1

MC LC
LI CM N.........................................................................................................
MC LC................................................................................................................1
M U...................................................................................................................4
1. L do chn ti..................................................................................................4
2. Mc tiu v nhim v nghin cu ti.............................................................4
3. Cc phng php nghin cu..............................................................................4
4. i tng v khch th ca ti nghin cu....................................................5
5. Gi thuyt khoa hc............................................................................................5
6. Lch s ti nghin cu....................................................................................5
7. Gii hn ti nghin cu..................................................................................5
NI DUNG ..............................................................................................................6
CHNG 1: TNG QUAN
1.1

S lc v nguyn t st.................................................................................

1.1.1 V tr v cu to ca st...................................................................................6
1.1.2

Tnh cht vt l v tnh cht ha hc..................................................6

1.1.3

Trng thi thin nhin v phng php iu ch...............................9

1.1.4

Mt s ng dng ca st.....................................................................10

1.2

S to phc ca st vi thuc th hu c..................................................11

1.2.1

Kh nng to phc ca Fe3+ vi thuc th axit sunfosalixilic..........11

1.2.2

Kh nng to phc ca Fe vi cc thuc th khc...........................11

1.2.2.1

. Thuc th SCN-...................................................................................11

1.2.2.2

.Thuc th o phenantrolin.................................................................13

1.2.2.3

.Thuc th bato phenantrolin............................................................13

1.2.2.4

.Thuc th 1 (2pyridylazo) 2naphthol (PAN)..............................14

1.2.2.5

. Thuc th 4 (2pyridylazo) rezocxin (PAR)...................................14

1.2.2.6

.Thuc th trioxyazobenzen (TOAB)...................................................15

Nghin cu v thuc th axit sunfosalixilic................................................16

1.3
1.3.1

Tnh cht ca thuc th axit sunfosalixilic........................................16

1.3.2

Kh nng to phc ca axit sunfosalixilic.........................................17

Cc phng php xc nh st.....................................................................17

1.4
1.4.1

Phng php khi lng....................................................................17

1.4.2

Phng php trc quang.....................................................................17

1.4.3

Phng php chun oxi ho kh..................................................18

1.4.4

Cc phng php khc xc nh st..................................................19

Cc phng php xc nh thnh phn phc............................................19

1.5
1.5.1

Phng php h ng phn t gam...................................................19

1.5.2

Phng php t s mol........................................................................19

Cc phng php xc nh h s hp th phn t ca phc...................19

1.6
1.6.1

Phng php h ng phn t gam...................................................19

1.6.2

Phng php x l thng k ng chun........................................20

1.6.3

Phng php Komar...........................................................................20

1.7

nh gi cc kt qu phn tch....................................................................21

CHNG 2: K THUT THC NGHIM

2.1 Dng c v thit b.........................................................................................22
2.2 Ha cht v cch pha ...................................................................................22
2.3 Cch tin hnh...............................................................................................23
2.4 Phng php nghin cu..............................................................................23
CHNG 3: KT QU V THO LUN
3.1 Kho st ph hp th ca phc...................................................................24
3.2 Kho st pH ti u v nh hng ca pH n s to phc.....................26
3.3 Kho st s nh hng ca thi gian n s to phc.............................27
3.4 Xc nh thnh phn phc...........................................................................29
3.4.1. Xc nh thnh phn phc khong pH th nht................................29

3.4.2. Xc nh thnh phn phc khong pH th hai.................................33

KT LUN..............................................................................................................38
Ti liu tham kho..................................................................................................39

M U
1.

L do chn ti
Trong cng ngh Ha hc th ha hc phn tch khng nh c vai tr ca mnh

qua vic s dng cc phng php ha hc, vt l, ha l khi nghin cu thnh phn
ca cht. Mt trong nhng phng php t c nhng thnh tu to ln trong khoa hc
nghin cu l phng php trc quang khi xc nh hm lng ca cc nguyn t, cc
cht v hp cht.
Vi nhng thnh tu t c t phng php trc quang m ra nhng c hi
mi cho vic nghin cu, i su hn tm hiu v ng dng ca phng php ny trong
thc tin, tm ra cc yu t nh hng,. V vy m ti chn ti: Nghin cu nh
hng ca pH n s to phc ca Fe3+ vi axit sunfosalixilic (SSal) lm bi kha
lun tt nghip .
2.

Mc tiu v nhim v nghin cu ti

2.1

.Mc tiu:

- Bit c vai tr ca phng php trc quang trong ha hc phn tch.

- Xc nh thnh phn ca phc st (III) vi axit sunfosalixilic bng phng php trc
quang.
- Vn dng phng php ny trong vic nghin cu nh hng ca pH n s to phc
ca Fe3+ vi axit sunfosalixilic (SSal)
2.2

.Nhim v:

ti cn thc hin cc nhim v trng tm sau:

- Nghin cu phng php trc quang trong ha hc phn tch.
- Nghin cu nh hng ca pH n s to phc ca Fe3+ vi axit sunfosalixilic (SSal)
3.

Cc phng php nghin cu

+ Nghin cu l lun: nghin cu cc ti liu, cc trang web, bi vit,.c lin quan

+ Nghin cu thc nghim:

- Tm hiu nguyn l hot ng ca my o mt quang

+ Nghin cu ton hc: v biu , th, phng php ly gi tr trung bnh, cng
thc ton hc thng k,.
4.

i tng v khch th ca ti nghin cu

.i tng:

4.1

i tng nghin cu ca ti l nh hng ca pH

4.2

.Khch th:

S to phc ca Fe3+ v axit sunfosalixilic (SSal )

5.

Gi thuyt khoa hc
ti nghin cu nh hng ca pH n s to phc ca Fe 3+ vi axit sunfosalixilic (

Fe(III) - SSal) bng phng php trc quang.

Nu ti nghin cu thnh cng, c th p dng cho vic xc nh hm lng Fe
trong rau mung v mt s cht khc.
6.

Lch s ti nghin cu
ti ny c nghin cu nhng ch dng li ch xc nh thnh phn phc

ca Fe(III) - SSal bng phng php trc quang. Ti chn ti ny tip tc nghin
cu v nh hng ca pH n s to phc ca Fe3+ vi axit sunfosalixilic ( Fe(III) SSal
) v tm ra mt s h s thch hp.
7.

Gii hn ti nghin cu
ti c thc hin trong phm vi:

Nghin cu phng php trc quang trong ho hc phn tch.

Nghin cu nh hng ca pH n s to phc ca Fe(III) SSal.

