Chng I:

LY MU V QUN L MU PHN TCH

1.1. Ti sao phi ly mu v x l mu phn tch
1.2. Ly mu phn tch
1.2.1. Mc ch v yu cu ca vic ly mu phn tch
1.2.2. Trang b v dng c ly mu
1.3. X l mu s b khi ly mu
1.3.1. Ti sao phi x l mu s b
1.3.2. Cc loi mu cn x l s b
1.3.3. Cc phng php hay cch x l s b mu
1.4. Cc cch ly mu phn tch
1.4.1. Cc kiu ly mu
1.4.2. Cch thc v tn sut ly mu
1.5. Ghi chp v lp h s khi ly mu phn tch
1.5.1. Ti sao phi ghi chp, lp h s mu
1.5.2. Cch ghi chp lp h s mu phn tch
1.6. Chuyn ch, vn chuyn mu v kho hay PTN
1.6.1. Cc yu cu v chuyn ch
1.6.2. Phng tin chuyn ch
1.7. Qun l v bo qun mu phn tch
1.7.1. Yu cu ca bo qun mu
1.7.2. Cc phng php v iu kin bo qun mu
1.8. Khi nim v QA/QC trong ly mu phn tch
1.8.1. Khi nim v QA
1.8.2. Khi nim v QC
1.8.3. Nhng vn v mi quan h QA/QC trong ly mu

LY MU V QUN L MU PHN TCH

1.1. Ti sao phi ly mu v qun l mu phn tch
Cc phng php v k thut phn tch ngy cng c pht trin v hon thin phc v cho
phn tch nh tnh (pht hin), phn tch nh lng v c phn tch xc nh thnh phn cu trc
ca cc cht. Nhng cn c theo mc v kh nng ng dng, ngi ta chia thnh hai nhm:
Nhm 1: cc phng php phn tch ha hc, n bao gm
- Cc phng php phn tch khi lng
- Cc phng php chun th tch
Nhm ny l cc phng php hay k thut phn tch xc nh hm lng ln (a lng)
ca cc cht, thng thng ln hn 0.05%.
Nhm 2: cc phng php phn tch cng c (my mc), nhm ny li c chia thnh
4 nhm da vo cc c trng ca n, c th l:
- Phng php phn tch quang hc.
- Phng php phn tch in ha hc
- Phng php phn tch sc k v
- Cc phng php phn tch khc
Nhm ny l cc phng php hay k thut phn tch xc nh hm lng nh (vi lng)
ca cc cht, thng thng nh hn 0.1%
Trong tt c cc phng php phong ph nh th, d l phn tch ha hc n gin hay phn
tch cng c, xc nh hm lng ca cc cht th gn nh khng c phng php no c
th o c, xc nh trc tip cc cht cn phn tch khi n ang tn ti trn thc a. V th
cn phi tch mt lng mu nht nh ca i tng cn quan st em v cc nh cc
cht cn quan tm trong i tng . Song sau khi c mu, chng ta cng khng th xc
nh cc cht ngay trong mu va c ly nguyn trng th nh th c m khng qua x
l a cht cn phn tch v dng thch hp, bi v:
a. Vi bt k mt phng php xc nh no, hay mt k thut phn tch no th mi cht
phn tch ch c th xc nh c n khi n tn ti mt trng thi nht nh ph hp
vi k thut . V d mun xc nh cc kim loi trong mu t, chng ta khng th b
mu t ngay vo my quang ph hp thu nguyn t o chng c m phi a cc
kim loi tn ti trong t v trng thi cc hp cht tan c trong dung dch nc, di
dng cc cation, th sau mi xc nh c chng trong dung dch nc.
b. Mu phn tch c nhiu loi v a dng, t loi c thnh phn n gin n nhng loi
c thnh phn phc tp. Chng c th tn ti cc trng thi khc nhau nh rn, lng,
khi v c huyn ph. Chng ta khng th b nguyn mu nh th vo my v xc nh
n c. Nn phi x l a cc cht cn phn tch v trng thi ph hp nht cho
mt phng php c chn xc nh n.
c. Cc cht cn xc nh li tn ti trong cc trng thi lin kt ha hc khc nhau, trong
cc hp cht v c, hu c khc nhau, c khi rt bn vng. Nn khng th xc nh ng
n hm lng ca n trong mt t hp phc tp bn vng v b cc nguyn t, cc cht
khc, mng li lin kt tn ti ca mu cn tr. Do cn phi x l mu ph v
cc hp cht m cht phn tch ang tn ti a n sang mt dng khc c nh
lng tt theo phng php chn.
Chnh v thc t nn mun xem xt hay phn tch mt i tng no ca thc t, chng
ta phi ly mu phn tch v mi mu phn tch phi c x l c c mu cho phn
tch xc nh cc cht chng ta mong mun. Vic ly mu v x l mu theo cch no l ty
thuc vo:
- i tng cn nghin cu phn tch
- Bn cht v s tn ti ca cht cn xc nh v hm lng ca n
- Loi mu, bn cht ca cc cht phn tch
- Trng thi tn ti v cu trc ca cht trong mu

- Phng php phn tch c chn xc nh chng

Ngy nay theo s pht trin ca khoa hc v ngnh ha hc, cc k thut, cc phng php
v cc loi trang b dng c... x l mu phn tch cng c pht trin v hon thin,
tin li v bo m c tt cc yu cu ca phn tch. Cc k thut l:
- K thut v c ha kh, x l kh
- K thut v c ha t, x l t
- K thut v c ha kh-t kt hp
- K thut x l t trong l vi sng
- K thut chit lng-lng, chit rn-lng v chit rn-kh
- K thut thng hoa cht phn tch
- K thut chlor ha cht phn tch
- K thut chng ct cc kiu
- K thut kt tinh hay ha lng nhit thp
- K thut in phn tch cht
Trong gio trnh ny chng ta s trnh by nhng nt c bn v bn cht nhng qu trnh vt
l v ha hc cng nh nhng u, nhc im v phm vi ng dng ca cc k thut ny,
nht l nhng k thut ang c s dng ph bin trong phn tch lng vt cc cht.
1.2. Ly mu phn tch
1.2.1. Mc ch v yu cu ca vic ly mu phn tch
1.2.1.1. Mc ch v yu cu ly mu phn tch
Mc ch ca vic ly mu phn tch l chn mt th tch (hay khi lng) nh ph hp v
ch va ca i tng cn nghin cu phn tch lm phn tch ngay ti hin trng
hay ng gi vn chuyn v phng th nghim x l v xc nh (nh tnh hay nh
lng) cc cht chng ta mong mun ca i tng nghin cu nhng li phi bo m gi
nguyn ng thnh phn ca i tng thc t ly mu. Do ly mu l giai on u ca
cng vic phn tch. Nu ly mu sai th kt qu phn tch khng phn nh ng thc t. V
th c kt qu phn tch phn nh ng thc t, vic ly mu phn tch phi m bo
c cc yu cu sau y:
- i din ng cho i tng cn nghin cu v phn tch
- p ng ng yu cu phn tch hay nghin cu xem xt
- Ly mu, khng lm mt mu hay nhim bn mu
- Ph hp vi phng php la chn phn tch
- C khi lng phn tch, khng qu nh v ng yu cu
- Mu phi c l lch, cc iu kin ly mu r rng
- m bo ng yu t ca QA/QC
1.2.1.2. Cc iu kin cn ca cng vic ly mu
Chng ta bit rng, mc tiu ca ly mu l chn mt phn th tch (hay khi lng) mu nh
ca i tng nghin cu (hay phn tch) vn chuyn c v phng th nghim phn tch
c cc ch tiu cn thit m vn m bo th hin ng c thnh phn thc t ca i tng
nghin cu. Do vic ly mu phi tun th theo nhng iu kin nht nh
- Theo mt quy trnh tiu chun nht nh cho mi loi v c chp nhn
- Theo tng i tng mu phn tch nht nh
- Theo nguyn t hay cht cn phn tch
- Dng c ly mu ng quy cch v phi m bo QA/QC
- Ngi ly mu phi c hun luyn v c tay ngh thc hin
- C s sch ghi chp v c h s mu r rng
Ch khi tha mn cc iu kin v yu cu trn th kt qu phn tch mi ni ln c thnh phn
(hm lng) ca cht trong mu phn tch. Cn nu khng tha mn cc iu kin th d phng
php phn tch c chnh xc i na th cng khng ni ln c ng nng (hm lng) ca
cht. Hay ni mt cch khc, chng ta phi thc hinQA/QC trong cng tc ly mu.
1.2.2. Trang b v dng c ly mu
1.2.2.1. Yu cu chung v dng c ly mu

Cc dng c phc v cho ly mu, cha mu v bo qun mu phn tch cn phi bo m cc iu

kin sau:
- sch yu cu ca di tng phn tch theo mc phn tch yu cu
- Khng gy nhim bn hay mt mu, cht phn tch
- Khng lm sai lch thnh phn cc cht trong mu phn tch
- Ph hp vi mi loi mu cn ly v trng thi, su, lng mu...
- C th ong, o c lng mu cn ly theo yu cu t ra
- Dng c phi c x l v kim tra trc khi dng bng mt cch ph hp cho nguyn
t hay i tng ca cc cht cn phn tch
1.2.2.2. Cc dng c ly v cha ng mu
1.2.2.2.1. Cc yu cu chung
Cc dng c ly v cha ng mu phi:
- Khng lm nhim bn v nh hng n mu khi ly v bo qun
- Ph hp cho mi i tng mu v ly c mu ng thc t
- Khng c tng tc vi cc cht mu khi ly, chuyn ch v bo qun
1.2.2.2.2. Cc trang b v dng c ly mu
Dng c ly mu bao gm cc loi theo cc loi mu sau, cho mi loi mu:
- Loi mu rn v mu bt
- Loi mu lng (nh cc mu nc, mu du)
- Loi mu c tnh c hi
- Loi mu c cht phn tch d b phn hy
- Loi ly mu kh, khng kh v bi
- Loi ly mu cho cc i tng sinh hc, nm
- Loi mu y nc su, trm tch, bn... (di bin, sng, h...)
- Dng c ly cc loi mu ph du, l lng
V th dng c ly mu rt a dng v phong ph, t n gin n my mc t ng, iu
khin t xa... ty theo yu cu ca cng vic ly mu. Ngy nay cc loi dng c ly mu c
nhiu hng sn xut v cung cp theo cc mc khc nhau cho mi loi. Cc quy trnh phn tch
v ly mu u c ch r cc iu kin v dng c ly mu cho cc loi cht phn tch.
1.2.2.2.3. Dng c ng, cha v gi mu phn tch:
Dng c ng, cha v gi mu phn tch rt a dng v ty thuc vo mi loi mu. Song chng ta
c th tm tt theo my loi chnh nh sau
- Loi mu rn v bt
+ giy hay vi gi mu (n phi tr v sch)
+ ti nilon hay bao nilon, hp
+ l, chai rng ming c nt bng thy tinh, thch anh hay PE
- Loi mu lng
+ can, thng (thy tinh hay nha) c nt kn
+ chai, l, bnh (thy tinh hay nha) c nt kn
+ ti nilon c nt
+ cc ng c nt kn
- Loi mu c tnh c hi v ha hc
+ can, thng (thy tinh hay nha) c nt v gn kn
+ chai, l, bnh (thy tinh hay nha) c nt v gn kn
+ ti nilon c nt
- Loi mu d phn hy
+ Chai l, bnh (thy tinh hay nha) chng nh sng cho mu lng
+ Giy hay ti en chng nh sng cho mu rn v bt
- Loi mu sinh hc: ty theo mi cht c th l
+ Cc l thy tinh hay thch anh
+ Cc l hay can polymer
+ Giy polimer

1.3. X l s b khi ly mu
1.3.1. Ti sao phi x l s b
Nhiu loi mu khi tch ra khi mi trng thc t, cc cht trong mu c th b thay i, b mt
hay b phn hy v th cn phi x l mu s b nhm mc ch l:
- Gi v bo ton c cht phn tch khng b mt do cch hin tng
+ S tng tc ha hc, t phn hy ca cht
+ s thy phn ca cc cht
+ S sa lng ca cht
+ S hp ph vo dng c cha mu
- Phc v cho di chuyn d dng v khng h hng mu
- Bo qun khng lm thay i thnh phn mu v cht phn tch
- Phc v cho bo qun c d dng v an ton sau khi ly
1.3.2. Cc loi mu cn x l s b: nhng loi mu ca cc cht sau y cn x l s b:
- Mu phn tch cc kim loi nng d thy phn
- Mu phn tch cc anion km bn
- Mu phn tch cc cht d b phn hy
- Cht phn tch l cc cht d b hp ph vo thnh bnh cha
- Mu phn tch mt s ch tiu sinh hc, nm mc
- Mu xc nh cc ng vt ph du
- Mu xc nh cc loi trm tch
1.3.3. Cc phng php x l s b
1.3.3.1. Phn tch kim loi v anion
- X l dng c: trng cc dng c trc tin bng mt dung dch ph hp nht, nc ct
hay acid long, dng cht no ty thuc vo cht phn tch, sau phi lm kh ht
dung mi trng
- X l mu khi ly: v d
+ X l bng acid HCl hay HNO3 (kim loi nng, cho 1 L mu)
+ X l mu bng kim NaOH long (kim loi kim, anion CN-, H2S,)
+ Mu xc nh pH (cc loi)
+ X l bng formol, alcohol (cc loi mu xc nh ch tiu sinh hc)
+ X l bng kh tr, sch
1.3.3.2. Phn tch cc cht hu c
Nhm cc cht thuc loi sau:
- Cc cht d b anh sang tc dng v phn hy
- Cc cht phi gi lnh (v d ly mu phn tch vitamin A trong mu)
- Cc cht d b oxyhoa hay kh
- Cc cht d b mt do chuyn ha sang cht khc, do t oxyhoa kh
- Cc cht d bay hi, thng hoa
- Cc cht d ng t, sa lng, bm vo thnh bnh cha ng,
y l nhng mu phi x l mu s b khi ly bo v chng bng mt cch ph hp cho
mi cht. V d: bo ha kh CO2 hay N2 cho cc cht d b oxy trong khng kh ph hy.
1.3.3.3. Cc i tng sinh hc
Vic ly mu ca cc i tng sinh hc yu cu gi rt nghim ngt cc iu kin. Nu
khng cc vi sinh vt, nm mc s b cht, hay bin dng khng cn ng vi thc t. Mt s loi
phi c nh chng bng mt dung mi hu c thch hp. V d cc loi mu sau y:
- Vi sinh vt, vi khun, nm mc
- Cc ch tiu sinh ha, COD, BOD, DO,...
- Cc mu y hc (phn tch kim loi v cc cht hu c c hi)
- Sinh vt l lng
- Cc cht l lng

Khi ly mu cc loi ny ngi ta phi c nh hay gi chng bng cc cht thch hp c

cho thm vo mu phn tch theo mt lng thch hp nh cht n nh, cht chng oxyhoa, cht
chng ln men, cht chng sa lng,...
1.4. Cc cch ly mu phn tch
Vic ly mu theo kiu no l ty thuc vo mc ch nghin cu, i tng, cht cn phn
tch... l xc nh hm lng i din, c trng hay kim tra tc thi hay phn tch ly kt
qu lm thng k nh gi hm lng, v biu , xem xt s bin thin, thay i,... ca cht
nghin cu. Ngha l vi mi mc ch nghin cu hay phn tch cc cht khc nhau, s phi c cc
cch ly mu thch hp cho n. Sau y ch nu ra mt s kiu in hnh v ang c p dng.
Tt nhin vic ly mu th no, theo cch no l ty thuc vo mc ch ly mu lm g, phn
tch cht g,... m chn phng php, cc dng c ly mu ph hp thu c mu tt. Hin nay,
mi i tng phn tch, hu nh cc nc trn th gii u c cc quy nh tiu chun cho cng
vic ly mu. Chng ta c th p dng TCVN hay cc tiu chun ISO-9000 thc hin ly mu.
V th ngi i ly mu phi c nhng hiu bit c bn v cng vic ly mu. l vn QA/QC
ca ly mu phn tch.
1.4.1. Cc kiu ly mu
Vic ly mu phn tch c th thc hin theo cc kiu sau y, ty theo yu cu, mc ch
phn tch t ra m thc hin ly mu cho ph hp:
- Ly mu n cho i tng nghin cu
- Ly mu lp, ly mu song song
- Ly my tch phn
- Ly mu c thm cht chun
Mt vn d na rt quan trng trong ly mu phn tch l phi m bo cc yu t ca QA/QC
trc lc (chun b), trong lc ly mu v sau khi ly xong mu cng nh vn chuyn v bo
qun chng. l c mt qu trnh m m ngi u phi thc hin ng cc quy trnh ly mu, c
nh th mi c c mu phn tch cho ra kt qu phn nh ng thc t ca i tng cn
nghin cu, phn tch.
1.4.2. Cch thc v tn sut ly mu
A. Ly mu theo thi gian
A1. Ly mu lin tc theo chung trnh thi gian nghin cu
Mc ch: theo di kim tra qu trnh bin thin ca cht phn tch nh th no.
Cch ly:
- chng trnh thi gian (lin tc theo chu k v d nh sau mi 5 pht, mi gi, mi
ngy, mi thng....)
- Chng trnh thi gian theo vng, tng ; khng gian tng khc nhau
A2 Ly nh (k theo chu k nht nh, thy triu, gi ma...)
Mc ch: nh k pht hin cc cht mong mun
Cch ly: nh k thi gian (tun, thng, qu, theo triu ln xung, theo tun trng...)
A3 Ly theo xc sut bt k khi no cn kim tra
Mc ch: thnh thong cn pht hin cc cht mong mun th ly mu
Cch ly: ly theo nhu cu mong mun kim tra t xut ti nhng v tr hay vng mong
mun kim tra th ly mu
B. Ly mu theo tng v lp
B1. Ly mu i din trung bnh
Mc ch: xc nh hm lng trung bnh i din
Cch ly: theo cch ly nhiu ch, sau trn li ly trung bnh
B2. Ly cch im khc nhau theo b mt nh gi theo v tr
Mc ch: xc nh hm lng ti mi ch nh gi s khc nhau
Cch ly: theo cch ly mu cho mi ch ring
B3. Ly theo cc tng, lp c su khc nhau (mu t, nc...)
Mc ch: xc nh hm lng ti mi tng su khc nhau
Cch ly: theo cch ly mi tng su khc nhau ring

C. Ly mu theo vng, mt ct hay theo im cn quan st

Mc ch: xc nh hm lng cht phn tch to mi vng kho st
Cch ly: theo cch ly mi vng ring bit nh
D. Ly mu theo dng chy, hng gi
Mc ch: xc nh hm lng cht phn tch theo hng gi khc nhau
Cch ly: theo cch ly mi hng gi thun hay ngc ring bit
1.5. Ghi chp lp h s mu khi ly
Khi ly mu, mi mu phi c ghi chp lp h s y . H s ly mu phi cc vn sau:
- a im ly mu
- V tr ly mu (ch ly, b mt, su, cch ng, b rung..., khi ly mu nc bin
phi ghi r kinh , v , su, ta ...)
- Ngy, gi, thng, nm ly mu
- iu kin thi tit (ma, nng, gi, nhit ...)
- Loi mu g, dng tn ti, trnh trng mu khi ly.
- Khi lng mu ly
- Ghi r cch x l s b (nu c)
- Ngi ly mu v ngi xc nhn (ghi r h tn)
H s ny phi c mt t i km theo mu v c bn giao cho ngi nhn mu di chuyn hay
bo qun v cho c ngi phn tch sau ny. Trn c s h s v tnh trng c th v y ,
ngi lm phn tch s d dng tm c mt cch x l mu thch hp nht cho phn tch t kt
qu tt.
1.6. Chuyn ch mu t ni ly v kho v phng th nghim
1.6.1. Cc yu cu ca chuyn ch
m bo khng lm nh hng n kt qu phn tch, vic chuyn ch mu cng phi
m bo cc iu kin:
- Bng cc phng tin ph hp, kp thi nhng khng tn km.
- Khng lm h hng mu, bong trc nhn, h hng bao gi, bnh cha
- Khng gy xo trn, va p, nht l mu d chy n
- ng iu kin gi mu, khng cho mu phn hy khi di chuyn
- Phng tin chuyn ch phi m bo sch, khng lm nhim bn mu
1.6.2. Cc phng tin chuyn ch
Ty iu kin thc t xa hay gn, khn cp hay thong th m chn cch chuyn ch thch
hp nht li khng tn km v phc tp, song phi m bo c cc yu cu chuyn ch, c th l
- Phng tin th cng n gin: xa p, xe my, xch l...
- Phng tin c gii chuyn dng c tin nghi khng ch cc iu kin nh mong
mun, bo v mu... v chuyn ch nhanh
Song mt iu cn lun qun trit l d bng cch ny th cng phi thc hin ng cc iu
kin ca QA/QC trong vn chuyn mu.
1.7. Qun l v bo qun mu phn tch
1.7.1. Cc yu cu ca qun l mu
Vic qun l, bo qun mu l mt khu k tip ca cng vic ly mu phn tch. Ly mu
tt nhng bo qun khng tt th s lm hng mu phn tch, v th trong cng tc bo qun mu
phi m bo c cc yu t sau:
- Theo ng yu cu m bo s tn ti ng cht phn tch
- ring tng loi, tng l, tng nhm....
- Trong mi trng thch hp (nh sng, m,nhit ...)
- Bo v c cht phn tch khng b phn hy hay sa lng,..
- Trong nhit thch hp theo yu cu ca cht phn tch
- Khng cho cc phn ng ha hc xy ra lm mt cht phn tch
Do mi mt cht phn tch v mi loi mu cn c chn theo nhng iu kin thch hp nht
bo qun chng trc khi phn tch.
1.7.2. Cc phng php bo qun mu

Ty loi mu v cht phn tch m mu c th c bo qun:

- Trong iu kin bnh thng, trong phng c khng kh sch
- Trong t lnh c khng ch nhit theo yu cu
- Trong kho kn, kh ro, khng bi v khng c c hi cho mu
- Trong t m c khng ch nhit theo yu cu
- Nhit thp di 0 (trong tuyt CO2) hay h khng ch nhit
- Trong mi trng kh tr (Ar, He hay N2)
Bng 1.2 l vi v d v cc loi dng c lm t cc vt liu khc nhau dng cha mu v bo
qun mu
Cht phn tch

Vt liu lm bnh cha

Thi gian bo qun ti

a
30 ngy
15 ngy

G, PTFE
G, PTFE
G, PTFE
G, PTFE
G, PTFE
G
G

Cht bo v/iu kin

bo qun
Khng
0.06g ascorbic acid/L
4 oC
4 oC
4 oC
Bnh thng
HNO3, pH<2
HNO3, pH<2
4 oC
HNO3, pH<2
0.008% Na2S2O3, pH
4-5, 4 oC
0.008% Na2S2O3, 4 oC
0.008% Na2S2O3, 4 oC
0.008% Na2S2O3, 4 oC
0.008% Na2S2O3, 4 oC
0.008% Na2S2O3, 4 oC
0.008% Na2S2O3, 4 oC
5 mL HCl, 4 oC

Cl-, SO42CN-

P, G
P, G

Nitrite
SO32H+ (pH)
Kim loi (II, III)
Hg
Cr(VI)
Kim loi kim
H acronitril

P, G
P, G
P, G
P, G
P, G
P, G
P, G
G, PTFE

H benzidines
H clor hu c
H dioxim
Halo ether
Nitro-aromatic
Du, m
Thuc tr su hu c
v phosphor hu c
H PCBs v phthalates
ethers
Chlor hu c
Radiological test

G, PTFE

4 oC

40 ngy

G, PTFE
G, PTFE

H2SO4, pH < 2, 4 oC
HNO3, pH < 2, normal

28 ngy
6 thng

48 gi
28 ngy
24 gi
3 thng
20 ngy
24 gi
36 thng
14 ngy
7 ngy
7 ngy
45 ngy
40 ngy
40 ngy
28 ngy
28 ngy

1.8. Khi nim v QA & QC trong ly mu phn tch

Ly mu l khu u tin v rt quan trng ca qu trnh phn tch. Nu vic ly mu khng
m bo c trung thc, ng cn v i din cho i tng cn phn tch th mi cng vic
phn tch sau d c cn thn v chnh xc n u i na, s liu phn tch thu c cng khng
th i din cho i tng nghin cu c. V vy m bo cho cng vic ly mu phn tch
c tt, nht thit phi thc hin cng tc QA(quality assurance-m bo cht lng)/QC(quality
control-kim sot cht lng). Vy QA/QC l g?
1.8.1. Khi nim v QA
Mc tiu chung ca QA l cung cp hay m bo cc iu kin cn thit c c kt qu
t cht lng mong mun. Ni mt cch tm tt th QA l mt h thng tch hp cc hot ng
qun l v nhng iu kin, quy tc v bin php l thut cn thit m bo cho mt sn phm

thu c trn bt k lnh vc no ca sn xut hay nghin cu khoa hc c c cht lng p

ng (hay tha mn) ng c mc tiu t ra. Do trong cng tc ly mu phn tch th QA l
h thng ca cng tc t chc qun l, cc quy tc, bin php, cc iu kin c nghin cu,
la chn v bin son thnh mt quy trnh phc v cho cng tc ly mu phn tch theo mi loi
i tng, nhm mc ch ly c mu phn tch i din ng i tng cn phn tch. V vy
vic thc hin QA trong ly mu phn tch l iu rt cn thit v ch c m bo c QA trong
ly mu th chng ta mi c iu kin y khng nh cc s liu phn tch thu c theo mu
ly c c s khoa hc v phn nh ng thc t cn nghin cu. V th QA trong ly mu phn
tch bao gm mt lot cc vn sau y m bo cho mi hot ng ly mu t kt qu tt v
n l mt k hoch bo m cht lng cho cng vic ly mu. K hoch bao gm:
- Cn b i ly mu phi c hun luyn y theo yu cu ly mu
- C phng php ly mu ng n v c ph chun
- Dng c trang b v phng tin ly cha mu c kim chun
- Ha cht, thuc th phc v ly mu c chun b v kim chun
- Xc nh ng a im, vng v v tr cn ly mu
- Xc nh r cc thong s cn kho st
- C cc iu kin cha ng, chuyn ch v bo qun mu
- Phng tin ghi chp lp h s khi ly mu c chun b
- C cc ti liu cn thit ti thiu phc v cho ly mu
1.8.2. Khi nim v QC
Mc tiu chung ca QC l cung cp cc iu kin v bin php gim st v kim sot
cht lng mt qu trnh sn xut hay nghin cu khoa hc no m bo cht lng ng thi
pht hin nhng sai st v tm cch khc phc nhng sai st m bo thu c sn phm c
cht lng mong mun t ra. Ni mt cch tng qut th QC l mt tp hp cc phng php, iu
kin k thut v cc hot ng k thut kim sot cht lng ca mt sn phm c to ra trong
mt qu trnh no .V th cng vi QA, trong cng tc ly mu phn tch cng phi thc hin c
QC. Trong cng tc ly mu phn tch th QC l mt t hp cc bin php v iu kin k thut c
th kim sot mi cht lng hot ng ca cng tc ly mu phn tch, ng thi pht hin cc
sai st v tm cc bin php khc phc m bo tt qu trnh ly mu. N l cc quy tc, bin php
v cc iu kin thc hin kim sot qu trnh ly mu t lc chun b i ly mu n cng vic
ly mu, vn chuyn v bo qun mu, cng nhm mc ch lm cho vic ly mu phn tch m
bo c tnh chnh xc, ng n v mu ly c phn nh v i din ng cho i tng cn
nghin cu, phn tch, ng thi cng trnh c cc sai st trong ly mu nh v trang b, dng c
ha cht, s nhim bn khi ly mu v cc tc ng khc. V th phi ly:
- Mu trng dng c cc loi
- Mu trng chuyn ch
- Mu trng thuc th khi c x l s b
- Mu thm chun kim tra
1.8.3. Nhng vn v mi quan h QA/QC trong ly mu
Nh vy t nhng khi nim trn QA/QC trong ly mu phn tch chnh l nhng cng c
ca qun l v kim sot cht lng c trin khai v p dng trong lnh vc ly mu phn tch.
N l ton b cc hot ng trong ly mu c thc hin mt cch c k hoch v c h thng.
Thc hin cc hot ng ny s m bo cho s tin tng ca mu ly c phc v phn tch.
QC l cc hot ng k thut c tnh cht tc nghip (nghip v) c th va theo di qu trnh
ly mu va nh gi cht lng ca mt sn phm do qu trnh ly mu to ra, va ng thi pht
hin v loi b hay khc phc nhng sai st ca tt c cc khu trong mt qu trnh ly mu phn
tch. Cc hot ng QA/QC trong ly mu phn tch gn b cht ch vi nhau v b sung cho nhau,
cng din ra trong khun kh ca h thng thng nht m bo cht lng ca mu ly c.
Ly mu l mt hot ng hin trng. N l hot ng khi u ca ton b dy chuyn
hay cng tc phn tch mu c c s liu (thng tin) v cc i tng cn quan st v xem xt.
V th mi sai st trong ly mu u nh hng n ton b kt qu thu c. V th phi quan tm
ng mc n vic bo m cht lng cho cng tc ly mu phn tch c c nhng la chn

trang b, phng php, cc quyt nh v cch ly mu, thi gian, a im, tn sut thch hp, cng
tc kim tra cc hot ng ly mu. chnh l ni dung ca QA/QC trong ly mu. V vn
ny cn c mt s quyt nh c th thc hin theo cc ni dung sau y:
- Chun b nhn s ph hp
- Lp k hoch theo mc ch kho st v ly mu
- La chn a im, vng, v tr ly mu cho i tng cn ly
- Xc nh c kiu v cch ly mu cho i tng cn ly
- Xc nh tn xut v thi gian ly mu
- La chn phng php ly mu
- Chn v chun b cc dng c thch hp cho ly mu
- Chn cch x l s b khi ly mu (nu cn)
- La chn dng c cha, ng hay gi v bo qun mu
- Xc dnh v chn cc cch vn chuyn mu thch hp
- Cng vic lp bo co, bn giao mu v h s lu tr
l nhng vn chung, cnc c phng php v quy trnh ly mu c th c trong cc
tiu chun ca quc gia v quc t. Mi ngi khi thc hin ly mu u phi nm vng cc quy
trnh o, cc vn ny c th tham kho mc ph lc cui chng ny.
ng thi theo cc khi nim nu trn, cng tc ly mu phn tch phi bao gm cc vn
sau y, bt u t lc chun b i ly mu cho n khi thu c mu em v v bo qun chng.
- QA/QC i vi tt c ngi thc hin ly mu
- QA7QC trong k hoch ly mu
- QA/QC i vi cc phng php, trang b v dng c ly mu
- QA/QC i vi ha cht phc v ly mu
- QA/QC i vi cc loi dng c ng, cha v bao gi mu
- QA/QC i vi cc hot ng ly mu, ghi chp h s ly mu
- QA/QC i vi cng tc chuyn ch mu v phng th nghim
- QA/QC i vi cng tc bo qun v lu gi mu sau khi ly c
Lm tt tt c cc vn ny tc l chng ta ly c mu phn tch tha mn c tt c cc
yu cu ca ly mu. Ngha l trong mi hot ng ca cng tc ly mu phn tch t lc bt u
chun b n lc ly c mu mang v v bo qun chng, hay phn tch ngay ti hin trng khi
cn thit. Ton b mi quan h ca cc cng vic ny c th m phng theo s hnh sau:
Bng XX: cc phng php tiu chun ly mu phn tch
STT
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K
hiu
tiu
chun
TCVN 5994-1995
TCVN 5996-1995
TCVN 5998-1995
TCVN 5999-1995
TCVN 6000-1995
ISO 5667-13-1993

Ly mu cho ch tiu no
Hng dn ly mu nc h ao
Hng dn ly mu nc sng sui
Hng dn ly mu nc thi
Hng dn ly mu nc bin
Hng dn ly mu nc ngm
Ly mu nc thi v bn

Ghi ch

Hnh 1.1. S chung v QA/QC trong ly mu v phn tch

Xc nh mc tiu ly mu
Lp chng trnh ly mu
Chun b: nhn lc, phng
tin, trang thit b, dng c,
ti liu... phc v ly mu
QA/QC

Thc hin ly mu theo

cc ch tiu yu cu phn tch
Bo qun v vn chuyn
v kho hay PTN
X l mu v phn tch
S liu phn tch
X l s liu
Bo co kt qu phn tch
Nhn xt v nh gi

Chng II. CC K THUT X L MU PHN TCH

2.1. Yu cu chung ca k thut x l mu
2.1.1. Yu cu chung ca k thut x l mu phn tch
X l mu l giai on u tin nhng rt quan trng ca qu trnh phn tch. Mi sai st
trong giai on ny u l nguyn nhn to ra sai s cho kt qu phn tch, c khi sai s rt ln.V
th mi cch x l mu phn tch, cng vi vic tun th theo QA/QC, cn phi bo m c
cc yu cu c th sau:
- Ly c hon ton, khng lm mt cht phn tch
+ Khng lm nhim bn thm cht phn tch vo mu t bt k ngun no
+ Kt qu x l phi ph hp vi phng php phn tch chn
- Dng cc ha cht phi m bo sch ng yu cu, mc ch v mc phn tch
- Khng a thm cc cht c nh hng vo mu
- C th tch hay lm giu c cht phn tch cng tt
2.1.2. Vn QA/QC trong x l mu phn tch
Mc tiu chung ca QA/QC trong x l mu phn tch l cung cp hay m bo cc iu
kin, cc bin php ti thiu cn thit m bo x l c tt mu phn tch t ng cht lng
mong mun.
X l mu l khu th hai v rt quan trng ca qu trnh phn tch. Nu vic x l mu
khng m bo c trung thc, ng n v loi c mi sai st nh hng nh mt hay
nhim bn cht phn tch th cc cng vic sau d cho c lm cn thn v chnh xc n u i
na th s liu phn tch cng khng cho ta ng thc t ca cht phn tch c trong mu. V vy
m bo cho cng vic x l mu c tt th nht thit phi thc hin cng tc QA/QC. Vy
QA/QC trong x l mu phn tch l g?
2.1.2.1 Khi nim v QA
Nh chng ta bit, mc tiu chung ca QA l cung cp hay m bo cc iu kin v
bin php ti thiu cn thit c c mt sn phm ca lnh vc nghin cu hay sn xut t
ng cht lng mong mun. Do c th ni mt cch tm tt l trong cng tc x l mu phn
tch th QA l cc quy tc, bin php v cc iu kin cn thit c nghin cu, la chn v
bin son thnh mt quy trnh (h thng), phc v cho cng tc x l mu phn tch nhm mc
ch ly c dung dch mu phn tch trung thc, khng mt cht phn tch, khng b nhim bn
v i din ng cho i tng cn phn tch. V vy thc hin QA trong x l mu phn tch l
iu rt cn thit v ch c m bo c QA trong x l mu th chng ta mi c y iu kin
khng nh cc s liu phn tch l c c s khoa hc, ng n v phn nh ng thnh phn
ca cht phn tch c trong mu nghin cu.
2.1.2.2. Khi nim v QC
Mc tiu chung ca QC l cung cp cc iu kin v bin php k thut cn thit gim
st v kim sot cht lng ca mt qu trnh no trong sn xut hay nghin cu khoa hc
m bo cht lng cho sn phm, ng thi pht hin cc sai st v tm bin php khc phc cc
sai st m bo thu c sn phm c cht lng ng yu cu mong mun. V th trong cng
vic x l mu cng vi QA, cng cn phi thc hin c bin php QC. Vy QC trong x l mu
phn tch l g?
Trong cng tc x l mu phn tch, QC l bin php, cc iu kin k thut v hot ng
gim st v kim sot cht lng ca mi cng vic trong x l mu phn tch. N l cc quy tc,
bin php v cc iu kin k thut c la chn, xy dng, bin son thnh nhng quy trnh
phc v vic kim tra, gim st, kim chun qu trnh x l mu nhm m bo cho vic x l
mu phn tch c c tnh chnh xc, ng n v dung dch mu thu c sau x l phn nh v
i din ng cho i tng cn nghin cu phn tch. ng thi trnh hay hn ch ti a c cc
sai st v trang b, dng c, ha cht, s nhim bn hay mt mt cht phn tch khi tin hnh x l
mu v cc tc ng khc ca mi trng lm vic m chng ta khng mong mun.V th bt buc
phi thc hin cc mu QC (nh mu trng hin trng, mu trng trang thit b, mu trng phng
php, mu thm chun, mu chun thm nh).
2.1.2.3. Ni dung v quan h QA/QC trong x l mu

X l mu l mt hot ng c thc hin c hin trng v trong phng th nghim m

ch yu l trong phng th nghim. N l bc hot ng th hai ca ton b dy chuyn hay cng
tc phn tch mu c c s liu, thng tin tin cy v cc i tng cn quan st. V th mi sai
st trong x l mu u nh hng n kt qu phn tch. Do chng ta phi quan tm ng mc
n vic bo m cht lng cho cng tc hay mi hot ng x l mu phn tch c c
nhng la chn v trang thit b, phng php, cc iu kin cn thit v cch x l mu. chnh
l ni dung ca QA/QC trong x l mu phn tch. V vn ny cn c mt s quyt nh c th
thc hin theo cc ni dung chnh sau y:
- Nhn s: xem xt tay ngh v kh nng ca cn b phn tch
- La chn phng php x l mu cho i tng cn phn tch
- Xc nh khi lng mu cn ly x l v s lng cn x l kp
- Chn trang thit b, dng c v cc iu kin cn thit x l mu
- La chn cch kim tra phng php ng dng x l
- La chn cc ha cht v thuc th cn thit cho x l t yu cu
- Kim tra mi trng xung quanh trong qu trnh x l mu
- Cng tc kim chun trong x l mu, mu lp v mu trng cc loi
- Chn phng php bo qun mu thu c sau khi x l phn tch, nu cha tin
hnh phn tch ngay c
ng thi theo cc ni dung nu trn th hot ng QA/QC trong cng tc x l mu
phn tch phi bao gm cc vn sau y, bt u t lc chun b cho cng tc x l mu phn
tch cho n khi thu c kt qu ca chng v bo qun, ngha l phi thc hin cng tc QA/QC
- i vi tt c nhng ngi thc hin x l mu phn tch
- i vi cc trang b, my mc v dng c dng x l mu
- i vi cc cht chun, ha cht v thuc th cn dng cho x l mu
- i vi cc loi dng c ng, cha mu thu c sau x l
- i vi cc hot ng trong khi tin hnh x l v ghi chp h s x l
- i vi cng tc kim chun trong qu trnh x l mu
- i vi cng tc bo qun v lu mu phn tch
- i vi vic pht hin sai st v cc bin php khc phc sai st
l cc vn t ra cho ngi lm phn tch trong giai on x l mu. Lm tt tt c
cc vn ny tc l chng ta thc hin c QA/QC v hot ng x l mu l tha mn c
cc yu cu ca phn tch. Ngha l trong mi hot ng ca cng tc x l mu phn tch t lc bt
u chun b cho n lc x l xong ly c dung dch mu v bo qun chng phn tch
theo mt phng php c la chn.
2.2. Phn loi mu phn tch
2.2.1. Phn loi theo ha hc phn tch
Theo quan im ha hc phn tch, ngi ta thng chia cc loi mu phn tch thnh hai nhm
chnh, da trn thnh phn nn (matrix) ca mu l v c hay hu c
- Nhm cc loi mu c cht nn v c
- Nhm cc loi mu c cht nn hu c
Trong mi nhm c th phi xc nh (phn tch) c cht hu c v v c, ty tng trng hp v
theo cc yu cu phn tch c th khc nhau.
2.2.2. Phn loi theo trng thi tn ti
Xt v mt trng thi ca i tng mu phn tch th li c cch phn chia sau:
- cc mu thuc trng thi kh: khng kh, bi, cc cht kh
- Cc mu thuc trng thi rn v bn rn: st thp, kim loi, t , qung, bn, cy, qu
ht cc loi, thuc dng bt, vin
- Cc mu thuc trng thi lng nh cc loi nc t nhin, ao h, sng sui, nc sinh
hot, nc gii kht, bia, ru, xng du

Vic phn chia theo cch ny, chng ta thy ch mt loi cng cha nhiu th mu khc
nhau v tnh cht, v c, hu c ln ln V th phn loi ny c th rt khng khoa hc v kh
xem xt khi cn chn cc phng php x l mu phn tch cc cht cn thit.
2.2.3. Phn loi theo nhm ngnh
- Mu nng nghip:
+ Cc cy ci, tho mc
+ Cc loi hoa qu, rau c, sn phm nng nghip ti sng
+ Cc loi phn bn, t trng trt
- Mu cng nghip
+ Mu cng nghip than v in
+ Mu cng nghip ha cht
+ Mu cng nghip du kh v tng hp hu c
+ Mu cng nghip thc phm
- Mu dn dng v sinh hot
+ Cc loi mu sinh hot hng ngy ca ngi v ng vt to ra
+ Cc loi mu bnh vin
- Cc loi mu t nhin n khong, qung, t
Cc phn loi ny khi mi nhn tng l chi tit nhng khi xem xt v cch x l mu th mi thy
nhiu iu khng hay. Do theo quan im ca ha phn tch th cch u tin l tng i n
gin v thch hp nht.
2.3. Trang b x l mu phn tch
2.3.1. Yu cu ca trang b v iu kin x l mu
x l mu ty iu kin v phn loi mu, v cht phn tch m c s la chn cc trang b v
phng php x l mu cho ph hp. Ngy nay trn th trng c nhiu loi trang thit b khc
nhau dng cho x l mu t n gin n phc tp v hon ton t ng. Song bt k loi thit b
no cng phi m bo cc vn sau:
a. Thc hin QA/QC trong x l mu
b. Cn ch thm cc yu cu c th ti thiu l:
+ Theo yu cu ca mc phn tch v cp hm lng
+ Ph hp vi mi loi mu, nu n gin, ph thng th cng hay
+ Khng lm mt v khng lm nhim bn cho mu phn tch
2.3.2. Cc loi dng c n gin
- Cc loi cc un v ng nghim
- Cc loi chn, bt nung (s, thch anh, kim loi qu)
- Cc loi ng nghim un c (chu nhit)
- L nung, t sy
- Cc loi h chit lng-lng, lng-rn v lng-kh
- Bnh Kendan cc loi
2.3.3. Cc loi trang b hon chnh
- Cc loi h chng ct khc nhau
- H thng bnh Kendan ng kn, hi lu v t ng
- Cc loi l vi song (n gin v hon chnh)
- Cc h ca k thut chit lng lng lien tc
- Cc h ca k thut chit lng-rn (chit pha rn)
- Cc h ca k thut chit kh-rn (chit pha kh)
- Cc h ca k thut chit siu m
- Cc trang b ca k thut chit Soxhlet
- Cc loi thit b thng hoa mu
- Cc loi khc
Song mt iu phi nh rng d chn cch no, dng c no th cng phi m bo x l
c mu mt cch tt nht m khng lm mt cht phn tch, khng lm nhim bn v a c

cht cn xc nh v dng ph hp nht cho phng php phn tch chn. Cc loi trang thit b
ny s c ni n trong cc k thut x l mu c th.
2.4. Khi qut v bn cht cc k thut x l mu
X l mu phn tch l mt qu trnh phc tp, c ha hc, ha l hay vt l v ha hc
phc tp kt hp chuyn cc cht hay cc nguyn t hay cc ion cn xc nh c trong mu phn
tch ban u, a chng v dng tan trong mt dung mi thch hp nh nc hay dung mi hu c
sau c th xc nh c n theo mt phng php phn tch thch hp. Tuy th, nhng vic
x l mu phn tch l c thc hin theo rt nhiu k thut c nguyn l, bn cht, c ch vt l
v ha hc c khi rt khc nhau ty theo mi loi mu v yu cu phn tch nhng cht no. V d
nh x l bng acid, x l bng kim, hay tro ha kh, tro ha t, s chit lng lng, chit pha
rn, chng ct. Song mt cch i th th chng ta c th phn loi theo mt s nguyn tc, c
ch da theo cc c ch sau y ca ha hc, ha l v vt l trong qu trnh x l mu.
V th trong chng ny ch trnh by v cc nguyn tc, bn cht ca cc k thut x l
mu phn tch, m khng i su vo cu to v cch vn hnh cc loi dng c hay trang thit b.
l cc k thut sau y:
- K thut v c ha t
- K thut v c ha kh
- K thut v c ha kh t kt hp
- Cc k thut chit thng thng
- K thut chit Soxhlet (kiu thng v t ng)
- K thut chit pha rn, pha kh
- K thut chit siu m
- Cc k thut chng ct (thng, chn khng, li cun)
- K thut ln men nu
- K thut thng hoa cht phn tch
- K thut chlor ha mu bng kh chlorine mi sinh
- K thut in phn
Trong cc k thut , mi k thut ch thch hp cho mt s cht hay mt nhm cht nht
nh v mi k thut cng c mt s u v nhc im ring v phm vi ng dng ca n. Ngha l
khng th c mt cch x l mu no l ph hp c cho mi loi mu, mi cht phn tch. V th
ty theo yu cu c th ca cng vic phn tch m ngi lm phn tch phi nghin cu, xem xt
v la chn mt k thut no cho thch hp trong c s ca mnh v m bo c kt qu phn
tch ng n v tin tng. Tc l phi thc hin QA/QC trong cng vic x l v trong cng vic
phn tch t ra.
Trong khi x l hay phn hy mu, c th c rt nhiu qu trnh vt l v cc phn ng ha
hc c th xy ra ng thi, ty thuc vo mi loi nn mu, thnh phn ca mu v cc cht c
cho vo dng thc hin x l mu. Ni chung mt cch tng th c th c cc qu trnh sau y
xy ra:
- S ph v mng li cu trc ca cht mu ban u, gii phng cc cht phn tch, a
chng v dng dung dch di dng cc mui tan ca cc ion.
- Qu trnh oxy ha kh lm thay i ha tr, chuyn i dng, lm tan v cu trc vt
cht mu ban u gii phng chat phn tch v dng hp cht tan trong dung dch.
- S t chy, ph hy cc hp cht hu c v mn, to ra kh CO 2, NO2, SO2, nc v
gii phng cc kim loi trong cht mu hu c ban u, a chng v dng cc hp cht
hay mui d tan trong acid.
- S to ra cc hp cht phc bn, t phn ly lm tan cht mu, to ra cc phc dng tan
ca cc cht phn tch trong dung dch (dung mi) qua m ha tan cht mu.
- To ra hp cht d bay hi, lm mt i anion ca cht mu ban u lm mu b phn
hy to ra cc cht khc tan trong dung dch acid hay kim hay acid.

