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Thm dung dch 1.10- phenantrolin vo lng mu v o hp thu ca phc cht mu da cam bc sng bng 510 nm. Nu xc nh lng st tng hoc tng st ho tan, them
hydroxyl- amoni clorua d kh st (II) n st (III). Nu c st khng tan, oxyt st hoc phc
cht st, cn phi x l s b ho tan cc cht (xem 7.1.2).
Phc cht st (II)- 1.10- phenantrolin bn trong khong pH t 2.5 n 9 v mu sc t l vi hm
lng Fe(II). Quan h gia nng st v hp thu l tuyn tnh vi nng st nh hn 5.0
mg/l. hp thu cao nht khi o = 510 nm {h s hp thu phn t 11x103l (mol.cm)}
4. Thuc th
S dng thuc th loi phn tch.
Dng nc cha cng t st cng tt; nng st trong thuc th thp hn t nht 3 ln so vi
sai lch tiu chun trong kt qu th nghim trng. Nc th ion hoc nc ct trong dng
c thu tinh c th tch thch hp cho phn tch ny.
4.1 Axit sunfuric = 1.84 g/ml.
4.2 Dung dch Axit sunfuric c(1/2H2SO4)= 4.5 mol/l
Va thm t t va khuy mnh mt th tch Axit sunfuric m c(4.1) vo 3 th tch nc
mt.
4.3 Axit nitric m c = 1.40 g/ml.
4.4 Dung dch Axit clohidric HCl =1.12 g/ml c(HCl)= 7.7 mol/l.
4.5 Dung dch m axetat
Ho tan 40g amoni axetat CH3COONH4 v 50 ml Axit axetic bng (CH3COOH) =1.06 g/ml
trong nc v pha long bng nc ti 100ml.
4.6 Hydro xyl- amoni clorua, dung dch 100 g/l
Ho tan 40g hydroxyl- amoni clorua (NH2OH.HCl) trong nc. Thm nc n 100ml.
Dung dch ny n nh t nht trong mt tun.
4.7 Dung dch 1.10- phenantrolin
Ho tan 0.5g 1.10- phenantrolin clorua, ngm 1 phn t nc (C12H9CIN2.H2O) trong nc v
pha long ti ml.
C th thay th bng cch ho tan 0.42g 1.10- phenantrolin ngm 1 nc (C12H9N2.H2O) trong
100 ml nc cha hai git axit clohydric HCl (4.4).
vch.
Ch thch: - Phng php thay th: hn hp c th hp trong bnh kn 100 ml, trong 30 pht, sau
lm ngui hoc pha long ti 100 ml. S pha long ny phi c tnh khi tnh ton kt qu
bng cch nhn vi c s 2.
Nu dung dch c sau khi oxy ho trc khi pha long, cn lc ngay qua mng lc (5.3) vo
bnh nh mc. Trng giy lc vi mt t nc, cho dch ra vo dch lc v thm nc n
vch.
7.1.1.2 Kh thnh st (II)
Chuyn dung dch sang bnh 100 ml, thm 1 ml hidroxylamoni clorua (4.6) v trn k. Thm 2 ml
dung dch m axetat (4.5) v chnh pH 3.5 5.5, tt nht l 4.5.
Ch thch: - S kh st (III) thnh st (II) c hiu qu nht vi pH =1, do thm dung dch m sau cng.
8.2 Bo co kt qu
Bo co kt qu, ghi r dng st xc nh
a. Lm trn ti 0.010 mg/l vi nng st t 0.010 n 0.100 mg/l;
b. Lm trn ti 0.01 mg/l vi nng st ln hn 0.100 n 10 mg/l;
c. Lm trn ti 0.1 mg/l vi nng st ln hn 10 mg/l.
9. chnh xc (Xem bng 1)
Bng 1 - Thng k s liu lp li ca phng php
Nng
st
Phng th
nghim
Chiu di
quang
hc1)mm
Gi tr trung bnh
ca 30 kt ta
mg/l
Mg/l
0.100
100
0.010
0/002
0.010
50
0.010
0.001
10
0.010
0.001
0.010
0.000
0.040
0.041
0.002
0.050
100
0.046
0.005
0.048
0.004
0.045
0.0046
10
0.048
0.011
50
0.104
0.015
0.102
0.004
0.100
0.500
1.000
2.000
0.096
0.006
10
0.101
0.014
0.099
0.006
50
0.48
0.025
0.500
0.012
0.494
0.005
10
0.498
0.016
10
0.97
0.05
1.003
0.008
1.009
0.006
10
1.004
0.019
1.018
0.004
1
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