NI DUNG

CHNG 1: TNG QUAN

1.1 .S lc v nguyn t st
1.1.1

V tr v cu to ca st

St l mt nguyn t kim loi ph bin (sau nhm), ng th t v hm lng tri

t, chim 1,5% khi lng v tri t.
K hiu : Fe
S th t: 26
NTK

: 55,847

Cu hnh electron: 1s22s22p63s23p63d64s2

St th 26 , thuc chu k 4 v phn nhm ph VIIIB
1.1.2

Tnh cht vt l v tnh cht ha hc

1.1.2.1. Tnh cht vt l:

St l kim loi mu trng xm, d rn, d dt mng v gia cng c hc. St c tnh
dn in, dn nhit tt. Di 8000C st c tnh nhim t, b nam chm ht v tr thnh
nam chm (tm thi).
St c 4 dng th hnh ( dng , , , ) bn nhng khong nhit nht nh:
0

C
C
C
C
Fe () 700

Fe () 911

Fe () 1390

Fe () 1538

Fe lng

Nhng dng v c kin trc tinh th kiu lp phng tm khi nhng c kin trc
electron khc nhau nn Fe () c tnh st t v Fe () c tnh thun t, Fe () khc vi Fe
() l khng ha tan C. Dng Fe () c cu trc tinh th lp phng tm din, dng Fe
() c cu trc lp phng tm khi nh dng v nhng tn ti n nhit nng
chy.

Cc hng s vt l quan trng ca st:

dn

tos (oC)

tonc (oC)

BKNT

1536

(Ao)
1,26

in
1,83

in(Hg=1)
10
2880
Nng lng ion ha:

KLR

cng

(g/cm3) (thang Mox)

7,91
4-5

Mc nng lng

I1

I2

I3

I4

I5

I6

ion ha
Nng lng ion

7,9

16,18

30,63

56*

79*

103

ha (eV)
* Gi tr cha tin cy.
1.1.2.2. Tnh cht ha hc:
St l kim loi c hot tnh ha hc trung bnh. iu kin thng nu khng c hi
m, chng khng tc dng r rt vi nhng nguyn t khng kim loi in hnh nh O2
, S , Cl2 , Br2 v c mng oxit bo v. Nhng khi un nng, phn ng xy ra mnh lit,
nht l khi kim loi trng thi chia nh.
Khi un nng trong khng kh kh, st to nn Fe2O3 v nhit cao hn, to nn
Fe3O4:
3Fe + 2O2

Fe3O4

Kh Cl2 phn ng rt d dng vi st to thnh FeCl3 l cht d bay hi nn khng to

c mng bo v:

2Fe + 3Cl2 2FeCl3

St tc dng trc tip vi kh CO to thnh cacbonyl kim loi. St tinh khit bn

trong khng kh v nc. Ngc li, st c cha tp cht b n mn di tc dng ca
hi m, kh cacbonic v oxi trong khng kh to nn g st:
4 Fe + 3O2 2Fe3O4
do lp g st xp v gin nn khng bo v st trnh b oxi ha tip.
St phn ng vi nc: nhit nng , st phn ng vi hi nc:
O

570 C
Fe + H2O

FeO + H2
0

570 C
3Fe + 4H2O Fe3O4 + 4H2

St to thnh hai dy hp cht Fe2+ v Fe3+. Mui Fe2+ c to thnh khi ha tan st
trong dung dch axit long tr axit HNO3. Mui ca Fe2+ vi axit mnh nh: HCl, H2SO4,
d tan trong nc, cn mui ca cc axit yu nh: FeS, FeCO3, kh tan. Khi tan
trong nc, mui st dng [Fe(H2O)6]2+ mu lc nht. Mu lc ca [Fe(H2O)6]2+ rt yu
nn thc t dung dch ca mui Fe2+ khng c mu. Mui FeSO4 l cht tinh th mu
trng, d ht m v d tan trong nc. Khi kt tinh t dung dch nc nhit thng,
thu c tinh th hidrat FeSO4.7H2O. Tinh th FeSO4.7H2O c mu lc nht, nng chy
nhit 640C, d tan trong nc v ru. Khi un nng tinh th FeSO4.7H2O mt dn
nc v tr thnh mui khan FeSO4. nhit cao hn (>5800C) mui khan b phn
hu thnh oxit:
0

580 C
FeSO4
Fe2O3 + SO3 + SO2

Quan trng vi thc t nht l (NH4)Fe(SO4)2.6H2O, c gi l mui Mohr. Tinh th

mui Mohr c mu lc, d kt tinh, khng ht m v bn vi oxi khng kh nn c
dng pha dung dch chun Fe2+ trong ho hc phn tch.
Fe(OH)3 bn trong khng kh, khng tan trong nc v trong dung dch NH3. Fe(OH)3
tan d dng trong axit to thnh dung dch mui Fe3+. a s mui Fe3+ d tan trong nc,
cho dung dch cha ion bt din [Fe(H2O)6]3+ mu tm nht. Khi kt tinh t dung dch
nc, mui Fe3+ thng dng tinh th hidrat nh: FeCl3.6H2O, Fe(NO3)3.9H2O mu
nu vng, phn st (NH4)Fe(SO4).12H2O mu tm nht Mui Fe3+ b thu phn mnh
nn dung dch c mu vng nu. Ch trong dung dch c phn ng axit mnh (pH<1) s
thu phn mi b y li. Cc mui st Fe3+ cng d b kh v mui Fe2+ bng nhiu cht
kh khc nhau nh: HI, N2H4 , .
2FeCl3 + 2HI 2FeCl2 + I2 + 2HCl
Fe2O3 c mu nu , c iu ch bng cch nung kt ta Fe(OH)3 . Fe2O3 khng
tan trong nc, c th tan mt phn trong kim c hay cacbonat kim loi kim nng
chy.

Ion Fe3+ trong dung dch tc dng vi ion SCN- to nn mt s phc thioxianat. Ho
phn tch thng s dng phn ng ny nh tnh v nh lng Fe3+ ngay c trong
dung dch long.
Kaliferixianua (K3[Fe(CN)6]) l mt trong cc phc bn nht ca st. Kaliferixianua
l cht dng tinh th n t, mu thng c gi l mui mu. Phc ny d tan
trong nc, cho dung dch mu vng v rt c. Kaliferixianua l mt thuc th thng
dng trong phng th nghim nhn bit Fe2+ trong dung dch:
FeCl2 + K3[Fe(CN)6] KFe[Fe(CN)6] + 2KCl
KFe[Fe(CN)6] kt ta mu xanh chm v c gi l xanh Tuabin. Kaliferixianua khi
un nng trong dung dch kim chuyn thnh Kaliferoxianua:
4K3[Fe(CN)6] + 4KOH 4K4[Fe(CN)6] + 2H2O + O2
1.1.3. Trng thi thin nhin v phng php iu ch
St l mt trong nhng nguyn t ph bin nht, ng th 4 sau O, Si, Al. St
trng thi t do trong cc mnh thin thch v cc khong vt,
Trong t nhin st c bn ng v bn: 54Fe (5,8%) , 56Fe (91,8%) , 57Fe (2,15%) ,
58