S kt tinh hay kt ta cht phn tch di dng hp cht khc, lm cht phn tch c
tch ra khi mu ban u v chuyn sang hp cht mi m chng ta ly c chng ra
khi mu ban u.
Nh vy trong qu trnh x l v phn hy mu c th c cc qu trnh vt l, cc phn ng
ha hc xy ra nh phn ng oxy ha kh, phn ng thy phn, phn ng to phc, phn ng ha
tan, phn ng kt ta ca cc phn t cht mu vi dung dch acid phn h mu v cc phn t
cht c trong mu vi nhau.
l ni chung tt c cc kh nng c th c, song trong thc t, ty thuc vo thnh phn
v bn cht ca mi loi mu, loi cht phn tch, phng php phn tch, ha cht x l mu m c
nhng qu trnh xy ra vi loi mu khi x l. Sau y chng ta s xem xt mt s k thut x l
mu c v ang c dng.
2.4.1. K thut v c ha t (x l t)
2.4.1.1. Bng acid mnh, c v c tnh oxy ha
a. Nguyn tc v bn cht
Dng acid mnh HCl, H2SO4 hay cc acid mnh, c c tnh oxy ha mnh (HNO3, HClO4)
hay hn hp 2 acid (HNO3-H2SO4) hay 3 acid (HNO3-H2SO4-HClO4) phn hy mu trong iu
kin un nng trong bnh Kendan hay trong ng nghim. Lng acid thng gp 20-15 ln lng
mu, ty loi mu. Thi gian ha tan mu (x l) trong cc h h, bnh Kendan thng t vi gi
ti vi chc gi, cng ty loi mu, bn cht ca cc cht. Cn nu trong l vi song h kn (c p
sut) th ch cn 50-60 pht. Di tc dng ca acid c v nhit , y cng c cc qu trnh vt
l v ha hc sau y xy ra, v d:
- S ph v mng cu trc ca cht mu, gii phng cc cht phn tch a chng v dung
dch di dng cc mui tan.
- Qu trnh oxy ha kh lm thay i ha tr, chuyn i dng, lm tan v cc cht mu,
gii phng cht phn tch v dng mui tan trong dung dch.
- Nu x l mu hu c phn tch kim loi th c s t chy, ph hy cc hp cht hu
c v mn to ra kh CO 2, nc v gii phng cc kim loi trong cht mu hu c v
dng mui v c tan trong dung dch.
- To ra hp cht d bay hi, lm mt i anion trong phn t cht mu lm mu b phn
hy to ra cc hp cht khc tan trong dung dch.
- Nh vy trong qu trnh x l mu y cng c th c cc phn ng ha hc xy ra
nh phn ng oxy ha kh, phn ng thy phn, phn ng to phc, phn ng ha tan,
phn ng kt ta ca cc phn t cht mu vi cc acid dng phn hy mu v cc
cht c trong mu vi nhau.
Sau y l mt vi v d th hin cc qu trnh trn, khi x l mu phn tch khc nhau:
- v d 1: ha tan qung mangan oxide bng HNO3 v H2O2.
+ MnO2 + HNO3 + H2O2 Mn(NO3)2 + H2O + NO2.
- V d 2: ha tan qung st bng vng thy
+ Fe2O2.Fe3O4 + HNO3 + HCl FeCl3 + NO2 + H2O
- v d 3: x l mu thc phm, rau qu
+ Nn mu + HNO3 + H2SO4 CO2 + H2O + mui kim loi ha tan
Cc dung dch acid dng ha tan v x l mu: trong x l t, ngi ta thng dng cc
loi dung dch acid c, song tt nhin chn loi no l ty thuc vo bn cht ca nn mu v cht
phn tch tn ti trong mu
- Cc n acid c HCl, H2SO4, HNO3, HClO4.
- Hn hp 2 acid: cng thy, HNO3-H2SO4, HF-H2SO4
- Hn hp 3 acid: HCl-HNO3-H2SO4, HNO3-H2SO4-HClO4.
- Hn hp 1 acid v 1 cht oxy ha: H2SO4-KMnO4, HNO3-H2O2,
- Hn hp 2 acid v 1 mui: HNO3-H2SO4-KMnO4,
Nhit khi x l mu l ph thuc vo nhit si ca acid dng phn hy mu. Khi
dng hn hp acid th nhit x l mu cn ty thuc thm vo thnh phn ca hn hp acid v
thng thng nhit ny nm trong gii hn gia nhit si ca acid d si nht v acid kh si

cht. i vi nhng mu kh phn hy, ta phi dng cc acid hoc hn hp cc acid c nhit si
cao v tnh oxy ha mnh.
Acid
HCl HNO3 H2SO4 H3PO4 HClO4 HF
C (%)
36
65
98
78
72
40
o
Tsi ( C) 110 121
340
213
203
120
b. Cc loi hay kiu x l t
Vic x l mu theo phng php t c th c thc hin trn cc loi trang thit b khc
nhau, ty thuc vo kh nng phng th nghim v tnh cht ca mu
- Trong iu kin thng, thit b n gin
+ Trong cc thy tinh, un nng trn bp in hay un cch thy.
+ Trong bnh Kendan thng
+ Trong bnh Kendan c hi lu
- Trong ni p sut cao: mu v acid c t trong cc hp kn sau t trong
+ T sy, bp cch ct, l nung
+ Luc trong ni nc si hay du si
- Trong l vi song (gm h kn v h)
+ H n gin: h bnh h hay h kn nhng khng iu khin nhit , p sut
+ H nhiu bnh, t ng hon ton: h h (c gim st nhit ) v h kn (c gim st
nhit v p sut).
Trong cc kiu x l trn, k thut x l t vi acid c c tnh oxy ha mnh trong bnh
Kendan hay trong l vi sng h kn ang c s dng rng ri, ph bin. cc nc pht trin, l
vi sng h kn c s dng mt cch ph bin trong x l mu do n trit , nhanh, hn ch mt
cht phn tch v nhim bn v tiu tn t ha cht.
c. Mt s th d v x l mu theo cch tro ha t
- V d 1: Ha tan mu kim loi v hp kim Cu hay Al bng acid HNO 3; ly 1 g mu
nghin nh (hay dng phoi bo) vo bnh Kendan, tm t bng vi git nc ct, thm 10 mL
HNO3 65%, 4 mL H2SO4 98%, lc u, cm phu nh vo bnh Kendan, un nh cho mu si v
phn hy cho n khi dung dch mu trong. S ha tan y lm thay i ha tr v trng thi
ca Ca, Al kim loi trong hp kim, chuyn chng thnh mui tan trong dung dch. Phn ng ha
hc chnh xy ra l:
Al + HNO3 Al(NO3)3 + NO2 + H2O
Cu + HNO3 Cu(NO3)2 + NO2 + H2O
- V d 2: ha tan mu thp chrome bng hn hp acid HNO 3 v HCl hay HNO3 v H2SO4.
Ly 0.5 g mu nghin nh (hay dng phoi bo) vo bnh Kendan, tm t bng vi git nc ct,
thm 15 mL HNO3 65%, 4 mL H2SO4 98%, lc u v un nh cho mu si v phn hy, cho n
khi dung dch mu trong. Qu trnh ny c s oxy ha kh ca Cl v N sinh ra Cl mi sinh phc
v cho phn hy mu. Di tc ng ca hn hp acid c ny v c nhit , mng li kim loi
b ph v, cc kim loi chuyn vo dung dch di dng cc mui tan. Phn ng ha hc chnh xy
ra y l:
Ni-Cr-Fe + HNO3 + HCl Ni(NO3)2 + Fe(NO3)3 + Cr(NO3)3 + NO2 + H2O
- V d 3: ha tan qung Mn oxide bng hn hp HNO 3-H2O2. xc nh Mn v cc tp
kim loi trong qung ny, qu trnh ha tan c s oxy ha kh, chuyn Mn(IV) v Mn(II) tan trong
dung dch. Ly 1 g mu qung nghin nh vo bnh Kendan, tm t bng vi git nc ct,
thm 15 mL HNO3 65%, 2 mL H2O2 30%, lc u v un nh cho mu si v phn hy cho n khi
dung dch mu trong. Phn ng ha hc xy ra l:
MnO2 + HNO3 + H2O2 Mn(NO3)2 + H2O + O2
- V d 4: X l mu rau qu bng hn hp hai acid HNO 3-H2SO4, trong bnh Kendan,
xc nh cc kim loi nng, c hi, nh Cd, Cu, Fe, Mn, Ni, Pb, Zn. Ly 5 g mu nghin mn v
trn u vo bnh kendan, thm 60 mL HNO3 65%, 5 mL H2SO4 98%, lc u v un nh cho mu
si v phn hy, cho n khi dung dch mu trong khng mu (6-8h ty loi mu). Chuyn dung
dch mu vo cc un 250 mL, lm bay hi ht dung dch acid cho n khi cn mui m, ngui,
nh mc bng dung dch HCl 2% thnh 25 mL. Trong qu trnh x l ny, cc nguyn t kim loi

di dng cc hp cht c kim ca mu rau qu s b acid c oxy ha, t chy cc cht hu c,

a cc kim loi v cc mui v c tan trong dung dch nc. Qu trnh ha hc chnh:
Nn mu + HNO3 + H2SO4 Mex(NO3)x + Men(SO4)m + H2O + CO2 + NO2.
- V d 5: X l mu tht c ti sng bng hn hp 2 acid HNO 3-H2SO4 trong bnh Kendan
xc nh cc kim loi c hi nh Cd, Cu, Fe, Mn, Ni, Pb, Zn. Ly 5 g mu nghin mn v
trn u vo bnh Kendan, thm 60 mL HNO3 65%, 8 mL H2SO4 98%, cm phu nh vo bnh
Kendan, lc u v un nh cho mu si v phn hy, cho n khi dung dch mu trong khng mu
(6-8h ty loi mu). Chuyn dung dch mu vo cc un 250 mL, lm bay hi ht dung dch acid
cho n khi cn mui m, ngui, thm 5 mL dung dch HCl 10%, nh mc bng nc ct thnh
25 mL. Trong qu trnh x l ny, cc nguyn t kim loi di dng cc hp cht c kim ca mu
rau qu s b acid c oxy ha, t chy cc cht hu c, a cc kim loi v cc mui v c tan
trong dung dch nc.
Tt c cc mu trong v d 1-3 c th x l trong l vi sng h kn v lng acid ch cn
dng l nhiu. Thi gian x l ch trong 50-60 pht l xong. Cn x l nh trn th phi mt t 610 gi m li khng trit bng x l trong l vi sng.
d. u nhc im v phm vi ng dng
Cc u v nhc im chnh ca k thut ny l:
- Khng mt cc cht phn tch
- Nhng thi gian phn hy mu rt di, nu khng dng l vi sng
- Tn nhiu acid c nht l khi s dng cc h h
- D b nhim bn khi x l bng h h do mi trng hay acid dng nhiu
- Phi ui acid d nn d b nhim bn do bi, hay mt mu
ng dng ch yu ca k thut ny l x l mu phn tch v mt s anion v c nh
halides, arsenate, sulfate, phosphate... trong cc loi mu sinh hot, mu hu c, v c, mu mi
trng, mu t, nc, bi, khng kh, mu kim loi, hp kim... K thut ny khng dng c cho
vic x l tch cc cht hu c phn tch v trong cc iu kin ny, cc cht hu c b ph hy
ht.
2.4.1.2. X l mu bng dung dch kim mnh c nng.
a. Nguyn tc chung
Trong phng php ny ngi ta thng dng cc dung dch kim mnh (NaOH, KOH) c
hay hn hp kim mnh v mui kim loi kim (NaOH-NaHCO 3) hay hn hp kim mnh v
peroxide (NaOH-Na2O2), nng ln (10-20%) phn hy mu trong iu kin un nng trong
bnh Kendan, trong hp kn hay trong l vi sng.
Trong qu trnh x l, di tc ng ca kim v nhit cao, c th xy ra:
- Ph v cu trc nn mu, chuyn cht phn tch v dng dung dch
- Cc cht ca mu tng tc vi kim to ra sn phm tan c
- C th sinh ra cc kh bay ra gip mu ha tan tt hn
- C th to ra cc hp cht bn, t phn ly v tan trong dung dch
- To ra cc sn phm kt ta vi nn mu
b. Cc cch ha tan v dung dch ha tan
Theo k thut x l ny, chng ta c th dng cc dung dch ca cc cht sau y x l
mu:
- Dung dch kim c nng (NaOH, KOH: 10-20%)
- Dung dch kim c nng c cht oxy ha mnh (NaOH-Na2O2)...
- Hn hp kim c nng c cht kh mnh.
- Hn hp kim mnh v mui ca n (NaOH-NaHCO3, NaOH-Na2CO3)
Qu trnh phn hy c thc hin khi un si dung dch mu, trong mt thi gian nht
nh, thng l t 6-10 gi trong bnh Kendan h. Cn nu trong l vi sng h kn (p sut cao) th
ch mt khong 40-60 pht.
Nhit si ca cc dung dch kim ty thuc vo thnh phn, nng ca dung dch kim
s dng x l mu. Ni chung trong khong t 115-230 oC v y l yu t thc y phn ng
xy ra nhanh.

c. Vi v d ng dng
- V d 1: ha tan oxid nhm bng dung dch naOH 10% nng. Ly 0.5 g mu dng bt vo
bnh Kendan, tm t bng vi git nc ct, thm 10 mL NaOH 10%, un si ha tan mu. C
ch y l chuyn trng thi tinh th rn oxid sang dng ion tan trong dung dch theo phn ng:
Al2O3 + NaOH NaAlO2 + H2O
- V d 2: Ha tan qung silicate bng dung dch NaOH 20% nng. Ly 0.5 g mu dng bt
vo bnh Kendan, tm t bng vi git nc ct, thm 15 mL NaOH 20%, un si ha tan mu.
C ch y l chuyn trng thi tinh th rn sang ion tan trong dung dch v bn dng mui
Na2SiO3 theo phn ng
SiO2.nX + NaOH Na2SiO3 + H2O + nX
d. u nhc im v phm vi ng dng
K thut tro ha t ny cng c u im l khng lm mt cc cht phn tch nht l cc
nguyn t v hp cht d bay hi. Nhng m c mt nhc im ln nht l tn nhiu kim tinh
khit cao, thng phi dng gp t 10-15 ln nhu cu cn thit mi c th x l c mu v v vy
kh nng nhim bn rt cao. Sau khi x l mu, phi loi b lng kim d bng cch trung ha vi
acid, song li lm long mu. y l mt phn vic kh khn v mt nhiu thi gi v cng hay l
nhim bn mu. V th cch ny ch c dng cho mt s trng hp khi khng c cch la chn
no khc. V d khi phn hy mu xc nh cc anion v c nh halides, nitrate, phosphate,
sulfate... trong cc di tng khng x l c bng phng php acid.
2.4.1.3. X l t trong l vi sng
a. Nguyn tc
K thut x l mu t trong l vi sng thc cht cng l phn hy mu khi un nng bng
dung dch acid mnh, c c tnh oxy ha hay bng dung dch kim c nng nh nu bn trn.
Tc nhn phn hy l cc acid v nng lng nhit cung cp cho mu do hin tng truyn nhit do
i lu t mt ngun nhit bn ngoi. i vi l vi sng, nng lng un nng mu c cung cp
bng bc x vi sng tn s cao, cc phn t mu u c nhn nng lng ng u v trc tip t
ngun vi sng, ph v cu trc nn mu t pha trong ra, v th qu trnh x l mu nhanh v trit
hn. Hn na, i vi h kn cn c p sut cao v nhit cao do hiu qu cao v rt nhanh
li tn t acid so vi phn hy iu kin thng trong bnh Kendan. Cc qu trnh vt l v ha
hc xy ra khi x l mu bng vi sng cng tng t nh cch x l mu t thng thng khc
nhng c tc nhanh hn v trit hn.
b. Trang thit b
Vic x l mu trong l vi sng c th thc hin trong h bnh h hay trong h bnh kn. Cc
thit b ny ngy nay hin din trn th trng vi nhiu loi, kch c khc nhau, phc v cho
tng mc ch nht nh. Cc thit b ny li c nhiu kiu rotor khc nhau c th thay i c
nh rotor phn hy mu, rotor lm bay hi dung mi v acid, rotor dng chit, rotor dng
sy mu, rotor dng nung mu (nh l nung cao tn)... v th rt thun tin cho cng vic x l
mu phn tch. K thut ny c s dng ph bin cc nc pht trin.
c. Cc v d ng dng
T cc v d trnh by trong mc 2.4.1.1.c v 2.4.1.2.c u c th thc hin trong cc h
h. Tuy vy nu c thc hin trong h kn th lng ha cht tiu hao ch khong v thi gian
rt ngn xung cn t 40-60 pht m hiu qu x l li trit hn, t mt cht phn tch hn.
2.4.2. K thut v c ha kh (x l kh)
2.4.2.1. Nguyn tc v qu trnh xy ra trong x l
K thut tro ha kho l k thut nung x l mu, song thc cht ch l bc u tin ca
qu trnh x l mu v sau khi nung, mu b cn li cn phi c ha tan (x l tip) bng dung
dch mui hay dung dch acid ph hp chuyn cht phn tch vo dung dch cho mt phng
php phn tch chn. Qu trnh nung x l mu c th khng thm cht ph gia, cht bo v hoc
c thm cc cht ny vo mu tr gip qu trnh x l c xy ra nhanh hn, tt hn v hn ch
mt mt cht phn tch.
Trong qu trnh nung x l mu, c th c cc qu trnh vt l v ha hc sau y xy ra ty
theo bn cht, thnh phn ca mi loi mu v ph gia thm vo, v d nh

Lm bay hi nc hp ph v nc kt tinh trong mu

S tro ha, t chy cht mn, cc cht hu c khc ca mu
Ph v cu trc ban u ca nn mu, chuyn sang cc nn n gin hn
Chuyn dng cc cht phn tch t phc to sang n gin
Qu trnh oxy ha kh thay i s oxy ha ca cc nguyn t trong mu
Gii phng mt s kh nh CO, CO2, SO2
C mt s tng tc ha hc gia cc cht trong mu vi nhau v vi ph gia thm vo
to ra cc cht mi.
Tt c cc qu trnh gp phn l tan v mu ban u, ha tan cht phn tch vo dung
dch. Bng sau y l vi v d v s nung mt s mu phn tch trong iu kin c v khng c
cht ph gia
Bng 2.1: v d v cc qu trnh trong x l kh trong l nung
Loi mu
t st
Qung silicate
Qung Ferit
Qung CuS
Dolomit
LnCO3F.xH2O
Nha ng
Thc phm
Rau qu
Rau qu
Cht hu c

Ph gia
KOH-Na2O2
KOH-Na2O2

KNO3-HNO3
KNO3-HNO3

Nhit
550-650
500-600
550-600
550-600
550-650
550-650
550-650
500-550
500-550
500-550
500-600

Sn phm sau khi nung

Na2SiO3-K2SiO3-H2O
Na2SiO3-K2SiO3-H2O-MeX
FeO-Fe2O3-SO2-H2O
CuO-SO2-H2O-MenXm
CaO-MgO-H2O-CO2-MenXm
Ln2O3-CO2-HF-H2O-MenXm
MexOy-CO2-SO2-H2O-MenXm
MexOy-CO2-H2O-KxXy-NO
MexOy-CO2-H2O-KxXy-NO
MexOy-CO2-H2O-MexXy
MexOy-CO2-H2O-NO2

l nhng qu trnh c th xy ra v tt nhin l a dng v phc tp, v xy ra nh th

no l ty vo thnh phn ca nn mu, cc iu kin nung nh nhit , mi trng nung l khng
kh hay kh tr, c ph gia hay khng trong nhit l yu t chnh. Kt qu ca qu trnh nung
l sn phm c thnh phn c th n gin hn (nh trong bng trn) v v vy tan trong cc dung
dch acid hay kim long.
K thut v c ha kh thng c dng cho cc mu hu c, x l xc nh cc kim
loi v cc mu qung v c c cu trc bn vng rt kh tan trong ngay c cc acid hay kim
mnh. Vic tro ha cng c th c thc hin khi c hoc khng c thm cc ph gia bo v vo
mu. Cc cht bo v thng c dng trong qu trnh x l mu ny l
- Cc acid mnh c: HNO3,H2SO4,H3PO4...
- Mt s mui: KNO3, Ca(NO3)2, Mg(NO3)2, LiBO2, Na2B4O7...
- Hn hp acid-mui: Mg(NO3)2-HNO3, HNO3-H2SO4,...
- Hn hp kim-mui: KOH-NaHCO3, KOH-Na2SO4,...
- Hn hp mui-peroxide: KHCO3-Na2O2, NaHCO3-Na2O2,...
- Hn hp kim mnh-peroxide: NaOH-Na2O2, KOH-Na2O2,...
- Hn hp kim-mui-cht oxy ho: KOH-NaHCO3-Na2O2...
- Mt acid mnh, c v mt cht to phc
Sau y chng ta ch im qua mt vi v d ca hai cch nung x l mu theo k thut tro
ha cp trn
2.4.2.2. Trang b x l mu kh
Cc trang b x l mu kh thng khng a dng, bao gm hai loi chnh
- Trang b thng thng: t sy v l nung cc loi
- Trang b hin i: cc loi l vi sng
2.4.2.3. Tro ha khng khng c ph gia bo v v cht chy
Nung mu khng c ph gia v cht bo v l qu trnh x l mu s b nh tc dng ca
nhit thch hp trong mt thi gian nht nh ph v mng tinh th ban u ca mu phn tch

 chuyn n sang dng khc, n gin hn, d ha tan vo dung dch acid hay kim trong cc giai
on x l mu k tip. Sau y l mt vi v d:
- V d 1: tro ha kh mu rau qu xc nh kim loi (Na, K, Ca, Mg, Cd, Co, Cr, Cu, Fe,
Mn, Ni, Pb, Zn). Cn 5 g mu vo chn thch anh, em sy kh t t cho n khi mu kh en, ri
em nung 3 gi u nhit 450oC, sau nng ln 530-550oC cho n khi mu ht than en, thu
c mu tro trng. Ha tan tro thu c trong 10 mL dung dch HCl 15%, un nh cho tan ht,
nh mc thnh 25 mL bng nc ct. Cc nguyn t Cd, Cu, Pb Zn s b mt mt t (8-15%) khi
nung.
- V d 2: Tro ha kh mu du m (du th) xc nh cc kim loi (Na, K, Ca, Mg, Cd,
Co, Cr, Cu, Fe, Mn, Ni, Pb, Zn). Cn ly 5 g mu vo bt hay cc thch anh, un nh trn bp in
hay sy kh mu t t sau em nung nhit 450 oC trong 3 gi, sau nng ln 530-550 oC
n khi ht than en, thu c mu tro trng. Ha tan tro thu c trong 15 mL dung dch HCl
18%, un nh cho tan ht, nh mc thnh 25 mL bng nc ct. Cc nguyn t Cd, Cu, Pb Zn s b
mt mt t (8-15%) khi nung.
Theo cch ny thng thng mt s nguyn t trong mu b mt khi nung nh Cd (10-18%),
Cu (7-12%), Pb (8-15%)... v lng mt i li khng n nh, khng kim sot v khng ch c
trong qu trnh nung. S mt mt ny cng nhiu khi nhit nung mu cng cao hay thi gian
nung cng lu v gy v vy l mt ngun sai s ln cho kt qu phn tch. Nh v d 1, nu nung
mu nhit 530oC, Cd v Pb s mt t 8-10% nhng khi nung 600 oC th Cd v Pb s mt n
gn 20%.
2.4.2.4. Tro ha c ph gia v cht chy bo v
Nung x l mu c cht ph gia v cht bo v cng l qu trnh x l mu s b nh tc
ng ca nhit c thm tng tc h tr ca cht ph gia, thng l cht chy, acid c..., trong
thi gian nht nh ph v cu trc tinh th dng ban u ca mu phn tch, chuyn chng sang
dng d ha tan hn trong acid hay kim. Khi c cht chy, nhit nung thng thp hn so vi
khi khng c cht chy, thi gian ngn hn song li trit hn nht l cc mu phn tch c matrix
bn, chu nhit hay mu hu c th tc dng ca cht ph gia v bo v li cng quan trng. Trong
hai v d trn, nu x l mu c cht bo v th khng xy ra s mt mt cc nguyn t nh trn.
V d 1: tro ha mu rau qu xc nh kim loi (Na, K, Ca, Mg, Cd, Co, Cr, Cu, Fe, Mn,
Ni, Pb, Zn) dng cht ph gia. Cn 5 g mu vo chn thch anh, thm 1 g KNO 3, 5 mL HNO3 65%,
trn u v un nh cho mu si u v cho n kh en. Nung mu nhit 450 oC trong 3 gi,
sau nng ln 500-530oC, n khi ht than en, thu c mu tro trng. Ha tan tro thu c
trong 15 mL dung dch HCl 18%, un nh cho tan ht, nh mc thnh 25 mL bng nc ct.
V d 2: Tro ha kh mu du m (du th) xc nh cc kim loi (Na, K, Ca, Mg, Cd,
Co, Cr, Cu, Fe, Mn, Ni, Pb, Zn) dng cht ph gia l 2 g KNO 3 v 10 g sodium benzene sulfonate.
Cn ly 5 g mu vo bt hay cc thch anh, thm cht ph gia, un nh cho mu si v cho n kh
en, sau nung nhit 450 oC trong 3 gi, sau nng ln 500-530oC n khi ht than en, thu
c mu tro trng. Ha tan tro thu c trong 15 mL dung dch HCl 18%, un nh cho tan ht,
nh mc thnh 25 mL bng nc ct.
V d 3: Tro ha mu sa xc nh kim loi (Na, K, Ca, Mg, Cd, Co, Cr, Cu, Fe, Mn, Ni,
Pb, Zn), dng cht ph gia l 8 mL H 2SO4 45% v 2 g KNO3 hay LiBO2. Ly 5 g mu vo chn
thch anh, thm cht ph gia, trn u, sy cn thn cho mu kh (mu d b si bt v bn ra
ngoi) v thnh than en sau nung nhit 450 oC trong 3 gi, sau nng ln 500-530 oC n
khi ht than en, thu c mu tro trng. Ha tan tro thu c trong 15 mL dung dch HCl 18%,
un nh cho tan ht, tip tc un ui acid cho n khi cn mui m. nh mc thnh 25 mL bng
HCl 2%.

V d 4: X l mu xc nh As trong qung hay b thi rn. Ly 0.5 g mu qung vo chn

Zr, thm 4 g KOH, un nh cho hn hp chy lng, thm cn thn 5 g Na2O2, lc u v nung 700
o
C trong 10 pht, ngui, ly chn cha mu ra, lau sch bn ngoi chn v b c chn vo cc
dung tch 400 mL cha sn 100 mL nc m 70 oC, lc k cho mu tan, ly chn Zr ra v trng
chn (trong v ngoi) 2 ln bng 20 mL nc ct. Thm vi mnh s xp nh vo cc, y knh
ng h v un si nh ui H2O2 (khong 15 pht), ngui. Lc dung dch qua giy bng ,
ra kt ta v giy lc 3 ln bng 20 mL dung dch KOH 0.05% nng. Gp nc lc v nc ra,
c cn cn khong 65 mL, thm 25 mL HCl 35%, lc u v nh mc 100 mL. y l dung dch
mu xc nh As bng k thut hydride ha. Cch x l ny thch hp cho cc mu rn nh
qung st, t , rc thi rn, bn, trm tch xc nh As, nhng hm lng Si trong cc mu
ny phi nh hn 10%.
2.4.2.5. u nhc im v phm vi s dng
- Thao tc v cch lm n gin
- Khng phi dng nhiu acid c
- X l mu c trit nht l cc mu c matrix hu c
- Khng lu nh phng php x l t thng thng
- Nhc im: c th mt mt s cht d bay hi nh Cd, Pb, Zn, Sb, Sn... nu khng
dng cht ph gia v bo v.
2.4.3. K thut v c ha tro-t kt hp
2.4.3.1. Nguyn tc chung
Nguyn tc ca k thut ny l mu c phn hy trong chn hay cc nung mu. Trc
tin ngi ta thc hin x l t s b trong cc hay chn nung bng mt lng nh acid v cht
ph gia ph v s b cu trc ban u ca matrix mu v to iu kin lu gi nhng cht d
bay hi khi nung. Sau em nung nhit thch hp. V th lng acid dng x l mu
thng ch bng hay 1/3 lng cn dng cho x l t. Qu trnh nung sau se nhanh hn v
trit hn, hn ch bt s mt mt cht phn tch so vi cc cch x l mu n (t hay kh)
Cc qu trnh vt l v ha hc xy ra khi x l mu kh-t kt hp cng tng t nh cc
qu trnh xy ra khi x l mu kh hay t, song y l s kt hp hai qu trnh k tip nhau. X
l t ban u l bo v mt s nguyn t cho x l kh k tip theo khng b mt mu. Cch
ny thch hp cho cc mu c matrix l cht hu c, x l xc nh kim loi v mt s anion.
2.4.3.2. Cc phng php v v d
V l x l kh-t kt hp, x l kh v t k tip nhau nn mi din bin s tng t
nh x l theo mt trong hai kiu ni trn. im khc bit ng k trong quy trnh x l mu ny so
vi kiu x l mu t l khng phi ui acid d. Sau y l vi v d.
- V d 1: X l mu rau qu xc nh kim loi (Na, K, Ca, Mg, Cd, Co, Cr, Cu, Fe, Mn,
Ni, Pb, Zn), ly 5 g mu cho vo chn nung, thm 10 mL HNO 3 65% v 5 mL Mg(NO3)2 5%, trn
u ri sy hay un trn bp in cho mu si nh v n kh thnh than en. em nung nhit
400-450oC trong 3 gi, sau nng ln 500-530 oC n khi ht than en, thu c mu tro trng.
Ha tan tro thu c trong 20 mL dung dch HCl 1:1, un nh cho tan ht, tip tc un ui acid
cho n khi cn mui m. nh mc thnh 25 mL bng HCl 2%. Dung dch ny dng xc nh
cc nguyn t ni trn.
- V d 2:X l mu sa xc nh kim loi (Na, K, Ca, Mg, Cd, Co, Cr, Cu, Fe, Mn, Ni,
Pb, Zn),. Ly 5 g mu vo chn nung, thm 15 mL HNO3, 2 mL H2SO4 98% v 5 mL Mg(NO3)2 5%,
trn u. x l mu t s b: sy mu cn thn trn bp in hay trong t sy cho mu kh
(mu d b si bt v bn ra ngoi) v thnh than en sau nung nhit 400-450 oC trong 3 gi,
sau nng ln 500-530oC n khi ht than en, thu c mu tro trng. Ha tan tro thu c trong
15 mL dung dch HCl 1:1, un nh cho tan ht, tip tc un ui acid cho n khi cn mui m.
nh mc thnh 25 mL bng HCl 2%.

- V d 3: X l mu tm, cua, c... xc nh cc kim loi (Na, K, Ca, Mg, Cd, Co, Cr,
Cu, Fe, Mn, Ni, Pb, Zn). Ly 5 g mu vo chn thch anh, thm 5 mL H 2SO4 98% v 5 mL
Mg(NO3)2 5% trn u. x l mu t s b: sy mu cn thn trn bp in cho mu kh v
thnh than en sau nung nhit 400-450oC trong 3 gi, sau nng ln 500-530oC n khi
ht than en, thu c mu tro trng. Ha tan tro thu c trong 15 mL dung dch HCl 1:1, un nh
cho tan ht, tip tc un ui acid cho n khi cn mui m. nh mc thnh 25 mL bng HCl 2%.
y l dung dch mu dng xc nh cc kim loi nu trn bng phng php ph hp thu phn
t hay ph nguyn t
2.4.3.3. u nhc im v phm vi p dng
u im ca k thut ny l tn dng v kt hp cc u im ca phng php x l mu
ut v kh
- Hn ch s mt mt ca mt s cht phn tch
- S tro ha l trit , sau khi ha tan tro s c dung dch mu trong
- Khng phi dng nhiu acid tinh khit
- Thi gian x l mu nhanh hn tro ha t
- Khng phi ui nhiu acid d, hn ch nhim mi trng, nhim bn mu
- Ph hp cho nhiu loi mu khc nhau xc nh kim loi
- Khng cn trang thit b phc tp, hin i, t tin
Cch ny c ng dng ch yu x l mu cho phn tch cc nguyn t kim loi v mt
s anion v c nh Cl-, Br-, sulfate, phosphate... trong cc loi mu sinh hc, mi trng, mu hu
c, v c. Cch x l ny khng dng c cho xc nh cc cht hu c. Trong cc phng th
nghim bnh thng, khng c trang b l vi sng th cch x l ny vn l mt phng php
thch hp, n gin m vn m bo c c kt qu tt.
2.4.4. Cc k thut chit
2.4.4.1. C s, nguyn tc v iu kin ca s chit
a. Nguyn tc v c s ca s chit
Chit da trn c s s ha tan (hay phn b) khc nhau ca cht phn tch vo trong hai
dung mi khng trn ln vo nhau. Tc l cht phn tch tan tt trong dung mi ny nhng li
khng tan tt trong dung mi kia, ngha l s phn b ca cht trong hai dung mi l rt khc nhau
nh m chng ta ly c cht phn tch ra khi mu ban u, chuyn n vo dung mi chng ta
mong mun sau xc nh n trong dung mi chng ta va chit vo. Nh th yu t quyt nh
s tch v x l mu y l h s phn b ca cht phn tch trong cc phase v iu kin thc
hin chit tch.
b. H s phn b ca cht
H s phn b l mt hng s vt l (hng s nhit ng) c trng cho s chit. N cho ta
bit s phn b (hay ha tan) ca cc cht phn tch trong hai dung mi (hay 2 pha) khng trn ln
vo nhau theo t l hay mc no. Nu gi tr hng s ny cng ln th s phn b cng khc
nhau nhiu v vy cng thun li cho s chit tch cc cht. V d cht X c phn b vo hai
dung mi khng trn ln vo nhau (A v B) th h s phn b ny c xc nh theo biu thc sau
C ( A)
KD X
C X (B )
Trong CX(A) v CX(B) l nng cht X trong hai dung mi A v B. Nu h s phn b
KD > 99/1 xem nh cht X chuyn hon ton vo dung mi A. l iu kin ca qu trnh chit
ly cht phn tch ra khi nn mu.
c. Cc iu kin ca s chit
c c kt qu chit tt, qu trnh chit phi c cc iu kin v t c cc yu cu
sau y
- Dung mi chit phi c tinh khit cao, m bo khng lm nhim bn cht phn tch
- Dung mi chit phi ha tan tt cht phn tch, nhung khng ha tan tt cc cht c
trong mu
- H s phn b chit phi ln s chit c trit
- Cn bng chit nhanh t, thun nghch gii chit c tt

- S phn lp khi chit phi r rng, nhanh v d tch ra ring bit

- Phi chn pH hay mi trng acid thch hp
- Chn nhit ph hp
- Phi thc hin lc mnh trong qu trnh chit
- Cho thm cht chng to bt khi cn c s phn lp tt
2.4.4.2. Cc phng php v k thut chit
2.4.4.2.1. Phng php chit lng-lng
a. Nguyn tc v iu kin
Nguyn tc: nguyn tc ca k thut chit ny l hai pha lng khng trn ln c vo nhau,
trong hai dung mi ny c th c mt dung mi cha cht phn tch c trong mt dng c
chit (phu chit). Khi lc chit, cht phn tch s c phn b vo hai dung mi theo tnh cht ca
chng t ti trng thi cn bng. V th h s nhit ng KD ca cn bng chit l yu t quyt
nh hiu qu ca s chit. Chit theo kiu ny c hai phng php l chit tnh v chit theo dng
chay lin tc. Trong phn tch, phng php chit tnh c s dng ph bin hn.
iu kin chit: qu trnh chit t hiu qu tt, phi c cc iu kin chit nh m t bn
trn.
b. Cc phng php, trang b v v d
- Phng php chit tnh: l phng pho chit rt n gin, ch cn mt s phu chit dung
tch 100-250 mL, c th tin hnh c mi phng th nghim. Vic lc chit c th thc hin
bng tay hay my lc nh. Tt nhin khi phi lm hng lot mu th s mt nhiu thi gian.
V d 1: Chit lng vt cc ion kim loi nng (Cd, Co, Cr, Cu, Fe, Ni, Pb, Zn) t nc bin
vo dung mi MIBK vi thuc th to phc APDC trong mi trng pH 3-4 xc nh cc
nguyn t ny bng phng php ph hp thu nguyn t. Ly 250 mL mu vo bnh chit, chnh pH
3-4 bng HCl 10%, thm 2 mL APDC 0.1% v 10 mL MIBK ri lc chit trong 5 pht. yn 5
pht cho phn lp, tch ly phn MIBK c cha phc kim loi Me-APDC. Sau xc nh cc kim
loi chit vo MIBK trc tip hay gin tip sau khi gii chit kim loi vo dung dch HNO 3
2.5M. Phng php ny thng c s dng tch chit v lm giu lng vt cc kim loi
trong cc loi mu nc nht l nc thi v nc bin.
V d 2: Chit ly tng iodine-triiodide t nc bin vo dung mi benzene trong s hin
din ca cht oxy ha mnh v mi trng acid chuyn iodide v iodine c chit vo
benzene. Sau xc nh n bng chun th tch hay bng trc quang. 200 mL mu + chnh
pH=3 + 5 mL H2O2 + 10 mL benzene + lc chit 6 pht, yn 5 pht cho phn lp. Tch ly lp
benzene cha Iodine i xc nh.
V d 3: Chit ly cc retinoid (vitamin A) t mu thc phm
Loi mu thc phm c cc dng sau
+ Thc phm lng nh sa ti. Ly 10 mL mu vo bnh chit, thm 20 mL ethanol tuyt i,
5-8 g Na2SO4 khan, trn u 2 pht, thm 10 mL dung mi hexane, lc mnh 4 pht, trong t
lnh 2 ht cho tch lp, lc ht chn khng, tch ly lp hexane c cha cc retinoid phn
tch chng bng HPLC hay MCEKC.
+ Cc loi mu bt, rau qu, trng tht: nghin hay xay thnh bt, bo qun -15 oC. Ly 5 g
mu vo bnh x l, thm 15-20 g Na2SO4 khan, trn u, thm 20 mL ethanol tuyt i, lc
mnh 2 pht, thm tip 10 mL hexane, lc mnh 4 pht, t trong t lnh 4 pht cho phn lp,
lc ht chn khng, tch ly lp hexane c cha cc retinoid phn tch chng bng HPLC
hay MCEKC.
+ Mu huyt thanh: ly 100 L mu huyt thanh cho vo ng nghim, thm 0.2 mL dung dch
NaCl 0.9%, 2 mL ethanol tuyt i, lc mnh 2 pht, thm 0.5 mL dung mi n-hexane, lc
mnh, ly tm cho phn lp, tch ly lp hexane c cha retinoid phn tch chng bng HPLC
hay MCEKC.
V d 4: chit v catotene t cc loi rau qu, l cy

Trc ht mu c chn v xay thnh bt, bo qun -15 oC trong t ng. Ly 5 g mu

cho vo bnh chit, thm 15 g Na 2SO4 khan, 1 g MgCO3 khan, trn u 2 pht, thm 20 mL dung
mi THF, khuy u trong 5 pht, lc ht chn khng, ly pha THF cha carotene vo bnh c quay
chn khng, ct cho n cn khong 1 mL, 1 pht cho kh, nh mc thnh 10 mL bng THF.
y l dung dch xc nh v catotene bng phng php HPLC.
- Phng php chit dng chy lin tc
Trong phng php ny khi thc hin, chit hai pha lng khng trn ln c vo nhau
c bm lin tc vi mt tc nht nh qua mt h chit nh phu chit hay bnh chit lin
hon ng kn. Hoc cng c th ch mt dung mi chuyn ng cn mt pha ng yn. Khi
cht phn tch s c phn b vo hai dung mi theo tnh cht ca chng, t ti trng thi cn
bng. V th y h s phn b nhit ng K D l yu t quyt nh hiu qu chit. Chit theo cch
ny nhanh, hiu sut cao, y l phng php chit c ng dng nhiu trong chit sn xut cng
ngh.
thc hin chit theo cch ny, phi c h thng my chit, ct chit, c bm bm cc
cht theo dng chy ngc chiu nhau v phi c b tch pha tch cc cht ngay trong qu trnh
chit, ly cht c chit ra lin tc hay theo tng thi im nht nh khi m cn bng t
c.
V d: Chit cc kim loi nng t nc bin. Ly V mL dung mi chit thng (V 25 mL
ty vo hm lng cht phn tch) cho vo bnh chit, thm 2 mL APDC 0.1% trong EtOH, cho
bnh chit vo h thng my chit, lp h cho kn. Ly 500 mL mu nc bin, chnh pH= 4 bng
HCl 10%. Bm tun hon lin tc dung dch mu qua bnh chit trong 30 pht, sau tch ly pha
hu c c cha cht phn tch. Nu khng c h thng bm th c th tin hnh chit theo cch gia
nhit bay hi dung mi chit.
- u nhc im v phm vi ng dng
Phng php chit n gin, d thc hin, c ng dng ph bin v rt c hiu qu
trong lnh vc tch chit v lm giu cc cht phn tch phc v cho vic xc nh hm lng vt
ca chng trong mu. Nht l tch v lm giu cc kim loi, cc cht hu c c hi trong cc loi
mu nc, nc thi, nc bin, nc khong. Cc u v nhc im chung ca k thut chit l:
+ Thch hp cho c chit phn tch v chit iu ch lng ln
+ Loi c cc cht nh hng, nht l matrix mu
+ Thch hp cho lm giu lng nh cht phn tch
+ Phc v cho chit cc mu v c v hu c
2.4.4.2.2. K thut chit Soxhlet.
a. Nguyn tc: chit Soxhlet l mt k thut chit c bit c thc hin nh mt loi thit
b ring ca n. Kiu chit ny cng nh kiu chit lng-lng nn v bn cht ca s chit vn l
nh lut phn b ca mt cht trong hai pha khng trn ln vo nhau. Song y hai pha khng
trn ln vo nhau. C th pha mu trng thi lng, bt, dng mnh hay l. Dung mi chit (hu
c) trong thi lng. V d chit ly du Meiton t l cy bc h bng dung mi hu c n-hexane
hay benzene. Chit cc thuc tr su hay bo v thc vt trong mu rau qu, mu t bng nhexane. V th y l kiu chit ca h chit c th c ng th v d th. Trong thc t, h d th l
ph bin v cht phn tch nm trong matrix rn.
b. Cc trang thit b v v d.
Trang b ca k thut chit ny c hai loi l
- H chit Soxhlet thng v n gin

