca
vch
cch bin i
ph, v tng
ng n l hai thang o mi W v
P.
vch
Theo
thang
ph
tnh
th
theo
en
cng
thc:
W = log.( ^ -1)
a
V theo thang P th en vch ph li c tnh theo cng thc:
S + W P =
Do thc t nn hin nay cc my o en u c c ba thang o en S, W v P. Vi thang

W en c th m rng c n 0,1. Cn vi thang P th c th n gi tr -0,3 n v S. V th trong
phn tch lng vt ngi ta hay dng thang P. Tt nhin t cc gi tr ca P ngi ta cng d dng tm
c cc gi tr ca S hay W tng ng, nh mt bng chuyn i en c sn (xem ph lc).
ng nhn quang in (Photomultiplier tubes)
Trong cc my quang ph hin nay, ngi ta c th pht hin v o trc tip cng ca cc vch
ph bng cc nhn quang in, m khng cn ghi ph ln knh nh. Do loi tr c sai s do knh nh
gy ra.
Nhn quang in kiu ng hay detector tubes l mt loi dng c quang hc thu nhn v pht
hin tn hiu quang hc (tc l o cng chm sng) theo hiu ng quang in ca n. Vi s pht trin
ca khoa hc v k thut, ngy nay ngi ta ch to c nhiu loi nhn quang in kiu ng
(photomultiplier tubes) thu nhn tn hiu quang hc v khuch i ln hng ngn, n hng triu ln,
lm cho cc my quang ph c th phn tch c nhiu nguyn t nng rt nh (t ^g n ng). Hnh
3.12 l s nguyn tc cu to ca nhn quang in v vng ph lm vic ca n. Nhn quang in l
mt dng c vn nng thu nhn tn hiu quang hc. N c nhy v chn lc cao. Vng ph lm
vic ca nhiu loi nhn quang in thng l t 190 n 900 nm, cho vng ph t ngoi v kh kin. Tt
nhin, vng ph
71
lm vic ca mt loi nhn quang in ph thuc vo bn cht kim loi dng ch to bn catot ca nhn
quang in (hnh 3.12). Cc kim loi ch to catot ca nhn quang in kiu ny thng l Na-Cs-K-LiSb. H s khuch i ca cc nhn quang in thng l t 10+ 5 n 10 +6, i khi c th n 10+ 7 ln.
72
73
X,
Hnh 3.14
Mt on ph ghi trn bng giy
Ph ICP-AES ca AI, Cr, Fe, Ni (200 ppm) ghi trn giy)
74
Chng 4
CC YU T NH HNG TRONG AES
Khi qut chung

Cc yu t nh hng n kt qu phn tch trong php o ph pht x nguyn t l rt a dng v
phc tp, c khi xut hin v cng c khi khng xut hin, c nh hng hay khng c l ty thuc vo
thnh phn ca mu phn tch v cht nn (matrix). Nhng nghin cu mt cch ton din, chng ta
im qua tt c cc yu t nh hng c th c trong php o ny. Cc yu t c th c chia thnh
nhm nh sau:
Nhm 1. Cc thng s ca h my o ph.
Cc thng s
ny cn c kho st
v chn cho tng trng hp c th. Thc hincng vic ny chnh l qu trnh ti
ha cc thng s ca my o cho mt i tng phn tch.

Nhm 2. Cc iu kin ha hi, nguyn t ha mu v kch thch ph. Cc yu t ny th hin rt
khc nhau ty thuc vo k thut c chn thc hin qu trnh ha hi, nguyn t ha, kch thch ph
v n c nghin cu k trong chng 2 .
Nhm 3. K thut v phng php c chn x l mu. Trong cng vic ny nu lm khng cn
thn s c th lm mt hay lm nhim bn thm nguyn t phn tch vo mu. Do kt qu phn tch thu
c s khng ng vi thc t ca mu. V th, vi mi mt loi mu ta phi nghin cu v phi chn
mt quy trnh x l ph hp nht, c c ng thnh phn ca mu v khng lm nhim bn mu. Vn
ny s c nghin cu trong mt chng ring.
Nhm 6 . Cc yu t ha hc.
Trong chng ny chng ta s nghin cu k cc yu t thuc cc nhm 4, 5 v 6 .
Mt s nh hng trong php o AES
Cc yu t v ph
S pht x ph nn
Yu t ny c trng hp xut hin r rng, nhng cng nhiu trng hp khng xut hin. iu
ny ph thuc vo vng ph v vch ph c chn o nm trong vng ph no. Ni chung, trong vng
kh kin th yu t ny th hin r rng, cn trong vng t ngoi nh hng ny t xut hin, v ph nn
trong vng t ngoi thng yu. Hn na, s pht x nn cn ph thuc rt nhiu vo thnh phn ca mu
phn
75
tch, c
bit
l matrix ca mu,
ngha l nguyn t c
s ca
mu,
v ngun nng
lng kch thch ph.

V d: Khi xc nh
Pb
trong
mu
sinh
hc
bng php o ngn la th

s
hp
th
ng
k.
nh
Pb
(nn
2,9%
nn
Nhng
trong
khng
khi
xc
nc
bin
NaCl)
I)x
th
nh
hng ny li l v cng
ln
bt
buc
phi
bo
chnh
loi
tr
(hnh
4.1).
Do
trong
mi
th
phi
trng
hp
xem xt tm bin loi

tr. loi
ngy
nay
thm
vo
nguyn
chnh
t
nn.
(nm)
tr ph nn,
ngi
ta
lp
my
quang
ph
thng
Hoc
vo
Hnh 4.1
nh hng ca s pht x ph nn a)
Khng b chnh nn; b) C b chnh nn
mu cc cht lm gim s
pht x nn.
S chen ln ca cc vch ph gn nhau

Yu t ny thng thy khi cc nguyn t th ba trong mu phn tch c nng ln v
thng l nguyn t c s ca mu. Tuy nguyn t ny c cc vch ph khng nhy, nhng do nng
ln, nn cc vch ny vn xut hin vi rng ln, nu n li nm cnh cc vch phn tch (bng 4.1), th
cc vch ph ny s chen ln cc vch phn tch, lm cho vic o cng vch ph phn tch rt kh
khn v thiu chnh xc, nht l i vi cc my c phn gii khng cao. V th trong mi mc ch
phn tch c th cn phi nghin cu v chn nhng vch phn tch ph hp loi tr s chen ln ca cc
vch ph ca nguyn t khc. Nu bng cch ny m khng loi tr c nh hng th bt buc phi tch
b bt nguyn t c vch ph chen ln ra khi mu phn tch trong mt chng mc nht nh, cc vch
chen ln khng xut hin na. Tt nhin vic ny l hn hu.
76
F(ml/ph)
Nhng
nu onh
vch ph
Ion th yu
t ny li l cn thit v ta phi chn iu kin qu trnh Ion
Bng 4.1
o
v
xc
theo
S
lnphp
v
s cao
trng
ca
cc nguyn
t nng ln ca nguyn t cn xc nh (phn tch) cao
phng
thm
tiunht,
hachen
t hiu
sut
vvch
n nh
c c
chun,
nht.
Nguyn t c vch chen ln

Nguyn t v vch phn tch
Pha
long
mu
Thc t cho thy rng, qu trnh Ion ha thng ch c ngha i vi cc kim loi kim v sau
(nm)
bng mt dung mi hay
l cc kim loi kim th, cn i vi cc nguyn t khc s Ion ha l khng ng k trong mi trng ca
Vch chen ln
Nng xut hin nguyn t chen ln
mt nn ph hp,
ngn la n kh v h quang in. loi tr s Ion ha mt nguyn t phn tch chng ta c th dng
(ppm)
Thm
vo
mu
cht
cc bin php sau y:
m cAl-308,215
nng ln,
V- 308,211
>800
+ Chn iu kin nguyn t ha c nhit thp, m trong iu kin nguyn t phn tch hu
Dng Cu-324,754
bm
y TI
Eu-324,753
>254
nh khng b Ion ha.
2
4
6
8
10
mu vi mt tc xc
Fe-271,903
Pt-271,904
>054
Hnh
4.2
Thmchng
vo mu
tch mt
cht
m cho s Ion ha. l cc mui halogen ca cc kim loi
nh +m
ta phn
mong
Pr-411,848
Fe-411,854
>050
ca nht n tc dn mu
kim c th Ion ha thp hn th Ionnh
hahng
ca nguyn
t phn tch vi mt nng ln ph hp. Nh vy
mun.
Mn-403,307
Ga-403,298
trong S
iu
kin
ca
nguyn
phntch
tch s khng
b Ion ha na.
Ion
ha
chttphn
>025
>200
Zn-213,856
Hin
t o
(tha
hpca
th)nguyn
caFe-213,850
vch
phng
Nu
otng
vch ph
trung
t, y
l yu t vt l th ba nh hng n kt qu phn
tch, vHin
qu trnh
ha
lm gim
nguyn
t do
ca nguyn
t phn
do hay
lmkhi
gim
cng
tngIon
ny
thng
xuts
hin
trongtvng
ngoi
ca plasma
l rtch,
rt nht
nng
cht
vch
pht
x ca nguyn
trung
t phn
tchcht
b Ion
hatch
cng
phn ph
tch
ln. V
nyca
c t
nhit
ha,
thp,khi
nnnguyn
cc nguyn
t ca
phn
li nhiu.
hp thNhng
chnh mc
tia pht
4.2.1:3
Svng
bc x
cc ht
rn
b Ion ha ca mi nguyn t l khc nhau, v ph thuc vo nhit ca mi trng pht x. Trong mt
x m Trong
cc nguyn
t trong
sinhngn
ra, vla
thn
lmkh,
mth
btquang,
i mtnhiu
phnkhi
cng
mi trng
pht li
x,ca
cngn
bit lla
trong
cn
c pht
cha x
c ca
cc
iu kin nht nh, ni chung cc nguyn t c th Ion ha cng thp th cng b Ion ha nhiu. Vi mt
ht
rt tch.
nh liiu
ti ca
vtcng
cht gp
muphn
cha gii
b ha
hiti
vsao
nguyn
t ha,
hayth
ccmi
ht quan
muih
cacbon
ca nhin
chtrn
phn
ny
thch
nng
ln
gia cng
nguyn t, khi nhit ca mi trng pht x cng cao th nguyn t cng b Ion ha nhiu hn. Bng
liu
cxt
chy
hon
htlloi
nycn
thng
lp
vchcha
ph pht
I^v
nng
ton.
Cx caCc
cht
khng
tuync
tnh
na.v ca ngn la v n cng b kch
4.2 l mt v d v iu ny.
thch pht x ra ph nn, do cng gy kh khn cho vic quan st hay o cng vch ph phn tch.
Trn y l mt s yu t vt l c th xut hin trong php o AES v c th nh hng n kt qu
Bng
Yu t4.2
ny th hin rt r khi chn khng ng chiu cao ca n nguyn t ha mu v cc iu kin ca
phn tch. Nhng mc xy ra l rt khc nhau trong mi trng hp c th, c khi c, c khi khng.
ngunkch
phmt
khng
ph hp.
Mc
Ion thch
ha ca
s nguyn
t
Mc ny xut hin ln hay nh ph thuc vo:
Cc yu t vt l
+ Nhitvloi
cayu
plasma,
Thuc
t vt l ny thng c:
nht
vkin
sc ca
cng
btrng
mt ca
dung
+ Cc
iu
mi
kch
thchdch
phmu
pht x,
Th Ionhay
ha(eV)
Smu
% btrong
Ion ha
nhitnu
mu
(oC): l dung dch,
TrongN.t
php o ICP-AES,
vi k thut nguyn t ha
ngn la,
+ Tnh cht ca nguyn t phn tch v hp cht ca n,
yu t ny nh hng nhiu n tc dn mu vo bung aerosol ha v hiu sut aerosol ha ca mu
2000
3000
4000nng
+ Cht
nnhng
ca mu
thnh
tch.tc dn ng
v t
m nh
nvkt
qu phn
phnca
tch.mu
Niphn
chung,
chun phi c cng
axit, loi
v thnh
phnxt
ha
ca tt
ctr
cc00,30
nguyn
khc,
nht
l cht
mu.
Yu t
5,21
05,00
Doaxit
Nacn
phi xem
hc,
tm vt
binl php
loi
khi
chngtxut
hin,
theo
tngnn
loica
mu26,00
c th.
ny thng th hin nhiu trong php o AES dng ngun ngn la v h quang in. loi tr nh
02,10
22,00
Cc yu t ha
K hc
4,32
82,00
hng ny chng ta c th dng cc bin php sau y:
TrongRb
php
onhau
ph pht
x nguyn
ccaxit,
nh nng
hng
a thnh
dng v
phc
tp.
4,16
09,00
34,00
Chnh
s
khc
v nng
axit,tloi
ha
chthc
nncng
ca rt
mu,
phn
ca90,00
ccN
chtxut
c
hin cng
khc nhau trong nhn
mi trng
hp c
th v
v
cng
nhiu
hp khng xut hin. mi
Cc nh
trong
dungrt
dch
gy ra khc
nhau
nht
ca trng
dung dch
Cs mu, nguyn 3,87
28,00
70,00mu. V th trong
96,00 qu
hngphn
ha tch
hc mt
thng
c th
n
ktphi
qu m bo sao cho mu phn tch v cc mu u lpmu t l
trnh
nguyn
t,dn
nht
thit
00,12
Mg
7,54
00,50
05,60
nghch vi nht ca dung dch mu (hnh 4.2)..
78
Ca
6,11
00,20
01,50
15,00
Sr
5,69
00,50
02,35
18,70
Ba
5,31
01,00
06,00
23,00
79
77
theo bn hng sau y:

Lm gim cng ca vch ph ca nguyn t phn tch, do s to thnh cc hp cht bn nhit,
kh ha hi v kh nguyn t ha. V d nh nh hng ca cc Ion silicat, sunfat, photphat, florua.
Lm tng cng ca vch ph, do s to thnh cc hp cht d ha hi v d nguyn t ha, hay
do hn ch c nh hng ca s Ion ha ca nguyn t phn tch. chnh l tc dng ca mt s hp
cht, ch yu l mui halogen ca kim loi kim v kim th hay lantan Clorua.
S tng cng vch ph khi nguyn t phn tch tn ti trong nn ca mu l nhng hp cht d
ha hi. Lc cc cht nn ny c tc dng nh l mt cht mang cho s ha hi ca nguyn t phn tch
v lm n c ha hi vi hiu sut cao hn. S gim cng ca vch ph khi nguyn t phn tch tn
ti trong nn mu l nhng hp cht bn nhit, kh ha hi. Lc ny cc nguyn t nn km hm s ha
hi ca nguyn t phn tch. Cc cht nn ny thng l nhng hp cht bn nhit ca cc nguyn t, nh
Al, t him, silicat, v.v...
V th vic nghin cu cc nh hng ha hc c trnh by trong chng ny c tnh cht khi
qut chung tt c cc loi c th c chng ta lu khi ng dng php o ph pht x nguyn t, vi
mc ch bit v loi tr cc nh hng ha hc, nu chng xut hin. Cc nh hng ha hc c th
c sp xp theo cc loi sau y:
Nng axit v loi axit trong dung dch mu

Ni chung nng axit trong dung dch mu lun lun c nh hng n cng ca vch ph
ca nguyn t phn tch v nh hng ny thng gn lin vi loi Anion ca axit. Cc axit cng kh bay
hi thng cng lm gim nhiu cng vch ph. Ngc li, cc axit d bay hi gy nh hng nh
(hnh 4.3). iu ny c th thy r rng khi xc nh Ca o vch ph Ca-422,7 nm trong cc mi trng
ca cc axit HClO4, CH3COOH, HCl, HNO3, H2SO4, H3PO4, HF vi cng mt nng l 2 % (hnh
4.4).
Ni chung, cc axit lm gim cng vch ph theo th t: HClO 4 < HCl < HNO3 < H2SO4 <
H3PO4 < HF, ngha l axit HClO4, HCl v HNO3 gy nh hng nh nht. Chnh v th trong thc t phn
tch ca php o ph pht x nguyn t (AES) ngi ta thng dng mi trng l axit HCl hai HNO 3 1
hay 2%, v nng ny nh hng ca hai axit ny l khng ng k (nh hn 5 %).
80
Hnh 4.4
nh hng ca loi axit n cng vch ph.
V d vch ph Ca - 422,7 nm trong php o F - AES (khng kh + C 2H2)
V nh hng ca cc Cation khc trong mu

Dung dch mu phn tch, ngoi nguyn t cn xc nh, cn cha cc nguyn t khc. Cc nguyn t ny
tn ti di dng cc Cation hay Anion tan trong dung dch
81
mu. Cc Ion ny c th lm tng, cng c th lm gim, hoc cng c th khng gy nh hng g n

cng vch ph ca nguyn t phn tch. Khi c nh hng th mc nhhng ca
rt
khc nhau trong
tngtrng
hp c
mi Ion cng
th.
Nhng mt cch tng qut th chng ta c th quy nh hng ca cc Cation theo 7 loi nh trong hnh 4.5
d xem xt.
Loi 1, khi nng ca Ion gy nh hng ln hn C2 th n khng lm tng cng vch ph
ca nguyn t phn tch na, nh hng ny c s dng tng nhy ca phng php phn tch mt
nguyn t, khi thm vo mu nguyn t nh hng c nng ln hn C2 (xem ng 1 , hnh 4.5).
Loi 2, th ti nng Cl ca nguyn t gy nh hng cng vch ph ca nguyn t phn tch
t gi tr cc i. V th nh hng ny cng c dng tng nhy ca phng php phn tch.
Nhng phi gi (khng ch) nng ca nguyn t gy nh hng gi tr khng i Cl (ng 2, hnh
4.5).
Loi 3. Trong trng hp ny cng vch ph gim lin tc theo ng cong li khi nng
nguyn t nh hng tng dn u (ng 3 trong hnh 4.5).
Loi 4. Cc Cation ch gy nh hng n cng vch ph ca nguyn t phn tch khi nng
ca n ln hn gi tr C4. Do vy, nu nng ca cc Cation trong mu nh hn gi tr C4 th khng
phi quan tnm n tm bin php loi tr (ng 4, hnh 4.5).
Loi 5. Trong trng hp ny cng vch ph ca nguyn t phn tch li b gim lin tc theo
ng cong lm, khi nng Cation gy nh hng trong dung dch mu tng dn v y nht thit phi
tm bin php loi tr nh hng ny (ng 5, hnh 4.5).
Loi 6 . Khi nng ca cc Cation khc trong mu ln hn gi tr C 5 th chng khng lm gim
cng vch ph ca nguyn t phn tch. Do nu khng tm c bin php loi tr ph hp, th
chng ta thm vo mu Cation gy nh hng vi nng ln hn gi tr C 6, a nh hng gim
thnh mt gi tr hng s cho tt c cc mu phn tch v mu chun. Nh th cng loi b c nh hng
Loi 7. y cc Cation l lm gim lin tc cng vch ph ca nguyn t phn tch theo chiu
tng dn nng ca n mt cch tuyn tnh (ng 7, hnh 4.5). Do cng cn phi tm bin php ph
hp loi tr nh hng ny, hoc gi cho cc Cation l c nng nht nh v khng i trong tt c
cc mu chun v cc mu phn tch.
nh hng ca cc Cation c trong mu n cng vch ph ca nguyn t phn tch trong php
o ph nguyn t cng rt khc nhau. V d: Ion La(III) trong php o F-AAS l yu t loi tr nh
hng ca cc Ion l c trong mu khi xc nh Ca, Mg, Mn, Al, Fe. Nhng chnh La(III) li l Ion nh
hng v lm gim cng
82
vch ph ca chnh Ca, Mg, Al, Fe rt ln trong php o F-AES. iu c ngha l mi Cation trong
tng trng hp c th v trong mi php li c tc dng khc nhau, m chnh n trong php o ny th
nh hng, nhng trong php o khc li khng gy nh hng.
Nh vy, nh hng ca cc Cation n cng vch ph ca nguyn t phn tch c th c hiu
ng dng, hiu ng nm v cng c th c hiu ng va nm va tng i vi mt Ion, khi n cc nng
khc nhau. minh ho v nh hng ca cc Cation i vi vch ph ca nguyn t phn tch chng
ta c th xem xt mt s v d trong cc hnh t 4.6 - 4.8.
Hnh 4.5
Khi qut v nh hng cc ion kim
loi
loi tr nh hng ca cc Cation n cng vch ph ca nguyn t phn tch chng ta c

th s dng mt s bin php sau y hoc ring bit, hoc t hp ca chng vi nhau, ty tng trng hp
c th, v d c th:
+ Thm cht ph gia kh nh hng;
+ Thay i nn ca mu loi tr nh hng;
+ Pha long mu bng cht ph gia lm gim thiu nh hng,
+ Thay i iu kin ha hi, nguyn t ha v kch thch ph;
83
+ Thay i mi trng kh quyn kch thch ph, dng kh tr argon, v.v.
12
16
20
24
28
HEIGHT ABOVE LOAD COIL (mml
Hnh 4.6
nh hng ca chiu cao o n cng vch ph
Nguyn t phn tch: (A) - Fe, (B) - Ca, v (C) -AI
200
Hlnh 4.7
nh hng ca T n Ba (1), Sr(2), v Ca (3)
(nh hng loi 6)
84
400
ng/mL.
nh hng ca cc Anion
Cng vi cc Cation, cc Anion cng nh hng n cng vch ph ca nguyn t
phn tch, v nh hng ny cng tng t nh nh hng ca cc loi axit. Ni chung, cc
Anion ca cc axit d bay hi thng lm gim t cng vch ph. Ch ring c hai Anion
ClO- 4 v CH 3CPPOO-, l gy hiu ng dng (lm tng), tc l lm tng cng vch ph
ca nguyn t phn tch trong mt s trng hp mt
85
vng nng nht nh. Cc Anion khc thng gy hiu ng nm (lm gim) theo th t
Cl-,ON3,CO3,SO4,PO4,SiO3. Trong Anion SiO3c nh hng ln nht, cn t
nht l hai Ion Cl- v NO-3. ng thi khi nng ca cc Anion tng th tc dng nh hng
cng tng theo (hnh 4.9). Do thc t nn trong mi php o phi gi cho nng ca cc
Anion trong mu phn tch v mu chun l nh nhau v mt gi tr nht nh khng i.
Mt khc, cng khng nn chn axit H 2SO4 lm mi trng ca mu cho php o AES m ch
nn dng axit HCl hay HNO 3 vi nng di 2%.
cr
Br'
NO;
so^
PO^
C AII
0,2
0,4
Hnh 4.9
Khi qut v nh hng ca cc anion
Thnh phn nn ca mu
Yu t nh hng ny ngi ta quen gi l matrix effect. Nhng khng phi lc no n
cng xut hin, m ch thy trong mt s trng hp nht nh. Thng thng l cc mu
c cha cc nguyn t nn di dng cc hp cht bn nhit, kh bay hi v kh nguyn t
ha. V d: Khi xc nh cc tp cht lng vt trong cc mu oxit t him, oxit kim loi
kim th, oxit nhm, oxit zircon, cc mu mui NaCl, th cc nn ny s kh cng ca
vch ph ca nguyn t phn tch; qua lm gim nhy ca phng php phn tch.
Trong nhiu trng hp, yu t ny lm gim hng chc ln, thm ch c trng hp lm gim
hng trm ln cng ca vch ph (bng 4.4). Nguyn nhn chnh ca nh hng ny l s
tn ti ca cc hp cht bn nhit trong mi trng pht x. Cc hp cht ny lm kh khn,
cn tr qu trnh ha hi v nguyn t ha ca cc nguyn t phn tch.
loi tr nh hng ca thnh phn nn ca mu phn tch ngi ta c th dng cc
bin php khc nhau, nh:
86
Tng nhit ca plasma kch thch ph;

Thm
vo mu cc cht ph gia c nng ph hp;
Chng
5
PHN TCH QUANG PH PHT X NH TNH
Thay i nn ca mu sang nn khc;
Tch loi b nguyn t nn cn tr, khi ba bin php trn khng t kt qu. Tt
nhin bin php ny l hn hu.
Nguyn tc chung
Bng 4.4
Nh chng ta bit, khi cung cp nng lng ha hi, nguyn t ha mu phn tch
nh
hng
ca m
thnhhi
phnnguyn
nn cat
mu
tch pht x th chng ta s thu c ph pht x ca
v kch
thch
phn
i n
mu phn tch. Ph gm ba thnh phn:

Ph vch caCht
nguyn
vmu
Ion.
nnt
ca
Ph m ca phn t v nhm phn t.
Cng vch ph C=30 ppb php o
AES
Mg-202,60 nm
Ca-422,70 nm
Trong
ba thnh
phn1%
, th ph vch l thnh phn 0,220
chnh c trng cho 0,250
nguyn t v
1. Dung
dch HCl
Ion trng thi hi t do, khi chng b kch thch, ngha l trng thi hi. Khi b kch thch,
2. Nh 1, thm 2% LaCl3
0,008
0,005
cc nguyn t v Ion s pht ra mt chm bc x quang hc gm nhiu tia c bc sng khc
3. trong
Nh 1,
nhau nm
dithm
ph 0,5%
quangLaCl
hc3(190-1100nm). Nu thu,0,050
phn li v ghi chm 0,060
sng li ta
Ph nn lin tc.
s c mt di ph gm cc vch pht x ca nguyn t v Ion ca cc nguyn t c trong

3. Nh 2, thm 1% NH4NO3+LiBO2
0,210
0,245
mu. Trong tp hp cc vch ph , th mi loi nguyn t hay Ion li c mt s vch c
trng ring cho n. Cc vch ph c gi l cc vch ph pht x c trng ca loi nguyn
t y. V d khi b kch thch: Nguyn t Al pht ra vch c trng trong vng UV: 308,215;
Trong Nguyn
cc bintphp
trn,rabin
th nht
cng
thc
hin c
trong nhng
309,271nm.
Cu pht
vchphp
c trng
trong
vngchUV:
324,754;
327,396nm.
- M
chng
mc
nht
nh,
v
chng
ta
khng
th
tng
nhit
nguyn
t
ha
ln
cao
mi
c,
do
pht ra vch c trng trong vng UV: 259,373; 260,570nm.
s hn ch ca trang thit b, bn cht ca khi t, hn na khi nhit nguyn t ha qu

Nguyn t m pht ra vch c trng trong vng UV:279,553; 280,270nm.
cao th li xut hin nh hng ca s Ion ha. Cho nn bin php hai v ba l thng dng
Chnh nh cc vch ph c trng ny ngi ta c th nhn bit c s c mt hay
nht. Cc cht ph gia thng hay c dng trong php o F-AES, ICP-AES l LaCl 3, SrCl2,
vng mt ca mt nguyn t no trong mu phn tch qua vic quan st ph pht x ca
LiCl, KCl, AlCl 3 v cht ph gia c dng nhiu nht l LiBO 2, NH4NO3 hay hn hp ca
mu phn tch, v tm xem c cc vch ph c trng ca n hay khng, ngha l da vo cc
hai cht ny vi mt nng ph hp.
vch ph pht x c trng ca tng nguyn t nhn bit chng. l nguyn tc ca phng
php phn tch quang ph pht x inh tnh.
T c s vt l chng ta c th khi qut qu trnh phn tch quang ph pht x nh
tnh gm cc giai on sau y:
Cung cp nng lng ha hi, nguyn t ha mu phn tch to ra m hi nguyn t
t do v kch thch m hi pht ra ph pht x ca chng.
Thu chm sng pht x , phn li v ghi ph pht x ca mu phn tch.
Quan st ph thu c ca mu phn tch theo cc vch c trng ca cc
88
87
nguyn t pht hin chng.

Cc giai on ny c thc hin nh mt h thng my quang ph pht x. H thng my ny
cng gm ba phn chnh tng ng vi ba nhim v nu trn. l:
Phn 1.
Ngun nng
lng ha hi,
nguyn t
ha v kch thch m hi
nguyn t ca mu n pht x.
Phn 2. My quang ph thu, phn li v ghi ph pht x ca mu.
Phn 3. H thng trang b quan st nh tnh v nh lng.
Trong phn tch nh tnh, khi quan st khng thy vch ph pht x c trng ca mt nguyn t
trong ph ca mu phn tch, iu c th xy ra hai kh nng: 1hoc l hon ton thc t khng c
nguyn t trong mu phn tch, 2. Hoc l nguyn t c trong mu phn tch, nhng nng ca
n nh hn nhy pht hin ca phng php phn tch. V th khng xut hin vch ph pht x c
trng ca n. V d: Nu dng 2 loi ngun HQ v ICP kch thch ph pht x th:
+ Vi ngun HQ: 2 vch Cu nu trn xut hin nng C > 0,0004%
+ Vi ngun
ICP:
Cng 2 vch Cu ny,
nhng xut
hin
nng
C >
00004%. Do vic kt lun kt qu phn tch phi theo phng php phn tch v cc iu kin trang b
dng thu ghi ph ca mu phn tch v nhy ca phng php s dng.
l hin tng thc t, song ngi ta thng hay quy c v coi nh l khng c nguyn t
trong mu phn tch, khi khng tm c cc vch c trng
(2
vch ph) ca nguyn t trong ph pht
x ca mu phn tch, theo k thut dng nh tnh.

Vch chng minh nh tnh v cch chn
Mun xc nhn s c mt hay khng c mt ca mt nguyn t no trong mu phn tch, ngi
ta phi tm mt s vch ph c trng ca nguyn t trong ph ca mu phn tch xem c hay khng,
t m kt lun c n hay khng c n trong mu phn tch. Nhng vch ph c trng c chn
c gi l vch chng minh ca nguyn t y. Ni chung, pht hin mt nguyn t t kt

qu chnh xc v chc chn, ngi ta phi chn t nht hai vch chng minh khi quan st ph ca
mu phn tch. Cc vch ph ny phi tha mn mt s iu kin sau y:
Nhng vch ph ny phi r rng v khng trng ln vi cc vch ca nguyn t khc, nht l
nguyn t nng ln.
N phi l nhng vch ph nhy, c th pht hin c cc nguyn t trong mu vi nng nh
(phn tch lng vt).
Vic
chn cc vch
ph chng minh cho
mt nguyn
t phi
xut pht
ngun nng lng dng kch thch ph ca mu phn tch, v trong ngun kch
89
thch c nng lng thp
th ph
ca nguyn t l
ch
yu v vch
nguyn t ca n
thng l nhng vch nhy. Ngc li, trong ngun kch thch giu nng lng (ICP) th ph ca Ion l
ch yu. Cho nn phi ty thuc vo ngun nng lng dng kch thch ph m chn vch chng
minh l vch nguyn t hay vch Ion cho ph hp.
Phi cn c vo my quang ph c th thu, phn li v ghi c trong vng sng no m chn vch
chng minh cho mt nguyn t nht nh. V d chng minh Na, nu ph mu c ghi trn my Q-24
(vng ph 200-400 no th ta phi chn hai vch Na 330,30 v Na 330,27 nm. Ngc li, nu ghi trn my
lng knh thy tinh (vng ph 360-780 nm.), th li phi chn hai vch Na 589,60 v 589,00 nm.
Nu
dng my cch t PGS-2 (vng ph 200- 1100 nm) th chn 4 vch trn u c.
nhy ph v kh nng pht hin
Trong phn tch quang ph pht x nguyn t ngi ta thng s dng hai khi nim v nhy.
l nhy tuyt i v nhy tng i xem xt hay nh gi kh nng phn tch ca mt phng
php.
nhy tuyt i (cn gi l nhy khi lng)
nhy tuyt i l lng gam nh nht ca mt nguyn t cn phi a vo kch thch ph trong
plasma cn pht hin c t nht hai vch ph c trng ca nguyn t y trong mt iu kin
nht nh chn, ngha l cn chng minh c nguyn t y. V d, ch c th pht hin c cc
nguyn t:
+ Pb khi trong plasma h quang kch thch ph phi c 0,000007 g Pb.
+ Al khi trong plasma h quang kch thch ph phi c 0,0000055 g Al.
Cn cc gi tr
nh hn th khng
th pht hin c
Pb v Al. Cc gi tr
(lng gam) 0,000007 g v 0,0000055 g c gi l nhy tuyt i ca Pb v Al trong php phn tch
. Nh vy, mi nguyn t khc nhau c nhy tuyt i khc nhau v ph thuc vo mi nguyn t,
cc iu kin kch thch v ghi ph ca mu (bng 5.1).
nhy tng i (cn gi l nhy nng )
nhy tng i l nng nh nht ca mt nguyn t phi c trong mu phn tch
cn c th pht hin c t nht hai vch ph c trng ca n, trong cc iu kin thc nghim
nht nh chn. Cn nu nh hn nng th ta khng th tm c mt vch c trng no ca n
trong ph ca mu phn tch. V d: pht hin c hai vch ph c trng ca cc nguyn t sau trong
ngun h quang, phi c:
90
+ Pb vi nng trong mu l => 0,0008 %

+ Al vi nng trong mu l => 0,0004 %
+ Cu vi nng trong mu l => 0,0005 %
Cc gi tr 0,0008; 0,0004; 0,0005 % c gi l nhy tng i ca Pb, Al v Cu trong php
phn tch ny. l nng nh nht cn pht hin c cc nguyn t theo
vch ph pht x ca
n trong mt iu kin nht nh chn .

Cng nh khi nim trn, mi nguyn t khc nhau
khc nhau. Ni chung, cc nguyn t c t vch ph thng c
Trong phn tch
cng c
nhy
tng
nhy cao (bng 5.1).
ngi ta hay dng khi nim nhy
tng i v ch
i khi cn
thit mi dng khi nim nhy tuyt i, v dng khi nim nhy nng chng ta d so snh
nhy ca cc nguyn t vi nhau hn. Nh vy, kh nng chng minh ca mt nguyn t ph thuc vo
nhy ph ca nguyn t . Nguyn t no cng nhy ph th cng c th pht hin c n ngay nng
rt nh (tt nhin l nng ny phi cn ln hn nhy tng i).
Ngoi nhy ph ca mt nguyn t, kh nng chng minh ca nguyn t cn ph thuc vo mt
s yu t khc, nh:
+ Cc iu kin thc nghim ha hi, nguyn t ha mu, kch thch cc nguyn t v iu kin
trang b ghi o ph ca mu phn tch.
+ Cht lng ca h thng quang hc ca my quang ph;

+ Cu to, thnh phn vt l v ha hc ca mu phn tch;
+ Mi trng kch thch ph;
+ Trng thi tn ti ca nguyn t trong mu;
+ Cht ph gia thm vo mu phn tch.
Nhng trong mt iu kin th nghim nht nh ph hp c chn, vi h thng trang b nh
nhau v cng mt loi mu, th kh nng chng minh ca mt nguyn t ch cn ph thuc vo nhy
ph ca nguyn t phn tch v trang b thu nhn ph m thi.
V th mun nh gi, so snh kh nng chng minh ca mt nguyn t bng ph pht x nguyn t,
chng ta phi nghin cu chng trong nhng iu kin nht nh nh nhau v ph hp, nh ngun nng
lng ha hi, nguyn t ha v kch thch ph, cng nh cc iu kin ghi ph ca chng.
Bng 5.1
91
Vch
ctrng
trng
cav
mt
s nguyn
5.4 S
vch
cch
loi tr t
Nguyn
pht(nm)
Cng
c khi nNng
xut
hinCc
(%)vch ny
Ph
pht t
x ca mtVch
nguyn
thng c rt nhiu
vch,
hng
ngn
vch.
phn b t vng sng ngn n sng di ca di ph quang hc (190-1100 nm). Nguyn t no c cu to
0,0001
I 328,068
5500R
lp v in t cng phc tp, nht l s in t ha tr cng nhiu, th ph pht x ca chng cng c nhiu
vch, v d Anh
pht x ca mu phn tch,
nht l cc mu a kim loi,
th ph pht x ca
g Fe. V th, ph
I 338,289
2800R
0,0006
n tt nhin cng c nhiu vch. Trong di ph tt nhin c th c hai nguyn t
khc nhau, nhng
0,02
I 520,907
100R
chng li c th pht ra tia bc x cng di sng, hoc khc nhau khng n 0,01 nm. Trong trng hp
I 546,549
100R
0,025
ny vch ph ca hai nguyn t l trng nhau hon ton hoc l chng ln nhau mt phn, ngha l c
I 257,510
48R
0,08
hin tng trng vch, hin tng
quy ri v chen ln ca
cc vch ph ca cc nguyn
t vi nhau.
Vch ph trng
I 308,216
320R
0,001
VchAlph trng l cc vch ph ca cc nguyn t khc nhau, nhng c cng mt gi tr di sng.

I 309,271
650R
0,0005
V th trn knh nh ta ch thy
c
mt
vch
duy
nht.
V
d
vch
La
412,323nm
trng
I 396,153
900R
0,0003vi vch ph Er
412,823nm (khng nhy). Nn khi nh tnh khng c chn vch La 412,323nm chng minh nguyn
I 249,678
420R
0,005
t La, mc du l mt vch nhy ca La.
Ba
480R
0,003
Vch quy ri v chen ln I 249,773
0,02
II 233,527
55R
Vch quy ri v chen ln l vch ph ca cc nguyn t khc nhau, nhng chng c i sng
Ba
xp x bng nhau m my quang
ph khng phn gii c
V th trn knh nh
II 234,758
16Rthnh cc vch ring r.0,05
455,404
hai vch ph ny nm k nhauII v
c mt phn chng ln6500R
nhau. Do khi quan st ta0,0005
cng ch thy c mt
vch rng. Song c trng hp
vch c th tch ra c
nng nh ca c hai 0,001
nguyn t, nhng khi
II hai
493,409
2000R
mt trong hai nguyn t c nng ln, tt nhin l vch ca nguyn t c nng ln s ln t vch ca
II 553,555
650R
0,006
nguyn t c nng nh. l s quy ri v chen ln ca cc vch ph ca cc nguyn t. V th,
20
II 315,887
0,05
chng minh nh tnh mt nguyn t chng ta cng phi loi tr nhng vch ph c hin tng .
0,02
II 317,933
50
Ph m
Ca
II 393,367
4420R
0,0005
Bn cnh s trng vch v s quy ri ca cc vch ph ca cc nguyn t khc nhau, th ph m
0,001
II 396,847
2200R
ca cc phn t v nhm phn
t cng l mt yu t gy
kh khn cho php phn tch nh tnh, v trong
nhiu trng hp th ph mIIca
cc phn t che lp mt
cc vch c trng ca cc0,003
nguyn t khc. iu
422,673
1100R
ny th hin rt r trong vngI kh
kin (380-780 nm), nu50ta kch thch ph ca mu0,05
phn tch trong mi
2824,34
trng khng kh, hay trong cc my quang ph c phn gii khng ln.
I 3247,54
5000R
0,0004
l
nhng
kh
nng
c
th
xy
ra
khi
quan
st
bt
k
mt
bng
vch
ph
no
ca cc nguyn t
Cu
0,001
I
3273,96
2500R
ha hc. Song khng phi v th m khng chng minh nh tnh c mt nguyn t theo ph pht x ca
I 5105,54
40
0,06
n. Bng thc t, ngy nay ngi ta c rt nhiu cch khc nhau loi tr cc yu t nh hng . V
0,001
I 248,328
280rh
d: Trong iu kin kch
Fe
92
I 259,941
200
0,003
I 302,065
280R
0,001
I 358,120
600R
0,0005
I 371,994
700R
0,00045
I 373,448
700r
0,0005
93
thch ph thng thng th tt nhin khng th xut hin cc vch ph ca cc cht kh nh oxy, halogen,
nit,... Hoc khi phn tch cc mu thng thng tt nhin khng th c kh nngtrng
nguyn
phng x,
vch vi
cc
him,nguyn tqu,...
Mt khc cn c vo cng ca cc vch ph hay nng xut hin ca cc vch ph khc nhau ca
cc nguyn t, chng ta cng c th d on c trong iu kin c th th vch ph c xut hin
hay khng, ngha l trong mi trng hp c th cn phi lun lun ch n nhng kh nng trng vch,
s quy ri v chen ln ca cc vch ph vi nhau. Song cng t cc trng hp c th m tm cch
khc phc cho ph hp.
Sau y
l mt s v d
v mt vi phng php loi tr
mt s yu t nh
hng nu.
Li dng tnh cht bay hi khc nhau ca cc nguyn t theo thi gian chn thi gian ghi ph
cho thch hp (theo ng cong bay hi). T c th loi tr c s quy ri ca cc nguyn t khc
i vi nguyn t phn tch.
Chn iu kin v ngun nng lng kch thch ph ph hp, to ra s kch thch ph c u tin
v chn lc i vi mt vi nguyn t chng ta cn kho st, phn tch.
Chn mi trng kch thch ph cho ph hp. V d: Khng kch thch ph trong khng kh m kch
thch chng trong mi trng ca mt kh tr hay hn hp ca kh tr vi oxy. Trong trng hp ny
ngi ta c th loi tr c hon ton nh hng ca ph m ca cc phn t v nhm phn t CN.
Chnh v th hin nay trong phn tch quang ph pht x, ngi ta thng kch thch ph ca mu phn tch
trong mi trng ca kh tr Al v hn hp ca argon vi oxy.
Thm vo mu nhng cht ph gia thch hp c th loi tr cc hp phn sinh ra ph quy ri
khng c li, nh to ra s bay hi chn lc, s bay hi phn on ca cc nguyn t khc nhau.
Chn my quang ph c phn gii ln v vng ph ph hp thu, phn li v ghi ph ca mu
phn tch. Trong thc t phn tch, th bin php ny trong nhiu trng hp c kh nng loi tr
hon ton cc yu t nh hng nu.
Nu tt c cc bin php trn s dng m vn cha loi tr c nh hng, th phi dng
phng php tch chit no loi cc nguyn t cn tr ra khi mu phn tch. Tt nhin y l bin
php cui cng v thc t hu nh rt t khi phi s dng n.
Cc phng php phn tch nh tnh
Mc ch ca phn tch quang ph pht x nh tnh l pht hin cc nguyn t, ch yu l cc kim
loi trong cc mu phn tch, n gm c hai loi yu cu, do cng c 2 kiu nh tnh:
94
Phn tch nh tnh tng phn v

Phn tch nh tnh ton din.
Phn tch nh tnh (T) tng phn tc l kim tra xem trong mu phn tch c cha nhng nguyn
t m ngi ta cn quan tnm n hay khng, cn cc nguyn t khc th khng cn bit n. V d ngi
a mu yu cu tm xem trong mu ny c Pb hay khng?
y l phn tch T tng phn, v ch cn tm nguyn t Pb trong mu. - Ngc li, phn tch nh
tnh ton din l phi xc nh xem trong mu phn tch cha bao nhiu nguyn t c thy. V d ngi a
mu yu cu tm xem trong mu ny c bao nhiu kim loi c thy? y l phn tch T ton din.
Chnh t thc t m ngi ta cng c mt s
cch quan st nh tnh
khc
nhau, da theo ph pht x ca mu.

Phng php quan st trc tip trn mn nh
Nguyn tc ca phng php ny l trn mn nh ca my quang ph (mt phng tiu) ngi ta t
mt mng m, trn mng m ny c nh du v tr cc vch c trng ca mt s nguyn t nht nh.
ng thi b tr mt h thng thu knh lp phng i quan st trc tip mn nh .
Nh vy, mun nh tnh mt mu no , ta thu ph ca mu phn tch, khi kch thch chng bng
mt ngun nng lng ph hp v quan st ph mt cch trc tip trn mn nh ca my nh h thng
knh lp phng i.
Khi da theo cc vch ph c trng nh du trn mng m m kt lun c mt hay khng c
mt nguyn t trong mu phn tch.
Phng php ny nhanh, n gin. Nhng ch gii hn trong nhng mu n gin v nhng nguyn
t cn phn tch c nh du cc vch ph c trng
ca
trn mng m ca my quang ph.

N ch yu phc v cho phn tch luyn kim, kim tra nhanh mt vi nguyn t cn thit, nh
Mn, Cr, Si, C, Al,...V cng v th m c mt loi my quang ph chuyn dng cho mc ch ny. l
cc loi my Styloscop. My quang ph ny phc v cho ni dung phn tch nh tnh tng phn ca ngnh
luyn kim l ch yu.
Phng php so snh ph
y l phng php n gin, chnh xc, nhng cng ch phc v cho mc ch phn tch nh tnh
tng phn.
Nguyn tc ca phng php ny l: Mun nh tnh mt nguyn t X no ,
95
chng ta phi ghi ph ca nguyn t X nguyn cht k vi ph ca mu phn tch. Ri tm mt nhm vch
c trng ca nguyn t X trong mu nguyn cht v so snh nhm vch ph vi ph ca mu phn tch
xem c nhng vch ph c trng hay khng trong ph ca mu phn tch.
Trn c s m kt lun c mt hay khng c mt ca nguyn t X trong mu phn tch. Phng
php ny tuy n gin, nhng vi mi nguyn t cn tm ta li phi ghi mt ph ca nguyn t nguyn
cht.
V th chng nhng tn km knh nh, in cc v thi gian, m nhiu khi cn khng c ca nguyn
t X tinh khit lm ph so snh. Do n cng b hn ch v khng c ng dng nhiu trong thc
t.
Phng php ph chun (Dng bn atlas)
Ph chun hay cn gi l bn atlas ph l cc bng vch ph ca Fe theo mt my quang ph nht
nh. N c xem nh l mt thang di sng phc v cho vic nh du v tr cc vch ph c trng
ca cc nguyn t. N c cu to gm 2 phn.
Phn trn l mt dy cc vch ph ca Fe trong mt vng ph nht nh ca my quang ph. Phn
di, tc l k vi ph ca Fe, l v tr cc vch ph c trng ca cc nguyn t khc v trn cng l
thang s sng (hnh 5.1).
Nh vy, mun nh tnh mt mu no , ta cn phi ghi ph ca Fe v k l ghi ph ca mu
phn tch.
Sau nh my chiu ph v bn atlas ta c th nhn bit c trong mu phn tch c cha nhng
nguyn t no khi quan st ph ca mu phn tch theo cc vch ph c trng ca tng nguyn t, bng
cch em ph ca Fe trn knh nh lm trng vi ph ca Fe trn bn atlas.
V th, nh tnh bao gi cng phi ghi ph theo tng cp, mt ph ca Fe v k l ph ca
mu phn tch, ngha l c bao nhiu mu phn tch th c by nhiu cp ph tng ng.
Phng php ny ph hp cho c hai mc ch phn tch nh tnh tng phn v nh tnh ton din.
Nhng mi my quang ph cn phi c mt b atlas hon chnh cho n i vi tt c mi nguyn t cn
nghin cu.
V th ngy nay hu ht cc phng th nghim ch dng phng php ny cho c hai mc ch phn
tch nh tnh. Cc hng bn my quang ph cng cung cp cc bng atlats cho cc my ca h.
Hnh 5.1 l v d v mt on ca bn atlas ca my quang ph.
96
47
VM
97
98
Chng 6
PHN TCH PH PHT X NH LNG
Nhng vn chung
Phng trnh c bn v nguyn tc
Phng php phn tch quang ph pht x nguyn t nh lng da trn c s gia
nng ca nguyn t cn phi xc nh v cng ca vch ph pht x do n pht ra, khi
b kch thch trong nhng iu kin thch hp, c mi lin h tuyn tnh v n tr theo hm
s.
I. = f (C)
(6.1)
trong mt gii hn nht nh ca nng C ca nguyn t phn tch, trong I. l

cng ca vch ph pht x ca nguyn t , cn C l nng ca nguyn t trong
mu phn tch.
Bng l thuyt v thc nghim ngi ta tm c mi lin h v c m t theo
phng trnh Lmaskin - Schraib nh trnh by trong chng II trn l:
I. = a.Cb
(6.2)
Theo phng trnh ny, nu c mt s mu u (mu chun) c nng C bit chnh

xc, v d Ci, C2, ... Cn v xc nh c cng ca 1 vch ph pht x
tng ng ca chng, th ta c th dng c ng chun I - C, ri t c th d dng tm
c nng Cx cha bit.
Nhng trc y (trc 1965), do khng xc nh trc tip c gi tr cng pht
x I. ca mt vch ph, m ngi ta phi chiu chm sng pht x cng I. ln knh nh.
Sau xc nh cng hay en ca chng trn knh nh ti ch b chm sng I. tc
dng ln. en S. ny c tnh theo cng thc:
S. = y.log.I.
trong Y l h s
(6.3)
nh tng ca knh nh.Nh vy, ta c phng trnh h qu
nh sau, vi k = y.log a:
S. = Y b.log.C + k
(6.3)
T thc t , hin nay chng ta c hai phng trnh c bn ca php phn tch nh lng
theo ph pht x ca nguyn t. Nu cc my cho php xc nh trc tip
99
6.1.2
Vch
phn tch
chn
c gi
tr cng
I xvthcch
chng
ta tnh ton theo phng trnh (6.2). Nu cc my quang ph phi xc
nh gin
nn
I x qua
nh
enS S,
thvch
phi tnh
l
tip
loicng
tr ph
khivic
xcxc
nh
en
ca
ph ton
phntheo phng trnh (6.4),
tch,ngha
ngi
phng trnh th nht c dng y = ax, cn phng trnh th hai th c dng y = ax + b, song chng
ta u l
phng trnh
ng
nusau:
o theo phng trnh en S, chng ta phi loi en
thng
thc ca
hinmt
theo
mt thng.
trong Nhng
hai cch
ca ph nn. V th trong trng hp ny phng trnh thc nghim s phi l:
Cch 1: o hiu s en gia vch ph phn tch v ph nn, tc l tnh gi tr AS
AS = Y.b.logC + ko
(6.5)
trong phng trnh (6.4) theo cng thc AS = (S v - Sn). Trong Sv v Sn l en ca vch
Do , phng trnh (6.3) v phng trnh (6.5) c gi l phng trnh c bn ca phng php
v en ca nn bn vch o (hnh 6.1).
phn tch quang ph pht x nguyn t nh lng. ng biu din cc phng trnh ny c m t
Cch 2: o hiu s en gia mt vch phn tch Spt v mt vch ph so snh S ss
trong hnh 6 .1 .
(hnh 6.1), ngha l c AS = (S pt - Sss). Trong :
+ Vch phn tch l nhng vch ph ca nguyn t cn phi xc nh c chn xc

Ix
/
c
nh nng ca
n trong mu phn tch. N c chn ra t nhng
vch c trng ca
y
/ .
(A)
Jtr
nguyn t y.0,4Khi cn xc nh nhng
nng nh thBphi chn/ nhng
vch c nhy cao.
+ Vch so snh l nhng vch ph ca mt nguyn t no c chn o en

phc v cho 0,3
vic b chnh nn theo phng php 2 vch ph. Nguyn t cung cp cho vch so
snh ny c gi l nguyn t so snh. N phi c nng khng i trong c mu u v
0,21
mu phn tch. N c th l nguyn t c s ca mu phn tch hay l mt nguyn t khc

c thm vo vi nng ph hp v khng i tt c mu v cng ca n phi nm
0,1
A
trong vng 10
- 25 %
en ca vng tuyn tnh.
Nh vy, vch ph phn tch v vch ph so snh to thnh mt cp vch phn tch. Do
0 kt qu chnh xc trong cp vch phn tch th vch so snh v vch
c*
, c c
phn tch
, * mt s iu kin
c 2 nht nhc 3nh sau:c 4
cn phi tha0,5mn
c5
Chng phi l hai vch cng loi, hoc l hai vch nguyn t,
2 vch
0,4
hocl
(B)
ln cng bc Ion ha.

Th kch
thch ca hai vch ny phi gn bng nhau. Nu bng nhau l iu l tng.
0,3
Tt nhin trng hp bng nhau l iu him c, do cn chn bi vch c th kch thch
ph cng gn bng nhau th cng tt. V nh th s loi b c nh hng ca s dao ng
0,2
ca nhit plasma.
Hai vch phi khng xa nhau qu 10 mm trn knh nh (mt phng tiu), v ch trong
iu kin h s nh tng knh nh Y mi thc s l hng s, ngha l hu nh khng ph
0,1
logC
thuc vo di sng ca cc vch ph.
Hai vch phi nt, r rng v gi tr AS ca chng phi thay i nhy vi s bin
0
logC,
logC
logC
logC
thin nng ca nguyn
t phnlogC
tch trong
mu, nhng
li khng
nhy vi nhng dao ng
2
ca iu kin thc nghim.

Hnh 6.1
Gi tr AS phi khng qu ln, m cng phi khng qu nh. N phi nm trong vng
Mi quan h gia cng vch ph v nng cht.
gi tr en tuyn tnh ng cong, c trng ca knh nh ghi ph.

(A): Mi quan h I-Cx; (B): Mi quan h S-logCx
100
101
Trong mt s trng hp c th khng nn chn vch phn tch l nhng vch d xut
hin hin tng t o (t hp th), v khi phm vi tuyn tnh ca ng chun s b hp.
Tt nhin yu t ny l khng bt buc cho mi trng hp. N ch l mt iu ch thm
trong nhng trng hp cn thit, khi xc nh vng nng khng qu nh.
Nhng hin nay, vi cc my quang ph th h mi, o trc tip cng vch pht x
Ix v trong my c sn h thng b chnh nn ca vch phn tch, th ngi ta ch cn o mt
vch phn tch l .
Cch biu din nng trong phn tch quang ph
Trong phn tch quang ph nh lng ngi ta thng dng v biu din nng theo
cc khi nim sau:
Nng phn trm (%).
Nng phn triu (ppm) v cc n v c s ca n.
Nng microgam (p,g/mL) v cc n v c s ca n.
Nng phn trm
Trong phn tch quang ph ngi ta thng hay biu din nng phn trm (%) theo
hai cch:
Nng phn trm tuyt i: Ch cho ta s phn trm ca nguyn t phn tch so vi
tng khi lng m ca mu phn tch, ngha l c tnh theo cng thc:
m
%C xt = m 100
m
(6.6)
trong mx l s g ca nguyn t phn tch c trong khi lng mu mg.