51

Fe (=0,25 giy) ,

52

Fe (=44,6 ngy) ,

60

Fe (0,25%). Ngoi ra st cn c tm ng v phng x:

(=8,27 gi),

53

Fe (=258,8 ngy) ,

55

Fe (=2,7 nm) ,

59

Fe
Fe

(=1,5.106 nm) , 61Fe (=182,5 ngy) , 62Fe (=68 giy). Nhng khong vt quan trng
ca st l manhetit (Fe3O4) cha n 72,42 % st, hematit (Fe2O3) cha 60% st, pirit
(FeS2) cha 46,67 % st v xiderit (FeCO3) cha 35% st. Ngoi nhng m ln tp
trung, st cn phn tn trong khong vt ca nhng nguyn t ph bin nh nhm,
titan, mangan, St cn c trong nc thin nhin, trong cc thin thch t khng gian
v tr ri xung tri t. Trung bnh trong 20 thin thch ri xung th c mt thin
thch st (cha 90% st).
Nhiu nc trn th gii c giu qung st nh: Thy in, Nga, Php, Ty Ban
Nha, Trung Quc, M, Canada, Cuba, Brazin, Nam Phi, Cch y hn 4000 nm, loi
ngi bit luyn st t qung. St luyn c cng v bn hn bronz nn l vt liu

10

cnh tranh vi bronz. Cch y khong 3000 nm thi i st thay th thi i

ng thic v tip tc pht trin cho n ngy nay.
My th k nay, st c sn xut vi quy m cng nghip bng l cao.
1.1.4. Mt s ng dng ca st
St l mt nguyn t vi cht dinh dng quan trng cho sc kho con ngi. Hu ht
lng st c trong c th u tn ti trong cc t bo mu, chng kt hp vi protein to
thnh hemoglobin. Hemoglobin mang oxi n cc t bo ca c th v chnh cc t bo
ny nng lng c gii phng. Do vy khi thiu st hm lng hemoglobin b gim
lm cho lng oxi ti cc t bo cng gim theo. Bnh ny gi l bnh thiu mu do
thiu ht st. Cc triu chng ca bnh thiu mu do thiu st l: mt mi, tnh lnh
m, yu t, au u, n khng ngon v d cu gin.
Vic tha st trong c th cng c nhng tc hi nh vic thiu st. Nu lng st
trong c th tha nhiu, chng gy nh hng c hi cho tim, gan, khp v cc c quan
khc, nu tch tr qu nhiu c th gy nguy c b ung th. Nhng triu chng biu hin
s tha st c th thy l:
-

T tng b phn tn hoc mt mi

Mt kh nng iu khin sinh l

Bnh v tim hoc tim b lon nhp p

Chng vim khp hoc au cc khp.

Bnh thiu mu khng phi do thiu st.

Bnh v gan hoc ung th gan.

Tt kinh sm ( n gii) hoc bnh lit dng ( nam gii).

Trong hu ht cc ngnh k thut hin i u c lin quan ti vic s dng st v

hp kim ca st. Nh chng ta bit, trong cng nghip cc hp kim ca st ng vai tr

ch cht trong cc lnh vc: xy dng, giao thng vn ti, quc phng, ch to my,
dng c sn xut v dng hng ngy, FeSO4 c dng chng su b c hi cho
thc vt, c dng trong vic sn xut mc vit, trong sn v c v trong nhum vi;

11

n cn dng ty g kim loi v c kh nng ho tan Cu2S to thnh CuSO4 c dng

iu ch ng bng phng php thu luyn. St l nguyn t quan trng cho s sng
v cng nghip. V th ngi ta tm nhiu cch thc v phng php tch v lm giu
nguyn t ny.
1.2. S to phc ca st vi thuc th hu c
1.2.1

Kh nng to phc ca Fe3+ vi thuc th axit sunfosalixilic

Fe3+ + m SSal [ Fe(SSal)m ](3-2m)+

i vi Fe2+ axit sunfosalixilic to phc vi Fe2+ c mu ph thuc vo nng axit

ca dung dch v c:
pH
1,5
5

max ( nm )
500
460

SSal c s dng rng ri xc nh Fe2+ trong khong pH = 2,0 2,8; trong mi

trng axit, hoc xc nh tng lng Fe2+ v Fe3+ trong mi trng kim.
i vi Fe3+ , ty thuc vo pH m phc to thnh c thnh phn nh th no v
cc bc sng khc nhau:
pH
Mi trng
Phc
Mu
max (nm)
+
1,8 - 2,5
axit
Fe[SSal]
tm
510
4-8
m axetat [Fe(SSal)2]
da cam
490
39 - 11
m amoni [Fe(SSal)3]
Vng da cam
420 - 430
> 12
Ba z
Phn hy
pH > 12 phc b phn hy do xy ra s hnh thnh phc hidroxo.
1.2.2
1.2.2.1

Kh nng to phc ca Fe vi cc thuc th khc

.Thuc th thioxianat (SCN-)

Thioxianat l mt thuc th nhy i vi Fe3+, c dng nh tnh v nh lng

hm lng st. V axit thioxianat l mt axit mnh nn nng SCN- t b nh hng
bi pH trong dung dch. Cng mu ca Fe3+ SCN- hp th cc i bc sng
= 480 nm, dung dch phc Fe3+ SCN- b gim mu khi ngoi nh sng, tc gim
mu chm trong vng axit yu v nhanh khi nhit tng. Khi c mt H2O2 hoc

12

(NH4)S2O8 cng lm cho cng mu v bn mu ca phc gim i. Khi nng

SCN- ln khng nhng n lm tng nhy ca php o m cn loi tr c nh
hng ca cc ion F-, PO43- v mt s anion khc to phc c vi ion Fe3+. Trong mi
trng axit c nhng ion gy nh hng n vic xc nh Fe

3+

bng SCN- nh C2O4 ,

F- . Ngoi ra cn c cc ion to phc mu hay kt ta vi ion thioxianat nh Cu2+, Co2+,

Ag+, Hg2+, S cn tr ca Co2+ l do mu ca bn thn n ta c th loi tr bng cch
o mt quang bc sng thch hp. Cc ion Hg2+, Cd2+, Zn2+ to phc vi SCN- s
lm gim cng mu ca Fe3+ - SCN- . Do mun s dng phng php ny cn
phi tch cc ion nh hng n mu ca phc.
Phng php dng thuc th SCN- c gii hn pht hin km, chnh xc thp m
c s dng rng v phng php ny n gin, nhanh, p dng c trong cc dung
dch axit mnh v chi ph ca n tng i thp. Phng php ny xc nh c hm
lng st t 1 10 ppm. Ngi ta cng s dng phc ca Fe 3+ vi SCN- chit ln
dung mi hu c nhm tng chn lc v nhy cho php xc nh Fe2+. Trong
nghin cu ny cc tc gi nghin cu thnh cng php chit Fe2+ - SCN- bng cht
chit tetrabutyl amoni sunfat (TBAS) bng dung mi clorofom. SCN- l mt trong s t
cc thuc th v c c dng xc nh st.
Cng da trn cc c s cc nghin cu trc v s to phc mu ca Fe v SCN-,
gn y mt s tc gi xut mt s phng php xc nh st tng v Fe 3+ trong
nc ma nng c ppb. y l phng php xc nh st n gin, c nhy v
chn lc cao. Phng php ny da trn phn ng to mu gia Fe3+ v SCN- v s
c mt ca mt cation mang hot tnh hot ng b mt, chng hn nh cetyl pyridin
clorua (CPC), trong mi trng axit HCl c, sau chit phc ny vi N octyl
axetamin bng dung mi toluen hoc clorofom. H s hp th phn t ca phc l

= 2,6.105 l.mol-1.cm-1 ti bc sng cc i l max = 480 nm v h s lm giu l 10.

