TIU CHUN VIT NAM TCVN 6177 : 1996

ISO 6332: 1988 (E)

CHT LNG NC- XC NH ST BNG PHNG PHP TRC PH DNG

THUC TH 1.10 -PHENANTROLIN
Water quality - Determination of iron Spectrometric method using 1.10phenantrolin
Li ni u
TCVN 6177: 1996 hon ton tng ng vi ISO 6332: 1988 (E)
TCVN 6177: 1996 do Tiu ban k thut nc tinh lc TCVN/TC/F9/SC1 thuc Ban k thut tiu
chun TCVN/TC/F9 ung bin son, Tng cc Tiu chun - o lng - Cht lng ngh.
B Khoa hc, Cng ngh v Mi trng ban hnh.
1. Phm vi v lnh vc p dng
Tiu chun ny quy nh phng php trtc ph xc nh st trong nc v nc thi bng
thuc th 1.10- phenantrolin. Quy trnh c miu t xc nh:
a. St tng (tng st ho tan v khng tan)
1. Xc nh trc tip
2. Xc nh sau khi phn hu
b. Tng st ho tan {tng st (II) v (III) ho tan}
c. Xc nh st (II) ho tan
Phng php ny c th p dng xc nh nng st trong khong 0.01 n 5 mg/l. C th
xc nh nng st cao hn 5 mg/l bng cch pha long mu thch hp.
i vi vic gy nhim xem iu 10.
2. Tiu chun trch dn
ISO 5667-1:1980 Cht lng nc - Ly mu. Phn1: Hng dn cc phng n ly mu.
3. Nguyn tc

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).

Dung dch ny n nh trong mt tun nu c bo qun trong ti.

4.8 Kali peroxodisunfat (K2S2O8) dung dch 40g/l
Ho tan 40g kali peroxodisunfat trong nc v pha long ti 100 ml.Dung dch ny n nh trong
vi tun vi iu kin ct gi trong l thu tinh sm mu nhit phng.
4.9 St, dung dch gc cha 0.10g st trong 1 lt
Cn 50.0 mg y st ( tinh khit 99.99%) v cho vo bnh nh mc 500 ml. Thm 20 ml
nc, 5 ml dung dch HCl (4.4) v h m t t cho ho tan. Lm ngui v thm nc ti vch.
1 ml dung dch gc ny cha 0.10 mg st.
Dung dch ny n nh t nht trong mt thng trong bnh thu tinh bn hoc bnh nha.
C th s dng dung dch gc bn sn.
4.10 St, dung dch chun 1, cha 20 mg st trong 1lt
Dng pipet ly 100 ml dung dch st gc (4.9) cho vo bnh nh mc 500 ml v thm nc n
vch.
Dung dch ny ch dng trong ngy.
4.11 Dung dch chun 2, cha 1 mg st trong 1 lt
Dng pipet ly 5 ml dung dch st chun (4.10) cho vo bnh nh mc 500 ml v thm nc n
vch.
Dung dch ny ch dng trong ngy.
5 Thit b
Tt c cc dng c thu tinh,k c bnh ng mu, cn phi ra bng dung dch HCl (4.4) v
trng bng nc trc khi dng.
Cc dng c trong phng th nghim bnh thng
5.1 Ph k, lng knh hoc loi v grating, ph hp vi o quang bc sng = 510 nm.
5.2 Cuvet vi chiu di quang hc nh nht l 10 mm v ph hp vi hp thu d kin ca
dung dch th.
Ch thch: - C th s dng cc cuvet c chiu di quang hc ln hn khi nng st nh hn
1.0 mg/l.