Nng phn trm tng i: Ch cho ta bit s phn trm ca nguyn t phn tch so
vi khi lng m ca nguyn t c s (nguyn t c thnh phn > 90%) ca mu phn tch.
N c tnh theo cng thc:
m
%C
xd =
^ 100
m
(6.7)
Trong hai cch biu din ny th cch biu din th nht c ng dng nhiu hn, cn
cch th hai ch dng khi so snh nng ca nguyn t phn tch vi nguyn t c s ca
mu. Trong thc t, ngi ta quy c rng, khi ni nng phn trm th ngi ta hiu l
nng phn trm tuyt i. Ngc li mun dng cch th hai ngi ta phi ni v ghi y
l nng phn trm tng i.
Tt nhin gia hai cch biu din ny u c quan h vi nhau v t cch biu din th
nht, ngi ta c th suy ra cch biu din th hai theo cng thc sau:
C ,m
%C =^x^L
m
102
(6.8)
Nng phn triu (ppm) v cc n v sau n

i lng nng ppm (phu pa mill Ion) l n v nng c tnh theo n v l
mt phn triu (1/1.000.000) theo n v khi lng hay mt phn triu theo n v th tch
ca mu phn tch (cho mu lng). Nn theo khi nim n v ny, mt nguyn t phn tch
c nng 10 -6g trong 1 gam mu, th gi tr ny c gi l 1 ppm. Nh th, nu vit theo
khi lng: 1g/T, hay 1 mg/kg, hay 1^g/g, hay theo th tch 1 pl/mL; hay 1 mL/L; hay 1 L/m 3,
th u tng ng 1 ppm.
Cn cc n v nh hn sau ppm l:
ppb v 1 ppb bng 0,001 ppm
ppp v 1 ppp l bng 0,001 ppb = 0,000001 ppm
ppf v 1 ppj l bng 0,001 ppp = 0,000001 ppb = 0,0000000001 ppp
Cc n v ny hn km nhau 1000 ln. Trong phn tch vi lng v siu vi lng, h
n v ny c dng ph bin nht.
Nng microgam
Loi nng ny c biu th theo hai cch, c th l:
Theo th tch mu (khi lng th tch)
A1. Microgam/L: S microgam ca cht phn tch c trong mt lt dung dch mu, k
hiu l 0.g/l. V d, nu vit nng ca Pb l Cpb: 1,2 0.tg/l th c ngha l c trong 1 lt
dung dch mu s c 1,2 microgam ca Pb.
A2. Microgam/ml: S microgam cht phn tch c trong mt mnh dung dch mu, k
hiu l p,g/mL. Nu t trng ca dung dch d = 1, th n v ny tng ng ppm. V d nu
vit Cpb: 1,2 p,g/mL th c ngha l trong 1 mun dung dch mu s c
microgam ca Pb.
Theo khi lng mu (khi lng/khi lng)
B1. Microgam/gam: S microgam ca cht phn tch c trong mt gam mu v k hiu
l pg/g. V d, nu vit Cpb: 2,5 p,g/g, th c ngha l c trong 1 gam mu s c
microgam ca Pb.
Cng hon ton tng t nh trn chng ta cng c cc n v biu din nng theo
khi lng mu l: p,g/g; mg/kg; g/T. Cc n v ny u l tng ng ppm.
B2. Microgam/ml: S microgam ca cht phn tch c trong mt ml dung dch mu v
k hiu l p,g/mL. V d, nu vit Cpb = 2,5 p,g/mL, th c ngha l c trong 1 ml dung dch
Cc n v c s ca ug
l nanogam (ng), picrgam (pa). Do cng c cc khi nim tng ng l:
103
capg/mL
cc muvu
phi
bnpg/g.
vng Cc
theo n
thi gian,
ngha
sau p,g
khi l:
chun
chng
ng/L, Thnh
ng/mL,phn
pg/L,
v nng
lsau
ng b
vxong
pg chng
agng/g
- hay
attogam;
khng
thaynhau
i v
mi ln
mt,v
t mi
nngtng
nquan
trng ca
thi lin
kt c
v cuch
trc.
u km
1000
chng
ra trong bng 6.1, 6.2, v 6.3.
pa - picogam.
Khi mu
vtch
muquang
phn ph
tch pht
thax
mn nhng iu kin trn, ngha l mu u v mu phn tch
Mu chun
trongu
phn
fg - femtogam;
ph hp
vi nhau
mi quang
mt th cc
trng
v phcadng
mu
l tng
nhau. Vphn
d: tch ca mt
Trong
phnvtch
phc
nh
lng,
mt
ngt chun
ngmc
- nanogam.
Nn
ca
phphc
l nh
nguyn+ t
no
vnhau,
cho
ch xc nh n trong mt i tng nht nh, hay
xc nh
cc hng
vt
ca
phng
bn,u
ngi
ta phi
mtging
dynhau,
mu chun
p,g
- c mu
+ ng
congs
bay
hilca
cc
nguyntrnh
t trong
v mu
chundng
c dng
(mu u). Thnh phn, tnh cht v nng ca dy mu u ny s quyt nh chnh xc
+ Thnh phn ph vch camicrogam.
nguyn t l nh nhau, c bit l nguyn t c s phi hon ton ng
v ng n ca kt qu phn tch. V vy, m bo cho php phn tch t kt qu tt th
nht trong cc mu,
ppm:
phnkin
triusau:
(part per mil Ion)
dy mu u ny phi tho mn
mtmt
s iu
+ Thi gian kch thch ph ca cc mu l nh nhau.
Bng 6.3
Chnh nh nhng c trng c s ny ca ph mu m ngi ta c th pht hin c xem mu
Bng
6.1
phn tch v cc mu u c ch luyn c ng nht hay khng. Mu chun v mu phn tch c th
Nng u c
Chuyn sang nng th hai

Nng
H s phi nhn vo
g/L
0,01 p
Mi
gia
n
v nng
quan
dng h
bt,
rncc
hayloi
dung
dch
l ty
thuc vo nguyn t phn tch, cc trang b v iu kin kch thch
ph no cho kt qu tt nht.
1 ppm
Gii hn chng minh v khong xc nh
p
1 ppm
p,g/L
Cng n
nh cc
phng php phn
tch ng
khc, phng
tch quang
phvi
pht
v gc
Tng
vi (*)php phnTng
ng
(*)x nh lng
1
ppm
Mol/L
(M)
0,0001
p.A
cng c mt gii hn nht nh i vi mi nguyn t trong mt i tng nht3 nh. l mt khong
1000 ppm
1 mg/mL
10" g/mL
nng ca1nguyn
m php
o nh lng cn cho kt 0,0001
qu tin cy, ngha l c
ppm t cn kho st (xc nh)
% trng
lng
6
1
ppm
1
p,g/mL
10"
g/mL
mt cn trn v cn di ca mt php xc nh i vi mt nguyn t. Vng nng nm gia gii hn
1 Mg/L
ppm
1/p
9
trn v gii 1
hn
di c gi l khong
xc nh ca phng php phn
Tt nhin khong xc
ppb
1 ng/mL
10"tch.
g/mL
11 Mg/L
% trng
1/10000.p
nh ca mt
phng php i vi mi nguyn
t l lng
khc nhau v ngay mt nguyn
t, nu o nh lng
ppp
1 pg/mL
10"12 g/mL
1
d
theo cc vch
khc nhau th khong xc
nh ca n cng khc nhau. Vch php no cng nhy th
ppph
ng/mL
1 ppfcng hp v n nm trong
1 fg/mL
10"15Gii
g/mL
khong xc nh
vng nng cng nh (bng 6.4).
hn chng minh v
khong xc nh
ca mt nguyn t c th
c xc nh theo hai cch:
1 ppa
1 ag/mL
10"18 g/mL
Phng
trong
:php thc nghim.
Phng php ton thng k.
p: T trng ca dung dch
Bng 6.2
Trong thc t ca phn tch, vic xc nh v m rng cn di ca mt phng php phn tch lun
A: Nguyn
t gamn
hay
phn
t gam ca cht phn tch.
Mi
quan
gialn,
ccvloi
v nng
lun c h
ngha
n rt cn
thit trong cng vic phn tch cc nguyn t vi lng v siu vi lng,
Mu u phi c thnh phn ha hc v vt l ging nh mu phn tch, ngha l trong
ngha l nng gii hn di pht hin c ca phng php phn tch cng nh, th trong nhiu trng
mu phn tch c cha nhng nguyn t no v tn ti trng thi hp cht no th cc mu

hp cn
th b
s b mu
cn phn
m tavvn xc nh c.
v qua
gcc giai on lm giu Tng
ng
vi tch,
cc n
u (mu chun) cng phi c thnh phn nh th, nht l cht nn ca mu. C nh th mi
1 mg
10-3
loi b c nh hng ca sai khc v thnh phn n kt qu phn tch.
1
-6
^g v mu10phn
10-3 c x l v ch luyn trong cng mt iu kin nh
Mu u
tch phi
nhau v cng
1 ng mt trng
10-9 thi.
10-6
10-3
-9
-3
Nng1
trong 10
cc-6 mu u
tht chnh xc. Khong nng
pg ca nguyn
10-12 t phn10tch
10phi
ca c dy mu u-15phi phn b
ri u trn
ton b -6phn vng-3 tuyn tnh ca ng
1 pf
10
10-12
10-9
10
10
chun.
1 ag
10-18
10-15
10-12
10-9
10'6
10-3
trong :
104
106
105
Trong phn tch quang ph, gii hn di ca phng php nh lng mt nguyn t c biu th
bng nng Cmin' m ng vi cc nng C x ca cht phn tch m nh hn Cmin th vch phn tch
ca nguyn t bin mt vo nn ca ph (khng xut hin), v ta khng quan st c n na. Ngc
li, ng vi cc nng Cx no ln hn Cmin th vch phn tch cn xut hin r rng, php o cho kt
qu tin cy V th khi khng thy vch phn tch ca mt nguyn t trong ph ca mu phn tch, th c th
xy ra theo hai trng hp. C th nng ca nguyn t trong mu l thc t bng 0, tc l khng c
nguyn t . Hoc cng c th l c nguyn t trong mu phn tch, nhng nng ca n trong mu
l nh hn nng gii hn di ca phng php phn tch (Cmin).
Theo Kaiser gii hn di (cn di) ca phng php phn tch quang ph mt nguyn t theo
vch ph nht nh c tnh theo cng thc sau:
(n) = 3(Iv - In)
(6.9)
trong : I(v) l cng pht x ca vch phn tch ng vi nng Cmin ;
(n) l cng ca nn; l s dao ng ca gi tr en ca nn.

Trong phng php phn tch quang ph, ngi ta phn bit cn di (gii hn di) thnh hai khi
nim:
Gii hn pht hin: L nng nh nht ca mt nguyn t trong mu phn tch cn pht
hin c cc vch ph ca n (t nht hai vch nhy) theo cc iu kin thc nghim chn.
Gii hn xc nh (nh lng) : L nng nh nht ca mt nguyn t trong mu phn tch

cn c th nh lng c nguyn t cho kt qu tin cy, chc chn v chnh xc (95%). Nu gi
gii hn pht hin l Ch v gii hn xc nh l C th chng ta lun c:
Cd > Ch
(6 .10 )
Khng nhng ch gii hn di, m gii hn trn (cn trn ca mi nguyn t trong mt php o
cng khc nhau. Trong mt nguyn t, nhng vch ph no cng nhy th nng
giihn trn l
nh.Nhng vch khng nhy
hn
th
nng gii
trn l tng i ln (bng 6.4).

Cn trn ca mt phng php phn tch quang ph cng c xc nh bng thc nghim. l
gi tr nng Cmax m t nhng nng Cx ln hn, th mi quan h gia cng pht x I x v
nng C ca nguyn t trong mu phn tch khng tuyn tnh na. Ngha l ng chun biu th mi
quan h bt u gc xung trc honh k t gi tr nng Cmax .
Gii hn xc nh, khong xc nh ca mt phng php phn tch khng nhng ph thuc vo
chnh tng nguyn t, vo tng vch ph c chn o nh lng, m cn ph thuc vo mt s yu t
khc, nh:
107
pht x ca nguyn t, Ion, phn t ca cc cht mu. Trong cc qu trnh ti in cc

+ iu kin ha hi, nguyn t ha v kch thch ph ca mu phn tch. + Trang thit b
v plasma th s bay hi, nguyn t ha ca mu v s kch thch m hi l qu
thu v ghi
phi
ca mu.
trnhchnh.
Song
vi mi nguyn t v i vi mi loi mu phn tch th cc qu
trnh ny rt khc nhau. Ngha l c nguyn t d ha hi, c nguyn t kh ha hi,
+ K thut v phng php nh gi nh tnh v nh lng.
c nguyn t bay hi nhanh, c nguyn t bay hi chm. V th cn phi nghin cu
mi 6.4
quan h gia cng pht x ca mt vch ph ca mt nguyn t vi thi gian
Bng
bay hi ca n vo vng kch thch ph (plasma). ng cong biu din mi quan h
V d v gii hn xc nh v khong xc nh
ny c gi l ng cong bay hi cua nguyn t . Ni cch khc, ng biu din
s bin thin cng pht x ca mt vch ph ca mt nguyn t theo thi gian bay
hi ca mu c gi l ng
bayhinhi.
Gii cong
hn pht
(%) V
d: Khi nghin cu s bay hi v
Nguyn t Vch
Khong xc nh (%) (Gii hn
pht x ca cc nguyn t trong nn oxit
nhyt him ta thu c cc ng biu din nh
trong hnh 6.2. ph(nm)
l cc ng cong bay hi ca cc nguyn
t Fe, Mn, Mg, Si, Ce...
trn v di)
Al 236,706
0,03
0,05 - 0,4
T nhng ng cong bay hi ny chng ta thy c nguyn t bay hi nhanh, c
237,208
- 2,0ta d dng
nguyn t bay hi
chm. Cng chnh t cc0,1ng cong bay hi ny 0,15
chng
chn c thi gian ghi ph ph hp cho 0,001
qu trnh phn tch nh lng tng nguyn
309,271
0,003 - 0,15
t. Cng nh trong trng hp no v i vi nguyn t no th cn chn thi gian
5 nhng nguyn t no0,0003
0,05ngay t lc bt u kch
khi phng v 396,
i 1vi
th phi 0,0005ghi ph
0,1 nguyn t Fe, Mn, Mg,...0,15
Bi 240,088
0,9 ghi ph
thch ph. Nh
v d (hnh 6.2), i vi cc
ta - phi
ngay t u cho ti giy th 150 l , ngc li, vi Ce ta c th b 100 giy u tin

262,791
0,03
0,04 - 0,5
v ghi ph bt u t giy th 100 cho n giy th 250 l thch hp. Chnh nh chn
289,798
0,003
0,005 - 0,2
c thi gian ghi ph ph hp nh th chng ta lm cho ph thu c ca mu
phn tch Fephc
tp v d quan st nh0,001
tnh cng nh nh lng.
238,204
0,002
- 0,25l ngha
thc tin ca vic nghin cu ng cong bay hi ca mi nguyn t trong cc i
0,0002
259,940
0,0003- 0,1
tng khc nhau, v trong thc t, khng nhng cc nguyn t khc nhau c ng
cong bay hi khc
nhau, m ngay mt nguyn
t, khi0,0004chng0,15
tn ti trong cc loi mu
259,957
0,0003
khc nhau, th cng c ng cong bay hi khc nhau. iu c ngha l dng ca
Si 230,302
0,3
cong bay hi ca cc nguyn
250,690
t ph thuc vo
thnh phn
0,001
nn ca mu phn tch, trng

251,612
thi lin kt vt l, ha hc ca
0,0003
mu, cu trc tinh th ca hp

Mg 278,142 280,270 285,213
cht mu, dng hp cht m
0,03
nguyn
0,001
mu,...
Nhn
tn
chung
ti
trong
trong
0,4 - 2,0
0,003 - 0,3
0,0005- 0,15
0,05 - 0,25 0,002 - 0,10 0,0005- 0,05
cc
0,0003
hp V
chtth,ha
hc,
kh
nng
mun nng cao nhy ca mt php phn tch, ngi ta c th chn nhng iu kin thc
bay hi ca chng theo th t
nghim no, ph hp nht i vi tng nguyn t cn xc nh.
MeX > Me(NO3 ) 2 > MeO >
SMe
bay
hi v ng
cong4 bay
> MeSO
> hi
MexSy
x(PO4)y
Hnh 6.2
ng cong bay hi ca cc nguyn t' Fe, Mn, Mg, Ce trong nn

t him
>Trong
Mecx phn
v.v... tch quang ph, mu phn tch c a vo ngun sng kch thch ph v khi n cng
trmi
thnh
tc l
nguncu,
phtxy
ra cc
tiang
ph
Chnh v th i vi
loingun
mu, pht
nht sng,
thit phi
nghin
dng
108
109
cong bay hi cho tng nguyn t v ch trn c s mi c th chn c thi gian

ghi ph ph hp.
6.1.7. Kh quyn kim tra
Mi trng kch thch ph c nh hng trc tip n thnh phn ph ca mu
Mi trng kch thch ph pht x phn tch. Nhiu trng hp chnh mi trng kch
thch ph lm cho ph ca mu phc tp thm v kh quan st; c khi khng th thc
hin c php nh tnh cng nh nh lng. V d: Khi kch thch ph trong mi
trng khng kh th ph ca mu lun c cc bng CN. l ph m ca nhm
phn t CN.
Ph ny che lp nhiu
vch phn tch ca nhiu
nguyn t v n th hin rt
r trong vng kh kin.
Nhng chnh trong vng ph
ny
li
trng
nhiu
nhy
nguyn
t.
vch
ca
th
c
nhiu
ngi
ta
thng khng kch thch ph

trong
m
mi
trng
khng
kh,
trong
mi
trng
kh
quyn kim tra c. l

mi trng kh tr, hay kh
tr c thm oxy.
Khi nim v kh quyn kim tra

Vi tn gi l kh quyn tr hay kh quyn kim tra, ngi ta hiu l mt mi trng kch
thch ph pht x ca mu phn tch c th iu khin v kim tra c Mi trng ny khng cha nit
(N2) nh khng kh bnh thng. N c th ch l mt kh tr thc s nh: He, Ne, hay l hn hp ca mt
kh tr vi oxy theo mt t l nht nh. V d nh hn hp ca (Ar + O 2) hay (He + O2) ... Mi trng
cng c th l CO2 hay hn hp ca (CO2 + O2). Nhng trong tt c cc loi th u vit nht v c s
dng nhiu nht vn l hn hp ca argon v oxy, bi v nu ch dng kh tr lm mi trng kch thch
ph th mu kh bay hi v thi gian kch thch ph qu di. Nhng nu thm vo kh tr mt lng oxy
ph hp th li to iu kin thun li cho mu bay hi v qu trnh kch thch ph d dng hn. Thnh
phn kh ca mi trng ny cn phi c khng ch v kim tra theo mt nhim v phn tch. Chnh v
th m xut hin khi nim S kch thch ph trong mi trng kh quyn kim tra. Mun kch thch
ph trong mi trng kh quyn tr, ngi ta phi thc hin trong mt bung kn. Kh tr v oxy dn vo
theo mt thnh phn nht nh, ph hp v phi gi
110
khng i sut trong qu trnh kch thch ph. Hn hp kh cn c trn u trc khi dn vo bung kch
thch ph. C nh th mi m bo cho qu trnh kch thch ph n nh.
Vai tr v tc dng ca kh quyn kim tra

Trong phn tch quang ph pht x nguyn t, a mu vo vng phng in v kch thch ph,
ngi ta phi dng in cc than hay graphit tinh khit, v nguyn liu ny tha mn c nhng yu cu
ca nguyn liu lm in cc. Nhng khi dng nguyn liu ny lm in cc kch thch ph trong mi
trng khng kh, tt nhin s c nhiu ph m trong ph ca mu phn tch. Trong ch yu l ph
m ca nhm phn t CN, MeO. Ph m ny che lp nhiu vch phn tch ca nhiu nguyn t lm kh
khn cho cng vic quan st nh tnh v nh lng; c khi khng th no thc hin c. V th nht thit
phi loi tr ph m CN. loi tr hay hn ch s xut hin ca ph m ca cc phn t v nhm phn
t CN, MeO,.. ngi ta nghin cu v nu ra nhiu bin php khc nhau. Song chng ta c th khi qut
theo ba hng sau y:
Cch l: Khng dng in cc than hay graphit a mu vo phng in v kch thch ph, v mu
phn tch khng trn vi bt than quang ph, m dng in cc kim loi. Nhng in cc kim loi thng
kh ch to thnh dng ph hp cho qu trnh kch thch ph. Mt khc kim loi thng nng chy nhit
cao. Nn khng th dng h quang kch thch ph. M h quang li l ngun kch thch tt cho phn
tch mu bt. ng thi khi phn tch cc mu qung, oxit, t ,... nu khng trn thm bt than quang
ph vo mu phn tch lm cht m th vic ha hi nguyn t ha mu rt kh khn v khng n nh,
nhit ca plasma li thp. Cho nn in cc kim loi vn khng c th thay th cho in cc than c,
m ch c th dng c trong mt vi trng hp phn tch dung dch. V th bin php ny khng thch
hp cho tt c v t c s dng.
Cch 2: Theo cch ny, ngi ta vn dng in cc than, nhng thm vo mu phn tch nhng cht
ph gia thch hp hn ch s xut hin ca ph m v ph bng (CN, MeO), v d thm mui halogen
ca kim loi kim CsCL, CsF, LiF,... Nhng bin php ny cng khng trit , v n ch hn ch bt, ch
khng loi tr hon ton ph m ca CN, MeO. Mt khc, mun loi tr c mt phn ph m, chng
ta phi thm mt lng ln cht ph gia. Nh th trong nhiu trng hp li lm gim cng vch ph.
iu ny khng ph hp vi yu cu ca php phn tch lng vt, ngha l trong nhiu trng hp khng
dng c bin php ny.
Cch 3: Cch th ba l kch thch ph trong mi trng kh quyn kim tra khng c nit. Nh th
s c kh nng loi tr c hon ton ph m ca nhm phn t CN m vn dng c in cc than v
bt than quang ph lm cht m. y l phng php tt nht. N chng nhng loi tr c cc bng
CN m cn c nhiu tc dng tch cc khc. Ngy nay phng php ny c s dng rt ph bin v
111
khng Cht
c iu
g phi
nghi ph
ng na
tc dng
li ph
ca n.
Sx
d nh vy l v vic kch thch ph trong
6.1.8
m
v cht
gia v
trong
phnc
tch
pht
mi trng kh quyn tr ny c nhng u vit nh sau:
Trong phn tch quang ph pht x, mu th nghim d dng rn, dung dch hay bt cng u c
Ph ca mu phn tch l tuyt i sch, khng c ph m ca cc phn t v nhm phn t CN,
lm bay hi trong mt ngun sng, nh ngn la n kh, h quang in, tia in, ICP,... ngha l mu phn
m thun khit l ph vch ca nguyn t v Ion. Do vic quan st nh tnh v nh lng khng kh
tch c chuyn thnh trng thi hi di tc dng ca nng lng nhit. Trong cc nguyn t, Ion, v
khn, c bit l trong vng ph kh kin. V d: Khi xc nh Gd-4184,26 th hon ton b bng CN che
c phn t trng thi hi cng c th c kch thch n pht sng v cng ca vch ph pht x do
lp. Nhng nu kch thch ph trong mi trng kh quyn kim tra ca hn hp Al (80%) v oxy (20%) th
cc nguyn t pht ra c dng xc nh nng
ca
vch ph ca Gd l mt vch nhy, r nt v rt thch hp cho phn tch Gd trong nn t him.
n
u im th hai l khi kch thch ph trong mi trng kh quyn kim tra, trong nhiu trng hp
trong
cng ca vch ph c tng ln r rng. y chnh l mt bin php tng nhy ca phng
mu
php phn tch. Vic xc nh Sm, Eu l mt v d v ngha ny (bng 6.5).
phn
tch, v
cng6.5
vch pht x ca mt nguyn t ph thuc
Bng
So snh kt qu trong hai mi trng kch thch ph
vo
nng
ca
trong
mu
phn tch.
Nguyn
t
Mi
trng
kh ca mtMi
trng
quyn
Nhng
trong nhiu
trng hp
cng
khng
vch ph
nguyn
t kh
trong
mukim
phntra
tch khng
nhng ch ph thuc vo nng ca n, m cn b nh hng bi nng ca cc hp phn khc c
Cng
nhy
Cng
nhy
trong mu phn tch. Nht l khi trong h c cha nhiu nguyn t v thnh phn phc tp m nguyn t
cn xc nh liEu
l nguyn
tng h gia cc120
hp phn trong0 ,mu
phn tch.
4435,60t vt. l
67yu t nh hng
0,0004%
0001 %
c bit l khi thm vo mu phn tch mt s hp cht ph no th ngi ta c th lm thay i cng
Sm 4424,34
65
0,0008%
104
0,0003%
vch ph ca cc nguyn t. Cc cht thm vo c gi l cht ph gia. Nhng cht khi
thm vo
lmph
thaytrong
i thnh
phn ca
v qua
lm
nh hng
thnh
phnvch
ca yu
ph li
v
Khimu
kch
thch
mi trng
khmu,
tr ph
ca
mu
thng
c nnn
sng,
nhiu
cng
khng
ca vch
ph.
CcDo
cht
th lm
hay cng
c thhn
lmsotng
vch
phthch
ca
bin
mt,
xut
hin.
ph
phgia
thucc
ca gim
mu thng
t vch
vicng
trnghp
kch
mt nguyn
trong
khng t.
kh.S d nh vy l v s thay i thnh phn ha hc ca mu thng nh hng n mi qu
trnh trong khi kch thch ph, nh:
Trong nhiu trng hp vic kch thch ph ca mu phn tch trong mi trng kh tr li to ra s
thaylc
ithun
nhitli
i
plasma,
bay hiS
chn
vi nguyn t phn tch. iu ny rt c ngha khi phn tch nhng mu c
thnh phn
tp, cng
nhtthch
Thayphc
i nng
in
(Pe)hp.
trong plasma,
Mt u im na l vic kch thch ph trong mi trng kh quyn kim tra trong nhiu trng hp
S khuch tn v chuyn vn ca cc phn t,
cn c kh nng loi tr c nh hng ca nguyn t c s ca mu (matrix effect). ng thi theo
Cc phn ng ha hc in cc v plasma,
nhng kt qu nghin cu ca V. F. Fassel th vic kch thch ph trong mi trng kh quyn tr cn c tc
Quch
trnh
hachihin
catng
cht mu,
dng hn
c
t o ca nhiu vch ph nhy. V th vng tuyn tnh rng hn. Tt
nhin bn
cnhhi
nhng
u im
th vic
S bay
v nguyn
t ha
cht kch
mu,thch ph trong mi trng kh kim tra cng c nhng kh
khn nht nh, nh cn c kh tr, oxy tinh khit cao (>99,99%), cn c nhng trang b ph tr. V th,
Thi gian tn ti ca cc phn t trong plasma,
ngy nay trong php do ph pht x hin i ICP-AES, ph pht x ca mu lun c kch thch trong
S Ion
s phn li ca cc cht,
mi trng
khha,
tr argon.
S kch thch ph ca cc phn t trong plasma.
Trong tt c cc thay i th s thay i p lc in t (Pe) v nhit ca plasma l yu
t
chnh, c tnh cht quyt nh. Cn cc thay i khc ch l hu qu ca hai thay i ny.
112
113
Nhm 1: Cc mui halogen ca kim loi kim v kim th: Lia, LiF, NaCl, NaF, CsF,
CsCL, AgCl, CaF2, CaCL2, MgCl2,... v mt vi kim loi nng Ti, Sb, Sn, Ga,...
Nhm 2: Mt s oxit kim loi, nh oxit ca Ga, Sb, Sn, Ti, Mg, Al, Fe,...
Nhm 3: Mt s mui cacbonat, borat ca kim loi kim v kim th, nh Na 2CO3,
Li2CO3, LiBO2, BaCO3,...

Nhm 4: Mt s halogen ca hp cht hu c, nh CF4,.
Nhm 5: Cc n cht v hp cht ca lu hunh: S. CaSO 4, SrSO4,.
Nhm 6 : Cc hp cht ca Si: SiO 2, Na2Sio3,...
Cc cht ph gia ny c th lm tng hoc lm gim cng ca vch ph ca mt

nguyn t. Song mt cht ph gia c th c mt hay nhiu chc nng khc nhau khi chng
c thm vo mu phn tch. N c th l cht m, cht mang mu, cht chy, cht pha
long, cht tr lc cho s ha hi v bay hi ca mu,... ngha l ty tng trng hp c th
m nhng vai tr no l ch yu.
Cht m. L nhng cht khi thm vo mu c tc dng n nh mt iu kin nay mt
qu trnh no trong s kch thch ph. V d m cho nhit plasma, m cho p lc in

t trong plasma. in hnh cho loi cht m l bt than quang ph. Bt than quang ph
khng nhng c tc dng m nhit cho plasma, m cn lm cho s bay hi ca mu c
d dng v n nh. Mt khc n cn gi cho plasma c nhit cao thch hp i vi s kch
thch ph ca nhiu nguyn t. V th n rt cn v quan trng i vi php phn tch cc mu
bt v mu khng dn in. V d: Khi phn tch cc mu qung, t , oxit,... ngi ta
thng nghin chng thnh bt v sau trn vi bt than quang ph theo mt t l thch hp.
Ngoi bt than, mt s mui halogen ca cc kim loi kim cng l cc cht m quang ph,
nh CsCl, CsF, LiF, LiCl,... Nhng cht ny c tc dng m cho p lc in t (P) trong
plasma t thay i trong qu trnh kch thch ph. Tt nhin ngoi tc dng m, cc halogen
ca cc kim loi kim v kim th cn c tc dng duy tr v n nh dng in qua ct kh
ca plasma.
Cht mang. Trong nhiu trng hp khi thm cht ph gia vo mu th s ha hi v
nguyn t ha ca cc hp phn trong mu li d dng hn, nhanh hn, hoc n nh hn.

Nhng cht ph gia c tc dng nh th c gi l nhng cht mang. N thng l nhng
cht d ha kh, d bay hi. V th khi vo trong mu, n bay hi c th ko theo c cc hp
phn mu bay hi, hoc tc dng vi cc hp phn ca mu to thnh nhng hp cht mi d
ha hi. Chnh v th m mu bay hi tt hn. Tiu biu cho cc loi cht ny l cc mui
halogen v cacbonat ca cc kim loi kim v mt vi kim loi kim th nh CsF, CsCl, LiF,
LiCl, NaF, NaCl, Li2Coa, Na2CO 3, CaCO3, SrCO3, BaCO3. ng thi c bt than quang ph
cng c tc dng ny rt r rt khi phn tch cc mu khng dn in. Ngoi ra, mt s oxit d
bay hi ca mt s nguyn t nh Ga, Sb, cng l nhng cht mang. Cc cht mang ny trong
nhiu trng hp cn c tc dng lm tng cng vch ph.
114
Cht tr lc cho s t chy, ha hi mu. Thng thng khi phn tch cc

mu bt, c bit l cc mu khng dn in, nh cc mu qung, t , khong st, thng chin tng
kh t
chy mu, kh ha
hi v
bayhithng khng
nh. Khi cng vic phn tch gp kh khn v kt qu thu c khng lp li tt Lc ny ngi ta
thng thm vo mu nhng cht lm cho s chy, s ha hi v nguyn t ha ca mu c d dng
hn. Nhng cht nh th c gi l cht tr lc cho s bay hi ca mu. Cht in hnh cho loi ny li l
bt than quang ph hay bt graphit quang ph. Sau l bt lu hunh, bt oxit nhm. Nhng bt lu
hunh v bt xit nhm khng th dng ring mt mnh, m phi lun lun dng cng vi bt than. V th
ngi ta gi bt than quang ph l mt cht ph gia vn nng.
Cht dn in. Khi phn tch cc mu khng dn in, vn n nh dng
in qua ct kh ca plasma h quang hay tia la in l mt yu t rt quan trng. V nu khng, s phng
in khng n nh v iu ny s a n nhng kt qu phn tch khng tt. Nguyn nhn chnh l do
trong nhng trng hp trong plasma khng c nng ln v n nh ca cc phn t mang in
tch dng v nm ( Ion dng v in t). V th ngi ta thng thm vo mu phn tch nhng hp cht
d bay hi ca cc kim loi d b Ion ha (c th Ion ha thp). Nhng cht c gi l nhng cht dn
in. i din cho nhm cht ny l cc mui halogen ca cc kim loi kim nh CsF, CsCl, LiF,... Nh c
nhng cht ny dng in qua ct kh c n nh, v qua cng lm chos phng
s
kch thch ph
in,
trong plasmacng
c n nh. S d nh vy l v nhng cht ny cung cp cho plasma mt nng ln ca Ion

dng v in t, m yu t khc (s b sung khc) v in tch nm v dng l khng ng k, ngha l
duy tr dng in n nh qua ct kh ca plasma.
Cht pha long. L nhng cht khi thm vo mu phn tch c tc dng lm long nng ca cc
hp phn trong mu, nhng li khng nh hng n cng vch ph ca nguyn t phn tch, ngc
li c khi cn lm tng cng vch ph phn tch. Thc t chng minh rng, trong hu ht cc trng
hp phn tch cc mu qung, khi pha long mu bng bt than quang ph, mui halogen kim loi kim,
th cng vch ph ca cc nguyn t cn xc nh ch c tng hoc khng i. Ngoi bt than quang
ph th mt s mui cacbonat, halogen ca kim loi kim v kim th, mt s mui sunfat kim loi kim
th, mt vi oxit, v d nh Li 2COa, Na2CO3, LiF, LiCl, BaCO3, CaCO3, CaSO4, SrSO4, SiO2, . . . cng
thng c dng cng vi bt than quang ph theo nhng t l thch hp. Tc dng ca cht pha long l
lm cho ph ca mu n gin hn v d quan st. Trong mt s trng hp cht ny c tc dng kh bt
ph ca nguyn t c s, lm tng cng vch ph ca nguyn t phn tch (bng 6 ).
Cht chy. L nhng cht d nng chy, c tc dng lm cho mu d nng chy v d ha hi. V d
nh LiBO2, cc mui hydropyrosunphat ca kim loi K v Na hay Li. i vi mt s mu c thnh phn
phc tp, nh cc mu qung a kim
115
loi
kimvthng
cha nhng
gy ra
nguyn
s bay
t hi
dng
chn
hplc
chtca
bnnhng
nhit, kh
nguyn
bay hi
t vt
ngi
trong
ta phi
muthm
c kh
vo mu
nngphn
to
tch
vi cc
cc cht
halogen
chy theo
nhng
nhng
hptcht
l ph
dhp
bayvi
hi.
mc
Trong
ch h
nhng
thp nhit
trng
nng
hp ny
chythng
ca muko
v lm
theomu
s
d
tng
baycng
hi. Ngoi
ca
tc dng
vchy,ph.
nhng
cht
l iu
chy c
kin
nhiu
thun
trng
lihp
trong
cn php
lm tng
phn
cng
tchnguyn
vch ph
tca
vi
nguyn
lng. t
cn
cng
nghin
l u
cu.
im
V d
ca
nhcht
LiBO2
phtrong
gia. bng 6 .6 .
Hng II. Ngi ta s dng cht ph gia nhm mc ch lm thay i cc qu trnh
Bng 6.6
chnh
s pha
phng
in
Vai trtrong
ca cht
long
muv kch thch ph ca mu. V d: S ha hi, s kch thch ph ca
mt hp phn trong plasma vi mc ch c th lm tng hay gim mnh cng vch ph
ca mt nguyn t. Nhng kt qu nghin cu n nay chng minh rng, nhng yu t gy
ra cc thay i trn phi l cc phn ng ha hc trong in cc v trong s bay hi ca mu
STT
Mu + cht pha long t l: (gng)
Cng vch ph
khi c mt ca cht ph gia.
Mu
Bt than
nm
Trong cc cht ph gia
th cc halogen
ca kim loiLiBO2
kim v mt s Fe-248,30
kim loi kim
th c
1
0
0
0,140ca cht ph
ngha ln i
vi mc ch1 ny, bi v s c
mt mt lng
ln v ph hp
2
1
1
gia nh th trong
mu phn tch
lm thay 1i tt c cc qu
trnh trong in0,230
cc v trong s
kch thch ph3 ca mu.
280
4 nhit v p1 lc in t trong
3 plasma l cc1 yu t chnh, quyt
0,260
Trong
nh cc yu t
khc. Nhng thay i cui cng dn n s thay i cng ca vch ph.

Cht kh nn. Trong mt s trng hp phn tch quang ph pht x, nh cc mu qung, th ph
Tc dng ny c th l dng v cng c th l nm, ty thuc vo tng trng hp c
thu c thng c nn ph lin tc rt en, nht l khi kch thch ph bng h quang. C khi nn ny che
th. Tt nhin trong thc t phn tch ngi ta lun lun chn tc dng no c li cho cng
lp mt c nhng vch phn tch c cng nh. Trong nhng trng hp nh vy ngi ta phi thm
vic phn tch, nh lm tng cng vch ph ca nguyn t phn tch v lm gim cng
vo mu nhng cht c tc dng lm gim bt nn ca ph lin tc. Nhng cht c tc dng nh th c
vch ph ca nguyn t nn.
gi l cht kh nn. Cht thuc loi ny thng l mt s mui sunphat ca kim loi kim th v mt vi
V mt ha hc, khi thm cht ph gia vo mu phn tch tt nhin c nhiu phn ng
oxit: CaSO4, BaSO4, SrSO4, SiO2, Al2 O3. Nhng cht ny c th dng ring bit hay ng hn hp ca hai
ha hc khc nhau xy ra, c phn ng chnh, c phn ng ph. Nhng c th tm chia thnh
cht vi nhau, nhng chng cng phi c ng cng vi bt than quang ph. V d: Khi xc nh V v
my loi phn ng sau:
Ni trong du m, ngi ta thng dng SiO2 hay SrSO4 thm vo mu khi tro ha mu du. Nhng cht
Phn
ng
oxylha;
ny va
c tc
dng
cht gp, cht bo v hay l n nh qu trnh tro ha trnh mt mt, mt khc li
chnh l
cht ng
kh bt
nn khi
ghi ph ca mu tro du .
Phn
sunfua
ha;
Trn y l mt s tc dng quan trng ca cht ph gia, nhng s trnh by v phn loi nh th
Phn ng cacbua ha;
ch l tng i, v trong thc t mt cht ph gia c th biu l ng thi nhiu chc nng v tc dng
Phn
halogen
ha; nng chnh, c chc nng ph. V d nh bt than quang ph va l cht
cng mt
lc.ng
Trong
c chc
m, va
l cht
tc dng
mcc
caphn
n l t,...
chnh. V th ngi ta thng gi bt than quang
Phn
ng mang.
phn liNhng
v phn
hy ca
ph l Trong
cht m
quang
cc
loiph.
phn ng th phn ng halogen ha l quan trng nht v c ngha
phvgia
c phn
nhiu ng
tc dng
nhau,phn
nn khi
dng
ngi
thng
phthp
t nhng
thc tCht
nht,
nh
ny khc
cc hp
casmu
dnha
hi,tac
bitxut
l cc
phn
mc ch
khc
Nhng
ccng
th khi
qut
theoph
hai ca
hng
chnh: t phn tch v lm gim cng
lng
vt,
quanhau.
lm
tng
vch
nguyn
vch ph
caI.nguyn
c s
nn.
Hng
S dngtcht
phvgia
nhm mc ch gy ra s bay hi chn lc ca mt s hp phn
trong mu
mgia
boto
choraphp
phn
tchny
thc
dng vca
t kim
kt qu
V d:
cc cht
Chtph
phn
ng
l hin
cc d
halogen
loitt.kim
vVic
mtthm
s kim
loi
ph giath.
l cc mui halogen ca cc kim loi
kim
Ngc li vi phn ng halogen ha, phn ng sunfua ha v carbua ha thng
116
117
to ra cc hp cht bn nhit, kh bay hi, kh nguyn t ha, ngha l gim qu trnh bay hi v
nguyn t ha ca cc hp phn v cui cng lm gim cng vch ph.
V th phn ng ny c s dng kh bt ph ca nguyn t c s.
Xut pht t nhng nghin cu nu, ngy nay trong phn tch quang ph pht x ngi ta
thng s dng cht ph gia khc nhau thm vo mu phn tch vi nhng mc ch sau:
To iu kin lm cho qu trnh ho hi, nguyn t ha mu, kch thch ph n nh, m bo
cho php phn tch t chnh xc v lp li cao, ngha l thu c kt qu tt.
Tng cng vch ph ca nguyn t nghin cu, ngha l tng nhy ca phng php phn
tch c th xc nh c nhng nng nh m khng phi lm giu mu phn tch (bng 6.7 v
hnh 6.4).
Loi tr bt nhng nh hng ca cc hp phn cn tr, nh ph nn lin tc, nh hng ca
nguyn t c s, nguyn t th ba.
Pha long mu phn
hng3ca hin 4tng t o,
hocc lm
n gin ph ca
0 tch 1 loi b nh
2
5
((ig/mL)
mu phn tch d quan st nh tnh v nh lng.
Hinh 6.4
iu chnh s bay
caca
mt
s ph
hpgia
phn
theoph
nhng
hng c li cho qu trnh
nh hi
hng
cht
ntrong
cngmu
vch
ca xu
Eu 4435,60
phn tch mt hay vi nguyn t.
Bng 6.7
Phn tch quang ph pht x bn nh lng
nh hng ca cht ph gia n cng vch ph
Phng php phn tch quang ph bn nh lng l php phn tch nh gi gn ng hm
lng (nng ) ca mt nguyn t trong mu phn tch da theo s quan st v so snh en S hay
cng IM ca vch ph phn tch.
Php phn tch quang ph bn nh lng c nhiu phng php khc nhau. Song trong cun
sch ny ch nu hai phng php chnh cn ang c s dng nhiu.
Phng php
so snh
Nguyn
t
Cng vch ph trong iu kin
Nguyn tc ca phng php

ny
mun phn tch bn
nguyn
Khng
phlgia
Cnh
cht lng
ph giamt
thm
vo: t X no ,
trc ht phi chun b mt dy mu u ca n c nng t nh n ln.
CsCl (2%)
LiF (2%)
V d: Dy mu u (mu chun) c nng ca nguyn t phn tch X l Cl, C 2, Ca, C4, C5,
C8.
4424,34 Sm
115
138
134
ng
thi cng
phn tch C x trong cng148
iu kin. Sau tin hnh
4435,60
Eu chun b mu 120
145 ghi ph ca
tt c dy mu cng mu phn tch trong mt iu kin ph hp c chn cho nguyn t X.
4262,10 Gd
90
105
110
Nhng vic quan st v nh gi d dng chng ta nn b tr ph theo th t:
Cl, Cx , C2, Cx , C3, Cx , C4, Cx , C5,. . .
Trn y
l khi qut chung
v tc dng ca cc loi cht ph
gia khc nhau.
Sau khi thu c knh nh ta chn mt vch phn tch ca nguyn t X v so snh cng ca
Song thc t phn tch rt l phong ph v phc tp, nht l khi phn tch cc mu qung c thnh phn
chng trn tt c cc nng xem nng C x nm trong khong
phc tp, nhiu vn cn phi c nghin cu v bn bc thm theo nhng kt qu nghin cu tip
tc hin nay v sau ny na, c bit l qu trnh kch thch ph pht x trong ngun nng lng mi
ICP ca php o ICP-AES.
118
119
Bng 6.8
no
ca cc
mu
ca vch
ph,
cnu.
phng trnh (b) l trng hp o en S ca vch ph trn knh nh.
Ri t cc cp gi tr (As/log C)
V d v
xcvy,
nhmun
Pb theo
phngnng
php
hin vch
Nh
xc
ca mt
t Xtatrong
Nu
hay nh
cng
theo
caC xvch
ph nguyn
phn tch,
quanmt
st mu
nm no
gia,trc
en
hay (VC)
ta en
dngS, ng
chun
ca
vch
- log
nng
vdy
Cghi
th
ta ni
nng Cx tln
hnnng
C2
nhng
li2, Ca,
nh Chn
2 ph
3mu
ht ta
chng
taS phi
chun
bCmt
u
c
X vi
o Ci, C
4,..
h
C(nu
trn
Nna
Ph
(%)
S cha
vch nguyn
xut hin tna
n 2 (A
)
C
ltacc
c th
vit:quang
3 , ngha
knh
my
phnh
thcc
h mu
.V
Cnh
mt
iu kin
phn ;tch.
Song dng 1 ng chun, trong
x trong
Cicng
0,001
2614,20
; 2802,00
2933,06
1thc
v nghim,
2) hay Ix
- C. cn
ng
nyu.
chnh C
l2 < Cx < C3
t nht
ba mu
C2 0,005
Ba vch trn r, c thm vch 2663,17 (m)
cc ng
chun
ngphp
cong
ly
l ni
dung (hay
ca phng
so snh.
V th phng php ny gi l phng php ba mu u, tc l s mu u cn thit
mu) Phng
Cxc
nh ny
nng
CBn
cha
x d
3 0,01
vch
r, c
thm vch
php
ngin,
thctrn
hin.
Nhng
mi 2873,30
khi phn tch mt mu li
dng
mt
ng
chun.
Nhng
trong
thc
t,
ngi
ta
hay
dng
5 mu u, cng v th
bit
phndytchmu
X. u,
Munnh th cng tn nhiu mu
phi ca
ghi nguyn
ph catmt
chun, in cc v
C4
0,05
Nm
vch
trn
r
nt.
phng
ny
c
gitrmt
chungc
l phng
php ng
chun.
th
tath
chphp
cn cm
cc gi
AStn
hay
x thng
mt
gi.
Phng
php
ny
ng dng
phn tch
cc mu dung dch. V
xcc
t
t
nc
k v
nh
kim
loi
trong
ncv
khong,
ttrn
nhin
(hnh
6.5).
Cln
5chun
0,1trc
Nm
vch
rphn
nt v
thm
Sau
khi
b tung
xong
cc
mu
u
mu
tch,
tinvch
hnh2474,38
ha hi, nguyn t ha,
xd,
ng
song hin
song
vi trc honh, n
Phng
php
kch thch
ph,
vvch
ghi ph ca ccSu
mu
trn
theor,
nhng
kin (cn
ph hp
C6 0,5
vch
thmiu
2393,61
m) c chn (theo
ct ng chun ti im A, t im
Nguyn
tc ca
phng php ny da trn c s s vch ph ca mt nguyn t
mt quy
trnh phn
tch).
A ny hC7ng
vung gc vi
trc
1,0
to, nhe,
2401,95;
2443,86
xut hin cng nhiu khi nng Ba
vch
ca u
nguyn
t thm
trong
mu cng
ln, ngha l ng
mt cp
tch o en S hay chn vch phn tch o
honh,Tip
th
ta chn
c c
Cx vch
(nu phn
o I)
vi mi mtC8nng
nht nhBath
c u
mtnhe,
s vch
ph sau
xut
hin trong iu kin th
1,5 o
vch
cc vch
m.
hay
l
logC
S) ri
suy ra
C
x (nu
x
cng
I
theo
mt
trong
hai
phng
trnh
c
bn
trn
ty
thuc
vo
trang
ca
nghim c chn ph hp i vi mt nguyn t trong mt h
ithng
tng
mub nht
cn tm (hnh 6.6).
phng th nghim. Tnh cc gi tr trung bnh ca cng vch ph I, hay en S tng
nh.
T ng chun trn, ngoi vic
V tng
d: nng
nng
0,001%
ca Pb mu, v nu kch thch ph trong iu kin h
ng vi
. Nh
th ta c:
hin: 2614,20; 2802,00; 2933,06;2633,17.
xc nh Cx
Cx chng ta cng c Xut
th xc
o
quang dng 10A th ch c ba vch ca Pb: 2614,20; 2802,00; 2833,06 A xut hin.
nh c h s a trong phng trnh

V
vy
mun
phn
tch
mt
v hPhng
s k php
cngnynh
y; hd s
bhin v c ng dng rt rng ri, c bit l trong
gin,
Bng 6.9. t
Dy no
chun,
ca n
phng
php
ng
chun
nguyn
trc
ht thc
ngi
ta
trong phng trnh (b). C th l:
Mu
Nng
ngnh a
v ta ch
bngmu
ph cc
ln0,0005%
u tin, sau c th
cng
phicht,
chun
b cn
mtlpdy
uvch ph xut hin
Ci
Dy chun
Theo
hnh
6.6a ta
c:X vi nng , v
cha
nguyn
tCht
s dng
bng ny
phn tch nguyn trong cc ln sau, m
khng phi ghi ph li ca
c*
C1(6.11)
C2 , Ca,
C4 , Cphp
Cbn
C7 ,...V
5,
6,
ad:
= tga
0,001%
mu
u.
Trong
hai phng
nh
lng trnh by,
th phng
php hin vch
2
Hnh 6.6
2 c
3
4
5
Cctheo
mu
c*
V
hnh phn
6.6b ta tch
c: Cx 1 , Cx 2, 0trong 1
c s dng rng ri, nht l trong nghnhng
a cht,
phng
php
d thc hin v c
chunv
phn
tch nh
lng
0,005%
cng
kin.
Sau ghi phCoca
Y.biu
= tga tch
v
kXl on
Cht
phn
Ci
C2c3
C3
C4
C5
(a)- Tho quan h I - C;c*(b)- Theo quan h AS - logC
nhiu u im.
cc mu trongOD
iu(6.12)
kin chn.
C4
0,01%
Cc
cht
khcph
(nn,
trng)
tt c cc mu
Quan
st
ph
thuphtmi
c
calng
tt c cc Nh nhau trong
Phn
tch
quang
x dinh
c*
Phng php ny rt thun li khi phn tch hng lot mu ca cng mt i tng, v
nng
xem
mi
nng
bao
c5
0,05%
I
I
Phng
phpng
ngchun
chun l c th xc nh c rtIinhiu mu
ch
cnlxmt
o
2 c*c nng
3 Cx cha
I4 bit.I5
nhiu
vch ph ca nguyn t Iophn
0,1% o ph pht x nh
Phng
php v
ng
da theo phng
trnh c bnc ca php
tch Nhng
xut hin
lpchun
hin
mu phn
tch
vmt
mu bng
u phi
cng
mtS3
iu kinS4v trnScng
o Sx
So ghi ph
Si[ trong S2
5
c,
ch
ra
trong
chng
II
l:
vch
ca
chng
ng
vi
tng
nng
.
mt knh nh. V th nu phn tch nhiu i tng 1m mi i tng0,2%
ch mt hoc hai mu
6
Bng
c
dng
nh,
phn thi
tch gian,...
th
tnny
mu
u,
knh
.............
c7
chnhl im
cha u vit ca
I = a.Cb (a)
X (Cu 3247,54 )
nguyn tphp
sau
ny.
6.8 lhin
mt phng
(Vch phan
phng
ny.
VBng
th xut
php
th tch)
khng i.Song trong nhng
hay
S = y. b.log C + k (b)
v d kin
v xcnht
nhnh
Pb trong
qung
iu
th n
cngtheo
vn l mt phng php c ng dng ph bin v c nhiu
Hnh 6.5
Trong
iu
kin
b:
1,
th
y
l phng trnh ca
ng thng c dng: y= a.x v y: a.x
phng
php
ny.
u vit.
Xc nh Cu trong nc khong theo
+ b.
phng php so snh
Phng trnh (a) l i vi nhng my o c trc tip cng pht x IM
122
120
121
123
6.3.2 Phng php th chun khng i

Nguyn tc ca phng php ny l mun xc nh mt nguyn t no , trc ht
ngi ta cng phi dng mt ng chun nh trong phng php ba mu u.
ng chun ny c gi l ng chun c nh (ng chun khng i). Nhng c
khc l ph ca cc mu u dng ng chun c ghi trn mt knh nh ring, gi l
knh nh c s; cn ph ca cc mu phn tch li c ghi trn mt knh nh khc, knh nh
th hai - knh nh phn tch. Nh vy, mun xc nh c nng C x cha bit, ta phi
chuyn cc gi tr S xl tng ng v cc gi tr S xo ca knh nh c s th mi chiu ln
th chun xc nh C x hay loa Cx c. gii quyt vn ny ngi ta c hai cch
khc nhau:
Cch th nht : Xc nh h s chuyn k theo cng thc:
S
xo k.Sxl
(6.13)
y k c gi l h s chuyn ca gi tr en ca vch ph gia hai knh nh

(knh nh c s v knh nh phn tch) trong cng mt iu kin th nghim.
Mun th trn knh nh phn tch ta ghi li ph ca mt mu u, v d nng Ca.
Nh th trn knh nh c s ta c S xo-3, v trn knh nh phn tch ta cng c S xl-3 v h
s chuyn k s c tnh theo cng thc:
(6.14)
Sau khi c h s k ta em n nhn vi cc gi tr en Sxl trn knh nh phn tch ta
s thu c cc gi tr en tng ng trn knh nh c s dng ng chun. By gi
ch chiu cc gi tr vo ng chun c nh l tm c loa Cx> Ri t suy ra C x.
Cch th hai : T thc t phn tch
I;
khi nghin cu cc ng chun ngi ta thy

rng, trong cng mt iu kin th nghim, i
vi mt nguyn t khi o trn mt cp vch
phn tch, th ng chun dng c t dy
ph ca cc mu u ghi trn cc ln khc nhau
ca mt loi knh nh, u l nhng ng thng
song song vi nhau hoc trng nhau (hnh 6.7),
ngha l cc ng c cng h s gc.
c
Phng php th khng i rt ph hp
i vi php phn tch hng lot mu t ngy
ny qua ngy khc, v trong mi ngy
124
Hnh 6.7
Cc ng chun ca dy mu u theo mi
ngy o
phn Trong
tch chng
ta tr
khng
phi
cc gi
C 1 ,
C2, ghi
C3, ph
C4 lli
nng dc thm vo ca nguyn t phn tch X
ca ton
b dy
mucu,
kim
di
dng mt
hp cht
dngnn
lin tit
kt ph
hpc
nh trong mu phn tch v theo cp s cng.
(I)
thi gian,
mughi
chun
vdy
knh
Sau in
cngcc,
tin hnh
ph ca
munh,
theo nhng iu kin ph hp, chn mt cp vch
ngha
l c tnh kinh t hn phng php
o en S hay gi tr cng I c tng ng. Nh vy ng vi mi nng ta cng s c c
(n)
ng
chun. Tuy th, nhng phng php
nh trong bng trn.
ng chun (Ba mu u) hay phng
n y chng ta dng phng php ngoi suy xc nh nng C x cha bit trong mu phn
php ng chun c nh u ging nhau
tch. Theo phng php ny, xc nh C x chng ta phi dng ng chun theo h to I x - C.
ch u phi chun b mt dy mu u c
Nh vy, nu cng vch ph I x c o trc tip th cng vic s n gin, ta dng ngay c
iu kin ca mu u trong php phn
ng chun Ix - C t nhng gi tr Ix o c. Nhng nu o theo cc gi tr S th chng ta
tch quang ph nh lng. iu ny nhiu
tnh
chuynthc
cc gi
tr
S thnh
Ix tng
khi
khng
hin
c.
c gi
bittr i
vi ng theo cng thc:
.log.I tch
= S c thnh
nhng trng hp mu phn
Hnh 6.8
(6.15)
ng chun c nh (I) v ng chun phn

phn Ri
phc
cha chun
th bit nh
sau tp m
cngchng
dng ta ng
trn Ix - C. ng
chun va dng
tch (II)
c
chnh
xc. thng. N ct trc tung ti im c ta (I x, Cx). By gi mun xc nh C x ta ch
c l
mt ng
Vdi
thng
cng chun
khngth
chun
b c
mt
dy chun
mu u
thnh
v vtC xl..
vic ko
pha
nng
nh,
ng
ny c
s ct
trcphn
honhha
ti hc
mt im
ng
nht
vi trmu
(hnh
l thc
chnh
l gi
nngphn
Ctch.
6.9).t v trong nhng trng hp th nh hng
x cn tm
nguyn
c s
v nguyn
nkhc,
kt qu
phn
iutany
th hin
rsong
khi
Tatcng
c th
xc nht
C xth
theobacch
ngha
l ttch
gcltortr.
chng
k ng
song
xc
nh cc
nguyn
Lctany
chngsong
ta phi
hoc
thay
i nn
ca mu
vi ng
chun
v t t
givitrlng.
I X chng
k ng
song
vi l
trc
honh;
hai ng
ny(modify
ct nhau
matrix)
c hiu
qu,
dng
phng
thm tiu
ti
im nu
B. Tcch
B kny
ng
vung
gchay
vi l
trc
honh,
n ctphp
trc honh
ti Cchun.
x. chnh l gi tr nng
Phng
Cx cnphp
tm. thm tiu chun
Nguyn tc ca phng php thm l mun xc nh mt nguyn t phn tch X no

trong mu phn tch, ngi ta dng ngay mu phn tch lm nn chun b mt dy mu u
bng cch ly mt lng chnh xc mu phn tch v thm vo nhng lng ph hp v
theo tng bc ca nguyn t X. Nu gi mu phn tch c nng l C x th dy mu chun
s l (bng 6.10):
Bng 6.10
Dy chun ca phng php thm
Cht
Co
C1
C2
C3
C4
C5
Cht PT X
Cx
Cx
Cx
Cx
Cx
Cx
X thm vo
AC1
AC1
AC1
AC1
AC1
I4
I5
Cht khccx
Hnh 6.9
o c Ix
0 AC, AC 2 AC 3 AC 4 c (ppm)
Nh nhau tt c
Io
I1
D th chun ca phng php thm
Hay o Sx
So
S1
I3
- Xc nh y: Nguyn tc da theo hai mu
S2
S3
S4
S5
chun bit chnh xc nng v
126
125
d: C1,C2 (C2 > C1).