Gii hn pht hin l 5.106 mg/ml. Cc ion thng i cng vi st khng gy cn tr ti
php xc nh. Phng php ny c kim tra bng phng php quang ph hunh

13

quang hp th nguyn t (GF AAS) v s dng xc nh hm lng st nng

c ppb trong cc mu nc.
1.2.2.2

.Thuc th o Phenantrolin

Thuc th o Phenantrolin l mt thuc th kh nhy, dng xc nh ion Fe 2+ da

trn s to phc gia thuc th v Fe2+ .
N
N

Fe2+

Fe2+/3

Phc ny hon ton bn, cng mu khng thay i trong khong pH t 2 9 v

phc c max = 510 nm. Mt s nguyn t nh hng n qu trnh ny nh: bc, st do
to nn kt ta; Cd, Hg v Zn to phc kh tan vi thuc th ng thi lm gim cng
mu ca phc st ; Be , Sn, Cu, Mo cng gy nh hng v cc nguyn t ny c th
hn ch nh hng bng cch iu chnh pH trong khong hp nh : Hg c th c mt
10 ppm (pH t 3 9), Be c th c khong 50 ppm (pH t 3 5,5), Co c khong 10
ppm (pH t 2 - 5), Sn2+ khng qu 20 ppm (pH t 2 3), Sn4+ nh hn 50 ppm (pH =
2,5) u khng cn tr s to mu ca phc gia st v thuc th.
Fe3+ cng to phc vi o Phenantrolin, phc ny c mu xanh lc nht

max =

585 nm. Tuy vy, phc ny khng bn theo thi gian v chuyn dn sang mu vng nht
c cc i hp th max = 360 nm .
1.2.2.3

.Thuc th bato phenantrolin

Phc ca Fe2+ vi bato phenantrolin c th c chit bng nhiu dung mi hu

c, trong tt nht l ancol n amylic v iso amylic v clorofom.

14

Ngi ta thng dng clorofom chit v n c t trng cao nn d chit. Phc ny

c th c chit bng hn hp clorofom ancol etylic khan vi t l 1:5 hoc 5:1, pH
thch hp cho s to phc l 4 7 . trnh hin tng thy phn i vi cc ion ta
cho thm vo dung dch mt t mui xitrat hay tactrat. Cu2+ gy nh hng cho vic xc
nh Fe2+ bng thuc th bato phenantrolin, ngoi ra mt s ion kim loi ha tr II
nh Co, Ni, Zn, Cd vi mt lng ln cng gy nh hng. Cc anion khng gy nh
hng cho vic xc nh st bng thuc th ny.
1.2.2.4

.Thuc th 1-(2-pyridylazo)-2-naphthol (PAN)

Thuc th to phc vi st c nghin cu trong mi trng kim pH ti u 6

8, phc bn theo thi gian v phc c thnh phn Fe : R l 1 : 2 max = 565 nm ,

= 2,7.104.
N=N
N
O
H2O

H2O

Fe
O
N
N=N

1.2.2.5

.Thuc th 4- (2- pyridylazo) rezocxin ( PAR )

Thuc th PAR c cng thc cu to nh sau:

OH

N=N
N
HO

PAR l cht bt mu thm, tan tt trong nc, ancol v axton. Khi tan trong
nc dung dch c mu vng. Trong thng mi, thuc th PAR thng c s dng
di dng mui c cng thc phn t C11H8N3O2Na.H2O.

15

Cc cn bng ca thuc th PAR trong dung mi nc:

K0=10-3,1
N

+
N

OH

OH

N
HO

HO

H3R+(pH<2,1)

H2R (pH=2,1-4,2)

K2=10-11,9

K1=10-5,6
N

O-

N
HO
HR- (pH= 4,2- 9)

O
R2- (pH= 10,5- 13,5)

PAR to phc vi Fe3+ ty thuc vo pH ca dung dch.

+ pH = 8 9,3 th max = 500 nm, = 6,04.104.
+ pH = 4 xc nh c thnh phn phc Fe : PAR l 1 : 2 , max bin ng cc gi
tr khc nhau nh

max = 517 nm , = 4,2.104.

max = 496 nm , = 6,05.104.
max = 720 nm .

1.2.2.6

.Thuc th trioxyazobenzen (TOAB)

Phc mu Fe3+ - TOAB to thnh tt nht pH = 8 12 , phc bn vi thi gian , c

nhy cao, c max = 452 nm v 610 nm, = 4,3.104 . Phc c thnh phn Me:R=1:2.
Trong mi trng kim phc mu mang in tch m, sau khi thm tetrabutyl amoni
clorua trung ha in tch th phc c th c chit bng mt s dung mi cha oxi,
c bit l ancol iso amylic. Theo phng php ny hm lng st c xc nh l
1,1 6 g/l vi sai s 2 8 %.

16

O-

O
N

Fe

N
N

O
H

O-

1.3.Nghin cu v thuc th axit sunfosalixilic

1.3.1.Tnh cht ca thuc th axit sunfosalixilic.
CTPT: C7H6O6S

; KLPT: 254,2

iu kin thng SSal dng tinh th ngm hai phn t nc : C7H6O6S.2H2O

CTCT:
O

OH

COOH

SO 3H
2-hydroxy-5-sulfobenzoic acid

OH

COO

COOH

SO 3H
2-hydroxy-5-sulfobenzoate

SO 3

2-hydroxy-5-sulfobenzoic acid

Axit sunfosalixilic (axit 2-hydroxy-5-sunfobenzoic hay axit salixylsunfonic vit tt l

SSal) l mt loi thuc th hu c tinh th mu trng hay hng, l mt axit bn vi cht
oxi ha, c tan ln trong nc, d ht m hay kt tinh thnh khi. Nhum hng khi
c vt Fe.
Loi khng nc nng chy 120oC, c b phn hy mt phn. Khi hp th m trong
khng kh th nhit nng chy gim xung 110oC v thp hn. Rt d tan trong nc,
ancol etylic v ete.