- H chit Soxhlet t ng (auto-soxhlet)

Cch chit theo h u tin l n gin, vn hnh bng tay, cn h th 2 vn hnh mt cch
t ng. K thut ny ch yu c s dng tch cc cht hu c. K thut ny rt thch hp
chit cht phn tch nm trong mu pha rn nh dng bt, mnh nh hay cc vt liu kh nh l
cy... V th n l h chit d th. K thut chit ny ch yu c s dng cho chit tch phn tch
cc cht hu c trong cc i tng mu khc nhau khng dng lng.
- V d 1: Chit soxhlet thng ly mt s ha cht BVTV t mu rau qu. Ly 10 g mu
c nghin nh v trn u vo cc chit ca h chit, thm 25-30 g Na 2SO4 khan, 30 mL dung
mi chit n-hexane c 20% CH2Cl2. Sau tin hnh chit trong vng 180 pht.
- V d 2: chit auto-soxhlet ly ha cht BVTV t mu t. Ly 10 g mu c nghin
nh v trn u vo cc chit, thm 25-30 g Na 2SO4 khan, 30 mL dung mi chit n-hexane c 20%
CH2Cl2 (hay ethyl acetate). Sau tin hnh chit trong vng 150 pht, yn 10 pht, tch ly pha
hu c n-hexane c cha cht phn tch v xc nh chng.
K thut chit ny c u im l chit trit , song cc iu kin chit phi nghim ngt th
mi c kt qu tt. V th h thng vn hnh t ng cho kt qu tt hn nhng phi c h thng
trang b hon chnh. N thch hp chit cc cht hu c t cc i tng mu khc nhau, cht phn
tch c trong mu trng thi rn, bt, vt mu xp kh (l cy)... K thut ny c ng dng ch
yu chit cc hp cht hu c t cc mu cy, l, rau qu hay mu t nh trong hai v d trn.
2.4.4.2.3. K thut chit siu m
a. Nguyn tc: qu trnh chit y vn da trn c s chung ca s chit l s phn b ca
cht phn tch vo hai pha khng trn ln vo nhau, im khc bit l c thc hin chit trong
mi trng c thm tc dng ca sng siu m. Pha cha mu phn tch l pha nc v pha lng
cha cht phn tch l dung mi hu c (pha th 2) u c cho vo bnh chit, sau c t
vo trong t chit v tin hnh chit di tc dng ca sng siu m thch hp. Cch chit ny c
th thc hin hai trng thi ng th v d th nh:
- H ng th lng lng, y cht mu phn tch tan trong dung mi lng nh nc v
dung mi chit cng l cht lng, thng l cc dung mi hu c.
- H d th rn lng, trng hp ny mu phn tch trng thi rn thng c nghin
thnh bt hay bm nh v b vo trong bnh chit c dung mi dung mi chit thng l cc dung
mi hu c.
Khi tin hnh chit di tc dng ca sng siu m c tn s cao, mng cu trc ca cc
phn t cht mu b ph v, cht phn tch c gii phng v phn b (hay tan) vo trong dung
mi chit theo tnh cht ca n v y h phn b ca cht gia hai pha cng l yu t quyt nh
hiu qu ca s chit. Cn nng lng siu m c tc dng chnh l ph v cu trc ban u ca
mu, to iu kin cho cn bng chit xy ra d dng hn, trit hn.
c. Cc kiu chit v trang b
thc hin theo k thut chit ny chng ta phi c h thng bnh chit kn v h thng
bnh chit to siu m. Cc thit b ny hin nay u c thng mi ha theo tng quy m v
mc chit khc nhau, chit phn tch hay chit iu ch sn xut. V nguyn tc n c hai b
phn
- Bung chit siu m khng ch nng lng siu m
- Cc rotor cha bnh ng mu chit (loi 6 bnh, 9 bnh hay 12 bnh)
Sau y l vi v d.
- V d 1: Chit cc hp cht Chlorphenol t cc mu nc bng n-hexane: ly 250 mL mu
vo bnh chit, thm 20 mL n-hexane, y np bnh, vn cht, b vo rotor chit. Tin hnh chit
trong 20 pht, yn 5 pht sau ly bnh mu ra khi rotor v tch ly phn dung mi n-hexane,

lm kh bng Na2SO4 khan v xc nh cc cht chlorphenol trong pha n-hexane bng HPLC hay
GC-MS.
- V d 2: chit cc hydrocarbon thm, a vng t mu b thi ma ng. Ly 20 g mu
nghin nh, trn u cho vo bnh chit, thm 30 mL n-hexane cha 20% dichloromethane (DCM),
25-30 g Na2SO4 khan, y np bnh, vn cht, b vo rotor chit. Tin hnh chit trong 20 pht,
yn 5 pht sau ly bnh mu ra khi rotor v tch ly phn dung mi n-hexane, v xc nh cc
cht cn phn tch trong pha n-hexane-DCM bng HPLC hay GC-MS.
- V d 3: Chit ly mt s ha cht BVTV t mu t hay mu rau qu (nh
Methylparathion, sumithion, diazinon...). Ly 20 g mu t c nghin nh, trn u vo bnh
chit, thm 20 mL EtOAc, trn u, t bnh vo h my chit, tin hnh chit trong 40 pht,
ngui yn trong 10 pht, tch ly pha hu c c cha cc cht BVTV. Di pha hu c qua ct sc
k hp ph cha Al2O3-than hot tnh-Na2SO4 khan. Ra gii ct ny bng 40 mL EtOAc. Dung
dch ra gio dng xc nh cc cht BVTV bng GC, HPLC hay GCMS.
K thut chit ny c u im l nhanh, trit v hiu sut cao nhng i hi phi c trang
b h thng chit siu m hon chnh, c rotor chit cho mi cch chit khc nhau.
2.4.4.2.4. K thut chit pha rn.
a.Nguyn tc v iu kin
- Nguyn tc chung: nguyn tc ca qu trnh chit pha rn l mu trng thi lng hay hi
cn cht chit dng rn, th ht nh, xp (5-10 m ng knh). Cht chit gi l pha tnh v
c nhi vo ct sc k nh (kch thc 10 x 1 cm hay dung lng 5-10 mL). Cht chit l cc ht
silica trung tnh, cc ht nhm oxide hay silicagel alkyl ha nhm OH - bng nhng nhm alkyl
mch thng C2, C4, C8 hay C18... hay nhm phenyl. N c ch to trong iu kin tng t nh
iu kin ch to pha tnh ca HPLC nhng cc ht ny c xp ln hn v din tch b mt xp
thng t 50-200 m2/g. Khi x l mu, dung dch cha cht phn tch c di ln ct c cha pha
rn ny. Pha tnh s tng tc vi cc cht mu v gi li mt nhm cht phn tch, cn cc nhm
khc s i ra khi ct cng vi dung mi hoa tan mu. Nh th nhm cht phn tch tn ti trn pha
tnh v s c ra gii ra khi ct bng mt dung mi thch hp. Cc cht chit pha rn c th
c ch to theo cc loi sau y
+ Cht hp ph pha thng (silica trung tnh v aluminium oxide)
+ Cht hp ph pha ngc (silica c alkyl ha nhm OH)
+ Cht c kh nng trao i ion (cationit, anionit, cp ion)
+ Cht ry hay sng lc phn t theo kch thc
+ Cht hp ph pha kh-rn (purge and trap extraction)
Chnh v c nhiu loi pha tnh nh th nn k thut chit pha rn cng c nhiu c ch v
qu trnh ng hc khc nhau, theo bn cht mi c ch . Sau y l mt s c ch v iu kin
chn h chit (pha tnh v pha ng). Ni chung pha tnh trong chit pha rn cng tng t nh pha
tnh trong HPLC.
- Cc iu kin ca chit pha rn
Qu trnh chit y thc cht vn l qu trnh phn b ca mt cht trn hai pha tnh (pha
rn) v ng (pha lng hay kh) trong nhng iu kin nht nh v nhit , pH, tc chy dung
mi qua ct chit. Nh vy h s phn b K D ca mt cht trn hai pha cng l yu t quyt nh
hiu qu ca s chit. Tm li phi c cc iu kin sau y
+ Pha tnh hp ph hay trao i chnn lc vi mt nhm cht phn tch
+ H s KD phi ln
+ Qu trnh chit xy ra nhanh, t cn bng nhanh
+ Qu trnh chit phi c tnh thun nghch cao ra gii thun li
+ S chit c thc hin trong mt iu kin nht nh, cng n gin cng tt.
a. Cc kiu chit v c ch chit pha rn
- Chit theo c ch hp ph pha thng

Trong kiu chit ny, pha rn l cc silica trung tnh, c b mt phn cc. N o dng tt vi
cc cht mu khng phn cc v t phn cc. l s tng tc hp ph ca pha tnh: cht chit rn
trong ct. Ty theo bn cht v cu trc phn t mi nhm cht phn tch v bn cht hp ph ca
silica trung tnh v cc iu kin thc hin s tch m nhm cht phn tch no b pha tnh hp ph
v b gi li trn ct. C ch ca s tng tc ny hon ton tng t nh c ch tng tc trong
HPLC pha thng. Sau y l minh ha ca tng tc
Dung mi ra gii cht phn tch trong loi ny thng l cc dung mi hu c khng hay t
phn cc v k nc hoc hn hp ca chng theo t l thch hp. V d: n-hexane, n-heptane,
CCl4, CHCl3, CH2Cl2, benzene... Cc dung mi ny c gi l pha ng v phi ha tan tt cht
phn tch.
+ V d 1: Chit x l mu xc nh nhm hp cht chlorophenol trong nc. Acid ha
250 mL mu n pH 2 bng H2SO4 10%, sau di mu ny qua ct chit loi LASi-5 tc 4
mL/pht. Di qua ct 10 mL nc ct, gii hp bng 40 mL acetonitril hay dichloromethane v xc
nh bng HPLC hay GC.
+ V d 2: Chit x l mu xc nh mt s hydrocarbon thm a vng (PAHs) hay mt
s pesticides trong nc thi. Acid ha 250 mL mu bng H 2SO4 2% n pH= 6, lc b cn nu c,
di dung dch ny qua ct loi SiOH vi tc 4 mL/pht. Gii hp cht phn tch bng ACN hay
DCM. Xc nh cc cht phn tch bng GC hay HPLC
- Chit theo c ch hp ph pha ngc
Trong kiu chit ny, pha tnh l Silica c alkyl ha nn c b mt khng phn cc. N
tng hp tt vi cc cht khng phn cc hay phn cc km. Tng tc gia cht phn tch vi
pha tnh v pha ng ty thuc vo bn cht ca cht phn tch ( phn cc, kch thc, cu trc),
pha tnh ( phn cc, din tch b mt ring...) v pha ng ( phn cc, thnh phn, tc
chy...). Tng tc ny tng t vi tng tc ca pha tnh-pha ng-cht tan gp trong HPLC pha
o. Dung mi ra gii s dng trong kiu chit pha rn pha o ny l cc dung mi c tnh phn
cc nh nc, acetonitril, methanol, ethylacetate... Minh ha cc tng tc pha tnh-pha ng-cht
tan nh sau
+ V d 1: Chit x l mu xc nh nhm hp cht chlorophenol trong nc. Acid ha
250 mL mu n pH 2 bng HNO3 1N, ly tm b cn, sau di mu ny qua ct chit loi Baker10 TPE-phenyl column, 6 mL No. 7095, tc 3 mL/pht. Ra ct bng 10 mL HNO 3 0.01N, gii
hp bng 40 mL acetonitril v xc nh bng HPLC, GC hay GCMS.
+ V d 2: chit x l mu xc nh nhm cc kim loi (Cd, Co, Cr, Cu, Fe, Ni, Pb, Zn)
trong nc: thm 1 mL thuc th Ultrex- 8-oxyquinolin vo 250 mL mu, chnh pH 8-9 bng NH 3
1N, lc u ri di mu qua ct Baker-10 C18 SPE 5 mL vi tc 2-4 mL/pht. Ra ct bng 10
mL nc ct. Gii hp cc phc kim loi trn ct bng 10 mL MeOH, xc nh cc nguyn t trong
pha MeOH bng AAS. xc nh kim loi, nn tro ha t dch chit MeOH bng HNO 3. C th
thay thuc th ny bng Na-diethyldithiocarbamate 0.1% trong EtOH.
+ Chit x l mu xc nh mt s thuc BVTV trong nc. Ly 250 mL mu nc,
chnh pH 5, lc b cn. Di dung dch qua ct chit loi LR C 18 vi tc 4 mL/pht. Ra ct bng
10 mL nc ct, ht chn khng 5 pht. Ra gii cc cht BVTV trong ct bng 20 mL EtOAc. Ly
dch ra gii ny di qua ct th 2 cha Na 2SO4-...-than hot tnh, ra gii bng 10 mL EtOAc. Lm
bay hi dung dch thu c bng dng kh Nitrogen n khi dung dch snh, nh mc thnh 2 mL
bng EtOAc. Xc nh cc ha cht BVTV bng GC hay GCMS.
- Chit theo c ch trao i ion v cp ion.
Nguyn tc: da trn c s ca qu trnh tng tc ca cht phn tch vi ion i (ca cht
trao i ion-pha tnh). Cht phn tch s b lu gi trn pha tnh v s c ra gii bng mt pha
ng thch hp.

Cht trao i ion ca kiu chit ny c th c hai loi sau

+ Trao i cation acid mnh (gc R-SO3Na) v acid yu (R-COONa).
+ Trao i anion baz mnh (gc R-NR3OH) v baz yu (R-NHOH)
C ch trao i loi cation
Support-SO3Na + Men+ support-(SO3)nMe + n Na+
C ch trao i loi anion
Support-NR3OH + Xn- support-(NR3)nX + nOHTrong qu trnh trao i, ty thuc vo mi loi cht phn tch v pha tnh m qu trnh c th c
thc hin tt trong mt khong pH nht nh no .
Cng vi s trao i anion v cation; trong s chit pha rn cn c c ch chit theo kiu cp ion
(ion-pair). N cng hon ton tng t nh sc k cp ion ca h pha o (RP-HPLC). Pha tnh
y l cht trao i pha ngc.
C ch trao i cp cation
+ V d 1: Theo c ch trao i cation. Chit tch cc kim loi nng (Cd, Co, Cr, Cu, Fe, Ni,
Pb, Zn) trong mu nc khong, nc m, nc thi Acid ha 250 mL mu nc n pH 4, lc
b cn. Np mu vo ct chit (chelex-100, dng H +) vi tc 3-4 mL/pht. Gii chit cc kim
loi trong ct bng 10 mL HNO3 2.5M. Xc nh chng bng AAS hay ICP.
+ V d 2: Theo c ch trao i anion. Chit tch ly cc anion nhm halogen, sulfate,
nitrate trong nc. Ly 250 mL mu nc, chnh pH = 8, lc b cn, di qua ct chit loi
SPE.OH, 5 m, 6 mL vi tc 2-4 mL/pht. Ra gii cht phn tch bng 10 mL NaOH 0.5M v
xc nh cc anion Cl-, Br-, NO3-, sulfate trong dung dch ny.
+ V d 3: theo c ch to cp trao i cation. Chit tch ly cc ion kim loi nng trong
nc thi bng R-C18. Ly 250 mL mu nc, chnh pH 5, lc b cn, thm cht to cp ion ri di
dung dch mu qua ct chit loi Hypersil ODS 5 m, 6 mL, tc 2-4 mL/pht, sau ra gii
cht cn phn tch bng 10 mL dung dch HIBA 0.25%, pH 4-5 hay EDTA, pH =5.
+ V d 4: theo c ch to cp trao i anion: chit tch cc anion nhm halogen, nitrate,
sulfate trong nc thi. Ly 250 mL mu nc, chnh pH =8.5, lc b cn, thm cht to cp ion
ri di dung dch mu qua ct chit loi Hypersil R-NOH 5 m, 6 mL, tc 2-4 mL/pht, sau
ra gii cht cn phn tch bng 10 mL dung dch NaOH 0.2-0.3N.
- Chit theo c ch sng v ry phn t
Nguyn tc: cht chit y l cc ht silica (pha thun hay pha o) c l xp ln. S tch
chit theo k thut ny da trn s khc nhau v kch thc phn t ca cht phn tch khi mu
c cho qua pha tnh trong ct chit. Cc phn t kch thc nh s b dn p vo pha su trong
cng ca l xp, cc phn t kch thc ln s pha ngoi. Cc phn t c kch thc to hn l
xp s nm bn ngoi ht pha tnh. Nh vy khi ra gii, cc phn t to s c ra gii ra trc v
tun t theo s l cc phn t c kch thc nh dn. y chnh l c s ca s tch chit theo
bng k thut sng v ry phn t.
Cc qu trnh v v d:
+ V d 1: chit tch cc nucleobazide trong mu dch sinh hc. Ly V mL mu, nh ha v
ng nht bng 50-100 mL hn hp dung mi MeOH-ACN. Lc k v gn ly dch trong, di qua
ct chit Backer 10 SPE-P, 6 mL vi tc 3-4 mL/pht. Gii hp cht phn tch bng 20 mL
DCM. Xc nh bng HPLC hay MKEC.
+ V d 2: chit tch cc cht ca nhm protein. Ly V mL mu, nh ha v ng nht bng
50-100 mL hn hp dung mi MeOH-ACN 8:2. Lc k v gn ly dch trong, di qua ct chit

Backer 10 SPE-P, 6 mL vi tc 3-4 mL/pht. Gii hp cht phn tch bng 20 mL DCM. Xc
nh bng HPLC hay MKEC.
u nhc im v phm vi s dng chit pha rn
Chit pha rn l k thut chit mi ra i, ang pht trin v c ng dng trong khong
vi chc nm tr li y nht l cc nc tin tin. Nhiu loi pha rn v cc dng c chit khc
nhau c thng mi ha. Cc pha rn thung da trn nn silica hot ha, bin tnh tng
chn lc v dung lng trao i. K thut ny c mt s u nhc im sau
+ c tnh chn lc vi cc hp cht hu c v th thch hp cho phn tch vt
+ Thao tc n gin, nhanh hn cc k thut khc
+ Trong qu trnh chit c c s lm giu cht phn tch.
2.4.4.5. K thut chit by hp ph dng kh (chit rn-kh)
2.4.4.5.1. Nguyn tc chung
K thut ny da trn c s l mt nhit thch hp, khi thi mt dng kh tr nng (Ar
hay He) vo dung dch mu, mt nhm cht phn tch s b bay hi v li cun theo dng kh tr
n ct hp ph, ti y cht phn tch s b gi li trn pha tnh trong khi cc cht khc i qua. V
th v bn cht n cng l s chit gia hai pha kh v rn theo c ch hp ph. gii hp, ct
c gia nhit v cht phn tch bay ra khi b mt pha tnh v theo dng kh tr i vo my phn
tch (GC) hay hp thu vo mt dung mi hu c ph hp cho cc php phn tch khc nh HPLC
hay UV-VIS. Phng php ny c dng cho cc mu rn v lng, bn hay b thi nhng ch
thch hp cho cc cht c nhit bay hi thp (< 150 oC). Nh th ty vo vic la chn pha tnh
v nhit m ngi ta c th tch c cc nhm cht ra khi nhau sau phn tch chng theo
cc phng php ph hp. Cch ny rt thch hp cho vic tch chit cc cht hu c trong cc mu
rn (bt, bn, nho). Tt nhin vic trc tin phi nh ha cc mu ny bng mt dung mi thch
hp nh nc hay mt dung mi hu c nng c nhit i si cao. Pha tnh thng l cc cht hp
ph da trn silica nh silica trung tnh hay bin tnh tng t nh cc h NP-HPLC, RP-HPLC.
2.4.4.5.2. Cc kiu chit, trang thit b v v d
Theo k thut ny trang thit b cng c hai loi l h n gin v h hon chnh, t ng
c theo chng trnh nh sn. Kh mang s dng l Ar, He hay N2 tinh khit > 99.9%.
V d 1: chit mt s hydrocarbon d bay hi trong cc loi nc hay mu rn: ct hp ph
l pha rn DSC 25x1 cm (DSC: diphenylene oxide polymer-silicagel-coconut charcoal 1:1:1), mu
c gi trong bnh cu v dng Ar thi qua bnh mu vi tc 0.8-1.0 mL/pht a cht phn
tch vo ct hp ph. Cc cht hu c benzene, bromobenzene, bromomethane, bromoethane,
chloromethane, chloroethane, ethylbenzene s c hp ph vo ct ny. Vic gii hp c tin
hnh bng dng kh tr Ar gia nhit 180oC v dn trc tip vo my GC, GCMS hay vo mt
dung mi ph hp nh n-hexane dng xc nh bng mt phng php khc.
+ V d 2: chit ly mt s hp cht pesticides d bay hi trong cc loi nc hay mu rn,
bn (method 502,2b). Ct hp ph l pha rn LC2 25x1 cm. Mu c gi l 150 oC v dng kh Ar
thi qua mu vi tc 0.8-1 mL/pht chuyn cht phn tch vo ct hp ph. Gii hp cc cht
hp ph bng dng Ar nhit 200oC trc tip vo my GC hay GCMS.
K thut ny rt thch hp cho vic x l cc loi mu xc nh cc cht hu c c nhit
si < 200oC v d bay hi trong cc loi mu rn, bn, b thi. N c u im l chn lc cho
mi nhm cht ty vo cht php ph, thch hp cho cc phng php phn tch HPLC, GC, GCMS
nn c s dng ch yu cho phn tch vi lng cc cht hu c trong cc loi mu khc nhau.
2.4.5. K thut chng ct
2.4.5.1. Nguyn tc chung: chng ct l k thut tch da trn s khc bit v im si ca cc
cht theo c th ly c mt cht hay mt nhm cht da vo mc sai bit v nhit si,
trang thit b v iu kin (nhit ) chng ct. C nhiu kiu chng ct khc nhau nh:

- Chng ct thng thng

- Chng ct li cun hi nc
- Chng ct p sut thp (c quay chn khng).
2.4.5.2. Cc kiu v phng php chng ct
2.4.5.2.1. Chng ct thng thng
a. Nguyn tc: y l qu trnh chng ct cc cht ch n thun da vo im si ca cc cht
tch chng theo tng phn on trong nhng iu kin bnh thng. Khi chng ct, cc
cht c nhit si khc nhau s ngng t li ti nhng phn on khc nhau.
b. Cch thc hin v v d:
- V d 1: chng ct ly MeOH tinh khit t MeOH bn. MeOH c nhit si l
64.5oC nn s chng ct c MeOH tinh khit nu thu dch chng ct ti phn on c
nhit ny.
- V d 2: Chng ct ly acetone t hn hp acetone v MeOH bn. Aceton c nhit
si l 56.5oC nn khi chng ct chng ta ch ly phn on ti nhit ny.
- V d 3: chng ct mu xc nh hm lng NH 4+. Ly 10 g mu nghin mn cho vo
bnh chng ct, thm 100 mL NaOH 10%, lc u, un si nh, thi mt dng N 2 sch
qua bnh chng ct, dn hn NH3 sinh ra sang bnh hp thu l dung dch H 2SO4 0.1 N.
Chun lng acid d, chng ta s tnh c hm lng NH4+ hay N trong mu.
2.4.5.2.2. Chng ct li cun hi nuc.
Nguyn tc: y l qu trnh chng ct tinh ch v tch cc cht cng da vo im si ca
chng tch cc cht theo tng phn on trong nhng iu kin nht nh theo nhit si v
bay hi khi chng ct. Tuy nhin trong trng hp ny cht phn tch cn chng ct khng bay hi
mt mnh m phi c mt cht khc c nhit si gn hay bng chng li cun chng theo. Sn
phm li cun l mt dung dch hn hp c ha tan cht cn phn tch. V d ct ly
cresol,formaldehyde; ngi ta phi chng ct li cun n cng vi hi nc, sau mi xc nh
chng t dung dch ny hay tch chng ta khi nc bng cch chit lng-lng hay chit lng-rn
trc khi phn tch.
Cc cch thc hin v v d.
- V d 1: chng ct bng li cun hi nuc ly formaldehyde t bnh ph, bn Ly 20
g vo ci m no, thm 20 mL nc ct, nghin mn, trn u, cho vo bnh chng ct, trng ci
bng 20 mL nc ct, thm 60 mL nc ct na (cho 100 mL), lc u, lp ng sinh hn v
chng ct t t trong 30-40 pht, thu c 50 mL dch chng ct. Dung dch ct ny dng xc
nh formaldehyde bng ph UV-VIS hay HPLC hay GCMS.
- V d 2: chng ct ly tinh du bc h nh li cun hi nc. L bc h c ct nh,
cho vo bnh chng ct, thm nc cho ngp l (1 kg l, 1.5 L nc). Chng ct cho n khi thu
c 60% dung dch th dng. Dng phng php chit lng lng tch tinh du ra khi nc vo
dung mi hu c. Cch ny c th va c dng cho mc ch phn tch va c dng cho mc
ch iu ch sn xut.
2.4.5.2.3. Chng ct p sut thp- c quay chn khng
a. Nguyn tc chung: y l qu trnh chng ct tinh ch cc cht da theo im
si ca chng m tch cc cht theo tng phn on trong nhng iu kin nhit nht nh p
sut thp (khng ch bng bm chn khng) nhm tch cc hp cht km bn nhit. Trong iu
kin ny nhit ha hi ca cht phn tch s h thp, qu trnh chng ct s nhanh hn m li c
hiu qu tch tt hn. Khc vi iu kin thng thung, p sut thpcc cht s c nhit si v
bay hi khc nhau v th sau chng ct phi th li tng phn on xem cht phn tch hin din
u. ???

b. Trang b v cch thc hin: x l theo k thut ny, phi trang b h thng my
c quay v my bm chn khng iu chnh nhit v p sut thp thch hp. Sau y l mt
vi v d.
- V d 1: chng ct lm bay n-hexane ly cht phn tch nhm Vitamin A v Caroten
bng ct quay chn khng. Ly 10 g mu nghin nh vo phu chit, thm 20 g Na 2SO4 khan,
100 mL dung mi THF hay n-hexane. Lc k trong 10 pht, lc qua phu Busner, ly dung dch cho
vo v cho vo bnh ct ca my c quay ct cho dung mi bay hi n khi cn b m, ngui.
Ha tan b ny trong 5 mL MeOH, dung dch ny dng xc nh Caroten bng HPLC.
- V d 2: Chng ct tch MeOH tinh khit t MeOH k thut (nguyn liu th) v thu ly
b cn li xc nh mt s tp cht c trong MeOH k thut. Ly 200 mL MeOH vo bnh chng
ct, lp h thng c quay chn khng v chng ct MeOH cho n khi dch lng trong bnh chng
ct cn khong 2 mL, ngui. Ly b ny ha tan trong 5 mL DCM, ly tm hay lc tch b cn.
Xc nh cc tp cht hu c trong dch lc bng GC, GCMS hay HPLC.
2.4.6. K thut ln men mu
2.4.6.1. Nguyn tc v c im
Chuyn hay ha tan mu vo trong nc thnh dung dch hay th huyn ph, thm 10-15
mg men xc tc, v chnh mi trng bng acid hay kim, hay mui acetate cho ph hp (pH= 7-8),
ri a mu vo bung ln men nhit t 37- 40 oC cho n khi mu trong hon ton, tc l
cc kim loi chuyn vo dung dch. Thi gian ln men t 7-10 ngy. Kiu ny rt thch hp cho
phn tch xc nh cc kim loi trong cc mu ng ma, nc ngt gii kht, bia, ru, cc mu
nc qu chn, cam, chanh...
K thut ny c cc u nhc im v c im nh sau:
+ K thut n gin, d thc hin
+ Khng tn km ha cht nhng cn t m iu chnh c nhit
+ Mt thi gian
+ Ch p dng c cho mt s loi mu
+ K thut ny c dng ch yu l xc nh cc kim loi trong mu dng lng nh nc ngt
gii kht, cc loi nc qu, ng hay dung dch ng.
2.4.6.2. Cc phng php v v d:
- V d 1: Xc nh lng vt kim loi nng trong ng vng hoa m, nc ngt. Ha tan 5
g ng vo 80 mL nc ct, chnh pH =7-8, un nng n 40 oC, thm men xc tc, y knh ng
h, trong t m duy tr 37- 40 oC cho ln men trong 7 ngy. Thm 10 mL HCl 35%, un si, ly
tm ly dch trong, lm bay hi cn mui m. nh mc thnh 25 mL bng HCl 2%, xc nh kim
loi nng trong dung dch ny.
2.4.7. Phng php pha long bng dung mi thch hp.
2.4.7.1. Nguyn tc v c im
Nguyn tc: chn mt dung mi thch hp ha tan tt cht mu pha long n theo mt t
l nht nh sau phn tch bng mt phng php chn. V d phn tch cc kim loi kim th
trong du nht. Pha long mu 20 ln bng dung mi MIBK, xc nh bng AAS hay ICP-AES.
Cc lm ny kh n gin, d thc hin v khng cn trang thit b phc tp nhng li ch thch hp
cho mt s trng hp hn ch nh hm lng cht phn tch trong mu ln c th vn xc
nh c khi pha long. Qu trnh pha long s gim thiu cc yu t nh hng n cht phn tch
nhu thnh phn nn, nht, cn khng tan...
2.4.7.2. Cch thc hin v v d
- V d 1: Xc nh cc kim loi kim th (Ca, Ba, Sr) trong du bi trn hay du nhn. Pha
long mu 20 ln bng MIBK, ly tm b cn. Dch lc em xc nh bng FAAS hay ICP-AES.
C th pha long mu bng CCl4 v xc nh bng GFAAS.

-V d 2: Xc nh cc hydrocarbon thm trong du m. Pha long mu du 25 ln bng nhexane v DCM. Lc u, ly tm ly dch trong. Xc nh bng GC hay GCMS.
- V d 3: pha long mu huyt thanh bng nc ct xc nh kim loi K, Na, Ca, Mg.
+Xc nh K, Na: ly 0.2 mL huyt thanh pha long bng nc ct thnh 20 mL.
+ Xc nh Ca, Mg: ly 0.2 mL huyt thanh pha long bng nc ct thnh 10 mL.
+ Xc nh Cu, Zn: ly 0.25 mL huyt thanh pha long bng nc ct thnh 1 mL.
2.4.8. K thut thng hoa ly mu phn tch.
2.4.8.1. Nguyn tc chung: da trn c s tnh cht hay c im ca cht phn tch c kh nng
thng hoa trong mt iu kin nht nh khi x l mu tch n ra khi matrix. V d kim loi Hg,
Ga.. ra khi mu t , qung hay b thi rn.
2.4.8.2. Trang b, cch x l v v d.
Cc trang b phc v cho kiu thng hoa cng c nhiu loi khc nhau, t n gin ti hon chnh
v t ng theo chng trnh.
- V d: thng hoa ly Hg trong mu qung. Cho 1 g mu qung nghin mn vo trong bnh
hai bu hay cc thng hoa. Thm 0.6 g Fe kim loi, 1 g CaO khan, lc nh cho ng nht. Lm lnh
phn ng thch anh n 10oC bng b iu nhit, nc hay tuyt carbonic v t nng bu cha
mu trn n kh, quay u bnh mu Hg thng hoa cho n khi hn hp mu trong bnh c mu
sm. t thm 2 pht na. Khi thng hoa, Hg s bm vo ng thch anh c lm lnh hay
y bnh ngng to thnh mt lp sng bng. p b bu cha mu bn di, ly phn ng thch
anh c Hg bm vo, ha tan Hg trong HNO31:1 nng 80oC, lc u, yn 30 pht, thu dung dch
ny v thm 0.1 mL K2Cr2O7 1%, nh mc thnh 25 mL hay 50 mL. Dung dch ny dng xc
nh Hg bng phng php ph hp thu nguyn t ha hi lnh.
- Cch ny c th c dng th x l cc loi mu t , qung, rc thi rn, bn,ct...
xc nh Hg hay Ga hay cc hp cht c kim d bay hi.
2.4.9. K thut chlor ha mu.
2.4.9.1. Nguyn tc: Nguyn tc ca k thut ny l sc mt dng kh chlorine qua mu un nng.
Mu thng c nghin nh dng nh ha trong nc hay acid long. nhit v p sut thch
hp, cc kim loi trong mu s tng tc vi kh chlorine v chuyn v cc mui chloride tan trong
dung dch. Ha tan mu vo acid long tch cc cht phn tch dng mun tan.
2.4.9.2. Trang b, cch tin hnh v v d
H thng chlor ha mu gm cc b phn
- Bung cha mu chlor ha
- H iu ch kh chlorine, h thng iu khin tc v dn kh chlorine mi sinh vo
bung cha mu
- H thng ha tan mui thu c sau khi chlor ha
- H thng iu khin nhit cho bnh mu v b ngng t hi mu thng hoa
V d: Chlor ha qung t him ly cc nguyn t t him trng thi mui chloride
tan trong dung dch nc. Ly 5 g mu nghin nh vo bnh chlor ha, thm 50 mL nc ct, lc
u, acid ha n pH 1 bng HCl 5%, lc k, un si hn hp, t trn ni cch thy hay bp iu
nhit, dn kh chlor mi sinh vi tc 0.8 mL/pht vo bnh mu. Duy tr phn ng trong 30 pht,
ngui, thm 10 mL HCl 10%, un si v lc ly dung dch mu. y l dung dch cha mui
chloride cc nguyn t t him c trong qung.
2.4.10. Kt ta hay ha lng nhit thp
2.4.10.1. Nguyn tc chung: chn iu kin thch hp v trong mt dung mi kt ta phn on
cht phn tch di dng mt hp cht khng tan, sau tch chng ta khi hn hp mu v x l
kt ta theo cch ph hp vi phng php phn tch la chn. Phng php ny gip tch ng
thi cng lm giu cht phn tch.

2.4.10.2. Cch tin hnh

- V d 1: kt tinh ly cc halides t mi trng khng kh. Dung dch AgNO3/HNO3 lm
lnh n 10oC c s dng hp thu cht phn tch di dng cc kt ta AgX. Mu khng kh
c bm sc qua dung dch hp thu tc 1-2 L/pht n khi c 250 L khng kh. Ly tm ly
kt ta xc nh halides theo cc phng php bit.
- V d 2: tch v lm giu xc nh mt s kim loi nng trong mu nc. Ly 250 mL
mu nc vo bnh kt ta, chnh pH =2 bng HCl 5%, lc b cn nu c, c cn cn 100 mL, thm
0.5 g NH4NO3, 1 mL FeCl3, lc u cho tan ht, un si, cho kh H 2S sc vo vi tc 3 bng kh/
giy trong 20 pht, khuy u dung dch khi sc kh, ngui n nhit phng, khuy mnh v
t cc trong chu nc 5 pht, lc kt ta sulfide qua giy lc bng xanh, ra kt ta 2 ln bng
20 mL NH4NO3 0.1% pH= 6. Ly kt ta ha tan trong HNO3 45% nng, un cho tan ht v lm
bay hi ht acid n cn mui m. nh mc n 25 mL bng HCl 2%. Dung dch ny c th dng
xc nh kim loi nng bng phng php trc quang, AAS hay AES.
- V d 3: H nhit kt tinh cc cht phn tch hu c. Ni chung cc cht hu c
trong iu kin thng nu tn ti trng thi kh th c th dng c phng php ny. V d nh
kh methane, ethane, propane, butane... Phng php ny ch yu dng trong cng ngh m t dng
trong phng th nghim v cc h trang thit b kh t tin.
2.4.11. K thut in phn
2.4.11.1. Nguyn tc v c im: Trong mt bnh in phn, nu p mt in th 1 chiu nht nh
ln hai in cc, nhiu cht, ch yu l cc ion kim loi s chy vo in cc m, nhn in t
tr thnh nguyn t trung ha v bm ln b mt in cc. C th dng phng php khi lng
xc nh cc cht bm trn in cc hay ha tan cht trn in cc ri xc nh n bng phng
php ph hp. Mt trong cc phng php loi ny l phng php Volt-Ampere ha tan.
Cc c im:
- Tch c cht phn tch ra khi hn hp mu
- Lm giu c cht phn tch t mu c nng rt long, khng th xc nh trc tip
- Cn phn b h trang thit b in phn v phng php ny ch gii hn cho mt s ion
kim loi trong mu mi trng dung dch nc.
2.4.11.2. Cc trang thit b, cch thc hin v v d
H thit b in phn bao gm
- Bnh in phn v h in cc (anode v cathode). in cc m (cathode) in phn
cho cc kim loi kt ta ln thng l cc in cc dng li hay thanh dp, c lm t cc in
cc tr v bn ha hc nh Pt, Au, Pd, W...
- Ngun cp th mt chiu c th iu chnh c theo yu cu in phn ca mi cht
in phn khc nhau.
- H thng iu khin v kim tra qu trnh in phn.
- V d: in phn tch Cu khi dung dch trong mu nc khong. in phn, ngi
ta dng in cc m bng mnh hay li bng Pt. Qu trnh in phn c thc hin vi ion
Cu(II) trong mi trng acid HCl long (0.2M) th mt chiu -0.5V. Sau ha tan kim loi Cu
kt ta trn cc Pt bng HNO3 long. Xc nh Cu theo cc phng php bit ty theo hm
lng ca n.
2.4.12. Cc phng php sc k
Sc k l mt loi phng php tch xc nh ng thi cc cht trong mt hn hp v
n cng l mt phng php x l mu tt cho nhiu trng hp tch ly cc cht cn phn tch.
Trong ng dng x l mu ch yu l sc k ct v sc k bn mng.
2.4.12.1. Phng php sc k ct
a. Nguyn tc v iu kin

Nguyn tc: Phng php x l mu ny da trn c s tnh cht hp ph hay phn b hay trao i
ca cc cht lu gi cht phn tch ln pha tnh trong ct sc k, tch chng ra khi mu
ban u. Sau dng mt dung mi thch hp (pha ng) ra gii v ha tan chng vo pha
ng tch n ra khi ct sc k ri xc nh chng trong pha ng ny bng mt phng php
ph hp. V d nh AES, AAS, UV-VIS, HPLC, GC, EC...V th trc ht phi a mu phn tch
v dng dung dch c th np vo ct sc k. S tch sc k y l da trn hai pha khng trn
vo nhau, pha tnh l cht rn, pha ng l cht lng (dung mi ra gii). V th n cng tng t
nh k thut chit pha rn. Ch yu y l sc k hp ph dng pha tnh l silicagel hay
aluminium oxide xp c tnh cht sc k tch cc nhm cht.
iu kin:
- Chn pha tnh c tnh cht chn lc cho mt nhm cht phn tch
- Chn pha ng ph hp cho cht cn x l thu c n tt nht
- Cn bng trong qu trnh sc k phi c tnh chn lc tt
- Chn iu kin sc k thch hp gp c cht phn tch vo mt nhm hay tch
tng cht th cng tt.
b. Trang b, cch x l v v d
Mun thc hin chit kiu ny chng ta phi c cc h sc k ph hp. C th ch l cc ct
tch n gin, v cng c th l cc h thng t ng hon chnh. N bao gm trc ht l ct sc
k cha pha tnh nh silicagel hay aluminium oxide xp c kh nng hp ph hay trao i ion vi
mt hay mt nhm cht phn tch. Th hai l cc dung mi ha tan mu phn tch v dung mi
ra gii cht phn tch ra khi ct sc k. Ty loi cht phn tch m chng ta c th chn h pha
sc k hp ph hay h pha trao i ion tch cht phn tch.
- V d 1: X l mu xc nh cc alkaloid. Ha tan mu v chuyn mu v dng lng
trong mt dung mi hu c thch hp, v d nh n-hexane hay acetonitril... Sau ly c dung dch
ny hay ch 1 th tch nh nht nh np vo ct sc k hp ph c pha tnh l aluminium oxide vi
tc chy 1 mL/pht cht phn tch c pha tnh hp ph v gi li. Sau dng n-hexane
hay hn hp n-hexane+DCM, t l 1:1, ra gii cht phn tch ra khi ct sc k vi tc 1.5
mL/pht. Nh vy cht phn tch s c ra gii v tan vo pha ng ra gii, v tin hnh xc
nh n trong pha ng ra gii ny bng mt trong cc phng php nh HPLC, GC, CEC...
- V d 2: X l mu xc nh cc chlorophenol trong mu t. Ha tan v chuyn mu
v dng lng trong mt dung mi thch hp v d THF, lc ly dung dch THF, lm kh bng mui
Na2SO4 khan. Ly dung dch hu c ny np vo ct sc k hp ph c pha tnh l pha ngc C 18
vi tc chy l 1 mL/pht cht phn tch c pha tnh lu gi. Sau dng 10 mL pha ng
(ACN-THF) ra gii cht phn tch ra khi ct sc k vi tc chy l 1.5 mL/pht. Nh vy
cht phn tch s tan vo pha ng ny v xc nh n trong pha ng thu c bg mt trong cc
phng php nh HPLC, GC, CEC...
- V d 3: X l mu xc nh lng vt kim loi nng trong nc bin. Ly 250 mL
mu, chnh pH =5, lc b cn, sau np ln ct sc k trao i loi DOWEX-50X12-Na (150 x
8mm) vi tc chy 1 mL/pht cc ion kim loi c gi li trn ct sc k. Khi mu chy ht,
di qua ct 5 mL nc ct hai ln. Sau dng 20 mL dung dch HNO 3 3M ra gii cht phn
tch ra khi ct sc k vi tc 1.5 mL/pht. Nh vy cht phn tch s tan vo dung mi ra gii
v c th c xc nh bng phng php phn tch ph hp nh AAS, AES, UV-VIS. Cch ny
c th dng cch x l mu cho vic xc nh cc kim loi trong cc loi nc mt, nc thi...
- V d 4: X l mu xc nh mt s anion trong mu nc (halides, nitrate, sulfate...).
Ly 250 mL mu, chnh pH =7.5-8, lc b cn, sau np ln ct sc k trao i loi DOWEX50A12-OH (150 x 8mm) vi tc chy 1 mL/pht cc ion kim loi c gi li trn ct sc k.
Khi mu chy ht, di qua ct 5 mL nc ct hai ln. Sau dng 20 mL dung dch NaOH 1M

ra gii cht phn tch ra khi ct sc k vi tc 1.5 mL/pht. Nh vy cht phn tch s tan vo
dung mi ra gii v c th c xc nh bng phng php phn tch ph hp UV-VIS hay sc k
ion.... Cch ny c th dng cch x l mu cho vic xc nh cc kim loi trong cc loi nc mt,
nc thi...
2.4.12.2. Sc k giy v sc k bn mng
a. Nguyn tc chung: qu trnh sc k y l da trn c s l trong h dung mi nht nh
th s phn b hp ph ca cc cht trn nn silicagel xp c trng trn bn thy tinh hay
polymer cng hay s hp ph ca cc cht trn bn giy xp sc k khc nhau. Trong qu
trnh sc k, cc cht s di chuyn khc nhau to ra mi cht c mt vng ring trn bn
mng v tch ra khi nhau. V th mi c tn l sc k bn mng v sc k giy.
b. Cc trang b, cch tin hnh v v d
Mun thc hin tch chit theo kiu ny chng ta phi c cc trang b sc k. N bao gm:
- Cc loi bn mng sc k l cc cht silicagel hay aluminium oxide xp c kh nng hp
ph cc cht phn tch.
- Cc h dung mi ha tan mu phn tch
- Cc bnh chy sc k v dung mi chy sc k
- Pha ng chy sc k
Ty loi cht phn tch, m chng ta c th chn h pha sc k giy hay sc k bn mng.
Bn mng hay giy sau khi chm ln c lm kh v ngm vo dung mi trong bnh sc k. Lc
ny cc cht phn tch s chy theo dung mi t di ln trn v to thnh tng vng cht. Sau khi
chy sc k, tch cc vng mu xc nh cc cht hay xc nh bng cc phng php ph phn
t (hp thu hay phn x).
- V d 1: tch mt s alkaloid t c bnh vi bng sc k bn mng. Ly 10 g mu
nghin mn v bnh nn, thm 20-25 g Na 2SO4 khan, thm 40 mL n-hexane, lc mnh 10 pht,
lng, lc hng ly dung dch. Lm bay hi dung mi bng dng kh nitrogen sch cho n khi cn
b m. Ha tan b ny trong 2 mL DCM v ly dung dch mu ny chy sc k bn mng (loi MA450) trong h dung mi A (30% n-hexane+10%THF+10%DCM+pH=6) tch ly cc alkaloid,
sau ly bn mng, tch ly vng cht, ha tan n trong mt dung mi thch hp nh DCM v xc
nh chng. Hay h dung mi khc thch hp.
- V d 2: Tch ly hp cht carotene t mu rau qu bng sc k bn mng. Ly 10 g
mu nghin nh v bnh chit, thm 25 g Na2SO4 khan, 40 mL THF, lc chit 10 pht, lc ly
dung dch THF, ct quay chn khng cho n cn b, ha tan b ny trong 5 mL n-hexane. Ly
dung dch mu ny chy sc k lp mng trn bn silica (loi Si-MA 560).