Nh vy ta c:
AS2 = y.b log C2 + k (a)

AS1 = y.b.log C1 + k (b)
Ly (a) tr (b) ta c:
(AS2 - AS1) = Y.b(log C2 - log C1)
(AS2 -AS1)
Do ta suy ra: Y - _r
"
'
log(C 2 / C1)
v b = 1
Phng php theo 1 mu chun
Khi c mu chun
Trong nhng trng hp n gin, chng ta khng cn pha mt dy chun dng
th chun, m c th tnh ngay gi tr C x nh mt mu chun Cl ca cht phn tch, ngha l
chng ta c:
Vi mu phn tch:
Ix = a.Cx
(a)
Vi mu u:
I1 = a.C1
(b)

Cx = (Ix/Io).C1
(6.17)
Nh vy khi o c gi tr I x v I1 ta c t s ca chng, v ch vic nhn n vi gi tr

Cl l chng ta c gi tr nng C x phi tm theo biu thc (6.17).
Nhng cn phi nh rng, nu o S trc ht phi tnh chuyn cc gi tr AS sang cc
gi tr cng I tng ng ri mi ng dng c phng php ny, gi tr nng chun
Cl v c nng cht phn tch phi nm trong vng tuyn tnh ca php o xc nh cht
m chng ta bit r trc.
Khi khng c mu chun
Ix = a.Cx
(a)
Itch = a(Cx + AC1)
(b)

Cng = [Ix/(Itch - Ix)]AC1
(6.18)
127
Nh vy khi
o c gi trIx v Itch
ta c tnh c nng Cx
phi tm theo
biu thc (6.18).

Nhng cn phi nh rng, nu o S trc ht phi tnh chuyn cc gi tr S sang cc gi tr
cng I tng ng ri mi ng dng c phng php ny v gi tr nng chun Cl v c nng
cht phn tch phi nm trong vng tuyn tnh ca php o xc nh cht chng ta bit.
Trn y l cc phng php nh lng ch yu hay c s dng. Tt nhin mi phng php
u c nhng u im v nhc im nht nh ca n, v ngi dng tu iu kin m p dng cho
thch hp.
Cc phng php xc nh gin tip bng AES
Nguyn tc
xc nh gin tip cc cht khng c ph pht x nguyn t theo php o ph pht x nguyn
t, ngi ta thng da theo mt trong hai nguyn tc sau y v ng vi mi loi nguyn tc ngi
ta c mt kiu xc nh ring nht nh theo bn cht ca cht phn tch.
Cch 1: Cho cht cn phn tch X (cn xc nh) tc dng vi mt thuc th l mui ca mt
kim loi c ph pht x nguyn t trong nhng iu kin thch hp v phn ng ny c tnh cht nh
lng hon ton. V d: xc nh Ion Cl, ngi ta cho mu c Ion Cl tc dng vi dung dch AgNO 3
trong mi trng axit HNO 3 2%, sinh ra kt ta AgCl theo phn ng:
C- + Ag+ = AgCl T
Sau lc hay li tnm ly kt ta AgCl, ho tan n trong dung dch NH 4OH 5% v xc nh hm
ljng Ag trong dung dch ny, ri suy ra nng ln C -, v theo phn ng trn, 1 Ion Cl s tng tc
vi 1 Ion Ag+.
Cch 2: Da theo hiu ng ca cht cn xc nh trong mt vng nng nht nh, n lm
gim hay lm tng cng vch ph pht x ca mt kim loi mt cch tuyn tnh. V d: xc
nh Anion F1- ta o ph pht x ca nguyn t Mg nng
ppm, v trong vng nng Anion F 1- t 2 - 20 ppm, th cng vch ph pht x Mg - 285,20 nm s
b gim mt cch tuyn tnh theo s tng nng F.
Cc phng php phn tch gin tip
Theo nguyn tc th nht

Theo phn ng to kt ta khng tan
Theo loi phn ng ny, ngi ta c th thc hin cc phn ng ha hc c tnh cht nh lng
bit, nh:
To kt ta l mui khng tan
128
Cc phn ng kt ta nh lng trong ha hc th c rt nhiu, v d nh phn ng to

kt ta: AgCl, AgBr, AgI, PbSO 4, BaSO4, v.v...Theo cch ny, ngi ta ly mt lng nht
nh cht mu (theo Vml hay a mg) cho tc dng vi mt thuc th thch hp v d, trong
iu kin nht nh phn ng kt ta xy ra hon ton. Sau li tnm hay lc tch kt ta
khi dung dch, ri thc hin xc nh kim loi theo mt trong hai cch sau:
+ Ho tan kt ta v xc nh kim loi trong kt ta, ri suy ra hm lng cht phn tch
X.
+ Xc nh lng kim loi thuc th d sau khi kt ta ht cht phn tch cn li.
T suy ra lng kim loi phn ng vi cht phn tch X, v tnh hm lng cht
phn tch X.
Cch ny thng c s dng xc nh cc mui: Halgen (F, Cl, Br, I), sunphat
2-
(SO4 ), photphat (PO43-), oxalat (C2O42-), v.v... Sau y l cc phn ng .

C- + Ag+ ^ AgCl xc nh Anion Cl Br + Ag+ ^ AgBr xc nh Anion Br I- + Ag+ ^ AgI xc nh Anion r
C2O42- + Ca2+ ^ CaC2O4 xc nh Anion C 2O42PO4 + Ca2+ ^ Ca3(PO4)2 xc nh Anion PO 4
SO42- + Ba2+ ^ BaSO4 xc nh Anion SO42SO42- + Pb2+ ^ PbSO4 xc nh Anion SO42PO43- + Mg2+ + NH4+ ^ MgNH4PO4 xc nh Anion PO 4
V d: xc nh hm lng Anion Cl - trong nc, ngi ta ly 100 ml mu nc,
thm 5 ml HNO 3 65%, thm 2 ml dung dch AgNO 3 5 mg/mL Ag (lng Ag thm vo l 10
mg), lc u, sinh ra kt ta AgCl theo phn ng:
C- + Ag+ -^AgCl
Lm mui kt ta, sau lc hay li tnm ly kt ta AgCl, ra sch kt ta bng 10ml
HNO3 1%, thu nc lc v nc ra nh mc thnh 100 ml bng dung dch HNO 3 1%, v
xc nh lng Ag d trong dung dch ny bng php o ph pht x ca nguyn t Ag. Nh
th ta tnh c lng Ag, v suy ra lng Ag phn ng vi mun Cl, sau tnh hm
lng mun Cr trong mu nc, v theo phn ng trn, 1 Ion Cl s tng tc vi 1 Ion Ag+.
To kt ta l sunphua khng tan
Mt s cht, v d cc hp cht hu c, dc phm thuc h thioo (c cha Ion S 2-,

trong nhng iu kin thch hp c th tc dng vi mt s Ion kim loi to ra hp
129
cht sunphua khng tan, v cng c s dng xc nh cc cht hu c .

V d: xc nh vitamin B 1 (trong 1 phn t B 1c 1 Ion S2-), ngi ta ly
a mg
mu c B1 cho tc dng vi b mg NaPbO 2 trong mi trng KOH nng chy trong ng

nghim, phn ng sinh ra PbS rt nh lng l c 1 phn t B 1, th bao gi cng to ra 1 phn
t PbS.
1 phn t vitamin Bl + NaPbO2 ^ PbS
Sau ho tan hn hp phn ng trong 20ml dung dch NH 4C11%, lc v ra kt ta
PbS, ho tan kt ta PbS trong 15 ml HNO 3 1/1, nh mc thnh 25 mg v xc nh Pb trong
dung dch ny. Sau suy ra hm lng vitamin Bi trong mu a mg. theo phn ng trn.
Phn ng ny trc y c dng xc nh vitamin B 1, cng nh hm lng
penicillin trong thuc, hay trong cc sn phm thc phm, bng phng php khi lng, nn
ch xc nh c hm lng ln, v tin hnh rt lu cc thao tc kt ta, sy kh, cn kt
qu. Hin nay nh php o ph AES hay AAS, xc nh c c hm lng nh, m li
nhanh.
Theo phn ng kh mui kim loi
y chnh l phn ng trng gng, phn ng kh Ion Ag v Ag + kim loi, dng thuc
th Tulen, l phn ng xc nh cc cht andehit. V th phn ng ny ch yu c dng
xc nh hm lng cc cht c chc andehit trong phn t. Trong phn ng ny, c 1
nhm chc andehit - CHO trong phn t cht, th lun gii phng ra 1 nguyn t Ag.
R- (CHO)n + n(Ag+) ^ nAgo
V th cch ny hin nay c s dng xc nh cc hp cht hu c c
cha
andehit dng R-(CHO)n, ch yu l theo phn ng trng gng.

V d: xc nh hm lng andehit fomic, ta ly V ml mu cho tc dng vi
ml thuc th Tulen, khi un nng nh, qu trnh kh Ion Ag+ xy ra theo phn ng:
HCHO + Ag+ ^ A go
Nh vy, kim loi Ag c gii phng v bm vo thnh ng nghim. Sau loi b
dung dch, ho tan kt ta Ag kim loi bng 10 ml axit HNO 3 1/1 nng, un nh cho tan ht,
nh mc thnh 25 ml, v xc nh Ag trong dung dch ny. Theo kt qu nng Ag, ta suy
ra hm lng andehit trong V ml mu theo phn ng trn.
Theo phn ng ho tan mt kim loi
Mt s cht, m ch yu y l cc axit hu c c kh nng ho tan cc kim loi hot

ng nh Cd, hay Zn rt nh lng, nn cng c s dng xc nh n, theo phn ng
to ra mui tan nh sau:
2R-(COOH) + Zn ^ (R-COO) 2Zn
130
Sau li tnm ly dung dch mui ny v xc nh nng Zn bng php o ph pht x

ca Zn, ri suy ra nng (hm lng) axit R-COOH tc dng vi Zn kim loi sinh ra
dung dch mui Zn(R-COO) 2.
Theo phn ng to hp cht phc bn chit c
Cch ny dng xc nh mt s Anion, hay cht hu c, ngha l cc Anion no c

th tc dng c vi mt Ion kim loi to ra c mt hp cht phc bn trong mt iu
kin nht nh v chit ra c khi dung dch mu, th u c th s dng xc nh cc
Anion .
V d: Xc nh Anion CNS -1 qua phn ng ca Anion ny vi dung dch mui FeCla
Fe3+ + CNS ^ Fe(CNS)
Sau chit phc Fe(CNS) vo dung mi etyl e v xc nh Fe trong dch chit ny
(c th gii chit phc vo dung dch HCI 2M, v xc nh Fe trong dung dch gii chit ny).
Sau ta cng tnh c nng ln CNS trong mu phn tch.
Theo phn ng to hp cht d a
Cch ny thng c dng xc nh P, Si, qua thuc th molipdic trong mi trng

axit nc c 6M, sinh ra hp cht d a ca P vi Mo, m chng ta dng trong phn
tch ha hc xc nh P trong t trng bng phng php trung ha. Cch lm cng hon
ton tng t nh th, nhng y sau khi c c hp cht kt ta d a ca P, ngi ta ho
tan n trong kim 0,5 M v xc nh hm lng ca nguyn t molipden, bng ph pht x
ca Mo, sau suy ra hm lng P trong mu phn tch, theo phn ng sau.
PO4 + NH4+ + MoO42- + HNO3 ^ (NH4)3 [P(Mo3 O10H]
Hp cht d a ca P
Phn ng kh hp cht c nhm Nitro (-NO 2 )

Chloramphenicol, qua chun lng Ion Cd(II) sinh ra trong phn ng hay o ph pht x
nguyn t (AES hay ICP-OES) ca dung dch Ion kim loi Cd(II). V d trong mi trng axit
long (HCl 0,05M), bt kim loi xp Cd kh nhm -NO2 v NH 2 hon ton nh lng theo
phn ng sau.
3Cd + R-NO2 + 6HCl ^ 3CdCl2 + H2O + R-NH2 Chloramphenicol
Nh vy sau khi phn ng kt thc, ly tnm ly dung dch Anion CdCl2 v xc nh Cd
bng php o AES v suy ra hm lng Chloramphenicol theo phn ng trn.
131
Vi cch ny c th xc nh c Chloramphenicol n nhy 0,005 ppm.

Hon ton tng t, nhiu hp cht hu c nitro u c th xc nh gin tip theo php o ph
hp th nguyn t.
Theo phn ng to hp cht hydrua bay hi
y l phn ng ca mt s Anion ca mt s nguyn t vi nguyn t hydro mi sinh to ra
hp cht kh hydrua dng MeHn (vi n = 3,4,5, v 6). V d: HgH 2, AsHa, ASH5, SbH3, SbH5, SeH4,
SeH8, TeH4, TeH 3, v.v... Phn ng ny rt nh lng, trong nhng iu kin ph hp cho mi cht. V
th n cng c s dng xc nh cc nguyn t Hg, As, Se, Te.. trong cc i tng khc nhau,
nh trong qung, trong nc, trong thc phm,.. bng php o ph pht x v hp th nguyn t. Song
trc ht l mu phn tch cn c x l a cc nguyn t ny v dng mui ca Ion tan trong
dung dch nc mi trng axit, v d HgCl 2, SbCl5, SnCl4, Na3AsO4, Na2SeO0, Na2TeO4. Sau thc
hin theo cc phn ng sau:
+ Vi Hg:
HgCl2 + Na2BH4 + HCl ^ HgH
+ Vi As:
ASO43" + Na2BH4 + HCl ^ AsH3

ASO43" + Na2BH4 + HCl ^ ASH5
+ Vi
Se SeO43- + Na2BH4 + HCl ^ SeH4

SeO43- + NA2BH4 + HCl ^ SeH6
+ Vi
Te: TeO43- + Na2BH4 + HCl ^ TeH 4

TeO43- + Na2BH4 + HCl ^ TeHs
Cc kh hydrua sinh ra trong cc phn ng trn c kh argon dn vo h thng nguyn t ha

mu ca my v o ph ca cc nguyn t theo cc iu kin thch hp cho mi nguyn t.
Theo k
thut ny, hin nay ngi ta c ring
mt h phng
php ha hi v
nguyn t ha lnh qua vic to hp cht kh hydrua d b phn hu phc v vic tch v xc nh cc
nguyn t ni trn. Phng php ny c nhy rt cao, c 1-5 ng. Cc hng sn sut my o AES v
AAS u c bn b trang b cho k thut ny vi cc kiu khc nhau, t n gin n hon chnh v t
ng.
Theo nguyn tc hai

Theo tc dng lm gim cng vch ph
Theo cch ny, ngi ta cho cht phn tch X (cn xc nh) tc dng vi dung dch mui ca
mt kim loi c ph pht x nhy mt nng nht nh ph hp v khng i to thnh hp cht
bn, v hp cht ny s lm gim cng vch ph pht x ca kim loi mt cch tuyn tnh trong
mt vng nng nht nh ca cht cn xc nh X, ngha l y chng ta c cng vch ph
(lc ph) c gi tr
132
Phn II
Trongmu
dchta dng
th ph
pht
x ca
hay Cavkhi
mtph
ca
nm.V V
d d:
xc nh
Aniondung
F - ngi
Mg c
nng
2 ppm (2Zr,^g/mL)
oc
vch
-4
-5
glucose,
amino
axit, haynm.
protein,
v.v.lng
trong Fvng
tphp
n. 10
- n.10
mol/l
c c
tng
pht x ca
Mg-285,20
v nh
theonng
phng
ng
chun.
Dyschun
theo
tuyn
tnh.sau.
Tnh cht ny c s dng xc nh glucose trong cc i tng mu
pha theo
bng
sinh hc (hnh 6.11).
Bng 6.11
Bng 6.11
Dy chun xc nh nng Anion F Dy chun xc nh nng Protein
Chng 7
NHNG VN CHUNG CA PHP O ASS
Cc cht
Cc cht
Ng Mg(ppm)
Ng. F (ppm)
Co
2
Co
Ci
C1
C2
C3
Dy chun
C2
2
C3
C4
2
C4
C5
2
C5
Cx
2
Cx
2
4
6
8
10
Cx
2
2
2
2
2
2
Nh chng ta
bit,vt cht c cu to bi cc nguyn t v nguyn t l
0 1 0,021 0,041
0,06
0,08
0,10
Cx
HClProtein
(%) (mm)
1
1
1
1
phn t c bn nh nht cn gi c tnh cht ca nguyn t ha hc. Nguyn t li bao gm
HCl
1khc(khong
1 nhau
1
nh
ht nhn nguyn
t(%)
nm gia v1chim 1mt th 1Cc
tch cht
rt nh
1/10.000
th 1tch ca
S xut hin
ph
hpCa(ppm)
th nguyn t 2
Nng
nguyn t) Cc
v cc
t (electron)Nh
chuyn
ng
xung
ht nhn
trong phn khng gian
I quanh
yuin
t khc
tt c,
nh
cht
o Ix (Mg285,20
nm)
Io nhau Ii
2 mi trng,
I3
I4 m,I5v.v. Ix
ln ca nguyn t. Trong iu kin bnh thng nguyn
t khng thu v cng khng pht ra
I
Io
I
2
I3
I4
I5
Ix
nng lng
dng ccnm)
bc x. Lc ny nguyn t tn ti trng thi c bn. l trng
o Idi
x (Ca-422,70
Sau
dng ng chun v pht hin nng ln F trong mu phn tch Cx
thi bn vng v ngho nng lng nht ca nguyn t. Nhng khi nguyn t trng thi hi
(hnh 6.10).
t do, nu ta chiu mt chm tia sng c nhng bc sng (tn si xc nh vo m hi
nguyn t , th cc nguyn t t do s hp th cc bc x c bc sng nht nh ng
ng vi nhng tia bc x m n c th pht ra c trong qu trnh pht x ca n. Lc ny
nguyn t nhn nng lng ca cc tia bc x chiu vo n v n chuyn ln trng tha
kch thch c nng lng cao hn trng thi c bn. l tnh cht c trng ca nguyn t
trng thi hi. Qu trnh c gi l qu trnh hp th nng lng ca nguyn t t do
trng thi hi v to ra ph nguyn t ca nguyn t . Ph sinh ra trong qu trnh ny c
gi l ph hp th nguyn t.
Nu gi nng lng ca tia sng b nguyn t hp th l XE th chng ta c:
AE = (Cm - Eo) = hv
(7.1)
hay l.
AE = h.c / X
(7.2)
c0 C
C2
c3 c4 c5
trong Eo v Cm l nng lng ca nguyn t trng thi c bn v trng thi kch

Hnh6.11b
thch m;Hnh
h l6.11a
hng s Plank; c l tc ca nh sng
trong chn khng; X l di sng ca
Cc pic ph
vch ph hp th.
ng chun phn tch
Theo tc dng lm tng cng vch ph
Nh vy,
vitng
mi gi
tr nng
lng
t hp
th ta
Cng
honng
ton
t nh
nguyn
tc AE;
ca m
cchnguyn
trn, nhng
c khc
l s
khiccmt
mtvch
ca
ph
hp
th
vi
di
sng
i
c
trng
cho
qu
trnh
,
ngha
l
ph
hp
th
ca
nguyn
t
cht phn tch X th cng vch ph ca nguyn t kim loi li c tng tuyn tnh theo
cng
l nng
ph vch.
s
tng
ca cht phn tch X c trong mu vi mt vng nht nh.
134
135
133
Nhng nguyn t khng hp th tt c cc bc x m n c th pht ra c trong qu

trnh pht x. Qu trnh hp th ch xy ra i vi cc vch ph nhy, cc vch ph c trng v
cc vch cui cng ca cc nguyn t.
Cho nni vi cc
vch ph qu trnh hp th v pht x l hai qu trnh ngc
nhau (hnh
7.1). Theo
phng trnh (7.1), nu gi tr nng lng AE l dng ta c qu trnh pht x; ngc li khi
gi tr AE l nm ta c qu trnh hp th. Chnh v th, ty theo tng iu kin c th ca ngun
nng lng dng nguyn t ha mu v kch thch nguyn t m qu trnh no xy ra l
chnh, ngha l nu kch thch nguyn t:
+ Bng nng lng Cm ta c ph pht x nguyn t,
+ Bng chm tia n sc ta c ph hp th nguyn t.
Trong php o ph hp th nguyn t m hi nguyn t ca mu trong ngn la hay
trong cuvet graphit l mi trng hp th bc x (hp th nng lng ca tia bc x) Phn t
hp th nng lng ca tia bc x hv l cc nguyn t t do trong m hi . Do , mun
c ph hp th nguyn t trc ht phi to ra c m hi nguyn t t do, v sau chiu
vo n mt chm tia sng c nhng bc sng nht nh ng ng vi cc tia pht x nhy ca
nguyn t cn nghin cu. Khi cc nguyn t t do s hp th nng lng ca chm tia
v to ra ph hp th nguyn t ca n.
Qu trnh pht x v hp th ca mt
nguyn t Eo: Mc nng lng trng
thi c bn; cm: Mc nng lng trng
thi kch thch; AE: Nng lng nhn vo
(kch thch);
+ hv: Photon kch thch;
+ hv: Photon pht x.
136
Hnh 7.1
Cng ca vch ph hp th nguyn t
Nghin cu s ph thuc ca cng mt vch ph hp th ca mt nguyn t vo nng C
ca nguyn t trong mu phn tch, l thuyt v thc nghim cho thy rng, trong mt vng nng
C nh ca cht phn tch, mi quan h gia cng vch phhp th v nng N ca nguyn t
trong
hi
cngtun theo
nh lut Lambe Bear, ngha l nu chiu mt chm sng cng ban u l I o qua m hi nguyn t
t do ca nguyn t phn tch nng l N v b dy l L cm, th chng ta c:
KN .L
(7.3)
trong Kv l h s hp th nguyn t ca vch ph tn s v v K v l c trng ring cho tng

vch ph hp th ca mi nguyn t v n c tnh theo cng thc:
( )2
K=Ke2
__A_
v-Vo
RT
( )2
V
(7.4)
Ko l h s hp th ti tnm ca vch ph ng vi tn s v o. A l
nguyn t lng ca nguyn t hp th bc x.
137
R l hng s kh.
T l nhit ca mi trng hp th ( oK).
Nu gi
Ax l cng
ca vch ph hp
th nguynt,
t cng
thc (7.3)
chng ta c:
A =
hay l:
= 2,303.K .N.L
Ax = 2,303.KV.N.L
(7.5)
y A chnh l tt nguyn t ca chm tia sng cng I o sau khi qua mi trng hp th.
A ph thuc vo nng nguyn t N trong mi trng hp th v ph thuc c vo b dy L ca lp
hp th (b dy chm sng i qua). Nhng trong my o ph hp th nguyn t, th chiu di ca n
nguyn t ha hay cuvet graphit l khng i, ngha l L khng i, nn gi tr A ch cn ph thuc vo
s nguyn t N c trong mi trng hp th. Nh vy cng ca vch ph hp th s l:
Ax = k.L
(7.6)
vi k = 2,303.K v.L
trong K l h s thc nghim, n ph thuc vo cc yu t.
H s hp th nguyn t Kv ca vch ph hp th,
Nhit ca mi trng hp th, v
B dy ca mi trng hp th L.
Song cng thc (7.6) cha cho ta bit mi quan h gia cng vch ph v nng C ca
nguyn t phn tch trong mu. Tc l qua h gia N v C. y chnh l qu trnh ha hi v nguyn t
ha mu phn tch. Nghin cu qu trnh ny, l thuyt v thc nghim ch ra rng, mi quan h gia
nng N v nng C trong mu phn tch c tnh theo biu thc sau:
N = 3.1012xFW's'nR C
QT n
(7.7)
y l cng thc tng qut tnh gi tr N trong ngn la nguyn t ha mu theo Winefordner v
Vicker. Trong :
F l tc dn mu vo h thng nguyn t ha (ml/pht),
W l hiu sut aerosol ha mu,
s l hiu sut nguyn t ha,
nR l s phn t kh nhit ban u (ambient), T o(oK), nT l s phn t kh
nhit T(oK) ca ngn la nguyn t ha,
138
Q l tc ca dng kh mang mu vo bung aerosol ha (lt/pht),

C l nng ca nguyn t phn tch c trong dung dch mu.
Phng trnh (7.6) cho ta bit mi quan h gia A v N, phng trnh (7.7) cho
ta bit mi quan h gia N v C. Mi quan h ny rt phc tp, n ph thuc vo tt c
cc iu kin nguyn t ha mu, ph thuc vo thnh phn vt l, ha hc, trng thi
tn ti ca nguyn t trong mu. Nhng nhiu kt qu thc nghim ch ra rng, trong
mt gii hn nht nh ca nng C, th mi quan h gia N v C c th c biu
th theo cng thc:
N = Ka.Cb
(7.8)
trong Ka l hng s thc nhim, ph thuc vo tt c cc iu kin ha hi v

nguyn t ha mu; cn b c gi l hng s bn cht, ph thuc vo tng vch ph
ca tng nguyn t, b c gi tr bng 1 v nh hn 1, tc l 0 < b <=l. Gi tr b = 1 khi
nng C nh v ng vi mi vch ph ca mi nguyn t phn tch, ta lun lun tm
c mt gi tr C = C o b bt u nh hn 1, ngha l ng vi:
+ Vng nng Cx < Co, th lun lun c b = 1, ngha l mi quan h gia
cng vch ph v nng C x ca cht phn tch l tuyn tnh c dng ca phng
trnh y = ax.
+
Vng
nng
Cx
>
Co
th
b lun nh hn 1, tc l b tin v
tt nhin l khng bng 0. Nh
vy trong vng ny mi quan h
gia cng vch ph v nng
Cx ca cht phn tch l khng
tuyn tnh.
Nn
Co
gi
gii
hn
trn ca vng tuyn tnh.

n
kt
hp
trnh (7.6) v (7.8) chng ta c:

Ax = a.Cb
(7.9)
phng
c (ng/mL)
Hnh 7.2
Mi quan h gia cng vch ph A\ v nng cht cx
AB: Vng tuyn tnh(b=1), BC:Vng khng tuyn tnh (b<1).
trong a = K.K a v c gi l hng s thc nghim, ph thuc vo tt c cc iu kin thc

nghim ha hi v nguyn t ha mu, nh trnh by trn. Chnh do thc t ny m trong mt
php o nh lng xc nh mt nguyn t phi gi cho cc iu kin ha hi, nguyn t ha mu n
nh v khng i. Phng trnh (7.9) c gi l phng trnh c s ca php o inh lng cc
nguyn t theo ph hp th nguyn t ca n. ng biu din ca phng trnh ny c 2 on, mt

on thng (trong on ny b = 1), v quan h gia Ax. v C l tuyn tnh) v mt on cong, trong
on ny b < 1 (hnh 7.2).
139
d
7.3 Cu
ca
vch
hp
th
nguyn
t tgp
Stark
ca
trc
cu
rng
trckp,
nguyn
Hph
"t.
khc
Hiu
vi
ng
nyrng
cng
nhin,
phn
lmrng
tng
kprng
li ca
c
vch
quyt
ph hp
nhth.
biDo
s
Cc
vch
ph
hp
th
nguyn
t
cng
c
cu
trc
nht
nh
nh
cc
vch
ph
chuyn
ngy
nhit
carng
nguyn t t do trong mi
trng
hp th nguyn
theo hng
,
mt cch
,
ca vch
phhp
t phicng chiu hay
l:
pht
tng
vi ng
n. ca
Nhng
vchtrong
ph mi
hp trng
th thng
n ny
sc ph
nh thuc
vch
ngcxchiu
ving
chuyn
phtn
. V khng
th rng
H
t
=
(H
n
+
H
d
+
H
l
+
H
c
)
(7.13)
ph
iu
l hp
rng
ca vch
ph ng,
hp th
lnc
hn tnh
theo
rng
nhiupht
vox.
nhit

ca c
mingha
trng
th. Mt
cch gn
thng
rng kp
ca
vch
ph pht
x tng
ng (hnh
7.3).
y
lthc:
cng
thc
tng qut
y
cng
cho
rngrngcavch
vch ph
hp
th-5 th
hp
Hph
= 1,76.10
.v Vt/A
(7.11)
nguyn t. Nhng trong thc t ca
c xc nh bi nhiu yu t v
php o
phT hp
th nguyn
y,
l nhit
t,
cakhi
mi trng hp th
(oK), A l nguyn t lng ca
n l tng nhiu rng ring phn
khng
tcth
dng
cav t
trng
nguyn c
t hp
bc x
v o l
tn s trung tnm ca vch ph hp th.
ca cc yu t khc nhau, mt cch
ngoi v vi cc my quang ph c
vy,
rng kp ph
thuc
vo ba yu t T, A v v o. Ni chung, rng ny ca
tngtnNh
qut,

rng
phnth
ca
sc nh
hn 2ton
/mm,
l
hu ht
cc th
vch
nguyn t thng nm trong khong t n.10 -3 n n.10-1 cm-1
vch
ph
baoph
gmhp
ccth
rng,
thuyt
vhp
thc nghim
ch
ra
(bng
7.2).
rng
chung
ca mt
rng
t nhin,
Hn. vch ph hp th
Bng
ch
do7.2
ba thnh phn u (chim trn
rng kp, H d.
95%) ca biu thc (7.13) quyt
rng kp ca mt s vch ph hp th
nh; rng Lorenz, HL.
Hnh7.3
~ , ,
rng ca vch ph pht x (w1) v hp th (w2)
TT
ngha l chng ta c:
rng cu trc tinh vi, Hc.
= (Hn + Hd + Hl)
(7.14)
Vch ph (nm) Nguyn H
tt lng
rng Hd cc nhit khc nhau ( oK).10-2 cm-1
Tc l:
iu ny hon ton ng i vi hu ht cc vch ph cng hng trong iu
t = (H
+ Hd -+ 3500
Hl +oCHcv
) p sut l 1 atm. y, phn
kin mi trng hp th c nhit H
t n1600
2500oC
3000oC
3500oC
t Htrn,
rng t nhin Hn c quyt

n. Trong
trung
tnmrng
ca vchtnhin,
ph l Hdo
rngbn
t yu
nhin
n v rng kp H d quyt nh, phn
nh
bi
hiuquyt
s ca
bc
chuyn
lng ca nguyn
t trng thi c22,00
bn v trng
rng
Lorenz
nh
(hnh
7.4).
Li-670,80
7 gia hai mc nng
5,70
9,10
thi kch thch. rng ny ph thuc vo thi gian lu ca nguyn t trng thi kch thch, v c
B -249,80
1,20
22,00
48,00
Trong tng rng11 ,
tnh theo cng thc:
rng Hn chim 45- 50 % cn li l
Cs 825,10
ca
rng
133
Hd
(25%)
1,00
Hi
H
1,60
4,00
(7 10)
=
'
(20%). Cn
rngH L:HL
thng
c yu
rng
Lorenz,
t th ba gp phn m rng rng ca vch ph hp th.
trong
k,
tm lnquyt
thi
ca
trng
thiphn
kch thch
s ccmi
trng
hp,hp
khng
ng
chgian
clubi
ngha
rng
ny
c
nh
snguyn
tngttc
ca cc
t khm.catrong
trng
-3
-1
rng
t
nhin
ca
pht
hptrong
th
thng
vt
(bng
7.1). mi trng .
khi
nguyn
t vch
c
mt
th vi
s chuyn
mc
nng
lng
cakhng
nguyn
tqu
hp1.10
th cm
bc x
trong
t
trng
Bng
7.1 mnh.
rng
Lorenz
HL c tnh theo cng thc:
Ngoi
trn,
rng nhng
t nhinnghin
ca mt cu
mt s
vch
ph hp th
HL = 12,40.1023.Po 2J^-( + )
L
so snh rng
ca cc vch
\RTph
AM
(7.12)
v
'
hp th vi nhau ngi ta thng
P.o laf
lc rng
kh vca
M l phn t lng ca kh trong mi trng hp th
dng trong
i lng
nap
-4
2
Vch
ph
hp
th
ng.t
trng
Ni
(cmx
1.10
)
n() ph
l tit
din va chm hiu dng gia nguyn
hpHth
bc
v phn
t kh tc dng
vch
(Wl/2).
vi n trong mi trng hp th. V cu trc hnh hc th rng Lorenz cng c dng ging
l 130 rng
ca vch
na (1/2) ca h s hp th cc i
Hg-253,70
nm ph hp th v tr ng vi mt
0,50
nh rng t nhin.
Kmax (hnh 7.5). Gi tr ny ca vch ph hp th lun lun ln hn ca vch ph pht x tng ng,
Trn y l ba yu t chnh
quyt nh rng ca vch
hp th. Ngoi ra cn c
nm ln
3,50 ph
tc l vch ph hp Na-589,90
th c rng
hn vch ph pht x nguyn
t tng ng vi n, v vch
cc yu t khc, nh s m rng rng do cu trc tinh vi ca lp v in t ca nguyn t.
ph pht x, rng t nhin H n quyt nh n 90% tng rng chung ca vch ph.
V d, khi m hiCd-228,80
nguyn tnm
hp th nng lng c t 2,70
trong mt t trng hay trong mt
in trng, th yu t ny mi th hin r. l hiu ng

142
140
141
7.4 Nguyn tc v trang b ca php o AAS

Phng php phn tch da trn c s o ph hp th nguyn t ca mt nguyn t
c gi l php o ph hp th nguyn t (php o AAS). Nh trong mc 7.1. chng ta
nghin cu, c s l thuyt ca php o ny l s hp th nng lng (bc x n sc) ca
nguyn t t do trong trng thi hi (kh) khi chiu chm tia bc x qua m hi ca
nguyn t y trong mi trng hp th. V th mun thc hin c php o ph hp th
nguyn t ca mt nguyn t cn thc hin cc qu trnh sau y:
Chn cc iu kin v mt loi trang b ph hp chuyn mu phn tch t trng thi
ban u (rn hay dung dch) thnh trng thi hi ca cc nguyn t t do. l qu trnh ha
hi v nguyn t ha mu. Nhng trang b thc hin qu trnh ny c gi l h thng
nguyn t ha mu (dng c nguyn t ha mu). Nh chng ta c c m hi ca
cc nguyn t t do ca cc nguyn t trong mu phn tch. m hi chnh l mi trng hp
th bc x v sinh ra ph hp th nguyn t.
Chiu chm tia sng bc x c trng ca nguyn t cn phn tch qua m hi nguyn
t va iu ch c trn. Cc nguyn t ca nguyn t cn xc nh trong m hi s
hp th nhng tia bc x nht nh v to ra ph hp th ca n. y, phn cng ca
chm tia sng b mt loi nguyn t hp th l ph thuc vo nng ca n mi trng
hp th. Ngun cung cp chm tia sng pht x ca nguyn t cn nghin cu gi l ngun
pht bc x n sc hay bc x cng hng.
Tip , nh mt h thng my quang ph ngi ta thu ton b chm sng, phn li v
chn mt vch ph hp th ca nguyn t cn nghin cu o cng ca n. Cng
chnh l tn hiu hp th ca vch ph hp th nguyn t. Trong mt gii hn nht nh ca
nng C, gi tr cng ny ph thuc tuyn tnh vo nng C ca nguyn t trong
mu phn tch theo phng trnh (7.9).
Ba qu trnh trn chnh l nguyn tc ca php o ph hp th nguyn t. V vy, mun
thc hin php o ph hp th nguyn t, h thng my o ph hp th nguyn t phi bao
gm cc phn c bn sau y:
Phn 1 . Ngun pht tia pht x cng hng ca nguyn t phn tch (vch ph pht x
c trng ca nguyn t cn phn tch), chiu vo mi trng hp th cha cc nguyn t

t do ca nguyn t. l cc n canh rng (HCL), cc n phng in khng in cc
(EDL), hay ngun pht bc x lin tc c bin iu (xem mc 9.1. chng 9).
Phn 2 . H thng nguyn t ha mu phn tch. H thng ny c ch to theo hai loi
k thut nguyn t ha mu. l k thut nguyn t ha bng ngn la n kh (lc ny ta c

php o F-AAS) v k thut nguyn t ha khng ngn la (lc ny ta c php o ETAAAS).
Trong k thut nguyn t ha bng ngn la, h thng ny bao gm:
143
+ B phn dn mu vo bung aerosol ha v thc hin qu trnh aerosol ha mu (to th sol

kh).
+ n
nguyn t ha
mu (Burner head)
t chy hn hp kh c
cha
mu th huyn ph sol kh (hnh 7.6).

Ngc li, khi nguyn t ha mu bng k thut khng ngn la, ngi ta thng dng mt l
nung nh bng graphit (cuvet graphit) hay thuyn Tangtan (Ta) nguyn t ha mu nh ngun nng
lng in c th thp (nh hn 12 V) nhng n c dng rt cao (50-800 A).
Hnh 7.6
H thng nguyn t ha mu trong ngn la
(1) n nguyn t ha mu, (2) Mng bo him, (3) ng thi phn mu tha, (4) ng dn
cht oxi ha, (5) ng dn mu vo bung aerosol ha, (6) ng dn cht chy C 2H2, (7) Vin bi to
bi aerosol.
Phn 3. H thng my quang ph hp th, n l b n sc, c nhim v thu, phn li v chn tia
sng (vch ph) cn o hng vo nhn quang in pht hin tn hiu hp th AAS ca vch ph.
Phn 4.
Hthng ch th tn
hiu
hp th ca vch ph (tc
vch ph hp th hay nng nguyn t phn tch). H thng c th l cc trang b:

+ n gin nht l mt in k ch nng lng hp th (E) ca vch ph,
+ Mt my t ghi lc ca vch ph,
+ Hoc b hin s digital,
+ Hay b my tnh v my in (printer).
+ Hoc my phn tch (lntergrator).
144
l cng
ca
Vi cc my hin i cn c thm mt microcomputer hay microprocessor, v h thng phn

mm. Loi trang b ny c nhim v iu khin qu trnh o v x l cc kt qu o c, v th, tnh
nng ca mu phn tch, v.v... Mt cch tm tt, chng ta c th minh ho mt h thng my o ph
hp th nguyn t nh s trong hnh 7.7.
H gng
H gng
b)
B pht hin
=Q
Ngun
H gng
H gng
a)
______________________________________________________________________
Hnh 7.7
S nguyn tc cu to h thng my AAS.
a) H 1 chm tia; b) H 2 chm tia
1- Ngun pht tia bc x n sc; 2- H thng nguyn t ha mu; 3- H thng n sc v
detetctor; 4- B khuch i v ch th kt qu o; 5- Microcomputer.
Nhng u v nhc im ca php do AAS
Cng nh cc phng php phn tch khc, phng php phn tch ph hp th nguyn t cng
c nhng u im v nhc im nht nh. Cc u im v nhc im l:
Php o ph hp th nguyn t c nhy v chn lc tng i cao. Gn 60 nguyn t ha
hc c th c xc nh bng phng php ny vi nhy t 1.10 -4
145
l mt
u5im
lnbit,
ca php
odng
ph hp
th nguyn
n
1.10"
%. c
nu s
k thut
nguyn t.
t ha khng ngn la th c th t n
-7
nhy
Chnh
vny
c
nhy
cao,
phn
nyphn
c
un.10
im %
th(bng
ba ca7.3).
phng
php
l cc
ng
tcnn
thcphng
hin nhphp
nhng.
Cctch
kt qu
tch
s
ribng
tronggiy
nhiu
xc
lng
ccvikim
l trong
li dng
c thrt
ghirng
li trn
hay lnh
gin vc
lu
ginh
li sau
ny.vt
Cng
ccloi
trangc
thitbit
b hin
nay
phn
vi lng
trong
tng
mut ytrong
hc,mt
sinhmu.
hc,Cc
nng
ngitch
ta ccc
thnguyn
xc nhtng
thi hay
lincc
tipi
nhiu
nguyn
kt nghip,
qu phnkim
tch
tra
ha
chtsaicsnh.
tinhTrong
khitnhiu
cao. trng hp sai s khng qu 15% vi vng nng c 1 - 2
li cc
rt n
nh,
Bng
7.3 na, bng s ghp ni vi my tnh c nhn (PC) v cc phn mm c hp qu trnh o v
ppm. Hn
x lnhy
kt qu
nhanh
v d
lu li
ca s
cc
nguvn
t dng,
theo php
ong
AAS chun cho cc ln sau.
Bn cnh nhng u im, php o ph hp th nguyn t cng c mt s hn ch v nhc im
nht nh.
ch trc ht l mun thc hin
php o ny cn phi c mt ETA-AAS
h thng my AAS
Noiu hnNguyn
F-AAS
t
tng i t tin. Do nhiu c sFlame
nh khng
xy dng phng
th nghim
v mua
iu
nhykin
(p,g/mL)
nhy
(ng/mL)
sm my mc.
01
(nm)
Ag-328,10
AA
0,05
0,10
Mt khc, cng chnh do php o c nhy cao, cho nn s nhim bn rt c ngha i vi
02
Al-309,30
NA
0,10
0,50
kt qu phn tch hm lng vt. V th mi trng khng kh phng th nghim phi khng c bi.
03
Au-242,80
AA
0,05
0,05
04
Ba-553,50
NA
0,10
0,50
05
Be-234,90
NA
0,10
0,30
06
Bi-223,10
AA
0,10
1,00
AA
qua cng07tc chunCa-422,70
b v o to cn b.
0,05
0,05
0,03
0,04
Cc dng c, ha cht dng trong php o phi c tinh khit cao. cng l mt kh khn khi ng
dng phng php phn tch ny. Mt khc, cng v php o c nhy cao nn cc trang thit b my
mc kh tinh vi v phc tp. Do cn phi c k s c trnh cao bo dng v chm sc, cn
cn b lm phn tch cng c thnh tho vn hnh my. Nhng yu t ny c th khc phc c
08
Cd-228,80
AA
Nhc im chnh ca phng php phn tch ny l ch cho ta bit thnh phn nguyn t ca
09 mu phn
Co-240,70
AA
1,00V th n ch
cht trong
tch m khng ch
ra trng thi lin 0,10
kt ca nguyn t trong mu.
10 php phn
Cr-357,50
AAhc ca nguyn t
0,10
l phng
tch thnh phn ha
m thi.
0,80
11 v phmCu-324,70
AA
i tng
vi ng dng ca AAS
0,05
0,04
12 tng chnh
Fe-248,30
AAphn tch theo ph
0,08
i
ca phng php
hp th nguyn t l phn0,10
tch lng nh
13 cc kimK-766,50
10cc trang b
(lng vt)
loi trong cc loiAA
mu khc nhau ca0,05
cc cht v c v hu c. 0Vi
v k thut
bng phng phpAA
phn tch ny ngi
ta c th nh lng c0,10
hu ht cc kim
14 hin nay,Mg-285,20
0,03
loi (khong
t) v mt s AA
kim n gii hn nng
bng k thut F15 65 nguyn
Mn-279,50
0,05 c ppm (micrgam) 0,06
AAS, v16
n nng
ppb (nanogam) bng
15%.
Na-589,60
AA k thut ETA-AAS
0,03vi sai s khng ln hn0,05
Trong
10 nm tr li y,AA
phng php phn0,10
tch ph hp th nguyn t 0,10
c s dng
17 khong
Ni-232,00
xc nh
loi trong cc mu AA
qung, t, , nc
khong, cc mu ca y hc,0,20
sinhhc,
18 cc kimPb-283,30
0,10
19
Sr-466,70
snphmnng nghip,
AA
0,08
cc
rau qu, thc
0,20phm, nc
ung, cc nguyn t vi lng trong phn bn, trong thc n gia sc, v.v... nhiu nc trn th gii,
20
Si-251,60
NA
0,30
1,00
21
Zn-213,90
AA
0,03
0,10
nht l cc nc pht trin, phng php phn tch ph hp th nguyn t tr thnh mt phng
php tiu chun nh lng nhiu kim loi.
Ghi
Ngn
khnh
+ Axetylen),
Ngn
laxc
(Khi
Bn ch:
cnh AA:
cc kim
loi,la
mt(Khng
vi kim
Si, P, S, Se, NA:
Te cng
c
nhN 2O + Axetylen)
ng thi cng do c nhy cao nn trong nhiu trng hp khng phi lm giu
nguyn t cn xc nh trc khi phn tch. Do tn t nguyn liu mu, tn t thi gian,
khng cn phi dng nhiu ha cht tinh khit cao khi lm giu mu. Mt khc cng trnh
c s nhim bn mu khi x l qua cc giai on phc tp. cng
146
147
bng phng php phn tch ny. Cc kim khc nh C, Cl, O, N, khng xc nh trc tip c bng
phng php ny, v cc vch phn tch ca cc kim ny thng nm ngoi vng ph ca cc my
hp th nguyn t thng ng (190 - 900nm). V d C- 165,701 N-134,70; O-130,20; Cl-134,78; S180,70 nm. Do mun phn tch cc kim ny cn phi c cc b n sc c bit. Cho nn n nay,
theo phng php phn tch trc tip, i tng chnh ca phng php phn tch theo ph hp th
nguyn t vn l phn tch lng nh v lng vt cc kim loi. Cn cc Anion, cc kim, cc cht
hu c khng c ph hp th nguyn t phi xc nh theo cch gin tip thng qua mt kim loi c
ph hp th nguyn t nhy nh mt phn ng ha hc trung gian c tnh cht nh lng, nh phn
ng to kt ta khng tan, to phc, y kim loi, hay ho tan kim loi, v.v... gia kim loi o ph v
cht cn phn tch. y l mt i tng mi, phong ph ang c nghin cu v pht trin.
Vi i tng , khong chc nm tr li y php o ph hp th nguyn t v ang c
pht trin rt nhanh, khng nhng phn tch cc kim loi m phng hng ang pht trin nht
hin nay l nghin cu xc nh cc cht hu c, nh cc hp cht hu c halogen, lu hunh,
photpho. N cng v ang c s dng nh l mt cng c phn tch c lc cho nhiu ngnh khoa
hc v kinh t. Nhiu phng th nghim v php o ph hp th nguyn t c xy dng. Cc hng
trn th gii ch to nhiu my mi c nhiu tnh nng u vit. Cc vin nghin cu khoa hc quc
gia, cc vin nghin cu nng nghip, vin a cht, cc ngnh a cht, cng nghip luyn kim, cng
nghip ha hc, cng nghip ha du, cng nghip thc phm, ngnh y, bnh vin, cc trng i hc
u c cc phng th nghim v php o ph hp th nguyn t. C th ni n nay, hu ht cc lnh
vc ca khoa hc k thut v kinh t u s dng phng php phn tch ph hp th nguyn t.
Ring nc ta, tuy mi tip thu k thut ny trong vng 5 nm, nhng n nay trong ton quc chng
ta cng c gn ba chc phng th nghim v h thng my o ph hp th nguyn t.
148
Chng 8
CC K THUT NGUYN T HA MU
Mc ch v nhim v
Nguyn t ha mu phn tch l mt cng vic ht sc quan trng ca php o ph hp th
nguyn t, bi v ch c cc nguyn t t do trng thi hi mi cho ph hp th nguyn t, ngha l
s nguyn t t do trong trng thi hi l yu t quyt nh cng vch ph hp th v qu

trnh nguyn t ha mu thc hin tt hay khng tt u c nh hng trc tip n kt qu
phn tch mt nguyn t. Chnh v th ngi ta thng v qu trnh nguyn t ha mu l hot ng
tri tim ca php o ph hp th nguyn t.
Mc ch ca qu trnh ny l to ra c m hi cc nguyn t t do t mu phn tch vi hiu
sut cao v n nh php o t kt qu chnh xc v c lp li cao. p ng mc ch ,
nguyn t ha mu phn tch, ngy nay ngi ta thng dng hai k thut. Th nht l k thut nguyn
t ha mu trong ngn la n kh. K thut ny ra i u tin cng vi s ra i ca php o ph hp
th nguyn t. Nhng k thut ny c nhy khng cao, thng l trong vng 0,05 - 1 ppm (bng
. Sau l k thut nguyn t ha khng ngn la. K thut ny ra i sau, nhng li c nhy rt
cao t n 0,1ng (bng 7.3) v hin nay li c ng dng nhiu hn k thut nguyn t ha mu bng
ngn la. Chnh v c hai k thut nguyn t ha mu khc nhau nn chng ta cng c hai php o
tng ng. l php o ph hp th nguyn t trong ngn la (F-AAS: Flame Atomic Absorpt Ion
Spectrophotometry) v php o ph hp th nguyn t khng ngn la (Electro-Thermal Atomizat Ion
Atomic Absorpt Ion Spectrophotometry: ETA- AAS).
K thut nguyn t ha mu bng ngn la
Theo k thut ny ngi ta dng nng lng nhit ca ngn la n kh ha hi v nguyn t
ha mu phn tch. V th mi qu trnh xy ra trong khi nguyn t ha mu ph thuc vo cc c
trng v tnh cht ca ngn la n kh, nhng ch yu l nhit ca ngn la. l yu t quyt
nh hiu sut nguyn t ha mu phn tch, v mi yu t nh hng n nhit ca ngn la n
kh u nh hng n kt qu.
Yu cu v nhim v ca ngn la
Trong php o ph hp th nguyn t, ngn la l mi trng hp th. N c
149
nhim v ha hi v nguyn t ha mu phn tch, to ra m hi ca cc nguyn t t do c kh nng

hp th bc x n sc to ra ph hp th nguyn t. V th ngn la n kh mun dng vo mc
ch ha hi v nguyn t ha mu phn tch cn phi tho mn mt s yu cu nht nh sau y:
Ngn la n kh phi lm nng u c mu phn tch, ha hi v nguyn t ha mu phn
tch vi hiu sut cao, bo m cho php phn tch t chnh xc v nhy cao.
Nng lng (nhit ) ca ngn la phi ln v c th iu chnh c ty theo tng mc
ch phn tch mi nguyn t. ng thi li phi n nh theo thi gian v c th lp li c trong cc
ln phn tch khc nhau m bo cho php phn tch t kt qu ng n. Yu cu ny c lc
khng c tha mn, v nhit cao nht ca ngn la cng ch n 3300 oC. Do vi nhng nguyn
t to thnh hp cht bn nhit th hiu sut nguyn t ha ca ngn la l km.
Yu cu th ba l ngn la phi thun khit, ngha l khng sinh ra cc vch ph ph lm kh
khn cho php o hay to ra ph nn qu ln quy ri php o. Qu trnh Ion ha v pht x phi
khng ng k v qu trnh ny lm mt cc nguyn t t do to ra ph hp th nguyn t.
Mt yu
cuna l
ngn la phi c b dy
ln
c c lp hp th
dy lm tng nhy ca php o. ng thi b dy ca lp hp th li c th thay i c khi cn

thit, o nng ln. Trong cc my hin nay, b dy ny c th thay i c t 2 ci n 10 cm.
Tiu tn t mu phn tch.
to ra ngn la, ngi ta c th t chy nhiu hn hp kh khc nhau, bao gm mt kh oxy
ha v mt kh chy, trong cc n kh thch hp. Nhng vi nhng yu cu ni trn th ch c mt
vi loi n kh l to ra c ngn la tng i ph hp cho php o ph hp th nguyn t. l
nhng mi trng nguyn t ha mu tng i bn vng v kinh t (bng 8.1). c bit c ng
dng nhiu nht trong php o AAS l ngn la ca n kh c t bng hn hp kh: (axetylen v
khng kh nn) hay ngn la ca n kh (N 2O v axetylen), hay (hydro v axetylen).
Bng 8.1a v 8.1b l mt s v d v nhit ca ngn la mt s n kh c dng trong php
o AAS (Ox: cht oxy ha; K.K: khng kh.).
Bng 8.1b
Quan h gia nhit v loi kh t
150
t nng cng vi cc ht sol kh (th aerosol) ca mu phn tch. Phn ny c nhit

thp (700-1200oC). Dung mi ha tan mu s bay hi trong phn ny v mu c
Loi kh
sy nng.
T l kh (l/ph)
Nhit (oC)
Phn K.K
b: L vng trung tm
ca ngn la. Phn
cao, nht l
Propan
6/1,4 ny c nhit 2200
nh b, v thng khng c mu hoc c mu xanh rt nht. Trong phn ny hn hp
K.K
Axetylen
4,2/1,2
2450
kh c t chy tt nht v khng c phn ng th cp. V th trong php o ph

K.K
Hydro
2050
hp th nguyn
t ngi ta phi
a mu vo phn 4/3
ny nguyn t ha
v thc hin
Oxyl ngun n scAxetylen
1/1ca ngn la.
php o, ngha
phi chiu qua phn ny
3000
2900
Phn Nc:2OL v v ui Axetylen
ca ngn la. Vng 2/1,8
ny c nhit thp,
ngn la c
mu vng v thng xy ra nhiu phn ng th cp khng c li cho php o ph hp

Bng
8.1b
th nguyn
t.
Thnh phn
khdo
v cc
nhitc
ngn
Chnh
imla
v cu to nn trong mi php phn tch cn phi kho
st chn c cc iu kin ph hp, nh thnh phn v tc ca hn hp kh

chy K.K
to ra ngn la, Axetylen
chiu cao ca ngn la, v
K.K
Axetylen
Mun
thc
hin
php
ph
hp
4,2/0,7
.v...
1800
4,2/0,9
2000
th
K.K
nguyn
t (F-AAS),Axetylen
trc ht phi chun b4,2/1,1
2300
mu K.K
phn tch trng
thi dung dch. Sau 4,2/1,2
Axetylen
dn dung dch mu vo ngn la n kh
2450
K.K
Axetylen
4,2/1,5
2400
thc K.K
hin php o. Axetylen
Qu trnh nguyn t ha4,2/1,6
trong ngn la gm hai bc k tip nhau.
2300
ha hi v nguyn t ha mu phn tch v
c
immt
v cu
to ca ngn
n mu
kh phn tch
Bc
l chuyn
dungladch
thnh
th cc
nh sng
m trn u
Nhit
l ht
mt nh
thng
s
vi trng
kh mang
kh la
chy.n l cc ht sol
c
ca v
ngn
kh Nhit
(th aerosol).
kh.
ngnQulatrnh
ca ny c gi l
quloi
trnh
hayrtnebulize ha. K
mt
naerosol
kh phha
thuc
thut vo
thc bn
hin cht
qu trnh
ny v hiu sut ca
nhiu
v thnh
n nh
phn
cahng
cht trc
kh tip
cn
tkt qu ca php
o AAS.
chy
to ra ngn la,
ngha lSaung
vi hn
mi hp
mtaerosol
hn cng hn hp kh t vo n (burner head) nguyn t
dn
hp
s hai
c kh t chy to ra ngn la. Thng thng ngi ta hay
ha.kh
Khchy,
mang ngn
l mtla
trong
mt
ha
xc (khng
nh v
dngnhit
kh oxy
khkhi
nn hay kh N 2O). Hai giai on trn c thc hin bng mt
thnh
phn kh
chy
i t ha mu (hnh 7.6). H thng ny gi l Nebulizer System, gm
h thng
trang
b thay
nguyn
thhainhit
ngn la cng b thay i (bng 8.1a v 8.1b). Ngoi yu t trn, tc
phn
chnh:
dn ca hn hp kh vo n t chy cng nh hng n nhit ca ngn la v
qua m nh hng n cng ca vch ph (hnh 8.1).
n nguyn t ha mu (burner head). Cc n ny thng c hai dng khc nhau, hoc
Xt v cu to, ngn la n kh gm ba phn chnh (hnh 8.2):
hnh trn c nhiu l hay hnh mt khe hp c rng t 0,5 - 1,0 mm v 152
Phn a: L phn ti ca ngn la. Trong phn ny hn hp kh c trn u v
151
chiu di 5 cm hay 10 cm.