17

Phn ng: dung dch SSal trong nc tc dng FeCl3 cho mu tm , thm
CH3COONa dung dch chuyn sang mu nu, thm dung dch NH3 (m c) dung dch
s chuyn sang mu vng.
Loi axit sunfosalixilic thng phm thng c nhiu tp cht, c th tinh ch nh
sau: pha ch dung dch bo ha axit SSal trong ru etylic nhit thng. yn
nhiu ngy, lc b kt ta, lp li nhiu ln.
1.3.2.Kh nng to phc ca axit sunfosalixilic
Xc nh so mu Fe. Xc nh gin tip Na. Axit sunfosalixilic tc dng vi cc ion
kim loi Al , Fe , Ti , to phc cht tan nn c th dng tch cc nguyn t (v d
tch Ti khi Fe). nh phn Be. Lm ch th kim loi xc nh nhiu ion theo
phng php complexon. kt ta v xc nh anbumin theo phng php o c.
1.4.Cc phng php xc nh st
1.4.1.Phng php khi lng
Lm kt ta st di dng hidroxit [Fe(OH)3] , sau tch ra khi mt s kim loi
kim, kim th, Zn, Pb,. Cc hidroxit ca cc kim loi ny kt ta pH cao hn
hidroxit st hoc n b gi li khi c mt ca NH3 trong dung dch. Cc ion tactrat,
xitrat, oxalat, pyrophotphat c th nh hng n qu trnh kt ta st hon ton. Khi c
mt cc ion , ta cho kt ta vi S2- trong c lng nh cadimi. Nhng phng
php ny khng c nh gi cao v sunfua cc kim loi t tan trong (NH4)2S d. Khi
kt ta st bng (NH4)2S c mt tactrat ta c th tch st ra khi titan, uran, vanadi,
photphat v mt s nguyn t khc.
1.4.2.Phng php trc quang
Phng php trc quang c dng ph bin xc nh st. Sau y l mt s
thuc th m cc nh phn tch nghin cu.
Xc nh st bng phng php trc quang v chit trc quang
Thuc th d

nhy

max

pH xc

Thi gian bin

nh hng

(nm)

nh

mu

thuc th d

18

,-dipyridyl
2,2,2-terpyridyl
Disodium-1,2-

0,007
0,005
0.009

522
39
552 3 10
430 8,5 9,5

1 nm
1 nm
Vi thng

Khng
khng
Vi thng

dihirobenzen
3,5-disunfonyl ferron
4-hidroxylbiPhenyl-3-

0,015
0.003

610
575

2,7-3,7
3

1-2 tun
1 ngy

Khng
C

cacboxylic axit
Mercapto axetic axit
Mui nitro-R
o-Phenantrolin
Axit salixilic
Axit sunfosalixilic
Thioxianat
Thioxiant/nc

0,014
0,0023
0,007
0,03
0,01
0,008
0,004

540
720
508
520
430
480
482

7-12
3,9-5,1
2-9
2,5-2,7
7
Axit
axit

Vi gi
6 gi
1 ngy
2-3 ngy
Hn 1 ngy
Gim
Bin i theo t

Khng
Khng
Khng
C
Khng
C
C

-axeton
1.4.3.Phng php chun pemanganat
Phn ng oxi ha bng ion pemanganat MnO4- l c s ca phng php
pemanganat. Phng php ny c th thc hin trong mi trng axit, kim v trung
tnh. Khi thc hin trong mi trng axit, mangan (VII) b kh ti mangan (II) v mu
tm ca dung dch b mt.
Thc hin chun mui st (II) bng kalipemanganat: Axit ha dung dch bng dung
dch axit sunfuric v chun ti im cui. St (II) b oxi ha thnh St (III):
5Fe2+ + MnO4- + 8H+ 5Fe3+ + Mn2+ + 4H2O
Bit nng ng lng v th tch cn chun ca KMnO4 d dng tnh c
lng st trong dung dch.
1.4.4.Cc phng php khc xc nh st
Mt s phng php khc xc nh st nh: phng php sc k ion , phng php
hp th nguyn t ngn la, phng php Vn Ampe,Tuy nhin cc phng php
ny c chi ph cao, dn n gi thnh cao v t c s dng.

19

1.5. Cc phng php nghin cu nh hng ca pH ti s to phc ca

Fe(III) vi axit sunfosalixilic bng phng php trc quang
Xc nh thnh phn phc:
1.5.1.Phng php h ng phn t gam ( phng php bin i lin tc, phng
php Oxtromxlenko-Job )
Chun b hai dy dung dch c nng hng nh.
Dy dung dch 1: CFe3+ + CSSal

=aM

Dy dung dch 2: CFe3+ + CSSal

=bM

Tin hnh o mt quang ca dung dch cc iu kin ti u v so snh vi mu

trng ti bc sng max . Suy ra thnh phn phc: Fe(SSal)m(3-2m)+
1.5.2.Phng php t s mol (phng php ng cong bo ha)
Pha 2 dy dung dch c

CFe3+ = const
CSSal thay i

CFe3+ thay i

CSSal = const
Tin hnh o mt quang bc sng max , ta cng thu c dy cc A
Suy ra thnh phn phc: [Fe(SSal)m](3-2m)+
1.6.Cc phng php xc nh h s hp th phn t ca phc
1.6.1.Phng php h ng phn t gam
Phng php ny c s dng rt ph bin xc nh thnh phn ca phc mu.
Pha mt dy dung dch: CFe3+ = CSSal v c CFe3+ + CSSal = const ( cng cc iu
kin ti u) .
o mt quang ca cc dung dch , ta c th:
A

CSSal

20

1.6.2.Phng php x l thng k ng chun

Khi nghin cu s ph thuc mt quang v nng ca phc s thit lp c
phng trnh ng chun c dng:
Trong :

a=
b=

Ai = ( a a ) Ci + ( b b )

n Ci .Ai Ci . Ai
n. Ci2 ( Ci ) 2

= phc

C . A C . C .A
n. C ( C )
2
i

2
i

1.6.3.Phng php Komar

Phng trnh:

M + qHR MRq + qH+

, Kcb

iu kin p dng phng php Komar:

- bit c thnh phn phc
- nghin cu c ch ca phn ng to phc t vit c phng trnh ca phn
ng to phc.
- Nhit , pH, lc ion, b dy cuvet v bc sng khng i.
- Nng ban u ca cc cu t tc dng c th thay i nhng lun m bo t l:
CHR = q.CM

1.7.nh gi cc kt qu phn tch

thu c kt qu ca php phn tch vi tin cy v chnh xc cao, ngoi vic
la chn phng php, cc iu kin ti u v cc thao tc th nghim th vic x l v
nh gi cc kt qu cng c mt ngha ht sc quan trng. nh gi chnh