S chung phn tch kim loi

Ly mu

Nghin trn
Cn a g

Bng phng
php Kendan,
l vi sng

X l
Phn hy
V c ha t

thm acid

Lm bay hi acid d

C th chit lm giu,
tch nhm trc khi phn tch

nh mc, thm ph gia

Phn tch

AES
AAS

UV VIS

HPLC
Ion CA

ECA

c th thm cc
cht cn thit

Ly mu

Nghin trn
Cn a g
X l
Phn hy
V c ha kh
Ha tan tro b trong acid

c th thm
cht bo v

Lm bay hi acid d

C th chit lm giu,
tch nhm trc khi phn tch

nh mc, thm ph gia

Phn tch

AES
AAS

UV VIS

HPLC
Ion CA

ECA

c th thm cc
cht cn thit

Ly mu

ng nht, trn u
Ly V mL
C th lc b cn
X l mu bng
- Cc cch chit tch
- Chng ct
- Sc k
- C c
....

C th chit lm giu,
tch nhm trc khi phn tch

nh mc, thm ph gia

Phn tch

AES
AAS

UV VIS

HPLC
Ion CA

ECA

c th thm cc
cht cn thit

Ly mu

Nghin, trn u
Cn a g
Nh ha, ha tan bng
dung mi ph hp
X l mu bng
- Cc cch chit tch
- Chng ct
- Sc k
- C c
....

C th chit lm giu,
tch nhm trc khi phn tch

nh mc, thm ph gia

Phn tch

UV VIS
HPLC
GC

GCMS
HVCEC

Fluorescen ce

c th thm cc
cht cn thit

So snh kt qu tro ha t v kh
Ng
CX Cch tro ha
t
Pb
10
t:
HNO3+HClO4
HNO3+HClO4+H2SO4
HNO3+H2SO4
Kh

Ph gia bo v

Khng
H2SO4
HNO3
Mg(NO3)2
Mg(OAc)2

Hg

Zn

As

Cu

10

10

10

10

t:
HNO3+HClO4
HNO3+HClO4+H2SO4
HNO3+H2SO4+K2Cr2O7
Kh
t:
HNO3+HClO4
HNO3+HClO4+H2SO4
HNO3+H2SO4
Kh

t:
HNO3+HClO4
HNO3+HClO4+H2SO4
HNO3+H2SO4
Kh

t:
HNO3+HClO4
HNO3+HClO4+H2SO4
HNO3+H2SO4
Kh

Khng

Khng
HNO3
H2SO4
Mg(NO3)2

Khng
HNO3
H2SO4
Mg(NO3)2

Khng
HNO3
H2SO4
Mg(NO3)2

Nhit
(oC)

Recovery
(%)

450
550
650
450
550
650
450
550
650
450
550
650
450
550
650

97-100
93-98
90-94
97-100
93-95
71-83
97-99
95-97
90-96
97-99
97-99
70-84
98-99
92-95
91-96
97-98
95-98
92-94

450
550

78-80
90-94
92-94
0
0

550
550
550
550

97-100
94-102
96-100
87-96
93-97
97-100
98-99

550
550
550
550

96-98
97-99
91-98
80-88
80-84
90-96
92-99

550
550
550
550

99-100
99-101
99-100
86-92
94-96
95-97
97-99

Co

Cd

Sb

Cr

Fe

Au

10

10

10

10

10

10

t:
HNO3+HClO4
HNO3+HClO4+H2SO4
HNO3+H2SO4
Kh

t:
HNO3+HClO4
HNO3+HClO4+H2SO4
HNO3+H2SO4
Kh

t:
HNO3+HClO4
HNO3+HClO4+H2SO4
HNO3+H2SO4
Kh

t:
HNO3+HClO4
HNO3+HClO4+H2SO4
HNO3+H2SO4
Kh

t:
HNO3+HClO4
HNO3+HClO4+H2SO4
HNO3+H2SO4
Kh

t:
HNO3+HClO4
HNO3+HClO4+H2SO4
HNO3+H2SO4
Kh

Khng
HNO3
H2SO4
Mg(NO3)2

Khng
HNO3
H2SO4
Mg(NO3)2

Khng
HNO3
H2SO4
Mg(NO3)2

Khng
HNO3
H2SO4
Mg(NO3)2

Khng
HNO3
H2SO4
Mg(NO3)2

Khng
HNO3
H2SO4
Mg(NO3)2

550
550
550
550

98-100
98-100
97-99
97-99
90-96
96-99
97-100

550
550
550
550

98-100
98-100
97-100
86-94
82-91
93-97
94-97

550
550
550
550

94-98
95-98
97-99
90-94
92-96
94-98
96-97

550
550
550
550

97-100
98-100
98-100
94-98
95-98
97-99
95-98

550
550
550
550

96-100
98-100
97-100
94-98
96-99
97-100
98-100

550
550
550
550

95-98
97-99
97-99
93-99
87-98
97-99
97-100

Phn loi v s chit pha rn, SPE

Khi lng Cht mu tan
M
M<1000

phn cc C ch Pha tnh

ca
cht SPE
phn tch
Tan trong dung Phn cc
NPC
Diol (COHCOH)
mi hu c
Cyano (CN)
Amino (NH2)
Amino (NH2/NH)
Phn
cc LSC
Silicagel
trung
trung bnh
tnh

Ion

Tan
trong
nc

Khng phn RPC

cc

Silica-C8
Silica-C18
Silica-phenyl
Silica-CN

Cation

IEC

Anion

IEC

Silica-SO3H
Silica-COOH
Silica-RCOOH
Silica-NH2
Silica-C6H5SO3H
Silica-NH2, -NH
Amin t cp
Silica-diol
Silica-CN
Silica-NH2
....
Silicagel
trung
tnh

Khng Phn cc
ion

NPC

Phn
cc LSC
trung bnh
Khng phn RPC
cc
Vt ion kim Tan trong nc
loi

IEC

Silica-C8
Silica-C18
Silica-phenyl
Silica-CN
Silica-SO3H
Silica-COOH
Silica-C6H5SO3H

Dung mi ra
gii cht phn
tch
n-hexane
CHCl3
Aceton
Methanol
n-hexane
CHCl3
Ethylacetate
Methanol
Nc
Methanol
Aceton
Acetonitril
n-hexane
m
Phosphate
Acetate
Amoni
Acid long
Baz long
CHCl3
n-hexane
Aceton
Methanol
Nc
Methanol
Acetonitril
THF...

m
Acid long
Baz long

Chung III. X l mu xc nh kim loi v kim

3.1. X l mu v c xc nh kim loi v kim
3.1.1. Khi nim v mu, v cc loi mu v c
3.1.2. X l mu ly cc ion kim loi d tiu (di ng, trao i)
3.1.3. X l mu ly tng cc ion kim loi
3.1.3.1. K thut x l mu t (v c ha t)
3.1.3.2. K thut nung chy s b trc khi ha tan
3.1.3.3. K thut luc mu trong hp kn
3.1.3.4. K thut x l mu trong l vi sng
3.1.3.5. K thut chit lng lng thng thng
3.1.3.6. K thut chit pha rn tch cht phn tch
3.1.3.7. K thut ngm chit trong acid long ly kim loi
3.1.3.8. K thut in phn
3.1.3.9. Phn tch kim loi trong b thi cng nghip v c
3.2. X l mu hu c xc nh kim loi v kim
3.2.1. Khi nim v mu hu c
3.2.2. Cc cch x l mu v v d
3.2.2.1. K thut tro ha kh
3.2.2.2. K thut tro ha t
3.2.2.3. K thut tro ha kh-t kt hp
3.2.2.4. K thut tro ha t trong hp kn
3.2.2.5. K thut x l t trong l vi sng
3.2.2.6. K thut ln men mu
3.2.2.7. K thut ngm chit trong acid long
3.2.2.8. K thut pha long bng dung mi thch hp
3.3. X l mu xc nh anion v mt s kim
3.3.1. Nguyn tc chung
3.3.2. Cc phng php v v d
3.3.2.1. K thut v c ha t dng acid c oxyha mnh
3.3.2.2. K thut v c ha kh vi kim v cht oxyha mnh
3.3.2.3. K thut chng ct
3.3.2.4. K thut chit thng thng (lng-lng)
3.3.2.5. K thut chit pha rn ly cc anion
3.3.2.6. K thut kt ta tch cht phn tch
3.3.2.7. Phng php thng hoa.

Chng III. X L MU XC NH KIM LOI V KIM

3.1. X l mu v c xc nh kim loi v kim
3.1.1. Khi nim v mu, v cc loi mu v c
Mu v c l cc loi mu trn nn (matrix) ca cc cht v c, n bao gm cc loi
- Kim loi, sn phm cc kim loi nh hp kim, thp...
- Cc loi nguyn liu ca cng ngh v c (luyn kim, xi mng, thy tinh, xy dng, gm
s...).
- Cc loi, mui, oxid, cc hp cht v c.
- Cc loi qung khong, t ...
- Cc loi nc (nc khong, nc thin nhin, nc ngm, sng, h, ao...)
- Cc loi cht thi cng nghip gang thp, in, xi mng, ha cht...
- ....
- Vic x l mu theo cch no l ty thuc vo mc ch phn tch cc cht c th trong loi
mu . Ni chung c th theo cc hng sau:
+ Xc nh ion kim loi di ng (d tiu)
+ Xc nh hm lung tng s mi nguyn t kim loi trong mu.
+ Xc nh cc anion hay kim.
+ Xc nh mt s cht hu c.
Sau y l mt s k thut x l mu uc s dng i vi cc mu v c xc nh cc
kim loi hay mt s anion ( kim).
3.1.2. X l mu ly cc ion kim loi d tiu (di ng, trao i)
A. Nguyn tc chung
Kim loi d tiu l cc ion kim loi d dng trao i trong iu kin bnh thng. Ch nhng
ion dng ny mi uc cy c (trong nng nghip), ng vt (trong y hc: Fe, Cu, Zn trong huyt
tng) c th hp thu c. Nguyn tc ca vic chun b mu y l:
- Xay hay nghin chuyn mu v dng bt hay huyn ph hay ht nh, mn, trn u.
- Dng mt dung mi thch hp (gi l dung dch chit) nh nc hay dung mi hu c hay
dung dch mui kim loi kim hay acid long chit cc nguyn t phn tch (ion di
ng, d tan) vo dung dch sau xc nh cc nguyn t ny trong dch chit bng mt
phng php thch hp.
- Cc dung dch chit thng dng l:
+ Nc ct pH 5 ly cc kim loi d trao i.
+ Dung dch mui: NH4OAc, NH4Cl, KCl, KNO3, 0.5-1M.
+ Dung dch acid long: CH3COOH, H2C2O4 0.05M.
+ Dung dch kim long: NaOH, NH4OH 0.01M
+ Hn hp: (NH4OAc + AcOH) 0.05M.
B. Cc trang thit b
- Cc bnh chit h h, ng nghim
- Cc bnh chit h kn, h thng chit siu m
3.1.3. X l mu ly tng cc ion kim loi
3.1.3.1. K thut x l mu t (v c ha t)
3.1.3.2. K thut nung chy s b trc khi ha tan
3.1.3.3. K thut luc mu trong hp kn
3.1.3.4. K thut x l mu trong l vi sng
3.1.3.5. K thut chit lng lng thng thng
3.1.3.6. K thut chit pha rn tch cht phn tch
3.1.3.7. K thut ngm chit trong acid long ly kim loi
3.1.3.8. K thut in phn
3.1.3.9. Phn tch kim loi trong b thi cng nghip v c
3.2. X l mu hu c xc nh kim loi v kim

3.2.1. Khi nim v mu hu c

3.2.2. Cc cch x l mu v v d
3.2.2.1. K thut tro ha kh
3.2.2.2. K thut tro ha t
3.2.2.3. K thut tro ha kh-t kt hp
3.2.2.4. K thut tro ha t trong hp kn
3.2.2.5. K thut x l t trong l vi sng
3.2.2.6. K thut ln men mu
3.2.2.7. K thut ngm chit trong acid long
3.2.2.8. K thut pha long bng dung mi thch hp
3.3. X l mu xc nh anion v mt s kim
3.3.1. Nguyn tc chung
3.3.2. Cc phng php v v d
3.3.2.1. K thut v c ha t dng acid c oxyha mnh
3.3.2.2. K thut v c ha kh vi kim v cht oxyha mnh
3.3.2.3. K thut chng ct
3.3.2.4. K thut chit thng thng (lng-lng)
3.3.2.5. K thut chit pha rn ly cc anion
3.3.2.6. K thut kt ta tch cht phn tch
3.3.2.7. Phng php thng hoa.
Trang 4
D.Vi v d ng dng.
+ V d 1: Phn tch t nng nghip. Chit cc ion kim loi di ng. Dng dung dch mui
NH4Ac 1M, pH=4.7 chit cc ion K, Na, Cu,Zntrong t trng trtv sau xcnh bng
phng php AES hay AAS. Ly 10g mu t nghin nh vo bnh chit thm 100mL dung dch
chit, lc chit 10 pht, yn 5 pht gn hay ly tm ly dch chit xc nh cc kim loi ni
trn.
+ V d 2: Phn tch t nng nghip. Chit cc ion kim loi di ng. Dng dung dch chit
(HCl 0.05 M+ H2SO4 0.025M) chit cc ion K, Na, Ca, Cu, Mg, Cd, Zn,Fe, Mn,Pb trong t
trng trtv sau xcnh bng phng php AES hay AAS. Ly 10g mu t nghin nh vo
bnh chit thm 100mL dung dch chit, lc chit 10 pht, yn 5 pht gn hay ly tm ly dch
chit xc nh cc kim loi ni trn.
+V d 3: Phn tch phn bn v c. Chit cc ion kim loi di ng. Dng dung dch mui
NH4Ac 1M, pH=4.7 chit cc nguyn t Cd, Co, Cu, Fe, Mn, Pb, Zn sau xcnh bng
phng php AAS. Ly 10g mu t nghin nh vo bnh chit thm 100mL dung dch chit, lc
chit 10 pht, yn 5 pht gn hay ly tm ly dch chit xc nh cc nguyn t kim loi ni
trn.
+ V d 4: xc nh hmLng ion cl d tiu trong t. Chit ly anion Cl: Ly 10g mu t
nghin nh vo bnh chit thm 100mL dung dch chit, lc chit 10 pht, yn 5 pht gn hay
ly tm ly dch chit. C th dng cc dung dch chit sau y:
- (NH4Ac 1M + H2SO4 0.025M) hay(NH4NO3 1M + H2SO4 0.025M).
T l mu/ dd chit = 1/10 (g/V).
3.1.3 X l mu ly hm lyng tng ca mi kim loi.
Yu cu y l phi ly c ht cc nguyn t cn phn tch c trong mu bt k dng
no vo dung dch sau xc nh hm lng ca n theo mt phng php thch hp no

chn. Do vi ccloi mu rn, c, trc tin mu phi c gia cng hay chun b s b theo
cc cch sau ty thuc vo mi loi mu:
- Chuyn mu v dng bt (mu mui, oxt, qung, t , x than..)
- Chuyn mu thnh phi bo (mu thp, hp kim..)
- X l chuyn mu thnh dng huyn ph, bt nho (sinh hc, rau qu..).
- Dng lng ng u (mu nc cc loi hay du).
Sau y l mt vi v d ng dng cck thut nu chng 2 x l mu ly cc kim
loi xc nh chng:
3.1.3.1 K thut x l t (v c ho t)
y l k thut dng cc acid mnh, c hay hn hp ca cc acid mnh c tnh cht cxi ha
mnh,hoc dung dch kim c ha tan, phn hy mu, nhit phng hay khi un si trong
bnh kendan, hay chng ct hi lu. Nh vy mu phn hy y nh c acid mnh v nhit
thch hp. Nhit si y l nhit ca acid dng x l mu. V th nu cn c nhit si
cao th dng acid c nhit si cao nh acid H 2SO4. Nhit si ph thuc vo bn cht ca acid.
V d acid HCl c nhit 115 oC V th ty yu cu ca mu m chn acid no hay thnh phn hn
hp no t c nhit si ca hn hp phn hy musao ph hp.
Trc khi x l cc mu qung, t cn nghin thnh bt. Cc mu kim loihp kim
cn phay thnh phoi bo mng, cc mu sinh hc, rau qu phi thi nh hay xay nhuyn v dng bt
nho ng nht. Sau c th s dng 1 acid c hay cc loi hn hp sau y phn hy mu.
V d:
- Dng 1 acid mnh nh: HNO3, H2SO4, HCl..
- Dng nc cng thy (HCl+ HNO3) v hn hp 2 acid c tnh oxi ha mnh nh HNO 3 +
H2SO4), (HClO4+ H2SO4 )..
- Dng hn hp 3 acid mnh
- Dng mt acid mnh v 1 peroxid (HNO3+H2O2)
- Dng dung dch kim mnh nh: NaOH 20%, KOH 20%.
- Dng hn hp acid v cht to phc (HCl + tartaric cho Sb)
Sau y l mt vi v d x l mu xc nh mt s kim loi nh Cd, Co, Fe, Mn,Ni,Pb,
Zn.
V d 1: Phn hy hp kim nhm: ly 1,000g mu (dng phi bo) vo bnh kendan, thm
0,5mL nc ct, lc u thm 20mL HNO3 1/1, lc u cm vo bnh mt phu nh, un nh cho
mu phn hy n khi no trong l c. Chuyn ton b mu vo cc un, lm bay hi nh
ui ht acid ra cn li mui m. nh mc thnh 25mL bng acid HCl 2%.
V d 2: Phn hy qung t him nhm nh: ly 2g qung dng bt vo bnh kendan, thm
1,0mL nc ct, lc u thm 40mL nc cng thy, lc u cm vo bnh mt phu nh, un nh
cho mu phn hy n khi no trong l c. Chuyn ton b mu vo cc un, lm bay hi nh
ui ht acid ra cn li mui m. nh mc thnh 25mL bng acid HCl 2%.
V d 3: Phn hy qung st: ly 1g qung dng bt vo bnh kendan, thm 1mL nc ct,
lc u thm 20mL nc cng thy, lc u cm vo bnh mt phu nh, un nh cho mu phn
hy n khi no trong l c. Chuyn ton b mu vo cc un, lm bay hi nh ui ht
acid ra cn li mui m. nh mc thnh 25mL bng acid HCl 2%. y l dung dch mu xc
nh cc nguyn t trong qung st v xc nh c st.
V d 4: Phn hy qung Mangan: ly 1g qung dng bt vo bnh kendan, thm 1mL nc
ct, lc u thm 20mL HNO3 65%, 4mL H2O2 15%, lc u cm vo bnh mt phu nh, un nh
cho mu phn hy n khi no trong l c. Chuyn ton b mu vo cc un, lm bay hi nh

 ui ht acid ra cn li mui m. nh mc thnh 25mL bng acid HCl 2% hay HNO 3 2% y

l dung dch mu xc nh cc nguyn t trong qung Mn v xc nh c Mn
V d 5: Phn hy b thi rn thnh ph: ly 5g mu dng bt vo bnh kendan, thm 2mL
nc ct, lc u thm 50mL HNO3 65%, 5mL dung dch H2SO4 98%, lc u cm vo bnh mt
phu nh, un nh cho mu phn hy n khi no trong l c. Chuyn ton b mu vo cc un,
lm bay hi nh ui ht acid ra cn li mui m. nh mc thnh 25mL bng acid HCl 2%
hay HNO3 2%. Nu dung dch c cn th phi lc qua giy mn, hay ly tm ly phn dung dch
trong. y l dung dch mu xc nh cc nguyn t kim loi nng trong rc thi
V d 6: Phn tch t trng trt. Xcnh hm lng ton phn ca cc ion kim loi (Na, K,
Ca, Mg, Cd, Cu, Fe, Mn, Mo, Pb, Zn) trong t. Cn ly 2,000g t c sy kh trong khng
kh v nghin mn vo chn Pt hay chn thch anh. Tm t bng 1mL nc ct thm 20mL acid
HCl 1/1(18%) lc mnh v un si cho mu phn hy trong vng 45 pht. Lc ly phn dung dch
(dd 1), chuyn phn b cn li sang chn Pt, thm 2mL HCl 35%, 5mL H 2SO4 98% v 8mL HF sau
un cch ct cho mu si v bc khi. n khi xut hin khi trng SO 2. Li thm 8mL c na
v tip tc bc khi v cho n khi cn b gn kh (mui m) l c. ngui ha tan b ny
bng 10mL HCl 18%, un nh cho tan. Gp ton b dung dch ny vo dung dch 1 trn v
chuyn sang cc, un si u v lm bay hi cho n khi cn mui m. Sau nh mc mui ny
thnh 50mL bng dung dch HCl 2%. y chnh l dung dch mu xcnh cc kim loi ni trn.
V d 7: Xc nh As trong mu qung, t bng hn hp acid mnh (HF+ HClO 4 +
HNO3). Cn 1g mu vo chn Teflon hay Pt, thm t bng vi git nc ct, thm 20mL HNO 3
65%, lcu v yn 20 pht thm 15mL HF 40%, v 5mL HClO 4 (d=1,68), lc u y np chn,
un nh chng 25 pht, m np chn ra, sau un tip ui HF v HNO 3 n khi xut hin
khi trng dy c th dng. ly mu pha long bng 50mL nc ct, thm 5mL H2SO4 45% kt
ta tch Pb. Lc qua giy bng xanh, ra kt ta bng 10mL nc ct,thu ly nc lc v nc ra
vo cc un 250mL, thm 4mL LaCl3 5%, thm tng git NH4OH 25% n pH=10, khuy k,
yn khong 30 pht, sau lc qua giy bng ly kt ta (trong c As), ra kt ta 2 ln
bng 10 mL ncct m. Ly kt ta ha tan bng 20mL acid HCl 36% v ra sch giy lc bng
HCl 15 (tng dung dch<50mL) thm 8-10 mL dung dch KI 20%, 30mL HCl 36%, 40 mL acid
tartric% (nu mu c Sb), nh mc thnh 100mL, yn 20 pht sau em o ph xcnh A
trong dung dch ny.Cch ny cng c s dng x l ccmu rc thi rn, bn, b thi rn
nng nghip xcnh As, khi hm lng Si> 10%.
Cc v d t s 1-5 v 7 u c th x l trong l vi sng h kn c, lc ny lng acid
ch cn 1/3 l v thi gian x l ch cn 1h l xong, nhng mu li c phn hy trit hn,
v khng b mt cc cht (cc kim loi) d b bay hi.
3.1.3.2 K thut nung chy s b trc khi ha tan.
Nhiu loi mu c cu trc rt bn vng, khng phn hy c bng bt k dung dch acid
no, hoc cho hiu sut rt km. Nn phi x l nung s b trc, ct l ph v cu trc bn ban
u ca mu, cho vic vic x l hay phn hy tip c d dng v hon ton. Nguyn tc l
ly mt lng mu a gam nht nh vo chn nung (v d a=2 hay 5 gam ty theo yu cu phn
tch). Nung mu mt nhit thch hp(450-700o C, ty loi mu), vi cc cht ph gia hay cht
chy ph hp, ph v cc cu trc mng tinh th ca cc cht mu chuyn chng sang dng c
cu trc d ho tan hn.Sau ha tan b thu c sau khi un trong nc hay acid hay trong dung
dch kim long, ly ht cc cht cn phn tch vo dung dch v xc nh chng theo cch
chn. Chng ta c th:

1.X l khng dng cht ph gia v cht chy. Ch nung mu nhit thchhp ph v cu
trc mng li tinh th ban u, lm cho mu d ho tan. Nhng cch ny thng t hiu qu, ch
c dng cho 1 s trng hpnn t c dng. V d
Qung H: LnCO3 F.xH2O Ln2O3 + H2O + CO2 + HF + Men Om
Qung st: Ferit.xH2O FeO + Fe2O3 + SO2 + H2O + Men Om
Qung Cu: CuS. xH2O CuO + SO2 + H2O + Men Om
2. X l c dng cht ph gia v cht chy: trn mu vi 1 cht chy hay hn hp cht chy, sau
nung mu nhit thch hp. cch ny c dng nhiu cho cho cc loi mu kh phn hy. cc
cht ny c th l:
- loi cht chy acid nh: NaHSO3, NaHCO3, NaH2PO4, pyrosunphate
- Loi cht chy kim nh: Na2CO3, KOH,NaOH, LiBO2, Na2O2, NaNO2
- Lai cht chy hu c nh C6H5SO3Na, SDS..
V d:
Qung H + NaHCO3 Ln2O3 + H2O + CO2 + HF + Men Om
t + LiBO2 + NaHCO3 Men Om + Na2SiO3 + H2O + Na2B2O7
3. Yu t quan trng khi x l theo k thut ny:
Phi chn c cc yu t thch hp sau y:
- Loi cht ph gia hay chy cn dng thch hp
- T l thnh phn gia cht chy v mu
- Nhit x l (nhit nung) thch hp v thi gian sy hay nung x l.
- Thi gian sy hay nung x l.
Sau y l vi v d c th ng dng k thut ny
+ V d 1: Phn hy qung t him nh Pasnesit: Cn ly 2,0 gam mu vo chn nung,
thm 2g Na2S2O7 + 1g NaHSO4, tm t bng 1 mL nc ct, sau em nung bt u t nhit
phng, 80 pht u t 250oC, sau nng ln 650oC v nung trong 50 pht. ngui v ly ra
x l theo phng php v c ha t bng hn hp acid (HNO3 + H2SO4) c hay cng thy theo
nguyn tc nh ni phn trn.
+ V d 2: Phn hy mu t trng trt. xc nh hm lng ton phn ca cc ion kim loi
(Li, Na, K, Ba,Ca, Mg, Cd, Co, Cu, Fe, Mn, Mo, Ni, Pb, V, Zn) trong t. Cn ly 200g, t
c sy kh trong khng kh v nghin mn vo chn Pt hay chn thch anh, thm 2g LiBO 2, 1g
NaHCO3 trn u. em nung 650oC trong 45 pht, ngui, tm t bng nc ct sau x l
theo tro ha t c th bng cc hn hp sau, ty thuc cht cn xc nh:
-

Hn hp HNO3+ H2SO4= (4/1)

Hn hp HNO3+ H2SO4 + HClO4= (4/1/1)
Hn hp cng thy.
Sau chuyn ton b dung dch x l sang cc v lm bay hi n cn mui m. Sau
nh mc mui ny thnh 50mL bng dung dch HCl 2%. y chnh l dung dch mu xc nh
cc kim loi ni trn (v d: Na, K, Ca, Mg, Cd, Cu, Fe, Mn, Mo, Pb, Zn)
+ V d 3: Xc nh As trong mu qung, t . c ly 0,5g mu vo chn Zr hay Pt, thm
3g KOH, 4g Na2O2 trn u, un nh cho mu chy v si ln tn (si bt v c th bn), cho n
kh ri em nung 650oC trong 0,5h, c hn hp ng nht. Ly ra ngui lau sch y

chn, th c chn v mu vo cc c cha 50mL nc si, lc u, y knh ng h v un si cho

mu tan. Ly chn nung ra v trng ra chn bng nc ct (tng th tch < 100mL) b vo dung
dch vi mnh s xp, un si ui ht H 2O2 (20 pht ), ngui loc qua giy lc bng , ra
giy lc 3 ln bng 15mL nc m, b kt ta, ly dung dch thm 40mL HCl 35%, nh mc thnh
100mL. y l dung dch mu xc nh As. Cch ny cng dng c x l cc mu rc thi
rn, bn, b thi rn xc nh As khi hm lng Sl < 10%.
3.1.3.3 K thut luc mu trong hp kn
y thc cht cng l k thut x l t (tro ha t) bng acid, ch c khc l qu trnh
nthc hin phn hy l trong hp kn, nn s c p sut cao v mu s c phn hy nhanh hn.
Cho mu vo 1 hp kn chu acid, chu p sut cao (hnh 3.3) thm cc cht phn hy l acid n
hay hn hp acid c tnh oxy ha mnh. Sau em sy nhit ph hp trong l nung hay luc
trong b nc si, hay luc trong b c nhit si cao, phn hy mu. y chnh l s phn
hy mu trong p sut cao v nhit cao tng theo p sut sinh ra trong bnh khi phn hy mu
(thng n 3 atm), nn qu trnh xy ra nhanh v trit hn, v li tn t acid(thng ch mt
k thut h) N tng t nh trong ni p sut. Tt c cc v d v cch x l t trong mc 3.1.3.1
trn u c th p dng c trong hp kn nhng lng acid ch cn dng bng l .
Qa trnh x l c th thc hin c theo mt trong cc cch sau
- sy bung mu trong t sy c khng ch nhit (80- 250o C)
- Luc bung mu trong b nc si
- Luc bung mu trong b du si (150- 250oC )
- Luc trong xx hay bp cch ct.
- Dng c x l theo kiu ny c ch ra trong trang sau (hnh 3.3 )

HNH 3.3
+ V d 1: Phn hy qung t him nh, ly 2g mu dng bt vo cc Teflon, thm 10mL
cng thyhay hn hp (HNO3 + H2SO4 ) v 1 gam (NH4)2SO4. sau cho cc mu vo hp thp
kn chu p, y nt, vn chy v b hp mu vo t sy 180 oC. ngui chuyn vo cc un,
lm bay hi ht acid n khi cn mui m v nh mc bng dung dch HCl 2% thnh 50mL. l
dung dch xc nh cc nguyn t t him v cc kim loi khc c trong qung ny. Trc ht
tch tng t him dng kt tia mui oxalat, cn c dng xc nh cc nguyn t khc (Na,
K, Ca, Mg, Cu, Fe, Pb, Zn)
+ V d 2: Phn hy mu ha tan qung vng. Ly 2g mu dng bt vo cc Terlon, thm
30mL cng thy, 4mL H2SO4. Sau cho cc mu vo hp thp kn chu p, y nt, vn cht v
b hp mu vo t sy v sy 180oC trong 180 pht. ngui chuyn vo cc un, lm bay hi
ht acid n khi cn mui m v nh mc bng dung dch HCl 2% thnh 50 mL. l dung dch
xc nh Au v cc nguyn t loi khc khc c trong qung ny
+ V d 3: Phn hy mu qung crm. Ly 2g mu dng bt vo cc Teflon, thm 30mL
HNO3 65%, 5mL H2SO4 98%. Sau cho cc mu vo hp thp kn chu p, y nt, vn cht v b
hp mu vo t sy v sy 180 oC trong 180 pht. ngui chuyn vo cc un, lm bay hi ht

acid n khi cn mui m v nh mc bng dung dch HCl 2% thnh 50 mL. l dung dch
xc nh cc nh crm v cc nguyn t kim loi khc c trong qung ny
3.1.3.4 K thut x l mu trong l vi sng.
y cng l k thut x l t dng nng lng cao tn ca l vi sng phn hy t mu
trong mi trng ca 1 acid oxy ha mnh, hay hn hp ca hai hay 3 acid mnh, c v c tnh oxi
ha. N l k thut x l t trong l vi sng di tc dng ca nng lng cao tn nn hiu qu
cao v nhanh hn cch tro ha t bnh thng. C 2 cch ca k thut ny l x l p sut
thng (h m) v p sut cao (h ng kn). Ngy nay nhiu hng cung cp cc h l vi sng rt
tin li chop x l mu phn tch. C cc kiu x l t, x l kh, lm bay hi, chng ct
(xem chng 2).
Tt c cc v d x l t trong mc 3.1.3.1 v v d trong mc 3.1.3.3 v cch x l t
trong hp kn nu trn u c th thc hin trong l vi sng. Nhng acid th cn t hn. C th thc
hin 1 trong 2 cch sau ty theo c iu kin trang b bnh x l mu v h l vi sng.
+ Trong h m: mu trong bnh kendan hay bnh x l mu v t trong l vi sng c
iu khin c cng sut vi sng phn hy trong iu kin chn. Mu c phn hy nh
cc acid mnh v nng lng cao tn ca l vi sng nn s phn hy l nhanh v trit v tn t
acid hn khi x l t bnh thng (xem c ch hnh 3.3b).
V d 1: Phn hy qung t him nh. x l mu qung t him, ly 2g mu dng bt
vo bnh x l, thm 20mL cng thy v 0,5 gam (NH 4)2SO4, lc u. Sau cho bnh mu vo l
vi sng trong 90 pht. ngui chuyn vo cc un, lm bay hi ht acid n khi cn mui m v
nh mc bng dung dch HCl 2% thnh 50mL. l dung dch xc nh cc nguyn t t him
v cc kim loi khc c trong qung ny.
V d 2: Phn hy mu ha tan qung vng. Ly 2g mu dng bt vo cc vo bnh x l
hay ng nghim, thm 20mL cng thy, 0,5 gam (NH 4)2SO4.Sau cho cc mu vo l vi sng
trong 20 pht. ngui chuyn vo cc un, lm bay hi ht acid n khi cn mui m v nh
mc bng dung dch HCl 2% thnh 50 mL. l dung dch xc nh cc nguyn tvng bc v
cc nguyn t khc c trong qung ny
Trong h ng kn: mu phi trong bnh knh v chu p cao. Sau cng phn hy bng
hn hp nh trn. Nhng v h kn p sut cao. Nn s phn hy nhanh v trit hn, v lng
acid cn t hn. cc h thng x l mu theo cch ny hin nay cc hng c cung cp y , t n
gin n hon chnh, c chng trnh iu khin v t ng tt c.
V d 1: phn hy ha tan qung t him nh. x l mu qung t him, ly 2g mu
(dng bt) vo cc Teflon, thm 15mL cng thy, 0.5g. sau cho cc mu vo hp kn, y nt,
vn cht v b hp mu vo l vi sng trong 90 pht. ngui chuyn vo bnh nh mc v nh
mc bng nc ct thnh 50mL. l dung dch xc nh cc nguyn t t him v cc kim
loi khc c trong qung ny.
V d 2: phn hy ha tan qung vng. x l mu qung vng, ly 2g mu cho vo
cc Teflon, thm 25mL nc cn hy, 0.5g. sau cho cc mu vo hp kn, y nt, vn cht, b
mu vo l vi sng trong 60 pht. ngui cho vo bnh nh mc, v nh mc bng nc ct
thnh 50mL (c th chuyn mu ra cc un, lm bay hi,cn mui m, sau ha tan b v nh

mc bng acid HCl 2% th tt hn). l dung dch xc nh vng,bc v cc kim loi khac
trong qung ny
3.1.3.5.K thut chit lng-lng thng thng thng:
Nguyn tc, cc iu kin v trang b ca k thut chit c nu trong chng 2 mu
phn tch c trong dung mi nc, sau dng mt dung mi hu c thch hp chit cht tch
vo pha hu c dng hp cht tan tt trong dung mi hu c. V d chit cc kim loi nng t
m nc thi vo CHCl3 dng phc kim loi Me-APDC. xc nh cc kim loi nng (Cd, Co,
Cr, Cu, Fe, Mn, Ni, Pb, Zn) trong .
Cc trang b ca k thut chit ny l cc bnh chit hay phiu chit khc nhau(hnh 3,4).
N l cc dng c thy tinh ph thng ca phng th nghim nn khng mc tin. Sau y l mt s
v d v chit x l mu phc v phn tch cc cht.
V d 1: chit xc nh cc kim loi nng nng c hi(Cd, Co, Cr,Cu, Fe, Mn, Ni, Pb, Zn...)
trong mu nc thi ly 250mL mu vo cc, acid ha mu n pH=1 lc b cn, chuyn mu vo
phiu chit, thm 2mL thuc th APDC 0.1% trong ru, v 15mL CHCl 3 chit 10 pht yn 5
pht tch ly pha hu c CHCl3 vo phiu chit khc v gii chit cc kim loi bng 20 mL dung
dch HNO3 2.5M. ly dung dich nc gii chit lm bay hi mui m, sau dnh mc thnh 10
mL bng dung dch HCl 1% . y l dung dch xc nh cc nguyn t nu.
V d 2: chit xc dnh cc kim loi nng c hi(Cd, Co, Cr,Cu, Fe, Mn, Ni, Pb, Zn...)
trong mu nc bin. Ly 250mL mu vo cc. Acid ha mu n pH=2, lc b cn, chuyn mu
vo phiu chit. Thm 2 mL thuc th APDC 0.1% v 10 mL MIBK lc chit 10 pht yn 5 pht
tch ly pha hu c MIBK, lp li s chit nh th mt ln na, th 2 ln MIBK vo phiu chit
khc, v gii chit cc kim loi bng 20 mL dung dch HNO3 2.5 M. Ly dung dch nc gii chit
lm bay hi cn mui m, sau dinh mc thnh 10 mL bng dung dch HCl 1% v xc nh cc
nguyn t bng phng php ph F-AAS
V d 3: chit tch xc nh cc kim loi nng(Cd, Co, Cr,Cu, Fe, Mn, Ni, Pb, Zn..) trong
ng vng hay ng th. Ha tan 10 gam dng vo 80 mL nc ct, lc cho tan ht, chnh c
pH=1 bng acid HCl 10% lc b cn (nu c). Chuyn mu vo phiu chit. Thm 2mL dung dch
APDC 0.1%, 10 mL CCl4 lc chit 5 pht, tch ly lp hu c vo cc cha lp li s chit nh th
mt ln na tch ly phn hu c v gp phn dung mi hu c ca c 2 ln chit vo 1 phiu lc
khc. Thm 30 mL HNO3 3M lc gii chit. Tch pha ly phn dung dich nc acid c cha cc
kim loi vo cc 250 mL. un si lm bay hi nc m v nh mc thnh 10 mL bng dung dich
HCl 2% y l mu xc nh cc kim loi trong ng bng phng php F-AAS hay phng
php UV-VIS hay ICP-AES

Hnh

3.1.3.6 Chit pha rn tch cht phn tch:

y l mt loi k thut mi, c nhiu u vit, mi c pht trin t khong 10 nm tr li
y. Hin nay ang c pht trin mnh v ng dng nhiu. Chi tit v k thut ny xem trong
mc 2.4 chng II.

Cch chit ny ch c p dng cho cc cht phn tch tan trong cc mu lng (dung mi
lng ), nh mu nc thi ca nh nc sn xut ru bia, in cng nghip khai thc than, cc loi
nc khong qung cc loi. Cng c th l cc loi cht mu ha tan c trong nc, trong dung
mi hu c, hay dung dch nc ca acid hay baz long. Sau y l mt vi v d ng dng.
V d 1: chit x l mu nc bin ly cc kim loi nng (Cd, Co, Cr,Cu, Fe, Mn, Ni, Pb, Zn....)
Xem v d 2 trong mc 2.4.4, 2.4.2.2 chng 2 (trang ) v v d 1, v d 3 trong mc 2.4.4,
2.4.2.3 chng 2 (trang ).
V d 2: chit x l mu nc xc nh mt vi anion (Halogen, Nitrat, v Sunphat ). Xem v d 2
v 4 trong mc 2.4.4, 2.4.4.2 chng 2 (trang ).
V d 3: Chit x l mu nc xc nh cc cyanua (CN ) xem v d trong mc XX chng 2
(trang )
V d 4: chit tch xc dnh hm lng ion CNS trong nc thi cng nhip thc phm. Ly 250
mL mu vo cc, chnh pH v 3 bng dung dch HCl 5% lc b cn. Ly dung dch trong di qua
ct chit (loi LA-ROH 7m) vi tc 3-4 mL/pht (nh ht p sut thp). Sau khi mu chy ht,
ht kh ct trong 2 pht. Ri ra gii ct chit ly ion CNS bng 10 mL dung dch NaOH 0.5 M.
Thu dung dch ny xc nh CNS.
3.1.3.7 K thut ngm chit mu trong acid long.
Nguyn tc ca k thut ny l xay mu thnh bt, sau ly mt lng nht nh, v ngm
chit trong dung dch acid long (3-5% ). Phng php ny l chit ly cc ion kim loi c trong
mu phn tch, khi mu c ngm trong acid th cc ion kim loi s chuyn vo dung dch, dng
mui tan. V d ngm chit mu bt go trong dung dch acid HCl 5% ly cc kim loi kim v
kim th ra khi bt go v xc nh chng bng phng php ph hp thu nguyn t. Cch chit
ny n gin d lm, khng cn my mc phc tp. Ch cn nghin mu thnh bt, hay th nho,
sau thm acid vo mu v ngm chit qua m.
ngm chit ngi ta thng dng cc dung dch acid long (5-7 % ) trong nc ca acid
HCl, HNO3, hay H2SO4... sau y l vi v d ng dng.
V d 1: Ngm chit tch ly mt s kim loi (Na, K, Cd, Cu, Pb, Zn,....) t bi, chanh hay
cam. Ly 10 gam mu c nghin nh hay xay thnh bt vo bnh nn 250 mL, thm 200 mL
dung dch acid HCl 5% ngm chit. Khuy u un si, ngm chit qua m. Sau lc k 2
pht. V lc ly dung dich chit vo cc 250 mL, un si k. Lm bay hi ti cn mui m. V
nh mc thnh 25 mL bng dung dch HCl 2% (nu c vn c, lc b vn c). y l dung dch
xc nh cc kim loi v c ion nitrat, sulfat.
V d 2: ngm chit tch ly mt s kim loi (Na, K, Cd, Cu, Pb, Zn,....) trong cc rau xu
ho bp ci. Ly 10 gam mu c nghin nh hay xay thnh bt nho vo bnh nn 250 mL,
thm 100mL dung dch acid 5% ngm chit. Khuy u, un si,, lc mnh 1 pht, ngm chit
qua m. Sau lc k 1 pht, v lc ly dung dch chit vo cc 250 mL. un si k,lm bay hi
n cn mui m v nh mc thnh 25mL bng dung dch HCl 2% (nu c vn c th lc b vn
c). y l dung dch xc nh cc kim loi v mt s anion nh NO3-, SO42-.....
3.1.3.8 K thut in phn
................... Ch yu l cc ion dng v m c trong mt in th mt chiu nht nh m
chng c th nhn electron, nu l ion dng hay l cho electron, nu l ion m, tr thnh phn
t trung ha (cc nguyn t v n kt ta bm vo in cc, nh m chng ta tch c cht
phn tch ra khi mu ban u v xc nh chng theo cch chn thch hp.
V d 1: in phn x l mu xc nh ng (Cu) t mu nc thi cng nghip luyn
kim. Ly 200mL mu vo cc, acid ha n pH=2 bng acid H 2SO4 5% lc b cn. Ly dung dch

cho vo bnh in phn (cc m l bn Pt, chnh pH v 0), 10g, thm cht in ly tr (NaCl hay
KCl). in phn cho Cu bm ln in cc Pt th 0.25V trong vng 1 gi. V xc nh hm lng
Cu theo phng php in khi lng.
V d 2: in phn x l mu xc nh ch (Pb) t mu nc thi nh my acquy. Ly
200mL mu cho vo cc, acid ha n pH=1 bng acid H2SO4 5%, lc b cn. Ly dung dch cho
vo bnh in phn (cc m l bn Pt, chnh pH v 0) thm cht in ly tr (LiCl hay CsCl). in
phn cho Pb bm ln in cc Pt th 0.4V trong vng 1 gi. V xc nh hm lng Pb theo
phng php in khi lng.
3.1.3.9 Phn tch kim loi trong b thi cng nghip v c
3.1.3.9.1 Khi nim v b thi v c
B thi cng nghip v c cng c nhiu loi, rt phc tp, a dng. N ty thuc vo mi
loi cng nghip.c th gm c nh sau:
B thi cc nh my ha cht, x luyn kim, gang thp
B thi cc nh my in, than..
B thi cng nghip khai thc, tuyn v ch bin qung khong sn.....
B thi ca cng nghip nguyn liu xy dng (xi mng, gch.)
B thi ca cng nghip thy tinh, snh s.......
..........
Nh vy mi loi khc nhau s phi dng cch phn hy khc nhau, nhng u dng k
thut x l t bng cc acid khc nhau trong bnh kenddan iu kin thng hay trong l vi
sng.
3.1.3.9.2 Cch x l v v d v phn tch kim loi
Nguyn tc
Nu xc nh cc kim loi trc ht mu cn c nghin nh, trn u mu, ly mt lng
nht nh (3-5 gam ) ph hp cho nguyn t cn phn tch v x l theo cch v c ha t (ha
tan) bng cc acid mnh c tnh xy ha nh nu trn trong trang b thng thng hay trong l
vi sng ty mi phng th nghim c trang b no.
Cch x l v v d.
V d 1: b thi luyn kim, nh my in, nh tro, x l cao.....(loi hm lng SiO 2< 5%).
Ly a gam mu c nghin nh v trn u (VD a= 2.000 gam ) vo bnh kendan, tm t bng
1 mL nc ct, thm 35 mL HNO3 65%, 4mL H2SO4 98%, lc u, cm vo bnh mt phu di
ui, un si nh trn bp cch ct n khi mu trong sut l c. Sau chuyn sang cc v un
nh ui cho ht acid n cn mui m . Sau thm 5mL HCl 10% vo mui m , lc v un
nh cho tan, nh mc thnh 25 mL bng nc ct. Nu nng cc nguyn t nh, th c th ly
lng mu ln hn v cng phi tng lng acid ln cho thch hp (tng 80% thi)
Mu loi ny c th x l trong l vi sng th nhanh v trit , m li khng lo mt nguyn
t phn tch
V d 2: b thi ca cc nh my ha cht v c, luyn kim, gang thp (c hm lng SiO 2
nh). Ly a gam mu c nghin nh v trn u (VD a: 2.00 gam) vo bnh kenddan, lm t
bng 1mL nc ct, thm vo 35mL cng thy, 5mL H2SO4 98% lc u, cm vo bnh phu nh
di ui, un si nh trn bp cch ct, n khi mu trong sut l c. Sau chuyn sang cc v
un nh ui cho ht acid n cn mui m. Sau nh mc thnh 25mL bng HCl 2%. Nu nng
cc nguyn t nh, th c th ly lng mu l 5 gam v lng acid thm vo cng phi tng
thm. Mu loi ny c th x l trong l vi sng th nhanh v trit m li khng lo mt nguyn t
phn tch.