Loi khe di 10 cm cho hn hp kh t axetylen v khng kh nn; loi khe di
5 cm l cho hn hp kh t axetylen v kh N 2O (hnh 8.3). Cn loi ming trn ch
thch hp cho php o ph pht x.
Phn hai l bung aerosol
ha mu. l bung iu ch
cc ht sol kh ca mu vi kh
mang. thc hin cng vic ny
ngi ta p dng hai k thut theo
nguyn l khc nhau. l k thut
pneumatic-mao dn (phun kh) v
k thut ultrasonic (siu nm). Do
n NTH
ca Perkin Elmer
cng c hai loi h trang b khc
nhau (hnh 8.4 v 8.5) iu ch

sol kh ca mu.
, Hnh 8.3
n NTH
ca Phillips
Cc loi n nguyn t ha mu
Aerosol ha mu theo k thutpneumatic-mao dn.

Theo cch ny ngi ta dng h thng nebulize v kh mang to ra th si kh ca
mu phn tch nh hin tng mao dn (hnh 8.4).
Trc ht nh ng mao dn S v dng kh mang K m dung dch mu c dn vo
bung aerosol ha. Trong bung ny, dung dch mu c nh tung thnh th bi (cc ht rt
nh) nh qu bi E v cnh qut Q, ri c trn u vi hn hp kh t v c dn ln n
nguyn t ha (burner head).
Khi hn hp kh t chy burner head s to ra ngn la, di tc dng ca nhit ca
ngn la cc phn t mu th si kh s b ha hi v nguyn t ha to ra cc nguyn t t
do ca cc nguyn t c trong mu phn tch.
l nhng phn t hp th nng lng v to ph hp
th
nguyn
ca
nguyn t cn nghin cu.
Nhng cn ch rng, ngoi nh hng ca thnh phn kh t v tc dn hn hp
kh n cng vch ph, th tc dn dung dch mu vo bung aerosol ha cng nh
hng ng k n cng vch ph (bng 8.2).
Tc dn mu ph thuc vo nhiu yu t v c tnh gn
ng theocng
thc:
153
(1)
_________________1______________________A.
Hnh 8.4
H thng to soi kh (nebulize) theo k thut pneumatic
K: Kh mang (oxy ha); S- ng dn mu; F- Kh chy; Q: Cnh qut quay u; GMng bo him; A: ng dn th aeresol ln n nguyn t ha.
nrP
V (ml / ph) = nLP
(81)
8Ln
trong :
r- bn knh ca ng mao dn dn mu;
P- chnh lch p sut gia hai u ng mao dn;
L- chiu di ng mao dn;
n- nht ca dung dch mu (g.cm.s).
Bng 8.2
nh hng ca tc dn mu n cng vch ph Cu - 324,70mm
Tc kh (lt/pht)
Cng vch ph
1,00
0,150 '
2,00
0,180
3,00
0,206
4,00
0,225
5,00
0,235
6,00
0,230
Ngha l tc dn mu V ph thuc vo cc tham s r, P, L v n Nhng trong mt h

thng my th r v L thng l c nh, P c gi khng i, cho nn V ch
154
cn ph thuc ch yu vo nht n ca dung dch mu (hnh 8.5).
Aerosol ha mu bng siu nm.

Theo
ha
thut
mu
phn
ny,
tch
ngi
aerosol
ta
dng
h thng siu nm c tn s t 1-4,5

MHz.
Lc
truyn
qua
hay
qua
dung
siu
tng
th
dch
nm
rn
lng
mu
th
(hnh
8.6a)
(hnh
8.6b)
thc
hin
vic
aerosol ha mu, ngha l di tc

dng
ca
lc
siu
nm,
mu
dung
dch cng c phn tn (nh ti)

thnh nhng ht rt nh v trn u
vi hn hp kh dn ln n (burner head) nguyn t ha. y ng knh (d)
ca
cc ht sol kh c tnh theo cng thc:
d = yj (n.s / 4.Di.F2)
(8.2)
trong :
s: sc cng b mt ca dung dch mu;
Di: t trng ca dung dch mu;
F: tn s ca my pht siu nm.
Nh
vy,
mun
cc
ht aerosol nh th phi s
dng tn s siu nm cao.
Tn s v cng sut ca my
pht siu nm u nh hng
n
kch
aerosol
thut
thc
(hnh)
aerosol
ca
Trong
ha,
hai
th
ht
k
k
thut pneumatic l n gin,

trang b r tin, khng phc
tp nh k thut siu nm.
Nhng k thut siu nm c
u
im
cho
nhy
cao
hn. V kch thc cc ht

sol kh kh nh, hiu sut
to sol kh cao v qu trnh aerosol t ph thuc vo kh mang v qu trnh dn mu. c bit l vic
aerosol ha cc dung dch mu c nng mui cao th n u vit hn
155
(cc
mui
ca cc cht)
trong s
ngn
la, v
c
dnnmtip
vo vng
trung
tnmttngn
Tip
s
k thut
pneumatic.
Mt khc,
aerosol
hanbng
siu
thng
cho
lp li
hn la.
(bng
8.3).
nung
Bng nng,
8.3 nng chy, cc qu trnh ha hi v nguyn t ha ca cc ht mu bt kh . y cc
cht s c cc qu trnh chnh sinh ra ph v qu trnh ph khng sinh ra ph din bin theo tnh cht
nhy theo hai k thut aerosol ha mu
nhit ha ca cht mu.
Cc qu trnh chnh: Xy ra thng theo hai c ch chnh:

Nu nng lng (nhit ) ha hi (E h) ca cc hp phn c trong mu nh hn nng lng
Pneumatic
Ultrasonic
nguyn t haNguyn
(E a) catn, tc l E h<Ea, th trc
ht cc hp phn ny s ha hi
dng phn t. Sau
cc phn t khCu
ny mi b phn li (nguyn t0,05
ha) thnh cc nguyn t t do (c0,03
ch I). Hoc cng
c th chng khng
t do, nu l cc hp cht bn 0,03
nhit.
Feb phn li thnh cc nguyn t0,0
Mg
C ch I: (E
h< Ea):
Pb
0,05
0,03
0,08
Ni
0,10
MnAm (l) ^ MnAm (k) ^ n.M(k) + m.A(k)
0,10
Cr
M(k) + n(hv)
0,10 ^ Ph AAS
0,08
0,06
Ni chung,Co
cc mui halogen (tr F), mui
axetat, mt s mui nitrat, mt s0,07
mui sunphat ca
0,10
kim loi thng xy
Cu(Ac) 2, Zn(Ac) 2.
Mn ra theo c ch ny. V d: Cc
0,05 hp cht: CuCl 2, ZnCl2, FeCl3,0,03
v.v... theo c ch 1Znny. C ch ny cho php o 0,03
AAS c nhy cao v n nh.
0,02
Ngc li, nu nng lng phn li E a ca cc hp phn ca mu nh hn nng lng ha hi E h

ca chnh n, th trc ht cc hp phn s b phn li thnh cc nguyn t t do, ri sau mi ha
hi (c ch II).
C ch II (Eh > Eo):

MnAm (l) ^ n.M(r,l) + mA(l.r) ^ n.M(k)
M(k) + n(hv) ^Ph AAS
Cc loi hp cht mui ca kim loi vi -sunphat, -photphat, -silicat, flo, thng theo c ch II.
C ch ny khng n nh, nn php o AAS km n nh, v nhy km hn c ch 1. V th ngi
ta thng thm vo mu cc mui halogen, hay axetat ca kim loi kim lm nn mu hng cc
qu trnh chnh xy ra theo c ch 1 u vit v c li hn.
l hai c ch ca qu trnh nguyn t ha mu phn tch (qu trnh chnh) trong ngn la n
kh. N l nhng qu trnh chnh to ra cc nguyn t t do quyt nh cng ca vch ph hp
th nguyn t ca nguyn t phn tch. Yu t quyt nh cc qu trnh ny l:
+ Nhit ca ngn la;
Nhng+qu
trong
la phn ca mu;
Bntrnh
cht xy
ca ra
cht
mungn
v thnh
Ngn
l nh
mi hng
trngca
nguyn
+ Tc la
dng
cht t
phha
giamu
thmca
vophp
mu.o ph hp th nguyn t (F- AAS). Trong
ngn la c nhiu qu trnh ng thi xy ra: c qu trnh chnh v cng c qu tr nh ph (th cp).
Cc qu trnh ph:
Trong nhit ca ngn la l yu t quyt nh mi din bin ca cc qu trnh .
Trc ht, khi mu th si kh c dn ln n nguyn t ha, di tc dng nhit ca ngn

la, ming n, l s bay hi ca dung mi ho tan mu v cc cht hu c (nu c) trong th si kh.
Nh vy mu cn li l cc ht bt mu rt nh mn
156
157
0C
Bng
8.5 cng
cho
ta
thy rng,
nhit
di
thskh
b
Bn Ha
cnh
ccnguyn
quchng
trnh
chnh,
trongtrong
ngnngn
la la
nckh
thng
cn3 0c00mt
qunng
trnh
hi,
t ha.
ph.
Cc ph
qu pht
trnhxph
ny thng
nhchng
n
vch
ph
nhng
mc
kch thch
l khng
ln v nu
cng ch
gicng
vai tr
quan
trng
itrong
vi cc
kim loi
kim
MeA(r) ^ MeA(l) ^ MeA(k)
khc
nhau, nh lm gim cng ca vch ph, n xy ra nh th no l ty thuc vo nhit
m thi.
caS
ngn
vli,thnh
phn
ca
mu,
v ha,
d nh:
Sla
phn
kcht:
thch,
hpngn
th, la,
Ion
pht
hp
th
ca
phn
Trong
ngoi
ccx.
nguyn t t do cng cn c c cc Ion v cc
t t
phn
tch.
Qutnh
trnh
ny
xy
dng
vivo
ccnhit
nguyn
t
o theo
phn tS Ion
trngha
thica
hi.nguyn
Cc phn
ny
cht
ca
n ra
vd
cng
tyi
thuc
ca
1 Mety
+ A (phn
li)
c
thla,
Ionvng
ha ph
thptav
mc
bcn
Ioncha
loi lng,
nguynstIonlha
tyhay
thuc
vo thch
nhit ph
ca
ngn
quan
st,m
s ca
hp mt
th nng
s kch
ca
1 Meo + vh (hp th bc x)
ngn
thtIon
ca qu
nguyn
.tuy
Nu
th trnh
Ion ha
thcntrng
b Ionhp
haccng
chnh la
cc v
phn
.ha
Nhng
trnh t
ny,
l qu
phcng
nhngnh,
cng
nh
o
MeA
^
1
Me
+
E
(kch
thch)
nhiu.
V th
qutrnh
ngha rt
ln i
ccvo
kimloi
kim
kim
hng n
cng
vchny
phc
ca nguyn
t phn
tch.vi
Thm
l s
hp v
th sau
ca
ccl
htcc
mu
rn
th
o gi.
cha(bng
b ha8.4).
hi. Yu t ny gi l s hp th
1 Me - e ( Ion ha)
Bng
Bng 8.4
8.5
1 Meo +.........
Mc
caph
ccpht
nguyn
t theo
nhit tngn
th Ion
ha ca
n
Mc
b
b Ion
kchha
thch
x ca
cc nguyn
- ngla
vivnhit
khc
nhau
S kh oxy ca oxit bi cacbon.
S % b Ion ha nhit 0C
NguyMeO + CTh
ha (eV)
^ MeIon
+ CO
Nguyn t
Th kch thch
nhit ( 0C). 3000
2000 T s (Nhng)
2500
Cc phn ng ha hc ph khc (hp cht bn nhit monoxit): Me + O ^
Na
Vch ph(nm)
o
K Me
5,21 (ev)
1,00
15,0
26,0
2000
3000
4000
Cs-852,10
1,48
Rb Me + C ^ MeCx 4,06
Na-589,00
Cs
3,872,11
4,40.10-4
7,20.10-3
3,00.10-2
-5
-4
5,90.10
70,0
-3
4,40.10
95,0
Ca-422,70
Ca
6,102,95
1 20.10
2,00 -6
3,70.10
10,0-5
6,00.10
16,0-4
Ba
Zn-213,90
5,505,89
3,00 -13
7,50.10
17,0-10
5,60.10
33,0-8
1,50.10
Al
4,32
10,0
14,0
1,00.10
30,0
6,60
30,5
44,0
0,60
1,00
80,5
89,0
09,0
Mgthnh hp cht bn
7,60
0,30n kh, mt s0,60
05,0
S to
nhit. Trong ngn la
kim loi c th hnh
thnh cc
hp cht bn
dng MeO, nh AlO, Bao, MgO, Beo,
ZrO,... Loi hp 01,0
cht ny rt
Benhit kiu monoxit
9,30
0,30
bn, khi hnh thnh th kh phn li thnh cc nguyn t t do trong ngn la n kh. V th lm
Nh vy, qu trnh Ion ha l lm gim s nguyn t t do trong ngn la, c ngha l
gim nhy ca php o.
lm gim cng ca vch ph hp th. V th cn phi hn ch nh hng ny, bng cch
Cc qu trnh ph tuy c mc khc nhau, nhng trong mt mi tng quan nht nh trong
chn cc iu kin ph hp gi cho nhit ca ngn la n nh v khng qu ln xy ra

ngn la, c bit l nhit ngn la, th tt c cc qu trnh u c th xy ra cng vi cc qu
s Ion ha nguyn t phn tch; hoc thm vo mu Anion ca mt nguyn t kim loi c th
trnh chnh ca php o F-AAS. Do iu quan trng i vi chng ta l phi chn cc iu kin ph
Ion ha thp hn th Ion ha ca nguyn t phn tch hn ch qu trnh Ion ha ca nguyn
hp hn ch n mc nh nht cc qu trnh ph v gi cho n khng i sut trong mt php o
t phn tch.
xc nh mt nguyn t. lmt
phn ca
cng vic
ti uha cc iu
S pht x: ng thi vi qu trnh Ion ha, cn c s kch thch ph pht x ca cc
nguyn
kincho phpo ph hp
th
tt do ca nguyn t
nguyn t trong ngn la.
phn tch di tc dng
nhit ca ngn la. S
nguyn t b kch thch v mc b kch thch ph pht x cng ph thuc vo nng lng
kch thch ph pht x ca tng nguyn t. Nguyn t no c nng lng kch thch ph pht
Bng
8.6 nh th s b kch thch cng nhiu (bng 8.5). Nhit ca ngn la cng cao th
x
cng
cng
b kch thch cng nhiu. loi tr yu t nh hng ny, ngi ta cng thm vo mu
Tm tt cc qu trnh khi nguyn t ha mu
Anion ca cc nguyn t kim loi c th kch thch ph pht x thp hn nguyn t phn tch,
Dn mu vo bung aerosol ha.
qu trnh ny ch xy ra vi nguyn t thm vo .

Qu trnh aerosol ha mu to ra th sol kh.
158 160
159
Hnh
8.8
S cc qu trnh trong ngn la

M1: Kim loi phn tch; M 2: Cc kim loi khc trong mu; A: Anion khng oxy; A xOz: Anion c oxy;
Mo: Kim loi t do trng thi hi; x, y v z nhn gi tr 1,2,3,4,...
161
a) Cc qu trnh trong ngn la ca CaCl 2 khng c PO4
162
cc qu trnh trong ngn la ca CaCl 2 khi c Al Hnh 8.9

V d v cc qu trnh trong ngn la n kh (a, b, c).
Ti u ha cc iu kin nguyn t ha mu
Nh trn chng ta xc nh, nguyn t ha mu l cng vic quan trng nht ca php o
F-AAS. Qu trnh ny thc hin khng tt s nh hng trc tip n kt qu ca php o. Do mun
t c kt qu chnh xc v ng n, chng ta phi kho st, pht hin v chn cc iu kin
nguyn t ha mu ph hp nht cho tng nguyn t cn phn tch trong mi loi mu c th. Cc iu
kin c th l: Thnh phn v tc ca hn hp kh t to ra ngn la. y l yu t quyt
nh nhit ca ngn la. V th qua vic thay i thnh phn v tc ca hn hp kh t to ra

ngn la chng ta c th chn c nhit ph hp ha hi v nguyn t ha nguyn t cn
nghin cu (hnh 8.1 v hnh 8.10) v (bng 8.1).
Tc dn dung dch mu vo h thng nguyn t ha. Ni chung, trong nhiu trng hp

tc dn mu ph hp nm trong khong t 4-5 ml/pht vi php o ca nhiu nguyn t (hnh 8.11).
Chiu cao ca n nguyn t ha. Yu t ny cng nh hng trong mt mc nht nh v

ty thuc vo tng nguyn t (hnh 8.12), nn chn chiu cao ca burner head sao cho c c cng
vch ph ln nht v n nh nht ...
163
C0H2l/niin
C2H2l/min
Hnh 8.10
nh hng ca tc kh chy n cng vch ph
Hnh 8.11
nh hng ca tc dn mu
Hnh 8.12
nh hng ca chiu cao quan st
n cng vch ph
n cng ca vch ph
B dy ca mi trng hp th L: Khi thay i b dy ca lp hp th (mi trng hp

th) chng ta c th tng hay gim nhy ca php o. Ngha l ty theo nng ln hay
nh ca nguyn t phn tch m chng ta thay i gc nghing ca n nguyn t ha mu
(burner head) c c b dy L ca lp hp th ph hp nht. Khi L ln nht ta s c
nhy cao nht, lm gim L th nhy gim theo, ngha l khi o nng ln th ta phi quay
n nguyn t ha mt gc cho ph hp m khng cn pha long, nhng sau cn phi gi
khng i sut trong qu trnh o.
Tn s my siu m: Nu to soil kh mu phn tch trong h thng aerosol ha bng
siu nm th tn s v cng sut ca h thng siu nm cng cn c chn cho ph hp. Yu t
ny cng nh hng n hiu sut nguyn t ha mu (hnh 8.7). Tip l tc dn mu
vo bung siu nm cng cn c chn cho ph hp.
nht ca dung dch mu: Tip theo cc yu t trn l nht ca dung dch mu. Yu
t ny nh hng rt nhiu n hiu sut nguyn t ha thng qua qu trnh aerosol ha mu
theo k thut pneumatic (hnh 8.5) v (bng 8.2). Do mu phn tch
164
v cc mu chun dng ng chun cn phi c chun b trong cng mt iu kin, phi c cng
thnh phn ha hc, vt l, c bit l thnh phn ca cht nn ca mu, axit, loi axit dng lm mi
trng chng c cng nht.
Trn y l cc yu t c nh hng n qu trnh nguyn t ha mu, ngha l nh hng n
kt qu ca php o F-AAS. Tt nhin mi yu t c nh hng trong mc khc nhau, c trng
hp xut hin, song cng c trng hp khng xut hin r rt. Trong yu t u tin, nhit ngn
la l quan trng nht, n quyt nh hiu sut ca qu trnh nguyn t ha mu. Cc yu t khc cn
li nh hng n yu t th nht v qua m gy nh hng n kt qu ca php o.
Do , vic nghin cu pht hin v chn cc thng s cho ph hp nht i vi mc ch
phn tch nh lng mt nguyn t vi lng trong mi i tng mu l mt cng vic ht sc cn
thit v quan trng cho k thut phn tch F-AAS, chn v xy dng mt quy trnh chun.
Mt khc, nu chn c cc iu kin nguyn t ha mu ph hp, th trong nhiu trng hp
li loi tr c mt s yu t nh hng nht nh, nh nh hng ca ph nn, s Ion ha, s pht
x hay cc qu trnh th cp trong ngn la khng c li cho php o. Thc hin cc cng vic trn
chnh l tiu chun ha xy dng mt quy trnh phn tch mt nguyn t bng php o ph hp th
nguyn t ca n.
K thut nguyn t ha khng ngn la
c im v nguyn tc
K thut nguyn t ha khng ngn la ra i sau k thut nguyn t ha trong ngn la. Nhng
k thut ny c pht trin rt nhanh v hin nay ang c ng dng rt ph bin, v k thut ny
cung cp cho php o AAS c nhy rt cao (mc nanogam ppb); c khi gp hng trm n hng
nghn ln php o trong ngn la (bng
. y l u im chnh ca k thut nguyn t ha khng ngn la. Do , khi phn tch lng vt cc
kim loi trong nhiu trng hp khng cn thit phi lm giu s b cc nguyn t cn xc nh. c
bit l khi xc nh cc nguyn t vi lng trong cc loi mu ca y hc, sinh hc, dc phm, thc
phm, nc gii kht, mu, srum.
Tuy c
nhycao
nhng trong
mt s trng hp, n
nh
ca php o
khng ngn la thng km php o trong ngn la, nh hng ca ph nn thng rt ln. l c
im v cng l nhc im ca php o ny. Song vi s pht trin ca vt l v ca k thut o hin
i, ngy nay ngi ta c th khc phc c nhc im ny khng kh khn lm. V th cc h
thng my o ph hp th theo k thut khng ngn la ca nhng nm 1980 lun lun c km theo h
thng b chnh nn v n nh ca n cng khng km cc h thng ca php o trong ngn la v
m bo nhy cao c ppb i vi nhiu nguyn t.
c im na ca php o khng ngn la l i hi mt lng mu tng i
165
nh. Thng thng mi ln o ch cn lng mu t 20 n 50 p,L. Do khng cn nhiu lng mu

phn tch, vic chun b mu cng d dng v khng tn nhiu ha cht cng nh cc dung mi tinh
khit cao t tin.
V nguyn tc, k thut nguyn t ha khng ngn la l qu trnh nguyn t ha tc khc trong
thi gian rt ngn nh nng lng ca dng in cng sut ln v trong mi trng kh tr. Qu trnh
nguyn t ha xy ra theo ba giai on k tip nhau: sy kh, tro ha luyn mu, nguyn t ha o
ph hp th v cui cng l lm sch cuvet. Trong hai giai on u l chun b cho giai on
nguyn t ha t kt qu tt. Nhit trong cuvet graphit l yu t chnh quyt nh mi s din
bin ca qu trnh nguyn t ha mu.
Cc yu cu h thng nguyn t ha mu
H thng nguyn t ha phi ha hi v nguyn t ha mu phn tch vi hiu sut cao v n
nh, m bo cho php o c nhy cao v lp li tt.
Phi cung cp c nng lng (nhit cao) ln, c th nguyn t ha c nhiu loi
mu v phn tch c nhiu nguyn t.
Cuvet cha mu nguyn t ha phi c tinh khit cao. Khng lm nhim bn mu, khng
c ph ph gy kh khn cho php o nguyn t cn phn tch.
Hn ch, c t hay khng c cc qu trnh ph trong qu trnh nguyn t ha mu thc hin php
o.
Tiu tn t mu.
l nhng yu cu ti thiu cn thit i vi mt h thng trang b nguyn t ha mu trong
php o khng ngn la. Trn c s cc yu cu ny, mi hng ch to my ph hp th nguyn t u
c nhng h trang b ring cho cc my ca h. Song v nguyn tc v cc bc ca qu trnh nguyn
t ha th u nh nhau.
Nguyn tc v cc giai on ca qu trnh nguyn t ha mu
Nguyn tc v cch thc hin ca k thut nguyn t ha khng ngn la l hon ton khc vi
k thut nguyn t ha trong ngn la. y ngi ta thng dng nng lng nhit ca mt ngun
nng lng ph hp nung nng, ha hi v nguyn t ha mu phn tch trong ng cuvet graphit hay
trong thuyn tng tan (Ta) nh. Ngun nng lng thng c dng hin nay l dng in c cng
dng rt cao (t 50 - 600 A) v th thp (di 12 V) hay l nng lng ca dng in cao tn cm
ng.
Di tc dng ca cc ngun nng lng ny, cuvet cha mu phn tch s c nung nng
tc khc v mu s c ha hi v nguyn t ha to ra cc nguyn t t do trng thi hi c kh
nng hp th bc x n sc, to ra ph
hp
th
nguyn t ca n. Dng c nguyn t ha mu theo k thut ny hin
nay c rt
nhiu loi khc nhau c ch to ty thuc theo tng hng v tng phng th nghim. Nhng c th
khi qut theo cc nhm chnh di y:
166
+ Cc loi cuvet graphit;

+ Cc loi cc graphit;
+ Cc loi thuyn kim loi chu nhit, nh Ta.
Trong cc loi trn, c dng ph bin nht l cc cuvet graphit, v n tho mn c
nhng yu cu chnh ca php do khng ngn la. v cuvet graphit, mi hng ch to my
quang ph hp th nguyn t u c cuvet graphit ring cho cc my ca h v h thng
nguyn t ha khng ngn la tng ng.
H thng nguyn t ha mu theo k thut khng ngn la gm c:
+ Bung nguyn t ha v cuvet graphit cha mu phn tch thc hin qu trnh
nguyn t ha;
+ Ngun nng lng nung nng l graphit n nhit nguyn t ha mu v b
iu khin hay b chng trnh (programer) t chng trnh v ch huy qu trnh nguyn
t ha mu theo cc giai on nht nh. V d: Hng Perkin Elmer c h thng khng ngn
la HGA-70, HGA-400, HGA-5001 Hng Philips'pye Unicam c SP9- 041.
Tuy mi hng c nhng dng c khc nhau, nhng qu trnh nguyn t ha trong cc
dng c u xy ra theo 4 giai on k tip nhau trong thi gian tng cng t 80 - 60 giy.
Cc giai on l:
Sy kh mu
y l giai on u tin ca qu trnh nguyn t ha mu. N l rt cn thit m
bo cho dung mi ho tan mu bay hi nh nhng v hon ton, nhng khng lm bn mu,
mt mu. V nu khng thc hin sy tt, mu s b bn lm sai lch kt qu phn tch.
thc hin qu trnh sy tt, i vi mi mt loi mu cn phi tin hnh nghin cu, pht hin
v chn nhit v thi gian sy cho ph hp. Nhit v thi gian sy kh ca mi loi
mu ph thuc vo bn cht ca cc cht trong mu v dung mi ho tan n. Thc nghim
cho thy rng, khng nn sy mu nhit cao v sy kh nhanh. Ni chung nhit sy
kh ph hp i vi ba s cc mu v c trong dung mi nc nm trong khong t 100 150oC trong thi gian t 25-40 giy vi lng mu c bm vo cuvet nh hn 100 pl Tt
nhin qu trnh sy kh chm nhit thp bao gi cng cho kt qu n nh. Vic tng
nhit khi sy, t nhit phng n nhit sy mong mun cng cn c thc hin t
t, vi tc tng nhit t 8 n 5 0C trong mt giy l ph hp.
i vi cc
mu c cha
cc cht hu c hay ho tan trong dung mi
hu c,
thng phi sy nhit thp hn v tc tng nhit phi chm hn dung mi nc.
Vi loi mu ny, nhit sy thng l di 100 0C. Hnh 8.13 l mt v d v qu trnh sy
kh mu. Trong T 8 l nhit sy ti a (ti hn) v trong 6 tc tng mhit sy, th
ch c qu trnh theo ng s 5 v 6 l cho kt qu tt. ng
167
thi trong quan h t l gia thi gian Ramp (thi gian tng nhit ) v thi gian sy
thng nm trong t l t 3/4 - 2/4 l
phhpcho nhiu nguyn t.
nguyn t cng c mt nhit sy ti a cho
(bng 8.6),
Mt khc, mi
ngha l nu sy mu
nhit cao hn nhit th kt qu phn tch km n nh v s mc sai s rt ln.
Tro ho luyn mu
y l giai on th hai ca qu
trnh nguyn t ha mu. Mc ch
l tro ha (t chy) cc hp cht
hu c v mn c trong mu sau
khi
sy
kh,
ng
thi
nung
luyn mt nhit thun li cho

giai on nguyn t ha tip theo
t hiu sut cao v n nh. Giai
on ny c nh hng rt nhiu
n
kt
qu
phn
tch,
nu
chn
nhit tro ha khng u ho th

mt s hp cht c th b phn hu mt trong giai on ny, nu nhit tro ha l
qu cao. L thuyt v cc kt qu thc nghim xc nhn rng, tro ha mu t t v
nhit thp hn nhit gii hn th php o lun lun cho
kt qun nh, v
nguyn t u c mt nhit tro ha luyn mu gii hn (T r.) trong
mi
php oETA-
AAS.
Nhit tro ha gii hn l nhit m s tro ha mu nhit v nh
hn n, th cng vch ph hp th l khng i (hnh 8.14). Cn nu tro ha mu
nhit ln hn nhit th cng vch ph b gim v khng n nh. Nhit
tro ha gii hn ca mi nguyn t
rt khc nhau,n ph thuc vo bn
mi nguyn t v ph thuc vo dng
hp cht mnguyn t
matrix (cht nn) ca mu (hnh 8.14).

Ni
chung,
mt
ha
hc, cc nguyn t bn nhit v

tn ti trong cc dng hp cht
bn
nhit
thng
phi
tro
ha
luyn mu nhit tng i

cao. Nh v d trong hnh 8.14,
Si c nhit tro ha gii hn
l 1100oC, Ni l 1000oC, cn Pb
l
600oC.
Ngay
vi
mt
nguyn t nhit tro ha gii

hn Tr cng c th khc nhau,
khi chng tn ti trong cc cht
168
tn
cht ca
ti,cng
nh
khc nhau
Khi Nn
nghin
cuca mu
k (matrix
qu effect), nht l cc cht nn bn nhit. Hnh 8.18 l mt v d
v vn
khi o
ph hp
th nguyn
trnh
tronyha
luyn
mu
ca t ca Mg trong cc nn khc nhau.
nhiu Ngha
nguynl Mg
t, trong
ngi
cc ta
chtthy
nn khc nhau c nhit tro ha gii hn l T 1, T2, T3 v T4 (tc
rng,
mi v
quan
h). gia
l 600, 1000
1100 oC
nhit
tro ng
ha thi
luyn
v ta
cng
qua mu
chng
thy ngha ca cht ph gia c thm vo mu phn tch.
ca vch ph hp th
nguyn t ca cc nguyn t
Bng 8.6
thng tun theo mt trong ba
Mt s v d v nhit sy, tro ha luyn mu, nguyn t ha mu gii hn ca mt s nguyn t
loi nh trong hnh 8.14. Loi
(theo W. Fuller)
l tiu biu cho cc nguyn
t Pb, Zn, Co, Mg. Loi (2) l
Ni, Cu. Loi (3) l Si, Ca, Al.
Mt
khc Nguyn
cc t kt
thc nghim cng ch ra rng,
qu
Nhit ti hn ca qu trnh ( oC)
khng nn tro ha luyn mu Sy

nhitmu
qu gii hn,
v nh th vic
luyn
mu chun
Tro ha
Nguyn
t ha
b cho giai on nguyn t ha s khng tt.
Al
130
1100
2850
Ch nn tro ha nhit cao nht l bng hay thp hn nhit tro ha gii hn mt t
(khong 30 - 50oC).Ba
150
1100
2900
Ngoi yu t nhit th tc tng nhit trong qu trnh tro ha cng c nh hng n

Be
130
1100
2750
n nh ca cng vch ph. Ni chung, tc tng nhit qu ln thng lm bn mu. Vic
1100
2800trong mt thi
tng chm bao giCa
cng cho kt qu tt 130
hn, ngha l phi thc
hin tro ha luyn mu
gian khng qu ngn. Thng thng l t 30 - 60 giy, vi lng mu a vo cuvet nh hn 100 ^L.
Cu
120
0650
2650
Trong tng thi gian tro ha, thng dnh 1/3 cho vic tng nhit t nhit sy n nhit tro
ha, ngha l tc
trong 1 giy l thch2700
hp. Sau thi
Fetng nhit nm trong
120 vng t 60-100
1000
gian cn li 2/3 l gi nhit khng i chn luyn mu.
Pb
100
0600
170
2500
Mg
150
1100
2850
Mn
130
1000
2700
Si
150
1200
2850
Na
139
0800
2200
Sr
130
1100
2800
Zn
110
0600
2500
Co
110
1100
2750
Cr
110
1100
2750
169
i vi cc mu c cht hu c hay trong dung mi hu c th giai on ny cng phi cn thn

v nhit chn tro ha phi thp hn dung mi l nc, trnh s bay hi trc ca nguyn t
phn tch dng hp cht c kim. Do , vi mi loi mu, trong mi loi dung mi, chng ta cn
kho st pht hin c nhit tro ha ph hp cho n.
Nguyn t ho
y l giai on cui cng ca qu trnh nguyn t ha mu, nhng li l giai on quyt nh
cng ca vch ph. Song n li b nh hng bi hai giai on trn. Giai on ny c thc hin
trong thi gian rt ngn, thng thng t 3 n 6 giy, rt t khi n 8-10 giy.
Nhng tc
tng nhit li l rt ln
t ngay
tc khc
n nhit
nguyn t ha v thc hin php o cng vch ph. Tc tng nhit thng l t 1800 2500oC/giy, thng thng ngi ta s dng tc ti a. nguyn t ha ca mt nguyn t rt khc
nhau (hnh 8.17).
ng thi mi nguyn t cng c mt nhit nguyn t ha gii hn Ta ca n. Nhit Ta
ny ph thuc vo bn cht ca mi nguyn t v cng ph thuc trong mc nht nh vo trng
thi v thnh phn ca mu m n tn ti, nht l cht nn ca mu (hnh 8.18).
2600 2800
Hnh 8.17
Quan h gia nhit nguyn t ha v cng vch ph ca cc nguyn t
171
2000
2400
2800
Hnh 8.18
nh hng thnh phn nn ca mu n nhit nguyn t ha mt nguyn t
Khi nghin cu qu trnh nguyn t ha ca nhiu nguyn t trong cc iu kin khc nhau,
ngi ta thy s din bin ca nhit nguyn t ha ca mt nguyn t v cng vch ph ca n
thng theo hai loi nh trong hnh 8.19. Cc nguyn t theo loi (1) c nhit nguyn t ha gii
hn l Ta1, ngc li, cc nguyn t theo loi (2) c nhit nguyn t ha gii hn l Ta2.
Tiu biu cho loi (1) l cc nguyn t Zn, Fe, Pb, Cu v Mo, tiu biu cho loi
l cc nguyn t, Si. Sn, Mg, Ca (hnh 8.17). Cc gi tr nhit Ta1 v Ta2 l nhit nguyn t ha
gii hn ca mi loi. Khi nguyn t ha mu o cng vch ph ca mt nguyn t nhit
cao hn nhit gii hn ny thng khng c li thm v cng , m kt qu thc nghim cho
thy cc kt qu o thng khng n nh v thng lm hng nhanh cuvet graphit.
172
8.3.4
Cc yu t nhchn
hng
Ngoi vic
nhit , vtrong
giai
Cng
i
cc
on
iny
u
chn
cn
ki
n cn
sy, phi
tro
thi v
gian nguyn
nguyn tt
ha
ha
cho ph
ha
mu hpnhlm
sao
m
bo cc
cngqu
vch
trnh
by lc
trn,
ph thu
c tphi
trnh
nguyn
hagn v
v
mch
u c
theomt knh.
thuNh
t
d trong
khng
ngnhnhla8.20
cnch c
btrng
nhhp h(a)
l
ngtt. bi
mt s yu t khc
na. Cc yu t ny
nh
hng
nhau
khc
vi
m i
"t----- - ! _ ... 1
H-------------4
. -!
i......i... :
h
41
i
i
J-----------
1------
T.
c khi li khng gy
-------------u
- - ----f-l|
4
:!
---------------!_
-
>
----------r -T .
4
nh hng.
4
----1
~T R
=t
i
1
-----------------T
~L-
=4
----1
1
t nguyn t ha.
Trc ht ltmi ----------------trng
kh ......7
tr thc hin qu
trnh
....
-4
1
-i_r
1 --------H
i-t '
1
-trri
Kh tr thng
qu trnh nguyn t ha l argon
c' dng lm mi tr ng hchot- ---t
----------(Ar), nit (N2) v hai (He), ngh a l ------qur- =fl
trnh nguyn
t ha 3__
thc!.... hin trong mi
N
- -- - -1- trng khng c oxy. 1Do I khng xut hin hp1chTt Tbn nhit lo^--------i MeO
hay----------j------MeOX.
-1
- r-""
------5
__u
-4.
>
,4-1
-
---....u
___L
-i__
nguyn
........- .............................
'
cng
/ ir
-
kiH
Nhng bn ch
;rit, thnh phn v tc dn kh tr vo trong cuvet graphit
=4=
nh hng ....
n cang ca vchb ph v nhit trongccuvet graphit (hnh
8.22).
d
Trong
ba Quan
loi hkh
tr dng
ni lc vch ph v thi gian nguyn t ha
Hnh 8.20
gia hnh
trn, th Ar l kh t t nht, sau
n N2. ng thi khi

a: 3vo
giy,cuvet
b: 4 giy, c: 6 giy v d: 8 giy
tng tcCa-422,7nm.
dn kh
chng
graphit n
th y
cng
tavc
chth
phkhi
qut ton b qu trnh nguyn t ha mu theo k thut khng
ngn la
lun
lunnhgitrong
m hnh
v 8.21.
mc Trong
: (1) l giai on sy mu; (2) l giai on tro ha luyn mu;
nguyn
ha
gi(3)
ml cgiai
ngon
khc
nhaut
i o
vicng vch ph v (4) l giai on lm sch cuvet graphit. on
thi gian
nhit
ca hai giai on u (thi gian Ramp).
mRilnguyn
ttng
(hnh
8.22a).
Do trong phn tch, khi o

cng vch ph bt buc
phi
gi
cho
tc
khng i, hoc c th tt kh
d n
Q | ---------------------1 -------------------1 -------------------1 -------------------1 -------------------1 -------------------1 ----------------------
100
200
400
(ml/ph)
Hlnh 8.22a
nh hng ca tc kh tr n cng vch ph
mi trng trong giai on nguyn t ha o cng vch ph.
174
173
Yu
th
hai
l cng sut t nng

cuvet. Nhn chung, khi
tng
cng
sut
nng cuvet th cng

vch ph tng theo
(hnh 8.23). Nhng s
ph
thuc
ny
cng
ch trong mt gii hn
nht
nh,
sut
khi
cng
nng
cuvet
nh hn 6 KW.
Cn khi t nng cuvet cng sut ln hn 7 KW th hu nh cng vch ph
khng tng na (hnh 8.23).
Yu t th ba l tc t nng cuvet. Tc t nng cuvet v thi gian nguyn t ha
t l nghch vi nhau. Nu o din tch ca lc th yu t ny hu nh khng nh hng,
nhng nu o chiu cao ca lc th li rt khc nhau (hnh 8.24). Ni chung chiu cao ca lc
t l vi tc t nng cuvet.
175
Hnh 8.24 l
cc
l c
vch ph
ca qu trnh nguyn t ha 10 ppb

Pb vi cc tc t nng cuvet: 1)
2300; 2) 1600; 3) 1000 v 4)
800oC/giy. y chng ta thy vi
tc t nng 1, vch ph c
chiu cao ln nht, sau n tc
2 v cui cng l tc 4.
Nhng vn chnh l ch, khi
Hnh 8.24
nguyn t ha vi tc t nng
nh hng ca tc t nng cuvet n cng vch Pb
cuvet thp, ta thng phi nguyn

t ha thi gian di, do trng
hp dn n lc ca vch ph khng nhng c chiu cao thp, m cn c nhi u nh
v dng phc tp gy kh khn cho vic nh gi nh lng.
Yu t th t l loi cuvet graphit dng nguyn t ha mu, ngha l cc loi nguyn
liu graphit khc nhau c ng nh hng n cng vch ph v thi gian nguyn t ha mu
(hnh 8.25).
Ni chung, cc
loi graphit hot ha ton phn thng
cho kt qu tt nht,
nhy cao, n nh.

Hnh 8.25 l mt v d v vn
ny. l vic nguyn t ha
Cr v Al vi ba
loi cuvet khc nhau. Pic 1 l v i cuvetgraphit c hot ha nhit ton phn; tc 2 l
cuvet graphit
chc hot
hot
ha.
176
ha b mt v tc
3 l cuvet graphit th ng khng
Cc qu trnh trong cuvet graphit

Cc qu trnh xy ra trong cuvet graphit v c ch ca qu trnh nguyn t ha mu l
nhng vn ht sc phc tp, nhng li quyt nh cng ca vch ph. Mun hiu bit
c ch ca vn ny, chng ta phi xem xt tt c cc yu t ng hc, nhit ng hc v
cc phn ng ha hc c th xy ra trong cuvet, v cc qu trnh l xy ra ng thi v c
tc ng qua li ln nhau. Nhng khi nghin cu mt yu t ny, thng thng ngi ta phi
c lp hay gi cho cc yu t khc khng i. Song thc cht khng phi nh th, cc qu
trnh xy ra trong cuvet graphit khng c lp v tch bit ln nhau, m chng gn cht vi
nhau v c tc ng qua li nh hng ln nhau nhng mc nht nh di tc dng
quyt nh ca nhit trong cuvet graphit. V th vic xem xt mt yu t trong khi cc yu
t khc c gi khng i ch l tng i trong mt iu kin nht nh dt ra, theo
di s thay i ca mt yu t.
Nhiu tc gi nghin cu cc qu trnh xy ra trong cuvet graphit, song cho n nay cng
ch c nhng kt qu bc u trong mt vi trng hp c th. Chnh v th cha th nu
mt c ch chung ca qu trnh nguyn t ha mu trong cuvet graphit, do chng ti ch
mun cp n mt vi vn chnh c th chp nhn
177
c theo quan im ng hc v nhit ng hc ha hc nhit cao, theo trt t ca qu

trnh nguyn t ha mu.
Qu trnh nguyn t ha mu xy ra theo ba giai on k tip nhau, nh hng ln nhau.
Trong hai giai on u l chun b cho giai on th ba nguyn t ha mu o cng
vch ph. l mt tng th lin tip din bin ca nhiu qu trnh. Nhng d hiu chng
ta c th tch ring v khi qut theo nhng vn sau y:
S bay hi ca dung mi. y l qu trnh vt l n gin, n xy ra trong giai on u
(sy mu) ca qu trnh nguyn t ha mu v nhit l yu t quyt nh s din bin ca
qu trnh ny. Nhng thnh phn ca mu, cc cht hu c c mt trong mu cng nh hng
n qu trnh ny. Sau khi dung mi bay hi s li cc ht mu l bt mn ca cc mui
kh trong cuvet.
S tro ha (t chy) cc cht hu c v mn. Qu trnh ny xy ra trong giai on th
hai ca qu trnh nguyn t ha. Khi cc cht hu c b tro ha, s to ra cc cht kh (CO,
CO2, H2O) bay i v li phn b v c ca mu. l cc mui hay cc oxit ca cc cht
mu. Tip b ny c nung nng, nng chy hay b phn hy ty theo nhit tro ha
chn v ty thuc vo bn cht ca hp cht mu tn ti trong cuvet sau khi sy kh. Lc ny
mu c luyn thnh th nng chy ng nht. ng thi y cng c s phn hu ca
mt s mui khng bn thnh oxit hay mui hay oxit n gin. V d, nu trong mu c
CaCO3 th c th c phn ng phn hy nh sau:
CaCO3 (r) ^ Cao(r) + Co2(k)
S ha hi ca cc hp phn mu dng phn t. Nu nhit ha hi (nng
lng ha hi) ca cc hp phn mu nh hn nhit phn li ca chng th cc hp phn mu
ny s ha hi dng phn t, sau chng b phn li thnh cc nguyn t t do. l c
ch ha hi ca cc phn t c p sut ha hi cao v nhit ha hi thp hn nhit phn li (Eh
< Ea). Tiu biu cho cc hp cht thuc loi ny l cc oxit Sb 2O3, Ga2O3,
halogen ca cc kim
loi nh SbCl5, SnCl4,
cc
mui
SnBr4, AlCl3,
TiCl4, GaCl3, cc mui axetat, Clorat ca kim loi, v.v... C ch din bin ca cc hp cht
loi ny c th minh ho theo hai kiu s sau y
C ch chnh 1:
MxXy(r,l) > MxXy(k) > xM(k) + X
MxOy (r,l) > MxOy(k) > xM(k) + O 2
M(k) + n(hv) ^ ph AAS
Qu trnh (a) xy ra i vi cc mui halogen kim loi v qu trnh (b) l i vi cc
oxit kim loi d ha hi. Nh cc hp cht ZnCl 2, CuCl2, FeCl3, CdCl2,...Cn qu trnh (c) l
s hp th bc x ca nguyn t, to ra ph.
178
Sau y l vi v d v c ch ny:
CdCl2(r,l) ^ CdCl2(k) ^ Cd(k)
CuCh(r,l) ^ CuCl2(k) ^ Cu(k)
SbCl5(r,l) ^ SbCl 5(k) ^ Sb(k)
Nhng ring mui AlCl 3 ngoi qu trnh chnh theo c ch (a) th cn qu trnh ph
sinh ra hp cht monooxit bn nhit dng AlO nh sau:
AlCl3 (r,l) ^ Al3(k) + Cl2
Alo(k) ^ A(k) + O2
Qu trnh ph ny ph thuc vo s c mt ca oxy v nhit ca cuvet. nhit
nh hn 2500oC th qu trnh (e) hu nh khng xy ra c. V th n lm mt nguyn t t
do Al, qua lm gim cng vch ph. Do phi tm cch ngn cn khng cho hnh
thnh AlO, tc l phi hn ch qu trnh (d) xy ra khi nguyn t ha mu. kh b qu
trnh (d), ngi ta phi nguyn t ha mu trong mi trng kh tr hay thm vo mu nhng
cht ph gia thch hp.
S phn li ca cc phn t cht mu trc khi ha hi. Khuynh hng ny thng xy ra
i vi cc phn t c p sut ha hi thp v nhit phn li nh hn nhit ha hi phn t ca
chnh n Eh > Ed. Cc phn t thuc loi ny, di tc dng ca nhit trong cuvet graphit,
trc ht chng b phn li thnh cc monooxit hoc thnh cc nguyn t t do trng thi rn,
hay lng, ri sau mi c chuyn thnh th hi theo cc tnh cht ring ca sn phm va
c hnh thnh. Din bin ca qu trnh thuc loi ny c th minh ho theo cc s di
y:
C ch chnh 2:
MxXy (r,l) ^ Mx(r,l) + yX(k)
_______________^ xM(k)
MxXy (r,l) ^ xMO(r,l) + yX(k)
_______________xM(k)
MxOy(r,l) ^ mX(r,l) ^ xM(K)
MxOy(r,l) ^ xMO(r,l) ^xM(r,l) ^ xM(k)
Sau l qu trnh hp th bc x ca cc nguyn t M(k).
M(k) + n(vh) ^ Ph AAS
Cc qu trnh (f) v (g) ny l i vi cc mui ca kim loi vi nitrat, cacbonat, sun
pht, phtpht, ngha l cc mui c oxy. Cc qu trnh (h) v (i) l i vi cc hp cht oxit.
Cc qu trnh theo cc c ch ny thng km n nh v cho kt qu nhy thp hn cc
qu trnh ca cc mui halogen trn. Tiu biu cho s din bin
179
theo kiu ny l cc hp cht, cc mui cacbonat, sunphat v photphat ca kim th Ca, Ba,
Si. V d:
FeCl3(r,l) ^ Fe(r,l) ^ Fe(k)
Mn(NO3)2(r) ^ Mno(r,l) ^ Mn(k)
CaO(r) ^ Ca(r) ^ Ca(k)
V2O5(r) ^VO(r) ^ V(k)
Nh vy, cc qu trnh ny xy ra trong cuvet nh th no ty thuc vo:
+ iu kin nguyn t ha mu (ch yu l nhit ).
+ Tnh cht nhit ha ca cc hp cht mu ,
+ nh hng thnh phn nn ca mu, v
+ Mi trng tin hnh nguyn t ha mu.
+ Cht nn ca mu, cht ph gia thm vo.
S to thnh hp cht cacbua kim loi.
Trong cuvet graphit s xut hin hp ht cacbua kim loi l iu tt nhin, nhng mc
rt khc nhau i vi mi kim loi. Ch yu l cc kim loi bn nhit nh kim th, t
him. Phn ng ny thng may xy ra gia cc monooxit kim loi vi cacbon ca cuvet
graphit hay ca kim loi th lng v rn vi cacbon:
(k) M + xC ^ MCx
(l) MO + xC ^ MCx + O2
trong x c th l 1,2,3,4.
Sau cc hp cht cacbua va hnh thnh s ha hi v b nguyn t ha theo tnh
cht, c trng nhit ha ca n. Tt nhin qu trnh ha hi v nguyn t ha ca cc hp
cht loi ny tng i kh khn v phi nhit kh cao, v n l cc hp cht bn nhit.
V th phi ngn nga khng cho cc qu trnh (k) v (l) xy ra. Mc hnh thnh cc hp
cht loi ny rt khc nhau i vi tng kim loi v ph thuc vo nhiu yu t nh:
+ Tnh cht ca mi kim loi;
+ iu kin nguyn t ha mu, nhit nguyn t ha;
+ Thnh phn ha hc ca mu;
+ Loi cuvet graphit nguyn t ha mu.
Ni chung, cc cuvet graphit hot ha nhit ton phn (pyrolitic coated graphit)
thng hn ch xu hng to thnh hp cht cacbua kim loi. Ngc li, cc loi cuvet
graphit thng (standard graphit cuvet) kh nng hnh thnh cc hp cht
180
cacbua kim loi l rt ln. Hin tng ny th hin rt r rng khi phn tch cc kim loi kim
th, nhm v cc t him. c bit khi cc nguyn t ny l nn ca mu, th s xut hin
cc hp cht cacbua kim loi c th lm gim nhy ca phng php phn tch hng trm
ln, thm ch c khi n ngn ln.
V th trong nhiu trng hp ngi ta phi chn nhng iu kin nguyn t ha mu
ph hp loi tr s xut hin cc hp cht cacbua, hoc thm vo mu cc cht chy nh
NH4NO3, LiBO2 Vi nng thch hp hn ch vic tip xc ca cht mu vi cacbon,
hoc tin hnh cacbua ha b mt cuvet graphit trc bng mt hp cht cacbua bn, sau
mi a mu vo nguyn t ha hoc t mu trong thuyn Ta trong cuvet.
S kh xit kim loi bi cacbon. Trong cuvet graphit, di tc dng ca nhit, mt s hp
cht mu cng c th b kh bi cacbon ca cuvet. Phn ng ny rt phc tp v n cng ph
thuc vo cc yu t nh trong qu trnh hnh thnh cc hp cht cacbua kim loi. ng
tc ca
phn ng
kh ny cnph thucvo p
ring phn ca nguyn t cacbon trong cuvet v kh tr
thi
sut
lmmi trng nguyn t
ha
mu. Phn ng ny thng din bin theo hai loi:

(m) MxOy(r,l) + C(r) ^ Mx(r,l) + CO
(n) MxOy(k) + C(k) ^ xM(k) + CO
Trong hai loi phn ng ny, loi qu trnh (m) thng
d xy ra v chim u th
hn v trong nhng trng hp ca cc oxit bn nhit, th qu trnh ny li lm cho vic

nguyn t ha mu c th tt hn. Sau y l mt vi v d v cc phn ng kh cc oxit:
NiO(4) + C ^ Ni(r,l)
--------------------- Ni(k)
PbO(r) + C Pb(r,l) +OC
--------------------->Pb(k)
Cc hp cht oxit CaO, Cr 2O3, MoO3, ZnO, CdO, CuO,.. thng xy ra theo kiu c ch
ny.
Trn y l minh ho cc qu trnh c th xy ra trong cuvet graphit. Tt nhin l c tnh
cht khi qut, nn khng phi lc no, trong mi loi mu u c cc qu trnh , m
trong thc t din ra cuvet graphit c s chn lc, c s tng tc ln nhau v ng thi
cng c s loi tr nhau. Trong , qu trnh chim u th hn l ph thuc vo nhiu yu t,
nh:
+ Nhit t nng cuvet (y l yu t quyt nh);
+ Bn cht ca nguyn t v hp cht m n tn ti trong cuvetl
181
+ Thnh phn ca mu phn tch, c bit l nguyn t c s (nn);

+ Trng thi b mt v loi cuvet graphit;
+ Mi trng kh tr tin hnh nguyn t ha mu;
+ Cui cng l cht ph gia c thm vo mu.
Chnh do c nhng quan h ph thuc ny, m chng ta c th iu chnh v
khng ch cho mt qu trnh no u vit s xy ra, cn qu trnh no khng c li
s c hn ch hay loi tr.
H thng trang b nguyn t ha mu theo k thut khng ngn la bao gm
hai phn chnh:
B
phn
ng
mu
nguyn t ha. chnh l

cc loi cuvet graphit, cc
graphit,
hay
thuyn
tantan,
hay l cc loi filamen cha

mu.
Trong
cc
loi
ny,
cuvet graphit c dng ph

bin nht v tt nht l cuvet
graphit
hot
ha
nhit luyn ton phn. V loi

ny th mi hng ch to my
o ph hp th nguyn t
cng c nhng loi c hnh
dng v kch thc ring cho
my ca h (hnh 8.26).
Phn th hai l ngun nng lng nung nng cuvet v gi cuvet.
Phn ny bao gm b chng trnh iu khin theo bn giai on (bn phase) sy, tro
ha, nguyn t ha v lm sch cuvet theo nguyn l ca php o v ngun nng lng c
cng sut cc i l c 3,5 - 7,5 KVA cung cp nng lng cho qu trnh nguyn t ha
mu.
N thng l ngun
nng lng in c dng rt cao (thay
600 A), nhng th rt thp (di 12 V).
182
i c t 50 n
Hnh 8.26b
H thng nguyn t ha mu trong ngn la (Philips Pye Unicam)
8.3.7 Ti u ha cc diu kin cho php o khng ngn la mu.