21

xc ca kt qu phn tch, y ti p dng phng php ton hc thng k vi mt

s ni dung chnh ch yu nh sau:

Xc nh lp li ca cc kt qu phn tch:
Khi tin hnh phn tch n ln vi cc gi tr X1 , X2 , X3 , X4 , Xi ta s c:

Hm lng trung bnh: X =

Phng sai: S

lch chun trung bnh: S X =

Xi
n

(X
=

X
n 1
i

S2
n

Xc nh tin cy ca cc kt qu phn tch:

tin cy: = t p ; k .S X

trong tp;k l hm phn b student ng vi bc t do k (k = n-1) v xc sut p

-

Khong tin cy: X a X +

Nu cng nh th cng gn ti gi tr thc

Hm phn b thc nghim: ttn =

X a
SX

So snh ttn vi tp;k nu ttn < tp;k th X a l do nguyn nhn ngu nhin hay kt qu
phn tch l tin cy v chp nhn c.
-

Sai s tng i:

q% =

t .S

.100 = p; k X .100
X
X

22

CHNG 2: K THUT THC NGHIM

2.1 Dng c v thit b
2.1.1 Dng c:
- Pipet, buret, kim tim 1 ml, bnh nh mc cc loi (10 ml, 25 ml, 100ml, 250ml).
- Cc thy tinh cc loi.
- ng nghim nh 1 cm .
- Cc ng nh c th tch khong 10 hoc 25 ml c np y.
2.1.2 Thit b:
Cn phn tch, my o quang, x l s liu (trn my vi tnh).
2.2 Ha cht v cch pha
2.2.1.Ha cht:
- Mui FeCl3.6H2O.
- Axit sunfosalixilic (SSal.2H2O).
- Axit HCl m c.
- Axit CH3COOH m c.
- CH3COONa tinh th ( hoc dung dch NaOH 10 %).
- Mui NH4Cl tinh th .
- NH3 m c.
- Mui NaNO3.
2.2.2.Cch pha ha cht:
+ Dung dch gc Fe3+ 10-3M: cn mt lng chnh xc FeCl3.6H2O ri thm nc ct
n vch ca bnh nh mc 250 ml, ta s thu c dung dch Fe 3+ c nng 10-3 M .
Xc nh li dung dch bng phng php chun Complexon vi ch th SSal
= 2,5 3,0.

pH

23

+ Dung dch thuc th axit SSal 10-3 M: cn mt lng chnh xc axit SSal
(C7H6O6S.2H2O), ri thm nc ct n vch ca bnh nh mc 250 ml, ta s thu c
dung dch SSal c nng 10-3 M .
+ Dung dch m axetat: pH = 4,2 4,5
Ho 60 ml axt axetic m c vo 300 400 ml nc, thm 100 ml NaOH 10 %,
thm nc thnh 1 lt, khuy u.
Hoc pha t:Axit CH3COOH m c v CH3COONa tinh th.
+ Dung dch HCl ( nng 0,01M ) to mi trng c pH khong 1,8 2,5
+ Dung dch m amoni: pH = 9,5 10,5
Ho tan 54 g amoni clorua vo 500 ml nc, thm 350 ml NH3 m c, thm nc
thnh 1 lt, khuy u.
+ Dung dch NaNO3 1M: cn mt lng chnh xc NaNO3 ri cho nc n vch
nh mc, dng c nh lc ion.
2.3 Cch tin hnh
Ht mt th tch xc nh thuc th SSal, thm mt th tch xc nh NaNO3 gi
lc ion, thm m, sau ht mt th tch chnh xc Fe3+ , thm nc ct n vch nh
mc.
20 pht ri o mt quang ca phc to thnh.
2.4 Phng php nghin cu
Dng phng php trc quang xc nh cc iu kin ti u cho s to phc
(

, pHt ,) s dng iu kin ti u xc nh thnh phn ca phc Fe (III)

SSal cc pH khc nhau, t xt nh hng ca pH n s to phc.

24

CHNG 3: KT QU V THO LUN

3.1 Kho st cc ph hp th
Xc nh ph ca dung dch v phc to thnh:
Chun b:
-

Dung dch Fe(III) c nng : CFe = 2,0.10-5 M; C NaNO = 0,1 M pH = 2,0 c

3+

iu chnh bng HCl.

-

Dung dch phc Fe(III) SSal c nng : C Fe

3+

= 2,0.10-5M; CSSal = 10.10-5M;

C NaNO3 = 0,1 M pH= 2 c iu chnh bng HCl v pH = 4,5 c iu chnh

bng m axetat .
o mt quang ca dung dch v phc cht to thnh.T ta xc nh c cc
bc sng (max ) ca phc.
Ta xc nh c max ca phc pH =2,0 v pH = 4,5. Thu c kt qu nh sau:
Bc sng (nm)

A (pH = 2,0)

A (pH = 4,5)

400

0,194

0,224

410

0,211

0,241

420

0,224

0,263

430

0,260

0,296

440

0,284

0,336

450

0,311

0,362

460

0,345

0,382

470

0,368

0,400

480

0,390

0,404

490

0,400

0,414

500

0,404

0,392

510

0,394

0,369

520

0,390

0,347

25

530

0,373

0,316

540

0,348

0,288

550

0,327

0,256

560
570
580
590
600

0,296
0,274
0,240
0,218
0,194

0,236
0,199
0,173
0,166
0,154

th:
Biu xc nh bc sng ti u
0.44

490 nm

500 nm

Mt quang(A)

0.39
0.34
pH = 2
pH = 4.5

0.29
0.24
0.19
0.14
370

400

430

460

490

520

550

580

610

Bc sng

T th trn nhn thy c hai khong max hai khong pH. pH = 2,0 ta o c
max = 500 nm ; cn khong pH = 4,5 ta o c max = 490 nm. Nh vy, ti s chn
hai khong pH hai buc sng ny xc nh thnh phn phc.
3.2 Kho st pH ti u v nh hng ca pH n s to phc

Tin hnh kho st nh hng ca pH n kh nng to phc ca Fe (III)

SSal xc nh phc bn khong pH no v pH ti u ca phc.

o mt quang ca phc cc gi tr pH khc nhau ti bc sng max.

26

Kt qu:

th:

pH

1,0

0,404

1,5

0,528

2,0

0,542

2,5

0,540

3,5

0,450

4,0

0,390

4,5

0,381

5,0

0,380

5,5

0,375

6,0

0,380

7,0

0,379

8,0

0,230

9,0

0,040

9,5

0,030

10

0,034

10,5

0,030

11

0,035

12

0,033

13

0,008

14

0,004

27

Biu xc nh pH ti u
0.6

Mt quang (A)

0.5

0.4

0.3

0.2

0.1

0
0

10

11

12

13

14

15

pH

Da vo th ta nhn thy c 3 khong pH m ti mt quang ca phc bn,

l pH = 1,8 2,5; pH = 4,0 7,0; pH = 9,0 12 ; tc l c 3 phc ring bit.
Tuy nhin phc th 3 (c pH = 9,0 12) do mt quang qu nh nn khng c gi
tr ng dng trong thc t. V vy ti quyt nh ch nghin cu 2 khong pH (pH = 2,0
chnh bng HCl v pH = 4,5 chnh bng m axetat).
3.3 Kho st nh hng ca thi gian n s to phc

Tin hnh kho st nh hng ca thi gian n kh nng to phc xt

xem khong thi gian no th phc c mt quang n nh.