V d 3: b thi cc nh my thy tinh snh s, vt liu xy dng (hm lng SiO 2 <10% )
ly a gam mu nghin nh v trn u (VD a=2.00 gam) vo bnh kendan, tm t bng 1mL
nc ct thm 35mL cng thy ,5mL H 2SO4 98% lc u cm vo bnh phu nh di ui, un si
nh trn bp cch ct n khi mu trong sut l c. ngui, chuyn b sang cc hay chn Pt.
Tm t, thm 5 mL H2SO4 28%, 10mL HF 40% v un nh cho bc khi trng SiF6 n khi thy
xut hin kh SO2 th dng un v li thm H2SO4 v HF ri bc khi ln na. ngui. Gp dung
dch lc...........b ny. Lm bay hi ui ht acid n cn mui m. Sau nh mc thnh 50
mL bng dung dch HCl 25%. cch ny c th p dng c cho cc mu qung t cha nhiu
silicat ca cc nguyn liu xy dng nh snh s thy tinh.v.v.v.....
3.2 X l mu hu c xc nh kim loi
3.2.1 Khi nim v mu hu c
Mu hu c c nhiu loi, ang dng, phc tp, n l cc loi mu thnh phn chnh. Cht
nn l cht hu c, matrix hu c v mu hu c thng gm c cc loi
Cc loi mu thc phm rau qu, tht c ti sng, v hp ca
Cc loi ng cc,go, khoai, u
Cc loi mu nc ngt gii kht, bia ru, nc qu p...
Cc loi mu tho mc, cy l thuc nam, thuoocs bc...
Cc loi mu du, m, nhin liu cht cao phn t...
Cc loi mu y sinh hc, cc loi nc, dc liu
Cc hp cht t nhin, hydrocacbon, than cc sn phm ha thch.
Cc loi rc thi, b thi thnh ph. Bnh vin, nh my thc phm. Cc loi cng nghip
hu c.
Mc ch ca x l mu y l phc v cho cc nhim v sau y:
Xc nh mt s kim loi, c bit l kim loi nng c hi.
Xc nh cc kim hay anion ca n.
Xc nh cc hp cht hu c.
V vy ty thuc vo mi mc ch phn tch th s c cch x l mu khc nhauthichs hp
theo n.
Vi cc loi mu ny, cho vic phn hy c d dng v trit , trc ht mu cn
c xay thnh bt (cc loi ht, qu cy, c), hay ct, thi nh(cy, rau, l...) trn u v cn ly
mu phn tch hay bo qun trong iu kin di 4oC, nu cha phn tch kp ngay. Vic x l
mu c th c thc hin theo mt s k thut c nu trong chng 2 trn.
3.2.2 Cc cch x l mu v v d
3.2.2.1 K thut tro ha kh (v c ha kh)
i vi cc loi mu hu c nguyn tc chung l:
1.Trc ht c xay nghin thnh bt nho, va hay th huyn ph.
2.Dng nhit tro ha mu, t chy cht hu c v a cc kim loi v dng acid hay cc
mui ca chng. C th l cn ly mt lng mu nht nh (a=5-10 gam ) vo chn nung. Nung
cht mu mt nhit thch hp t chy ht cc hp cht hu c, v ly b v c cn li ca
mu l cc acid, cc mui...sau ha tan cc b thu c ny trong acid v c nh HCl (1:1)
HNO3 (1:2) chuyn cc kim loi vo dng cc ion trong dung dch. Quyt nh vic tro ha ay
l nhit nung v thi gian nung (nhit tro ha v thi gian tro ha). Nhit tro ha cc hp
cht hu c thng c chn thch hp trong vng t 400-500 oC, n ty theo mi loi mu v cht
phn tch.
Qu trnh tro ha kh c th c thc hin c thm cht bo v, gi cho cht phn tch
khng b mt khi tro ha. Vic c dng hay khng dng cht bo v l ty thuc vo mi loi mu
v cht phn tch c th c b mt hay khng m dng cht bo v cho ph hp.
3.2.2.1.1 Tro ha khng c cht bo v v ph gia
Cch x l: cn ly mt lng mu nht nh (thng t 2-3 gam) cho vo chn nung,bt,
hay cc, ri em nung nhit thch hp, t chy, phn hy cc hp cht hu c ca mu,
chuyn cc nguyn t kim loi v dng b (tro ca cc mui v c hay cc oxit ca chng. Ha tan

tro ny trong HCl khi chng tan c dung dch mu phn tch, v d xc nh Ca, Mg, Na, K...
trong cc mu rau qu, thc phm, chng ta c th tro ha mu m khng cn dng cht bo v. V
cc nguyn t ny khng b mt khi nung.
Cc v d:
V d 1: Phn tch mt s kim loi nh: Al, Mg, Na, K,... trong mu rau qu. Ly 5 gam mu
cho vo chn nung, sy trn bp in cho n kh dn, ri nung 3 gi u 450 oC sau nung
530oC n khi c tro khng cn en (ht than en 10-8 gi). Sau ha tan tro cn li bng 15
mL HCl 1/1, un nh cho tan ht, v ui ht acid d n cn mui m v nh mc thnh 25 mL
bng dung dch HCl 2% lc u (nu c cn th lc b). l dung dch mu phn tch cc
nguyn t ni trn.
V d 2: phn tch mt s kim loi Al, Ca, Cd, Cu, Co, Fe, Mg, Mn, Na, K, Zn,.. trong mu
thc phm, tm, c,..ly 5 gam mu vo chn nung, sy cho kh dn. Ri nung 8 gi u 450 oC
sau 520oC n khi c tro khng cn en(ht than en). Sau ha tan tro cn li bng 15mL
HCl 1/1 un nh cho tan ht v ui ht acid d n cn mui m v nh mc thnh 25 mL bng
dung dch HCl 2%. Nu dung dch c cn th nn ly tm hay lc b cn. Cch ny d b mt cc
nguyn t Cd, Pb, Zn (8-15%) khi tro ha. Nht l khi tro ha nhit trn 530 oC. V th cch
ny khng thch hp cho Cd, Cu, Pb, Zn.
V d 3: Phn tch mt s kim loi Al, Ca, Mg, Na, K...trong mu dc phm thuc v y
hc. V d xc nh cc nguyn t Al, Na, K, Fe, Mn, Ni,...trong cao h ct. Ly 1 gam mu cho
vo chn nung, sy cho kh dn. Sau em nung 3 gi u 450 oC, sau 530oC n khi c
tro khng cn en(ht than en ). Sau ha tan tro con li bng 15 mL dung dch HCl 1/1 un nh
cho tan ht, v ui ht acid d cn mui m v nh mc thnh 25 mL bng dung dch HCl 2%.
Nu dung dch c cn th lc b cn ly phn trong xc nh cc cht. Trong v d ny cc
nguyn t Cd, Cu, Pb v Zn cng b mt nh v d 2.
3.2.2.2 Tro ha kh c cht bo v v cht chy
Nguyn tc v cch lm:
i vi mt s nguyn t c th b mt khi nung, nh Cd, Pb, Zn,.. nn nu ch nung nh
trn s b mt mt t (7- 20 %), m chng ta khng th bit c, nh v d 2 trn. V vy chng
ta phi thm vo cht bo v, khi tro ha. V d xc nh Cd, Cu, Pb, Zn trong mu rau qu v
thc phm, trong cc phng php tro ha kh cc nguyn t ny thng b mt t 10- 15 %. S
mt ny li khng khng ch c trong qu trnh tro ha. V th ngi ta phi thm cht bo v l:
H2SO4, HNO3, KNO3 hay Mg(NO3)2 hay hn hp (Mg(NO3)2 + LiBO2 ), th cc nguyn t ny s
khng b mt (xem bng ph lc cui chng).
Bng 3.3 kt qu x l c cht ph gia v khng c cht ph gia bo v

Cc v d:
VD1: phn tch Cd, Co, Cu, Fe, Mn, Ni, Pb, Zn,Cr.. trong mu rau qu (rau mung rau ci).
Ly 5 gam mu cho vo chen nung thm cht bo v l KNO3 10% 10mL H2SO4 98% trn u say
hay un cho si. Ri kh dn, nung 3 gi u 450 oC, sau 530 oC n khi c tro khng cn
en(ht than en ). Sau ha tan tro con li bng 15 mL dung dch HCl 1/1 un nh cho tan ht,
v ui ht acid d cn mui m v nh mc thnh 25 mL bng dung dch HCl 2%. Gii thch c
ch.

VD2: phn tch Cd, Co, Cu, Fe, Mn, Ni, Pb, Zn, Cr.. trong mu thc phm (tm c tht).Ly 5 gam
mu cho vo chen nung thm cht bo v l 5mL Mg(NO3)2 10% + 10mL H2SO4 98% trn u sy
hay un cho si. Ri kh dn, nung 3 gi u 450 oC, sau 530 oC n khi c tro khng cn
en (ht than en ). Sau ha tan tro cn li bng 15 mL dung dch HCl 1/1 un nh cho tan ht,
v ui ht acid d cn mui m v nh mc thnh 25 mL bng dung dch HCl 2%, lc u. (nu
c cn th lc b)
VD3: phn tch Cd, Co, Cu, Fe, Mn, Ni, Pb, Zn,.. trong mu thc phm sa bt, sa c c ng.
Ly 5 gam mu cho vo chn nung thm cht bo v l 12mL H2SO4 778% 5mL Mg(NO3)2 10%
trn u sy hay un cho si. Ri kh dn, nung 3 gi u 450 oC, sau 530 oC n khi c
tro khng cn en (ht than en ). Sau ha tan tro con li bng 15 mL dung dch HCl 1/1 un
nh cho tan ht, v ui ht acid d cn mui m v nh mc thnh 25 mL bng dung dch HCl
2%, lc u.
VD4: phn tch Cd, Co, Cu, Fe, Mn, Ni, Pb, Zn,...trong mu rc thi ca thnh ph Ly 5 gam mu
cho vo chn nung thm cht bo v l 5mL LiBO 2 10% + 5mL Mg(NO3)2 10% v 5mL H2SO4 98%
trn u sy hay un cho si. Ri kh dn, nung 3 gi u 450 oC, sau 530 oC n khi c
tro khng cn en (ht than en ). Sau ha tan tro cn li bng 15 mL dung dch HCl 1/1 un
nh cho tan ht, v ui ht acid d cn mui m v nh mc thnh 25 mL bng dung dch HCl
2%, lc u. (nu c cn th lc b).
Trong vic x l mu hu c ly cc kim loi th k thut ny c nhng u v nhc im l:
Tro ha trit c mu ht cc hp cht hu c.
n gin v d thc hin
Khng tn nhiu acid tinh khit cao v khng c acid d
Hn ch c s nhim bn do dng d thuc th
Qua mu x l khng lu, kh phng php t.
Mu dung dch, mu thu c s sch.
Nhng..: nu khng dng cht bo v.
3.2.2.2 K thut tro ha t (bng acid c oxy ha mnh)
Ni chung nh nu trong chng 2 c th dng mt acid c c tnh oxy ha mnh, hay hn
hp cc acid c c tnh oxy ha mnh, hay hn hp ca mt acid c tnh oxy ha mnh v mt
khng c tnh oxy ha nh (HNO 3 + HCl) hay (HF + HClO 4) t phn hy ht cc cht hu c ca
mu trong bnh Kendan, chuyn cc kim loi dng hu c v dng cc ion trong dung dch
mui v c. Vic phn hy c th thc hin trong h ng kn (p sut cao) hay trong h m (p
sut thng). Lng acid thng phi dng gp t 15 40 ln lng mu thi gian 10 12 gi.
Nn khi phn hy xong thng phi ui ht acid d.
Sau y l mt s hn hp acid c dng phn hy cc mu ly cc nguyn t kim loi
vo dung dch di dng cc mui tan.
+ Dng mt acid mnh hay c tnh oxy ha mnh: HCl, HNO3, H2SO4
+ Dng nc cng thy (HCl + HNO3)
+ Dng hn hp acid mnh c tnh oxy ha mnh (HNO3 + HClO4)
+ Dng mt acid mnh c tnh oxy ha mnh HNO3 vi H2O2
+ Dng hn hp a acid: (HNO3 + HClO4 + H2SO4)
+ Dng hn hp (HF + H2SO4 + HClO4) cho mu nhiu silicat.
+ Dng dung dch acid c v cht oxy ha mnh (HNO3 + H2O2)
+ Dng dung dch acid mnh cng vi cht to phc (HCl + Tartric)
Tt nhin mt hn hp ch thch hp cho mt s loi mu. V th phi kho st tm chn
cho thch hp nhm thu c hiu qu cao, khng mt cht v li ph hp vi phng php phn
tch chn. Sau y l mt s v d ng dng.

+ V d 1: x l mu xc nh cc nguyn t Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Zn

trong rau qu ti sng. Mu phi c xay thnh bt nho, trn u. Cn ly 5 gam mu vo bnh
Kendan, thm 60mL HNO3 65% - 5mL H2O2 30% lc u, cho vo bnh bng phu lc nh, un nh
cho mu phn hy n khi no c dung dch trong khng mu (khong t 7-8h). Chuyn ht mu
sang cc lm bay hi ht acid d, n cn mui m v nh mc thnh 15mL bng dung dch HCl
2%.
+ V d 2: x l mu xc nh cc nguyn t Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Zn
trong mu cha nhm (tm, c, tht). Mu phi c xay thnh bt nho, trn u cn ly 5 gam
mu vo bnh Kendan, thm 60mL vng thy v 10 mL H2SO4 98%, cm vo bnh bng phu lc,
un nh cho mu phn hy cho n khi no uc dung dch trong khng mu (khong 8-10h).
Chuyn ht sang cc, lm bay hi ht acid n cn mui m v nh mc thnh 25 mL bng HCl
2%, lc u, lc b cn silicate.
V d 3: X l mu xc nh cc nguyn t Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Zn,... trong mu rc thi
thnh ph. Trc tin mu phi c xay thnh bt, hay ht nh, trn u ri cn ly 5 g mu vo
bnh Kendan, thm 50 mL HNO3 65% v 10 mL H2SO4 98%, lc u, cm vo bnh mt phu lc
nh, un nh mu phn hy cho n khi no uc dung dch trong khng mu (khong 8-10h).
Chuyn ht sang cc, lm bay hi ht acid n cn mui m v nh mc thnh 25 mL bng HCl
2%, lc u, lc b cn (nu c).
V d 4: X l mu xc nh cc nguyn t Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Zn,... trong mu bt ng
cc (bt go, ng, sn, khoai, u...). Cn ly 5 g mu xay thnh bt vo bnh Kendan, tm t
bng 2 mL nc ct, thm 50 mL HNO 3 65% lc u, cm vo bnh mt phu lc nh, un nh mu
phn hy cho n khi no uc dung dch trong khng mu (khong 8-10h). Chuyn ht sang cc,
lm bay hi ht acid n cn mui m v nh mc thnh 25 mL bng HCl 2%. Mu ny dng
xc nh c kim loi kim v kim th.
V d 5: X l mu xc nh cc nguyn t Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Zn,... trong mu nc
ngt gii kht, v d Cocacola, Pepsi... Ly 50 mL mu vo cc un dung tch 250 mL, thm 5 ,mL
HCl 36%, un cho cn cn 1/3, chuyn mu vo bnh Kendan, thm 50 mL HNO 3 65%, lc u,
cm vobnh mt phu lc nh, un nh cho mu phn hy trong 2h, thm 2 mL H 2O2 30%, un
tip n khi no uc dung dch trong khng mu (khong 6-7h). Chuyn ht mu sang cc, lm
bay hi ht acid n cn mui m v nh mc thnh 25 mL bng HCl 2%, nh vy sau khi x l,
mu uc lm giu 10 ln. Mu ny dng xc nh c kim loi kim v kim th.
V d 6: l mu xc nh cc nguyn t Cu, Fe, Mn, Ni, Pb, Zn,... trong mu nc tiu. Ly 50 mL
mu vo cc un dung tch 250 mL, thm 5 ,mL HCl 36%, un cho cn cn 1/3, chuyn mu vo
bnh Kendan, thm 50 mL HNO3 65%, lc u, cm vo bnh mt phu lc nh, un nh cho mu
phn hy trong 2h, thm 2 mL H2O2 30%, un tip n khi no uc dung dch trong khng mu
(khong 6-7h). Chuyn ht mu sang cc, lm bay hi ht acid n cn mui m v nh mc thnh
25 mL bng HCl 2%, nh vy sau khi x l, mu uc lm giu 10 ln. Mu ny dng xc
nh kim loi kim v kim th.
u v nhuc im ca k thut ny l:
+ Khng mt mt s nguyn t kim loi nh Pb, Fe, Zn, Cu
+ Nhng thi gian phn hy lu, thng l t 10 18h
+ Tn nhiu acid tinh khit, acid d nhiu, phi ui sau khi x l rt lu.
+ D gy nhim bn, nu cc ha cht khng c sch cao
+ Phi ui acid d lu, c khi kh khn khng ht c.
Cch ny vi cc v d 1 6 nu thc hin trong l vi sng th nhanh, trit v tn t acid (ch
) hn x l t bnh thng ny. Ngha l cch x l t, c th thc hin trong bnh Kendan
iu kin bnh thng, hay thc hin trong l vi sng ca h m hay trong h ng kn. L d nhin
l k thut x l t trong l vi sng s nhanh v t tn acid hn k thut x l t thng thng.

3.2.2.3 K thut tro ha kh v t kt hp

Trong iu kin khng c l vi sng th y l mt cch x l mu tt xc nh cc kim loi.
Trc ht x l s b, nhng ta ch dng mt lng nh acid v cht bo v x l s b mu,
sau sy kh, ri tip tc tro ha kh trong t nung nhit thch hp t chy ht cht hu
c ca mu. Nh th s trit v nhanh, li khng mt cc kim loi. Sau ha tan tro b thu
c trong acid, ta s c dung dch xc nh cc kim loi. Nh th s khc phc c nhng
nhc im v tn dng c cc u im ca mi k thut ring.
Chng ta c th thc hin x l t s b mu bng cc hn hp sau y
+ Bng acid HNO3 c
+ Bng hn hp acid (HNO3 + H2SO4) c hay cong thy
+ Bng HNO3 c v c cht bo v KNO3, LiBO2, Mg(NO3)2
+ Bng acid H2SO4 45% c cht bo v MgSO4, KNO3, Mg(NO3)2
+ Bng acid (HNO3 + H2SO4) 45% c cht bo v Mg(NO3)2
+ Bng acid (HCl + H2SO4) c c cht bo v Mg(NO3)2
u v nhc im chnh ca k thut ny l:
+ Tn t acid tinh khit cao (ch bng 1/3 )
+ Nhanh v trit hn cch x l thng thng
+ Hu nh khng mt cht phn tch
+ Hn ch c s nhim bn do dng qu nhiu ha cht khi x l mu.
+ Dung dch mu thu c trong khng c acid hu c sinh ra.
+ Ph hp cho nhiu loi mu xc nh kim loi XXXXX anion
+ V d 1: x l mu xc nh Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Zn trong mu rau
qu v thc phm. Ly 5gam mu vo chn nung, thm cht bo v l 2mL Mg(NO 3)2 10%, 10mL
HNO3 65%, trn u, sy hay un nh cho kh dn v thnh than en. Ri nung 5h u 450 oC,
sau 530 oC n khi c tro khng cn en (ht than en). Sau ha tan tro cn li bng
15mL HCl 1:1, un nh cho tan ht, v ui ht acid d n cn mui m v nh mc thnh 25mL
bng dung dch HCl 2%, lc u, lc b cn nu c. Mu ny xc nh c c mt s kim loi
kim v kim th.
+ V d 2: X l mu xc nh Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Zntrong mu sa
bt, sa cLy 5gam mu vo chn nung, thm cht bo v l 2mL Mg(NO 3)2 10%, 4mL LiBO2
10%, 10mL HNO3 65%, trn u, sy cho kh dn v thnh than en. Ri nung 4 gi u 450oC,
sau 530oc n khi tro khng cn en (ht than en). Sau ha tan tro cn li bng 15mL HCl
1:1, un nh cho tan ht, v ui ht acid d n cn mui m v nh mc thnh 25mL bng dung
dch HCl 2%, lc u, lc b cn nu c. Mu ny xc nh c c mt s kim loi kim v kim
th.
+ V d 3: X l mu xc nh Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Zntrong mu rc
thi thnh ph. Ly 5gam mu vo chn nung, thm cht bo v l 1mL Mg(NO 3)2 10%, 4mL
LiBO2 10%, 10mL HNO3 65%, trn u, sy cho kh dn v thnh than en. Ri nung 4 gi u
450oC, sau 530oc n khi tro khng cn en (ht than en). Sau ha than tro cn li bng
15mL HCl 1:1, un nh cho tan ht, v ui ht acid d n cn mui m v nh mc thnh 25mL
bng dung dch HCl 2%, lc u, lc b cn nu c.
3.2.2.4. Tro ha t trong hp kn
y cng l mt k thut (phng php) x l t. Nn cng phi dng mt acid c tnh oxy
ho mnh, hay hn hp cc acid c tnh oxy ha mnh phn hy ht cc cht hu c trong bnh
kn, chuyn cc kim loi v dng cc ion trong dung dch mui v c. Vic phn hy c th thc

hin trong hp kn nn c p sut cao, n tng t nh ni p sut. S phn hy nhanh v trit ,

v cn t acid hn k thut thng thng ni trn. Song y phi c hp x l mu c bit,
chu acid, chu nhit v p sut cao. Cc bnh x l thng bng Teflon v t trong v thp dy
bo v, chu c nhit v p sut cao.
Tt c cc v d v x l t trong mc 3.2.2.2 nh ni trn u c th thc hin c trong
hp kn nhng lng acid th cn t hn (ch 30% l ) v qu trnh x l nhanh hn.
Mu v cc dung dch acid phn hy mu c cho vo hp phn hy, y kn, t trong v
thp, vn cht. Sau luc trong b nc si hay trong b du si, hay trong l vi sng, trong vng
60-120 pht, cho mu phn hy. Sau ngui, chuyn mu sang cc, lm bay hi ht acid d,
n cn mui m. Sau cng nh mc thnh th tch nht nh. Nu mu c cn th nn lc ly
dung dch mu trong.
+ V d 1: x l mu xc nh Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Zn trong mu rau
qu v thc phm. Ly 5gam mu vo chn nung, thm 40mL HNO 3 65%, 5mL H2SO4 98%, trn
u, y kn, vn cht. Ri cho hp mu vo t sy hay ni nc un si trong 1,5h. Ly ra ngoi
ngui. Chuyn mu sang cc, lm bay hi ui acid v n cn mui m. Sau ho tan nh
mc thnh 25mL bng dung dch HCl 2% lc u. Mu ny xc nh c c mt s kim loi kim
v kim th.
+ Vi d 2: x l mu xc nh Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Zntrong mu sa
bt, sa cLy 5gam mu vo chn nung, thm 40mL HNO 3 65%, 5mL H2SO4 98%, trn u,
y kn, vn cht. Ri cho hp mu vo t sy hay ni nc un si trong 2h. Ly ra ngoi
ngui. Chuyn mu sang cc, lm bay hi ui acid v n cn mui m. Sau ho tan nh
mc thnh 25mL bng dung dch HCl 2% lc u. Mu ny xc nh c c mt s kim loi kim
v kim th.
+ V d 3: X l mu xc nh Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Zntrong mu rc
thi thnh ph. Ly 5gam mu vo chn nung, thm 40mL HNO3 65%, 5mL H2SO4 98%, trn u,
y kn, vn cht. Ri cho hp mu vo t sy hay ni nc un si trong 2h. Ly ra ngoi
ngui. Chuyn mu sang cc, lm bay hi ui acid v n cn mui m. Sau ho tan nh
mc thnh 25mL bng dung dch HCl 2% lc u. Mu ny xc nh c c mt s kim loi kim
v kim th.
u v nhc im chnh ca k thut ny l:
+ Vic x l tng i nhanh hn x l trong iu kin h h bnh thng
+ Trit hn v khng mt cc cht
+ Tn t acid hn k thut thng thng
+ Thch hp cho nhiu loi mu phn tch
+ Nhiu phng th nghim c th dng c
3.2.2.5 K thut x l t mu trong l vi sng
y cng l k thut x l tro. Nn cng phi dng mt acid c c tnh oxy ha mnh hay
hn hp cc acid c tnh oxy ha mnh phn hy ht cc cht hu c trong bnh kn, trong l vi
sng, chuyn cc kim loi v dng cc ion trong dung dch mui v c d tan. Trong l vi sng,
di tc dng ca nng lng vi sng, s phn hy nhanh v trit . C th phn hy mu trong
bung h hay trong bung kn. Nht l trong h kn th lng acid cn dng l rt t (1/3-1/2 so vi
cc cch thng thng) v li bo m hon ton khng mt cht phn tch no. Tt c cc v d v
x l t nh ni mc trn u c th thc hin trong hp kn nhng lng acid cn t hn (ch
50% l ) v nhanh hn (50-90 pht).
K thut phn hy mu bng acid c tnh oxyha mnh trong l vi sng hin ti c hai cch thc
hin ty thuc vo trang b ca l vi sng:
Trong h m: Mu trong bnh Kendan hay ng nghim, thm acid c tnh oxyha mnh v t
trong l vi sng x l cho mu phn hy (oxyha) ht cc cht hu c, gii phng cc kim loi
vo dung dch. Cch ny khng c p sut cao.

V d 1: X l mu xc nh Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Zntrong mu rau qu thc phm.
Ly 5 g mu vo hp x l, thm 25 mL HNO 3 65%, trn u ri cho hp mu vo l vi sng trong
1.5h. Ly mu ra ngui, chuyn mu sang cc lm bay hi ht acid n cn mun m. Sau
ho tan nh mc thnh 25mL bng dung dch HCl 2%.
V d 2: X l mu xc nh Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Zntrong mu rc thi thnh ph.
Ly 5 gam mu vo hp x l, thm 35 mL nc cng thy, trn u ri cho hp mu vo l vi
sng trong 1.5h. Ly mu ra ngui, chuyn mu sang cc lm bay hi ht acid n cn mun m.
Sau ho tan nh mc thnh 25mL bng dung dch HCl 2%.
V d 3: X l mu xc nh Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Zntrong mu rc thi thnh ph.
Ly 5gam mu vo hp x l, thm 30 mL nc cng thy, 5 mL H 2SO4 98%, trn u ri cho
hp mu vo l vi sng trong 1.5h. Ly mu ra ngui, chuyn mu sang cc lm bay hi ht acid
n cn mun m. Sau ho tan nh mc thnh 25mL bng dung dch HCl 2%.
Trong h kn c p sut cao: y cng l k thut v c ha t. Ch c khc l dng thm nng
lng ca l vi sng x l mu thay cho cch gia nhit truyn thng. Mu c trong bnh
Teflon c np y, t trong v bo v chu p sut cao. t mu trong l vi sng, cc cht hu c
trong mu s b phn hy, t chy, oxyha. Nh vy mu s c phn hy trong acid p sut
cao.
+ V d 1: x l mu xc nh Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Zn trong mu rau qu
ti sng. Ly 5gam mu vo hp x l, thm 30mL cng thy, trn u, y np cht. Ri cho
hp mu vo l vi sng trong 50 pht. ngui, ly ra v chuyn mu sang cc, lm bay hi
ui acid v n cn mui m. Sau ha tan mui m v nh mc thnh 25mL bng dung dch
HCl 2%. Sau c th xc nh cc kim loi trong dung dch mu ny bng php o ph hp thu
nguyn t, pht x nguyn t hay phng php in ha
+ V d 2: x l mu xc nh Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Zn v cc nguyn t
t him trong mu qung t him. Ly 2gam mu vo hp x l, thm 20mL cng thy, trn
u, y np cht. Ri cho hp mu vo l vi sng trong 45 pht. ngui, ly ra v chuyn mu
sang cc, lm bay hi ui acid v n cn mui m. Sau ha tan mui m v nh mc thnh
25mL bng dung dch HCl 2%. Nu dung dch c cn th lc hay ly tm ly phn trong.
+ V d 3: X l mu xc nh Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Zntrong mu rc
thi thnh ph. Ly 5gam mu vo hp x l, thm 25mL nc cng thy, 5mL H2SO4 98%, trn
u, y np cht. Ri cho hp mu vo l vi sng trong 50 pht. ngui, ly ra v chuyn mu
sang cc, lm bay hi ui acid v n cn mui m. Sau ha tan mui m v nh mc thnh
25mL bng dung dch HCl 2%. Sau c th xc nh cc kim loi trong dung dch mu ny bng
php o ph hp thu nguyn t hay phng php in ha
u v nhc im chnh ca k thut ny l:
+ Qu trnh x l tng i nhanh (40 100 pht)
+ X l kh trit v khng mt cht phn tch
+ t c kh nng b nhim bn, nht l trong h kn c p sut cao
+ Khng phi ui acid d nhiu, nn hn ch c s nhim bn
+ Nhng phi c h trang b l vi sng thch hp
+ Thch hp cho nhiu loi mu phn tch
3.2.2.6 K thut ln men mu
Trc tin phi chuyn hay ha tan mu vo trong nc thnh dung dch hay th huyn ph
(vi nng mu khong 5 10%) thm 10 15mg men xc tc v chnh mi trng bng acid
hay kim, hay mui acetat cho ph hp theo yu cu ln men. V d pH = 7 8 khi ln men mu
ng en, ri a mu vo bung ln men nhit t 37 40 0C cho n khi mu trong hon
ton, tc l cc kim loi chuyn vo dung dch, cn cc cht hu c, khi ln men chuyn thnh
acid, nh acid acetic, kh CO2 v nc. Thi gian ln men t 7 10 ngy. Kiu ny rt thch hp

cho phn tch xc nh cc kim loi trong cc mu ng ma, nc ngt gii kht, mt s mu
nc qu chn p nh: chui, da, chanh, cam
+ V d 1: x l mu xc nh hm lng vt kim loi nng trong ng en, ng
vng hoa m, l cc loi mu c th c x l theo cch ny. Cn 10gam ng, ha tan trong
100mL nc ct, un nng n 400C, thm men xc tc, y knh ng h v trong t m ln
men nhit 37 40 0C cho mu ln men trong 7 ngy. Sau thm 10mL acid HCl 35% un si,
ly tm ly dung dch trong xc nh cc ion kim loi. Hay lm bay hi cn mui m, sau nh
mc bng mi trng acid thch hp theo phng php phn tch chn.
+ V d 2: x l mu xc nh hm lng vt kim loi nng trong mt ong. Cn 5
gam mt ong, ha tan trong 100mL nc ct m, un nng n 40 0C, thm men xc tc, y knh
ng h v trong t m ln men nhit 37 40 0C cho mu ln men trong 8 ngy. Sau
thm 10mL acid HCl 35% un si, lm bay hi cn mui m, thm 5mL HCl 10%, nh mc thnh
50mL bng nc ct, ly tm ly dung dch trong xc nh cc ion kim loi nng.
+ V d 3: x l mu xc nh hm lng vt kim loi nng trong nc qu p. Lm
nh sau: cn 5gam mu, ha tan trong 80mL nc ct m, un nng n 40 0C, thm 15mg men xc
tc, y knh ng h v trong t m ln men nhit 37 40 0C cho mu ln men trong 8
ngy. Sau thm 10mL acid HCl 35% un si, lm bay hi cn mui m, thm 5mL HCl 10%,
nh mc thnh 25mL bng nc ct, ly tm ly dung dch trong xc nh cc ion kim loi nng.
K thut ny c nhng u v nhc im chnh l:
+ n gin, d thc hin, khng mt cht phn tch
+ Khng tn km ha cht nhiu
+ Nhng phi mt nhiu thi gian, ch qu trnh ln men lu
+ Ch mt s loi mu dng lng. hay mu tan trong nc mi p dng c k thut
ny.
3.2.2.7 K thut ngm chit trong acid long
x l mu theo kiu ny, trc ht mu phi c ha tan trong mt dung mi thch hp
nh nc ct hay nh ha mu thnh dng huyn ph, thm cht m, cht to phc, hay cht to
mi trng, ngm qua m. Sau chit cht phn tch hay hp cht phc ca n t dung dch mu
vo mt dung mi hu c thch hp. Cch x l ny n gin, khng mt cht phn tch, khng cn
my mc dng c v trang b nhiu, nhng phi ngm mu qua m v ch thch hp cho mt s
loi mu.
+ V d 1: x l mu xc nh cc kim loi kim v kim th trong cc mu ng.
Ly 5gam mu ng vo bnh nn, thm 50mL nc ct, lc cho tan ht, thm 15mL HCl 36%, lc
u, un si, lm bay hi cn mui m, ri nh mc thnh 25mL bng dung dch HCl 2%. y l
dung dch mu xc inh cc kim loi kim, kim th. Vi cc loi nc qu p cng x l c
theo cch ny xc nh cc kim loi kim v kim th.
+ V d 2: x l mu xc nh cc kim loi km v kim th trong cc loi mu bt
go, bt m, bt khoaiLy 5gam mu bt vo bnh nn, thm 50mL nc ct, lc nh ha cho
huyn ph, thm 15mL HCl 36%, lc u k, un si, y nt bnh. ngm qua m. Sau lc
hay ly tm ly dung dch, un si, lm bay hi cn mui m ri nh mc thnh 25mL bng dung
dch HCl 2%. y l dung dch mu xc nh cc kim loi kim kim th.
3.2.2.8 K thut pha long mu bng dung mi thch hp
Cch x l ny l thch hp cho xc nh cc cht c nng khng cao v loi mu c th
ha tan tt trong nc ct, hay mt dung mi hu c no to thnh dung dch mu ng th.
Cch x l ny n gin, khng mt cht phn tch, khng cn my mc dng c v trang b nhiu
nhng ch thch hp cho mt s mu tan c trong mt dung mi nht nh v cht phn tch c
nng ln, khi pha long mu vn cn xc nh c n, theo phng php chn.
+ V d 1: x l mu xc nh Cu, Zn, Fe trong huyt thanh. Ly 0.5 mL dung dch
huyt thanh, thm 1.5 mL nc ct hai ln, lc u. y l dung dch mu xc nh Cu, Fe, Zn
trong huyt thanh bng phng php AAS. Nh vy mu c pha long 4 ln.

+ V d 2: x l mu xc nh Na, K trong huyt thanh. Ly 0.1 mL dung dch huyt

thanh, thm 4.9 mL nc ct hai ln, lc u. y l dung dch mu xc nh Na, K trong huyt
thanh bng phng php AES. Nh vy mu c pha long 50 ln.
+ V d 3: x l mu xc nh Ca v Mg trong huyt thanh. Ly 0.2 mL dung dch
huyt thanh, thm 4.9 mL nc ct hai ln, lc u. y l dung dch mu xc nh Na, K trong
huyt thanh bng phng php AES v xc nh Ca, Mg bng phng php AAS. Nh vy mu
c pha long 25 ln.
3.3.
X l mu xc nh mt s anion v kim
3.3.1. Nguyn tc chung
Trc ht chuyn mu thnh dng dung dch hay dng huyn ph. Sau ly mt lng nht nh
x l, ri phn hy mu bng hn hp acid c tnh oxyha mnh, hay hn hp kim v cht
oxyha theo cch tro ha t trong bnh Kendan hay tro ha kh nhit thch hp trong l nung,
phn hy cc cht hu c, a cc kim trong cc hp cht hu c v cc dng cc anion ca
mui tan trong dung dch nc. V d cc dng hp cht hu c sau:
- R-X v dng anion X (Cl, Br, I, F).
- R-S v dng anion SO42-.
- R-P v dng anion PO43-.
- R-As v dng anion AsO43-.
Sau xc nh chng theo cch thch hp.
Ni chung l c hai cch x l cc mu hu c xc nh cc anion.
3.3.2. Cc phng php v v d
3.3.2.1.
K thut v c ha t dng acid oxyha mnh
A. Nguyn tc: dng mt hn hp acid c v c tnh oxyha mnh nh hn hp ca
HNO3+HClO4, HNO3+H2SO4, HNO3+H2SO4+HClO4, H2SO4+HClO4 phn hy mu
ly cc nguyn t S, P, As, Br, F c trong mu cc dng hp cht hu c, cc mu sinh
hc a cc nguyn t ny vo trong dng anion ca mui tan trong dung mi nc hay
mt pha ng no tan tt v khng lm mt chng. K thut v c ha t ny thng lu,
ko di t 8-12 h mi hon thnh v dng lng acid gp 10-15 ln lng mu.
B. Cch x l v v d:
V d 1: X l mu xc nh cc nguyn t As, N, P, Cl v Br.. trong cc loi mu rau qu
ti sng. Trc tin nn xay mu thnh bt nho, trn u. Cn 5 g vo bnh Kendan, them 5
mL KMnO4 2%, 60 mL HNO3 65%, 8 mL H2SO4 98%, lc u v y bng phu ui di. un
nh bnh cha cho mu phn hy n dung dch trong mi thi. ngui, kim ha dung dch
mu bng dung dch NaOH hay Na 2CO3 10% n mi trng trung tnh hay kim yu (pH = 7,5
8,5). Sau nh mc thnh 50mL v ly tm hay lc ly dung dch trong xc nh cc
anion Cl, Br, I, PO4. Qu trnh x l ny c th thc hin trong l vi sng, th s nhanh hn v
trit .
+ V d 2: x l mu xc nh As, P, v Cl trong cc loi tm, cua, c. Trc tin mu
cn c xay thnh bt nho, trn u. Cn 5gam vo bnh Kendan, thm 5mL KMn 4 2%, 70mL
HNO3 65%, 5mL H2SO4, lc u, v y bng phu di chui. un si nh bnh cha mu cho
mu phn hy, cho n khi no c dung dich trong th thi. ngui, kim ha dung dch mu
bng dung dch NaOH hay Na2CO3 20% n mi trng trung tnh hay kim yu (pH = 7,5 8,5).
Sau nh mc thnh 50mL v ly tm hay lc ly dung dch trong xc nh cc anion Cl, Br, I,
PO4 theo mt cch thch hp c chn. Qu trnh x l ny c th thc hin trong l vi sng,
th s nhanh v trit . (Nu cn xc nh ion SO 4 th thay acid H2SO4 bng acid HClO4 th khng
xc nh Cl hay bng HNO3 th xc nh c c Cl).
+ V d 3: xc nh As trong qung a cht. Ly 0.5 gam mu vo chn Teflon, thm
t bng vi git nc ct, thm 10mL HNO 3 65%, un si nh khong 15 pht, thm 15mL HF
40% v 2mL HClO4 78%, y np chn v un nh tip 10 pht na (lc nh u khi un), m np
chn, un tip cho mu bc khi trng, n khi gn ht khi trng, ly ra (cn b 8mL), ngui
bt, pha long thnh nc ct thnh 80mL, thm 2mL H 2SO4 98% lc u kt ta tch Pb. Lc
b kt ta PbSO4 qua giy lc bng xanh v ra kt ta 2 ln bng 10mL nc ct. Thu ly nc lc