N c nghin cu k trn. Do y ch nu li mt s iu cn ch . C th
vi php o ETA-AAS bao gm nhng iu kin:
Cc iu kin nguyn t ha mu:
+ Thi gian, nhit nung nng cuvet ca cc giai on sy mu, tro ha luyn mu v
nguyn t ha o cng vch ph,
183
+ Kh mi trng cho qu trnh nguyn t ha mu (tc , loi khi)

+ Cng sut, tc t nng cuvet graphit nguyn t ha mu;
+ iu kin lm sch cuvet graphit;
+ Lng mu v cch a vo cuvet nguyn t ha cho php o.
Cht nn ca mu phn tch v cc mu chun cn phi c pha ch v chun cho ng
nht.
Mi trng axit v loi axit pha ch mu v lm mi trng cho dung dch mu chun
v mu phn tch.
Cc yu t nh hng sau y cng cn c xem xt.
+ Cc nh hng v ph;
+ Cc nh hng v vt l;
+ Cc nh hng ha hc ca cc Cation v Anion c trong mu;
+ V nh hng ca thnh phn nn ca mu.
184
Chng 9
TRANG B CA PHP O ASS
Ngun pht bc x n sc
Mun thc hin c php o ph hp th nguyn t ngi ta cn phi c mt ngun
pht tia bc x n sc (tia pht x cng hng) ca nguyn t cn phn tch chiu qua mi
trng hp th. Ngun pht tia bc x n sc trong php o ph hp th nguyn t thng l
cc n canh rng (HCL), cc n phng in khng in cc (EDL) v cc n ph lin tc
c bin iu ( c n sc ha). Nhng d l loi no, ngun pht tia bc x n sc trong
php o ph AAS cng phi tha mn c nhng yu cu ti thiu sau y mi c th chp
nhn c.
Ngun pht tia bc x n sc phi to ra c cc tia pht x nhy (cc vch pht x
nhy, c trng) ca nguyn t cn phn tch. Chm tia pht x phi c cng n nh,
phi lp li c trong nhiu ln o khc nhau trong cng iu kin, phi iu chnh c vi
cng mong mun cho mi php o.
Ngun pht tia bc x phi cung cp c mt chm tia pht x thun khit ch bao
gm mt s vch nhy c trng ca nguyn t phn tch. Ph nn ca n phi khng ng
k. C nh th mi hn ch c nhng nh hng v vt l v v ph cho php o AAS.
Chm tia pht x n sc do ngun cung cp phi c cng cao, nhng li phi
bn vng theo thi gian v phi khng b cc yu t vt l khc nhiu lon, t b nh hng bi
cc dao ng ca iu kin lm vic.
Ngun pht tia bc x n sc phi bn lu, khng qu t tin v khng qu phc tp
cho ngi s dng.
Tt nhin trong 4 yu cu trn th 3 yu cu u tin l quan trng nht v bt buc phi
tha mn, cho php o t kt qu chnh xc, n nh v tin tng. Ring yu cu th 4 th
c th chnm chc c trong nhng trng hp c th nht nh.
Xut pht t nhng nhim v v yu cu phi tha mn, hin nay trong php o ph hp
th nguyn t, ngi ta thng dng ch yu ba loi ngun pht tia bc x n sc. l:
+ n catot rng (HCL - Hollow Cathode Lamp),
185
+ n phng in khng in cc (EDL- Electrodeless Discharge Lamp),

+ n pht ph lin tc c bin iu (D 2-lamp, W-lamp).
+ Cc loi ngun n sc khc.
Trong ba loi , n HCL c dng ph bin nht. n pht ph lin tc mi c
pht trin v s dng trong vi nm nay, nhng li c nhiu u vit trong cc my nhiu knh
v qu trnh phn tch t ng lin tip nhiu nguyn t, tuy nhin gi thnh cn t v
nhy cn km nn cha c dng ph bin.
n catot rng (HCL)
n pht tia bc x n sc c dng sm nht v ph bin nht trong php o S l
n catot rng (HCL). n ny ch pht ra nhng tia pht x nhy ca nguyn t kim loi lm
catot rng. Cc vch pht x nhy ca mt nguyn t thng l cc vch cng hng. V th
n catot rng cng c gi l ngun pht tia bc x cng hng. N l ph pht x ca cc
nguyn t trong mi trng kh km.
V cu to, n catot rng gm c ba phn chnh:
Phn 1 l thn n v ca s,
Phn 2 l cc in cc catot v anot, v
Phn 3 l kh cha trong n. l kh tr He, Ar hay N 2.
Thn v v. Thn n gm c v n, ca s v b cc in cc anot v catot. B
bng nha PVC. Thn v v n bng thu tinh hay thch anh. V n c hai dng (hnh 9.1).
Ca s S ca n c th l thu tinh hay thch anh trong sut trong vng UY hay VIS l
ty thuc vo loi n ca tng nguyn t pht ra chm tia pht x nm trong vng ph no.
Ngha l vch pht x cng hng o ph hp th vng no th nguyn liu lm ca s S
phi trong sut vng .
in cc. in cc ca n l catot v anot. Anot c ch to bng kim loi tr v bn
nhit nh W hay Pt. Catot c ch to c dng hnh xylanh hay hnh ng rng c ng knh
t 3 - 5 mm, di 5 -6 mm v chnh bng kim loi cn phn tch vi tinh khit cao (t nht
99,9 %).
Dy dn ca catot cng l kim loi W hay Pt. C hai in cc c gn cht trn b
ca thn n v cc catot phi nm ng trc xuyn tnm ca n (hnh 9.1). Anot t bn
cnh catot hay l mt vng bao quanh catot. Hai u ca hai in cc c ni ra hai cc gn
cht trn n, cm vo ngun in nui cho n lm vic. Ngun nui l ngun 1 chiu c
th 220-240 V.
Kh trong n. Trong n phi ht ht khng kh v np thay vo l mt kh tr vi p
sut t 5 - 15 mHg. Kh tr l argon, heli hay nit nhng phi c sch
186
cao hn 99,99 %. Kh np vo n khng c pht ra ph lm nh hng n chm

tia pht x ca n v khi lm vic trong mt iu kin nht nh th t s gia cc
nguyn t b Ion ha v cc nguyn t trung ho phi l khng i. C nh th n
lm vic mi n nh.
Ngun nui n. n c t nng pht ra chm tia pht x cng hng
nh ngun in mt chiu n nh. Th lm vic ca n HCL thng l t 250 220V ty thuc vo tng loi n ca tng hng ch to v ty thuc vo tng nguyn
t kim loi lm catot rng.

Cng lm vic ca cc n catot rng thng l t 3- 50 ma v cng ty
thuc vo mi loi n HCL ca mi nguyn t do mi hng ch to ra n.
Th v cng dng in lm vic ca n HCL c lin quan cht ch vi cng
tch kim loi ra khi b mt catot rng to ra hi kim loi sinh ra chm tia pht
x ca n HCL.
Dng in qua n
HCL ca mi nguyn t
rt khc nhau. Mi n
HCL u c dng in
gii hn cc i m n
c th chu ng c v
gi
v
tr
n.
ny
Tt
nhin
c
khi
ghi
s
Cu
trn
to
ca
Hnh
n
catot
9.1
rng
dng khng bao gi c

php dng n dng in cc i , m thch hp nht l trong vng t 65 - 85 % gi tr cc
i, v iu kin dng cc i n lm vic khng n nh v rt chng hng, ng thi
php o li c nhy v lp li km.
Theo l thuyt v thc nghim ca thc t phn tch theo k thut o ph hp th nguyn
t, tt nht ch nn dng cng dng trong vng t 60 - 85 % dng gii hn cc i ghi
trn n HCL.
Mun c nhy cao, nn s dng cng dng gn gii hn di. Mun c n
nh cao, nn dng cng dng gn gii hn trn. Nhng nn nh rng cng dng
lm vic ca n HCL v cng ca vch ph hp th c quan h cht ch vi nhau.
Ni chung, nhiu trng hp cng ca vch ph hp th l t l nghch vi cng
dng in lm vic ca n HCL (hnh 9.2), tuy nhin cng c vi trng hp khng tun
theo quy lut .
187
Quan h gia cng vch ph v cng dng in lm vic ca n HCL

(A) l trng hp ph bin (Cd-228,8 nm), Cu, Ca, Fe; (B) l ca Pb 283,3 nm, c
bit;
(C) l ca Al 309,3 nm, c bit.
Khi n lm vic, catot c nung , gia catot v anot xy ra s phng in lin tc.
Do s phng in m mt s phn t kh b Ion ha. Cc Ion va c sinh ra s tn cng
vo catot lm b mt catot nng v mt s nguyn t kim loi trn b mt catot b ha hi
v n tr thnh nhng nguyn t kim loi t do. Khi di tc dng ca nhit trong n
HCL ang c t nng , cc nguyn t kim loi ny b kch thch v pht ra ph pht x
ca n. chnh l ph vch ca chnh kim loi lm catot rng. Nhng v trong iu kin c
bit ca mi trng kh tr c p sut rt thp, nn ph pht x ch bao gm cc vch nhy
ca kim loi m thi. chnh l s pht x ca kim loi trong mi trng kh km. Chm
tia pht x ny l ngun tia n sc chiu qua mi trng hp th thc hin php o AAS.
Cc n catot rng c cu to nh m t trn l nhng n HCL n nguyn t,
ngha l mi n HCL ch phc v cho phn tch mt nguyn t. Ngy nay ngoi cc n
HCL n, ngi ta cng ch to c mt s n kp i, kp ba hay kp su nguyn t.
V d cc n kp i l (Ca+Mg), (Cu+Mn), (Cu+Cr), (Co+Ni), (K+Na), (Cu+Pb); cc n
kp ba nh (Cu+Pb+Zn) v n kp su l (Cu+Mn+Cr+Fe+Co+Ni).
ch to cc n kp ny, catot ca n HCL phi l hp kim ca cc nguyn t .
Hp kim ny phi c thnh phn ph hp, sao cho cng pht x ca cc nguyn t l
gn tng ng nhau; ngha l s pht x ca kim loi ny phi khng c ln t s pht x
ca nguyn t kia. Do phi ch to trong iu kin dung ha cho tt c cc nguyn t. V
d: n HCL kp su ca Cu, Mn, Cr, Fe, Co, v Ni th hp kim lm catot rng phi cha
25% Cu, cc nguyn t khc c thnh phn l 15%.
188
Xt
nhy,
ni thch
chunganh
ccchu
n nhit,
kp thng
cm,
nhy
km knh
hn cc
tng
Thnvn:
Mt ng
di 18 c
- 15
ng
6 - n
5 cm.n
Mt
u
ng,n
hayEDL
tt nht
ch s
gnS.bng
Mt khc,
vqua
chcng
to li
khtrong
khnsut
hnvi
nchm
n.
ca
cngcng
c ca
Ca l
s cng.
cho chm
sng i
phi
V th.cng ch c mt s t n kp v cng ch c dng trong mt s trng hp khi vic
sng
thay i
n ng
c nh
hng
qu trnh
phn ng.
tch vCun
trongcm
cc c
my
nhiu
th n
HCL
Ngoi
thch
anh n
l cun
cm bng
cng
sutknh
t 800
- 400
W
kp
l
u
vit
hn
n
n.
ty loi n ca tng nguyn t, v c ni vi ngun nng lng cao tn HF ph hp
nn
HCL
lmlm
vic
ti (hnh
mi ch
Ngoi
dng nht
cho nhit.
chm sng pht x c cng
nui cho
EDL
vic
9.4).
cngnh
l vth
tschu
nht
nh.
Cht
trong n l vi miligam kim loi hay mui kim loi d bay hi ca nguyn t
Mi
s lm
dao sao
ngkhi
vton
dngbin
nh hi
hng
ca
phn tch,
chtlm
havic
hi ca
bo n
mu
cho lm
p sut
ca n
kimcng
loi trong
chm
tia sng
x
(hnh
9.2).
Do oCltrong
mitphp
o mmHg.
c th phi chn mt gi tr cng
n
iu
kinpht
nhit
t 800
- 550
khong
1 - 1,5
dng
in
phthay
hpcho
v gi
ctrong
nh trong
sut qu
trnh
o nh
mt nguyn
t.x ca
Cht
ny
catot
n HCL,
n l
ngun
cunglng
cp chm
tia pht
n phng
intch,
khng
ccb(EDL)
nguyn
t phn
khidin
chng
kch thch, trong qu trnh n EDL hot ng.
Kh trong
n EDL
ht ht khng kh v npthhai
thay vo
l mt
Ngun
phtn.
tia Trong bc
x cng
n phisc
cdng
kh
trphp
Al, He hay Nit c po
sutph
thp,hp
vi mmHg
trong
th khi u cho s lm vic ca n EDL.
nguyn
t l nui
n phng
in
khng
in
cc.lng cao tn nui n EDL lm vic c ch
Ngun
n lm
vic.
Ngun
nng
to theo
hain
tnny
s. Tn
sng
v tnv
s cung
sng cp
raiochm
27,12tiaMHz,
sut
Loi
cngsnh
nngn
HCL450
uMHz
c nhim
pht c
x cng
c trng
di
1 kW. t phn tch, c bit l cc kim, th n EDL cho nhy cao hn, n nh hn
ca nguyn
n HCL.
Bng 9.1
9.3lng
l nhng
d in
v iu
. hai tn s khc nhau nn n EDL
Do ngun
nuivlhnh
nng
cm vng
t vi
cng
Bng c
9.1 chia thnh hai loi: 1. n EDL sng ngn, ngun nui tn s 450 MHz, v 2. n
EDL
sng
sng
raio
MHz.
So snh
raio,
nhy ngun
v giinui
hn tn
phtshin
ca
n27,12
HCI v
EDL
Nguyn t
nhy (pl/mL)
Gii hn pht hin (pl/mL)
HCL
EDL
HCL
EDL
As-193,70
1,10
0,80
0,80
0,400
Cd-228,80
0,03
0,02
0,01
0,008
Pb-283,20
0,10
0,07
0,05
0,030
Hg-253,60
6,00
4,50
0,50
0,200
Sn-286,30
2,50
1,60
0,20
0,100
Zn-213,90
0,03
0,02
0,02
0,018
V cu to, n EDL thc cht cng l mt ng phng in trong mi trng kh km c

cha nguyn tcn phn tch vi mt nng nht
nh ph hp to ra
c chm tia pht x ch bao gm mt s vch ph nhy c trng ca nguyn t phn tch.
Hnh 9.3
n EDLn
cng
gm
cc
b phn:
phng
in
khng
in cc
190
189
191
Cng vch ph v vng tuyn tnh ca As-193,7 v Se-196,1 i vi hai loi n

HCL v EDL. Khi n lm vic, di tc dng ca nng lng cao tn cm ng n c nung
nng
, kimloi hay mui
kim loitrong
n c ha hi v b
nguyn t ha. Cc nguyn t t do c sinh ra s b kch thch v pht ra ph pht x ca

n trong iu kin kh km di tc dng nhit khi n lm vic. chnh l ph vch ca
kim loi cha trong n EDL.
Ngoi u im v nhy v gii hn pht hin, n EDL ca cc kim hay bn kim
thng c bn cao hn n HCL. ng thi vng tuyn tnh ca php o mt nguyn t
khi dng n EDL thng rng hn so vi vic dng n HCL (hnh 9.4).
Ngy nay cc hng sn xut my o ph hp th nguyn t sn xut c n 30 loi
n EDL cho 30 nguyn t. Nhng tt v c dng nhiu ch c 12 nguyn t kim v bn
kim l As, Bi, Cd, Hg, P, Pb, Se, Sn, Te, TI v Zn. Cc n EDL ca cc nguyn t ny u
c bn theo cc my ca hng. Nhng n EDL ca cc nguyn tkhc cnli t c
dng, v n khng
u vithn nHCL, m gi
thnh li t hn.
Ngoi n catot rng v n phng in khng in cc, ngi ta cng ch to ra
c nhiu loi n pht tia bc x n sc ca cc nguyn t, nh n catot rng cng
cao (trnh intensity cmiss Ion lamp - HIEL), n gradient nhit (controlled temperaturegradient lamp - CTGL), n phng in c chi sng cao (glow- discharge lamp - GDL).
Cc loi kin ny c u im hn n HCL mt cht v nhy, v vng tuyn tnh, v gii
hn pht hin. Nhng cc n loi ny li kh ch to v t tin, mt khc li km bn vng.
V th n t c dng v khng c bn ngoi th trng, ch yu ch c ng trong
nghin cu l thuyt v ph.
n ph lin tc c bin iu
Trong khong vi nm li y, mt loi ngun pht x ph lin tc cng c dng lm
ngun pht bc x cng hng cho php o AAS. l n hydrogen nng (D 2-lamp), cc
n xenon p sut cao (Xe-lamp), cc n hot ca kim loi W. l cc loi n pht ph
lin tc trong vng t ngoi v vng kh kin (UV-VIS). Cc tc
192
gi Fassel, Ivanop, Gibson, Mc G, Winerfordner l nhng ngi u tin nghin cu v s

dng cc loi n ny lm ngun pht bc x cng hng cho php o AAS.
n ny tuy pht ra ph lin tc, nhng nh h thng bin iu v h lc giao thoa, nn
chm sng pht x b bin iu v lng t ha thnh chm sng khng lin tc c ph
dng rng ca, mi rng ca cch nhau 0,2 nm, nn mi rng ca c coi nh l 1 tia n
sc. Hnh 9.5 l mt v d v h my o ph hp th nguyn t dng ngun sng bc x lin
tc. Trong ngun sng c t trc h thng bin iu v b lc giao thoa. Chm sng
ny khi i qua h thng bin iu v b lc giao thoa s b bin iu theo nhng di sng
nht nh dao ng vi bin nh nhau. Sau cng c chiu vo mi trng hp th l
ngn la hay cuvet graphit. Cc nguyn t t do trong mi trng hp th s hp th mt
phn nng lng ca chm sng ng vi mt di bin iu A, ca vng ph. Phn cn li s
i vo b n sc v detector pht hin v o cng sau khi qua b khuych i bng
sng theo di ph ca n nn li tn s. Tip cng vch ph hp th cng c o
v ch th theo cc cch bit, nh hin s digital, ghi pic trn recorder, hay dng printer in
ln bng giy.
Hnh 9.5
H thng my AAS dng ngun ph lin tc
1- Ngun ph lin tc; 2- H thng bin iu v lc giao thoa; 3- B phn nguyn t ha mu;
4- B n sc v detector; 5- B nn v khuych i tn hiu o
AAS.
Ngun pht ph lin tc c u im l d ch to, r tin v c bn tng i
193
cao, v ch cn mt n c th thc hin c php o AAS i vi nhiu nguyn t trong

mt vng ph UY hay VIS. Do n rt u vit i vi cc my ph hp th nhiu knh v
xc nh ng thi hay lin tip nhiu nguyn t trong cng mt mu phn tch, m khng
phi thay n HCL cho vic o ph mi nguyn t. Vi n ny, vng tuyn tnh rng, li
khng c hin tng t hp th ring (t o). Song v n sc v chn lc hay
nhy, th ni chung trong nhiu trng hp cn km cc n HCL hay n EDL nhng li u
vit v d dng i vi qu trnh phn tch t ng hng
ph hp
lot
trong cc my
thnhiuknh. Chnh v th
m trong
khong nm nm li y cc loi n ph lin tc c pht trin, ci tin v bt u

c s dng rt nhiu trong php o AAS v nhiu h thng my o ph hp th vi ngun
pht ph lin tc cng c bn trn th trng th gii.
Cc loi ngun n sc khc
Ngoi ba loi ngun pht bc x n sc ch yu c trnh by trn, trong php
o ph hp th nguyn t, ngi ta cng s dng mt vi loi ngun pht tia bc x n sc
khc na nh n catot rng c di cao, ng pht x c bit, tia laze. Nhng nhng loi
ny ch ch yu dng trong nghin cu l thuyt vt l.
nguyn t ha mu, trong php o ph hp th nguyn t ngi ta thng dng hai
k thut khc nhau. l k thut nguyn t ha bng ngn la ca n kh v k thut nguyn
t ha khng ngn la. ng vi hai k thut nguyn t ha c hai loi dng c nguyn
t ha mu.
K thut ngn
la. H thng
nguynt ha mu
bng ngn la
gm hai phn
chnh:
+ Bung aerosol ha (Nebulizer system), to th si kh mu,
+ n nguyn t ha mu (burner head).
Kh to ra ngn la nguyn t ha mu thng hay c dng l hn hp ca
cht kh (1 cht oxy ha v 1 cht chy), v d nh hn hp khng kh nn vi axetylen hay
kh N2O vi kh axetylen. i khi cng dng hn hp ca kh hydro vi axetylen hay khng
kh v kh propan.
H thng nguyn t ha khng ngn la. H thng ny gm ba phn chnh l:
+ Cuvet graphit hay thuyn Ta cha mu, nguyn t ha.
+ Ngun nng lng nung cuvet hay thuyn Ta.
+ B iu khin thc hin vic nguyn t ha mu theo cc giai on ca mt
chng trnh ph hp.
Nguyn l cu to, qu trnh hot ng ca cc loi trang b nguyn t ha mu
c m t chi tit trong chng 8 v k thut nguyn t ha mu.
194
H thng n sc v my quang ph hp th nguyn t

H thng n sc chnh l h thng thu, phn li, chn v pht hin vch ph hp th
cn phi o. Trong php o ph hp th nguyn t h thng n sc ny l mt my quang
ph c phn gii tng i cao c th l h my mt chm tia hay h my 2 chm tia. Cu
to ca n gm ba phn chnh:
H chun trc, chun trc chm tia sng vo;
H thng tn sc (phn li) phn li chm sng a sc thnh n sc;
H bung ti (bung nh) hi t, hi t cc tia cng bc sng li.
c trng cho h quang ca my AAS l cc thng s.
+ tn sc gc;
+ tn sc di;
+ phn gii (tn sc);
+ Vng ph lm vic ca h.
Bn thng
s
ca
ny
cng l cc
yu t xem xt cht
lng
mtmy quang
ph AAS.
Trc h chun trc l khe vo ca chm sng a sc v sau h bung nh l khe ra ca
chm tia n sc cn o. Hnh 3.6 l s quang hc, nguyn tc ca h thng my quang
ph hp th nguyn t. Theo s ny, chm tia pht x cng hng ca nguyn t cn
nghin cu c pht ra t n catot rng sau khi qua mi trng hp th, s c hng vo
khe my v vo h chun trc, ri vo b phn tn sc, vo h hi t chn 1 tia cn o.
Nh vy chm sng a sc c chun trc, c phn li v sau ch mt vch ph cn o
c chn v hng vo khe o tc dng vo nhn quang in (detector-photomultiveler)
pht hin v xc nh cng ca vch ph hp th .
Mun h thng
my quang ph hp thnguyn
t cho c kt qu tt th h
thng tn sc phi bo m c mt s yu cu bt buc sau y:

N phi c tn sc ln c th tch v c lp c tt cc vch ph
cn o, trnh s quy ri, s chen ln ca cc vch ph khc bn cnh. Trong cc my hin
nay, b phn ny thng l mt h ccht c hng s t 1200
n 2400
vch/mm.
Phi khng gy ra bt k mt hin tng sai lch no lm mt nng lng ca chm
sng trong my, nh s hp th, s tn x, s khuych tn ca cc b phn cu to thnh
my. c bit l cc h thng gng, cc thu knh, khe vo, khe ra ca chm sng. Cc thu
knh phi trong sut trong vng ph lm vic ca my.
Khe vo v khe ra ca my phi c m chnh xc v phi iu chnh c cho ph
hp vi tng vch ph v c lp li cao trong mi php o.
195
Detector pht hin cng vch ph phi c nhy cao. C nh th mi c th

pht hin c s thay i nh trong qu trnh hp th ca vch ph ca mi nguyn t. l
cc iu kin ti thiu ca h quang hc trong my ph hp th nguyn t. Vi s pht trin
ca khoa hc v k thut, ngy nay ngi ta c th tha mn c tt c cc yu cu . Chnh
v th hin nay c rt nhiu my o ph hp th nguyn t c cht lng cao c bn
trn th trng quc t. l cc my o ph hp th nguyn t ca hng Perkin Elmer,
Varian, Becman, Philips Pye Unicam, Wet Zeiss, Shimadu, Instr, Lad, Alpha,...
Hnh 9.6
S quang hc ca h thng my AAS
(1)- Loi 1 chm tia; (2)- Loi 2 chm tia; V d v 1 h my AAS ca hng
196
Perrkin Elmer
Trang b pht hin, Detector, Photomultivlier
Detector l mt loi dng c quang hc dng thu nhn v pht hin tn hiu quang
hc theo hiu ng quang in ca n. Trc y thu nhn cng ca chm sng ngi
ta thng dng knh nh hay phim nh sau l t bo quang in. l cc dng c c in
c nhy km, nht l knh nh, v knh nh c nhiu nhc im, nh kh bo qun, d b
nh hng bi m, nhit , thi tit. Mt khc, n li l mt dng c trung gian thu
nhn chm sng v sau phi x l tip mi c c cng vch ph. Tc l o en
ca knh nh b chm sng tc dng vo. Vi s pht trin ca khoa hc v k thut, ngy
nay ngi ta ch to ra c nhiu loi detector quang hc kiu ng c th khuych i tn
hiu o ln c n c triu ln. l cc ng nhn quang in (photomultivler tube). Hnh
9.7 l s ca mt nhn quang in kiu ng .
Nhn quang in kiu ng l mt loi dng c thu nhn tn hiu quang hc c tnh
cht vn nng, n c nhy v chn lc cao. Nhiu hng ch to c cc detector
loi ny. Vng ph hot ng ca cc detector kiu ng loi ny thng l t 190 - 900 nm,
c khi n 1100 nm. Tt nhin l thng s ny ph thuc vo bn cht ca nguyn liu ch
to bn catot ca n.
Hnh 9.7
H s khuch i ca loi detector ny thng n 106, i khi c loi n 107.
Nguyn liu ch to bn catot ca cc detector kiu ng l cc hp kim ca cc kim loi
kim vi Sb, Ga hay As, v d hp kim Cs-Sb; Ga-As; Na-K-Cs-S (hnh 9.8).
197
9.5 K thut o cng vch ph hp th

Cng ca cc vch ph hp th sau khi c detector pht hin v khuych
i s c a sang h thng ch th kt qu. y n c th c khuych i tip
v x l c c cng thc ca vch ph hp th. n nay ch th (biu th)
cng ca vch ph hp th nguyn t, c nhiu cch khc nhau t n gin n
tinh vi phc tp. Sau y l mt vi k thut v ang c s dng trn cc my o
ph hp th c bn trn th trng quc t.
Thang o mt quang (thang o
nng lng hp th ca vch ph).
y l mt phng php n gin
nht v c dng t khi my quang
ph hp th nguyn t mi ra i.
Theo cch ny, cng ca vch
ph hp th c biu th theo thang
o mt quang D. Thang o ny
c cu to v phn chia theo quy
lut ca thang logarit ca t s gia
cng tia sng i vo v i ra khi
mi trng hp th.
Nh vy, im gc ca thang o s c mt quang D = 0, ngha l khng c s hp
th. im cui ca thang o l im c hp th l 100%, ngha l D = 2. Trn tt c cc
my hin nay u c thang o ny. Cc gi tr D c c trc tip trn thang o theo lch
ca kim in k ch nng lng hp th E ca vch ph.
Phng php hin s (digital) ch hp th ca vch ph. y l mt k thut biu th
cng vch ph cng ang c dng hin nay. Cc s o hin trn mn digital ch trc
tip nng lng hp th ca vch ph cn o. Cng tng t nh thang o mt quang D,
cc s o ny cng t l vi nng ca nguyn t trong mu theo phng trnh c bn ca
php o AAS. Ngy nay tt c cc my o ph hp th nguyn t u c b phn ch th
cng vch ph theo nguyn tc ny. N c tn l b Readout. B Readout ca cc my
thng c 4 hng s l t 0 n + 9999.
Ghi cng vch ph dng pic. Cng ca vch ph hp th c th c a
sang my ghi (Recorder) ghi li di dng cc lc. S o cng vch ph lc ny c th
c tnh theo chiu cao ca lc hay din tch ca lc. V trong mt gii hn nht nh nng
C ca nguyn t phn tch chng ta lun lun c quan h:
H = kC
hay l
S = kC
Trong H l chiu cao v S l din tch ca lc. Cn k l mt h s t l. Hnh 9.9 l

mt v d v cc lc ca vch ph hp th vi cc nng khc nhau.
198
detector,
x lqua
theovic
cc o
yugi
cutrHthay
ra v
ta
chcng
theo mt
nht
nh ca
s o
Nhnvy,
S sau
chng
dngcch
c
ng
chun
v
cng
vch
nh
ghi bit
chiutheo
cao hay
lc,hp
hoc
hin s
trnCc
mnmy
vi deo.
xc nh
cph,
nng
printer,
C x cha
mt din
cchtch
ph
tng
ng.
o
V
yth
l k
thut vn
nngnay
nht.
phth
hp
nguyn
t hin
u c u sang my t ghi th o 0 - 10 mV v
a raTrn
b intergrator
0 - 1 V.
y l cc t
phng
php ang c dng ch th cng ca vch ph.
Phng
php
in my
trc
Hin
nay, cc
h thng
o ph hp th nguyn t bn trn th trng quc t u c
tipccgi
o bng
myphinnh th. Song chng ta c th s dng ng thi, hay chn
cchtro cng
vch
(printer).
mtthuc
k vo
thut
mt
k thuty
no l
l ty
mc trang b hin c ca tng phng th nghim v tng
hin i,
nhanh
v nhng
tin li.
cn thit nht nh cho ph hp. Nhng mun c c
ngi
nghin
cu c
yu cu
yqu
ccng
s n
o v
cng
kt
chnh
xc,vch
ngoi vic c c trang b hin i, cn phi c con ngi c
ph
hp
th
c
in
ngay
trn
kin thc v hiu bit chnh xc v php o AAS; Nh th mi lm ch c trang b phc v
bngcng
giy
nh
mycu
in ca
(printer)
cho
vic
nghin
mnh.
theo tng ln o v sau c
gi tr trung bnh ca n ln o.
y l k thut mi c pht
trin. Do ch nhng my o
ph hp th nguyn t hin i
mi c u a tn hiu ra
ch th theo cch ny. Bng 9.2
l mt v d v cch o ny.
Bng 9.2
V d v bng kt qu o ph ca mu (trch trong Report 09/20 - hng Philips)
Sample ID
Cu Abs
Cu Conc.
Fe Abs
Fe Conc.
Al Abs
Al Conc.
Saple 1
0.4583
2.9201
0.1523
2.1677
02085
29.6433
Saple 2
0.6738
4.3051
0.2003
2.8481
0 1128
16.0784
Saple 3
0.2856
1.8102
0.3589
5.0961
0 3789
53.7964
Saple 4
0.4126
2.6220
0.4126
5.8566
0 4055
57.5667
Saple 5
0.4933
3.1453
0.1855
2.6383
0 2369
33.6688
Saple 6
0.6337
4.0475
0.3333
4.7333
0 1278
18.2046
Saple 7
0.8568
5.4806
0.3725
5.2889
0 3014
42.8112
Microcomputer v mn video. y l mt k thut ch th s o hin i nht hin nay,

nhanh v tin li. Cc my o ph hp th nguyn t hin nay u c u ghp vi b
phn ny. Microcomputer l trung tnm ch huy ton b mi hot ng ca h thng my AAS,
iu khin mn video ch th cc thng s nghin cu v cc kt qu o c t ra theo
mt chng trnh nht nh. Microcomputer nhn s o t
200
199
Chng 10
CC YU T NH HNG TRONG AAS
Khi qut chung

Cc yu t nh hng n kt qu phn tch trong php do ph hp th nguyn t rt a
dng v phc tp, c khi xut hin v cng c khi khng xut hin, c nh hng hay khng
l ty thuc vo thnh phn ca mu phn tch v matrix ca n. Nhng nghin cu mt
cch ton din, chng ta im qua tt c cc yu t nh hng c th c trong php o ny.
Cc yu t c th c chia thnh 6 nhm sau:
Nhm l: Cc thng s ca h my o ph. Cc thng s ny cn c kho st v chn
cho tng trng hp c th. Thc hin cng vic ny chnh l qu trnh ti u ha cc thng
s ca my o cho mt i tng phn tch.
Nhm 2: Cc iu kin nguyn t ha
nhau ty thuc vo k thut c chn thc
mu. Cc yu t ny th hin rtkhc

hin qu trnhnguyn t ha mu v n
c nghin cu k trong chng II.

Nhm 3: K thut v phng php c chn x l mu. Trong cng vic ny nu
Do kt qu phn tch thu c khng ng vi thc t ca mu. V th, vi mi mt loi
chng ring.
Mt s nh hng trong php do AAS
Cc yu t v ph
S hp th nn
201
Yu t ny c trng hp xut hin r rng, nhng trong nhiu trng hp khng

xut hin. iu ny ph thuc vo vch ph c chn o nm trong vng ph no.
Ni
chung,
trong
vng
kh kin th yu t ny th
hin r rng. Cn trong vng
t ngoi th nh hng ny t
xut hin, v ph nn trong
vng t ngoi yu. Hn na,
s hp th nn cn ph thuc
rt nhiu vo thnh phn nn
ca mu phn tch, c bit l
matrix
ca
mu,
ngha
nguyn t c s ca mu. V
d: Khi xc nh Pb trong
mu sinh hc bng php o
ngn la th s hp th nn l
khng
ng k, nhng
khi xc nh Pb trong
nc
bin (nn
2,9% NaCl) th nh
hng ny l v cng ln (hnh 10.1).

Do , trong mi trng hp c th phi xem xt tm bin php loi tr.
loi tr ph nn, ngy nay ngi ta lp thm vo my quang ph hp th nguyn t h
thng b chnh nn.
Trong
ngi
ta
h
dng
thng
n
ny
hydro
nng (D2-lamp) b chnh

nn trong vng t ngoi v
dng n W (W-habit lamp)
cho vng kh kin. Do ,
trong mi php o xc
nh mt nguyn t chng ta
c th thc hin b chnh
nn hay khng l ty thuc
vo yu t c nh hng
hay khng. Hn na, ngy
nay ngi ta dng c hiu
ng
Zeeman
nn.
thut
b
ny
chnh
khng
nhng b chnh c nn c
hiu
qu
cao
hn
(hnh
10.2b), nht trong cc mu
202
nng
mui
nnln,
mgy
cnratng
csaisnhy
o cng
ln nhiu
hiuthc.
ng
hp th
gi, do
cng
nhng
cho ca
kt php
qu o
ln,
vchvph
Zeeman
dng
cng
khng
ca vch
phchiu
hp th
t ca
cc nguyn
K
Yu t c
nytcth
hinlm
rttng
r khi
chn
ng
caonguyn
ca n
nguyn
t ha t.
mu
thut
b hn
chnh
thkh
ba chy
l dng
n HCL
ng
chdo
thnh
k tip:
ch ca
dng
thp kh
(o
v khi
hp
khng
c hot
t chy
tt,haihay
phn
hn hp
tn
hiu
hp th
tng)
chhp
dng
caol(ch
hp th nn). Hiu gia 2 ln o
chy
khng
c
chnvph
(thng
quodcng
axetylen).
l tn hiu
hp tth
Cc yu
vtthc
t ca vch ph. Cch b chnh ny tuy c tin hn, v ch cn 1 n
HCL, nhng n HCL li chng hng, do phi dng ch dng cao lin tc trong qu trnh
Thuc v loi yu t vt l ny thng c:
o ph.
chen
nhtln
v ca
sc vch
cng ph
b mt ca dung dch mu
S
Trong php o AAS, vi k

thut nguyn t ha mu
trong ngn la, yu t ny
nh hng nhiu n tc
cc vch phn tch (bng 10.1a), th cc vch ph ny s chen ln cc vch phn tch, lm cho
dn mu vo bung aerosol
ha v hiu sut aerosol ha
c phn gii khng cao. V th, trong mi mc ch phn tch c th cn phi nghin cu
ca mu v t m nh
v chn nhng vch phn tch ph hp loi tr s chenln ca
cc
vch
phca nguyntkhc. Nubngcch ny m
Ni chung, tc dn mu t
khng loi tr c nh hng th bt buc phi tch b bt nguyn t c vch ph chen
l nghch vi nht ca
ln ra khi mu phn tch trong mt chng mc nht nh, cc vch chen ln khng xut
dung dch mu (hnh 10.3).
hin na.
Bng 10.1a
Chnh s khc nhau v nng axit, loi axit, nng cht nn ca mu, thnh phn
cachen
cc cht
cs
trong
dung
l nguyn
S
ln v
trng
vchdch
camu
cc nguyn
t nhn gy ra s khc nhau v nht ca dung
dch mu. V th, trong mi qu trnh phn tch mt nguyn t, nht thit phi m bo sao
cho mu phn Nguyn
tch v cc
chun phi
cngchen
nng
axit, loi axit v
t mu u lp ng Nguyn
t ccvch
ln(ppm)
thnh phn ha hc, vt l ca tt c cc nguyn t khc, nht l cht nn ca mu. Yu t ny
v vch
phn tch
(nm)
Vch
chen
Nng
xut
hin stachen
lndng
thng th
hin nhiu
trong
php o FAAS.
ln
loi tr nh
hng
ny chng
c th
/\
V-308,211
800
+ o v xc nh theo phng php thm tiu chun,
Cu-324,754
Eu-324,753
254
+ Pha long mu bng mt dung mi hay mt nn ph hp,
Fe-271,903
Pt-271,904
0,54
+ Thm vo mu mt cht m c nng ln, ng nht nht,
Mn-403,307
Ga-403,298
0,25
+ Dng bm y mu vi mt tc xc nh m chng ta mong mun.
200
Zn-213,856
Fe-213,850
Hiu ng 1u li
cc bin php Al-308,215

sau y:
Yu t ny th hin r rng c bit trong php o ph hp th khng ngn la v cng

Scht
hp phn
th ca
cccht
rn ln, ng thi cng ph thuc vo bn cht ca cc nguyn
ln khi
tch
nng
t, hp
Trong
cht mi
n tn
trng
ti trong
hp th,
mu,
ccng
bit nh
l trong
loi ngn
cuvetla
graphit
n kh,
cnhiu
dngkhi
cn
nguyn
c cha
t ha
c
mu.htNi
nguyn
t kh
baycha
hi v
cht bn
nhithay
lun
ra
cc
rnchung,
nh licc
ti ca
vt cht
mu
b d
hasinh
hiravhp
nguyn
t ha,
cclun
ht gy
mui
nh hng
t hon
graphit
Cc
hot ht
haloi
thng
hn chc
c
cacbon
ca ny.
nhinCc
liucuvet
chac
cch
t to
chy
ton.
ny thng
th hiu
c ng
lp
ny.ca
Hn
na,la.
b mt
ca cuvet
v
ngn
Cc bn
ht trong
ny hoc
hp th hoc chn ng i ca chm sng t n HCL
chiu vo mi trng hp th. Yu t ny c gi l s
204
203
6,11
00,20
Cayu
17,00
ha hi
ca
nguyn
t phn
tch.
Cc
cht
nn
nylthng
l
nhng
cht
bn
cng
lmt
ng
gp
vo
hiu
ng
ny,
ngha
bphn
mt 01,50
cng
mn hp
th
hng
cng
loi
trtnh
hng
ca
s
pht
x
ca
nguyn
t
tch
chng
ta nh
c
th
dngnhit
cc
ca
cc
nguyn
t,
nh
Al,
t
him,
v.v...
nh,
mt
cng
hng cng ln. 01,00
Do tnh cht ny m
khi nguyn thamu
bin b
php
sau
y:xp th nh
Ba
5,31
06,00
23,00 o
th
vic nghin
culngnh
cc nh hng ha hc c canguyn
trnh by trongtchng
ny
cngV
nhit
vchph
th mt
Chn
nguyn
t ha mu thp ph hp m ti nhit
s kch phn
thch ph
c tnh
chttkhi
tt c
ccIon
loiha
c thng
th c
chng
ta lu i
khi
Thc
cho qut
thy chung
rng,
qu
trnh
cv c
ngha
vi ng
cc dng
kim
tch
b nguyn
chng
c
li vi
trnnguyn
b mt ch
cuvet
phtkhng
x l khng
ngtkha,
hoc
khng
xylu
ra i
t
phn
tch.th tch t li qua mt
php
o
ph
hp
th
nguyn
t,
vi
mc
ch
bit
v
loi
tr
cc
nh
hng
ha
loilnkim
v t
sauha
mu.
l cc
kim n
loimt
kim
th,
cnthi
vibcc
nguyn
t theo
khcvsdoIon
s
nguyn
Nhng
ln
no
n
li
nguyn
t
ha
Thm
vo
mu
cc
cht
m
hn
ch
s
pht
x
ca
nguyn
t
phn
tch.
chnh
l
hc nu chng xut hin. Cc yu t nh hng v mt ha hc c th c sp xp
ha
khng
ng
k
trong
mi
trng
hp
th
ca
php
o
ph
hp
th
nguyn
t
(Fcc
mui
halogen
ca
cc
kim
loi
kim,
c
th
kch
thch
ph
pht
x
thp
hn
th
kch
thch
tora
docchcanguyn
t phn tch tng
t ngt
theo cc loi sau y,
dsnguynt
xem xt vt
tm
loi tr:
ph
pht
x
ca
nguyn
t
phn
tch.
AAS
hay
ETA-AAS).
loi
tr
s
Ion
ha
ca
mt
nguyn
t
phn
tch
chng
c
khngNng
theo
nng
l lm tng cng ca vch ph v dntan
axit
vca
loin
axittrong
trongmu,
dungngha
dch mu
Bng
th
dng
cc
bin
pht
sau
y:V th cn phi loi tr nh hng ny. loi tr nh hng
Nng
kt
axit
trong
lm
sai10.2
lc
qu
phn
tch.
dung
lun
ny chng
ta mu
ciu
thlun
theo
cch t
sau:ha c nhit thp ph hp, m trong iu kin
+dch
Chn
kin cc
nguyn
Mcnh
bhng
kch thch
pht x ca cc nguyn t trong cc nhit khc nhau No- S
c
nph
cng
nguyn
phn
tch
hu
khng
bnguyn
Ion ha.t
+ t
Lm
sch
cuvet
sau
habmu,
lmph
baypht
hix
ht cc cht cn li
nguyn
t
trung
ho
ban nh
u;
Ni -ln
S
nguyn
kch
thch
ca
vch
ph
cami
Nguyn
ttch phi
Tnhit
s Ni/No
nhittha nguyn t
trong +cuvet.
Ttvo
nhin
hin
nhitm
cao
nguyn
nguyn
t
phn
Thm
mu thng
phnthc
tchthch
mt(eV)
cht
cho hn
s Ion
ha.
l cc
mui halogen
Th
kch
oC
oC
qua
tc
dn
mu,
kh
phn
tch;
2000
3000
4000oC
ca cc kim loi kim c th Ion ha thp hn th Ion ha ca nguyn t phn
tch vi
nng ha hi v nguyn t
+ Dng
c vy
ch trong
to t iu
cc loi
c
hot
ha
ton
phn,
c
mt nng
cc
ln loi
ph cuvet
hp. Nh
kingraphit
t phn
tch3,00.10
s khng
b
-4 nguyn
-3
-2
4,00.10
-
7,10.10
ha caCs-852,10
cht mu. nh 1,76
b
mn;
Ionmt
hachc
na.v
Hnh
10.4
mt v d v tc dng ca cht m KCl v NaCl trong vic
hng
ny
thng
gnl lin
2,12
Na-589,00
1,00.10-5
6,00.10-4
4,00.10-3
loi loi
tr
s phn
Ion
ca o
haicc mu c nng nh trc;
vi
Anion
caha
axit.nn
+ Khi
tch
Ni
chung,
cc tch
axit Ba
cng
nguyn
t
phn
v 2,95
Ca-422,70
1,10.10-7
4,10.10-5
6,00.10-4
+
Thm
vo
mu
nhng
cht
m
c
nng
ph
hp;
kh bay hi v bn nhit,
Rb. Trong trng hp ny
Zn-213,90
5,86
7,00.10-13
6,00.10-8
1,10.10-6
+
Trng
b
mt
trong
ca
cuvet
graphit
bng
mt
lp
cc
hp
cht
bn
nhit.
nng ca kim loi m
Tt nhin
l nhng
nguyn tc chung. Cn trong thc t phi ty tng trng
phi thm
vo y
ti ch
thiu
l
Trn y l mt s yu t vt l c th c xut hin trong php o AAS v c th nh
hp
c
thgim
m
chn
cc
bin
php
ph
hp
nht.
cng
lm
nhiu
cng
vch
ph
hp
th
nguyn
t phn
250
^g/mL
hng
hng
n
ktth
qunh
phn
tch.
Nhng
mc
xyca
ra l
rt khc
nhautch.
trong mi trng hp c
th, c
c,
cca
khil
khng.
nynh
xut(hnh
hin10.5).
ln hay
nhny
l c
c th
phthy
thuc
ca
s
Ion
ha
khng
Skhi
Ion
ha
cht
phn
tch hng
Cc
axit
d
bay
hi
gy Mc
nh
iu
r vo
rngnhit
khi xc
ca
mi
trng
hp
th,
tnh
cht
ca
nguyn
t
phn
tch,
v
thnh
phn
ca
mu
phn
tch.
cn Ca
na.
khibaCa-422,7
nh
o tchung,
vch
ph
ccphn
mitch,
trng
ccIonaxit
4,
ylc
lNi
yu
vt
l th
nh hngnm
ntrong
kt qu
v quca
trnh
haHClO
thng
Do
cn
phi
xem
xt
tm
bin
php
loi
tr
khi
chng
xut
hin.
CH
COOH,
HCl, HNO
3, do
H2
SO4nguyn
, H3POt
4,phn
HF vi
mt
nong
lhp
2%th
(hnh
.6). do
xc3gim
nhs nguyn
cc
nguyn
tca
lm
t t
tchcng
trong
mi
trng
to 10
ra ph,
Cc yu
t
ha
hc
chung,
axitvch
lmtagim
cng
nu
vch ph theo
th t:tch
HClO
4 < HCl:
kim
th
th ccngi
lmNi
gim
cng
ph nguyn
hp
th,t
t phn
b Ion
hadng
cngvnhiu.
Trong
php
o
ph hp th
cc nguyn
nh hng
ha hc
cng
rt a
phc
thng
dng
KCl,
khi
phn
Nhng
mc
b
Ion
ha
ca
mi
nguyn
t
l
khc
nhau,
v
cn
ph
thuc
vo
nhit
ca
tp, n xut hin cng rt khc nhau trong mi trng hp c th v cng nhiu trng hp
Hnh 10.4
tch
cc
kim th.
loi
khng
xut hp
hin.
Cc
nhkim
hng
ha kin
hc thng
c th
ncc
ktnguyn
qu theo
hng
sau
mi
trng
Trong
mt iu
nht nh,
ni dn
chung
t bn
c th
Ion ha
Tc dng ca KCI v NaCI trong vic loi tr s ion ha ca Ba (10
y: thp
ngi
ta th
thng
cng
cng thm
b Ion CsCl
ha nhiu.
Vi mt nguyn t, th khi nhit ca mi trng hp
ng/mL) v Rb (10 |ig/mL)
Lm
gim
cng
ca
vch
ph
canhiu
nguyn
t Bng
phn 10.1b
tch, do
cht
vo
mu
phn
tch
theo
th cng cao, nguyn t cng b Ion ha
hn.
l s
mttovthnh
d vcc
iuhp
ny.
bn nhit,
hi (500
v kh- nguyn t ha, v d nh nh hng ca cc Ion silicat, sunfat,
trong
kh
phha
hp
Bng
10.1b
photphat,
florua.
1000 ppm).
Mc
Iontng
ha cng
ca mtsca
nguyn
t do s to thnh cc hp cht d ha hi v d nguyn
Lm
vch ph,
Shay
phtdo
x hn
ca nguyn
t phn
t ha,
ch c
nh tch
hng ca s Ion ha v s kch thch ph pht x ca
nguyn
t
phn
tch.
chnh
l
tc
dng
ca nng
mt s
ch yu t
l trung
mui halogen
ca
Yu t ny xut hin thng lm
gim
hp
cacht,
cc nguyn
ho c kh
kim loi kim v kim th hay lantanClorua.
nng hp th bc x trong mi trng hp th, do cng lm gim cng o ca vch ph
Nguyn
t
Ion ph
ha khi
(eV)nguyn t phn tch
S %
Iontrong
ha nn
nhit
( C):
S
tng cng
vch
tnbti
ca
mu
l nhng hp
hp th. Ni chung cc nguyn t c th kch thch ph pht x thp thng b nh hng
cht d ha hi. Lc cc cht nn ny c 20,00
tc dng nh l mt cht mang cho s ha hi
30,00
40,00
nhiu.
ngtthi
mi
trng
hp
thncc
nhit
hi
cng
caosut
th cao
nh
hng ny cng
ln (bng
ca nguyn
phn
tch
v lm
cho
ha
hiu
hn.
Na trong nhit 5,21
10.2). Nhng
ca php o AAS,00,30
th s kch thch 05,00
ph pht x thng26,00
ch xy ra
S gim cng ca vch ph khi nguyn t phn tch tn ti trong nn ca mu l
mnh
cc kh
kim
loihi.
kim
vny
sau
nguyn
l cc kim
th,
v hm
cc nguyn
t ny c
02,10
22,00
Kchti
4,32ha
nhngch
hpyu
bnvi
nhit,
Lc
cc
t nn
km
s 82,00
th kch thch
cc kim loi khc34,00
th s kch thch 90,00
ph pht x
Rb ph pht x tng
4,16 i thp. Cn09,00
l khng ng
2).
Cs k (bng 10.3,87
28,00
70,00
96,00
206
208
205
207
HN03 < H2S04 < HaP04