Dung dch phc: C Fe = 2,0.10-5M ; CSSal = 10.10-5 M; C NaNO = 0,1 M

3+

o mt quang ca dung dch phc Fe (III) - SSal c nng xc nh

cc

khong thi gian khc nhau ti bc sng v pH ti u.

28

Kt qu:
Thi gian
(pht)
1
5
10
20
40
60
80
100
120
140
160
180

A
(pH=2)
0,155
0,158
0,160
0,170
0,170
0,171
0,170
0,172
0,169
0,170
0,170
0,171

A
(pH=4,5)
0,162
0,167
0,173
0,178
0,178
0,177
0,178
0,178
0,177
0,178
0,178
0,178

th:

B i u xc nh thi gi an ti u
Mt quang (A )

0.18
0.175
0.17

pH=4,5

0.165

pH=2

0.16
0.155
0.15
0

20

40

60

80

100

120

140

160

180

200

Thi gian
Nhn xt: phc c mt quang n nh v t cc i v n nh 20 pht, do ti
quyt nh ly khong thi gian ny tin hnh cc th nghim tip theo.

29

3.4. Xc nh thnh phn phc (xt ln lt tng phc max ti cc pH ti u)

3.4.1.Xc nh thnh phn phc khong pH th nht (max = 500 nm )
3.4.1.1.Phng php ng phn t gam
Pha dy dung dch Fe(III) SSal c nng CM nh nhau v trn chng vi nhng t
l khc nhau, nhng CFe3+ + CSSal = const , pH = 2,0 ( HCl ), thm NaNO3, thm nc n
vch bnh nh mc 25 ml .
Sau 20 pht , o mt quang t = 500 nm , pHt = 2,0 , ng nghim nh 1 cm.
Dy dung dch : CFe3+ + CSSal = 10.10-5 M . Ly V ml SSal 10-3 M , thm NaNO3,
thm HCl, sau thm (2,5 V) ml Fe3+ 10-3 M , ri thm nc n vch bnh nh mc
25 ml.
Kt qu :
STT

V (ml)
3+

SSal

0,00
0,50
0,75
1,00
1,25
1,50
1,75
2,00
2,25
2,50

2,50
2,00
1,75
1,50
1,25
1,00
0,75
0,50
0,25
0,00

Fe
1
2
3
4
5
6
7
8
9
10

th:

C . 10-5 (M)
Fe 3+
SSal
0
2
3
4
5
6
7
8
9
10

10
8
7
6
5
4
3
2
1
0

A
0,060
0,420
0,639
0,860
0,990
0,870
0,650
0,438
0,220
0,100

Mt quang (A)

30

1
0.9
0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0
0

10

11

-5

C (Fe) . 10

Biu xc nh thnh phn phc khong pH th nht theo

phng php ng phn t gam

Nhn xt:
Ta thy, mt quang t cc i V(Fe3+ ) = V( SSal ) , tc l thnh phn phc c t l

[ Fe ] = 5.10
3+

[ SSal ]

5.10

5
5

1
. Nh vy khong pH = 2,0 ta xc nh c thnh phn phc
1

c t l 1: 1 .

Xc nh h s hp th phn t gam theo phng php ng phn t gam:

CFe3+ ( M ) CSSal (M )
Cphc M
A
=A/l.Cphc
-5
-5
0.10
10.10
0,060
///
Cphc = CFe3+
-5
-5
2.10
8.10
0,420
1 = 2,10.104
-5
-5
3.10
7.10
0,639
2 = 2,13.104
4.10-5
6.10-5
0,860
3 = 2,15.104
5.10-5
5.10-5
0,990
4 = 1,98.104
6.10-5
4.10-5
0,870
5 = 2,18.104
7.10-5
3.10-5
0,650
6 = 2,17.104
8.10-5
2.10-5
0,438
7 = 2,19.104
C
=
C
phc
SSal
9.10-5
1.10-5
0,220
8 = 2,20.104
-5
-5
10.10
0.10
0,100
///
S dng chng trnh Descriptive Statistics trong Microsoft Excel , thu c gi tr

h s hp th phn t gam l:

31

2,14.104 0,05991 ( l.cm-1.mol-1)

Gi tr tng i ln, do phc ny kh bn .
3.4.1.2. Phng php t s mol
o mt quang ca 2 dy dung dch: C Fe3+ = 10-3 M v CSSal = 10-3 M, nh mc n
bnh 25 ml.
- Dy 1: CFe3+ = const , CSSal thay i
- Dy 2: CFe3+ = thay i , CSSal = const
Kt qu:
Dy 1: CFe3+ = const , CSSal thay i

Mt quang (A)

V Fe 3+ (ml)
1,0
V SSal (ml) 0,2 0,4
0,6
0,8
1,0
1,5
1,7
1,9
2,0
2,5
A
0,182 0,363 0,495 0,670 0,856 0,855 0,856 0,857 0,856 0,856
th:
1
0.9
0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0
0

0.5

1.5

2.5

V (SSal)

Biu xc nh thnh phn phc khong pH th nht theo phng

php t s mol vi nng SSal thay i

Nhn xt: da vo th ta nhn thy, tng t nh trn ta cng c thnh phn phc
VFe 3+
VSSal

= 1:1.

Dy 2:

VSSal ml

CFe3+ = thay i , CSSal = const

2,0

32

VFe3+ ml

0,5

1,0

1,5

2,0

2,5

3,0

3,5

4,0

4,5 5,0

0,12

0,47

0,98

1,70

1,70

1,72

1,71

1,7

1,70 1,71

th:

Mt quang (A)

2
1.8
1.6
1.4
1.2
1
0.8
0.6
0.4
0.2
0
0

V (Fe)

Biu xc nh thnh phn phc theo phng php t s mol

vi nng Fe thay i

Nhn xt: da vo th ta nhn thy, tng t nh trn ta cng c thnh phn phc
VFe 3+
VSSal

= 1 : 1 hay thnh phn phc xc nh c cng c t l Fe (III): SSal =1: 1

3.4.2.Xc nh thnh phn phc khong pH th hai ( max = 490 )

3.4.2.1.Phng php ng phn t gam
Pha dy dung dch Fe(III) SSal c nng CM nh nhau v trn chng vi nhng
t l khc nhau, nhng CFe3+ + CSSal = const , pH = 4,5 (m axetat), thm NaNO3 ,
thm nc n vch nh mc.