v nc ra vo cc 250mL, thm 4mL LaCl 3 5%, lc u, un nng thm dung dch NH 3 25% n
pH = 9 v thm d 4 git. Lc u, yn kt ta khong 10 15 pht, lc ly kt ta qua giy
bng . Ha tan kt ta bng acid HCl 25% nng (15mL), cho tan ht, nh mc thnh 50mL. y
l dung dch mu xc nh As bng phng php ph hp thu nguyn t.
3.3.2.2.V c ha kh dng hn hp kim mnh v cht oxy ha
Dng mt cht oxy ha mnh (Na2O2) trong mi trng kim mnh (KOH,NaOH) khi un
nng phn hy cu tr ca cc cht hu c, v a cc kim c trong hp cht hu c v dng
cc anion ca mui ca cc kim loi kim tan c trong nc, hay trong dung dch acid long.
Sau ha tan mu tro ha tch ly cc anion ca cc nguyn t . Cch ny trit v
nhanh hn cch x l t. Nhng iu kin y l cht oxy ha v lng kim phi ng hn
lng mu cn x l.
Theo k thut ny ngi ta thng dng cc hn hp kim sau y, v cch ny c dng
c hiu qu hn cc cch ni trn.
Dng hn hp (mui + kim + cht oxy ha mnh), v d nh cc hn hp:
(NaHCO3 + KOH + Na2O2); (Na2CO3 + KOH + Na2O2); (Na2CO3 + NaOH + Na2O2); (K2CO3 +
KOH + Na2O=); (LiBO2 + KOH + Na2O2)
Cch x l v v d
+ V d 1: x l mu xc nh cc nguyn t kim: Cl, S, P, Astrong mu rau qu.
Trc ht mu phn tch cn c xay thnh bt nho, v trn u. Cn ly 5gam, vo chen nung
thch anh, thm 2g NaHCO3, 4g KOH, 6g Na2O2, 5mL nc ct trn u thnh mt hn hp nho
nh va, un nh cho mu si u (ch d si bt v bn khi un). Tip tc un nh mu n khi
ht si bt, ri un tip cho n khi thnh than en. Sau em nung, 3h u 450 0C, sau nng
ln 5300C n khi no ht than en l c. ngui, em mu ha tan trong 100mL dung dch
NH3NO3 2% pH = 4. Lc manh u, lng. Sau lc hay ly tm ly dung dch xc nh cc
cht anion: AsO4, Cl, PO4, SO4. Trong dung dch ny Cl (ni chng l nguyn t nhm Halogen
dng anion (Cl-, Br-, I-) cn S dng anion SO42-, P dng ion PO43-, As dng ion AsO43-. Ni
chung cch tro ha bng kim tt hn cch tro ha bng acid ni trn.
+ V d 2: x l mu xc nh cc nguyn t kim: Cl, Br, S, P, Astrong mu thc
phm c, tm, cuaTrc ht mu phn tch cn c xay thnh bt nho v trn u. Cn ly 5g
vo chn nung, thm 2g NaHCO3, 4g KOH, 6g Na2O2, 5mL nc ct trn u thnh mt hn hp
nho nh va, un nh cho mu si u (ch d si bt v bn khi un). Tip tc un nh mu
n khi ht si bt, ri un tip cho n khi thnh than en. Sau em nung, 3h u 450 0C, sau
nng ln 5300C n khi no ht than en l c. ngui, em mu ha tan trong 100mL dung
dch NH3NO3 2% pH = 4. Lc manh u, lng. Sau lc hay ly tm ly dung dch xc nh
cc cht anion: AsO4, Cl, PO4, SO4. Trong dung dch ny Cl (ni chng l nguyn t nhm Halogen
dng anion (Cl-, Br-, I-) cn S dng anion SO42-, P dng ion PO43-, As dng ion AsO43-.
+ V d 3: x l mu xc nh As trong qung hay b thi rn. Ly 0.5g mu qung vo chn
Zr, thm 4g KOH, un nh cho hn hp chy lng, thm cn thn 5g Na 2O2 lc u v em nung
7000C cho chy lng trong 10 pht ngui. Ly chn c mu ra lau sch y, v b c chn vo
cc dng trn 400mL c sn 400mL nc ct nng 700C, lc k cho mu tan. Ly chn Zr ra v
trng chn 2 ln bng 20 mL nc ct (tng mu di 130mL). Thm vi mnh s xp nh vo cc
mu. y knh ng h v un si nh ui ht H 2O2 khong 15 pht, ngui. Sau lc ly
dung dch qua giy bng , ra kt ta v giy lc 3 ln bng 20mL dung dch KOH 0.05% nng.
Ly nc lc v ra, c cn cn khong 65mL, thm 25mL HCl 35%, lc u v nh mc thnh
100mL. y l dung dch mu xc nh As bng phng php AAS theo k thut Hydrua ha.
Cch x l ny thch hp cc loi mu rn, nh qung t, , rc thi rn, bn, trm
tch xc nh As. Nhng hm lng Si trong cc mu ny phi nh hn 10%
3.3.2.3. K thut chng ct
Mt s nguyn t kim, hay anion c kh nng to c cc acid hay cc hp cht d bay
hi nhit thp nht nh u c th dng cch ny tch chng ra khi mu ban u. V dun
nh kim As (bay hi di dng AsH3), anion CN, S ( dng acid HCN v H2S)Mun thc hin
x l theo cch ny trc tin mu phn tch cn phi ha tan trong nc to thnh dung dch trong

hay th huyn ph ng u. Sau khi chng ct ngi ta thm acid mnh hay thuc th ph hp
vo hn hp mu to ra cht bay hi v chng ct n cho tan hay hp th vo mt dung dch
thuc th c tnh cht nh lng.
V d 1: x l mu xc nh hm lng anion S trong b thi. Ly 20gam mu c
xay hay nghin mn vo bnh chng ct hai c (hnh 3.8), thm 80mL nc ct v hai ht s xp
(SiO2), lc u v lp vo h thng chng ct. un si mu chng ct v nh tng git acid
H2SO4 45% xung bnh lin tc (2 git trong 1 giy) trong thi gian chng ct v dng k nit sch
chy qua (3 bng kh trong 1 giy), n khi ht 25mL acid H 2SO4. Khi s c phn ng to ra kh
H2S bay ln
S2- (trong mu) + H+ H2S
Kh H2S bay ra ny c dng kh nit dn vo bnh hp th c cha sn 25mL dung dch
kim NaOH 0.01M. Khi ht kh H2S bay sang bnh hp th (30 40 pht), thu ly dung dch mu
ny v xc nh hm lng NaOH d, ta s suy ra c hm lng NaOH tc dng vi H 2S, v
suy ra c hm lng anion S2Ch : Chng ta cng c th cho kh H2S sinh ra vo bnh c cha 20mL dung dch mui
Pb(NO3)2 0.1M c pH = 1. Sau ly tm b kt ta xc nh hm lng Pb d bng phng php
AAS. Th cng suy ra c hm luwowjgn ion S2- theo phn ng:
Pb2+ + S2- = PbS
V d 2: X l mu xc nh hm lng anion CN - trong b thi. Ly 20 g mu uc xay hay
nghin mn vo cc 250 mL , thm 50 mL nc ct, kim ha n pH 8, khuy k, un si, thm 2
mL dung dch mui sulfate Cd(II) v Zn(II) 1%, lc k, un si nh, nu c kt ta th tch b anion
S2- di dng cc sulfide kh tan, kim hoa tip n pH 10, khuy u, lng 1h, ly tm hay lc
b kt ta . Ly nc lc v nc ra (khong 30 mL) cho vo bnh chng ct nh v d 1 nu
trn, lc u v lp vo h thng chng ct. un si bnh mu chng ct, nh tng git acid
H2SO4 45% xung bnh lin tc v cho kh nit chy qua nh v d 1 trn trong thi gian chng
ct, n khi dng ht 25 mL H2SO4 45% th dng. Khi s c phn ng to acid HCN (dng kh)
bay ln.
CN- + H+ HCN
Kh HCN sinh ra uc dng kh Nit dn vo bnh hp th c cha sn 25 mL dung dch NaOH
0.01M. Khi ht kh bay sang bnh hp thu (30-40 pht) , thu ly dung dch mu ny v xc nh hm
lng NaOH d, ta s suy ra lng NaOH tc dng vi HCN hay lng anion CN trong mu.
V d 3: Chng ct tch ly As t cc mu b thi rn hay thc vt, rau qu: Ly 10 g mu c
xay thnh bt vo bnh phn ng , nh ha bng 50 mL nc v thm HCl 35% c nng
khong 4M, lc u, un si nh cho mu phn hy n ht. ngui, yn 5 pht, thm 2 mL dung
dch KI 5%, un cch thy v lc u kh As(V) v As(III) trong 20 pht. Chuyn ton b mu
vo bnh chng ct, thm 10 mL HCl 35%, lc u, lp h thng chng ct. Cho kh mang Ar hay
N2 chy qua theo tng bong bng (3 bong bng / s), cho my khuy chy khuyy u mu, nh
tng git NaBH4 0.1M v bnh phn ng vi tc 1 mL/pht n ht 25 mL.Lc ny AsH 3 sinh ra
uc kh mang Ar dn sang bnh hp thu c cha dung dch thuc th R (Ag-DDC trong pyridin
20 oC). Chng ct cho n khi nh ht dung dch NaBH 4 th thi, ly dung dch hp thu xc nh
As theo phng php quang ph hp thu phn t UV-VIS.
3.3.2.4. K thut chit thng thng
Cc anion ca mt s nguyn t kim tn ti trong dung dch mu l cc mui c kh nng phn ly
thnh cc anion v tc dng uc vi mt s thuc th, trng nhng iu kin ph hp th c th tch
chng ra khi mu ban u. V d: NCS, CN, S. Mun thc hin x l theo cch ny trc tin mu
phn tch cn phi uc ha trong nc thnh cc dung dch hay huyn ph ng nht. Sau iu
chnh mi trng (thm acid hay kim) v thuc th ph hp vo hn hp mu to ra hp cht
c th chit uc vo mt dung mi hu c. Sau xc nh anion trong dung mi chit thu uc.
V d 1: Chit x l mu xc nh hm lng anion CNS trong b thi. Ly 20 g mu c xay
hay nghin nh vo bnh chit, thm 50 mL nc ct, chnh pH 2 bng H 2SO4 10%, lc u, thm 1
g Na2S2O3, thm 2 mL dung dch Co(NO3)2, lc u 10 pht, thm 20 mL ru isoamylic tinh khit,
y nt phu chit, buc cht v tin hnh chit trong 10 pht, yn 5 pht cho phn lp. Tch ly

phn dung mi hu c xc nh anion CNS uc chit vo di dng hp cht phc

Co(SCN)42-.
V d 2: Chit x l mu xc nh hm lng anion CN- trong b thi. Ly 20 g mu uc xay
hay nghin mn vo bnh chit , thm 50 mL nc ct, chnh pH 12 bng dung dch NaOH 5%, lc
u, thm 5 mL dung dch huyn ph CuCO 3 2%, 1 mL KCN 1%, y nt phu chit, buc cht v
tin hnh chit trong 30 pht, tt nht bng my lc, yn 5 pht cho phn lp. Tch ly phn
dung dch trong, nh mc thnh 50 mL bng nc ct v xc nh anion CN tan vo dung dch
ny dng phc Cu(CN)3- bng phng php AAS cho kim loi Cu. Suy ra hm lng ion CN theo
phn ng:
Cu2+ + 3CN- Cu(CN)3V d 3: X l mu xc nh cc nguyn t kim: As, Cl, Br, S, P, ... trong thc phm, c, tm,
cua.. Trc ht mu phn tch cn uc xay thnh bt nho v trn u. Cn 5 g mu vo chn
nung, thm 2 g NaHCO3, 4 g KOH, 10 g Na 2O2, 5 mL nc ct, trn u ri un nh cho mu si
u. (ch : mu d si bt v bn khi un). Tip tc un nh cho n khi mu ht si bt ri un
mnh n khi thnh than en. Nung 3 h u 450 oC sau nng ln 530 oC n khi no ht than
en l c. ngui, em ha tan mu trong 100 mL dung dch NH 4NO3 2% pH 4. Lc mnh, u
v lng. Lc hay ly tm ly phn dch trong xc nh cc nguyn t As, Cl, P, S trong dung
dch dng AsO43-, Cl-, PO43-, SO423.3.2.5. K thut chit pha rn ly cc anion
y thc cht l k thut sc k, nguyn tc v trang b c nu trong chng II, mc
2.4. Sau y l mt s v d c th cho x l tch mt s anion. Cch ny c dng ch yu
cho mu lng, hay cc mu rn c th ha tan trong dung dch nc c acid hay kim lng.
V d 1: X l mu tch ly anion Nhm Halogen trong mu nc:
Ly 250 mL mu nc vo cc, kim ha n pH = 8, lc hay khuy k, lc b cn kt ta. Ly
dung dch trong di qua ct chit anion (DVA Chrompack 5 m) vi tc 3-4 mL/pht (c
ht chn khng mi chy c). Khi ht dung dch mu qua ct chit, ht chn khng tip 2
pht. Cho chy qua ct chit 5 mL nc ct. Sau ra gii cc anion halogen ra khi ct chit
bng 25 mL dung dch HNO3 0.5M, ra ct thm 5 mL nc ct. Thu ly dung dch ra gii
ny, un si v lm bay hi n cn mui m, sau nh mc thnh 25 mL bng dung dch
HNO3 0.5%. V xc nh cc anion Halogen trong dung dch ny.
V d 2: X l chit tch cc anion nhm sunfat (Vn ny c th xem thm v d 2 v v
d 4 trong mc 2.4.4,2.4.2.3 chng 2).
Ly 250 mL mu nc vo cc, acid ha n pH = 1, lc hay khuy k, lc b cn kt ta. Ly
dung dch trong di qua ct chit anion (DVA Chrompack 5 m) vi tc 3-4 mL/pht (c
ht chn khng mi chy c). Khi ht dung dch mu qua ct chit, ht chn khng tip 2
pht. Cho chy qua ct chit 5 mL nc ct. Sau ra gii cc anion SO 42- ra khi ct chit
bng 25 mL dung dch HCl 0.75M, ra ct thm 5 mL nc ct. Thu ly dung dch ra gii ny,
un si v lm bay hi n cn mui m, sau nh mc thnh 25 mL bng dung dch HCl
0.5%. V xc nh cc anion SO42- trong dung dch ny.
3.3.2.6. K thut kt ta tch cht phn tch:
Dng mt thuc th kt ta v acid phn hy mu v kt ta ngay cht phn tch di dng
hp cht khng tan. V d dng acid HNO 3 v thuc th AgNO3 x l mu v kt ta tch
cc anion ca nhm Halogen. Hay l dng acid HCl v BaCl2 x l mu v kt ta tch
anion. Cch ny cng c ng dng ch yu cho cc mu lng, hay mu rn ha tan c
trong cc mi trng acid yu (pH = 2-5)
Cch x l v v d

V d 1: X l mu xc nh anion nhm Halogen trong mu nc thi.

Ly 200 mL mu, thm acid HNO3 35% n pH = 0, un si (nu c cn th ly tm lc b cn),
lm bay hi bt cn 50 mL, thm 5 mL HNO 3 65%, thm 10 mL dung dch AgNO3 0.1 M,
un cch thy 10 pht. ngui, lc ly kt ta, ra kt ta bng dung dch HNO 3 0.05% 2 ln.
Ly kt ta xc nh cc anion Halogen (ion Cl- Br- I-).
V d 2: X l mu xc nh hm lng anion SO42- trong mu nc.
Ly 200 mL mu, thm acid HNO3 35% n pH = 0, un si (nu c cn th ly tm lc b cn),
lm bay hi bt cn 50 mL, thm 5 mL H 2SO4 98%, thm 10 mL dung dch Ba(NO3)2 2%,
un cch thy 10 pht. ngui,thm 25 mL ru etylic 96%, lc , ly tm hay lc ly kt ta,
ra kt ta bng dung dch HNO3 0.05% c 20% ru etylic 2 ln. Ly kt ta xc nh
anion SO42-.
V d 3: X l mu xc nh hm lng As trong mu qung, t, , b thi rn( y ta
dng phng php cn kt As vi La(OH)3 dng As(OH)5 v As(OH)3 )
Cn ly 1g mu ( c xay hay nghin mn) vo chn teflon, hay chn Pt t bng nc ct,
thm 10 mL HNO3 65%, lc nh u v yn 10 pht, thm 12-15 mL HF 40%, 3 mL
HClO4 70%, y np chn, lc nh u v yn 15 pht. M np v un cho mu si v bc
khi, n khi thy khi trng dy c v khi xut hin nhiu thi thi. Pha long mu thm 50
mL nc ct, thm 3 mL H2SO4 98%, lc u, ngui v lc b kt ta PbSO 4 qua giy bng
xanh, ra kt ta 3 ln bng 20 mL nc ct. Thu ton b nc lc v ra vo cc sch khc,
thm 5 mL dung dch LaCl 3 5%, lc u, un si, va khuy v thm dung dch NH 3 25% n
pH = 9, thm d 5 git na, un si v lc nng kt ta qua giy bng . Ra kt ta 2 ln
bng 10 mL dung dch NH3 1%. Nh vy As s kt ta cng La(OH)3. Ly kt ta ha tan bng
20 mL HCl 35%, trng giy lc bng 10 mL HCl 5%. Thu dung dch v nh mc thnh 50 mL.
y l dung dch xc nh As bng phng php AAS vi k thut hydrua ha.
Cch ny thch hp cho cc loi mu c nhiu Si (hm lng Si>10%) v khi hm lng SiO3
trong mu ln th ta phi thm HF nhiu, gp hai hay gp ba s lng ni trn mi .
3.3.2.7. Phng php thng hoa
Phng php ny l da trn c s s thng hoa ca cht phn tch trng thi rn, khi chng ta
un nng mu phn tch ti mt nhit nht nh. Cht phn tch khi thng hoa s c ng
li trn y bnh ngng lnh.
V d: Xc nh hm lng iod trong b thi rn hay loi mu tng t. Ly 5g mu nghin
mn u vo cc thng hoa, thm 5g tinh th Al 2O3 v 2g CaO khan, trn u. Lp bnh ngng
ln trn cc thng hoa (hnh 3.12). un nh cho cht phn tch (iod) thng hoa, khi thy mu
nng chy th dng. Ly bnh ngng t ra ngui v nhng vo cc c sn 50mL benzen
ha tan iod. Ly dung dch benzen xc nh iod.
Hnh 3.12: Dng c thng hoa mu ly cht phn tch

CHNG VI:
X L MU XC NH CC CHT HU C
4.1. khi nim v phn loi mu hu c
4.1.1. mu hu c, cc loi v c im ca n
Mu hu c l cc loi mu m cht nn (matrix) ca mu l cc cht hu c. V d cc mu thc
phm, go, bt, thc vt, rau qu, cy l, sa, du m v.v. cc loi mu ny c th tn ti trng

thi rn, lng, kh, hay huyn ph. Cc mu hu c cng c c cc cht v c, cc cht kim loi,
chng tn ti trong mu dng hp cht c kim hay c hu c. V th c c xc nh cc cht hu
c v xc nh cc cht v c, cc nguyn t kim loi trong mu hu c. V d nh xc nh cc
thuc tr su dit c trong mu t nng nghip, l xc nh cht hu c trong mu v c. Nhng
trong mc ny ch yu trnh by cc k thut x l mu ly cc cht hu c trong cc i tng
mu hu c v v c khc nhau xc nh chng. Cht hu c c rt nhiu, song ngi ta phn
chia thnh cc loi sau y:
1. Cc loi hp cht hydrocacbua mch thng v mch vng.
2. Cc loi hp cht carbonyl (acid v aldehyd).
3. Cc loi hp cht amino acid, cc amin v vitamin.
4. Cc loi hp cht hu c c Halogen (Cl, Br) c nit.
5. Cc loi hp chy c kim loi
6. Cc loi hp cht d vng, c phosphor v nit v.v.
Tt nhin cch phn chia ny l theo quan im ca ho hc hu c. Trong cc loi ny, nu xt v
bay hi ca chng th ngi ta li xp thnh ba nhm nh sau
- Nhm 1: l cc cht d bay hi, im si thp (im si <150oC )
- Nhm 2: cc cht c bay hi trung bnh (im si 150-200oC)
- Nhm 3: cc cht kh bay hi (im si 250oC)
Trong x l mu phn tch xc nh cc cht hu c, chng ta s cp v s dng c hai
cch phn chia ny.
4.1.2. Cc yu cu ca x l mu cho phn tch cc cht hu c.
Cc cht hu c l rt phong ph, nhiu loi cht a dng, nhiu gp hng t ln cc cht v c
mc d ch c vi nguyn t ho hc chnh l C,H,O,S, cho ra cc cht hu c b ln men, b
oxy ho, b t chy, b ph v phn t sinh ra cc sn phm khc nht l cc hp cht trong
phn t c lin kt (ni i, ni ba, mch cacbon khng no). V th, ngoi cc yu cu chung
ca x l mu phn tch ni trn, th cc k thut x l mu phn tch cc cht hu
c cng c nhng im khc vi cc cht v c. Vn c th l:
+ v tnh a dng, phc tp nn kh tch cc cht phn tch ra khi mu.
+v tnh khng bn nn d b mt khi x l hay phn hu.
+phi c nhiu loi trang b khc nhau cho mi loi cht.
+trong x l cn nhiu dung mi hu c, c dung mi im si thp.
+phi khng ch nghim ngt cc iu kin khi x l mu
+ thng phi bo qun nhit thp (t +4 n -20oC).
4.2. Cc k thut x l mu xc nh cht hu c
4.2.1 Nguyn tc chung
- ly c tt cc cht phn tch, trc ht phi chuyn mu thnh dng bt hay huyn ph
hay dung dch ng nht trong mt dung mi thch hp, nc hay dung mi hu c, tu cch x
l, loi mu, v cht phn tch.
- Sau ly mt lng nht nh v x l bng mt k thut thch hp, v d nh chng ct hay
chit, hay kt tinh d ly cht phn tch ra khi mu ban u v chuyn n vo mt dung mi
thch hp. Sau xc nh chng trong dung mi .
4.2.2. Cc phng php, k thut x l v v d
4.2.2.1. Cc k thut chng ct
4.2.2.1.1. K thut chng ct thng thng
4.2.2.1.1.A. Nguyn tc
Chn cc iu kin thch hp chng ct tch ly chng ra khi mu phn tch ban u v c
th cho n tan vo mt dung mi khc tt hn, ph hp vi phng php xc nh (phn tch )
chn. Sau xc nh n trong dung mi ny (xem thm c s ca s chit trong chng II
trn)
4.2.2.1.1.B. Cc trang b, cch lm v v d

Trang b cho k thut ny l cc h chng ct khc nhau t mc nh n ln(hnh 20 ).

Trong qu trnh chng ct tu thuc vo im si ca cht m nc lm lnh ngng ct c
th l nc my nhit thng, hay nc my c lm lnh n nhit nht nh ph
hp ngng c tt cht cn chng ct. Cc v d v cch chng ct, sinh vin t xem trong
gio trnh thc tp ho hu c, nh:
- V d 1: chng ct tch cc hp cht cacbua hydro thm.
- V d 2: chng ct tch cc hp cht clo-phenols.
- V d 3: chng ct ly Benzen t benzen k thut v ly cn xc nh tp cht trong
benzene.
Hinh 4.20 Cc b phn ca b chng ct thng thng
4.2.2.1.2. K thut chng ct li cun
A. Nguyn tc chung: Ha mu vo dung mi li cun v d ha bnh ph v nc ct ct li
cun formaldehyde cng hi nc. Chn iu kin thch hp chng ct ly cht phn tch theo
nhit si ca chng, chng ct tch ly chng cng i theo mt cht li cun c nhit si
xp x nhng bay hi tt, ko n ra khi mu phn tch v cho n ngng t vo dung mi li
cun tt hn, sau xc nh n trong dung mi ny. Cch chng ct ny c th tham kho trong
gio trnh ha hu c.
B. Cc trang b, cch lm v v d:
Trang b ca k thut chng ct ny cng l cc b chng ct nh k thut chng ct thng thng,
gp trong ha hu c.
V d 1: chng ct li cun ly cresol.
V d 2: Chng ct li cun hi nc ly formaldehyde t bnh ph hay bn. Ly 20 g bnh ph
vo ci m no, nghin mn, thm 50 mL nc ct, trn u, chuyn vo bnh chng ct, trng ci
nghin bng 50 mL nc ct, gp ht vo bnh ct, thm 12 mL H 3PO4 m c, un si nh
chng ct cho formaldehyde bay hi cng hi nc (khi thu uc 50 mL l chng ct ht
formaldehyde), nh vy ti bnh ngng ta s thu uc dung dch formaldehyde trong nc. Xc
nh formaldehyde trong dung dch ny bng HPLC, GCMS hay ph UV-VIS.
4.2.2.1.3. K thut chng ct trong p sut thp
A. Nguyn tc chung: y ch l mt kiu ca k thut chng ct, do v nguyn tc th cng
ging nh nguyn tc ca chng ct nu. im khc l s chng ct y din ra p sut thp
kim sot nh h my ht chn khng. Trong iu kin p sut thp, nhit si v bay hi ca cc
cht s thp hn so vi iukin nhit bnh thng, v th qu trnh chng ct s din ra nhanh,
trit v an ton hn. Cc cht skhng b phn hy v c th tch ra khi mu d dng hn
iu kin thng. Chng ct c quay chn khng chnh l mt kiu ca chng ct di p sut thp.
phng php ny thng c p dng cho cc cht d bay hi v km bn hay loi(ui) dung
mi khi mu.
4.2.2.1.3.B Cc trang b cch tin hnh v v d
thc hin x l mu theo phng php chng ct ny chng ta phi cn c h thng
chng ct my iu nhit v mt bm chn khn g to p sut thp (hnh 4.21). K thut
ny hin nay c ng dng theo hai mc ch nh:
1. chng ct ly dung mi hay cht tinh khit t dung mi khng tinh khit
2. chng ct ui dung mi ly cn b cn li xc nh mt s tp cht hu c v
v c c trong dung mi hay trong cc mu lng.
V d 1: Chng ct x l mu MeOH khng tinh khit xc nh cc tp cht hu c kh
bay hi trong MeOH. Ly 200mL mu MeOH cho vo bnh chng ct(hnh 4.21) cho my
ht chn khng, my iu nhit chy, my iu nhit nc lm lnh khng ch 10 oC, tc
21 pht. Ri tin hnhun cch thu chng ct mu n khi mu cn khong 2 mL
th dng li ngui, lc ny ch cn b c snh bm vo y bnh, ho tan b ny bng 5
mL dung mi diico-methane c 20% acetonitril, hay ho tan trong n-hexan. Ly dung dich
ny xc nh cc cht hu c bng phng php HPLC, hay GC hay GC-VIS.

V d 2: X l mu xc nh hm lng Vitamin tong mu rau qu. Ly 10g mu

nghin min vo bnh nn c nt nhm, thm 20g Na2SO4 khan ( sy kh trong 4 gi
400oC). 10g MgCO3 khan, 40 mL n-Hexan vo b v lc chit tip. Lc ly dung dch v
gp c hai ln dung dch n-hexan vo bnh ct quay. Ct quay t t cho dung mi bay hi
(gi nc lm lnh 4oC) n cn 1mL ngui, ho tan b snh cn li ny trong 5mL
dung mi MeOH, hay n-hexan, ta c dung dch mu xc nh xc nh cc cht bng
phng php HPLC.
4.2.2.1.4. K thut chng ct trong mi trng siu m
4.2.2.1.4.A Nguyn tc chung
y cng ch l mt kiu ca k thut chng ct do v nguyn tc th cng nh nguyn
tc ca chng ct nu trn xong y ch c mt iu khc l qu trnh chng ct
c thc hin trong mi trng c nng lng siu m, to iu kin cho s chng ct
chn lc v nhanh hn. Trong iu kin ca siu m, nhit si v bay hi ca cc cht s
khc (thng l thp hn) iu kin bnh thng. v th qu trnh chng ct nhanh hn,
trit v an ton hn, cc cht li c th c tch ra khi mu ban u d dng hn.
Chng ct theo kiu ny thng c p dng cho mt s hp cht hu c a vng, a
nhn, kh bay hi v trong cc nn mu phc tp nh sa, t, bn, trm tch,v.v.
Hnh 4.21. S quay h thng trn khng
4.2.2.1.4B. Cc trang b, cch tin hnh v v d:
Mun thc hin x l mu theo phng php ny chng ta cn phi c h thng chng ct v
bung to sng siu m cung cp nng lng siu m cho qu trnh chng ct (hnh 4.22 ). K thut
ny hin nay cn rt mi song cng c vi hng sn xut v bn cc thit b trn th trng phc
v x l mu xc nh cc cht hu c v v c.

Hnh 4.22. S h thng chit siu m.

V d 1: Chng ct tch cc hp cht h chlorophenols v pesticide t mu t, b thi, thc phm.
Ly 20 g mi nghin nh vo bnh chng ct, nh ha trong 50 mL dung mi hu c, v d
CH2Cl2+n-hexane (1:1), thm 25 g Na2SO4 khan, lc k, chng ct ly cht phn tch vo bnh
ngng. Ly dung dch mu ngng c, lm bay hi dung mi bng dng kh nitrogen sch hay c
quay. Ha tan b cn li trong 5 mL MeOH v xc nh cc cht trong dung dch ny bng LC hay
GC
V d 1:X l mu xc nh cc v Caroten trong cc loi rau qu ti. Ta nghin
mu thnh bt nho,bo qun 40C, sau cn ly 5g mu vo phu chit (hay bnh nn c nt
nhm). Thm 20g Na2SO4 khan, 1g MgCO3 khan, v thm 40mL dung mi THF, lc chit mnh
trong 5 pht, lc ht chn khng tch phn dung dch THF.Lp li s chit bng 40mL THF nh
th ln na.Gp hai phn dung dch THF li v nh mc thnh 100mL bng THF. l dung dch
xc nh cc cht Caroten bng phng php HPLC [Method CH,Hng 1].
Hnh 4.23.H thng chit thng thng
V d 2:Xc nh Vitamin A trong Serum (huyt thanh). Ly 0.10mL Serum vo ng nghim, thm
0.90mL dung dch NaCl 0.9%, bo ho kh Nit trong 1 pht, thm 0.50mL C 2H5OH tuyt i lc
mnh, thm 1.0mL n-Hexane, lc u, ly tm vi tc 4000Vg/pm trong 5 pht.Tch ngay ly lp
hu c (lp n-Hexan c cha Vitamin A) bm vo ct sc k NP-HPLC (pha thng c ht 5
m, ct 250 x 4.6 mm), xc nh Vitamin A.

V d 3:Xc nh h clo-phenols trong mu rn, bt(nh thc phm hay mu t).Trc ht cng
phi xy mu thnh bt nho, trn u. Cn 5g mu vo phu chit, thm 20mL nc ct trn u,
chnh pH n 2 bng acid HCl 4M, lc u, thm 20mL dung mi dietyl-ete, lc chit mnh trong 5
pht, lng yn trong 5 pht.Sau tch ly lp hu c. Lp li s chit nh th mt ln na. Gp
pha hu c trong 2 ln chit li, lm kh bng Na 2SO4 khan, ri chuyn vo bnh nh mc 50mL,
v nh mc bng dung mi chit. y l dung dch mu xc nh cc clo-phenols bng GC. Vi
cc loi mu nc nh nc thi, nc sng hLy 250mL mu, chnh pH v lm tip tng t.
Nu nng nh th ly 500mL mu.
V d 4:Xc nh h hp cht clo-phenoxy trong mu rn, bt(nh thc phm, t, bn, rau qu.
[Method 3221A]. Trc ht cng phi xy mu thnh bt hay bt nho, trn u, cn 5g vo phu
chit, thm 10mL nc ct, trn u, chnh pH n 2 bng acid HCL 4M, lc u, thm 20mL dung
mi dietyl-ete, lc chit mnh trong 5 pht, lng yn trong 5 pht.Sau tch ly lp hu c.
Lp li s chit nh th mt ln na. Gp pha hu c trong 2 ln chit li, lm kh bng 20-25g
Na2SO4 khan.Lm bay hi dung mi chit nh dng kh nit hay ct quay chn khng cn 1mL,
ngui v ho tan b rn ny trong 5mL MeOH ri xc nh bng HPLC,GCVi cc loi mu
nc nh nc thi, nc sng h,..Ly 250mL mu, chnh pH v lm tip tng t, nu nng
nh th ly 500mL mu.
V d 5:Xc nh h hp cht Carbamate trong mu rn, bt (nh thc phm, t, bn, rau qu)
[Method 8321A].Trc ht cng phi xay mu thnh bt hay bt nho, trn u.Cn 5g mu vo
phu chit, thm 10mL nc ct, trn u, chnh pH n 4-5 bng acid HCl 4M, lc u, thm
20mL dung mi Diclo-metylen (CH2Cl2), lc chit mnh trong 5 pht, lng yn 5 pht. Sau
tch ly lp hu c. Lp li s chit nh th mt ln na. Gp pha hu c trong 2 ln chit li, lm
kh bng 20-25g Na2SO4 khan.Lm bay hi dung mi chit nh dng kh nit hay ct quay chn
khng cn 1mL, ngui v ho tan b rn ny trong 5mL MeOH ri xc nh bng
HPLC,GCVi cc loi mu nc nh nc thi, nc sng h,..Ly 250mL mu, chnh pH v
lm tip tng t, nu nng nh th ly 500mL mu
4.2.2.2.2.K thut chit dng lin tc
4.2.2.2.2.A.Nguyn tc chung
Qu trnh chit y ch chit cch chit thng thng l khi chit mt trong hai pha l
chuyn ng lin tc, hay c th c hai pha cng chuyn ng nguc chiu nhau. Trong nu pha
chit (dung mi chit) c t khi ln hn dung mi (pha) cha mu nhiu, th s chit cng thun
li hn. V th qu trnh chit xy ra nhanh v hiu qu cao hn chit thng thung. Trong thc t,
ngi ta thung gi yn pha cha mu trong bnh chit, cn pha ng chit (dung mi chit) th
uc duc bm lin tc tun hon sc vo bnh chit, m khng phi lc chit k thut chit ny
hay uc dng trong chit sn xut, quy trinh chit cng ngh.
4.2.2.2.2B. Trang b cch tin hnh v v d
Mun thc hinchit theo k thut ny phi c h thng chit gm bnh chit, bnh tch pha, v
h my bm bm pha ng chit theo yu cu mong mun sc vo bnh cha mu (hnh 4.24)
Hnh 4.24. S h thng chit dng lin tc n gin
V d: Chit tch 1 s cht hu c trong nc thi [ methode 3520 ]. Ly 500 ml mu vo bnh
chit. Cho my chy, bm dung mi chit ( CCl4 + CH2Cl2 ) sc vo bnh chit tun hon lin tc
trong 30 pht. Sau lng cho phn lp v tch ly phn dung mi hu c, lm kh bng
Na2SO4 khan lm bay ht dung mi chit v ha tan b cn li trong dung mi MeOH v xc nh
cc cht trong mu ny bng phng php HPLC v GC.
4.2.2.2.3 K thut chit Soxhlet.

4.2.2.2.3.A Nguyn tc chung.

V nguyn tc th y cng l qu trnh chit da theo s phn b ca cht trong 2 dung mi ( 2
pha ) khng trn ln vo nhau nh cch chit thng thng, song c iu khc l c thc hin
trong trong kiu trang b khc m thi, vi mc ch thu c kt qu chit tt v nhanh, chn lc.
Nhn h trang b trong hnh 4.26, chng ta cng thy c s chit ca phng php ny hot ng
khc hn kiu thng thng. Kiu chit ny p dng c c cho mu rn v mu lng.
4.2.2.2.3.B trang b cch tin hnh v v d.
H trang b thc hin kiu chit ny c ch ra trong hnh 4.26. trong cng c hnh kiu n
gin ( simplet soxhlet ) v kiu t ng ( auto soxhlet ). Cc trang b ny hin nay hin nay u c
bn trn th trng v c cc mc chit khc nhau.
V d 1 : Chit tch cc cht hu c c bay hi trung bnh v kh bay hi trong mu t b thi [
methode 3540 ] bng k thut soxhlet. Ly 10g mu nghin mn. trn u vi 25g Na 2SO4 khan,
cho dung mi chit vo ( 50 ml dung mi CH 2Cl2 v n- hexane t l 1/1 ), tin hnh chit trong 6
gi, sau chit ly dung dch pha chit) xc nh cc cht trong pha chit ny bng phng
php HPLC hay GC.
V d 2: Chit tch cc cht hu c c bay hi trung bnh v kh bay hi trong mu t b thi
[ methode 3540 ] bng k thut soxhlet t ng. Ly 10g mu nghin mn. trn u vi 25g
Na2SO4 khan nung li trong 4 gi 400 oC, cho dung mi chit vo ( 50 ml dung mi CH 2Cl2 v
n- hexane t l 1/1 ), tin hnh chit trong 6 gi, sau chit ly dung dch pha chit) xc nh
cc cht trong pha chit ny bng phng php HPLC, GC MS hay GC.
V d 3:Chit tch cc cht hu c c bay hi trung bnh v kh bay hi tong mu khng kh
[Method 3542] bng k thut Soxhlet t ng.Ly 10g Na2SO4 khan vo bnh chit, cho dung mi
chit vo (50mL dung mi diclo methylen hay n-Hexan), Lc du tin hnh chit khi bm mu
khng kh lin tc vo bnh chit vi tc 2-4 l/pht, n khi no c 500l khng kh qua
bnh.Sau tch ly dung dch (pha chit) xc nh cc cht trong pha chit ny bng phng
php HPLC hay GC. Nu nng cht nh th c th ly 1000 lt mu khng kh.
Hnh 4.26.S cc h thng chit Soxhlet
4.2.2.2.4.K thut chit trong siu m
4.2.2.2.4A.Nguyn tc chung
y cng l mt kiu ca k thut chit nh s chit bnh thng, ch c khc l qu trnh
thc hin chit l xy ra trong mi trng c thm tc dng ca sng siu m trong h chit, thc
y s chit xy ra tt hn, trit hn v nhanh hn so vi iu kin tch chit bnh thng.Tt
nhin y, cc cht mu v cht phn tch phi khng b nh hng bi sng siu m.K thut ny
ph hp cho cc loi cht kh bay hi, nh cc loi clo-PAH 6, clo-Pestide, chit cc cht trong mu
rn mu bt, mu l.v.v
4.2.2.2.4B.Trang b, cch tin hnh v v d.
thc hin cch chit ny, th h chit phi c t trong cabin (hp) kn c b phn cp
sng siu m trong vng tn s thch hp cho s chit (Hnh 4.27). Cc trang b ca cc h chit
theo kiu ny, hin nay c sn xut bi nhiu hng ch to dng c th nghim phn tch v c
bn trn th trng, t mc phn tch n mc bn sn xut.
V d 1:Chit tch mt s cht hu c a vng kh bay hi v bay hi trung bnh trong m t
bn, trm tch..[Method 3550].Ly 10g mu nghin mn vo bnh chit, thm 25-30g mui khan

Na2SO4, thm 50mL dung mi chit (diclo-methylen + n-Hexan trong t l:v/v=1/2), trn u, y
np v t vo bung siu m, ng cht my siu m, chn v t cc thng s siu m thch hp
chit.Tin hnh chit trong 50 pht. ngui ly hn hp mu ra tch pha, ly dung dch pha
hu c, lm bay hi dung mi bng dng kh nit sch (hay ct quay chn khng), n khi cn b
t.Ho tan b trong 3mL (hay 5mL) dung mi MeOH. y l dung dch mu xc nh cc cht
bng phng php GC hay HPLC.
V d 2:Chit tch mt s cht hu c thuc h Pesticide trong mu t, bn, trm tch, rau
qu[Method3550b]. Ly 10g mu nghin mn vo bnh chit, thm 30g mui khan Na2SO4, thm
50mL dung mi chit (diclo-methylen + n-Hexan trong t l:v/v=2/1), trn u, y np v t vo
bung siu m, ng cht my siu m, chn v t cc thng s siu m thch hp chit.Tin
hnh chit trong 50 pht. ngui ly hn hp mu ra tch pha, ly dung dch pha hu c, lm bay
hi dung mi bng phng php ct quay chn khng khi cn 1mL, ngui,
Ta c b t.Ho tan b ny trong 5mL dung mi MeOH (hay n-Hexan). y l dung dch mu
xc nh cc cht thuc h Pesticide bng phng php GC hay HPLC hay GC-MS
Mt s v d khc c th xem trong mc 2.4.4.2.3 chng 2
Hnh 4.27.S h thng chit siu m
4.2.2.2.5 K thut chit cc cht phn tch dng kh rn.
4.2.2.2.5.A Nguyn tc chung.
Nguyn tc ca cch chit ny l cc cht phn tch cn chit phi trng thi kh hoc l mu
dng kh hay nh 1 cch thch hp, ti 1 nhit thch hp chuyn cht mu thnh kh, cn pha
tnh chit l cht rn xp. Pha tnh cht chit trong ct chit hay l dng a. Pha tnh chit
y l Silica Gel xp loi trung tnh hay pha ngc, c kh nng hp ph tt cht phn tch. V th
gi l k thut chit rn kh. Trong qu trnh chit, mu c ha kh v c dng kh mang tr
N2 hay Ar sch ( > 99,99% ) dn cht mu vo ct chit theo tnh cht hp ph ca n, cn cc cht
khc th i qua. Sau dng mt dung mi thch hp nh acetonitril hay CH 2Cl2 ra gii cht
phn tch ra khi ct chit, phn tch chng trong dung dch ny. Nu cc cht phn tch d bay
hi, ngi ta cng c th gii hp cht phn tch ra khi ct chit bng ca1hc tng nhit ct chit
lm cc cht d bay hi v nh dng kh tr sch mang cc cht phn tch trc tip vo my GC
phn tch n.
4.2.2.2.5.B Trang b, cch tin hnh v v d.
thc hin cch chit ny th phi c h chit kn ( hnh 4.28 ). Ngun cp kh tr tinh khit
( Nit hay Ar 99,99% ) v khng ch c tc dng mong mun. Cc trang b ca h chit theo
kiu ny hin nay c sn xut bi nhiu hng ch to dng c th nghim phn tch v c bn
trn th trng. Cc ct chit hay a chit c cha silica gel xp loi pha thng v pha ngc
cng c ch to v bn sn trn th trng. Cc ct chit ny thng c dung tch cht chit t 6
10 ml.
V d 1: X l mu chit tch cc cht hu c d bay hi trong nc thi [ methode 5035 v 5022 ].
Ly 250 ml mu vo bnh chit, un nng n 60o+C, sc kh tr ( Ar ) tinh khit vo bnh cha mu
theo tng 2 bong bng trong 1 giy v dn kh ny vo ct chit c cha cht hp ph c tm
bng 1 dung mi hu c thch hp trong vng 120 pht. Sau ra gii trong ct chit bng 10 ml
dung mi CH2Cl2 c 20% n hexane . ly dung dch ra ny lm kh bng Na 2SO4 khan v xc
nh cc cht ni trn. Vi cc mu rn hay bt hay rau qu b thi trc ht ta phi nghin
bt mn, sau cng ly 10 g mu, thm 30g Na 2SO4 khan, lc k vo bnh chit v cng tin
hnh nh trn.
Hnh 4.28. H thng chit kh rn

V d 2:Chit tch cc hp cht cacbonyl(aldehid hay aceton) d bay hi trong khng kh [Method
0011 v 0100].Mu khng kh c dn vo ct chit silicagel(ct chit bng silicagel xp c
ch ho trc vi dung dch nc ca 2.4-dinitro-phenylhyrazin, pH=2)vi tc 3-4 l/pht.Trong
qu trnh ny aldehid c gi li trong ct chit theo tnh cht hp ph ca silicagel, v to ra cc
sn phm th ho ca cc aldehid.V d nh fodmandehyd dinitrophenyldazzone.Sau cht phn
tch trong ct chit c ra gii ra khi ct bng 10mL dung mi acetonitril hay diclomethane, v
xc nh cc cht trong dung dch ra ny bng phng php HPLC,GC, hay ph UV-VIS.
4.2.2.26.K thut chit pha rn (rn -lng ).
4.2.2.26A.Nguyn tc chung
Da vo tnh cht hp ph ca mt s silica xp c sn xut trong iu kin thch hp,
gi l pha tnh rn(chi tit v bn cht ca phng php ny xem mc 2.4 chng ).Khi ngi ta
di dung dch mu ca pha tnh , th mt nhm cht c pha tnh hp ph v gi li trn pha
tnh, cn cc cht khc .qua.Sau dng mt lng nh dung mi thch hp ra gii cht phn
tch ra khi pha tnh v xc nh chng trong dung mi .Pha tnh ca k thut chit ny hin
csn xut v cung cp trong 2 kiu ct chit:
Np trong cc ct sc k dung tch 6-10 mL
Ch to cc dng a xp
ng thi cc hng cng cc bn c cht chit dng nguyn liu cha np vo ct v bn
ct trng, ngi dng c th t np vo ct chit theo th tch yu c mong mun ring
cho th nghim cn thit ca mnh.
4.2.2.2.6B.Trang b, cch tin hnh v v d.
Trang thit b ca k thut chit ny cng tng i n gin. N gm b phu lc p sut
thp (Hay ht chn khng), ct hay di chit v ng hng mu chit(hnh 4.29). H chit kiu ct c
th lp mt dn t dm ct n hng chc ct chit ;nu lm hng lot mu).cc ct chit
(extraction carriridge:c dung tch 5-10 mL.Cn cc da chit:emporre extraction disk)c dy 2-3
mm. ng knh l 4-9 cm, phc v chit mu lm phn tch.
K thut ny c th chit cc cht phn tch trong mu lng, mu rn, mu nungc ra.
thc hin chit theo kiu ny vi cc mu khng phi .lng, trc ht chng ta phi chn mt
dung mi ph hp, ha tan c hon ton mu thnh dung dch
Hnh 4.29: s cc h thng chit pha rn
V d 1: Chit tch xc nh mt s cht hu c trong cc loi mu nc [ methode 5252 v
3535 ]. Ly 500 ml mu chnh pH = 4 5, lc b cn ri di qua ct chit vi tc 2 4 ml/
pht ( hnh 4.29 ). Khi ht mu di qua ct chit 2 ml nc ct , ht kh 3 pht. Sau ra gii
cht phn tch ra khi ct bng 10 ml CH 2Cl2. y l dung dch mu chit cc cht hu c
nh Acetanaphthene, Aldrin, Atraton, Alpha chlordane, Caloneb, Chlorobenzilate,
Chlopropham, 4,4 DDD , 4,4 DDT, 2 Chlorobiphenil Vi cc mu rn hay bn p dng
c cch ny nhng trc ht phi chn 1 dung mi ph hp v d n hexane hay acetonitril
ha tan thnh dung dch, lc b cn b, ly dung dch v lm kh n bng Na 2SO4 khan sau
mi chit nh trn.
V d 2: Tch chit nhm Aflatoxins ( B1, B2, G1, G2) t ht u v lcly 5g mu v xay
thnh mnh nh, cho vo ct v thm 50 ml ca hn hp MeOH/ H 2O ( 85/15 ), lc 10 pht, lc
ly dung dch thm 30g Na2SO4 khan, lc u chit tch b cc cht bo bng 50 ml n hexane.
Ly dung dch MeOH di qua ct chit vi tc 1ml/pht.Sau ra gii cht phn tch ra
khi ct chit bng 10 ml hn hp CHCl 3/CH3CN ( 60/40 ). Ly dung dch ra gii ny xc
nh bng phng php HPLC hay GC.
V d 3: Chit tch xc nh mt s cht Polyciclio Aromatic trong cc loi mu nc
[ methode 5501 ]. Ly 500 ml mu chnh pH = 3 5, lc b cn ri di qua ct chit vi tc
2 5 ml/ pht, sau ra gii cht phn tch ra khi ct bng Acetonitril.y l dung dch mu
chit cc cht thuc h Hydrocacbon thm a vng nh Acenaphthene,