< HF, ngha l axit HCIO4 <
HC1 v HNO3 gy nh hng
nh nht trong vng nng

nh. Chnh v th trong thc t
phn tch ca php o ph hp
th nguyn t (AAS) ngi ta
thng dng mi trng l
axit HC1 hay HNO3 1 hay 2%.
V nng nh th nh
hng ca hai axit ny l
Hnh 10.6
10.2.3.2 v nh hng nh hng ca loi axit n cng vch ph

ca cc Cation c trong mu:
Ca-422,7nm trong php o F-AAS (kh.kh + C2H2)_______________________
Dung dch mu phn tch, ngoi nguyn t cn xc nh, thng cn cha cc

nguyn t khc. Cc nguyn t ny tn ti di dng cc Cation hay Anion tan trong
dung dch mu. Cc Ion ny c th lm tng, cng c th lm gim, hoc cng c th
khng gy nh hng g n cng vch ph ca nguyn t phn tch. Khi c nh
hng th mc nh hng ca mi Ion cng rt khc nhau trong tng trng hp c
th. Nhng mt cch tng qut th chng ta c th quy nh hng ca cc Cation theo
7 loi nh trong hnh 10.7 d xem xt.
Nh vy nh hng ca cc Cation n cng vch ph ca nguyn t phn
tch c th c hiu ng dng, hiu ng nm v cng c th c hiu ng va nm va
dng i vi mt Ion, khi n cc nng khc nhau.
Khng c
4
76
3
C[
c2
c3
c4
C5
Nng nguyn t nh hng
209
Hnh 10.7
Khi qut v nh hng ca Cation bao gm 7 loi
Loi 1: Khi C > C 2 khng nh hng; Loi 2: nh hng cc i Ci ; Loi 3: Gim
lin tc theo ng cong li; Loi 4: Khi C < C 2 khng nh hng; Loi 5: Gim theo ng
cong lm; Loi 6: Khi C > C2 khng nh hng na; Loi 7: Gim lin tc tuyn tnh, khi C
tng.
Loi l: Khi nng ca Ion gy nh hng ln hn C 2 th n khng lm tng cng
ln hn C2.
Loi 2: Ti nng C 1 ca nguyn t gy nh hng, cng vch ph ca nguyn t
phn tch t gi tr cc i. V th nh hng ny cng c dng tng nhy ca
gi tr khng i C1.
Loi 3: Trong trng hp ny cng vch ph gim lin tc theo ng cong li, khi
nng nguyn t nh hng tng dn u (xem v d ng 5 trong hnh 10.8).
Loi 4: Cc Cation ch gy nh hng n cng vch ph ca nguyn t phn tch
nh hn gi tr C2 th khng phi quan tnm n tm bin php loi tr.
Loi 5: Trong trng hp ny cng vch ph ca nguyn t phn tch li b gim
dn v y nht thit phi tm bin php loi tr nh hng ny (xem v d trong hnh
10.10a).
Loi 6: Khi nng ca cc Cation khc trong mu ln hn gi tr C 2 th chng khng

lm thay i cng vch ph ca nguyn t phn tch.
Do , nu khng tm c bin php loi tr ph hp th chng ta thm vo mu
Cation gy nh hng vi nng ln hn gi tr C 2, a nh hng gim thnh mt gi
tr hng s cho tt c cc mu phn tch v mu chun. Nh th cng loi b c nh hng
Loi 7: y cc Cation l lm gim lin tc cng vch ph ca nguyn t phn
tch theo chiu tng dn nng ca n mt cch tuyn tnh (xem v d trong hnh 10.10b,
ng s 7).
Do cng cn phi tm bin php ph hp loi tr nh hng ny, hoc gi cho cc
Cation l c nng nht nh v khng i trong tt c cc mu chun v cc mu phn tch.
210
nh hng cc Cation trong dung dch mu n cng vch ph ca nguyn t phn

tch trong php o ph hp th nguyn t vi k thut nguyn t ha trong ngn la v khng
ngn la cng rt khc nhau.
V d. Ion La(III) trong php o F-AAS l yu t loi tr nh hng ca cc Ion l
khi xc nh Ca, Mg, Mn, Al, Fe. Nhng chnh La(III) li l Ion lm gim cng vch ph
ca chnh Ca, Mg, Al, Fe rt ln trong php o ETA-AAS. iu c ngha l mi Cation
trong tng trng hp c th v trong mi php li c tc dng khc nhau, m chnh n
trong php o ny th nh hng, nhng trong php o khc li khng gy nh hng.
minh ho v nh hng ca cc Cation l i vi vch ph ca nguyn t phn tch
chng ta c th xem xt mt s v d trong cc hnh t 10.8 - 10.11.
Hnh 10.8 l nhng v d v cc nh hng cc Cation thuc loi 1, 2 v 3. Cc ng
1, 2 v 3 l thuc loi 1. ng 4 v 6 thuc loi 2. ng 5 l thuc loi 3. Khi
ng trong hnh 10.7 l
biu din cc nh hng ca
cc
cc Cation thuc
loi 4. Trong hnh 10.10b, ng s 1, 2 v 3 m t cc nh hng thuc loi 6. Cui cng

ng s 5 m t cc nh hng thuc loi th 7 nh trnh by trn. Ngc li vi cc
nh hng trn, hnh 10.9 l m t nh hng tng hp ca cc Ion Mg(II), TI(IV), Al(III),
Fe(III), Si, P n cng vch ph ca nguyn t Ca 422,7 nm trong php o F-AAS vi
ngn la n kh nguyn t ha mu bao gm khng kh v axetylen, khi khng c mt v c
mt LaCl3 vi nng khc nhau.
y vi s c mt ca LaCla dung dch mu nng t 1 % tr ln th nh hng
ca cc Ion l nu l hon ton c loi tr. V th mui LaCla l mt cht ph gia c
dng loi nh hng ca cc Cation v Anion trong php o F-AAS vi hiu lc tt nht.
nhau:
211
Hnh 10.8
nh hng ca cc Cation thuc loi 1, 2 v 3
ng 1: Na/Rb 780 nm, n kh (khng kh + C 2H2);
ng 2: K/Ba 553,6 nm, n kh (N 2O + C2H2); ng
3: K/Sr 460,7 nm, n kh (N2O + C2H2); ng 4: La/P
213,6 nm, n kh (ETA-AAS);
ng 5: Fe/Ca 422,7 nm, n kh (O 2 + C2H2); ng 6:
Sr/Ca 422,7 nm, n kh (N2O + C2H2).
212
10
100
1.000
10.000
(ng/mL)
Hnh 10.9
ng 4: Si/ca 422,6 nm. F-AAS

nh hng ca cc Cation : (thuc loi 4)
ng 5: Si/Mg 285,2 nm. F-AAS
(-nt- )
(-nt- )
(khi c
1% LaCl
3) +
ng
6:283,3
Si/Ca,Mg,
F-AAS
Al, Fe, Ca
n Pb
nm, ETA-AAS;
Cu. Ni, Fe n As 193,7
nm,mt
F-AAS
(kh.kh
C2H2).
(kh. kh + C2H2)
ng 7: Ti/Mg 285,2 nm, F-AAS
nh
hng
ccx
anlIon
c ph
tronghp
mu
+
Chn
iuca
kin
mu
loi cc nguyn t nh hng ra khi dung dch
Cngtch
vicc
mu phn
oCation,
ph. cc Anion cng nh hng n cng vch ph ca nguyn t
phn tch nh hng ny v tnh cht tng t nh nh hng ca cc loi axit. Ni chung,
+ Chn cc thng s ca my o thch hp.
cc Anion ca cc axit d bay hi thng gim t cng vch ph.
+ Thay i hay chn vch ph khc, c th km nhy mt cht.
Ch ring c hai Anion ClO - v CH3COO- l gy hiu ng dng (lm tng), tc l lm
+ Thm vo mu phn tch nhng cht ph gia ph hp chuyn mu sang cht nn
tng cng vch ph ca nguyn t phn tch trong mt s trng hp mt vng nng
khc ph hp nhm loi tr cc nh hng ca cc Cation, nh LaCl 3, SrCl2, AlCl
3 trong php
nht nh. Cc Anion khc thng gy hiu ng nm (lm gim) theo th t Cl - < NO- < CO- <
o -F-AAS
v LiBO2, NH 4NO3 hay hn hp (LiBO2 v NH 4NO3) trong php o ETA-AAS
SO < F- < PO4- < SIO^- v.v...Trong Anion
hay nhng
cht ph gia khc.
SIO^- c nh hng ln nht, cn t nht l Ion Cl. ng thi khi nng ca cc Anion tng
Tt nhin trong
mitrng hp c th cn phi nghin cu chn c loi
th tc dng nh hng cng tng theo (hnh 10.5).
cht v nng ph hp ca n.
Do thc t nn trong mi php o phi gi cho nng ca cc Anion trong mu
+
Chn
cc chun
iu kin
nguyn
mugi
thch
hp v
chn
lc.i.
phn tch
v mu
l nh
nhautvha
mt
tr nht
nh
khng
+ Vi tt c cc bin php trn m khng c, th bin php cui cng l bt buc
Mt khc cng khng nn chn axit H 2SO4 lm mi trng ca mu cho php o AAS
chng
phi
tchaxit
HCl
loi hay
b cc
Cation
c nh hng. Tt nhin bin php ny rt t khi phi
m chtann
dng
HNO
3 vi nng di 2% (hnh 10.12).
p dng.
1 Ax
------------------------------------6
Php o ETA-AAS
\ \\ 7
\4
|ig/mL NaCl
100
Hnh 10.10a
200
C(jj.g/mL)
Hlnh 10.10b
nh hng ca nng NaCl/Pb-217,0 nm nh hng ca cc Cation loi 5, 6, 7
214
ng 1: Ti/Ca 422,7 nm, F-AAS
(kh. kh +
ng 2: Ti/Sr 460.7 nm, F-AAS
(-nt- )
ng 3: Ti/Ba 553,6 nm, F-AAS
(-nt- )
C2H2)
213
2% hin c trong
LaCl nhng
Trong bn bin php trn, bin php th nht cng ch thc
3
chng mc nht nh, v chng ta khng th tng nhit
1,5% LaCl3
nguyn1t
ha3 ln
% LaQ
cao mi c, do
s hn ch ca trang thit b, bn cht ca kh t, hn na khi nhit

LaCl
nguyn t ha qu cao
0,5%
3
th li xut hin nh hng ca s tn ha v s pht x.

Cho nn bin php hai l thng dng nht. Cc cht ------0,1%
ph gia LaCl
thng hay c dng
3
trong php o F-AAS l LaCl 3, SrCl2, Li3, KCl, AlCl3, ------------ y LaCl3 c
0,05% s
Lad dng rng ri
3
nht, cc cht cn li ch cho mt s trng hp ring bit. Ngc li, trong php o ETA(Loi 5)
AAS cht ph gia c dng nhiu nht l LiBO 2, NH4NO3 hay hn hp ca hai cht ny
trong mt nng ph hp. iu ny chng ta c th thy trong v d ca bng 10.4.
**
nh hng ca dung mi hu c
'
0% LaCl 3
C(ig/mL)
Trong php o ph hp th nguyn t, c bit l i vi k thut nguyn t ha mu

trong ngn la, s c mt ca dung mi hu c trn ln vi nc trong dung dch mu phn
tch, hay mu phn tch ha tan trong dung mi hu c thng lm tng cng ca vch
2,5
7,5
125
250
375
40
60
10 p
ph hp th nguyn t 5ca nhiu nguyn

t ln
10 5). y l mt phng
10
15 nhiu ln20(bng
Si
500 Al, Fe
php
tng nhy. V
nguyn t c
rt nh st
Bng
10.4
25th, khi phn
50 tch cc 75
100nng
Ti
20
gii
80 Mg
thm vo mu phn
nh hng ca thnh hn
phndica
nn caphp
mu o,chng
phn tch ta c th
tch mt dung mi hu c c nng ph hp th c th tng nhy ca phng php phn
Hnh 10.11
tch ln n hai hay i khi n ba ln so vi khi ch dng dung mi nc. Song dung mi hu
Cht nn ca mu
Cng
vch
ph
C=30
ppb php
nh
hng
nguyn
t n
422.7nm
trong
php
o F-AAS
khi o
c v
c thm
vo t
hp
phica
trnmt
us
c
vi nc
v Ca
phi
c tinh
khit
cao.
ETA-AAS
khngNu
c mt
LaCl
dung
mi3 khng tinh khit cao th chng ta li lm nhim bn mu phn tch. Hoc
Thnh
phn
mutan trong nc th chng
nu dung
mi
hunn
c ca
khng
ta c th
nguyn t
Mg-202,60
nmchit
Ca-422,70
nmphn tch t
dung mi
dng
phc,
d cc
Me-APDC
trong
dungphi
mi lc
huno
c,
Yu nc
t nh
hnghp
nycht
ngi
ta v
quen
gi phc
l matrix
effect. vo
Nhng
khng
0,220
1
Dung
dch
HCl
1%
0,250
sau
o ph
ca nguyn
t phn
dung hp
mi hu
Thng thng l
cngxut
hin,hp
mth
thng
ch thy
trong tch
mttrong
s trng
nht c
nh.
dung
micc
MIBK
(Methyl
Izobutyl Ketone)0,020
l hp
dungcht
mibn
hunhit,
c in
chit
2.d
Nh
1,
thm
2%nguyn
LaCl
0,025
3 t nn di dng cc
nhngV
mu
c
cha
khhnh
bay
hi
v
cc
phc
Me-APDC
cho
php
o
F-AAS
(Me:
l
cc
Ion
kim
loi
nng,
APDC
l
Amonium
kh nguyn t ha.
3. Nh
1, thm 0,5% LaCl
0,050
0,060CHCl 3, CCl4
Pyrolydine
Dithio-carbamate.
Cc3 phc Me-APDC c
chit tt vo MIBK,
V d: Khi xc nh cc tp cht lng vt trong cc mu oxit t him, oxit kim loi
trong mi trng pH t 2 - 6).
kim th,4.oxit
nhm,
oxit1%
zircon,
cc +LiBO2
mu mui NaCl,0,210
th cc nn ny s kh
cng ca
Nh
2, thm
NH NO
0,245
Vic s dng dung mi hu4 c 3 y c hai cch:
vch ph ca nguyn t phn tch, qua lm gim nhy ca phng php phn tch.
Nu dung mi hu c tan trong nc th ngi ta thm vo dung dch mu phn tch
Trong
trng
yu
t phn
ny
hng
ln, php
thm phn
ch
trng
loi
tr nh
hng
ca
thnh
nn gim
ngi
ta ca
c chc
th
dng
nhiu
binc
php
khchp
mt nng
nhiu
dung
mi
huhp,
c
thch
hp
lm
tng
nhy
phng
tch.
hng
trm ln cng ca vch ph (bng 10.4). Nguyn nhn chnh ca
nh
nhau:
Nu dung mi hu c khng tan trong nc th ngi ta chit cht phn tch dng hp
hng
nyca
lnhit
sntn
cathuc
cc
cht
nhit
Tng
nguyn
t hp
ha
cht phc
viti
mt
thmu.
thchbn
hp
votrong
dungmi
mitrng
hu chp
.th.
Nh th va tng
Cc
hp
cht
ny
lm
kh
trqu
hi v
hacc
ca
cc
nhy, va
loi
tr
c
cc
Ion
cnkhn,
tr.ccn
Thm
vo
mu
cc
cht
ph
gia
nng
phtrnh
hp ha
ngn
cnnguyn
s xut t
hin
hp
cht
bntnhit.
nguyn
phn tch.
chuyn mu sang cht nn khc, y l 1 bin php c dng kh ph bin trong php
o AAS loi tr nh hng ca cht nn mu.
Tch b nguyn t nn, khi hai bin php trn khng t kt qu. Tt nhin bin php
ny l hn hu.
216
217
215
Bng 10.5
nh hng ca dung mi hu c n cng vch ph
STT
Dung mi hu c thm vo
Cng Cu-324,70
Chng 11 1
Dung dch HCl 0,1 M
PHN TCH NH LNG BNG PH AAS
2
Nh 1, thm 40% CH3OH
3
1,000
1,670
Nh 1, thm 40% C2H5OH
1,750
Nhng vn chung
4
Nh 1, thm 40% Axeton
Phng trnh c bn ca php o
2,000
5 o ph
Nhhp
1, thm
20 % Izobutanol
2,400
Trong php
th nguyn
t, mi quan h gia cng ca mt
vch ph hp
th ca mt nguyn t phn tch v nng ca n trong mi trng hp th cng tun theo
6
Nh 1, thm 70 % Axeton
2,500
nh lut hp th quang Lamber-Bia. Ngha l, nu chiu chm tia sng n sc cng I o i
qua mt mi trng
cha
loi nguyn
t t do nng N v cb
7
Nhmt
1, thm
50 % EAK
mi quan h gia Io
v
phncng
sng
8
Nh
1,80
%
Ethyl
Amine
Ketone
(EAK)
trng c tnh theo cng thc:
9
Trong MIBK
log10 K(Methyl
'N L Izobutyl Ketone)
(11.1)
dyl
2,600 L cm, th
Itqqua mi
2,800
3,000
y i lng lgI o/I chnh l nng lng ca tia sng b mt i do s hp th ca

cc nguyn t t do trong mi trng . Nh vy, n chnh l cng ca vch ph hp th
v chng ta c:
Ax = k'.N.L
(11.2)
Cng thc ny cho chng ta bit mi quan h gia cng ca mt vch ph hp th

v nng ca nguyn t trng thi hi trong mi trng hp th. Nhng n cha cho bit
mi quan h gia cng ca vch ph v nng ca nguyn t trong mu phn tch.
Nh vy, nu gi nng ca nguyn t trong mu phn tch l C th chng ta cn phi tm
mi quan h gia C v N v t s suy ra c mi quan h gia C v A. M t nng C
trong dung dch chuyn thnh nng N trng thi kh, c c bi qu trnh ha hi v
nguyn t ha mu phn tch. Nghin cu vn ny, nhiu kt qu thc nghim ch ra rng,
mi quan h ca s chuyn ha gia C v N l rt phc tp v n ph thuc vo nhiu yu t
nh:
+ Bn cht ha hc ca mi nguyn t, trng thi lin kt,
+ Tnh cht ca hp cht m cc nguyn t tn ti trong mu,
+ Thnh phn vt l v ha hc ca mu phn tch, c bit l cht nn,
+ Cc iu kin thc hin qu trnh nguyn t ha mu.
Tuy c phc tp, nhng t nhng kt qu thc nghim v trong mt phm vi nht
218
219
nh ca nng C ca nguyn t cn nghin cu trong mu phn tch, mt cch tng qut,

th mi quan h gia C v N c xc nh theo cng thc:
N = k.Cb
(11.3)
trong k l mt hng s thc nghim, n ph thuc vo tt c cc iu kin ha hi

v nguyn t ha mu v khng i trong nhng iu kin nht nh c chn cho mt
php o, c bit l nhit ca mi trng hp th.
Cn b l mt hng s, c gi l hng s bn cht, n ph thuc vo nng C, tnh
cht hp th ph ca mi nguyn t v tng vch ph ca nguyn t . Hng s b c gi tr
bng v nh hn 1 (0 < b < 1).
Khi nng C ca nguyn t phn tch nh th b lun lun bng 1. Khi C tng th b nh
dn xa gi tr 1, tin v 0, tt nhin khng bao gi bng 0. Nh th, vi mi mt vch ph ca
mt nguyn t phn tch, chng ta lun lun c mt gi tr nng Co, m vi mi gi tr:
+ Cx < Co th b lun lun bng 1, lc ny A ph thuc tuyn tnh vo C.
+ Cx > Co th b nh hn 1. A ph thuc vo C theo cng thc (11.4) - khng tuyn tnh.
Nh vy, t hai phng trnh (11.2) v (11.3) chng ta c:
Ax = K.L.Cb
(11.4)
trong K = k'.k v c gi l hng s thc nghim ca php o AAS. ng thi t

cng thc (11.4) ny chng ta thy, cng A ca mt vch ph hp th ph thuc vo ba
i lng (thng s K, L v C).
Nhng trong mt php o th K lun lun l hng s, L l chiu di ca ngn la trong
php o F-AAS hay chiu di ca cuvet graphit trong php o ETA-AAS, tc l b dy ca
mi trng hp th v nh th trong mt php o th n cng khng i. Do A ch cn ph
thuc vo nng C ca nguyn t cn xc nh trong mu phn tch. Do vy, mt cch
tng qut chng ta c:
Ax = a.Cb
(11.5 )
y chnh l phng trnh c s ca phng php phn tch nh lng da theo vic
o ph hp th ca mt nguyn t xc nh nng (hm lng) ca n v mi quan h
ny c minh ho trong hnh 11.1.
220
Nu b bng 1 th mi quan h gia A

v C l tuyn tnh theo phng trnh c
dng y = a.x. Khi ng biu din mi
quan h ny l mt ng thng i qua gc
to . Nhng thc nghim cho thy rng
trng hp ny l ch c trong mt vng
nng nh. y l trng hp l tng,
n ch c c i vi mt s vch ph
khng nhy ca mt vi nguyn t nh Fe,
Ni, Si (hnh 11.1b). Ph bin nht l trng
hp trong hnh 11.1a. l trng hp
chung cho hu ht cc vch ph hp th ca
cc nguyn t. N gm mt on tuyn tnh
(b=1) v mt on khng tuyn tnh (b< 1).
Ni chung trong trng hp ny thng
lun lun c mt on thng ca ng biu
din mi quan h gia A v C vng nng
nh ca nguyn t phn tch. l on
OA. Vi cc vch ph cng nhy th on
OA ny cng ngn. Tc l vng nng
ng vi on tuyn tnh l hp. Vng nng
ng vi on tuyn tnh OA c gi l
vng tuyn tnh ca php o AAS.
i vi mi nguyn t v mi mt vch ph th vng ny l khc nhau r rng (bng
11.4). Trng hp th ba cn li (hnh 11.1c) l mt dng phc tp. Trong trng hp ny
mi quan h gia A v C l khng tuyn tnh trong bt k vng nng no. Song ch rt t
vch ph, c bit l cc vch ph rt nhy v c kh nng t o ln mi tun theo quan h
ny. Trong phn tch, nu gp phi trng hp ny cn phi ht sc ch khi lp ng
chun, ngha l phi dng nhiu mu u c nng gn nhau dng ng chun v ch
c nh th chng ta mi xc nh c chnh xc v tr ca ng chun. Vch ph hp th
Na-589,00 nm i din trng hp ny.
Mu chun trong php o AAS
Trong phng php phn tch nh lng theo ph hp th nguyn t, mu u (mu
chun) dng ng chun cng bt buc phi tha mn mt s iu kin nht nh. Cc
iu kin l:
Cc mu u phi c trng thi vt l v ha hc nh mu phn tch, ngha l mu phn
tch tn ti trng thi, dung mi, mi trng v dng lin kt no th mu u cng phi c
tnh cht ging nh th. C nh th mi loi tr c nh hng ca cht nn, ca thnh phn
ca mu n kt qu phn tch.
221
Cc mu u v mu phn tch phi c pha ch hay ch luyn, x t trong cng mt

iu kin nh nhau.
Cc mu u phi bn vng theo thi gian, ngha l khng b thay i thnh phn sau
khi ch luyn v bo qun s dng lu di, khng b sa lng, khng b phn hy to
thnh cc cht khc lm thay i thnh phn ca mu u. C nh th mi bo m c
thnh phn ca n nh tnh ton pha ch v s dng lu di.
Nng ca cc nguyn t cn phn tch trong cc mu u phi rt chnh xc theo yu
cu ca phng php phn tch. ng thi khong nng ca mt dy mu u phi phn
b u trong vng tuyn tnh hay trong ton b ng chun ca php o v bao trm nng
ca cc mu phn tch.
Ngha l nng cc mu phn tch phi trong vng tuyn tnh ca ng chun. Cn
nu khng, chng ta phi pha long mu phn tch cho ph hp.
Biu din nng trong php o AAS
Trong php o ph
hp thnguyn t, ngi ta thng biu din nng
ca
nguyn t phn tch theo cc cch sau y:

Nng phn trm (%)
y l khi nim thng thng, n c biu th bng s gam ca cht phn tch, c trong
100g mu em phn tch. Nng ny c tnh theo cng thc:
C (%) = .100
m
(11.6)
trong mx l s gam cht phn tch c trong mu ly phn tch, cn m l s gam

mu phn tch.
V d, nu vit dung dch NaOH 0,1%, ngha l trong 100 gam dung dch c 0,1 gam
NaOH.
Nng microgam 1 ml hay microgam li
Loi nng
ny c c s dng ph bin
trong phn tch lng vt v
thng c biu th theo hai cch:

S microgam ca cht phn tch c trong mt lt dung dch mu (p,g/mL) hay s
microgam cht phn tch c trong mt mnh dung dch mu (p,g/mL).
V d, nu vit Cpb = 1,2 p,g/l th c ngha l c trong 1 lt dung dch mu s c
microgam ca Pb. Hay nu vit C pb: 1,2 p,g/mL th c ngha l trong mt minilit dung dch
S microgam ca cht phn tch c trong mt gam mu (p.g/g), hay s microgam cht
phn tch trong 1 kg mu (p,g/kg). V d, nu vit C pb = 2,5 p,g/g th c ngha l c trong 1
gam mu s c 2,5 microgam ca Pb.
222
Khi nim
Bng
11.2 v nhy
Bng
11.1
nhy l mt i lng ch ra kh nng ca mt phng php phn tch theo mt k thut o
Mi
quani
h gia
gia cc
cc nng
loi n
Chuyn
v nng (d=1)
no c p dng cho phng php phn tch . Phng php phn tch c nhy cao tc l
nng gii hn di c th phn tch c l nh. Cng nh cc phng php phn tch khc,
Nng u c
Chuyn sang nng th 2
n vphp
gc phn tch theoTng
ng
vi (1) t cng phTng
ng
viyu
(1) t khc
nhy ca phng
ph hp
th nguyn
thuc vo
nhiu
Nng
nhau, nh.:
mpp
H s phi nhn vo
g/L
-3
0,001p
ppm
mg/mL
Trc1000
ht phi
k n cc c trng, 1
tnh
cht ca h thng my o, nh10hg/mL
quang hc, dng c
p
thu nhn v pht
hin
tn hiu cn o, h thng
khuch
i v ch th tn hiu 10
o.-6g/mL
chnh
l cc c
ppm
Mg/L
1 ppm
1 p,g/mL
trng k thut ca h thng

my quang ph.
m
1 ppbpp
1 n/mLmol/ (m)
10-90,000.1p.A
g/mL
Yu t th hai l cc iu kin v k thut thc hin nguyn t ha mu o ph ( nghin
% (trng lng)
-120,0001
1
pppppm
1 pg/mL
10
g/mL
cu k trong chng
2). V th phng php
nguyn t ha trong ngn la c
nhy km phng
php nguyn t1ha
khng ngn la. Bng 11.3
v bng
ppf
1 fg/mL
p,g/mL
ppm
l nhng v d v vn
ny.
10-15g/mL
1/p
1 ppa
1 ag/mL
10-18
p,g/mL
% (trng
1ca
/g/mL
10000
.p
Yu t th
ba
l kh nng v tnh cht
hp
th bclng)
x ca mi vch ph,
mi nguyn
t.
Vch ph no, nguyn
mnh th php o theo vchP c nhy
ppbt no c kh nng hp th cng
ng/mL
n v gc
Tng ng vi cc n v sau
cng cao. Ngha l i vi mt nguyn t cc vch ph khc nhau cng s c nhy khc nhau
(bng 11.3, bng 11.4 v bng 11.5). V th, khi ni n nhy ca mt nguyn t phn tch l phi
n
g c th nht
^g nh ca
Ngmt php o.
g
trong
: iu kin phn tch
gn lin
vi nhng
pa
fg
-3
mgt chnh, tt nhin

10
l ba1yu
cn nhiu yu t khc cng nh hng n nhy ca mt
p: t trng ca dung dch

-6
-6
1
phng php phn
ca
mu, 10
nguyn
t c s ca mu. V vy, nu lm tt, ngha l
^gtch, nh axit10
A: nguyn t gam hay phn t gam ca cht phn tch.
tiu chun ha c cc yu t nu,-9 chng ta -9
s thu c-9 nhy tt nht ca mt php o. Nh
-6
10
ng Nu trong 110
Vi mu1 rn:
gam mu10
c cha 10
g cht phn tch th gi tr ny (10 -6g)
vy nhy l g? V vn ny, hin nay ngi ta c hai khi nim.
-12 l ppb, -12

-12ppa. Cc n v ny km
c gi l 1ppm.
Cc c s ca
n v10
ppm
10-12
10ppp, ppf10v
1 pa
nhy
tuyt i. Trong php o AAS, nhy tuyt i l lng gam (khi lng nh
nhau 1000 ln (bng 11.1). V d: Hm
lng
Cu trong-15thp l 5 -15
ppm, ngha
l c 1 kg thp
-15
nht ca nguyn
mi trng
cn thu
cng ca
10-15c trong
10-15
10 hp th10
10c
1 t
fg cn phn tch phi
th c 5 mg Cu, hay 1 Tn thp c 5 gam Cu.
vch ph hp th chn chim 1% ton
bng-18
hp th, hay
bng 3 ln
tn hiu-18
nn. Nh vy,
mi
-18
-18
10-5-18
10-18 ca
ag Nu trong 110mL
Vi mu1lng:
mu10c cha 10
g cht 10
phn tch10
v khi t trng
nguyn t v mi vch ph s c nhy tuyt i khc nhau (bng 11.4). Do , khi phn tch cc
-5
dung dch
mu
bng
1 th
ichn
lng
g/mL
c
nh
ngha
nguyn
t c
nng
nh
phi
cc10
vch
c mu
nhycng
cao
o v
ngc
li.l 1 ppm.
V d: Hm lng Fe trong nc l 2 ppm, ngha l c 1 lt nc th c 2 mg Fe.

nhy
tng
i.
tng i cn c gi l nhy nng . nhy ny
trong
: agattogram;
fg-nhy
femtogram;
Hai khi
nim
ny c
dng
tng t nh nhau. Khi mu phn tch l cht rn th
c nh ngha l nng nh nht ca nguyn t phn tch c trong mu cn c th pht
ngipata thng
dng
v l g(p,g/g),
picogram;
ng-n
nanogram
v p,g-kg(mg/kg),
microgram.hay tn(g/t); cn khi mu l cht lng th
hin c tn hiu hp th ca n theo mt vch ph nht nh chn v tn hiu ny phi bng
dng n v mu l m(p,g/mL), Lt(mg/L).
1% ca
bng
hpton
tontng
phn, t,
hayngi
bng 3taln
ng
nn.
nhy ny c dng
Cng
hon
cndao
dng
ccca
ngi
vtr
c
s Loi
ca p,g.
Nng
mol/lit
(M)
ph bin trong php o AAS hn khi nim v nhy tuyt i. K c cc phng php phn tch
l nanogam (ng), picrogam (pa). Do cng c cc khi nim nng ng/L, ng/mL,
Khi
ny
nycng
biuc
th s
phn
gam
cht
phnlng
tch cc
c cht
trongtrong
mtmu
lt dung
khc, th
khinim
nimnng
nhy
dng
pht
bin
hn,
v hm
phn
ng/g, pg/L,pg/mL v pg/g. Cc n v p,g, ng v pa u km nhau 1000 ln v mi tng
dchhay
mu.
l khi
nim
thng
haDophn
tch so
(xem
trnhgia
Ha phn tch
tch
muN
chun
thng
c
biuthng
th theo trong
nng .
, vic
snhgio
nhy
quan ca chng c ch ra trong bng 11.1.
nh lng c s).
Nng
ppm
v c
V d
vit
NaOH
0,1sM,ca
thn
c ngha l c trong 1 lt dung dch NaOH th c 0,1 phn
Loi
nng ppm (part per mill Ion: mt phn triu) thng hay c dng trong phn
t gam
NaOH.
tch lng vt cc cht, v cng c biu th theo hai cch, da theo mu dng lng (theo
n v ml hay lt), hay dng rn, hay bt (theo n v g, hay kg.):
224
225
223
Bng
11.5a
11.4
cc
A v
nguyn
C
lGii
tuyn
t, hn
giapht
cc
tnh,
vch
ng
phng
vi nhau
vi phng
s d dng
trnh
v thun
(11.8).tin
Khong
hn. Bng
nng
11.3 l
mt
C vi
ca
11.1.5
hin
trong
0,001
Mg 285,2
KK
- C2AAS
H2
0,005
0,1 - 4
v
nguyn
d
vt
phn
nhy
tch
ca
ng
mt
ng
sv
nguyn
phng
t
kimnh
trnh
loi
(theo
11
.8mt
) nguyn
ny
vi
c
vch
phlAAS
hp
khong
th nguyn
xc nh
t(hay
nhy,
gii
hn
pht
khong
cc
t gi
theo
Gii
hn
pht
hin
ca
php
ovi
ETA
- xc
AAS
theoca
cc
my
khc
nhau
Be
234,90
Bihin
0,002
1.000
0,00003
3ca
0,01
Mn
279,5cnh khi nim
KKv-
C2Hnhy
0,03
0,05
-pht
5 hin
2
Bn
ngi
ta
cn
s
dng
khi
nim
v
gii
hn
(theo
VH2/2P)
n
l khong
trong nhng
tuyniu
tnh)kin
ca nguyn
nguyn t
t ha
theo
nht phng
nh caphp
ngnla
nu.
nTrong
kh.
khong
y cc
nng
nguyn
ny
t
i
vi
mt
nguyn
t
khi
dng
mt
vch
ph
chng
minh
n.
Gii
hn
pht
hin
cng
Hg
253,7
KK
C
H
4,0
0,5
10
150
2 cng
2
khc
th quan
nhau,
h cc
gia
A422,70
vph
C c
khc
dng
nhau
ca
phng
c
trnh
nhy
ton
khc
hc
nhau.
y (pa)
= trng
ax.
Nguyn
t no, vch ph20
no c
223,10
Cavch
0,003
500.000
0,0002
Cc
c
cai
AAS
Nguyn
t
Gii
hn
pht
hin
tuyt
n
kh
Nguyn
t
Vch
khi
nim
tng
tx
nh
nhy.
o
l gii
hn
pht hin
i v
tng
Mo
813,3
KK
-C
H2php
1,9
0,15
- 200 mi
chai
kh
nng
hp
th cho
bc
mnh
th
vch
ctuyt
nhy
tng
i4i.
cao.
Thc
nghim
thy
rng
khong
xctheo
nh
i
vismi
nguyn
t
l khc
nhau,
nguyn
t2
ha
Vch
o(nm)
HGA-74
CRA-63
A-3470
IL-355
nhy
Gii
hn
pht
Khong
xc
nh0
Cd
228,80
o
(nm)
1.000
0,00001
Gii
hn
phtlnim
hin
tng
i
ca
mt
t theo
vch
0,2vph
313,3
N
2O nhau
-trong
C0,003
2H
1 - 100
Trong
hai
khi
trn,
php
onguyn
ph0,5
AAS,
nhmt
ngha
nht
nhynh
tng
i (
vchMo
ph
khc
nhau
rt khc
(bng
11.4).
0,1
(^g/mL)
0,2
hin (p,g/mL)
(p,g/mL)
Ag
328,1
4,
c th
xem
llun
nng
nh
nht
ca nguyn
t hay
trong mu
phn
tch php
cn phn
c thtch
pht
nhy
)
c
dng
ph
so snh
cc
0,02
Ninng
232,0
KK 2,0
-t
C2th
Hbin
0,07khc nh
0,2
- 15 tnh
2 cc vch ph
Ngay
trong
mt
nguyn
nhaugi
cng
sphng
c khong
tuyn
10,0
Al
309,3
30,0
90,
0,001
1.000
0,000001
1
1
2
3
4
5
hpth ca n theo vch ph trong mt iu kin nht
chin
th
cho
tng ctn
i tng.hiu
0,1
Ninhau
341,5
KK10,0
- C2no
H2 c hp- 0,4
- 80tuyn
khcAu
(bng 11.6). Vch
ph
th cng nhy0,6
th
c khong nng
242,8
101,
0,00005
nh
chn.
1,0 3.000
0,2
Al309,3
N2O - C2H0,003
2
2 - 200 10
0,0001
Mg
285,20
Bng
11.3
0,1
0,1
288,8
tnhCd
cng
hp v ko v pha
Nb
334,9
n2onng
- C2
H2 nh.
25,0
50,0
1002-, 4000
hin
t l khi lng
ti thiu ca
0,00002
SbNgc
217,6 li gii hn
KK pht
- C 2H
2 tuyt i ca
0,4 mt nguyn0,1
1 - 60
8,0
nhy
ca
mt
s
nguyn
t 5,0 xc nh ca4,0
Co
240,7
40,
V
th
khi
nim
v
khong
mt
nguyn
t
trong
mt
phng
php
phnth
Os
290,9
n
1,5
0,5
2
- 250hp
2 o - C 2H
2
nguyn
t cn c trong
trng hp th0,5
2.000
cn c th 0,2
pht
hin c1tn
hiu
As
193,7
Ar -mi
H20,001
- 50
2
Mn
279,50
0,00003
10,0
2,0
Cr
357,9
5,0
20
,
tch
gn
lin
mtmt
vch
ph
chn
v cc
iu
kin
th nghim
chn.
0,1
Pd
247,6
KK
- c
C 2H
0,25
1vn
- 40
2
ca
n
cngvi
trong
iu
kin
nht
nho
chn.
Bng
11.5
l
mt
vi v dvc
ny.
1,2
2,0
10,0
As324,7
193,7
KK - C2,0
2H20,01
10 - 7,
100 3
Cu
4,0
10.000
0,000001
Mo
313,30
Bng
11.6
l
mt
s
v
d
v
khong
xc
nh
ca
mt
s
nguyn
t
theo
cc
vch
ph
ca
n
1,0
Pd 247,6
O - C2t
H2v mi mt 2,2
5 - 200
Nh vy, mi mt 2nguyn
vch ph cng 0,2
c
gii hn pht 100
hin
khc nhau.
FeBa
248,3
3,0
4,0
,
0,2
553,6
n2o. c2h2
0,3
0,6 - 60
trong php
o AAS.
Trong
mt
nguyn
t,
vch
ph
no
c
kh
nng
hp
th
mnh
s
c
gii
hn
Vch
ph
(nm)
Tng
i
(pg/l)
Tuyt
i
(pa)
0,02
0,01
K
766,6
KK
C
H
0,04pht
- 0,1
4 hin
2
2
0,1
0,1
Mg
285,2
0,06 5.000
3,0
0,001
0,0001
Na
589,00
0,02
0,01
Be
234,9
n
0,04
4
2o - c2h2
Blng
chnhnh
nnhay
trong
php
AAS 11.5).
nng
o
nh
Pt 265,9
KK(bng
- C 2H 2
55,- 300
0,2
Mn
275,9
0,51,5
-0,3
0,2
Bi
223,1
KKnn
- C 2H 2
0,3
1 - 50
Ti
sao
phi
b
chnh
Nhng
ngoi
cc
yu
t
trn,
gii
hn
pht
hin
mt
nguyn
t
theo
php
o
ph hp th
20,0
Mo
313,3 Ag 328,10 n2o -3,0
13,0
10,0
8,0
Pt
C0,001
2H 2
0,002
100
0,00001
03,5 25 - 2000 1
C 265,9
357,90
12,0
10,0
B 249,7
n2ovo:
- ct2hlun
- 1500
2
nguyn
t
cn
Ph
hp
thph
cathuc
nguyn
c ph nn
l ti v tr25vch
ph
10,0km theo. Ngha
10,0
Ni
200
, cng
0,1
1,100
Rh232,0
343,5
KK10,0
- C 2H 2
0,5
0,010
238,30
07,5
0,01
Cd
228,8
KK
- C2,0
2H
2 v phn
0,003
0
,02
c cng
nn
cng thm
vo.
Trong
0,002
tch
nng
2.000
0,000002
ppm
hay
ppb)
phnca
Pb
Cu
217,0
3,0
3,0
10-,2th0,2
+324,70
Tnh
cht,
chtlng
cc c
trng
k nh
thut(mc
ca
mi
my
quang
ph
Rb 780,0
KK - C2H2
0,05
0,03
0,1 - 10
0,1
100,0
Cs
852,1
KKo
-200,0
Cnn
2Hhp
2nyth
0,03
Pt
265,9
catng
ph
nn
cng
khmy
ln,
ph
l:nguyn
hng
sn
ph
t (bng 11.5a).
Alxut
309,30
0,04
45,00,2 -- 10
1,0
Ru
349,9
KK - C2H
0,3
2 - 150 3
2
0,02
200.000
Fe
248,30
0,00003
100,0
SnCa
9,0
100
422,7
-nhn
Cph
2Htn
2
0,05
0,006
- n
8, h nhn
+
Cc
iu
kin
thu
hiu
cng
vch ph. 200,0

Yu
t ny lin
quan
+235,5
Ph
lin
tc,
cheKK
vch
AAS
chnh
cn
o,
396,20
0,07
60,00,1
0,2
0,2
1,20
Se
196,0
Ar
H
2
100,0
V Ca
318,5
400,0
400,
quang
in
422,7v vng ph.
N2O - C-2
H2
0,032.000
0,008
0,0002
K+766,50
0,00000580,00,05 - 4 0,3
Tng
dn
t
sng
ngn
sang
sng
di,
0,10
308,20
2,0
Se 213,9
196,0
KK 0,05
- C 2H 2
0,5
Zn
0,08
0,08
12, - 50
Bng
0,02
Cr11.5
357,9
KK - C2H2
0,08
0,2 - 15
Cng 394,40
ph nnNt
1,20
120,0 4 - 400
2,0n 2,0 aufs. 0,7
Si+251,6
2O0 -n
C21,7
H2 aufs, c khi
Gii
Pht
hin ca ncc
t theo
AAS
Crhn
357,9
cca
0,15
- 25
2o -nguyn
2h2 hng
Ghi
ch:
- HGA-74:
My
Perkin
Elmer,
CRA-63: 0,15
My
ca hng 0,4
VARIAN,
0,01
20.000
0,00002
2
Pb
217,00
AgV328,1
KK -lCkhi
0,1 - 10
2H2o nng 0,05
th phi loi tr, nht
nh trong vng0,006
VIS.
Cr 357,90
0,05
15,00,2 - 20
0,1
0,02
Co 240,7My
KK -Shandon,
C2H2 USA.
A-3470:
ca hng
0,01
Na
589,0
KK
C
H
0
004
0,02 -200
2
2
2
0,1
100,000
0,002
PtCc
265,90
phng359,40
php b
chnh
nn
0,01
Cu
324,8
KK
C
2
H
2
0,04
0,1
10
0,10
23,0
IL-355: My ca hng Instrumentat Ion Lao.0,1
0,02
Sr 460,7
n 2 o - C 2H 2
0,2 - 20
Hin
nay c425,40
4 phng
b chnh (loi
tr) ph nn:0,1
1,0
Ga
287,4
KK -php
C2H
20,04
2 - 150 10
0,20
45,0
0,0001
Sb
217,60
250.000
Khong
xc nh trong phpn2o
12,0
Ta 271,5
o -AAS
C 2H 2
4,0
30 - 2000
Nguyn
t
php o F 1,5
- AAS
Theo
- AAS.
Ge
265,2
n
o
- c2hTheo
0,4 php ETA
3 - 200
2
2
Phng
php
2
vch
ph.
Khi
nim nygn linKK
vi- C H mt nguyn0,5t v mt vch
ph ca nguyn
0,2
Te
214,3
1
- 80t
2 2
0,2
Se
196,00
50.000
0,0005
50
0,2
Cu
324,80
0,008
27,0
Au
242,8
KK
C
H
0,5
0,5
20
Vch
o
Tng
i
Tuyt
i
Tng
i
Tuyt
i
2
2
c s
dng phn tch n trong
mt tc
iu
nht nh chn. Trong php o ph hp
kin
b chnh.
TiPhng
276,8 php dng ngun
KK -sng
C2Hlin
0,4
0,06
1 - 80
2
(nm)
( a)phng trnh
( a)
10,0
th nguyn
Hf 307,3
t, vic
nhNlng
2O - Cmt
2H 2
nguyn t da
15,0
vo
c bn 54,0
30 - 2000
327,40
0,015
(p,g/mL)
p
(pg/mL)
p
Phng
php
da
theo
hiu
ng
Zeeman.
0,1
Sn
224,6
KK - C2H
0,4
1 - 6010
2
b
0,02
100.000
0,0001
Sn
235,50
In 303,9 216,50KK -Ax.
C 2H
0,4
1 - 100
= 2K.C
(11.7) 0,2
0,050
162,0
0,000001
Ag 328,10
0,6
SnPhng
224,6
n2o -n
C20,002
Hsc
2,45.000
5 - 3001
2 hot ng theo
php dng ngun
2 ch dng.
1,0 trong mi0,6
Ir 208,9
KK - C
2H2trn (mc 11.1.1),
2,5ch
- 200
Nh
chng ta nghin
cu
quan
h ny A
ph thuc
10.000
Sr
460,70
0,00005
0,02
20.000
25b
Alnay
309,30
2,0
Ti
364,3
N2Obn
- C0,002
2trn
H2 th trng0,005
0,4
20php
-1500
Hin
cc
my AAS
thng
thit k0,00002
dng 2 20,0
phng
Fe
248,30
tuyn tnh
vo
C
khi
b
=
1,
ngha
l
khi
nng
C
rt
nh.
Khi
chng
ta
c
th
vit:
8,0
Ir 208,9
n2o - c2h2
3,0
20 - 1500
chnh
193,70
l phng
php
Ngi mua
ty
yu cu m chn
loi35,0
no300-20000
cho thch 20
hp.
10,0
Wnn.
255,1
N2O2-v
C23.H
4,0
0,0001
As
0,15
25.000
248,80
0,007
100.000(II.8) 0,02
0,002 0,2 - 20
2000
TiFe364,30
0,1
248,3
KK -ACx2=HK.C
20,05
Sau U
y
l nguyn tc ca N
mi
phng php b150,0
chnh nn (BC). 80,0
358,5
2 - 15010
2O - C 2H2
0,01
100,000
0,0001
Au
242,80.
302,10
0,025
72,0h
Ngha
l
ch
trong
mt
khong
nng
C
nht
nh v nh,0,05
th
mi quan
Pb 2 1 7,0
KK - C2H2
0,15
0,3gia
- 25
20.000
318,50
1,0
2,00,001
VV318,4
n2o - C2H0,05
0,02 -100
2
2
Pb 283,3
0,320.000
0,07
0,75 - 50 50
252,30KK - C2H20,01
0,030
Ba 553,50
0,0005100,0
0,01
Zn 213,9
KK - C2H2
0,003
50 - 2000
0,02
Li 670,8
KK - C2H2
0,005
0,05 - 4
Zi 360,1
n 2 o - C 2H 2
15,0
5,0
4 - 400
226
232
230228
231
227
229
Phng php 2 vch ph

Nguyn tc:
Chn 2 vch ph o, l:
+
vch
ca
nguyn
phn
tch (gi l vch PT- pt) ta c APT

+ v
vch ca
nguyn
t so
snh (vch so snh- ss) ta c Ass

+
Cng
thc
tnh
nh sau (hnh 11.2):

Ath = (APT - Ass)
iu kin:
+ Cng ca ASS nm trong vng tuyn tnh, nhng phi nh.
+ Nng ca cht so snh phi nh v khng i trong mi mu.
+ Vch so snh phi gn vch PT, phi cch nhau t hn 10 nm.
+ Vch XSS phi gn, v r rng.
u v nhc im:
+ n gin, khng cn trang b BC.
+ B chnh trit .
+ Nhng li lm gim mt nhy.
Phng php dng ngun sng lin tc
Nguyn tc:
+ V ph nn l lin tc,
+ Nn dng ph lin tc BC.
+ Ngun sng lin tc c dng:
n HQ Hydro (D2-lamp) cho vng t ngoi (UY: 190-3 60nm), n W-Halid
cho vng kh kin (VIS: 380-1000 nm).
Cch o ph:
+ Phi o cng ca vch ph phn tch 2 ln.
+ Trc tin o cng tng Atot (khi D2-lamp khng hot ng), o nn An, khi D2lamp hot ng (n HCL khng hot ng).
233
Nh vy cng thc s l: Am = (Atot - An)

iu kin:
+ D thc hin, nhanh
+ C trang b BC h n D 2B chnh
trit
, n(VIS),
ht c 2 aufs cng nn.
Lamp+(UY)
v n
W-Halid
C b
mch
BChi(BC'++Thm
phnin
trang t
b BC
t tin:
Modul).
Phng php dng ngun n sc hot ng 2 ch dng
u v nhc im:
Nguyn tc:
+ Trang
BC khng
Da
theobhin
tng t,
t o ca vch ph cng hng (vch nhy) ca nguyn t
cng +D
n
HCL
rt ln. Lc ny vch ph b ch i, phn tnm vch ph ch cn nn.
thc
hin,
+ B
trit ,
ch cng n HCL bnh thng ta s c A ,
Nh
vychnh
nu ta khng
o cng
lc u
tot
c
khi
nn
nh
hn
1,3
aufs.
sau cho n HCL ln cng cao (100-150 bnh thng) v o th ta ch c cng
Phng
php
da theo
hiuca
ngvch
Zeeman
- Nguyn
tc:
ph nn.
Nh vy
cng
thc
ph Ath
l:
+ Khi c hiu ng Zeeman, vch ph ca
nguyn t PT b phn thnh 2,4,... nhnh i
Ath = (Atot - An)
xng qua tnm vch (v tr o), cn ti v tr tnm
(1)
Hiul ng
Hieftje
Lan) pht hin. Nn phng php ny gi l phng
vch ch
nn ny
ca do
phSmith
lin tc
(hnh(H
11.4).
php BC
Hieftie.
+ Smith
Nh vy
nu o ph khi c v khng
c hiu
iung
kin:Zeeman th ta kh b c ph
nn lin tc.
+ C mch BC theo nguyn.l Smith Hieftje.
iu kin:
+ C n HCL hot ng c dng rt cao.
+ C h thng in t iu khin BC
Cch
o ph:
(BC- Modul),
X
0,00 5 run
a+
(2)
a-
++Trc
tin o cng
hp
C trang
b ngun
cp th,
hiukhi
ngHCL dng bnh thng,
(1
A
^
+Zeeman.
o cng hp th, dng
~~
Hnh 11.4
cao ca-Cch
n HCL,
o:
Bchlnhni
c hiu ng Zeeman
Dtot dng bnh thng
hiu ng
Zeeman
Ath
Saunn
ly ta
hiu
2 ln
ta phn
+ BC
o s
ph
ca o,
vch
tch
ti 2 cng
thi im:
c
thc.
o cng
u v +
nhc
im: tng Atot, khi khng c hiu ng Zeeman,
theo hiu ng Zeeman

Dn dng cao
+ Sau
ny
o cng
.
nn An, khi c hiu ng Zeeman.
+ Phng
php
BC trit
cng
thc
+ n Nh
HCLvy
dng
kh cao
l rtca vch ph Ath l:
Hnh
Ath =Hnh
(Atot
11.5- An)
t (gp 3 ln n HCL thng).
u im v nhc im:
+ n HCL hot ng c dng
BC nn theo phng php Smith Hieftje
rt cao, rt chng hng.
234
235
11.1.8 Ti u ha cc iu kin cho php o AAS