33

Sau 20 pht , o mt quang t , pHt , ng nghim nh 1 cm.

Dy dung dch : CFe3+ + CSSal = 20.10-5 M. Ly V ml SSal 10-3 M , thm NaNO3,
thm HCl, sau thm (5,0 V) ml Fe3+ 10-3 M , ri thm nuc n vch bnh nh mc
25 ml.
Kt qu :
STT

V (ml)
Fe

1
2
3
4
5
6
7
8
9
10
11

th:

0,0
0,5
1,0
1,5
2,0
2,5
3,0
3,5
4,0
4,5
5,0

3+

SSal
5,0
4,5
4,0
3,5
3,0
2,5
2,0
1,5
1,0
0,5
0,0

C . 10-5 (M)
Fe 3+
SSal
0,0
2,0
40
6,0
8,0
10
12
14
16
18
20

20
18
16
14
12
10
8,0
6,0
4,0
2,0
0,0

A
0,270
0,562
1,136
1,710
1,680
1,435
1,150
0,865
0,579
0,294
0,120

34

1.8

Mt quang (A)

1.6
1.4
1.2
1
0.8
0.6
0.4
0.2
0
0

10

12

-5

14

16

18

20

22

C (SSal) . 10

Biu xc nh thnh phn phn phc khong pH th hai theo

phng php ng phn t gam

Nhn xt:
V

12 14

SSal
= :
Ta nhn thy mt quang t cc i khong V
.
8 6
Fe
3+

SSal
= (do n nguyn dng v
Tc l khong 1,5 < n < 2,3 ; hay thnh phn phc V
1
Fe
3+

tha iu kin 1,5 < n < 2,3 th ch c duy nht n = 2 ).

V

SSal
= . T cho thy thnh phn phc c t l Fe3+: SSal = 1: 2
Nh vy: V
1
Fe
3+

Xc nh h s hp th phn t gam theo phng php ng phn t gam:

CFe3+ (M)
0,0.10-5
2,0.10-5
4,0.10-5
6,0.10-5
8,0.10-5
10.10-5
12.10-5
14.10-5
16.10-5

CSSal (M)
20.10-5
18.10-5
16.10-5
14.10-5
12.10-5
10.10-5
8,0.10-5
6,0.10-5
4,0.10-5

Cphc (M)
Cphc = CFe3+

Cphc =

1
CSSal
2

A
0,270
0,562
1,136
1,710
1,680
1,435
1,150
0,865
0,579

= A/l.Cphc
///
1 = 2,810.104
2 = 2,840.104
3 = 2,850.104
4 = 2,700.104
5 = 2,870.104
6 = 2,875.104
7 = 2,883.104
8 = 2,890.104

35

18.10-5
2,0.10-5
0,294
9 = 2,940.104
20
0,0
0,120
///
S dng chng trnh Descriptive Statistics trong Microsoft Excel , thu c gi tr
h s hp th phn t gam l:
2,852.104 0,05157 ( l.cm-1.mol-1 )
Gi tr tng i ln, do phc ny kh bn .
3.4.2.2. Phng php t s mol
o mt quang ca 2 dy dung dch: - Dy 1: CFe3+ = thay i , CSSal = const
- Dy 2: CFe3+ = const ,

CSSal thay i

Kt qu:
Dy 1:

CFe3+ = thay i , CSSal = const

VSSal(ml)
2,0
3+
VFe (ml) 0,1
0,5
0,8
1,0
1,5
1,7
2,0
2,1
2,3
2,5
A
0,200 0,590 0,910 1,140 1,143 1,144 1,147 1,150 1,150 1,151

th

36

1.4

Mt quang (A)

1.2
1
0.8
0.6
0.4
0.2
0
0

0.5

V (Fe)

1.5

2.5

Biu xc nh thnh phn phc khong pH th hai theo

phng php t s mol vi nng Fe thay i
V

SSal
= , thnh phn ca phc t t
Nhn xt: khi pH= 4,5 ta c thnh phn phc V
1
Fe
3+

l:

V Fe3+
VSSal

1
. Hay thnh phn phc Fe (III): SSal = 1: 2
2

Dy 2:

CFe3+ = const , CSSal thay i

VFe3+(ml)
1,0
VSSal(ml) 0,2
0,6
0,8
1,0
1,6
2,0
2,2
2,4
2,5
A
0,230 0,480 0,650 0,760 0,940 1,140 1,138 1,140 1,140

th:

37

Mt quang (A)

1.2
1
0.8
0.6
0.4
0.2
0
0

0.5

1.5

2.5

V (SSal)

Biu xc nh thnh phn phc khong pH th hai theo

phng php t s mol vi nng SSal thay i

Nhn xt: Nh vy thnh phn phc khong pH th hai (pH = 4,5) ta xc nh c

phc c

VFe 3+
VSSal

1
, nh vy thnh phn phc gia Fe(III) : SSal = 1 : 2 .
2

38

KT LUN
Nh vy, cc khong pH khc nhau m thnh phn phc gia Fe (III) vi SSal c t
l 1:1 hoc 1:2
pH
Mi trng
Phc
Thnh phn phc
Mu
max (nm)
1,8 - 2,5
axit
[FeSSal] +
1: 1
tm
500
4,0 7,0 m axetat [Fe(SSal)2]
1: 2
da cam
490
>12
Ba z
Phn hy
pH c nh hng ln n s to phc ca cc cht, in hnh l nh hng n s to
phc ca Fe(III) SSal. Tu theo khong pH no m thnh phn phc c mt t l xc
nh.
Theo l thuyt, khong pH = 9 11 , ta c thnh phn phc Fe(III) SSal = 1: 3 .
Tuy nhin, khi lm thc nghim t l ny khng c xc nh do mt quang qu
nh. V thc t cho bit vic xc nh thnh phn phc hai khong pH u c ngha
quan trng hn khong pH th ba.

39

TI LIU THAM KHO

1.

Hong Nhm. Ho hc v c, Tp 3. NXB Gio dc

2.

H Vit Qu - Nguyn Tinh Dung. Cc phng php phn tch ho l.HSP H Ni

1991
3.

L Th Yn Kiu. Kho lun Tt nghip. HSP ng Thp, nm 2008

4.

Nguyn Duy i , Nguyn Tinh Dung, Trn Thnh Hu, Trn Quc Sn, Nguyn Vn

Tng Mt s vn chn lc ca ha hc Nh xut bn gio dc , 2003.

5.

Trn T Hiu. Phn tch trc quang. H Tng hp H Ni, 1994

6 A. T. o
B. . oo
. . Cepea
. . eeo

A. T. Pilipenko
V. Ia. Pochinoc
I. P. Xeraa
Ph. . Sepchenko