Acenaphthylene,Antracen, benzo antracene,pyrene Cch ny cng p dng cho mu rn v

nho nhng trc ht phi chn 1 dung mi ph hp nh ha mu thnh th huyn ph, hay ha
tan thnh dung dch c th cng tt lm kh n bng Na 2SO4 khan sau ly dung dch ny
di qua ct chit.
V d 3: Chit tch xc nh 1 s hp cht aldehid v carbonyl trong mu nc v mu lng. ly
500ml mu nc, chnh pH = 5, lc b cn, di dung dch qua ct chit vi tc 2 4 ml/pht.
Sau ra gii cht phn tch ra khi ct chit bng 10 ml acetonitril. y l dung dch xc
nh cc cht acetaldehid, aceton, benzaldehydCn cc loi mu rn chng ta phi nghin nh
ha tan mu trong mt dung mi thch hp, lm kh bng Na2SO4 khan, sau lc hay ly tm
ly dung dch di qua ct chit.
Cc k thut sc k
Sc k ct
4.2.2.3.1A. Nguyn tc v iu kin
Da trn c s tnh cht hp ph hay trao i ca cc cht hp ph cht phn tch ln cht
nhi (pha tnh) trong ct sc k tch chng ra khi mu ban u. Sau dng mt dung
mi thch hp (pha ng) ra gii v ha tan chng vo pha ng, tch n ra khi ct sc
k, ri xc ng chng trong pha ng ny bng mt phng php ph hp. V d nh HPLC,
GC, UV-VIS V th trc ht phi a mu phn tch v dng dung dch, c th np vo
ct sc k c. S tch sc k y l da trn hai pha khng trn vo nhau, pha tnh l cht
rn, pha ng l cht lng (dung mi ra gii). V th n cng tng t nh k thut chit pha
rn. Ch yu y l sc k hp ph dng pha tnh l cc Silicagel hay nhm oxit xp c tnh
cht sc k.
iu kin y l:
- Chn pha tnh c tnh cht chn lc cho mt nhm cht phn tch.
- Chn pha ng ph hp cho cht cn x l, thu c n tt nht.
- Cn bng trong qu trnh sc k phi c tnh thun nghch tt.
- Chn iu kin sc k thch hp gp c cht phn tch vo mt nhm hay tch ra thnh
tng cht th cng tt.
4.2.2.3.1B. Trang b, cch x l v v d:
Mun thc hin chit kiu ny chng ta phi c cc h trang b sc k ph hp (hnh 4.30). N bao
gm ct sc k cha cc cht sc k l cc cht Silicagel hay oxit Al xp c kh nng hp ph
cc cht phn tch, cc dung mi ha tan mu phn tch v dung mi ra gii cht phn tch ra
khi ct sc k. Ty loi cht phn tch, m chng ta c th chn h pha sc k hp ph hay h pha
trai i ion sc k cc cht phn tch.
V d 1: X l mu xc ng cc alcaloit. Trc ht phi ha tan v chuyn mu v dng lng
trong mt dung mi hu c thch hp. V d nh n-Hexan hay acetonitril Sau ly c dung dch
ny hay ch mt th tch nht nh V mL. Ta np choco65t sc k hp ph c pha tnh l oxit nhm
cht phn tch c pha tnh hp ph v gi li trn pha tnh. Sau dng V mL n-Hexan (pha
ng) hay hn hp (n-Hexan + CH2Cl2 trong t l 1/1), ra gii cht phn tch ra khi ct sc k.
Nh vy cht phn tch s tan vo pha ng ra gii v tin hnh xc ng n trong pha ng ra
gii ny.
Hnh 4.30: Cc loi h ct sc k phc v chit mu

Thiu trang 24
K thut chuyn ha ha hc
4.2.2.4A. Nguyn tc chung:
Dng mt loi phn ng ha hc ca cht phn tch vi mt thuc th c tnh cht nh lng
trong mt iu kin thch hp, to ra mt sn phm l mt cht bn, tch cht phn tch ra
khi mu dng sn phm ca phn ng . Sau xc nh n trong sn phm . Cch ny

thng kt hp vi phng php sc k, m ch yu l tch ly mt s cht thuc h aldehid

mch thng. V bn cht y chnh l phng php th ha trong sc k tch v xc nh cc
cht khng c tnh cht sc k tt.
iu kin y l phn ng chuyn ha phi:
+ c tnh cht nh lng.
+ Thuc th c kh nng tng tc vi mt nhm, hay mt cht phn tch.
+ Qu trnh th ha hay chuyn ha ny thng xy ra trong ct sc k, hay trong vng phn
ng v phi nhanh.
4.2.2.4B. Cc trang b, cch x l v v d:
Cc trang b cho k thut ny ch yu l cc ct sc k, cc vng phn ng cun phc
v qu trnh tch cht. V th k thut ny thng hay i song song vi k thut sc k hay chit
(hnh 4.32). y l mt khu ca qu trnh tch v phn tch mt s cht hu c nh h aldehid.
Hnh 4.32: Cc trang b ca k thut chuyn ha ha hc
V d : Chit tch xc nh 1 s hp cht aldehid v carbonyl trong mu b thi hay mu
rn. Nu l mu rn ly 10g trc tin ta phi nh ha hay ha tan mu trong dung mi thch
hp ( 50 100 ml ) ly cc cht phn tch han ton vo dung mi ny, lc hay ly tm ly
dung dch mu.Ct tch chit y l cht hp ph silicagel c ch ha vi dung dch
thuc th l dinitro phenylhydrazin axit ( DNPH, pH = 2 ), mu lng th c nn qua ct
chit vi tc 2l/pht n khi c 500l qua ct ( c th ly lng kh n 1000l ).Nh vy
cc cht phn tch s c gi li trong ct chit dng sn phm hp cht phc ca phn ng
th ha. Sau ra gii cht phn tch ra khi ct chit bng 10 ml CH 2Cl2 hay CH3CN.Ly
dung dch ra gii xc nh cc cht formaldehyd.
4.2.2.5 Phng php pha long bng dung mi.
4.2.2.5.A Nguyn tc chung.
Nguyn tc ca cch ny l ly ( cn hay ong ) mt lng mu phn tch nht nh. Sau pha
long bng dung mi thch hp theo s ln nht nh. V d ly 5 ml mu tinh du nh mc
bng acetonitril n thnh 200 ml, nh th mu c pha long 40 ln. Sau xc nh 1 s
hydrocacbon trong dung dch pha long ny bng phng php GC hay HPLC. Phng php
ny c p dng ch yu cho cc mu du hay mu lng m cht phn tch tan trong mu ny.
Do khi pha long mu n cng c pha long ng u theo.
4.2.2.5.B Trang b, cch x l v v d.
K thut ny rt n gin khng yu cu k thut my mc g ht, m ch cn 1 s dng c thy
tinh ong o th tch mu v dung mi, cn cn mu phn tch.
V d 1 : Pha long mu du th bng dung mi n hexane xc nh 1 s cht hu c c
trong du m th [ Methode 3580 ] y ngi ta thng pha long mu phn tch t 50 n
200 ln bng dung mi hu c c kh nng ha tan mnh v d nh n hexane hay CH 2Cl2. sau
lc b cn khng tan ( nu c ) v xc nh bng phng php GC hay HPLC.
V d 2: Pha long mu du bi trn bng dung mi n hexane xc nh 1 s cht hu c c
trong du [ Methode 3580b ] y ngi ta thng pha long mu phn tch t 50 n 100 ln
sau xc nh cc cht bng phng php GC hay HPLC trong dung dch pha long ny. Vic
pha long bao nhiu ln l ty thuc vo mi cht cn xc nh c n tt theo phng
php chn.

X L V PHN TCH MU MI TRNG

5.1. Khi nim v mu mi trng v phn loi
5.1.1. Khi nim v mi trng v mu mi trng
5.1.2. Ngun gy nhim mi trng
5.1.3. Phn loi mu mi trng
5.1.4 Ly mu mi trng phn tch
5.2. Cc phng php x l mu v v d
5.2.1. Nc, nc thi v phn tch chng
5.2.1.1. Khi qut v nc v nc thi
5.2.1.2. Nc thi v s nhim nc
5.2.1.3. Cc ngun gy nhim cho nc
5.2.1.4. Cch x l mu nc phn tch kim loi
5.2.1.5. Cch x l mu nc phn tch cht hu c c hi
5.2.2. X l cc loi mu b thi
5.2.2.1. Khi nim v b thi
5.2.2.2. Cc ngun sinh ra b thi
5.2.2.3. X l mu b thi phn tch kim loi v anion
5.2.2.4. X l mu b thi phn tch cc cht hu c
5.2.3. X l mu khng kh, khi v bi
5.2.3.1. Khng kh, kh quyn v mi trng
5.2.3.2. Ngun gy nhim kh quyn v khng kh
5.2.3.3. Ly mu khng kh, bi phn tch
5.2.3.4. Cch x l mu khng kh v bi phn tch kim loi
5.2.3.5. Cch x l mu khng kh v bi phn tch cc cht hu c
5.2.4. X l mu t, bn v trm tch
5.2.4.1. Khi nim v t, bn v trm tch
5.2.4.2. Cc ngun gy nhim cho t v bn
5.2.4.3. Ly mu t v bn
5.2.4.4. X l mu t,bn phn tch kim loi v anion v c
5.2.4.5. X l mu t,bn phn tch cc cht hu c c hi
5.2.5. X l mu trong ru, trong nc
5.2.5.1. Khi nim v loi mu ny
5.2.5.2. Cc ngun nhim trong ru
5.2.5.3. X l mu rong, ru phn tch kim loi v anion v c
5.2.5.4. X l mu rong, ru phn tch cc cht hu c

X L MU MI TRNG PHN TCH

1. Khi nim v mu mi trng v phn loi
Khi nim mi trng v mu mi trng:
Mi trng hay mi sinh l nhng iu kin, vt cht, khng vt cht tn ti khch quan
xung quanh chng ta, v cng tn ti, tc ng tng h vi cuc sng ca chng ta, con
ngi, ng vt v ngay c thc vt cy c trn Tri t ny. l t, nc, khng kh,
gi, nh sang, m thanh, nng, m, s sng ca sinh vt, con ngi lun tn ti. Trong
c th l vt cht c th nhnh thy c, c th khng c th v khng nhnh thy c
V d nh kh th (khng kh), n l mt loi thc n ca con ngi. Tt c nhng ci
bao quanh chng ta v lun c quan h khng kht vi cuc sng ca con ngi, ng vt v
cy ci. Con ngi, ng vt khng th tch ri khi mi sinh. Khng c nh sang th cy
ci khng th sng c. Khng c nc v khng kh (oxy th) th con ngi cng
khng th tn ti c V th c th ni khi nim mi trng bao gm 4 b phn sau
y, chng c quan h cht ch vi nhau:
1. Kh quyn
2. Thy quyn
3. a quyn
4. Sinh quyn
Mu mi trng l cc loi mu tn ti trong mi sinh ca con ngi, v ng vt.N l
nhng sn phm chnh ca t nhin nh khng kh, t nc, nh sngNhng cng c th
l nhng sn phm sinh ra trong qu trnh hot ng sn xut, sinh sng ca con ngi,
dng vt v cy ci. N l cc loi mu lun tn ti trong khng kh v trong mi trng
xung quanh. N c th l tn ti cc trng thi lng, trng thi rn, trng kh v bi. V d
nh t, nc, khng kh, bi, khi nh my, cc loi b thi sinh hot, b thi bnh vin, b
thi ca sn xut cng nng nghip Ni chung l u u xung quanh chng ta cng u
c. Song ch c iu l khc nhau mc , s lng khc nhau trong mi vng, mi
quc gia v tnh c hi nhiu hay t, hay khng c hi khc nhau ca n i vi con ngi
v mi sinh m thi. Chnh con ngi trong qu trnh sinh sng v pht trin, cng li rt
nhiu loi sn phm, b thi khng c li, v chnh n li c tc hi ngay tr li cho chnh
con ngi trong qu trnh sinh sng v tn ti. Con nhi s lm nhim mi sinh nu con
ngi khng c gio dc v khng c hiu bit y v mi trng xung quanh ta v
vai tr ca n. Khong trn chc nm tr li y, vn nhim mi trng sng l 1
vn ton cu m khng phi ring mt nc no.

1.2 Ngun gy nhim mi trng.

Mi trng xung quanh chng ta lun b nhim bi nhiu ngun khc nhau, c ngun ca
chnh t nhin v c th l do chnh ca con ngi trong qu trnh sng, sn xut v pht
trin to ra. Mt cch tng qut chng ta c th tm tt cc ngun sau y c th gy ra
nhim mi trng.
1. Do chnh thin nhin to ra. Nh ma, gi, bo lt, thy triu, ging t, ng t, ni
la, chy rng, s st l ca ni non, v cc qu trnh t vn ng ca sinh quyn,
ca khng kh, nc sng bin
2. Do ng thc vt . S sng cht ,phn hy ca xc ng vt cht , s thi ra ca cy
ci , ca l cy trong qu trnh tn ti v pht trin.
3. Do vi sinh vt, nm mc. S sinh sng v pht trin mt s vi sinh vt, nm mc c hi
hay s gi cht ca chng cng li cho mi trng nhiu th khng c li.
4. Do cuc sng sn xut v pht trin ca con ngi to ra trn cc lnh vc khc nhau
nh:
Nc thi sinh hot, bnh vin nc thi cc nh my chn nui
Cc thi, rc thi, trong n ung, rc thi ca bnh vin
B thi ca nng nghip, chn nui, trng trt nh my sn xut thc phm phn bn, thuc
tr su, dit c

Cc b thi ca sn xut cc ngnh cng nghip ha cht, luyn kim

Cc kh thi, khi bi ca nh my ha cht, lc du,nh my in..
Sn phm ca v kh nh nhau, khi chin tranh khi n, thuc n, cht c ha hc, th
v kh ng tu v tr
- Do bi phng x nghin cu th v kh ht nhn ca cc nc ln nh M, Nga , php
Cc yu t ca con ngi ny nhiu hay t ty thuc vo iu kin nn kinh t, khoa hc thin
nhin ca mi n, nn sn xut v cuc sng, s vn minh hiu bit ca h. Tt c cc th
nhim c vo xung quanh mi trng chng ta, ln mt t ra sng ra bin, ra khng
kh lm cho mi trng b nhim khng cn trong sch v thun khit. Nh th l lm cho mt
t, nc sng , h, ao, bin, nc ngm u b nhim bn. Kt qu l chng ta phi nhn ly
cc th , chng co th lm hi, lm hy dit mi sinh v cuc sng. V th bo v mi trng,
gi mi trng trong sch l nhim v ca mi ngi.
V d v mc nhim, thnh phn cc cht trong mi trng nc, khng kh, hy xem trong
cc bng 1,bng 2, bng A3 v A4 phn ph lc.
1.3Phn loi mu mi trng
Theo khi nim trn th mu mi trng l rt a dng v ngun sinh ra n cng rt khc
nhau. Song theo trng thi tn ti, ngun sinh ra ca n, ngi ta tm chia thnh cc loi
nh sau:
1.
2.
3.
4.

Cc loi mu nc thin nhin, h ao, nc thi cc loi (thy quyn)

Cc loi phn bn, phn thi ca chn nui. (a quyn)
Mu khng kh, mu bi, tro v khi nh my (kh quyn)
Cc loi mu b thi ca cng nghip, nng nghip, sinh hoi, bnh vin(a quyn, do
sinh quyn to ra)
5. Cc loi mu t v bn(a quyn)
1.3 Ly mu mi trng phn tch
Vic ly mu l ty thuc vo mc ch phn tch v loi mu. Nhng d th no, loi no
th n cng cn phi tha mn cc iu kin sau:
1. i din ng cho i tc\ng cn gnhie6n cu phn tch
2. Khng lm mt cht cn nghin cu phn tch
3. Khng lm nhim bn thm cht cn phn tch
4. Khi lng cho cng vic nghin cu phn tch
5. Ph hp vi phng php chn x l v phn tch
6. Mi mu phi c h s y
7. Phi thc hin QA/QC trong ly mu v qun l mu.
V th phi ly mu theo mt quy trnh chun nht nh (Quc gia hay Quc t). Cc vn
ny c trnh by cc mc trn khi ni v mu phn tch v mu mi trng. V trong
phn tch th mu mi trng cng ch l mt loi hay mt nhm ca cc mu phn tch m
thi.
2. Cc phng php x l mu v v d:
Mc ch ca x l mu ca i lng mi trng l :
1. Xc nh cc nguyn t kim loi, nht l kim loi c hi
2. Xc nh mt s kim (As, Se, Te) v anion (Cl, Br, I, NO2, SO2,)
3. Xc nh mt s cht hu c, nht l cc cht c hi
4. Xc nh mt s vi sinh v vi khun c hi
5. Xc nh cht rn l lng (trong nc v khng kh)

6. Xc nh cc sinh vt ph du (trong nc)

7. Xc nh mt s kh (CO2, SO2, NO2, NH3) trong nc v khng kh
8. Xc nh hm lng oxy (DO, COD, BOD trong nc)
Mu mi trng l rt a dng v khc nhau, nn cch x l cng c nhiu cch khc nhau, ty
thuc vo mi loi, v vic x l l theo mi mc ch phn tch c th ring. Sau y l mt vi v
d c th minh ha mt s cch hay phng php x l ang c ng dng. Cc k thut hay
phng php c dng x l cc mu phn tch, cng c ng dng cho mu mi trng
phn tch cc cht. l cc phng php c trnh by trong mc 2.4 chng II v sau y
ch l mt s ng dng
1.
2.
3.
4.
5.
6.
7.
8.

K thut phn hy kh, x l kh c v khng c ph gia

K thut phn hy t iu kin thng, hp kn, v trong l vi sng
K thut chit Lng-Lng
K thut chit pha rn (Rn-Lng)
K thut ln men
K thut chng ct cc loi
K thut thng hoa cht phn tch
K thut clo ha mu.
..
V th trong phn ny ch trnh by mt s v d c th v x l mu m trng phn tch
cc cht theo cc nhm mu tiu biu, m khng trnh by li ni dung cc k thut .
l 5 loi sau:
_ Mu nc v nc thi
_ Cc loi mu b thi rn
_ Kh quyn, khng kh, khi v bi mi trng
_ Mu t, bn v trm tch
_ Cc mu rong ru sng trong nc

Nc, nc thi v phn tch chng:

Khi qut v nc v nc thi
Nc l mt loi khong cht ph bin v rt qu ca t nhin lun tn ti trn Tri t.
N l mt th nguyn liu v cng quan trng cho cuc sng ca con ngi, ng vt, chn nui,
trng trt v trong cc ngnh sn xut cng nng nghip. C th ni khng c nc th hu nh kh
c th c loi ng vt, cy ci v con ngi c th sng v tn ti c lu di trn mt t ny.
C th ca con ngi v mi loi ng vt u cha mt lng nc kh ln, t 50-80% khi
lng c th ca chng. C th ni nc ng ngha vi cuc sng ca sinh vt trong c con
ngi v mi qu trnh ca sn xut.
Tng lng th tch c trn v qu t vo khong 1372 triu km 3. Trong trn 1/3 l tn ti
dng bng tuyt v khong 1/3 lng ny nm trong lng qu t, n l cc loi nc ngm.
Trong c khong 55 triu km3 l nc ngt, cn li hu ht l nc mn c hm lng mui
NaCl t 1.2-3.5%.
Nc ngt phn b ch yu cc sng, bin, ao h, trong t lin v c khong 50000 km 3
trng thi hi trong khng kh, n to ra m ca mi trng khng kh. Quanh nm nc ha
hi vo kh quyn, ri li quay tr li b mt Tri t nh ma v tuyt. Ma v tuyt l yu cu tt
yu ca cy ci v s sng ca con ngi v sinh vt.
Nc c th tn ti 3 th (trng thi) khc nhau:
Rn (<0oC), lng (0-100oC), kh (>100oC). N trng thi no l ty thuc vo nhit ca mi
trng. Trong iu kin bnh thng, nc trng thi lng, tnh cht vt l ca nc trong iu
kin ny l:

1.
2.
3.
4.
5.
6.
7.
8.

Dng tn ti bnh thng: Th lng

T khi 0.99707 g/dm3 25oC
Nhit khi: 4.18 KJ/oC
nht ng lc n= 0.985 mPa.s 25oC
Sc cng b mt: 72.75 dyn/cm 20oC
dn in: 4.2 S/L.m 20oC
Hng s in mi: 80 FaraSteradian/m
Tnh cht quang hc: trong sut trong vng UV-VIS (190-800nm)

V mt ha hc, nng lng to thnh phn t nc l 242 kl/mol (hay l 58 Kcal/mol).

Nc l mt phn t phn cc. Hai nguyn t Hydro lin kt vi mt nguyn t oxy theo kiu
cng ha tr phn cc. Nn nc l mt dung mi phn cc. N ha tan tt nhiu cht phn cc
nh mui NaCl, NH4Cl, ng, cc cht hu c phn cc, amin, cc alcol Nc cng ha tan
c mt s cht kh nh N 2 (23 mg/l), O2 (54.3 mL/l), CO2 (2314 mg/l), H2S (5112 mg/l), CH4
(32 mg/l), H2 (1.6 mg/l) Khi ha tan cc cht, nc khng cn l nc sch na, nht l khi
c cc cht bn, cht c hi.
Nc l mt dung mi ca ha hc, n cng phn ly thnh ion, v trong iu kin chun n
c phn ly l 1.10-7 mol/l. nhng khi c mt ca cc cht khc tan vo nh acid, bazo th
n s phn ly t i, m bo tch [H +].[OH-] = 10-14. Nh vy nc l mt cht lng tnh, n
l mt acid hay bazo rt yu.
V mt sinh hc, nc l mi trng trao i cht ca mi t bo sinh vt. Khng c nc
th mi t bo u khng tn ti v pht trin c. Nc l trung tm ca s sng ca t bo, l
cht nn ca mi qu trnh dinh dng. Song cng l trung tm cuc sng ca mi loi vi
khun. V th, c nc mi c sinh vt v s sng. Nc l mt nguyn liu v ti nguyn v
cng quan trng cho cuc sng trn tri t. Nc v s sng l 2 phm tr c quan h cht ch
vi nhau. C th ni u c nc th c s sng.
Mt cch l tng nc sch l nc khng ha tan v cha bt k mt cht khc . Song
trong thc t iu khng th c c m nc lun ha tan mt s cht nht nh , cc cht
khc nhau v vi hm lng nh cng khc nhau ( xem bng A9) . Nu hm lng cc cht ha
tan trong nc cng nh , th nc cng sch . V th phc v sinh hot con ngi , chn nu
trng trt v sn xut cng nng nghip, nc cho mi mc ch phi c mi sch v yu cu
nht nh cho php, theo cc tiu chun ca mi ngnh ring. Xem bng v d sau y v tiu
chun ca php , m cn ca Vit nam xem phn ph lc.
Nc thi v s nhim.
Nc thi l nc bn n c ha tan nhiu cht khc nhau hu c, v c, vi sinh vt ,c th
khng c hi v b nhim, lm cho nc vt qua cc ch tiu ca cc cht c th c hay tan
trong nc vi gii hn cho php bnh thng. Khi l nc b nim.
Bng 2.5: Bng tiu chun nh gi cht lng nc sch :
Cc cht
1A
1B
2
3
dn in S/Cu
=< 400
400 750
750 1000
1500 3000
o
Nhit ( C )
=<20
20 22
22 25
25 30
Gi tr pH
6,5 8,0
6,5 8,5
69
5,5 9,0
MES ( mg/l )
=< 30
=<30
=<30
30 70
Oxy ha tan ( mg/l ) >7
57
35
Ym kh
DBO5 ( mg/l )
=<3
35
5 10
10 25
DOC ( mg / l )
=<20
20 25
25 40
40 80
NH4+ ( mg/l )
=< 0,1
0,1 0,5
0,5 2,0
2,0 8,0
NH3
=<0,1
< 44
44 100
N ton phn
12
23
Fe ( mg/l )
=<0,5
0,5 1
1 1,5
1,5 4

Mn ( mg/l )
=<0,1
0,1 0,25
0,25 0,5
F ( mg/l )
=<0,7
0,7 1,7
0,7 2,0
2,0 4,0
Cu ( mg/l )
=< 0,02
0,02 0,05
0,05 1,0
1,0 3,0
Zn ( mg/l )
=< 0,05
0,05 1,0
1,0 5,0
> 5,0
As ( mg/l )
=< 0,01
=0,01
0,01 0,05
> 0,05
Cd ( mg/l )
<0,001
=< 0,001
=< 0,001
0,002
Cr( mg/l )
< 0,05
0,05
0,05
>0,05
Ni ( mg/l )
<0,05
0,05
0,05
>0,05
CN=<0,05
0,05
0,05
>0,05
Pb ( mg/l )
<0,05
=0,05
0,05
>0,05
Se ( mg/l )
<0,01
0,01
0,01
>0,01
Hg ( mg/l )
<0,005
=<0,005
0,005
0,005
Phenol ( mg/l )
<0,001
0,001 0,05
0,05 0,5
Cht ty ra ( mg/l ) <0,02
0,02
0,02 0,05
> 0,05
Khun
Coli <50
50 - 5000
5000 - 50000
(con/100)
Eshcoli
=<20
20 - 2000
20 - 20.000
Khun cu chui
=< 20
20 - 1000
1000 - 10000
Ch gii:
Nhm 1A: cht lng cao tha mn cc nhu cu sinh hot n ung.
Nhm 1B: cht lng trung bnh dng tm c cho mc ch nh trn
Nhm 2: t yu cu cho nng nghip , ti, chn nui trng trt
Nhm 3: cht lng tm thng cho trng trt v chn nui.
V d sn xut 1000 lt bia, ngi ta thi ra trn 5-6 mt khi nc thi. Nc thi c ha tan
v cha nhiu cht, c c cht v c, cht hu c, cc cht kh, cc ht keo, ht rn khng tan l
lng, cc vi sinh vt. V th nc thi l mt hn hp phc tp. Thnh phn v tnh cht ca n l
ty thuc vo loi c thi ra t ngun sn xut hay sinh hot no. Cc cht trn vo trong nc
thi, s lm cho nc thi c tnh c hi khc nhau. Tnh c hi ny ph thuc nng ca cc
cht tn ti trong nc thi, v ty thuc vo iu kin ngnh sn xut thi ra. V d As 0.01 ppm,
Hg 0.005 ppm, Pb 0.1 ppm, NO2 0.002 ppm l gy nguy him cho con ngi v ng vt chn
nui. V th bt buc phi kim tra mi loi nc thi, pht hin cc cht ha tan, cc cht l
lng, cc vi sinh vt, vi khun nh gi nhim bn ca nc thi, c hi ca mi loi v
tm cch x l nc thi trc khi cho thi vo sng h, hay ng rung. Nu khng nc thi s l
mt ngun v cng to ln lm nhim mi trng ca con ngi, hy hoi con ngi v ca sn
xut. Nht l khi mi ngnh sn xut cng nghip cng pht trin th nc thi a ra mi trng
cng nhiu. Mt khu quan trng u tin ca cng vic ny l phi kim tra v phn tch nc thi
pht hin cc cht c trong n khuyn co v ra cc bin php x l thch hp. l mt
ni dung ca chuyn ngnh ha hc mi trng. Sau y l vi v d v cc ngun gy nhim
nc v nc thi.
Cc ngun c th gy nhim cho nc:
Song song vi cuc sng ca con ngi v s pht trin ca x hi, nc thi cng lun lun
tn ti, ch c trong mc khc nhau ca mi vng, mi th, mi quc gia m thi. N ty
thuc vo trnh khoa hc, trnh sn xut cng nng nghip, v vn minh ca cc nc, s
bo v ngun nc m nc thi b nhim khc nhau. Nhng cc ngun to ra nc thi co
th bao gm t cc lnh vc sau:
1. Sinh hot ca con ngi hng ngy, thnh th, bnh vin, nng thn thi ra a cc cht
bn vo nc.
2. S sinh sng v pht trin ca ng vt, phn thi ca chng
3. Sn xut cng nghip, cc nh my cng nghip thi ra cc cht chng tan hay phn b
l lng vo nc.
4. Khai thc khong sn cc loi a vo nc nhiu cht khc nhau
5. Sn xut nng nghip, cc nh my nng nghip, thc phm

6. Giao thng vn ti, ng b, ng st, ng thy

7. Chin tranh, th v kh, bom n, phng x
8. Ging t, thin tai, bo lt, ni la, chy rng
Cc cht thi vo nc gm loi, nh:
+ Cc cht v c, hu c tan vo nc
+ Cc cht v c, hu c khng tan vo nc m l ht l lng
+ C cht l lng, sau mt thi gian lng xung y, c cht khng lng
+ C cc loi vi sinh vt, vi khun, vi trng gy bnh
+ C cht rt c hi cho sinh vt v ngi
+ C cht tc hi ngn ngy, c cht ko di v hn
+ C cht xc tc cho cc qu trnh sinh ha bt li
Tt c cc ngun thi vo h, ao, sng, bin, bay ln khng trung ri ma ko xung lm
mi ngun nc sch b nhim dn dn theo thi gian. Cc cht thi, c cht tan vo trong
nc c, c cht l lng khng lng c, c cht s lng xung y dn dn trong qu trnh
tn ti v chuyn vn ca nc t ni ny n ni kia, ri gy nhim. Cc th thi ra c th
l cc cht v c, cc cht hu c, cc vi sinh vt, vi khun, nm mc. Trong tp hp , c th
khng c hi, c th c hi t, c th c hi nhiu, thm ch cc c hi cho ngi v sinh
vt. V th bt buc phi kim tra xem xt v x l nc thi ca mi loi.
Vic x l nc thi v tch b cc cht bn, cc cht lm nhim nc, to tr li nc c
th dng c cho nhng mc ch nht nh, hay thi ra sng h bnh thng, n bao gm cc
cng on chnh sau y:
1. Trc tin l phn tch, pht hin, v nh gi thc cht cc th gy nhim cho nc
thi, nht l cc cht vi sinh, vi sinh vt, xem cc th c hi mc no, ri c khuyn
co phng v x l.
2. X l nc thi loi tr nhng cht hay vi sinh vt, vi khun c hi.
3. Phn tch kim tra li nc sau kh x l.
4. Thi vo sng h hay dung li sau khi kim tra t yu cu.
(Xem cc bng A8, B1, B2, B4, phn ph lc 2 v 3)
Vic kim tra nh gi cht lng ca mt ngun nc thng phi xem xt theo mt s thng s
v yu t sau y:
1. Mu sc ca nc.
2. c ca nc.
3. o pH.
4. Hm lng cht rn trong nc, gm:
Tng cht rn ( )
Cht rn trong dng huyn ph ( )
Cht rn dng ha tan ( )
Cht rn c th bay hi ( )
Cht rn c th lng ng c ( )
5. acid hay kim.
6. cng ca nc (tm thi, vnh cu)
7. mui, mn.
8. Hm lng cc kim loi tan trong nc, nht l kim loi c hi.
9. Hm lng mt s kim v anion kim loi c hi (As, Se, F, NO2, CN, )
10. Hm lng Oxy ha tan (DO)
11. Hm lng Oxy sinh ha (BOD)
12. Hm lng Oxy ha hc (COD)
13. Hm lng Nito (N, NH2, NH3, NO2)

14. Hm lng du m
15. Hm lng mt s cht hu c c hi cho sinh vt v ngi:
+ Nhm khun Coliform (chnh l E-Coli)
+ Nhm khun Streptocxx (chnh l Streptocicus fecalis )
+ Nhm khun Clorstridca (chnh l Clostridium Perfringents )
Gii quyt vn ny l c mt h thng nhiu vn ca quc gia t cc quy ch php lut,
chnh sch, n cc bin php kim tra quan trc, cng nh cc phng php cng ngh x l
v iu kin kinh t.
Ngy nay cc nc c cc chun v cc loi nc, v u quy nh r hm lng , cc ch
tiu ny c th cho cc cht tan trong nc . Xem ch tiu v cc loi nc ca vit nam v USA
( iso ).
Gii quyt cc vn trn l c mt dy chuyn ng b. bt u l phn tch kim tra pht hin
cc cht , sau l giai on x l theo nhng k thut thch hp cho mi loi nc thi v ri
li kim tra phn tch li nc thi c x l, xem n t cc yu cu cha. Song
y chng ta ch im qua mt s vn trong phm vi cho php, lm v d minh ha m
thi, cn thc t th rt a dng v phong ph. Ch yu l giai on ly mu, x l mu phn
tch kim tra v pht hin cc cht.
Cch x l mu nc phn tch kim loi.
Vic x l mu nc phn tch tho nhng i tng sau y:
1. Xc nh cc kim loi ch yu kim loi c hi.
2. Xc nh mt s kim v anion.
3. Xc nh cc cht hu c c hi.
4. Xc nh pH, kim, mui.
5. Xc nh cc cht l lng khng tan
6. Xc nh cc sinh vt ph du
7. Xc nh hm lng oxy ( DO, COD, BOD )
8. Xc nh mt s vi khun nm mc gy hi.
x l mu xc nh kim loi , mt s kim v anion, chng ta c th s dng 1 s k thut
sau y:
1. k thut chit thng thng ( chit lng lng )
2. k thut chit pha rn ( rn lng )
3. Phng php kt ta, v kt ta cht gp ( sunphua hay hidroxit ).
4. Cc phng php sc k.
5. Cc phng php chng ct.
Nguyn tc v ni dung cc k thut ny xem trong mc 2.4. sau y ch nu mt s v d c th.
V d 1 : X l mu phn tch kim loi nng c hi ( Cd, Co, Cr, Cu, Fe,Mn, Ni, Pb, Zn..)
Cc kim loi nng c hi thng c hm lng nh v gii hn cho php ca n cng nh.
Cho nn khi x l mu ngi ta thng kt hp lm giu lun. V th chit l k thut c nhiu u
vit trong i tng ny.

a/ Phng php 1: Chit thng thng (chit lng-lng) ly hm lng tng cc kim loi
nng ra khi mu ban u.
Chit bng: (APDC + MIBK) hay (APDC + CCl4)
Chit bng: (Ditizon + CCl4) hay (Ditizon + CHCl3)
+ Nguyn tc: (Xem mc chit pha lng-lng trn)
Dng thuc th to phc: APDC v dung mi chit l: CCl4 hay CHCl3 hay MIBK.
+ Cch tin hnh:
Ly 250 mL nc thi vo phu chit, acid ha n pH = 4 bng HCl.10%, thm 2 mL APDC
0.1%, thm 25 mL CCl4, lc chit mnh trong 5 pht. lng yn 5 pht, gn tch ly phn
dung mi hu c CCl4 xc nh cc kim loi. H s lm giu F = 10. Cng c th gii chit
kim loi trong pha hu c ny vo pha nc bng acid HNO 3 3M, hay v c ha pha hu c, ri
ha tan tro bng acid ly kim loi v phn tch chng trong pha nc.
b/ Phng php 2: Chit pha rn (Rn-lng)
+ Nguyn tc chung: (Xem mc chit pha rn trn)
y l mt dng ca k thut sc k rn-lng (S-L), m cht chit l dng ht Silicagel v
xp. N tng t nh cc cht pha tnh ca sc k HPLC.
+ Cch tin hnh:
Chit tch lng vt cc kim loi kim: tch chit lng vt cc kim loi kim (Li, Na,
K), y ngi ta dng cht nhi kiu hp ph trao i ln ca hng Baker (Baker-10-SPEColumn, Cat-No.7020-3). Sau khi ct chit c lm sch bng nc ct (10 mL), cho chy qua 10
mL HNO3 1N, sau ra sch li ct bng 10 mL nc ct. Ly 200 mL mu, acid ha n pH = 5,
lc b bn v np dung dch ln ct chit va chun b vi tc 2-3 mL/pht. Sau ra ct bng
2 mL nc ct. Ht chn khng ct bng phu lc Busmer trong 3-4 pht. Ri ra gii cc ion kim
loi ra khi ct (pha rn) bng 15 mL dung dch NH 4NO3 2.5M, pH = 5.5. Khi pha ng chy ht
di ln ct 2 mL nc ct. Thu ly dung dch ra ny, lm bay hi cn mui m, them cht nn,
cht m v nh mc bng acid HCl 2% thnh 10 mL. y l dung dch mu xc nh cc kim
loi kim bng php o AAS hay ICP-AAS.
Chit tch lng vt cc kim loi nng: tch chit lng vt cc kim loi nng (Cd, Co,
Cr, Ca, Fe, Zn, Ni, Pb) t mu nc, y ngi ta dng cht nhi u hp ph ra ngc C18 ca
hng Baker (Baker-10-SPE-Column, Cat-No.7020-3). Sau khi ct chit c lm sch bng nc
ct (10 mL), cho chy qua 10 mL HNO 3 1N, sau ra sch li ct bng 10 mL nc ct. Ly 200
mL mu, acid ha n pH = 4.5, lc b cn, ly dung dch them 3 mL thuc th APDC 0.1%, lc
u v cho chy vo ct chit va chun b vi tc 2-3 mL/pht. Sau ra ct bng 2 mL nc
ct. Ri ra gii cc ion kim loi ra khi ct (pha rn) bng 15 mL dung dch NH 4NO3 2.5M, pH =
5.5. Khi pha ng chy ht di ln ct 2 mL nc ct. Thu ly dung dch ra ny, lm bay hi cn
mui m, them cht nn, cht m v nh mc bng acid HCl 2% thnh 10 mL. y l dung dch
mu xc nh cc kim loi kim bng php o AAS hay ICP-AAS.
V d 2: X l mu xc nh hm lng tng ca thy ngn (Hg). Ly 100 mL nc vo
bnh dung nn tch 250 mL, thm cn thn tng git n 10 mL H 2SO4 98%, 2.5 mL HNO3
65% v lc u. Sau thm 2 mL KMnO4 2% v 8 mL K2S2O3 5%. Lc k sau 15 pht, nu
thy mt mu hng tm nht th nh thm vi git KMnO 4 2% n xut hin mu bn. un cch
thy trong 2 gi, ngui n nhit phng. Sau kh cht oxy ha cn d bng dung dch
hydroxylamin 10%, n ht mu tm v ht c MnO 2, thm 2 git K2Cr2O7 2%. y chnh l
dung dch xc nh Hg theo phng php AAS bng k thut to Hydrua. Cch ny cng
dung c x l mu xc nh Hg trong cc mu nc ngt, bia, v mi loi nc thi.
V d 3: X l mu xc nh hm lng tng ca arsen (As).Ly 200 mL mu vo bnh
Kendan, thm 5 mL H2SO4 98%, 5 mL HNO3 33%, b vo vi mnh s xp nh, chm vo bnh
mt phu nh di chui. un trn bp in n khi thy xut hin khi trng, ri ngui.
Chuyn hon ton mu sang cc 400 mL, trng bnh Kendan 2 ln bng 20 mL nc ct. Thm
40 mL dung dch LaCl3 5%, thm tng git dung dch NH 4OH 12% n pH = 9. Ha tan kt ta
trn giy lc bng 20-25 mL HCl 25% nng, trng ra giy lc 3 ln bng 15 mL HCl 5%, thu

ton b dung dch vo bnh 100 mL v thm 4 mL KI 20%, lc u, nh mc thnh 100 mL, lc
u, un cch thy 20 pht, ngui. y chnh l dung dch xc nh Hg theo phng php
AAS bng k thut to Hydrua. Cch ny cng dung c x l mu xc nh Hg trong cc
mu nc ngt, bia, v mi loi nc thi.
V d 4: X l mu xc nh hm lng tng ca Selen (Se).
Ly 200 mL mu vo bnh Kendan dung tch 400 mL, thm 10 mL HClO 4 70%, 5 mL H2O2
30%, cm vo bnh mt phu nh, un nh cho mu si, n khi no thy khi trng dy c
xut hin th ly ra v ngui. Chuyn ton b mu sang cc un 400 mL, thm 4 mL LaCl 3
10 %, khuy u v thm dung dch NH4OH 25%, n pH = 10, khuy k v un cch thy 10
pht, lc qua giy bng ly kt ta La(OH)3 c hp ph Selen, ra kt ta 2 ln bng dung
dch NH3 c pH = 9. Ha tan kt ta bng 25 mL HCl 1M nng, thu nc lc v nc ra giy
lc vo bnh nh mc 20 mL v nh mc bng nc ct. y l dung dch mu xc nh
Selen. Cch ny cng dng c x l cc loi mu nc, nc thi xc nh Telu (Te), cng
nh cc mu nc ngt, bia, ru v mi loi nc thi.
V d 5: X l mu xc nh cc kim loi trong trng thi l lng trong nc.
Cc nguyn t kim loi hay cc ion trng thi l lng trong nc tc l chng khng tan trong
nc, m kt ta hay bm theo cc ht nh tng, cc ht rn nh, tn ti trong nc, lm cho
nc khng trong. V th nc cng khng trong th lha3 nng c cc ion kim loi cng nhiu.
V th xc nh hm lng ca cc kim loi tn ti cng vi cc ht khng tan trong nc,
trc ht phi tch c cc ht l lng bng cch lc hay ly tm cng vi cht ng t. Ly
200 mL nc vo bnh x l, thm 0.5 g cht ng t, lc u mnh, yn 20 pht, v ly tm
hay lc ly phn cn. Ha tan cn ny bng dung dch acid HCl 1/1 (6M) nng, thu dung dch
nay xc nh cc kim loi bng phng php AAS hay ph phn t UV-VIS
2.1.5. X l mu nc phn tch hu c c hi:
tch cc cht hu c trong loi mu ny chng ta c th dng
_ K thut chi (chit lng lng hay chit lng rn hay trong siu m)
_ K thau65t chng ct
_ K thut sc k: ch yu sc k hp ph trn Silicagel hay nhm oxit
V d 1: X l mu tch ly cc cht hu c nhm hp cht clo-phenois trong nc cc loi
Phng php 1: Chit pha lng lng thng thng, xc nh cc clo-phenol (v d: 2- clophenol, 2,4- diclo-phenol, 2,6-diclo-phenol, 2,4,6- triclo-phenol, 2,4,5- triclo-phenol, 3,4diclophenol, 2,3,4,6- tetraclophenol, Pentaclophenol). Ly 250 mL mu nc, kim h n
pH = 14, lc b cc cn b, dng 50 mL n-Hexan chit b cc cht bo v du m. Ly phn
dung dch nc, v acid ha n pH = 2, chit ly cc clo-phenol bng 20 mL dung mi
Dietylete. Lm bay hi dung mi bng ct quay chn khng hay bng dng kh nito nng, cn
li b m mu, ha tan trong 5 mL propanol v xc nh cc Clophenol bng phng php
HPLC v GC.
Phng php 2: Chit tch 1 s cht hu c thuc h Pesticide trong mu nc[ methode
3550b]. Ly 250 ml mu vo bnh chit chnh pH =2, thm 40 ml dung mi chit ( CH 2Cl2 n
hexane theo t l V/V = 2/1 ), trn u, y np v t vo bung siu m, ng cht my siu
m, chn v t cc thng s siu m thch hp tin hnh chit trong 40 pht. ngui lc
hn hp mu ra tch pha, ly dung dch pha hu c, lm bay hi dung mi bng phng php
chng ct quay chn khng n khi cn 1 ml, ngui ta c b t. Ha tan b ny trong
5 ml dung mi MeOH hay n hexane. y l dung dch mu xc nh cc nhm Pesticide
bng phng php GC, HPLC hay GC MS.