Bng 11.6
Mun
xctnh
nhca
mtphp
nguyn
Vng
tuyn
o t theo mt k thut o no , chng ta cn phi c mt quy trnh
phn tch c th theo k thut . Ngha l phi c mt phng php phn tch n nh. C nh th
Nguyn t vch (nm)
nhy (p,g/mL)
Vng tuyn tnh (pg/mL)
chng ta mi thu c kt qu chnh xc. Mun th, nhng ngi lm phn tch trc ht phi tin hnh
nhng nghin cu, th nghim ti u ha cc iu kin phn tch v xy dng mt quy trnh phn tch
Al 309,3
0,2
1,2
2 - 30,
2,5
4, - 50,
Cc thng s ca h my o ph AAS thng bao gm cc yu t.
1 - 20,
,
-
237,3
Chn cc thng s ca my o ph
257,4
0,5
396,2
nhng vn sau
y cn c gii quyt:
c th theo k thut m mnh nh p dng cho mc ch ca mnh t ra. Cng vic ny bao gm
Ba 553,6
0,08
0,1 - 10,
Vch ph o. Vch ph c chn xc nh nguyn t mnh mong mun.
455,4
0,1
0,5 - 15,
Vch ph ny phi tha mn iu kin:
350,1
48,0
0
,
0
5
0
5
+ Khng
b cc vch khc quy ri, chen ln gy nhiu
Cr 357,9
0,03hay trng lp.
0,1 - 10,
+ Phi r359,4
rng v nt, c di sng chnh xc.
0,2 - 15,
0,06
+ Cng425,4
vch ph hp th A phi ph thuc tuyn0,3
tnh vo nng C 1trong
- 25,mt vng nng
nht nh.
429,0
0,6
1,2 - 30,
+ Vch
phi nm trn mt nn khng qu ti. 0,05
Fe ph
248,3
0,1 - 10,
Tt nhin
khi cn xc nh cc nng rt nh th0,15
phi chn vch ph c
nhy cao v ngc
252,3
0 3- 15,
li, khi xc nh cc nng khng nh th cn chn cc vch km nhy hn.
271,9
0,25
0,5 - 25,
Cng dng lm vic ca n HCL. Cng dng in lm vic ca n catot rng
372,0
0,5
0
0,1 - 6,
,
3
-
0,02
Mg 279,5
(HCL), ni chung nn chn cng dng nm trong vng t 60% n 85% so vi cng cc i
ghi trn n HCL. Khi cn nhy cao th chn cn di, cn khi cn n nh cao th chn cn trn.
279,8
0,04
0,2 - 8,
Khe o ca my quang ph. Khe o (khe vo v khe ra ca chm tia) c nh hng n nhy
0,1 ph hp th thng c khe o thay i
v vng tuyn280,1
tnh ca php o. Ni chung nhiu my quang
0,3d 0,2; 0,4; 0,8; 1; 2 v 10 nm. Nhng i
c theo cc 403,1
gi tr t 0,2 n 10 nm theo 5 hay 4 bc. V
5
,
2
-
vi nhiu vch
ph th khe o ph hp l nm trong vng0,04
t 0,2 n 1 nm. Do 0,1
cn
phi chn ch mt
Ni 230,0
- 10,
gi tr ph hp331,1
nht cho php o nh lng mt nguyn t 0,1
theo vch ph c chn, lm sao ch cho
6
,
-
2
0
va vch ph cn o vo khe o l tt nht.
,
2
-
234,6
0,25
Burner Head Hight. Chiu cao n nguyn t ha mu, nu chn khng ng ra s khng
341,5
0,3
0
,
3
1
nhng thu c nhy km v tn hiu o khng n nh, m ng thi li b nhiu yu t nh hng.
Cu 324,7
0,01
0,1 - 5,
Thi
gian o. Thi gian o, s ln o cng vch ph. Yu t ny ph thuc vo c
327,4
0,02
0,7
1 - 25,
Si 251,6
0,06
250,7
1,2
288,2
8,0
2,
1
216,5
0,8 - 20,
0,5
2
0
217,9
,
-
trng k thut ca tng my quang ph v ty thuc vo k thut nguyn t
,
2
2
236
10 - 80,
237
ha mu. Vi php o F-AAS th l thi gian thu c tn hiu hp th n nh, vi php o ETAAAS th li l thi gian nguyn t ha mu (xem chng 8 ).
6.
Lng mu. l tc dn mu, lng mu bm vo.
Vng
tuyn tnh ca vch ph c chn nh lng. Yu t ny cng cn c xc nh
chnh xc cho tng vch ph chn nh lng nguyn t phn tch. C nh th mi c th chun b
mt dy mu chun ph hp cho php o ca mnh. V cc kt qu thu c nm trong vng tuyn tnh
ca vch ph bao gi cng c chnh xc cao.
Phng tin ch th kt qu o. N c th l my t ghi lc cng vch ph, my hin s

digital, my printer hay my tnh ch trc tip hm lng (nng ) ca nguyn t phn tch. Tt nhin
chn phng tin no l ty thuc vo trang b m mnh hin c v l ph hp nht i vi mnh trong
iu kin thc t .
B chnh nn khi o. Yu t ny c thc hin hay khng l ph thuc vo vch ph c chn

o. Nu nn ca ph c nh hng th phi thc hin php o c b chnh nn loi tr nh hng
v ngc li, nu khng nh hng th khng cn thit. Trong php o ETA-AAS th yu t ny rt
quan trng, n nh hng rt ln n kt qu phn tch. Do cn phi ht sc cn thn trong mi
trng hp c th ca mi loi mu phn tch. V nn ca mu l mt nguyn nhn gy ra nh hng
n kt qu phn tch.
H nhn quang in nhn tn hiu AAS. Yu t cui cng trong vn ny l th lm vic ca

nhn quang in. Yu t ny l thang nng lng hp th ca php o AAS. Trn cc my thang ny
c chia thnh 100 n v.
Trong vng t 70 n 100 l vng lm vic ph hp ca th nui nhn quang in cho cc my
o ph hp th nguyn t v vng ny c nh du mu xanh hay mu en. Trong cc php o phi
iu chnh nm GAIN kim ch thang nng lng nm trong vng ny v phi gi mt gi tr
chn trong sut qu trnh o nh lng mt nguyn t.
1.8.2
Cc iu kin nguyn t ha mu
Vn ny ty thuc vo k thut c chn nguyn t ha mu. N c nghin cu k

trong chng II. Do y nu li mt s iu cn ch . C th l:
Vi php o F-AAS. Cn phi chn cc thng s sau y:

Nhit ngn la, tc l chn thnh phn kh chy to ra ngn la c nhit ph hp.
+ Chiu cao ca n nguyn t ha mu (burner head).
+ Tc kh mang v tc dn mu vo bung aerosol ha.
+ B dy ca lp hp th, tc gc nghing n nguyn t ha mu (burner head).
Vi php ETA-AAS. Bao gm nhng iu kin:
238
Thi gian, nhit ca cc giai on sy mu, tro ha, luyn mu v thi gian nguyn
t ha o cng vch ph.
+ Kh mi trng cho qu trnh nguyn t ha mu.
+ Cng sut t nng cuvet graphit nguyn t ha mu.
+ Lm sch cuvet graphit.
+ Lng mu a vo cuvet nguyn t ha o ph.
Cc yu t nh hng
Cc nh hng v ph.
Cc nh hng v vt l.
Cc nh hng ha hc ca cc Cation v Anion c tng mu.
nh hng ca thnh phn nn ca mu.
Cc yu t ny c cp k trong chng 10. Tt nhin cc yu t ny cng ch c
trong mt s trng hp nht nh v nhiu trng hp l khng c. Nhng cng cn phi
bit chnh xc khi n xut hin th tm bin php loi tr ph hp.
Chn quy trnh x l mu ph hp
X l mu l cng vic u tin ca ngi lm phn tch. Nu x l mu khng tt th tt
nhin s c kt qu phn tch sai, hoc nh (lm mt), hoc ln (lm nhim bn thm).
Trong phn tch lng vt (vi lng), giai on x l mu l cc k quan trng i vi
c qu trnh phn tch. V trong giai on ny chng ta c th lm mt hay lm nhim bn
thm nguyn t cn xc nh c khi n hng chc, thm ch c khi n hng trm ln nu
chn quy trnh x l mu sai v cc ng tc trong qu trnh x l mu thc hin khng cn
thn.
Cc ngun gy sai trong qu trnh x l mu c th l:
+ Mi trng lm vic khng sch yu cu.
+ Dung mi, ha cht (axit) dng x l mu khng tinh khit.
+ Dng c ng, cha mu khi x l khng tt, khng sch.
+ Nc ct khng tinh khit.
Phng php chn x l mu khng tch chit c tt nht nguyn t cn phn tch
vo dung dch phn tch.
Cc cht chun khng t yu cu cao.
l cc vn cn c ch trong mi trng hp c th.Cc vn ny s
239
c trao i chi tit trong mt xemina ring.
Phng php chun ha nh lng

Ngoi 4 yu t trn, nhng nu phng php chun ha c chn nh lng khng ph hp
th cng cha thu c kt qu chnh xc v ph hp vi thc t. Vn ny ty thuc vo bn cht v
thnh phn vt l ha hc ca mu phn tch.
V th phi ty theo tng trng hp c th m chn phng php ng chun hay phng php
thm tiu chun xc nh nng ca nguyn t phn tch trong mt i tng mu nht nh.
Trn y l tm tt cc vn cn thit trong qu trnh ti u ha cc iu kin th nghim
chn ra cc iu kin ph hp xy dng mt phng php theo mt k thut o nht nh.
Ngha l mun xut mt phng php phn tch th phi tr li c nhng vn mt cch
chnh xc v r rng.
chnh l cng vic nghin cu xy dng quy trnh ca cc nh phn tch. Cn khi c mt
quy trnh phn tch n nh ri th bt k k thut vin phn tch no cng c th tin hnh phn tch
c.
Cc phng php phn tch c th
xc nh nng (hm lng) ca mt nguyn t trong mu phn tch theo php o ph hp
th nguyn t ngi ta thng thc hin theo cc phng php sau y, da theo phng trnh nh
lng c bn ca php o ny qua vic o cng ca vch ph hp th ca nguyn t phn tch v
xc nh (hay pht hin) nng ca cht phn tch trong mu o ph theo mt trong cc phng php
chun ha sau:
Phng php ng chun;
Phng php thm tiu chun;
Phng php th khng i;
Phng php dng 1 mu chun.
Phng php th chun (ng chun)
Phng php ny cn c gi l phng php ba mu u. V nguyn tc ca phng php ny
l ngi ta da vo phng trnh c bn ca php o A - K.C v mt dy mu u (t nht l ba mu
u) dng mt ng chun v sau nh ng chun ny v gi tr A x xc nh nng Cx
ca nguyn t cn phn tch trong mu o ph, ri t tnh c nng ca n trong mu phn tch.
240
Do trc ht ngi ta
phi chun b mt dy mu u,
dy mu chun (thng thng l 5
mu u) v cc mu phn tch
trong cng mt iu kin. V d
cc mu u c nng ca
nguyn t X cn xc nh l C i,
C2, C3, C4, C5 v mu phn tch l
Cx1, Cx2 ,... Sau chn cc iu
kin ph hp v o cng ca
mt vch ph hp th ca nguyn
t phn tch trong tt c cc mu
u v mu phn tch c
chun b trn.
Hnh 11.6
V d ta thu c cc gi tr th chun ca phng php ng chun
cng tng ng vi cc nng

l Ai,
A
2 , A3 , A 4 , A5
x1, Ax2
v A
v.v... By gi trn h ta A - C
theo cc im c ta (C 1A1),
(C2A2), (C3A3), (C4A4), (C5A5)
ta s dng c mt ng biu
th mi quan h A - C. chnh l
ng chun ca phng php
ny (hnh 11 .6 ).
Hnh 11.6
th chun ca phng php ng chun
Tip nh ng chun ny v cc gi tr Ax chng ta d dng xc nh c nng C x. Cng

vic c th l em cc gi tr Ax t ln trc tung A ca h ta , t k ng song song vi trc
honh C, ng ny s ct ng chun ti im M, t im M ta h ng vung gc vi trc honh v
n ct trc honh ti im Cx, Cx y chnh l nng phi tm (hnh 11 .6 ).
Phng php ny n gin, d thc hin v rt thch hp vi. mc ch phn tch hng lot mu
ca cng mt nguyn t, nh trong kim tra cht lng thnh phm, kim tra nguyn liu sn xut. V
mi khi dng mt ng chun chng ta c th xc
241

(Aoc
, O). Sau

xc
C xt
cha
bithng
chngtrm
ta lmmu
nh phn
sau: tch. l u im ca
nh
nng
canh
mtnng
nguyn
trong
phng
phpI. ny.
trong nhiu
hptri,
chng
khng
chun
cCmt
dy
Cch
Ko Song
di ng
chuntrng
v pha
n tact
trc th
honh
ti bim
x. on
muX chnh
u tha
iu
quy
nh
cho phng php ny ( trnh by trong mc
OC
bngmn
gi trcc
nng
kin
Cx cntm
(hnh
11.7).
11.1.2)Cch
nn II.
khng
xccnh
xc
v tr ca ng chun v nh th tt nhin kt
Cng
thc
xc chnh
nh C
x bng cch t gc ta k mt ng song
qu phn
s mc
sai v
s ln.
NghaAlo khi
phn
tch song
c thnh
v chng
song
vi tch
ng
chun
t im
k mu
ng
song
vi phn
trc phc
honh,tphai
ng
ta cha
khng
th chun
c mt
dy gc
mu vi
u trc
nghonh,
n nnng
s b nh
ny
ct bit
nhauchnh
ti xc
imthM,
t im
M hb ng
vung
ny
hng
ca nn,
ca Cthnh
phn ca mu. chnh l nhc im ca phng php ny.
ct
trc honh
ti im
o, Chnh on OAC x l bng gi tr Cx phi tm (hnh 11.7).
Trong nhng trng hp nh th, tt nht l dng phng php thm tiu chun xc nh
Phng
php
ny
nng ca nguyn t phn tch trong mu, hay bin i ca mu sang nn t to ph hp
im l qu trnh chun b mu
cho c mu u v cc mu phn tch.
d dng, khng cn nhiu ha

Phng
phpkhit
thm cao
tiu chun
cht
tinh
chun b
dy
Trong
phn tch,
mu thc
u tnhn
to. c
Mtbit l xc nh lng vt cc kim loi, khi gp phi cc i
tng phn
tch ctrthnh
phnhon
phc tp v khng th chun b c mt dy mu u (mu
khc
li loi
c
chun)nh
ph hng
hp v v
thnh
phn phn
vi mu phn tch, th tt nht l dng phng php thm tiu
ton
thnh
chun.
Chcng
nh th
tr c
ca
mu
nhmi
culoitrc
vt yu t nh hng v thnh phn ca mu (matrix effect).
l ca cc
cht to
Nguyn
tcthnh
ca mu.
phng php ny l ngi ta dng ngay mu phn tch lm nn
Nhng
ch mu
u,
rng,bng
nng
chun bphi
mt dy
cch ly mt lng mu phn tch nht nh v gia thm vo
thm lng
vo nht
ca nh
nguyn
t
nhng
ca nguyn
t cn xc nh theo tng bc nng (theo cp s
phn
tch
phi
theo
tng
bc
v
cng). V d lng thm vo l AC1S AC2, AC3, AC4, nh th chng ta s c mt dy mu
khong
cch
chun nh
trongca
bngcc
sau, bc
trong Cx l nng (hm lng) ca nguyn t cn xc nh
phi
xp phn
x bng
trong mu
tch. nng Cx
phi tm.
Bng dy chun ca phng php thm tiu chun.

C nh th th phn ni suy tuyn tnh mi c ngha chnh xc.
Phng php ny c s dng rt nhiu trong phn tch lng vt v lng cc nh cc nguyn
t kim loi trong cc loi mu khc nhau, c bit l cc loi mu c thnh phn vt l v ha hc phc
tp, cc mu qung a kim.
ng
Co
thi y cng l mt
Lng mu phn tch
phng php phn tch.
thm
vo c nh
PhngLng
php
th chun
Cx
0
C1
C2
C3
C4
phng php xc nh pht
Cx
Cx
Cx
Cx
AC1
AC2
AC3
AC4
C5
hin ca
mt
Cx
AC5
Nguyn tc ca phng php ny l mun xc nh mt nguyn t no , trc ht ngi ta
Cht khc
Cc cht khc l nh nhau
cng phi dng mt ng chun nh trong phng php ba mu u, phng php ng chun.
Ax o c
Ao
Al
ng chun ny c gi l ng chun c nh (ng chun khng i) v ng chun ny

c dng lu di. Nh vy mun xc nh c nng C x cha bit, ta phi chuyn cc gi tr A xl
v cccng
iu kin
thnh
nghim
v gii
mtquyt
vch vnph
ca
tng Tip
ng
gi trchn
A xocc
ca ng
chun c
xc ph
nh hp
Cng.
ny
nguyn
tch,
tin
hnh ghi cng hp th ca vch ph theo tt c dy mu u.
ngi
ta t
c phn
hai cch
khc
nhau:
V d chng ta thu c cc gi tr tng ng l A o, Al,A2, A3, v A4.. By gi t cc gi tr
cng ny v ng vi cc nng thm vo ca nguyn t phn tch chng ta dng mt

ng chun theo h ta A - AC. chnh l ng chun ca phng php thm (hnh
11.7). ng chun ny ct trc tung A ti im c ta
242
243
y k c
xo kAxl
gil h s
chuyn ca
(a)
gi tr cng
ca vch
ph gia hai
ln o trong cng mt iu kin th nghim.

Mun th mi khi phn tch ta ghi li ph ca mt mu chun, v d thng dng nng Ca.
Nh th, ta c gi tr Axo-3 ca ng chun c nh, v hm nay ta li c gi tr A xl-3, do h s
chuyn k s c tnh theo cng thc:
xo-3/Axl-3
k: A
(b)
Sau khi c h s k ta em n nhn vi cc gi tr cng A xl ca ngy lm phn tch ta s thu

c cc gi tr cng tng ng vi ng chun c nh. By gi ch chiu cc gi tr vo
ng chun c nh l tm c cc nng C x.
Cch th hai: T thc t phn tch khi nghin cu cc ng chun ngi ta thy rng, trong cng
mt iu kin th nghim, i vi mt nguyn t khi o trn mt vch phn tch, nu ng chun dng
c t dy ph ca cc mu chun ghi trn cc ln khc nhau, th chng u l nhng ng thng
song song vi nhau hoc trng nhau (hnh 11. 8 a). Ngha l cc ng c cng h s gc. T thc t
ny c th suy ra cch dng ng chun phn tch mi ch nh mt mu chun m khng phi tnh h
s chuyn k nh trn. Mun th, khi ghi ph ca cc mu phn tch chng ta cng ghi li ph ca mt
mu chun dng dng ng chun c nh, v d nng Ca. Sau cng chn mt vch phn
tch dng dng ng chun c nh, o cc gi tr Ax ca chng v gi tr Ax-3 ng vi nng
Ca. T cc gi tr Ax-8 v nng Ca t ln h to dng ng chun c nh chng ta c mt
im A, ri qua im A ny ta v mt ng song song vi ng chun c nh th ng ny chnh l
ng chun phn tch. Dng n v cc gi tr A x ta s tm c cc nng C x ca mu phn tch (hnh
11 .8 b).
Trong thc t, nu my o tt, iu kin mi trng khng kh ( m, nhit ) khng i v cc

iu kin thc nghim tht n nh, th cc ng chun (I) v (II) hu nh trng nhau Trong hai cch
nu, th cch th hai c ng dng nhiu hn v n n gin v khng phi tnh ton phc tp nh
cch th nht.
Phng php th khng i rt ph hp i vi php phn tch hng lot mu t ngy ny qua
ngy khc. V trong mi ngy phn tch chng ta khng phi ghi ph li ca ton b dy mu u nn
tit kim c thi gian, mu chun, ngha l c tnh cht kinh t hn phng php ng chun.
Tuy th nhng phng php ng chun (ba mu u) hay phng php ng chun c nh
u ging nhau l u phi chun b mt dy mu chun c iu kin ca mu u trong php phn
tch quang ph nh lng. iu ny nhiu khi khng thc hin c. c bit i vi nhng trng
hp mu phn tch c thnh phn phc tp m chng ta cha th bit c chnh xc. V th cng khng
th chun b c mt dy mu u c thnh phn ha hc v vt l ng nht vi mu phn tch. l
244
thc t v trong nhng trng hp th nh hng nguyn t c s v nguyn t th ba n

kt qu phn tch l rt r. iu ny th hin r khi xc nh cc nguyn t vi lng. Lc ny
chng ta phi hoc l thay i nn ca mu (Modify matrix) nu cch ny c hiu qu, hay l
dng phng php thm tiu chun.
Phng php mt mu chun
Khi c mu chun
Trong nhng trng hp n gin, chng ta cng khng cn pha mt dy chun dng
th chun, m c th tnh ngay gi tr C x nh mt mu chun Cl ca cht phn tch. Ngha
l chng ta c:
V i mu phn tch:
Ax = a. Cx (a)
Vi mu u:
Ao = a.Cl (b)

C: (Ax/Ao).Cl (11.6) Nh vy khi o c
v ch vic nhn n vi gi tr Ci l chng ta
gi tr Ax
vAo ta c t scachng,
c gi trnng Cx phi tm theo
biu
thc (11.6).
Khi khng c mu chun
(a)
a C
. x
245

Atch= a.(Cx + ACl)
(b)
Do cm (a) chia cho (b) chng ta c:

C = [Ax/(Atch-Ax)]. AC1
(11.7)
Nh vy khi o c gi tr Ax v Atch ta c tnh c nng Cx phi tm theo biu

thc (11.7).
Nhng mt iu phi ch l nng thm vo ACl v cc gi tr C x phi nm trong
vng tuyn tnh ca phng php.
Trn y
l cc phng
php
nh
lng ch
yuhay csdng. Tt
nhin
mi phng
php u c nhng
u im v nhcimnht
nh ca n, v ngi

Cc kiu phng php phn tch theo AAS
Trong php o ph hp th nguyn t xc nh mt nguyn t hay mt hp cht

ngi ta c th tin hnh phn tch ngay chnh cht theo ph hp th nguyn t ca n,
nh phn tch cc kim loi, hay qua vic o ph hp th nguyn t ca mt cht khc, khi
cht phn tch khng c tnh cht hp th nguyn t, nhng cht ny li c mt s tng tc
rt nh lng v mt ha hc theo mt phn ng ha hc nht nh vi mt kim loi c ph
hp th nguyn t nhy. Do xut hin hai loi phng php phn tch nh lng theo ph
hp th nguyn t, l:
Cc phng php phn tch trc tip, cho cht c ph AAS v
Cc phng php phn tch gin tip, cho cht khng c ph AAS.
Sau y chng ta s nghin cu mt cch tm tt v hai loi phng php phn tch ny.
Cc phng php xc nh trc tip
V nguyn tc
th tt c cc nguyn
tv cccht c
phhp
th
nguyn
chng ta u c th xc nh n mt cch trc tip theo ph hp th nguyn t ca n t dung
dch mu phn tch. Ngha l cc phng php xc nh trc tip ch ph hp cho vic xc
nh cc kim loi c vch ph hp th nguyn t. V cc kim loi u c ph hp th nguyn
t ca n trong nhng iu kin nht nh. Theo cch ny, ni chung trong nhiu trng hp,
mu phn tch trc ht c x l theo mt cch ph hp c dung dch mu c cha
cc Ion kim loi cn phn tch. Tip tin hnh nh lng n theo mt trong cc cch
chun ha bit (nh theo phng php ng chun, phng php thm, hay phng php
mt mu u,... c trnh by trong mc 11.2 trn). y l cc phng php phn tch
thng thng, v ang c dng rt ph bin, xc nh lng vt cc kim loi trong
cc i tng mu hu c v v c khc nhau theo ph hp th nguyn t ca n. V th
ngi ta gi i
246
tng ca cc phng php phn tch ny l phn tch kim loi trong cc loi mu v c v hu c. V
d cc mu v c l qung, t, , khong liu, mui, oxit, kim loi, hp kim, xi mng, nc, khng
kh v cc mu hu c l mu thc phm, ng, sa, hp, rau qu, ung, gii kht, mu, se rum,
nc tiu, cc mu cy v sinh hc.
Khi phn tch cc loi mu ny th nguyn tc chung l gm hai giai on.
Giai on I: X l mu a nguyn t kim loi cn xc nh c trong mu v trng thi dung
dch ca cc Cation theo mt k thut ph hp, chuyn c hon ton nguyn t cn xc nh vo
dung dch o ph.
Giai on II: Phn tch nguyn t cn thit theo ph hp th nguyn t ca n theo nhng iu
kin ph hp (mt quy trnh) c nghin cu v chn ra.
Tt nhin, y giai on I l cc k quan trng. V nu x l mu khng tt th c th lm mt
nguyn t cn phn tch hay lm nhim bn thm vo. Ngha l vic x l mu khng ng s l mt
ngun sai s rt ln cho kt qu phn tch, mc du phng php phn tch c chn l ph hp
nht. Vn ny c bit c ngha ln trong phn tch lng vt cc nguyn t.
Cc phng php phn tch trc tip ny l thch hp xc nh cc kim loi, m bn thn
chng c ph hp th nguyn t. Nhng trong khong nm nm li y, nhiu phng php phn tch
gin tip xut hin phn tch cc cht khng c ph hp th nguyn t, v d nh xc nh cc
Anion, cc nhm phn t, cc hp cht hu c, cc dc phm.
Cc phng php xc nh gin tip cc cht bng AAS
Nguyn tc chung
y l mt phm vi ng dng mi ca php o ph hp th nguyn t phn tch cc cht
khng c ph hp th nguyn t hay ph hp th nguyn t ca n km nhy. Cc phng php ny
hin nay ang c pht trin v ng dng phn tch cc Anion v cc cht hu c.
Ni chung cc phng php xc nh gin tip cc cht khng c ph hp th nguyn t bng
php o ph hp th nguyn t c da theo hai nguyn tc chnh sau y.
Nguyn tc th nht ca cc phng php ny l nh mt phn ng ha hc trung gian c tnh
cht nh lng ca cht ta cn nghin cu X (cht X cn xc nh) vi mt thuc th thch hp c ph
AAS trong mt iu kin nht nh.
Nguyn tc th hai l da theo hiu ng l khi cht phn tch X c mt trong mu vi mt vng
nng nht nh, th n lm gim hay lm tng cng , vch ph hp th nguyn t ca mt kim
loi mt cch tuyn tnh. Sau y l mt vi phng php c th.
247
3.12 Cc phng php phn tch gin tip Cc

phng php theo cc phn ng ho hc
Theo cch xc nh gin tip ny, ngi ta c cc phng php phn tch c th sau y da theo
mt s phn ng ha hc bit:
Phn ng to ra kt ta khng tan (mui hay sunphua)

Ni chung, cht no khi tc dng vi mt Ion kim loi trong dung dch to ra c mt kt ta t
tan, c tnh cht nh lng v c th tch ra c khi dung dch mu th phn ng c th dng c
cho php o ny. Theo nguyn tc ny ngi ta xy dng phng php phn tch cc Ion SO 42-, Cl
C2O42-, po43-, NH4 +. V d xc nh SO42- ngi ta cho Ion ny tc dng vi dung dch BaCl 2 hay
Pb(NO3)2 c nng xc nh trong iu kin ph hp to ra kt ta BaSO4 hay PbSO 4- lc tch kt
ta khi dung dch. Sau xc nh Ba hay Pb theo hai cch hoc l trong kt ta sau khi ha tan chng,
hoc l xc nh lng Ba hay Pb cn d c trong dung dch sau khi phn ng vi Ion sunphat. Nh
vy t lng Ba hay
2-
ta Ion SO4 chng ta d dng tnh c hm lng ca Ion sunphat c
Pb tiu tn
kt
trong mu
phn tch. V d cc phn ng c s dng trong cch ny:

Cl- + Ag+ ^ AgCl ^ xc nh Anion ClBr - + Ag+ ^ AgBr ^ xc nh Anion Br
+ Ag+ ^ AgI ^ xc nh Anion IC2O42- + Ca2+ ^ CaC2O4 ^ xc nh Anion C2O42PO43- + Ca2+, Ca3(PO4)2 ^ xc nh Anion PO43SO42- + Ba2+ ^ BaSO4 ^ xc nh Anion SO42SO42- + Pb2+ ^ PbSO4 ^ xc nh Anion SO42PO43- + Mg2+ + NH4+ ^ MgNH4PO4 ^ xc nh Anion PO43Cng bng cch ny ngi ta tin hnh xc nh penicillin, vitamin B i, v.v... theo php o AAS
bng cch cho mu vitamin B l tc dng vi mt lng xc nh NaPbO 2 trong KOH nng chy 280oC
V trong iu kin ny, c mt phn t vitamin B i bao gi cng to ra mt phn t PbS. Sau tch ly
kt ta PbS, ra sch v ha tan n trong axit nitric 6 M v xc nh Pb. Ri t hm lng Pb ta tnh
c hm lng ca vitamin Bi trong mu phn tch.
Mt khc, y chng ta cng c th xc nh lng Pb trong phn NaPbO 2 d khng tc dng
vi vitamin B1, ri sau cng tnh c hm lng B 1.
Hin nay, theo cch ny, c nhiu hp cht hu c c cha S (lu hunh) c xc nh bng
php o ph hp th nguyn t, nu Ion S 2- trong phn t hu c tc dng c vi mt Ion kim loi
trong mt iu kin nht nh to ra c mt
248
sunphua kh tan c tnh cht nh lng. V th thuc vitamin B1 cc hp cht hu c kiu

diol cng c xc nh theo cch ny.
Penicillin + NaPbO2....................^ PbS
Vitamin B1 + NaPbO2..................^ Pbs
Theo phn ng to hp cht phc
Cht phn tch X phn ng vi thuc th l mt hp cht phc. Nguyn tc ca cch
ny l cho cht X cn xc nh tc dng vi mt phc cht thuc th kim loi to ra mt
hp cht phc bn c th chit tch ra c. Nhng phn ng ny phi c tnh cht nh
lng. Sau tch ly phc cht v xc nh hm lng kim loi trong phc cht , ri t
tnh ra hm lng ca cht cn phn tch X. V d axit phthalic hay cc mui phthalat c th
c xc nh qua phn ng ca n vi thuc th phc Cu(I)-Neocuproine to ra phc cht
mi l Cu(I)-(Neocuproine) 2 Phthalat. Sau chit ly phc cht ny vo mt dung mi hu
c ph hp, nh MIBK v xc nh hm lng Cu trong phc ny, t tnh ra hm lng
phthalic trong mu phn tch.
Cng tng t nh vy, ngi ta xc nh nng NO- qua phn ng ca Ion NO vi thuc th Cu(I)-Neocuproine to ra phc cht Cu(I)-(Neocuproine) 2_NO3_ chit c
vo MIBK. Sau xc nh Cu trong phc ny bng php o AAS, v sau suy ra hm
lng Anion NO- trong mu.
Cht phn tch X phn ng vi dung dch mui kim loi. Cch ny dng xc nh cc
Anion. Tt c cc Anion no c th tc dng c vi mt Ion kim loi to ra c mt hp
cht phc bn trong mt iu kin nht nh v chit ra c khi dung dch mu th u c
th s dng xc nh cc Anion .
V d xc nh Anion SCN qua phn ng ca Anion ny vi dung dch mui FeCl 3
Fe3+ + SCN
Fe(SCN)2+
Sau chit phc Fe(SCN) vo dung mi etyl ete v xc nh Fe trong dch chit ny
bng php o AAS (c th gii chit phc vo dung dch HCl 2M v xc nh Fe trong dung
dch gii chit ny). Sau ta cng tnh c nng ln SCN trong mu phn tch.
Qua phn ng to thnh hp cht d a axit
Theo cch ny, nhng kim loi, Ion hay hp cht c kh nng to thnh nhng hp cht
axit d a u c th xc nh c mt cch gin tip qua hp cht d a. V d nh photpho
(P), Anion photphat (PO 43-) hay ton silicat (SiO 32-),... c th c xc
249
nh bng cch cho n tc dng vi thuc th molipat trong mi trng axit HNO 3 a 6M,
to ra hp cht d a photpho-molipat kt ta, tch ly sn phm ny, ho tan n trong dung
dch kim 0,5M v xc nh Mo trong dung dch hp cht d a theo vch ph hp th nguyn
t Mo-313,0 nm. T tnh ra lng P c trong mu. Mui asenat v mt s hp cht alcaloit
cng c xc nh theo cch gin tip ny.
Cch ny c dng xc nh P, Si qua thuc th molipic trong mi trng axit
nc c 6M sinh ra hp cht d a ca P vi Mo theo phn ng:
PO4 3- + NH4+ + MoO42- + HNO3 ^ (NH4)3[P(Mo3O10)4]
m chng ta c dng trong phn tch ha hc xc nh P trong
t trng
bng phng php trung ha. Nhng y sau khi c c hp cht kt ta
d a ca
P, ngi ta ho tan n trong kim 0,5 M v xc nh hm lng ca nguyn t molipden, bng

ph hp th nguyn t ca Mo, sau suy ra hm lng P trong mu phn tch.
Qua phn ng kh Ion kim loi v kim loi
Mt s cht hu c khi tc dng vi mt s mui kim loi trong nhng
iu kin
xc nh, n kh cc kim loi v trng thi kim loi t do c tnh cht nh lng. V d nh
phn ng ca chc andehit vi mui AgNO 3 trong mi trng NH 3 (thuc th Tulene). Tnh
cht ny c ng dng phn tch cc cht hu c c nhm -CHO bng php o AAS.
Cc andehit c xc nh bng cch cho andehit tc dng vi mt lng d AgNO 3 ton
b andehit trong mu phn ng vi AgNO 3 , gii phng ra Ag kim loi, tch Ag kim loi, ha
tan n trong axit HNO 3 v xc nh Ag bng php o AAS theo vch ph Ag-328,1 nm, t
tnh ra hm lng andehit c trong mu phn tch. V trong iu kin ny c 1 nhm -CHO th
lun lun gii phng ra 1 nguyn t Ag kim loi theo phn ng sau:
R-(CHO)n + n(Ag+) ^ nAgo
V d vi andehit focmic (HCHO), th ta c:
HCHO + Ag+ ^ Ago
Phn ng th hay ph hu hp cht phc
Nguyn tc ca cch ny l cho cht phn tch X tc dng vi mt hp cht phc trong
mt iu kin xc nh, to ra sn phm mi bn hn phc ban u. Bng cch ny ngi
ta c th xc nh c cc Anion hay mt s kim loi khng nhy ph hp th qua mt kim
loi nhy ph hp th.
V d nh xc nh Anion F - khi cho n tc dng vi phc Fe(III)-SCN c nng xc
nh. Sau chit tch phn phc Fe(III)-SCN d v xc nh Fe trong phn phc d ny
theo vch ph hp th Fe-248,3 nm trong ngn la n kh axetylen khng kh.
250
Bng cch ny La v Ce l cc nguyn t khng nhy ph hp th nguyn t trong ngn

la axetylen-khng kh (DL > 20 p,g/mL) li xc nh c n nhy l
5 - 1 pl/mL. Bng cch bm mu phn tch cha La hay Ce vo dng cht mang nn l dung
dch phc Fe(III)-tartat hay Fe(III)-EDTA. Khi chiu cao ca lc hp th ca vch ph Fe248,3 nm l ph thuc tuyn tnh vo nng ca La v Ce trong phm vi t 0,5 - 18 p,g/mL.
y chnh l mt hng mi phn tch lng vt t him bng php o F-AAS vi
nhy cao.
Phn ng kh hp cht c nhm Nitro (-NO2)
Chloramphenicol, qua chun lng ln Cd(II) sinh ra trong phn ng hay o ph hp th
nguyn t ngn la (F-AAS ) ca dung dch Ion kim loi Cd(II). V d trong mi
axit long (HCl 0,05M),
trng
bt kim loi xp Cd kh nhm -NO2
NH2 hon ton nh lng theo phn ng sau.

3Cd + R-NO2 + 6HCl ^ 3CdCl2 + H2O + R-NH2
Chloramphenicol
Nh vy sau khi phn ng kt thc, ly tnm ly dung dch mui CdCl2 v xc nh Cd
bng php o F-AAS v suy ra hm lng Chloramphenicol theo phn ng trn. Vi cch ny
c th xc nh c Chloramphenicol n nhy 0,1 ppm.
Hon ton
tng
t, nhiu hp cht hu cnitro u
c thxc nh gin
tip
theo php o ph hp th nguyn t [20].

Theo hiu ng tng hay gim cng vch ph AAS
Vic xc nh theo cch ny l da trn nguyn tc l cc cht cn xc nh trong mt
gii hn nng no n c kh nng lm tng hay gim tn hiu hp th (cng ) ca
mt vch ph ca mt nguyn t mt cch tuyn tnh. S tng tc ny c th theo ba cch
sau.
Tng tc an Ion-Cation
y Anion cn phn tch khi tc dng vi Ion kim loi s lm gim cng ca vch
ph hp th ca n, mt cch tuyn tnh, hay lm tng, khi Anion ny nm trong mt khong
nng nht nh. V d dung dch nn Mg 5 p,g/mL, Anion F - lm gim cng hp th
ca vch ph Mg-285,2 nm trong ngn la n kh axetylen- khng kh rt tuyn tnh, khi
nng ca Ion F- trong dung dch mu tng t 1-20. p,g/mL. V d, theo tc dng lm gim
cng vch ph, ngi ta cho cht phn tch X (cn xc nh) tc dng vi dung dch mui
ca mt kim loi c ph hp th nhy mt nng nht nh ph hp v khng i to
thnh hp cht bn v hp cht
251
nhng
ny s
li
lm
cgim
tc
cng
lmmt
tng
vch
hay
ph
gim
ca
cng
kim
loi
mt
cath
cch
mt
vch
tuynph
hp
trong
th
mt
catrong
kim
vngloi
nng
mt
hp
th
nguyn
t
qua
kim
loi
nhy
ph
hp
nguyn
ttnh
hn.
V d
ngn
la
+ Vi
As:dng
cch
nht u
nhn,
ca khi
X.kh
Ngha
nng
ca
yn
chng
bin
tathin
c
trongAAS
mt
vch
khong
ph
nht
ph)
nh.
cnm
Do
gi tuyn
tr
nm.
ngy
axetylen-khng
Ionl
Ti(IV)
lm
tng
tn cng
hiu
ca
vch(pic
Fe-248,3
tnhnay
khi
3ASO
4
+
Na
2
BH
4
+
HCl
^
AsH
3
ngi
dng
tnh
cht
nh
cht
c

bng
php(2
o|ug/mL)
AAS.
V
nng ta
TI(IV)
thay
i
t
2Anion
-ny
50
p,g/mL.
Cc
Ion
La(III),
lm
tng
tn
hiu
AAS
ca
V
dli
mun
xc
nh
F xc
ngi
tacc
dng
Mghu
cCe(IV)
nng
2 ppm
vd
o
3glucoz
vpht
hp
amino
tcLa
dng
lm
tngphng
cng
vch
phchun
hp th
ASO
4cc+nm
Naca
2cht
BH
4
+ HCl
^hu
AsH
5
+ nh
Vi
Se:
vch ph
Fe-248,3
cng
tuyn
tnh
khic
nng
v Ce
mu
i tphp
x
Mg-285,20
nm.
c
lng
F - trong
theo
ng
dy
nguyn
t p,g/mL.
capha
Ca,theo
Zr,...
tuynny
tnh
khiang
nngc
ca
cc cht
bin
trong
vng
nhCe
hn
5 n 20
Tnh
cht
hin
nghin
cu ng
dngthin
xc
nh
Ti La,
v
3-bng
chun
c
SeO4
+ Nasau.
2 BH4 + HCl ^ SeH4
-6
1.10
M.
mt sDy
nguyn
khc
hp thFtrong ngn la n kh axetylen-khng kh nn.
chunt
xckm
nhnhy
nngph
Anion
SeO43- + Na2 BH4 + HCl ^ SeH6
Dy
chun
xcto
nh
nng
d
protein
Theo
phn
ng
ra hp
cht
bay hi
+ Viphn
Te:
Theo
hydrua
Ccng
chtsinh hp cht
Dy
chun
Cc3 cht
Dy chun
Cch nyTeO
ch4 yu
c
dngCo
^xc
nh
tCAs,
Ge,
Hg.
+ Na
TeH
2BH4 + HCl
C41 cc nguyn
C2
3 Bi, C
4 Pb, Sb,
C5 Sn, Te,Cx
Co
C
1
C
2
C
3
C
4
C
5
Cx
V n cho kt qu vi
nhy cao hn php o trc tip bnh thng hng chc n hng
TeO43 + Na2 BH4 + 2HCl ^ TeH8
Ng Ca(ppm)
2
2
2
2
2
2
trm ln
(bng
sau).(ppm)
y ngi ta cho
Nng
Mg
2 Zn kim
2 loi tc
2 dng vi
2 cht 2phn tch
2 trong2mi
Cc kh hydrua
sinh ra trong 0cc phn0,02
ng trn c kh0,06
argon dn
vo h0,10
thng nguyn
(mM)
0,08
Cx ,
trng Protein
axit HCl,
hay cht kh NaBH
4 sinh ra 0,04
cc hp cht hydrua,
v d AsH 3, SbH
3
(ppm)v o ph ca cc
0 nguyn
2 t theo
4 cc iu
6 kin8thch hp
10 cho Cx
t haNng
mu
caF my
mi
PbH2 trong
HCl mt
(%) h thng phn ng1 ng kn,
1 sau 1 nh mt1 dng kh
1 mang tr
1 (v d 1nh
nguynHCI
t. (%)
1
1
1
1
1
1 ha v
1 o
kh argon) m hp cht hydrit ny c dn vo mi
hp nh
th
nguyn t
Cctrng
cht khc
nhau
Theo
thut
ny, t
hin
nayhp
ngi
c
ring
h phng nh
php
ha hiA v nguyn t
ph hp
thk
ca
nguyn
trong
chttahydrua
.mt
Cc
A
A
A nhau
o Ax. (Ca-422,70 nm)
Ao
1
2 cht Akhc
3
4
5
Ax
ha lnh qua vic to hp cht kh hydrua d b
phn huphc
v vic tch
A
A
o AN (Mg-285,20 nh
Ao
A1
2
A3
4
A5
Ax
v xc nh cc nguyn t ni trn. Phng php ny c
nhyrt cao, c 1 - 5 ng.
V d trong mu dung dch th vch ph hp th ca Ca-422,70nm, khi c mt ca
Cc
hng
sn nng
sut myto
AES
AAS
u c bn b
trang
btuyn
cho ktnh,
thut ny
vihin
cc
-5
glucoz,
trong
vng
n.10
- v
n.10
mol/l
tng
theomu
thc
Sau
dng
ng
chun
v-4pht
hin
nngsc
ln F
trong
phn tchkhi
Cng,
(hnh
Nguyn
ca F-AAS (p.g/L)
kiu khc nhau,
t la
nt
ginkh
nlhon
chnh
vnhy
tvng.
php
ngn
n
khng
kh nn
axetylen (hnh
11.9aovtrong
11.9b).
.11.
Phn
ng Tnh
sinh ra
hpny
chtalkyl
v s
cacbonyl
10a v Theo
10b).
cht
c
dng
xc nht)
mt Hydro
s glucoz hay amino axit
Trc
tip
Qua
s tng
cng
vch
ph
(tng
tc Cation-phn
trong cc
icch
tng
sinhta hc.
Sau phn
y lng
dyca
chun
xc
Theo
nymu
ngi
da vo
Ion kim
loinh
vi glucoz
nhm Coqua
hayph
gcAAS
alkyl
Cng honAs
ton tng t nh nguyn
nhng c khc l khi c mt ca
140 tc ca cch trn,0,2
ca
Ca. ra mt hp cht cacbonyl hay mt nhm alkyl ca kim loi trong mt iu kin xc
sinh
cht phn tch XSbth cng vch 30
ph ca nguyn t kim0,1
loi li c tng tuyn theo s
nh v c tnh cht nh lng, m cc kim loi li khng c kh nng sinh ra cc hp
tng nng ca cht phn tch X c trong mu vi mt vng nht nh.
cht hydrua kim Bi
loi.
29
0,2
V d Ni trong
Se cc hp cht hu
30c c th c xc nh
0,2qua vic iu ch hp cht Nicacbonyl, ri sau nh mt kh mang tr dn hp cht ny vo mi trng hp th ca php o
Sn
110
0,5
F-AAS xc nh Ni vi nhy c 1 ng.
Cng tng t, Pb cng c xc nh qua phn ng ca Pb(II) vi LiCH 3 sinh ra
y l phn ng ca mt s Anion ca mt s nguyn t vi nguyn t hydro mi sinh
Pb(CH3)4 v sau dn hp cht ch alkyl ny vo mi trng hp th o ph ca Pb vi
to ra hp cht kh hydrua dng MeHn (vi n = 3, 4, 5 v 6). V d nh: HgH 2 , ASH3 ,
nhy cao hn nhiu ln so vi php o bnh thng nguyn t ha Pb trong ngn la n
ASH5 , SbH3 , SbH5 , SeH4 , SeHs, TeH4 , TeH6, v.v... Phn ng ny rt nh lng, trong
kh.
nhng iu kin ph hp cho mi cht. V th n cng c s dng xc nh cc nguyn
phng
php
phnkhc
tnh nhau,
gin tip
nay
l mttrong
hng
mitrong
ng dng
t Hg,Ni
As,tm
Se, li
Te..cc
trong
cc i
tng
nhhin
trong
qung,
nc,
thc
t
c
c,
c
c
c
c
0
2 3 4 5
php o bng
ph hp
thonguyn
t,x
mvrng
tcht.
ccSong
kim,
Anion
vmu
cc phn
hp cht
phm,...
php
ph pht
hp
thphn
nguyn
trc
ht l
tch hu
cn
c,
loi m
ph v
hpdng
th mui
nguyn
t Ion
ca tan
n trong
qu km
nhy.
l mt
chay
xphn
l tch
acc
cckim
nguyn
t ny
ca
dung
dchy
nc
mi
hng
mi,
ang
trin v
s dng
trong
vi11.10b
nm li y, nhng c nhiu trin vng.
Hnh
11.10a
trng
axit,
v dc
nh pht
cc mui:
HgCl2,
SbCl
SnCl
5,Hnh
4, Na 3ASO4, Na2SeO4, Na2TeO4, Sau
pictheo
ph cc phn ng sau.
thc Cc
hin
ng chun phn tch
Tng
Cation-Cation
+ Vitc
Hg:
Cchlny
c
xc
mt nguyn
kim nhiu
loi khng
nhy
y
hiuthng
ng ca
s dng
tng
ca^nh
Cation-phn
t. t
Trong
trng
hp,ph
mt s cht
HgCl2
+ Na2BH4
+tc
HCl
HgH
phn tch dng phn t, m bn thn n khng c ph hp th nguyn t,
252
254
253
255
c bit l trong vic phn tch cc cht hu c, cc sn phm dc v ha du cc nc cng

nghip pht trin, nh M, Php, CHLB c, Anh, Nht, H Lan,v.v... Theo hng ny mt cun sch
mang tn "Organic compound Analysis hy Atomic Absorpt Ion Spectrometry" c cng b bi tc
gi H. Hassan, 1988.
256
- Vch
ph
o
AAS:
Chiu
cao
Burner:
5Nol:
- ph
6 mm.
nhy
No
LOD
vch
Vch
0,1
(nm)
p,g/mL (ppm).
Ghi ch
Khe
o:
0,5
- 0,7
nm.
4.20.
Nguyn
Mc
nhyL/ph
ph(V/V).
km
Loi
Burner:
cm.
11.
Nguyn
t.
Nguyn
t.- la:
Khe
o:t.
0,5
0,710
nm.
No
Vch
ph
(nm)
Ghi ch
Kh
ngn
(N
C2H
l
5,5/4,2
2O +
2) vi t
Mc nhy ph km vch s
No
Vch
ph
(nm)
Ghi
ch
Kh
ngn
la:
(Khng
kh
+
C
H
)
vi
vi
t
l
5,2/1,3
5,211,3
L/ph
L/ph
(VN).
(V/V).
2
2
2
2
Khe
o:
0,7n
- 0,5
nm.-608,0
vchph
s 1km vch
Vng
tuyn
tnh:
0,5
p,g/mL.
Cng
HCL:
- 80%
I max Mc nhy
Chiu
cao
Burner:
585,4680.
- 6 mm.
Cng
n
HCL:
50-80%
I
max
1
137,3400.
Th
Ion
ho
I:
8,29
eV.
Nguyn
Nguyn
t
t
lng:
lng:
63,5460.
Th
Ion
ho
I:
7,72
4,18
eV
eV
nhy LOD vch Nol: 0,5 p,g/mL (ppm).
Ni-232,00
11LOD
Co-240,70
nhy
vch
Nol:
0,05
pg/mL
p,g/mL(ppm).
(ppm). 1s1 1
Cng
n (Khng
HCL:
60kh
- 0,025
80%
Nguyn
Kh
t.
ngn
la:
+ C 2IHmax
2) vi t l 5,2/1,2 L/ph (V/V).
Loi
Burner:
10
cm.
Loi
Burner:
5
cm.
Ch
ph:
F-AES
(Phtth
xnguyn
ngn la).
Ch
ph:
F-AAS
t).
Vng
tnh:
1Ni-341,50
-Nol:
15(Hp
pglml.
2tuyn
Co-242,50
1,5ln
lnkm
km
2oo
2,5
Chng
12 nhy
vch
0,05
p,g/mL (ppm).
1LOD
Ag-328,10
1
Loi
Burner:
10
cm.
Vng
tuyn
tnh:
0,1
5,0
8,0
p,g/mL.
pg/mL.
Nguyn
t
lng:
28,0860.
Th
Ion
ho
I:
8,15
eV
cao
Burner:
5 Co-241,20
-Ni-305,10
3cao
2,5
ln
kmX
Chiu
Burner:
56HP
-mm.
6 TH
mm. NGUYN T
CCChiu
IU
KIN
O
PH
V
PHT
AAS:
Vch
Vch
ph
o
oAAS:
F-AES:
3ph
4,5
ln
km
Vng
tnh: 0,1
- 68,0
p,g/mL.
Nguyn
t. tuyn
Chiu
cao
2
Burner:
5
Ag-328,30
mm.
2,5
ln
km
4No
Co-252,10
8,5
ln
km
o
F-AAS
(Hp
th
t).
NGN
LA
CA
MT
S
NGUYN
T nguyn
Noph:
Vch
Vch
ph
(nm)
Ghi
Ghich
ch
Nguyn
Nguyn
t.
t.
KhCh
ngn
la:
(Kh
N
+
C
H
l
5,5/4,5
L/ph(V/V).
4
Ni-234,60
8
ln
km
2O ph
2(nm)
2) vi t
Mc
nhy
ph
km
Mc
nhy
ph
km
vch
No
Vch
ph
(nm)
Ghi ch
Kh ngn la: (Khng kh + C 2H2) vi
t l
5,2/1,25
L/ph(VN).
Mc
nhy
ph
km
Nguyn
t
lng:
208,9806.
Th
Ion
ho
I:
7,29
eV
Kh
nhy
LODla:
vch
Nol: 0,5
p,g/mL
Nguyn
t. ngn
(Khng
kh0,025
+ C 2Hp,g/mL
vi t
l 5,2/1,3 U/ph (V/V).
2)(ppm).
nhy
LOD
vch
Nol:
(ppm).
Vch
pht
o
vch
s 1
s s
1eV
Khe
o:
0,7
--AAS:
0,5
nm.
Nguyn
lng:
65,3700.
39,1000.
Th g/mL
Ion ho
I:vch
9,39
4,34
Khe
o:
0,7
0,5
nm.
1
nhy
LOD
vch
Nol:
0,05
(ppm).
Khe
o:
0,5
0,7
nm.
Vng
tuyn
tnh:
2 -F-AAS
10
p,g/mL.
Ch
1o
ph:
(Hp
thIon
nguyn
Nguyn
t
lng:
24,3050.
Th
ho I:t).
7,64 1eV
Rb-780,00
1
Cu-324,76
Cng
n
HCL:
60
-- 80%
tuyn
o
ph:
F-AAS
F-AES
(Pht
(Hp
th
xIImax
ngn
nguyn
la).
t). 11
Vng
tuyn
tnh:
0,1
5,0
p,g/mL.
Phn I. Ch
PH
P
O
NGN
LA
Cng
No
PH
n
HCL:
Vch
ph
(nm)
80%
Ghi ch
max .
1
Ba-553,60
Vng
tnh:
0,1
--60
5,0
g/mL.
Cng
n
HCL:
60
80%
Imax
Mc
nhy
ph
km
2o o
Rb-794,80
2,5 ln
km
Vchph
AAS:
Ch
ph:
F-AAS
(Hp
th
nguyn
t).
2 o AAS:
Cu-327,40
2 ln km
Loi
Burner:
10
cm.
Vch
ph
F-AES:
2
Ba-455,40
6vch
ln km
s 1
Loi
Burner:
Khe
di
10 cm.
10
cm.
3
Rb-420,20
100 ln km
NguynLoi
t. Burner:
3
Cu-217,90
4,5 ln km
1 o
Si-251,60
Chiu
Burner:
55 -- 66 mm.
3cao
Ba-350,10
20
ln1ln
km
AAS:
Chiu
cao
Burner:
mm.
NguynVch
t. ph
No
Vch
ph
(nm)
Ghi ch
4t Burner:
Rb-421,60
260
km
Chiu
cao
5
6
mm.
Nguyn
lng:
112,4000.
Th
Ion
ho
I;
6,12
eV
Mc
nhy
ph
km
22
ln
km
No42 t lng:
VchCu-222,60
ph
(nm)
Ghi ch
Nguyn
22,9898.
Th
Ion
ho
I:
5,14
eV
Si
250,70
3
ln
km
Mc
nhy
ph
km
vch
No la: (Khng
Vch ph
(nm)
Kh
ngn
kh
C 2H
t
l
5,2/1,25
L/ph (V/V). Ghi ch
2) vi
Mc
nhy
ph1 L/ph
km
Khngn
ngn
la:
(Khng
kh+++
H
vi
t
l
5,2/1,2
vch
s
2))vi
Kh
la:
(Khng
kh
CC
t
l5,98
5,2/1,30
L/ph(V/V).
(V/V).
22H
2nguyn
Nguyn
t
lng:
26,8915.
Th
Ion
ho
I:
eV.
Ch
o
ph:
F-AAS
(Hp
th
t).
Khe
o:
0,7
0,5
nm.
nhy
LOD
vch
Nol:
0,1
p,g/mL
(ppm).
Khe
o:
0,2
0,5
nm.
s
1
Si-251,40
4vch
ln km
Chnhy
31o
ph:
F-AES
(Pht
x
ngn
la).
s
1
Khe
o:
0,5
- 0,7
nm.
LOD
vch
Nol:
0,05
p,g/mL
(ppm).
Zn-213,90
K-766,50
1

nhy
vch
Nol:
0,05
1ph
Bi-223,10
1 (ppm).
Ch
ph:
F-AAS
(Hp
th
nguyn
t).
Vng
tuyn
tnh:
0,5
- 8,0
p,g/mL.
Cng
LOD
n
HCL:
60
- 80%
Ip,g/mL
Vch
o
AAS:
max
41o
Si-252,90
12 ln1 km
Loi
Burner:
10
cm.
Mg-285,20
Vngph
tuyn
tnh:
0,1
6,0
p,g/mL.
Vng
tuyn
0,1
--8,0
p,g/mL.
Cng
HCL:
60
- 80%
Imax
2 n
Zn-307,60
K-769,90
2000
3 ln
lnkm
km
Vch
otnh:
F-AES:
2
Bi-222,80
4 ln
kmkm
Vch
ph
o
AAS:
Loi
Burner:
5
cm.
2
Mg-202,60
40
ln
Chiu
5 - 6 mm.
200 ln km
10. Nguyn
t.3cao Burner:
Loi
Burner:
10 cm.K-404,40
Nguyn
t.
Nguyn
t.o:
Khe
o:
0,5 nm.
-Bi-306,80
0,7 nm.
3 3 0,5
4,5
ln ln
kmkm
Khe
Mg-279,60
100
Chiu
cao
5K-407,70
- 6 kh
mm.+ C 2H2) vi t
4 Burner:
210
ln
kmL/ph (V/V).
Kh
ngn
la:
(Khng
l
5,2/1,2
Chiu
cao
5 - 6 mm.Th
Vch
ph (nm)
Ghi ch
Nguyn
tBurner:
lng:
51,9960.
Ion
ho
I:ln
6,76
eV
4
Bi-227,70
20
km
Nguyn
t
lng:
207,2000.
Th
Ion
ho
I:
7,42
eV
Mc
nhy
ph
km
vch
Cng
n
HCL:
50
80%
I
maxIon ho
ngn
nhy
LOD
vch
Nol:
0,05
p,g/mL
(ppm).
No
Vch
ph
(nm)
Ghi ch
60
Nguyn
t
lng:
196,9665.
Th
I: 9,22
eV.
max
Kh
la.
(N
O
+
C
H
)
vi
t
l
5,514,5
L/ph
(V/V).
2
2
2
Mc nhy ph km
Vch
(nm)
Ghi ch
Khengn
o:No
0,5
- 0,7
nm. ph
Mc
nhy
ph
km
Kh
la:
(Khng
kh
+
C
H
)
vi
t
l
5,2/1,2
L/ph
(V/V).
s
1
2
2
Khe
Ch
o:
o
o
0,2
ph:
- tnh:
0,5
F-AAS
nm.
(Hp
thnguyn
nguyn
t).
nhy
LOD
vch
Nol:
0,5p,g/mL.
p,g/mL
(ppm).
Ch
ph:
F-AAS
th
t).
Vng
0,1
- (Hp
5,0
Loi
Burner:
cm.
510vch
cm.
Ch
tuyn
o
ph:
F-AAS
(Hp
th
nguyn
t).
vch
max
nhy
LOD
Nol:
0,025
p,g/mL
(ppm).
vch s
s 11
Cng n HCL: 60-80% I
Khe Burner:
o:
-AAS:
0,5cm.
Loi
10
Vch
ph0,7
otnh:
AAS:
Vng
tuyn
2nm.
- 18 p,g/mL.
Vch
ph
o
Cd-228,80
1
Chiu
cao
5 -- 64,0
mm.
Vch
ph
AAS:
Vng
tuyn
tnh: 0,1
p,g/mL.
11 Burner:
Na-589,00
11
Nguyn
t.Burner:
Loi
10 cm.Al-309,30
Cngcao
Burner:
n HCL:
- 80% Imax
Chiu
5 -60
6 mm.
la: (N
(Khng
vi
t 2,5
lkm
5,2/1,2
L/ph (V/V).
2 Cd-326,90
Na-589,60
ln
km
NguynKh
t. ngn
2Ht
2)500
+ Ckh
)C
vi
l 5,5/4,5
L/ph
(V/V).
ln
2O
2H2+
2 tBurner:
Al-396,20
1,5
ln eV
km
No
Vch
ph
(nm)
Ghi
ch
Nguyn
lng:
121,7500.
Th
Ion
ho
I:
8,68
Chiu
cao
5
6
mm.
Nguyn
t.nhy
No
Vch
ph
(nm)
Ghich
ch
Mc
nhy
ph
km
vch
vch
Nol:
0,02
p,g/mL
Loingn
Burner:
cm.
Kh
No
la: 10
(Khng
Vch
ph
kh
(nm)
+ C 2H(ppm).
vi
t
l
5,2/1,25
L/ph
(V/V).
Ghi
2)Mc
nhy
ph
km
vch
3
Na-330,30
300
ln
km
Mc nhy ph km
nhy
LOD
vch
Nol:
0,5
p,g/mL
(ppm).
Nguyn
t
lng:
9,0122.
Th
Ion nguyn
ho
I: 9,32
eV
nhy
LOD
vch
Nol:
p,g/mL
ss1eV
Ch
3t
o
ph:
F-AAS
th
t).
Kh
ngn
la:
(K.kh
Al-308,20
C(Hp
H
l(ppm).
5,2/1,25
1,8
ln
km
(V/V).
20,05
2) vi
1L/ph
Nguyn
55,847.
Th
Iont
ho
I: 7,87
Vng
tnh:
-+2,5
p,g/mL.
Chiutuyn
cao lng:
Burner:
6p,g/mL.
mm.
vch
s
1
20,1
-520
nhy
LOD
vch
Nol:
0,02
p,g/mL
(ppm).
Khe
o:o
0,2ph:
- 0,5
0.5
nm. (Hp th nguyn t).
Ch
Khe
o:
-tnh:
F-AAS
nm.
Vng
0,1
- 8,0 p,g/mL.
1tuyn
Cr-357,90
1 1ln km
Vch
o
AAS:
40,7la:
Al-394,40
1ph
Pb-217,00
Ch
o
ph:
F-AAS
(Hp
1
Au-242,80
1
Kh
ngn
(Khng
kh
+ th
C 2Hnguyn
l3,5
5,2/1,3
L/ph (V/V).
2) vi tt).
NguynVng
t. tuyn tnh: 0,1 - 3,0
Nguyn
t.
p,g/mL.
Loi
Burner:
10
cm.
Vch
Cng
ph
o
n
AAS:
HCL:
50
80%
I
max
Nol: 0,1 p,g/mL