5.3 Mng lc kch thc l trung bnh 0.45 m.

5.4 Bnh oxy, dung dch 100 ml.
6. Ly mu v chun b mu
Cnh bo - Cn thn trng v p dng bin php an ton v khi axit ho mu c th to ra
cc kh c hi.
6.1 ly mu
Ly mu theo ISO 5667-1 v mi hng dn c th cho loi nc kim tra. Dng c ng c th
s dng nh nha polyetylen.
6.2 St tng
A xit ho mu ngay n pH bng 1 sau khi ly mu. Ni chung. Dng 1 ml axit sunfuric m c
(4.10 l cho 100 ml mu. Nu cn chnh pH bng cch thm dung dch axit sunfuric long
(4.20 v nh tnh pha long trong khi tnh kt qu cui cng.
6.3 Tng st ho tan
Lc mu (6.1) ngay sau khi ly mu.
Axit ho dung dch lc cho n khi pH bng1 (khong 1 ml axit sufuric m c (4.1) cho 100 ml
mu).
6.4 St (II)
Cho 1 ml H2SO4 c (4.1) vo bnh oxy (5.4). y mu nc vo bnh. Trnh mu tip xc
vi khng kh.
7. Cch tin hnh
7.1 St tng
7.1.1 Xc nh trc tip
Ly 50.0 ml (ch : chnh xc) mu axit ho (6.2)
Nu c mt st khng tan, oxit st, phc cht st th chuyn mu (7.1) sang bnh un th tch
100 ml v tin hnh s l s b nh sau:
7.1.1.1 Oxy ho
Thm 5 ml dung dch kali peroxodisunfit (4.8) v un si nh trong 40 pht, m bo th tch
khng cn qu 20 ml. Lm ngui v chuyn vo bnh nh mc dung tch 50 ml v thm nc ti

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.

7.1.1.3 S to thnh cht hp thu

Thm 2 ml dung dch 1.10- phenantrolin (4.7) vo dung dch 7.1.1.2 v ch ti trong khong
15 pht.
7.1.1.4 o quang
hp thu ca dung dch 7.1.1.3 s dng ph k (5.1) vi 510 nm dng nc trong cuvet so
snh.
7.1.2 St tng sau khi phn hu
Cho 50.0 ml mu a xit ho (6.2) vo cc c m 100 ml thm 5 mlHNO3 (4.3) v 10 ml HCl
(4.4), lm nng ti 70- 800C cho ti khi ho tan hon ton. Sau 30 pht, thm 2 ml H2SO4 (4.1)
v lm bay hi dung dch ti khi xut hin khi SO3 mu trng. Trnh un cn. Lm ngui ti
nhit phng v thm 20 ml nc, chuyn sang bnh nh mc 50 ml v nc n vch.
Lm tip nh m t trong 7.1.1.2 n 7.1.1.4.
7.2 Xc nh st ho tan
Ly 50.0 ml mu th (6.3) v chuyn sang bnh nh mc 100 ml.
Tin hnh nh m t trong 7.1.1.2 n 7.1.1.4.
7.3 Xc nh st (II)
Ly 50.0 ml mu (6.4) v chuyn sang bnh nh mc 100 ml.

Tin hnh nh m t trong 7.1.1.2 nhng khng thm hidroxylamoni clorua.

Tin hnh nh m t trong 7.1.1.3 v 7.1.1.4.
Trnh mu tip xc vi khng kh.
7.4 Th mu trng
Chun b dung dch th trng, thc hin chnh xc theo quy trnh nh i vi mu, nhng thay
50 ml mu bng 50 ml nc.
7.5 Hiu chun
7.5.1 Chun b dung dch chun
Chun b dy dung dch st chun trong khong nng nh d tnh ca mu th bng cch
cho mt th tch chnh xc bit dung dch Fe chun (4.10) v (4.11) vo mt lot bnh nh
mc 50 ml. Thm 0.5 ml dung dch H2SO4 long (4.2) vo mi bnh v thm nc ti vch.
X l lot dung dch st chun nh lm vi mu, tng ng vi quy trnh cho mi dng Fe
cn xc nh (xem 7.1 n 7.3).
7.5.2 Dng ng chun
Vi mi dy dung dch st chun, chun b th chun bng cch t nng dung dch st
(mg/l) trn trc honh tng ng vi hp thu trn trc tung. Yu cu mt ng chun ring
cho mi dng Fe, mi mt my quang ph v mi chiu di quang hc ca cuvet.
7.5.3 Thng xuyn lp ng chun
nh k kim tra ng chun v c bit i vi mi m thuc th mi.
8. Biu th kt qu
8.1 Tnh ton
Nng st ca mu, biu th bng miligam trn lt c tnh theo cng thc:
F (A1- A0)
Trong :
F l dc ca ng cong chun tng ng (7.5.2);
A1 l hp thu ca dung dch o (7.1.1.4);
A0 l hp thu ca dung dch th mu trng (7.4).

Ch thch: - Th tch H2SO4 thm vo mu cn c a vo khi tnh ton.

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

lch chun 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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