Phng php 3: Chit pha rn. Chit tch 1 s cht hu c thuc h Pesticide trong mu
nc[ methode 3550b]. Ly 250 ml mu vo bnh chit chnh pH =2,lc b cn ri di ln ct
chit loi XAD 2, 5 m vi tc 2 4 ml/pht, cho n khi chy ht mu qua ct chit.Sau
gii chit cht phn tch ra khi ct chit bng 20 ml dung mi n hexane c 15% CH 2Cl2.
Thu dung dch ra ui cho ht dung mi bng dng kh tr sch n cn b m, ha tan b ny
trong 5 ml dung mi MeOH.y l dung dch mu xc nh cc nhm Pesticide bng
phng php GC, HPLC hay GC MS.

2.2. X l cc loi mu b thi:

2.2.1. Khi nim v b thi:
B thi l mt loi sn phm m chng ta khng mun. Nhng n l sn phm hay l cc
th tt yu phi c ca qu trnh sn xut cng nng nghip v cuc sng sinh hot ca con ngi
hng ngy thi ra. V d nh b ma ca sn xut ng, cc th x ca l cao luyn kim loi, cc
th b ca nh my bia, ru, cc th thi ca cng nghip lm hp, rc thi ca tri chn nui
g ln, cc th b thi ca bnh vin, v.v. T chc bo v mi trng th gii c tnh, trung
bnh 1 ngi, mt ngy thi ra khong 0.5 kg b thi. Nh vy th tnh, mt nc 60 triu dn, th
mt ngy l bao nhiu tn rc thi cc loi. Tt c cc th hn tp a dng c gi mt tn
chung l B thi. B thi c chia thnh cc nhm (loi) nh ni trn.
2.2.2. Cc ngun sinh ra b thi:
B thi c chia thnh cc nhm, loi nh sau theo ngun sinh ra n.
1. B thi sinh hot ca con ngi hng ngy (rc thi), nht l th.
2. B thi ca bnh vin.
3. B thi ca sn xut nng nghip, chn nui gia sc.
4. B thi ca cc ngnh cng nghip khc nhau, nh ca cng nghip ha hc, in, than,
cng nghip thc phm, du kh v lc du.
5. B thi do sinh vt sinh sng pht trin to ra.
6. Cht thi ca thin nhin sinh ra, lt, bo, ng t, ni la
7. Cht thi qun s v chin tranh.
Trong cc loi ny, mi loi c tnh cht nguy hi khc nhau. C mc c hi khc nhau. Nht
l b thi bnh vin, loi ny cn phi t ngay, thiu hy ht cc vi trng, trnh ly nhim. V
th phi c cch thu gom khc nhau v x l khc nhau cho mi loi cht thi. Sau y ch nu vi
v d v x l mu cht thi phc v phn tch xc nh mt s cht trong b thi. Cc ngun b
thi thng gp l.
A. Ngun sinh b thi nng nghip, gm c:
- Do chn nui trng trt.
- Do qu trnh ch bin sn phm nng nghip.
- Do d tha ca cc loi phn bn hu c.
- Cng ngh ch bin thc n gia sc
B. Ngun sinh b thi cng nghip, gm c:
- Cng nghip khai thc v ch bin qung.
- Cc ngnh cng nghip ha hc nh ha du, polymer, t si, thuc da
- Cng nghip in, than, nng lng.
- Cng nghip thc phm.
- Cng nghip nguyn liu xy dng
- Cng nghip luyn kim, gang, thp
- Cng nghip thy tinh, gm s.
- Cng nghip giao thng v giao thng vn ti
- Cng nghip quc phng.
C. Ngun sinh b thi thnh ph v khu dn c:
- B thi ca thc phm, thc n, rau qu, ung hng ngy loi ra.
- Cc th thc phm hng, rau qu hng, thc n tha, v.v.

- Cc loi dng c, giy bao gi.

- Cc loi cn b thi loi ca cc l m, tri git sc vt n tht...
- Cc th thi loi ca ca hng thc phm, thc n, rau qu
D. Ngun v tnh nguy him ca b thi bnh vin:
C th do cc ngun sau:
- Cc loi vi, bng bng sau khi dng.
- Cc th sn phm ca phu thut loi ra.
- Cc th thuc , cht st trng dng bt, thi ra.
- Cc th thc n thi loi.
- Cc th giy, hp, l bao gi trong bnh vin.
- Cc loi b thi khc
Cc loi ny ngoi tnh c v ha dc, cn c rt nhiu vi khun, vi trng gy bnh ly lan
nguy him. V th cn phi:
- Thu gom ring.
- Khng c cho xung cc ngun nc, u gi.
- Khng c ni ng ngi, khu dn c sinh sng,
- a n mt ni ring thiu t hon ton.
Theo thng k ca t chc Y t th gii, trong cuc sng, mi ngy trung bnh mt ngi thi ra
0.5 kg rc. Cng thm cc loi b thi ca sn xut cng nghip, nng nghip, chn nui chng ta
thy lng cc cht thi l v cng ln, trung bnh khong 1 kg/1 ngi-ngy.
2.2.3. X l mu b thi phn tch kim loi v anion:
Vic x l mu cc cht thi, l phn tch theo nhng mc ch chnh:
- Xc nh cc kim loi, ch yu l kin loi c hi.
- Xc nh mt s kim (As, Se ) v anion (Cl-, CN-, CNS-, F-, NO2- )
- Xc nh cc cht hu c c hi.
- Xc nh cc vi sinh vt, vi khun
xc nh kim loi, mt s kim v anion, ngi ta thng dng cc k thut x l l:
- K thut tro ha t bng hn hp acid c tnh oxy ha mnh, trong iu kin thng hay
trong l vi sng.
- K thut tro ha kh c cht bo v.
- K thut tro ha kh v t kt hp.
- K thut thng ha
- K thut chit (lng-lng, hay lng-rn).

Cn xc nh cc hp cht hu c, ngi ta thng dng cc phng php:

- Cc phng php chit lng-rn, kh-rn, siu m.
- Cc phng php chng ct (thng thng, hay li cun, siu m...)
- Phng php kt ta cht phn tch.
Chi tit v cc k thut ny xem mc 2.4 nu trn. Sau y l mt s v d c th v
x l b thi xc nh mt s cht m chng ta cn quan tm trong phn tch mu mi trng b
thi.
X l mu xc nh cc kim loi nng c hi. xem cc v d trnh by chng III, nh
v d (trang ), v d (trang ), v d (trang ). Hay v d (trang ), v d (trang ) v x l mu xc
nh mt s anion v c. Sau y ch trnh by thm vi v d khc trong i tng b thi mi
trng.
V d 1: B thi luyn kim, nh my in, nh tro, x l cao, gang thp, nh my in. Ly 2
gam mu c nghin nh v trn u vo bnh Kenddan, tm t bng 1 mL nc ct, thm 35
mL HNO3 65%, 4 mL H2SO4 98%, lc u, cm vo bnh mt phu di chui, un si nh trn bp
cch ct, n khi mu trong sut l c. Sau chuyn sang c v un nh ui cho ht acid n
cn mui m. Sau nh mc thnh 25 mL bng acid HCl 2%. Nu nng cc nguyn t nh,
th c th ly lng mu ln hn, v cng phi tng lng acid ln cho thch hp (tng 80% thi).

Mu loi ny c th x l trong l vi sng th nhanh v trit , m li khng lo mt nguyn t phn

tch.
V d 2: B thi cc nh my ha cht hu c v cng nghip hu c, thc phm Ly 2
gam mu c nghin nh v trn u vo bnh Kenddan, ln t bng 1 mL nc ct thm 35
mL cng thy, 5 mL H2SO4 98%, lc u, cm vo bnh phu nh di chui, un si nh trn bp
cch ct, n khi mu trong sut l c. Sau chuyn sang c v un nh ui cho ht acid n
cn mui m. Sau nh mc thnh 25 mL bng acid HCl 2%. Nu nng cc nguyn t nh,
th c th ly lng mu l 5 gam, v lng acid thm vo cng phi tng thm. Mu loi ny c
th x trong l vi sng th nhanh trit m li khng lo mt nguyn t phn tch.
V d 3: B thi cc nh my thy tinh snh s. Ly 2 gam mu c nghin nh v trn
u vo bnh Kenddan, lm t bng 1 mL nc ct thm 30 mL cng thy, 5 mL H 2SO4 98%, lc
u, cm vo bnh phu nh di chui, un si nh trn bp cch ct, n khi mu trong sut l
c. ngui.Sau lc ly dung dch chuyn b sang cc hay chn Pt, tm t thm 5 ml H 2SO4
98%, 10 ml HF 40% v un nh ui cho ht HF ri bc khi ln na, ngui, gp dung dch lc
u vo b ny, lm bay hi ui ht acid n cn mui m. Sau nh mc thnh 25 mL bng
acid HCl 2%. Cch ny c th p dng c cho cc mu qung t c cha nhiu silicat v cc
nguyn liu xy dng, xi mng, snh s, thy tinh
V d 4 : xc nh Cd, Co, Cr, Cu, Fe, Mn, Zn, Pb, Nitrong mu b thi rau qu v thc
phm. Ly 10g mu vo chn nung thm cht bo v l 2 ml Mg( NO 3 )2 10%, 10 ml HNO3 65%,
trn u sy hay un nh cho kh dn v thnh than en. Nung 3 gi u 450 oC, sau 530oC
n khi c tro khng cn en ( ht than en ). Sau ha tan tro cn li bng 15 ml HCl 1M
nng, chuyn mu ht sang cc v un nh cho tan ht v ui ht axit d cho n khi cn mui m
v nh mc bng 25 ml bng dung dch HCl 2% lc u. Mu ny c xc nh cho c kim loi
kim v kim th.
V d 5 : X l xc nh thy ngn. Dng k thut thng hoa ly Hg. Ly 2g mu vo
bnh thng hoa Hg ( xem hnh v ), thm 1g bt Fe, 2g CaO, trn u, qun phn ng ngng Hg
bng vi tm bng tuyt CO2 hay nc . Kp hay t nm ngang ng. un nh bu bnh cha
mu, cho nng u v chy bng n kh, xoay u khi un. Lc ny Hg bay hi v ngng vo
thnh ng. sau khi ton b hn hp chy u v mu l mu thm, un thm 2 pht ngui.
tch b bu cha mu ly ng ngng v nhng vo ng nghim c cha sn 15 ml dung dch HNO 3
, ly dung dch thm 2 git dung dch K 2Cr2O7 1%. nh mc thnh 50ml. l dung dch xc
nh Hg. Cch x l ny co th p dng x l mu t, qung b thi rn xc nh Hg.
V d 6: X l mu xc nh As. Dng k thut x l kh vi cht oxi ha mnh. Cn 2g
mu vo chn Pt, Zr, thm 3g KOH, 4g Na 2O2, trn u, un nh cho mu si v chy u v n
khi kh, nung tip 1 gi 650 oC, ngui lau sch bn ngoi chn mu v c chn vo cc
250ml c sn 50ml nc ct un si, lc u, y kn ng h, dn trn bp in cho si, khuy
cho mu tan ht, ly chn nung ra v trng sch chn bng 5 mL nc ct, thm vi mnh s xp
nh, tip tc un si 20 pht na, ui ht H2O2 lc u, lc b b qua giy lc bng . Ly dung
dch lc v nc ra, thm 30 mL HCl 36%, 5 mL acid tartric 10%, nh mc thnh 100 mL. y l
dung dch xc nh Arsen. Cch x l ny c th dng c x l cc mu t bn, trm tch,
qung, b thi rn xc nh As.
V d 7: X l mu bn t xc inh Selen (Se). Dng k thut x l kh vi cht oxy
ha mnh. Cn ly 2 gam mu vo chn Pt hay Zr, thm 3 gam KOH, 4 gam Na 2O2, trn u, un
nh cho mu si v chy u, v n khi kh, nung tip 1 gi 650 0C, ngui, lau sch bn ngoi
chn mu, v th c chn vo cc 250mL c sn 50 mL nc ct un si, lc u, y knh ng
h, un trn bp in cho si, khuy cho mu tan ht, ly chn nung ra v trng sch chn bng 5
mL nc ct, thm vi mnh s xp nh, tip tc un si 20 pht na, ui ht H 2O2 lc u, lc b

b qua giy lc bng . Ly dung dch lc v nc ra, thm 30 mL HCl 36%, nh mc thnh
100 mL. y l dung dch xc nh Selen. Cch x l ny c th dng c x l cc mu t
bn, trm tch, qung, b thi rn xc nh Se.
V d 8: X l mu xc nh hm lng CN -. Trc tin mu c xay nh thnh bt, trn
u, ly 10g vo bnh chit, thm 2 mL NaOH 1M, thm 50 mL nc nng (55-60oC), chnh pH n
9-10 bng NaOH, thm 10 mL huyn ph CuCO 3 (10% trong nc), t vo my siu m trong 5
pht, lc u, ly tm ly dung dch trong xc nh Cu bng AAS, ri suy ra hm lng CN - v
trong qu trnh trn c phng ng to ra phc Cu(CN)3 nh sau:
CuCO3 + 3CN- = Cu(CN)3 + CO32Ngha l 1 mol Cu tng ng vi 3 mol ion CNV d 9: X l mu xc nh hm lng CNS. Trc tin mu c xay nh thnh bt, trn
u, ly 10g vo bnh chit, thm 2 mL NaOH 1M, thm 50 mL nc nng (55-60oC), chnh pH n
0-1 bng HCl, lc u,thm 2 mL FeCl3 5%, t vo my siu m trong 5 pht, lc u, ly tm ly
dung dch phc Fe(CNS) xc nh CNS. Ta chit ly phc Fe(CNS) vo Dietylete hay MIBK
hay CHCl3. Sau xc nh phc ny bng php o ph hp thu phn t trong vng = 480-500
nm.
5.2.2.4. X l b thi phn tch cc cht hu c:
Theo sch cch c trinh by trong chng 2 muc 2.4 chng ta p dng cho x l mu
b thi phn tch cc cht hu c
V d 1: X l xc nh mt s cht hu c c hi. Dng k thut chit rn lng. Ly
10g mu c nghin nh v trn u vo bnh chit, nh ha mu bng 20 mL nc nng, lc
k 5 pht. Thm 20 mL n-Hexan, lc chit 10 pht, tch ly phn hu c, ri lp li vic chit mt
ln na. Gp 2 phn chit n-Hexan li. l dung dch mu xc nh mt s hp cht hu c
c hi, nh nhm cc clo-phenol, cc cht dn xut clo,brom ca cc hydrocacbon thm a vng.
V d 2: Chng ct tch cc hp cht h clo-phenois v pesticide t mu t,b thi [Metho
3550] Ly 10g mu nghin mn vo bnh chng ct, nh ha trong 50mL dung mi hu c, v d
diclo-methylen + n-hexan (1/1), thm 25g Na2SO4 khan, lc k v chng ct ly cht phn tch vo
bnh ngng, lm bay hi ht dung mi bng dng kh nito sch, hay ct quay chn khng n cn
b sn st. Ha tan b cn li trong 5 mL MeOH v xc nh cc cht trong dung dch mu ny
bng phng HPLC hay GC.
V d 3: Chit tch mt s cht hu c thuc h pesticide trong mu t, bn, trm tch,b
thi [Method 3550b] Ly 20g mu nghin mn vo bnh chit thm 30g mui khan Na 2SO4, thm
50mL dung mi chit (diclo-methylen + n-hexan trong t l: V/V = 2/1), trn u, y np v t
vo bungn siu m, ng cht my siu m, chn v cc thng s siu m thch hp chit.
Tin hnh chit trong 50 pht. ngui, ly hn hp mu ra tch pha, ly dung dch pha hu c,
lm bay hi dung mi bng phng ct quay chn khng n khi cn 1mL, ngui, ta c b
t. Ha tan b ny trong 5 mL dung mi MeOH (hay n-hexan). y l dung dch mu xc nh
cc cht trong nhm Pesticaide bng phng php sc k GC, GC-MS hay HPLC.
2.3. X l mu khng kh, khi v bi:
2.3.1. Khng kh, kh quyn v mi trng
Khng kh l mi trng xung quanh chng ta. Khng kh thun khit c thnh phn chnh
l Nit (78.2%), oxy (gn 19.7%), kh CO2 (khong 2%), vmt lng rt nh 5 kh khc khng
ng k (tng di 0.2%), nh ozon (0.000001%), kh NH 3, v.v. ng thi thm vo l cc loi

kh thi ca sn xut cng nng nghip, ca sinh hot ca con ngi. (Xem cc bng 1, 2, A3, A4,..
trong ph lc 1 v 2 cui.)
Nhng trong qu trnh sinh sng v pht trin cng nng nghip v c nghin cu khoa hc,
con ngi thi vo mi trng khng bit bao nhiu cht khc nhau, c cht v c, c cht hu
c, c cht dng kh, nh kh NO 2, SO2, CH4, NH3, cc hi kim loi (Hg, As), bi kim loi, hp
cht c kim (Etyl-Pb). Cc cht dng cc ht bi l lng cng khng t, nh kh nh my in,
nh my xi mng, nh my ha cht, bi khai thc than, khong sn. Trong t hp phong ph v
phc tp , c rt nhiu cht c hi, hay rt c hi vi chnh cuc sng ca con ngi, m c khi
chng ta cha thy c. C cht ph tng kh quyn bo v cho con ngi bi cc tia sng mnh
(cc cht hu c ca F, nh CH2F2, CHF3,..) Ri cc v th v kh, nht l v kh ht nhn. ng
thi cng thi ra mt khi lng khng l cc cht lng d bay hi, cc cht tan vo nc chy ra
cc sng sui. Tt c nhng vic lm a vo khng kh, mi trng sng ca chng ta bit
bao nhiu th m hu qu ang e da con ngi hng ngy.
Bng 9. Thnh phn ca khng kh, kh quyn
Thnh phn cht
Nng (%) (bnh thng) Tng lng (Tn)
N2 (Nit)
78.08
3.90. 109
O2 (Oxy)
20.94
1.20. 109
H2O (Hi nc)
20 100%
50.000 km3 (tng)
Ar (Argon)
0.93
6.70. 107
CO2 (Cacbonic)
0.035
2.80. 106
Ne (Neon)
0.0018
6.60. 104
He (Heli)
0.0005
3.70. 103
CH4 (Metan)
0.00016
4.60. 103
H2 (Kh Hydro)
0.00005
1.70. 102
O3 (Ozon)
0.000004
3.40. 102
NO2 (Dioxit nit)
0.000003
1.60. 102
Vn vn
2.3.2 Ngun gy nhim khng kh v kh quyn.
Hng ngy mi trng xung quanh chng ta lun b nhim do nhiu ngun khc nhau thi vo
khng kh. Cc th thi , c th khng c hi nhng cng c th rt c hi cho con ngi,
ng vt v cy ci ang sinh sng. cc ngun gy nhim c th l
1. Do chnh thin nhin to ra.
Ni la, ng t, sc l ca ni
Nn chy rng
Ging t, gi bo, l lt..
2. Do con ngi to ra
Trong sinh hot hng ngy thi ra, un ci, than t cc th
Do khi v bi ca cc nh my cng nng nghip thi ra
Kh thi ca cc nh my nh ha cht du kh cng nghip
Do xe t v cc phng tin my chy xng du khi thi ra
Nghin cu khoa hc , l phn ng ht nhn.
Chin tranh, th v kh.
Chi cc loi pho, dng thuc n nh c.
Tt c cc th thi vo khng kh xung quanh ta ( kh quyn tri t ), cc th cht thi bao
gm.
1. cc cht v c:
Cc kh CO, CO2, SO2, NO, NO2, Cl2,Br2, H2S, HCN
Cc hi kim loi ( Hg, Pb, Cd, Mn, Cr ), hi mui kim loi
Cc bi silic, amiang, xi mng, bt thy tinh
2. cc loi hp cht hu c.
Mt s hydro cacbua dng kh, aldehyd, alcol, axetylen, aceton..

Cc hp cht c kim, c nguyn t ca Pb, Hg, Cd, Mn, c Halogen

Cc ht cht hu c l lng, cc ht bi rn nh mn.
3. cc loi khi v bi
y l nhm b thi ht mn nh c thi ra khng kh, chng c th sa lng, song cng c th l
lng theo gi i khp ni, lm nh hng n s h hp ca ngi v ng vt n bao gm:
- Ca sinh hot con ngi, un than ci du.
- Ca cc ngnh cng nghip thi ra, in than, in mazut.
- Ca cc phng tin giao thng thi ra.
- cc loi bi ca bom n, pho cc bi phng x
- Nn t rng, dn t rng lm ry
2.3.3 Ly mu khng kh phn tch.
Vic ly mu khng kh nh th no vi dung lng bao nhiu l ty thuc yu cu phn tch cc
cht no, nguyn t no trong khng kh. Mi loi nhm cht c cc cch ring, thu c n
trung thc v ng nht. Song c 1 dng c chung nh my bm ht khng kh, cc cht hp ph
hay giy hp ph, cc dung dch hp ph thu cc cht cn phn tch. C 2 kiu ly khng kh v
bi:
Cch 1: Dng giy hp ph ( thu cht phn tch vo giy lc hay giy xp )
Cch 2: Dng dung dch hp ph ( thu cht vo dung mi )
Chn cch no l ty cht phn tch v iu kin cho php thch hp nht.
V d nh ly cht phn tch kim loi nng c hi, hay phn tch Hg, As ngi ta thng ht khng
kh chy qua giy lc hp ph Whatman No 42 tm t ca hng Whatman vi 1 tc thch
hp trong 1 tjo2i gian nht nhi qua giy lc thng thng l trong vng 250 1000 lt v vi tc
2 4 l/ ph. Khi cc ion kim loi nng hay nguyn t kim loi c trong khng kh s b hp th
v gi li trn giy lc ny. Sau ha tan giy lc, x l t bng axit oxi ha mnh nh HNO 3
H2SO4 l chng ta c mu xc nh cc kim loi trong khng kh. Nhng xc nh cc nhm
kh thuc nhn NO3-, SO42-, CO2 th chng ta phi hp ph chng vo cc dung dch thch hp. V
d dung dich NaOHloa4ng c nng nht nh . Ni chung mi loi cht phi c quy trnh c th
ring cho n [ TCVN. V ISO].
2.3.4 Cch x l mu khng kh v bi phn tch kim loi.
Cc qu trnh cng nghip hng ngy thi vo khng kh v vn cc cht khc nhau, trong c cc
bi kim loi, cc ht bi l lng trong mi trng khng kh ca chng ta phi th v tip xc. Cc
kim loi nng c hi ( As, Cd, Co, Cr,Cu, Fe, Hg, Mn, Ni, Pb, Se, Zn) nu nng ca n vt
khi gii hn cho php th rt nguy hi cho con ngi. V th phi kim tra v pht hin v tm cch
loi tr c khng kh sch.
Mc ch ca ly mu khng kh, bi v x l mu l :
- xc nh kim loi ch yu l kim loi c hi.
- xc nh 1 s kim ( As, Se v anion ( Cl, NO2-, F-) )
- Xc nh 1 s kh c hi ( NO2, SO2, NH3, Hg( CH3 )2)
- Xc nh 1 s cht hu c c hi.
Vic x l mu phn tch cng p dng cc k thut nu trong chng 2. Sau y l 1 s v d
c th.
V d 1: X l mu xc nh cc lim loi nng c hi ( As, Cd, Co, Cr,Cu, Fe, Hg, Mn, Ni, Pb,
Se, Zn).Dng my ht ly 500 lt khng kh cn phn tch qua phu c giy lc Whatman ( No
42E ) vi tc 2l/ph cc ion kim loi v cc ht bi gi li trn giy. B giy c hp ph vo
bnh kendan, them 20 ml HNO 3 65%, lc u, cm vo bnh 1 phu nh di chui v un trn bp
in cho dung dch mu si, ha tan ton b mu v giy n khi no c dung dch trong l
c. Thm 2 ml H2O2 30%, un tip 5 pht ngui bt chuyn hon ton mu sang cc 250 ml,
trng bnh v phu 2 ln bng 15 ml nc ct. un si v lm bay hi n ht axit khi cn mui m.

Ha tan mui m ny bng 10 ml HCl 10%, nh mc thnh 25 ml. l dung dch mu xc

nh cc nguyn t ni trn v cc kim loi kim v kim th. Cch ny nu x l trong l vi song
th cng tt.
V d 2: X l mu khng kh xc nh hm lng tng Hg. Mu xc nh Hg cng c ly
theo cach hp ph vo giy lc Whatman. B giy lc vo bnh kendan, tm t bng 1 ml nc
ct, them 20 ml HNO3 ( 1/1) . 1 ml KMnO 4 5% v 5 git dung dch K 2Cr2O7 2%, lc u cm vo
bnh 1 phu nh di chui v un cch thy bnh kendan, ha tan ton b mu v giy n khi
no c dung dch trong l c. ngui thm tng git dung dch Hydroxilamin kh KMnO 4
d n ht mu tm, thm 2 git K2Cr2O7 10% nh mc thnh 50 ml. l dung dch mu xc
nh Hg bng phng php AAS theo k thut hydride ( ha hi lnh ).
V d 3: X l mu khng kh xc nh hm lng tng As. Mu xc nh As cng c ly theo
cach hp ph vo giy lc Whatman. B giy lc vo bnh kendan, tm t bng 1 ml nc ct,
thm 10 ml H2SO4 98%, 5 ml K2S2O3 10%, lc u cm vo bnh 1 phu nh di chui v un cch
thy bnh kendan, ha tan ton b mu v giy n khi no c dung dch trong l c.
ngui, chuyn ton b mu ra cc 250ml trng 2 ln bnh v phu bng 10 ml nc ct un si cho
per sunphat phn hy ht, thm 1 ml K 2Cr2O7 10% nh mc. l dung dch mu xc nh As
nu x l bng l vi sng th cng tt.
V d 4: X l mu xc nh 1 s kh c hi ( SO 2, NO2, Cl)Ba cht ny c xc nh theo 3
cch khc nhau, v vy khi x l mu cng c x l theo 3 cch khc nhau cho cc cht . V
d:
- Xc nh tng (SO2, NO2 ), hp thu vo dung dch NaOH.
- Xc nh ring SO2 th s dng dng kt ta BaSO4.
- Xc nh ring NO2 hp th vo dung dch to phc diazo v o quang.
- Xc nh ring Clo. Phng php kt ta cng AgX vi AgNO3.
Cc cht ny u phi cho hp th vo dung dch kim NaOH c nng bit v c thuc th
thch hp. Sau xc nh lng kim d. Ri suy ra hm lng ca cc cht .
V d: xc nh Clo: dung my ht khng kh vi tc 2l/ph vo bnh ng mu c cha 30 ml
dung dch AgNO3 2000ppm Ag, trong mi trng HNO 3 2% n khi 500 lt i vo. Sau un
si nh mu, ly tm hay lc kt ta, ly dung dch nh mc thnh 50 ml, xc nh lng Ag cn
d bng php o ph AAS ca Ag. T lng d ca Ag, ta tnh c lng Ag phn ng vi Cl
v suy ra hm lng ca Cl trong mu.
Mt s v d khc c th xem trong TCVN.
2.3.5 Cch x l mu khng kh phn tch cht hu c.
X l mu xc nh hi ca cac cht c hi trong khng kh ngi ta thng dung phng php
hp th cc cht vo trong dung mi hu c vi 1 dung mi thch hp v thuc th hu c thch
hp, hay chit vo dung mi hu c, da trn c s mi nhm cht s tan tt vo 1 trong nhng
dung mi hu c khi ngi ta cho kh i qua v i vo trong dung mi .
Hp th vo dung mi n hexan, dietyl eter, benzene, CHCl3, CCl4.
Hp ph vo silicagel ct.
V d 1: chit tch cc hp cht carbonyl ( aldehyd v ceton ) bay hi trong khng kh. Mu
khng kh c dn chit vo ct chit silicagel xp c ch ha trc vi dung dch ca 2,4
dinitrophenylhydrazin , pH=2 vi tc 3 4 l/ph. Trong qu trnh ny cc aldehyd c gi li
ct chit tnh theo cht hp ph ca silicagel v to ra cc sn phm th ha ca aldehyd. V d nh
formaldehyde dinitrophenylhydrazone c gi li trn ct. Sau cht phn tch c ra gii
trn ct bng 10 ml acetonitril hay diclomethane v xc nh cc cht trong dch ra ny bng
HPLC, GC hay ph UV VIS.

V d 2: chit tch cac cht bo v thc vt trong khng kh nh my sn xut cc kh ny. Mu

khng kh.Mu khng kh c dn chit vo ct chit VDL silicagel vi tc 3 4 l/ph. Trong
qu trnh ny cc pesticide c gi li ct chit tnh theo cht hp ph ca silicagel ny. Sau
cht phn tch c ra gii trn ct bng 10 ml diclomethane c 20% n hexane v xc nh cc
cht trong dch ra ny bng HPLC, GC hay ph UV VIS.
Mt s v d khc c th xem trong chng 4 trn.
2.4 X l mu t bn v trm tch.
2.4.1 Khi nim t ,bn v trm tch.
t, bn v trm tch l nhng dng tn ti ca a quyn n tn ti xung quanh chng ta. Chng ta
hng ngy sng v sinh hot , lm vic u trn mt t. N cng thng xuyn b nhim do
nhiu ngun khc nhau v cng c tc ng li n cuc sng ca chng ta v ca cc sinh vt sng
trn mt t v di nc. v con ngi sng trn mt t v lun lun tip xc vi t t lc sinh
cho n lc cht. V th nu t b nhim th con ngi, cy ci cng b nh hng. Cn bn l
ni c tr ca nhng loi c, nn khi bn b nhim th n cng s b nh hng, c th c cng s
chtt nu c cht c hi, nng. Nhng nhiu trng hp c khng cht m tch t vo c th c
ngi b nhim c khi n phi c b nhim c.
2.4.2 Ngun gy nhim cho t v bn.
S nhim ca t v bn c th l do nhiu ngun khc nhau, v d nh cc ngun sau:
1. cc cht thi ca cc nh my sn xut hot ng thi cc th cn b ra mt t tri
xung song h, sau lng xung bn.
2. cc th thi ca cc ngnh khai thc khong sn, nguyn liu ra mt t, ri tri
xung sng h sa lng lm nhim bn cho bn.
3. Cc cht thi ca nng nghip, chn nui gia sc nh b tha, phn ng vt, nc
thi ra chung tri, thuc tr su dit c.
4. Cuc sng sinh hot ca con ngi thi ra, nht l rc thi th, rc thi ca bnh
vin.
5. ng vt, vi sinh vt sng pht trin loi thi ra.
6. Do going t, bo lt, ni la, nn chy rng.
7. Cc th sn phm ca v kh ha hc, v kh ht nhn.
2.4.3 ly mu t bn v trm tch.
Vn ny xem trong chng I v cc phng php ly mu phn tch. V mu mi trng dng l
mu phn tch theo cc tiu chun Xx v tiu chun ISO.
2.4.4. Cch x l mu t bn phn tch kim loi v ion v c:
t v bn l cc mu v c, nhng c cha thm c cht hu c, m ch yu l cht mn hu c.
Vic x l mu cng l :
- Xc nh mt s kim loi, ch yu kim loi c hi.
- Xc nh mt s kim v anion.
- Xc nh mt s cht hu c c hi v cc cht bo v thc vt.
Ty theo nhim v phn tch cc cht, v d phn tch cc kim loi, kim v anion, ngi ta
thng s dng cc k thut:
- X l t vi acid c tnh oxy ha mnh.
- X l kh c cht bo v trong kim mnh.
Chi tit v cc k thut ny hy xem trong chng II trn.
Cn xc nh cc cht hu c ngi ta hay dng:
- Cc phng php chit lng-lng, rn-lng, rn-kh.
- Cc phng php chng ct
Chi tit v cc k thut ny hy xem trong chng II trn. Sau y l mt s v d c th:

V d 1: X l mu ly cc kim loi nng c hi trong t bn, v trm tch. Ngi ta

thng dng phng php x l t thng thng, hay x l t trong l vi sng. V loi mu ny
cng tng t nh cc mu qung, t , b thi rn. hy xem trong cc v d trnh by trong
chng III v chng IV trn, nh v d (trang ), v d (trang ). Cn xc nh mt s anion v c
xem trong v d (trang ), v d (trang ) v cc mu qung, t v b thi.
V d 2: X l mu bn t xc inh Hg. Dng k thut thng hoa ly Hg. Ly 2 gam
mu vo bnh thng hoa Hg (xem hnh v), thm 1 gam bt Fe, 2 gam CaO, trn u, qun phn
ng ngng Hg bng vi tm tuyt CO2 hay nc . Kp hay t nm ngang ng. un nh bu bnh
cha mu, cho nng u v chy bng n kh, xoay trn u ng khi un. Lc ny Hg bay hi v
ngng vo thnh ng. Sau khi ton b hn hp chy u v mu l khi mu nu, un thm 3
pht. Tch b bu cha mu, ly ng ngng v nhng vo ng nghim c cha 15 mL dung dch
HNO3 1:1 nng (khong 750C). Lc u mt pht, ly dung dch thm 2 git dung dch K 2Cr2O7
1%. nh mc thnh 50 mL. dung dch xc nh Hg. Cch x l ny c th dng c x
l cc mu t bn, trm tch, qung, b thi rn xc nh Hg.
V d 3: X l mu bn t xc inh As. Dng k thut x l kh vi cht oxy ha mnh.
Cn ly 2 gam mu vo chn Pt hay Zr, thm 3 gam KOH, 4 gam Na 2O2, trn u, un nh cho mu
si v chy u, v n khi kh, nung tip 1 gi 650 0C, ngui, lau sch bn ngoi chn mu, v
th c chn vo cc 250mL c sn 50 mL nc ct un si, lc u, y knh ng h, un trn
bp in cho si, khuy cho mu tan ht, ly chn nung ra v trng sch chn bng 5 mL nc ct,
thm vi mnh s xp nh, tip tc un si 20 pht na, ui ht H2O2 lc u, lc b b qua giy
lc bng . Ly dung dch lc v nc ra, thm 30 mL HCl 36%, 5 mL acid tartric 10%, nh
mc thnh 100 mL. y l dung dch xc nh Arsen. Cch x l ny c th dng c x l
cc mu t bn, trm tch, qung, b thi rn xc nh As.
V d 4: X l mu bn t xc inh Selen (Se). Dng k thut x l kh vi cht oxy
ha mnh. Cn ly 2 gam mu vo chn Pt hay Zr, thm 3 gam KOH, 4 gam Na 2O2, trn u, un
nh cho mu si v chy u, v n khi kh, nung tip 1 gi 650 0C, ngui, lau sch bn ngoi
chn mu, v th c chn vo cc 250mL c sn 50 mL nc ct un si, lc u, y knh ng
h, un trn bp in cho si, khuy cho mu tan ht, ly chn nung ra v trng sch chn bng 5
mL nc ct, thm vi mnh s xp nh, tip tc un si 20 pht na, ui ht H 2O2 lc u, lc b
b qua giy lc bng . Ly dung dch lc v nc ra, thm 30 mL HCl 36%, nh mc thnh
100 mL. y l dung dch xc nh Selen. Cch x l ny c th dng c x l cc mu t
bn, trm tch, qung, b thi rn xc nh Se.
V d 5: X l mu xc nh mt s anion trong mu t, bn, trm tch, ngi ta thng
dng phng php x l t trong l vi sng hay phng php x l kh trong kim mnh KOH v
cht oxy ha Na2O2 xc nh anion. Hy xem trong v d XXX
V d 6: X l mu xc nh mt s anion S trong t, bn, trm tch v b thi
[Mehod.3550].
Ly 10 g mu nghin thnh bt, cho vo bnh chng ct, (hnh 4.35), nh ha bng 100
mL nc ct, lc u, lp h thng chng ct cho kn, cho nc lm lnh (nc ngng) chy vi tc
2 mL/pht. un bnh mu cho si X tan u, sau khng ch khong 70-80 oC, ri nh t t
acid H2SO4 4M vo tng git (n ht 20 mL), v sc kh nito tinh khit vo bnh un vi tc 3
bong bng trong 1 giy trong khi ct, ui kh H 2S sang bnh hng B c cha 20 mL dung dch
CdCl2 0.02M (c pH = 0). Chng ct 30 pht l xong, ngui, ly bnh hng B ra xc nh
lng d bng phng php ph XX, t bit c lng Cd tc dng vi ion S: H 2S) v
tnh c hm lng ion S trong mu.
2.4.5. X l xc nh cc cht hu c c hi:

Mu mi trng n bao gm c mu hu c v v c. V th xc nh cc cht hu c

trong cc loi mu ny, chng ta c th p dng tt c cc phng php v k thut c trnh
by trong chng 2. Sau y l trnh by thm mt vi v d na.
V d 1: X l xc nh mt s cht hu c c hi. Dng k thut chit rn lng. Ly
10g mu c nghin nh v trn u vo bnh chit, nh ha mu bng 20 mL nc nng, lc
k 5 pht. Thm 20 mL n-Hexan, lc chit 10 pht, tch ly phn hu c, ri lp li vic chit mt
ln na. Gp 2 phn chit n-Hexan li. l dung dch mu xc nh mt s hp cht hu c
c hi, nh nhm cc clo-phenol, cc cht dn xut clo,brom ca cc hydrocacbon thm a vng
(Xem thm trong v d 4 trong mc 4.2.2.1, v d 2 trong mc 4.2.2.2.5 v v d 3 trong mc
4.2.2.2.7 trong chng 4 trn.)
V d 2: Chng ct tch cc hp cht h clo-phenois v pesticide t mu t,b thi [Metho
3550] Ly 10g mu nghin mn vo bnh chng ct, nh ha trong 50mL dung mi hu c, v d
diclo-methylen + n-hexan (1/1), thm 25g Na2SO4 khan, lc k v chng ct ly cht phn tch vo
bnh ngng, lm bay hi ht dung mi bng dng kh nito sch, hay ct quay chn khng n cn
b sn st. Ha tan b cn li trong 5 mL MeOH v xc nh cc cht trong dung dch mu ny
bng phng HPLC hay GC.
V d 3: Chit tch mt s cht hu c thuc h pesticide trong mu t, bn, trm tch,b
thi [Method 3550b] Ly 20g mu nghin mn vo bnh chit thm 30g mui khan Na 2SO4, thm
50mL dung mi chit (diclo-methylen + n-hexan trong t l: V/V = 2/1), trn u, y np v t
vo bung siu m, ng cht my siu m, chn v cc thng s siu m thch hp chit.
Tin hnh chit trong 50 pht. ngui, ly hn hp mu ra tch pha, ly dung dch pha hu c,
lm bay hi dung mi bng phng ct quay chn khng n khi cn 1mL, ngui, ta c b
t. Ha tan b ny trong 5 mL dung mi MeOH (hay n-hexan). y l dung dch mu xc nh
cc cht trong nhm Pesticaide bng phng php sc k GC, GC-MS hay HPLC.
2.5 X l cc mu rong ru sng trong nc.
2.5.1 Khi nim v mu loi ny.
Rong ru l cc loi thc vt thn mm sng trong cc ngun nc.chng c th sng st mt bn
v trm tch sng h hay sng l lng trong nc, hoc sng bm vo cc vt khc hay cy kha qc
tn ti trong nc nh v tu thuyn, bm vo ct cu, thnh cng , mng mng dn nc hoc
cng c th tri theo dng ncrong ru c nhiu loi v rt a dng , n ph thuc vo mi loi
ngun nc khc nhau. Song y chng ta khng bn n vn ny m ch quan tm chnh l
vn n b nhim th no khi cc ngun nc khng cn trong sch na.Nc v cc th tn ti
trong nc, nh cc cht v c, hu c chnh l ngun dinh dng ca rong ru.m rong ru li l
ngun dinh dng ca ng vt sng di nc. V th nu nc b nhim th cc loi thc vt v
ng vt sng di u b nhim c theo.do khi nh gi s nhim ca ngun nc th cng
phi xem xt lun c cc loi thc vt ny c c nh gi ton din v ng n.
2.5.2 Cc ngun gy nhim cho rong ru.
V cc loi rong ru sinh sng trong nhng ngun nc nn mi yu t lm nhim nhng ngun
nc u c th lm cho rong ru cng b nhim theo. Song tt nhin tng loi rong ru v bn
cht sinh sng ca n m n b nhim c hi l khc nhau.Do cc ngun lm nhim ngun
nc cng chnh l cc yu t lm rong ru b nhim c hi.Nhng cng c thc t l 1 s loi
rong ru trong qu trnh sinh sng v pht trin n cng ly i mt mt s cht hu c c hi trong
nc lm gim bt s nhim c hi ca nc. Do thc t ny, hin nay nhiu nc pht trin nh
Php, c, H Lan nghin cu v nui 1 s loi rong ru v vi khun c li th vo cc ngun
nc sng, sui, ao h n kh cc cht c hi trong ngun nc. Nhng cng c khng t cht
c hi ch lm cht hi rong ru v vi sinh c li trong nc, nh cc acid v c ( HCl, H 2SO4, HF,
HBr) Cc cht hu c bo v thc vt ( thuc tr su, dit c, dit cn trng) V th cn phi
theo di pht hin v loi tr cc cht c hi ny.

2.5.3 X l mu xc nh kim loi v anion v c.

Rong ru l cc mu thc vt, n l thuc nhm cc mu hu c do cch x l ny xc nh
cc kim loi v cc cht v cchng ta c th p dng cc phng php nu trong chng
trnv cc phng php x l cc mu hu c tng t nh cc loi rau qu ti xc nh kim
loi v mt s anion v c.
2.5.4. X l mu xc nh mt s cht hu c
Rong ru l cc mu thc vt, n l thuc nhm cc mu hu c. Nh vy y tc l x l mu
xc nh cht hu c trong mu hu c. Do cch x l mu ny xc nh cc hu c, chng
ta c th p dng cc phng php nu trong chng 4 trn v cc phng php x l cc mu
hu c xc nh cc cht hu c cc loi.

TI LIU THAM KHO:

1. Markas Stoeppler (Ed.)
Sampling and Sample Preeparation
(Practical Guide for Analytical Chemists)
2. Phm Lun & Steve Morton
In brief about Sample and techniques for Sample Treatment for AAS
University of Amsterdam 1993
3. Daniel C. Harris
Quantitative Chemistry Analysis. Chapper 28
Fifth Edition W.H.Freeman and Company. New York 1998
4. Stanley E. Manahan
Enviromental Chemistry Sixth Edition 1994
Lewwis Publ. Boca Raton Ann Arbor. London Tokyo
5. Douglas A.Skoog, Donald M. west & F James Holler
Fundamentals of Analytical Chemistry Chapper 32
Seventh Edition 1995, Sauders College Publ
New York, Toronto, London
6. Trung tm o to ngnh nc v mi trng
S tay x l nc Tp I & II
(Bn dch t ting Php: Memento Techbique Lcau)
NXB Xay dng H Ni 1999
7. O.G. Koch & G.A. Koch- Dedic
Handbuch der Spurenanalyse Teil 1&2
Fourth Edition 1989
NXb Springer Berlin, Heideibeg & New York
8. Company Perkin Elmer
Analytical methods for metal ions
Perkin Elmer Company 1988, 1996
9. Phm Lun
S tay v d v x l mu phn tch
HTH H Ni 1994
10. J.T. Baker Chemistry Company
Guide and Application Notes for Solid Phase Extraction (SPE) Vol I&II
J.T. Baker Chemical Company (USA) 1996