(ppm).
2 LOD vch
Pb-283,30
lnkm
km
2ph
cr-359,40
2 2ln
Nguyn
t. nhy
Vch
o
AAS:
2 No
Au-267,60
2,5
lneV
km
Nguyn
t
lng:
91,2200.
Th
Ion
ho
I:
7,80
87,6200.
5,69
Vch
ph
(nm)
Ghi ch
Khe
0,7 - 0,5
nm.
Nguyn
t: o:
Mc
nhy
ph km
3
Pb-261,40
40
ln
km
Loi
Burner:
10
cm.
Vng
tuyn
tnh:
0,5
8
p,g/mL.
Chiu
cao
Burner:
5
6
mm.
3 t lng:
Cr-360,30
ln eV
km
Nguyn
6,9410. Th Ion ho 3,6
I: 5,39
Ch No
3
o ph:
F-AAS
th
nguyn
t).vch
Au-312,30
900
ln km
Vch
ph
(nm)
Ghi ch
s vch
1
Cng
HCL:
60
-(Hp
80%
I max
. ho
4 tn
Pb-368,40
100
lnkm
km
Mc
nhy
ph
Nguyn
lng:
54,9380.
Th
Ion
I:
7,43
eV
No
Vch
ph
(nm)
Chiu
cao
Burner:
5
6
mm.
4
Cr-429,00
10
ln
km
Mc
nhy
ph L/ph
km (V/V). Ghi ch
Nguyn
t.ngn
Kh
la:
kh
+ Cx
t l
5,2/1,2
Ch
o
ph:(Khng
F-AES
(Pht
la).
2Hngn
2) vi
1
Sb-206,80
1
s 1
VchBurner:
ph o Khe
AAS:di- 5 cm.
Loi
Ch
ola:
ph:(Khng
F-AASkh
(Hp
vch
s 1 L/ph (V/V).
Kh ngn
+ Cth
) vi t t).
l
5,2/1,2
2H2nguyn
Nguyn
40,0800.
Th
Ion ho
I: 26,11
Vch
ph
olng:
F-AES:
2t
Sb-217,60
lneV
km
nhy
LOD
vch
Nol:
0,02
p,g/mL
(ppm).
1
Be-234,90
1
Khe o:
o:
0,5
- 0,7
0,7 nm.
nm.
1 0,5
Fe-248,30
1
Chiu
cao
Burner:
7
6
mm.
Khe
nhy
LOD
vch
Nol:
0,025
g/mL
(ppm).
Vng
tuyn
tnh:
0,05
- 2,0
p,g/mL.
Khe
0,7ph:
- 0,5
nm.
3o
Sb-231,20
8 ln
km
Ch
F-AAS
(Hp
th
nguyn
t).
No
Vch
ph
(nm)
Ghich
ch
2o:
Be-313,04
10nhy
ln
km
No
Vch
ph
(nm)
Ghi
Mc
ph
km
Mc
nhy
ph
kmvch
2
Fe-248,80
2,5
ln
km
Vng
tuyn
tnh:
0,1
2,5
g/mL.
Cng
n
HCL:
60
80%
I
Vch
ph
o
AAS:
max
Kh
ngn
la:
(N
C2-H80%
t l 5,5/4,5
L/ph
(V/V).
2O +60
2) viI max
Cng
n
HCL:
No
Vch 50
ph- 80%
(nm) Imax Mc
Ghi ch
3 ph
Be-332,14
80 ln
km
Cng
nAAS:
HCL:
nhy
ph
ss
1 1 km
Vch
o
vch
nhy
LOD
vch
No1:
0,2
p,g/mL (ppm).
No
Vch
ph
(nm)
Ghi
ch
3
Fe-271,90
3,5
ln
km
Nguyn
Khe
t.
o:
0,5
0,7
nm.
Mc nhy ph km
Loi
Burner: 10
10 cm.
cm.
NguynLoi
t. Burner:
vch
s
1
1
sr-460,70
1
Loi tuyn
Burner:
10 1cm.
Zr-360,10
Vng
- 1260
p,g/m.
41 tnh:
Fe-372,00
12 ln1s
km
Cng
n HCL:
- 80%
IIon
max ho I:vch
Nguyn
t
lng:
58,7900.
Th
7,611eV
eV1
Chiu
cao
Burner:
5
6
mm.
Khe
o:
0,7
0,5
nm.
1
Li-670,80
Nguyn
t
lng:
58,9332.
Th
Ion
ho
I:
7,86
Chiu cao
Burner:
5
6
mm.
2
Sr-407,80
25
ln
No Burner:
Vch
Ghi ch
Mn1 km
Chiu 12cao
5 - 279,50
6 ph
mm.(nm)
Zr-303,10
2 ln
km
Mc
nhy
ph km
A Burner: 10 cm.
Loi
NguynKhe
t.
g
o:
0,5
0,7
nm.
Kh
ngn
2
la:
(Khng
Li-323,30
kh
+
C
H
)
vi
t
330
l
5,2/1,3
ln
km
L/ph
(V/V).
2
2
Cng
n
HCL:
60kh
- 80%
I max
Ch ngn
2
ola:
ph:(Khng
F-AAS
(Hp
t).
Kh
+ Cth
) vi t 1,5
l 5,2/1,25
L/ph
(V/V).
2H
2nguyn
vch
sL/ph
1 (V/V).
Mn279,80
ln
km
Khnhy
ngn
3 0,5
la:
(Khng
Zr-352,00
kh0,1
+C
t l
2 ln
5,2/1,2
km
2H2) vi
LOD
vch
Nol:
p,g/mL
(ppm).
Khe
o:
nm.
nhy
LOD
vchLi-610,40
Nol:
p,g/mL
(ppm).
Chiu
cao
Burner:
560
- 6- 0,1
mm.
3
1400
lneV.
km
Cng
n
HCL:
80%
Ip,g/mL
max
Nguyn
lng:
107,8680.
Th
Ion ho
I:3 7,57
Loi
Burner:
5AAS:
cm.
nhy
1 LOD
vch
Nol:
Ca-422,70
0,05
(ppm).
1
Vch
ph
o
AAS:
3t
Mn280,10
ln km
Vch
ph
o
Vng
tuyn
tnh:
0,5
8,0
p,g/mL.
4
Zr-298,50
4
ln
km
Cng
n
HCL:
- 80%
Vng
tuyn
tnh:
0,5 60
- 8,0
p,g/mL.
Kh
ngn
la:
(Khng
+th
CImax
l 5,2/1,25 L/ph (V/V).
2H
2) vi t
Loi
Burner:
10
cm.
Ch
ph:
F-AAS
(Hp
nguyn
t).
Vng
tuyn
0,1
-6403,00
5kh
p,g/mL.
4o
Mn10150
ln ln
kmkm
Chiu
cao
Burner:
5 -Ca-239,90
mm.
Khe
o:
-tnh:
0,5
nm.
20,2
Loi Burner: 10 cm.
Ba
Cu
Rb
Si
Bi
Zn
K
Mg
Cd
Na
Al
Cr
Pb
Au
Sb
Be
Fe
Zr
Si
Li
Mn
Ca
Ni
Co
268
258
270
264
266
262
260
259
269
265
271263
267
257
261
Cd
Cu
Be
V
s
s
B
+
Cng
Giai
chnh
nhy
on
LOD
nn:
n
sy:
C
vch
HCL:
Nhit
BC
Nol:
60
:
- 0,25
120
I-Ion
250
(ppb).
,II:Thi
gian:
iu
kin
nguyn
t
ho:
Cng
n
HCL:
60
-80%
80%
I-Ion
Nguyn
t. Sb
Nguyn
t
lng:
63,5460.
Th
ho
I:9,32
eV
Kh
trCng
mi
trng:
Argon.
9,0122.
Th
Ion
ho
eV
n
HCL:
60ng/mL
80%
Nguyn
t
lng:
112,4000.
Th
ho
I:7,72
6,12
eV30 giy.
Ag-328,10
Si 251,60
Mo-
Vng tuyn
- 50 ng/mL.
ph
ph (nm)
N
No tnh: 2Vch
Mc
ph
km2 vch
McoCnhy
ph
Kh
+
iu
Khe
Giai
tr
o:
kin
on
mi
0,5
nguyn
trng:
lm
-o:
sch
nm.
t
Argon.
ho:
Cuvt:
Nhit
2700
, Thi
gian:
giy.
11.
8.
Nguyn
t.
t.
5. Nguyn
B
chnh
nn:
C
BC
Khe
o:
0,7
-0,7
0,5
nm.
Khe
0,5
nm.
Loi
Cuvt
Graphit:
Hot
ho
ton:
phn.
Phn
II.
PHP
O
KHNG
NGN
LA
22. Nguyn t.
11
max
max
Ghi
Ghi ch
11
oC
max
11
Nguyn t lng: 50,9441. Th Ion ho

I: 6,75 eV
oC oC
iu
Vng
Loi
Cuvt
kin
tuyn
nguyn
Graphit:
tnh:
tro
ho:
2tBC
-Graphit:
Nhit
Hot
20
ho:
ng/mL.
ho
:
ton
550
-phn.
700
, Thi
gian:
30 giy.
Loi
Cuvt
Graphit:
Hot
ho
phn.
+
Giai
on
sy:
Nhit
:
120
-ton
200
, Thi
gian:
30 giy.
Ch
o
ph:
F-AAS
(Hp
th
nguyn
t).
B
chnh
nn:
C
Loi
Cuvt
Hot
ho
ton
Ch
o
ph:
F-AAS
(Hp
th
nguyn
2
2
Ag-328,30
2,5
lnkm
km
Si 250,70
Mo- Th Ion hot).
2,6
Ln
ln
km
Nguyn t lng: 121,7500.
I:phn.
8,68
eV
Ch o ph: F-AAS (Hp th nguyn
t).
oC oC oC
Kh
tr
mi
trng:
Argon.
Vch
ph
o
AAS:
iu
kin
t
ho:
+Kh
Giai
tr
on
mi
sy:
trng:
NTH:
Nhit
Nhit
Argon.
:
:
120
2550
- 200
Thi
, Thi
gian:
3gian:
giy.
30km
giy.
tro
ho:
Nhit
:
450
-, 600
,gian:
Thi
20 giy.
Vch
ph
onguyn
AAS:
tr
mi
trng:
Argon.
3Kh
Si-251,40
Mo4Ln
ln
km
Vch
o
AAS:
Nguyn
t. ph
Ch
o
ph:
F-AAS
(Hp
th
nguyn
t).
Khe
o:
0,7
0,5
nm.
Vch
ph
(nm)
Ghi
Vch
ph
o
AAS:
oC
Nguyn
t.
N
o
Vch
ph
(nm)
Ghi ch
ch
oC oC
N
B
chnh
nn:
C
BC
+Giai
Giai
on
sy:
Nhit
:
120
- oC
200
, Thi
30
giy.
Mc
nhy
ph
km
vch
Vch
ph
(nm)
Ghi
ch
+
B
Giai
chnh
N
on
oonn:
lm
tro
C
ho:
sch
BC
Nhit
Cuvt:
:
Nhit
600
:
800
2700
, Thi
,gian:
Thi
gian:
gian:
30 2giy.
giy.
+
on
NTH:
Nhit
:
2300
,- Thi
gian:
3 ln
giy.
Mc
nhy
ph
km
vch
4B
Si
252,90
Mo10
Ln
km
km
chnh
nn:
C
BC
Mc
nhy
ph
km
vch
NguynNt
lng:
54,9380.
Th
Ion
ho
I:
7,43
eV
Vch
(nm)
Ghi ch
oto
Cng
n
HCL:
50
-ph
80%
Imax
s
11 km
Vch
ph
AAS:
Mc
nhyeV
ph
vch
Nguyn
lng:
26,8915.
Th
Ion
I:oC5,98
s
iu
kin
nguyn
t
ho:
+Giai
Giai
on
tro
ho:
Nhit
:
500
oC -ho
700
, oC
Thi
gian:
s
1 20 2giy.
+
iu
nhy
kin
on
LOD
nguyn
NTH:
vch
t
Nhit
Nol:
ho:
:
0,25
2600
ng/mL
,
Thi
(ppb).
gian:
3
giy.
lm
sch
Cuvt:
Nhit
:
2500
,
Thi
gian:
giy.
kin nguyn(Hp
t ho:
Cho:
11iu
o
th nguyn t).
Khe
o:
0,5ph:
- 0,7F-AAS
nm.Cu-324,76
Khe
0,5
nm.
s111 1
Be-234,90
oC
Loi
Cuvt
Graphit:
Hot:
ho
ton
phn.
Cd-228,80
NTH:
Nhit
:120
2550
, oC
Thi
gian:
3 giy.
Ch
+ Giai
1N
on
o
ph:
sy:
F-AAS
Nhit
(Hp
th
- nguyn
200
, Thi
t).
30 giy.
oC
oC gian:
Vch
ph
(nm)
Ghi ch
o
+
Vng
Giai
tuyn
on
lm
tnh:
sy:
sch
Nhit
2,5Nol:
-Cuvt:
25
:
ng/mL.
120
Nhit
- 200
:(ppb).
,2700
Thi
gian:
,, Thi
30
giy.
giy.
nhy
LOD
vch
0,25
ng/mL
nhy
ph
km230
vch
1 gian:
on
sy:
Nhit
:
120
-Mc
200 oC
Thi
gian:
giy.
221+ Giai
V-318,50
Cu-327,40
2
ln
km
Vch
o
AAS:
Cngph
n
HCL:
60
80%
I
Cng
n
HCL:
60
80%
I
Be-313,04 max
8 ln
max
2
oC oC
Cd-326,90
500
lnkm
km
B
chnh
nn:tro
Cho:
BC
lm
sch
Cuvt:
, Thi
gian:
2 giy.
+ Giai
on
Nhit
:Nhit
400 -:
6002700
20 giy.
oC , Thi gian:
skm
1 20 giy.
2 LOD
oC
ph
o
AAS:
+Vch
Giai
nhy
on
tro
vch
ho:
Nol:
Nhit
0,25
:
ng/mL
550
800
(ppb).
,
Thi
gian:
Vng
tuyn
tnh:
2,5
25
ng/mL.
V-306,60
3
ln
33N
+oGiai onVch
tro
Cu-217,90
ho:
Nhit
: 450 - 700
4,5
ln
, Thi
km
gian: 20 giy.
ph
(nm)
Ghi ch
Nguyn
t.
Be-332,14
100
ln
km
Loi
Cuvt
Graphit:
Hot
ho
ton oC
phn.
Loi
Cuvt
Graphit:
Hot
ho
ton
phn.
Mcgian:
nhy3ph
1 LOD
1 km vch
Sb-206,80
Giai
nhy
vch
Nol:ph
0,5(nm)
ng/mL
+
on
NTH:
Nhit
:
2300
,(ppb).
Thi
giy.
Kh
tr
mi
trng:
Argon.
Vch
Ghi ch
N
o
oC
Khe
o:
-tnh:
0,5 nm.
V-437,90
53ln
kmkm
oC
Mc
nhy
ph
vch
Vng
+ Giai
tuyn
on
NTH:
2,5
Nhit
- 25222,60
:
ng/mL.
2550:, 2300
Thi
gian:
giy.
43+0,7
Cu
21
Giai
on
NTH:
Nhit
, Thi
gian:
s
1 3 giy.
Nguyn
t.
Nguyn
t
lng:
47,90.
Th
Ion
ho
I:
6,82
eV
2
oC
Kh
trtuyn
mi
trng:
Argon.
Kh
tr
mi
Argon.
Sb-217,60
ln km
Vng
tnh:
2,5
-Cuvt:
25 ng/mL.
+
Giai
on
lm
sch
Nhit : 2500 ,2 Thi
gian:
2 giy.
Khe
o:
-trng:
0,5
B
chnh
nn:
Cnm.
BC
1
410,7
V-385,60
lns
1km
Cng
n
HCL:
50
- 279,50
80%Nhit
Imax : 2700 oC, 7Thi
MnoC
+ Giai
on
lm
sch
Cuvt:
gian:
2
Khe
o:
0,5
0,7
nm.
+
Giai
on
lm
schTh
Cuvt:
Nhit
, Thi giy.
gian: 2 giy.
Nguyn
t.chnh
Ch
o
ph:
F-AAS
(Hp
th
nguyn
Nguyn
lng:
137,3400.
Ion(ppb).
ho t).
I: :
8,292500
3t
Sb-231,20
3 eV
ln 1km
1nn:
B
chnh
nn:
C
BC
B
C
BC
Al-309,30
t.
nhy
LOD
vch
Nol:
0,5
ngi
Nguyn
Cng
n
HCL:
60
80%
I
max
iu
kin
nguyn
t
ho:
2
Mn279,80
1,5
ln
km
Loi
Cuvt
Graphit:
Hot
hong/mL
ton
Kh tr mi trng: Argon.
nhy
LOD
vch
Nol:
0,5
(ppb).
Cng
n
HCL:
50vch
- 80%
Imax phn.
Khe
o:
0,5
- AAS:
0,7
nm.
nhy
LOD
Nol:
ng/mL
(ppb).
2 o
Nguyn
t
lng:
207,2000.
Th
IonoC
ho t).
I: 7,42
eVln km
Vch
ph
Ch
o
ph:
F-AAS
(Hp
th 0,1
nguyn
Al-396,20
1,5
iu
kin
nguyn
t
ho:
iu
kin
nguyn
t
ho:
Vng
tuyn
tnh:
4
40
ngi.
Khe
o:
0,5
0,7
nm.
Loi
Cuvt
Hot
ho
ton
phn.
tGraphit:
lng:
51,9960.
Th
Ion
ho
I: 6,76
+Nguyn
Giai
on
sy:
Nhit
:280,10
120
- 200
, Thi
gian:
30km
giy.
3
Mn3 eV
ln
B
chnh
nn:
C
BC
Loi
Graphit:
Hot
ho-ton
phn.
VngCuvt
tuyn
tnh:
2 -tnh:
25
ng/mL.
Cng
n
HCL:
60
80%
I
Vng
tuyn
0,5
10
maxng/mL.
3
Al-308,20
1,8
ln
km
Vch
ph
(nm)
Ghi ch
oC
oC
N
o
Ch
ph
oAAS:
ph:
(Hp
th--250
nguyn
t). gian:
Vch
+Ch
Giai
on
gy:F-AAS
Nhit
:
120
Thi
gian:
30km
giy.
+
Giai
on
sy:
Nhit
120
,,Thi
30
giy.
oC t).
Mc
nhy
ph
km
vch
Nguyn
t.
4on
Mn403,00
10 gian:
tn
ph:
F-AAS
th
nguyn
Kh
tr
mi
trng:
Argon.
60:
-(Hp
80%
Imax250
+Cng
Giai
on
troHCL:
ho:
Nhit
:
500
- 800
, Thi
20
giy.
Kh
mi
trng:
iutr
kin
nguyn
tArgon.
ho:
Al-394,40
3,5 s
ln1 km
Loi
Cuvt
Hot
ho(nm)
ton phn. oCoC
Vch
ph
Ghi ch
N4ooGraphit:
Nguyn
t.
Vch
ph
AAS:
+
Giai
on
tro
ho:
Nhit
:
600
900
, ,Thi
gian:
30
+
Giai
on
tro
ho:
Nhit
:
600
Thi
gian:
30giy.
giy.
oC-- 1000
Mc
nhy
ph
km
vch s
Vch
ph
o
AAS:
B
chnh
nn:
C BC
Nguyn
t NTH:
lng:
40,0800.
Th
Ion
ho
I:
6,11
eV
+
Giai
on
Nhit
:
2550
,
Thi
gian:
3
giy.
oC
Loi
Cuvt
Graphit:
Hot
ho
ton
phn
B
chnh
nn:
C
BC
Khe
o:
0,5
0,7
nm.
+ Giai on sy: Nhit : 120 - 200 , Thi gian: 30 giy.
Kh
tr N
mi
trng:24,3050.
Argon.
1t
oC ho I: 7,64 eV 11
oC
Vch
ph
(nm)
Ghi ch
o0,7
Nguyn
lng:
Th
Ion
Ti-3:
64,30
+Ch
Giai
on
NTH:
Nhit
;
2700
Thi
gian:
giy.
+
Giai
o:
on
NTH:
- 0,5sch
nm.
Nhit
,, Thi
gian:
33 giy.
oC
o
ph:
F-AAS
(Hp
th
nguyn
t).
Mc
nhy
ph
km2 vch
iu
kin
nguyn
t
ho:
+Khe
Giaikin
on
lm
Vch
Cuvt:
ph2700
Nhit
(nm)
:
2700
, Thi
gian:
giy.
Ghi ch
N
o
iu
nguyn
t
ho:
nhy
ph
km
vch
n
HCL:
50 - 80%
Imax - 600 oCMc
+Cng
Giai
on
tro
ho:
Nhit
:
400
,
Thi
gian:
20
giy.
Kh
tr
mi
trng:
Argon.
12 nn: C BC Ba-553,60
11
B
chnh
oC
oC
s
Ch
o
ph:
F-AAS
(Hp
th
nguyn
t).
oC 2800
ln
km
+Cng
Vch
Giai on
ph
on
o
lm
AAS:
schTi-365,40
Cuvt:
Nhit
:
2800 gian:
Thi
gian:
giy.
n
lm
HCL:
sch
Cuvt:
60
80%
Nhit
Imax
:
,,1,6
Thi
22 giy.
+
Giai
sy:
Nhit
:-0,25
120
250
Thi
30
giy.
oC(ppb).
sgian:
1
nhy
LOD
vch
Nol:
ng/mL
+
Giai
on
sy:
Nhit
:
120
-- 200
,, Thi
gian:
30
giy.
oC
Cuvt
Graphit:
Hot
ho
ton
phn.
1
1
+Loi
Giai
on
NTH:
Nhit
:
2200
,
Thi
gian:
3
giy.
Pb-217,00
B chnh
2 1nn:
C t
BCho:
iu
kin
nguyn
Ba-455,40
5ln
lnkm
1km
oC
Vch
ph
o
AAS:
Cr-357,90
nhy
LOD
vch
Nol:
ng/mL
(ppb).
3N
Ti-320,00
Loi
nhy
Cuvt
LOD
Graphit:
vch
Nol:
Hot
10,5
ho
ng/mL
ton
(ppb).
ph
(nm)
Ghi ch
oC , Thi2 gian:
+
Giai
on
tro
ho:
Nhit
:
550
800
20km
giy.vch
otro
+
Vng
Giai
tuyn
on
tnh:
ho:
1 -Vch
Nhit
20
ng/mL.
:
450
-- phn.
600
, Thi
gian:
20
giy.
Mc
ph
oC nhy
2
Pb-283,30
2 ln 2
km
tron
mi lm
trng:
+Kh
Giai
schArgon.
Cuvt:
Nhit :
2400
,
Thi
gian:
giy.
oC
+iu
Giaikin
on
:
120
- 250
, Thi gian:
30
giy.
2 sy: Nhit
Vch
ph
(nm)
Ghi ch
3mi
Ba-350,10
22 ln
km
N
Cr-359,40
n
t
ho:
oC
Vng
tuyn
tnh:
60
ng/mL.
Kh
tuyn
tnh:
trng:
55Nhit
-- 100
Argon.
ng/mL.
skm
1km vch
+Vng
Giaitr
on
NTH:
Nhit
:
2600oC
Thi
gian:
giy.
Mc
nhy
ph
4 onguyn
Ti-399,00
53321ln
+
Giai
on
NTH:
:
2400
,, Thi
gian:
giy.
3
Pb-261,40
40
ln
km
B nhy
chnhLOD
nn: C BC
Nol:
0,05 ng/mL (ppb).
Nguyn
oC
11 20
31 trovch
Cr-360,30
3,6
ln
km
+ t.
Giai on
ho: Nhit
: 550 - 700
, Thi
gian:
giy.
Ca-422,70
s
oC
oC
oC
chnh
nn:
C
BC
2700
giy
+B
Giai
on
sy:
Nhit
:
120
180
,
Thi
gian:
30gian:
giy.
+
Giai
on
lm
sch
Cuvt:
Nhit
:
2500
, Thi100
giy.
40,7 - 0,5 nm. Pb-368,40
ln 2km
Khe
o:
Nguyn
t.
Nguyn
t.
iu
kin
t -ho:
Vng
tuyn
tnh:
0,5
15 ng/mL.
Nguyn
t
lng:
196,9665.
Th
Ion
eV
oC ho I: 9,22
2 nguyn
Khe
o:
0,5
0,7nm.
4
Cr-429,00
6
ln
km
Ca-239,90
150
ln
km
1
1
+ Giai on
NTH: Nhit
: 2700 , Thi gian: 3 giy.
Mg-285,20
nhy
LOD
Nol:
0,5:
ngi
(ppb).
iu
kin
nguyn
t
ho:0,2
oC
ng/mL
+
Giai
on
trovch
ho:
Nhit
400
-(ppb).
600
,5,69
ThieV
gian: 30 giy.
Cng
n
HCL:
60
80%
I
Nguyn
t
lng:
58,7900.
Th
Ion
ho
oC I:
I:
7,61
eV
Nguyn
t
lng:
87,6200.
Th
max
Ion
ho
+
Giai
on
Nhit
:
120
200 , Thi
30 giy + Giai on tro
Khe
o:
0,5
-gy:
nm.
o
ph:
F-AAS
(Hp
th
t).oCgian:
Cng
n
HCL:
60
- 80%
I-maxnguyn
0,5
0,7
Khe
o:
-0,7
0,5
nm.
2 0,7
+Ch
Giai
on
lm
sch
Cuvt:
Nhit
:oC2800
, 40
Thi
gian: 2 giy.
NguynVng
t.
Mg-202,60
ln
tuyn
- 20
ng/mL.
ngi.
+ Giai
ontnh:
sy:12Nhit
: 120 - 250
,
Thi
gian:
30km
giy.
oC
Loi
Cuvt
Graphit:
Hot
ho
ton
phn.
oC
Ch
on
ph:
F-AAS
(Hp
th
nguyn
t).
Ch
o
ph:
F-AAS
(Hp
th
nguyn
t).
+
Giai
on
NTH:
Nhit
:
2400
, Thi
gian: 3 giy.
ho:
Nhit
:
500
- 700
,ho
Thi
gian:
20
giy.
Cng
HCL:
60
80%
I
Vch
ph
AAS:
Loi
Cuvt
Graphit:
Hot
ton
phn.
max
max
Cng
n
HCL:
60
80%
I
max ho
nhy3t
LOD
vch
Nol: 0,5Th
ng/mL
(ppb).
Nguyn
lng:
58,9332.
Ion
I: 7,86100
eVln km
+t.
Giai on tro ho:Mg-279,60
Nhit : 600 - 800oC, Thi
gian: 25 giy.
NguynKh
tr
mi
trng:
Argon.
oC
Vch
ph
o
AAS:
Vch
ph
o
AAS:
oC
NguynLoi
t.
+
Giai
on
NTH:
Nhit
:
2450
, phn.
Thi
gian:, Thi
3 giy.
Loi
Cuvt
Graphit:
Hot
ho
tonphn.
lm
sch
Cuvt:
Nhit
:
2600
gian: 2 giy.
Cuvt
Graphit:
Hot
ho
ton
Kh
tr
mi
trng:
Argon.
Vngtuyn
tnh:F-AAS
5Vch
- 80 (Hp
ng/mL.
ph (nm)
Ghi ch
Noph:
Ch
o
th
nguyn
t).
oC
Mc
nhy
ph
km vch
+
Giai
on
NTH:
Nhit
:
2650
,
Thi
gian:
3
giy.
Nguyn
t
lng:
55,847.
Th Ion ho I: 7,87oCeV
B
chnh
nn:
C
BC
Khe
o:
0,5
0,7
nm.
Nguyn
t
lng:
208,9806.
Th
Ion
ho
I:
7,29
eV
Kh
tr
mi
trng:
Argon.
+
lm
sch
Cuvt:
Nhit
2600 , Thi gian: 2 giy.
Vch
ph
ph
Ghi
Ghi ch
Kh
tron
mi
trng:
Argon.
N
N
onn:
B
chnh
C
BC
Giai
nhy
LOD
vch
Nol:
0,5 (nm)
ng/mL:
(ppb).
Mc
Mc nhy
ph
ph
s
1 km vch
o
AAS:
NguynVch
+t.
Giai
on
lm
sch Cuvt:
Nhit
: 2800
Ch
ph
o
ph:
F-AAS
(Hp th
nguyn
t). oC, Thi gian: 2 giy
iu
kin
nguyn
tBC
ho:
Cng
n
HCL:
50(Hp
- 0,2
80%
Imax
1 LOD
Ch
o
ph:
F-AAS
th
nguyn
Bchnh
chnh
nn:C
CBC
nhy
vch
Au-242,80
ngi
(ppb).t).
B
nn:
s
s1 11
iu
kin
nguyn
tNol:
ho:
Vng
tuyn
tnh:
2,5
40
ng/mL.
Vch
ph
o
AAS:
Vch
ph
(nm)
Ghi ch
N11ot
nhy
LOD
vch
Nol:
0,5
ng/mL
(ppb).
-
Nguyn
lng:
65,3700.
Th
Ion
ho
I:
9,39
eV
oC Mc nhy ph
11 giy.
km vch
2
Sr-460,70
Ni-232,00
+
GiaiCuvt
on
sy;
Nhit
:
120ton
- 250phn.
, Thi gian:
30
Loi
Graphit:
Hot
ho
2,5 ln
kin
nguyn
ho:
Vch
ph
o
AAS:
Vng
tuyn
tnh:
1t-tAu-267,60
20
ngi.
iu
nguyn
ho:
+iu
Giaikin
on
sy:
Nhit
:
120 - 250oC, Thi gian:
30 km
giy.
s
1km
2o ph:
Vch
ph
(nm)
Ghi
Vng
tnh:
2,5Au-312,30
- (Hp
25
ng/mL.
Ch
tuyn
o
F-AAS
th -nguyn
t).
N
oC oC
Sr-407,80
Ni-341,50
2,5
50
ln
ln
km
oC
Vch
ph
(nm)
Ghi ch
ch
N
32mi
o trng:
600
ln
km
nhy
ph
km
vch
+t.
Giai
on
sy:
Nhit
;:
120
,oC
Thi
gian:
30
giy.
+
Giai
tro
ho:
Nhit
600250
- 900
, Thi
gian:
30
giy.
Nguyn
Kh
tron
Argon.
:
,Thi
Thi
gian:
30
giy.
oC Mc
Mc
nhy
ph
km
vch
+
Giai
on
sy:
Nhit
:
120
200
,
gian:
30
giy.
tro
ho:
Nhit
:
600
900
,
Thi
gian:
20
giy.
1
1
Co 240,70
Nguyn t.
3on
Ni-305,10
4,5 s
ln
1 km
oC
Vch
ph
oNTH:
AAS:
oC - 800 oC
1 20
+Giai
Giai
tro
Nhit
500
Thi
gian:
20giy.
giy.
600
,,Thi
gian:
+
on
Nhit
::
2600
3 s
giy.
Nguyn
t.
B
chnh
nn:
Cho:
BC
oC gian:
oC, Thi
Khe
o:on
0,5
nm.
20,7
+Nguyn
Giai
tro
ho:
Nhit
:
450
550
,
Thi
gian:
20
giy.
Khe
o:
0,5
nm.
t
lng:
NTH:
28,0860.
Nhit
:
Th
2650
Ion
,
ho
Thi
l:
gian:
8,15
eV
3
giy.
Co-242,50
1
5
ln
km
1
1
Fe-248,30
Nguyn14t lng: 95,94.
Th Ion ho
I: 7,80 eV8 ln1 km
Ni-234,60
Bi-223,10
oC
oC
oC
2600Ion
+Giai
Giai
on
NTH:
Nhit
:(nm)
2550
, Thi
3eV
giy.
Vch
ph
Ghi ch
N
otn
+
on
lm
sch
Cuvt:
Nhit
:
2700
, Thi
gian:
giy.
iu
kin
nguyn
t
ho:
Nguyn
lng:
107,8680.
Th
ho
I:gian:
7,57
oC
oC
Cng
HCL:
60
80%
I
3
Co
252,10
6,5
1nkm
Mc
nhy
ph
km22vch
max
22 n
+ Giai on
NTH:
Nhit
:
1900
,
Thi
gian:
3 ln
giy.
Cng
HCL:
50
80%
I
lm
sch
Cuvt:
Nhit
2800
, 4Thi
gian:
giy.
max :
Fe-248,80
2,3
km
ph: F-AAS
Bi-222,80
ln
km
Ch o ph:
(Hp th nguyn t). oC
oC
oC 2700 , Thi
+Giai
Giai
on
sch
Cuvt:
Nhit
:
Khe
o:
0,5
- lm
0,7
nm.
s301 gian:
nhy
LOD
vch
Nol:
0,5
ng/mL
(ppb).
+
on
gy:
Nhit
:
120
- 250
, Thi
giy. 2 giy.
Ch
on
o
ph:
F-AAS
(Hp
th
nguyn
t).
oCgian:
Loi
Cuvt
Graphit:
Hot
ho
ton
phn.
3
Fe-271,90
3Thi
ln
km
+
Giai
lm
sch
Cuvt:
Nhit
:
2200
,
gian:
2 giy.
phn
nhy
LOD
vch
Nol:
0,5
ng/mL
(ppb).
3
Bi-306,80
4,5
ln
km
Khe
0,5 nm.
Vcho:
ph
o- AAS:
10,7
1
ph
Zn-213,90
nhy
LOD
vch
Nol:
0,5
ng/mL
(ppb).
nhy
LOD
vch
Cng
n
HCL:
60ng/mL.
-0,5
80%
Imax - (ppb).
Vng
tuyn
tnh.4
- Nol:
40
+
Giai
on
tro
ho:
Nhit
:ng/mL
600
900oC, Thi
20 giy. + Giai on
Vch
ph
o
AAS:
44
Fe-372,00
10 gian:
ln
Bi-227,70
35
ln km
km
Kh
trtuyn
mi
trng:
Vng
tnh:
52-Argon.
80
Vng
tuyn
-60
20-ng/mL.
ng/mL.
Cng
HCL:
80%
I
max
2 ntnh:
2000 ln km
Vng tuyn tnh: 2 Zn-307,60
- oC30 ng/mL.
Loi Cuvt
Graphit:
Hot ho ton phn.
NTH:
Nhit
B
chnh
nn::
C2600
BC , Thi gian: 3 giy.
Mn
Al
Ti
Ba
Pb
Cr
Ca
Mg
Au
Ni
Si
Co
Fe
Bi
Zn
Si
Mo
Ao
272
274
280
284
286
282
276 288
278
279
277
275
273
283
285
281
287
TI LIU THAM KHO
RiChard D. Beaty & Jack D. Kerber, 1979 & 1983, Concepts on Instrumentation and Techniques
in Atomic Emission Spectrophotometry, Perkin Elmer Company.
Hobart H. Willard, Lynne L. Merritt, John A. Dean & Frank A. Settle, 1993, Instrumental
Methods for Analysis, Wadsworth Pub. Company, 6th Edition.
E.L. Grove, 1978, Applied Atomic Spectroscopy, Plenum Press, New York.
M. Pinta, 1979, Atomic Absorption and Emission Spectrometry, Vol. I & II, London, Hilger.
Peter J. Whitesside, 1979 & 1985, Atomic Spectrometry Data Book, Pye Unicam, Ltd.
R.E. Stuegeon & C.L. Charrabarti, 1979 & 1985, Recent Advances in Atomic Emission
Spectrometry, Perkin Elmer.
Douglas A. Skoog & James J. Leary, 1995. Principles of Instrumental Analysis, Saunder8 College
Pub., 4th Edit Ion, New York, London.
Perkin Elmer Company, 1985-90, Some Application Notes In AAS, Perkin Elmer Ltd.
S.S. M. Hassan, 1984, Organic Analysis Using Atomic Spectrometry, Amsterdam, Hilger, London.
J.B. Dowson, 1989, Annual Reports on Analytical Atomic Spectroscopy, Vol. 7 & 8, Amsterdam,
London.
Daniel C. Harris, 1998, Quantitative Chemical Analysis, Fifth Edit Ion, W.H. Freeman &
Company, New York.
Douglas A. Skoog, Donald M. West & F. James Holler, 1995. Fundamentals of Instrumental
Analysis, 7th Edit Ion, New York, London, Amsterdam, Tokyo.
James D. Ingle, Jr. & Stanley R. Grouch, 1992, Spectro-chemical Analysis, Prentice Hall, Upper
Saddle River, New Jersey.
Geoge R. Harrison, 1979, Wavelength Tables, The M.I.T. Press, Cambridge, London.
R.M. Barnes, 1987, Application Inductively Coupled Plasma Emission Spectroscopy, Easten
Analytical Symposium.
John H. Kennedy, 1990, Analytical Chemistry Principles, Saunders College Pub., 2nd Edit Ion,
New York, London.
289
Nguyn Phng Tho, 2005, Lun n thc s, Trng H KHTN - HQG H Ni.
Jose A.C. Broekaet, 2002, Atomic Analytical Spectrophotometry, Wiley CH. Ltd., New York London - Amsterdam - Tokyo.
Shimadzu Company, 2002, AAS Cook Book, Shimadzu Company.
Phm Th Qunh Lng, 2002, Lun n thc s, Trng H KHTN - HQG H Ni.
290
MC LC
PHN 1..........................................................................................................................................................3
Chng 1: I CNG V PHNG PHP AES...................................................................................3
S phn loi ph.............................................................................................................................................3
S phn chia theo c trng ca ph....................................................................................................3
Phn chia theo di sng....................................................................................................................4
S xut hin ph pht x nguyn t..........................................................................................................5
Tm tt v cu to nguyn t................................................................................................................5
S xut hin ph pht x.......................................................................................................................7
Nguyn tc ca php o ph pht x (AES)............................................................................................. 9
i tng ca phng php phn tch ph pht x................................................................................14
Cc u im v nhc im....................................................................................................................14
Kh nng v phm vi ng dng...............................................................................................................15
Chng 2: S KCH THCH PH PHT X NGUYN T..................................................................17
Yu cu v nhim v ca ngun kch thch............................................................................................17
Cc loi ngun kch thch ph pht x....................................................................................................18
Ngn la n kh.................................................................................................................................18
H quang in.....................................................................................................................................23
Tia la in..........................................................................................................................................28
Plasma cao tn cm ng ICP...............................................................................................................34
Nguyn tc v cch chn ngun kch thch ph......................................................................................40
Cng vch ph pht x nguyn t....................................................................................................41
Cng vch ph :...........................................................................................................................41
Cng vch ph v nhit plasma..............................................................................................44
Hin tng t hp th (t o)................................................................................................................45
Bc x nn trong ph pht x..................................................................................................................46
Chng 3: MY QUANG PH V S PHN LI CHM SNG...........................................................47
Nguyn tc cu to ca my quang ph pht x.....................................................................................47
Cc loi my quang ph pht x............................................................................................................. 50
Lng knh v my quang ph lng knh..............................................................................................50
Cch t v my quang ph cch t.....................................................................................................61
Vng lm vic ca my quang ph.........................................................................................................67
Trang b ca h thng my quang ph pht x........................................................................................68
Trang b pht hin v thu nhn ph..........................................................................................................68
Knh nh quang ph.............................................................................................................................68
o en S x ca vch ph trn knh nh.........................................................................................70
ng nhn quang in (Photomultiplier tubes)....................................................................................71
Chng 4: Cc yu t nh hng trong AES..............................................................................................75
Khi qut chung.......................................................................................................................................75
291
4.2 Mt s nh hng trong php o AES...............................................................................................75

Cc yu t v ph.................................................................................................................................75
Cc yu t vt l...................................................................................................................................77
Cc yu t ha hc...............................................................................................................................79
Chng 5: PHN TCH QUANG PH PHT X NH TNH...............................................................88
Nguyn tc chung......................................................................................................................................88
Vch chng minh nh tnh v cch chn................................................................................................89
nhy ph v kh nng pht hin.........................................................................................................90
nhy tuyt i (cn gi l nhy khi lng) ............................................................................90
nhy tng i (cn gi l nhy nng )................................................................................90
S trng vch v cch loi tr..................................................................................................................93
Vch ph trng.....................................................................................................................................93
Vch quy ri v chen ln...................................................................................................................93
Ph m................................................................................................................................................93
Cc phng php phn tch nh tnh......................................................................................................94
Phng php quan st trc tip trn mn nh.....................................................................................95
Phng php so snh ph....................................................................................................................95
Phng php ph chun (Dng bn atlas)...........................................................................................96
Chng 6 : PHN TCH PH PHT X NH LNG..........................................................................99
Nhng vn chung................................................................................................................................99
Phng trnh c bn v nguyn tc.....................................................................................................99
Vch phn tch v cch chn.............................................................................................................101
Cch biu din nng trong phn tch quang ph..........................................................................102
Mu chun trong phn tch quang ph pht x.................................................................................104
Gii hn chng minh v khong xc nh.........................................................................................106
S bay hi v ng cong bay hi....................................................................................................108
6.1.7. Kh quyn kim tra..................................................................................................................110
Cht m v cht ph gia trong phn tch ph pht x.....................................................................113
Phn tch quang ph pht x bn nh lng.........................................................................................119
Phng php so snh......................................................................................................................... 119
Phng php hin vch......................................................................................................................120
Phn tch quang ph pht x dinh lng................................................................................................121
Phng php ng chun................................................................................................................121
Phng php th chun khng i................................................................................................124
Phng php thm tiu chun...........................................................................................................125
Phng php theo 1 mu chun.........................................................................................................127
Cc phng php xc nh gin tip bng AES.................................................................................... 128
Nguyn tc.........................................................................................................................................128
Cc phng php phn tch gin tip................................................................................................128
Phn II.........................................................................................................................................................135
292
Chng 7: NHNG VN CHUNG CA PHP O ASS................................................................135

S xut hin ph hp th nguyn t.....................................................................................................135
Cng ca vch ph hp th nguyn t..........................................................................................137
Cu trc ca vch ph hp th nguyn t.............................................................................................140
Nguyn tc v trang b ca php o AAS.............................................................................................143
Nhng u v nhc im ca php do AAS........................................................................................145
i tng v phm vi ng dng ca AAS............................................................................................147
Chng 8 : Cc k thut nguyn t ha mu....................................................Error! Bookmark not dened.
Mc ch v nhim v...........................................................................................................................149
K thut nguyn t ha mu bng ngn la..........................................................................................149
Yu cu v nhim v ca ngn la..................................................................................................149
c im v cu to ca ngn la n kh.......................................................................................151
Trang b nguyn t ha mu........................................................................................................152
Nhng qu trnh xy ra trong ngn la............................................................................................156
Ti u ha cc iu kin nguyn t ha mu...................................................................................163
K thut nguyn t ha khng ngn la...............................................................................................165
c im v nguyn tc....................................................................................................................165
Cc yu cu h thng nguyn t ha mu........................................................................................166
Nguyn tc v cc giai on ca qu trnh nguyn t ha mu .......................................................166
Cc yu t nh hng.......................................................................................................................174
Cc qu trnh trong cuvet graphit .....................................................................................................177
Trang b nguyn t ha mu........................................................................................................182
Ti u ha cc diu kin cho php o khng ngn la mu...........................................................183
Chng 9: TRANG B CA PHP O ASS............................................................................................185
Ngun pht bc x n sc...................................................................................................................185
n catot rng (HCL).......................................................................................................................186
n phng in khng din cc (EDL)...........................................................................................189
n ph lin tc c bin iu...........................................................................................................192
Cc loi ngun n sc khc............................................................................................................194
Trang b nguyn t ha mu............................................................................................................ 194
H thng n sc v my quang ph hp th nguyn t......................................................................195
Trang b pht hin, Detector, Photomultivlier......................................................................................197
K thut o cng vch ph hp th................................................................................................198
Chng 10: Cc yu t nh hng trong AAS..........................................................................................201
Khi qut chung....................................................................................................................................201
Mt s nh hng trong php do AAS.................................................................................................201
Cc yu t v ph.............................................................................................................................201
Cc yu t ha hc............................................................................................................................207
Chng 11: Phn tch nh lng bng ph AAS.....................................................................................219
Nhng vn chung.............................................................................................................................219
293
Phng trnh c bn ca php o......................................................................................................219

Mu chun trong php o AAS.........................................................................................................221
Biu din nng trong php o AAS.............................................................................................222
Khi nim v nhy.......................................................................................................................225
Gii hn pht hin trong AAS...........................................................................................................229
Khong xc nh trong php o AAS...............................................................................................231
B chnh nn trong php o AAS.....................................................................................................232
Ti u ha cc iu kin cho php o AAS.....................................................................................237
Cc phng php phn tch c th........................................................................................................240
Phng php th chun (ng chun)........................................................................................240
Phng php thm tiu chun...........................................................................................................242
Phng php th chun c nh....................................................................................................243
Phng php mt mu chun............................................................................................................245
Cc kiu phng php phn tch theo AAS..........................................................................................246
Cc phng php xc nh trc tip.................................................................................................246
Cc phng php xc nh gin tip cc cht bng AAS .................................................................247
Chng 12: CC IU KIN O PH HP TH NGUYN T V PHT X
NGN LA CA MT S NGUYN T..............................................................................................257
Phn I. PHP O PH NGN LA........................................................................................................257
Phn II. PHP O KHNG NGN LA................................................................................................272
TI LIU THAM KHO..........................................................................................................................289
294

16 Hng Chui - Hai B Trng - H Ni in thoi: (04) 9718312; (04) 7547936;
Fax: (04) 9714899 Email: nxb@vnu.edu.vn
***
Chu trch nhim xut bn:
Gim c: PHNG QUC BO Tng bin
tp: PHM THNH HNG Chu trch nhim ni dung:
Hi ng nghim thu gio trnh Trng
HKHTN - i hc Quc gia H Ni Ngi nhn xt:
GS. TSKH TRNH XUN GIN TS. NGUN
HONG
Bin tp:
H TH IP - QUC THNG Bin tp ti
bn:
INH QUC THNG
V hnh:
INH QUC THNG
Trnh by ba:
NGUYN NGC ANH
PHNG PHP PHN TCH PH NGUYN T

M s 1K-25 H2006
In 1000 cun, kh 19 x 27cm ti Xng in Tng cc Cng nghip Quc phng S
xut bn: 105 - 2006/CXB/62 - 08/HQGHN, ngy 10/02/2006.
Quyt nh xut bn s: 173 KH/XB In xong v np lu chiu qu 11 nm 2006.
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PHM LUN

PHNG PHAP PHAN TICH

NH XUT BN I HC QUC GIA H NI

Php o ph pht x v hp th nguyn t l nhng k thut phn tch ha l, v ang

licn sdng k thut phn tch

1.1 S phn loi ph

im hini cac lng

chnh ca nguyn8t (n). Trong

Qu trnh pht x v hp th ca mt nguyn t.

ph ca phn t MeO, CO v nhm phn t CN. Cc m ph ny xut hin thng c mt

B. Trang b hon chnh:

(theo ba cch khc nhau)

Quan st trc tip

Knh nh cha ph mu p.t.

Thu, phn li, ghi trc tip ph mu p.t.

1.4 i tng ca phng php phn tch ph pht x

Yu cu v nhim v ca ngun kch thch

kim tra thnh phm.

(mc 1) n cn phi m bo trn u hn

t bng hn hp kh axtylen v oxy hay

chng b kch thch v pht x ^ c ph pht x (AES).

th c mt tia in c nh qua khong E, nh th lp tc trn mch dao ng L 1c1 xut

H quang l ngun kch thch c s mch tng i n gin, nhng li c nhiu

Trong A v B l cc hng s, Ri l in tr plasma h quang. Cng thc ny gii

S nguyn tc cu to ca my pht h quang

Khi h quang lm vic, in cc F s c t nng v di tc dng ca in

quang thng lun lun xy ra

thng l cc qu trnh nhit

plasma cng c mt nhit

S kch thch ph trong plasma h quang in

+ S nung nng v nng chy,

Chm tia pht x

C ch 2 ny cho nhy v n nh cao ca s pht x. Cc hp cht mui halogen

Chm tia pht x

C ch 2 ny cho nhy v n nh km so vi c ch 1 ca s pht x. Cc

Do c im ca 2 c ch chnh , nn trong phn tch ngi ta thng to diu kin

V vy, mun m bo cho qu

S kch thch ph trong plasma ca tia la in

dch cn li), bt mu b nung

in cc l cc yu t quyt nh din bin ca cc qu trnh trn.

in mnh (v th phng in rt cao gia 2 in cc, 15- 20 kV), nn cc nguyn t b bt ra

Nguyn t b kch thch:

Nguyn t b Ion ha:

Ion b kch thch:

Me(k)* ^ Me(k) + n(hv)

Me(k)+* ^ Me(k) + n(hv)

Trong my ny c mt tia in chnh v mt tia in ch huy. Theo s hnh

n khi ta ngt cng tc K.

(nhit cao) th th Vf phi rt ln.

cun cm Li5 L2 ngn khng cho

Khi cho in vo my, bin th Tr tng in, t C c tch in dn, m t M quay u

Chnh do nhng c im v u vit ca ngun nng lng ICP nh th, nn n

Me(k) + E ^ Me(k)* ^ MeO + n(hv)

Chm tia pht x

C ch 1 ny cho nhy v n nh cao ca s pht x. Cc hp cht mui halogen

Chm tia pht x

C ch 2 ny cho nhy v n nh km so vi c ch 1 ca s pht x. Cc hp

Ion habc hai ca nguyn t

kim loi kim v cc nguyn t c

Hnh 2.13 S qu trnh nguyn t ha

A trng thi ban u, nng

lng Eo v trng thi kch thch nng lng cm;

lng kch thch nguyn