tcvn

tIu chun vIt nam

TCVN 6637 : 2000 ISO 10530 : 1992

cht lng nc - xc nh sunfua ho tan Phng php o quang dng metylen xanh
Water quality - Determination of dissolved sulfide Photometric method using methylen blue

H ni - 2000

Li ni u
TCVN 6637 : 2000 hon ton tng ng vi ISO 10530 : 1992 TCVN 6637 : 2000 do Ban k thut tiu chun TCVN/TC147 Cht lng nc bin son, Tng cc Tiu chun o lng Cht lng ngh, B Khoa hc, Cng ngh v Mi trng ban hnh.

TIu chun vIt nam

tcvn 6637 : 2000

Cht lng nc Xc nh sunfua ha tan Phng php o quang dng metylen xanh

Water quality Determination of dissolved sulfide Photometric method using methylen blue

1 Phm vi p dng

1.1 Khong nng p dng

Tiu chun ny qui nh ph ng php o quang xc nh sunfua ha tan trong n c. Ph ng php ny p dng xc nh sunfua ha tan nng 0,04 mg/l n 1,5 mg/l. Nhng nng cao hn c th c xc nh bng cch gim l ng mu v pha long mu n c. Ph ng php ny c p dng cho n c thi, n c t nhin khng yu cu lc.

1.2 Cn tr
Nhng ion sau y khng cn tr vic xc nh nu nng ca chng ch a t hoc v t Xianua Iodua Thiosunfat Thioxianat Sunfit 2 mg/l 20 mg/l 900 mg/l 900 mg/l 700 mg/l

TCVN 6637 : 2000

Xc nh phn sunfua trong polysunfua bng ph ng php ny l khng hon ton. Cacbon disunfua khi nng < 10 mg/l v / hoc etyl mecaptan < 1 mg/l khng nh hng n phng php. N c khng lc c theo iu 6 khng th phn tch bng ph ng php ny. Trong tr ng hp ny, sunfua d gii phng pH 4 c th c xc nh (mt tiu chun quc t v vn ny ang c son tho).

2 Tiu chun trch dn

TCVN 5993:1995 (ISO 5667-3:1985) Cht l ng n c - Ly mu - H ng dn bo qun v x l mu.

3 Nguyn tc
Lc mu tch cht rn l lng v sunfua kh tan. Gi sunfua trong n c lc bng cch thm dung dch ascobic. Gii phng sunfua t n c lc bng nit v chuyn vo bnh hng cha dung dch n c km axtat. Thm axit dimetyl- p -phenylendiamin vo bnh hng to leucometylen xanh, ri oxy ha thnh metylen xanh bng cch thm ion st (III). o hp th ca phc b c sng 665 nm.

4 Thuc th
Ch dng thuc th tinh khit phn tch v n c ct hoc n c c tinh khit t ng ng. N c cn ui oxy bng bin php thch hp nh un si hoc sc kh nit.

4.1 Axit sunfuric , (H 2 SO 4 ) = 1,84 g/ml 4.2 Natri hydroxyt (NaOH) , dung dch 32 % (m/m), c (NaOH) 10 mol/l. 4.3 Dung dch km axetat
Ha tan 20 g km axetat Zn(CH 3 COO) 2 2H 2 O trong n c v pha thnh 1 lt. Dung dch c th b c nh ng iu khng nh h ng n vic xc nh.

4.4 Dung dch m phtalat , pH 4,0 + 0,1

Ha tan 80 g kali hydrophtalat (C 8 H 5 KO 4 ) trong 920 ml n c. Kim tra pH dung dch v nu cn iu chnh pH n 4,0 bng dung dch natri hidroxit pha long [ c (NaOH) = 1 mol/l] hoc dung dch axit clohidric [ c (HCl) = 1 mol/l].

TCVN 6637 : 2000

4.5 Dung dch atcobic , pH 10 + 0,1
Ha tan 10 g axit atcobic (C 6 H 8 O 6 ) trong 90 ml n c v iu chnh n pH 10 bng dung dch NaOH (4.2). y ngay bnh. Chun b dung dch ny ngay tr c khi dng.

4.6 Dung dch thuc th to mu

Ho 2 g N,N-dimetyl-1,4-phenyl diamoni clorua (C 8 H 14 Cl 2 N 2 ) vo 200 ml n c trong bnh nh mc 1000ml. Thm cn thn 200 ml axit sunfuric H 2 SO 4 (4.1), lm ngui v thm n c n vch.

4.7 Dung dch amoni st (III) sunfat

Cho 50 g amoni st (III) sunfat (NH 4 Fe(SO 4 ) 2 12H 2 O) vo bnh nh mc 500 ml. Thm 10 ml H 2 SO 4 (4.1) v thm n c n vch.

4.8 Dung dch gc natri sunfua

Cho mt l ng natri sunfua Na 2 S xH 2 O (x = 7 9) t ng ng vi 0,5 g sunfua vi hm l ng thiosunfat < 5 % trong bnh nh mc 1000 ml. Thm n c (iu 4) n vch. Dung dch ny bn 2 n 3 ngy. Tr c khi dng, xc nh nng chnh xc bng ph ng php iod (xem ph lc A).

4.9 Dung dch chun natri sunfua

Dng pipet ht 10 ml dung dch gc natri sunfua (4.8) cho vo bnh nh mc 1000 ml. Thm nc n vch. 1 ml dung dch tiu chun ny cha khong 5 g sunfua. Nng chnh xc c xc nh bng ph ng php iod (xem ph lc A). Chun b dung dch tr c khi dng.

5 Thit b, dng c
5.1 Thit b lc, th d bm tim 3 vng dung tch 50 ml, c mng lc mt chiu (c l 0,45 m) (xem

hnh 1).

TCVN 6637 : 2000

Vi n c kh lc th c th dng thit b lc d i p sut bng mng lc (c l 0,45 m) (xem hnh 2).

5.2

Thit b phn gii tch sunfua , th d ch hnh 3, gm bnh phn ng dung tch 250 ml

c c bn ni vi phu nh git dung tch 100 ml, c ng dn kh n tn y bnh phn ng. C ng sinh hn ng hoc ng ng v bnh hp th. Kch th c nu hnh 3.

5.3 ng ong , dung tch 25 ml .

5.4 Bnh nh mc , dung tch 50 ml, 100 ml, 500 ml v 1000 ml. 5.5 Pipet ,dung tch 1 ml v 10 ml. 5.6 Pipet mt vch , dung tch 1 ml, 2 ml, 5 ml, 10 ml, 20 ml, 50 ml v 100 ml.

5.7 My pha ch . 5.8 Bm tim microlit . 5.9 Cp kh nit, tinh khit [99,996 % (m/m)].

5.10 Thit b o tc kh , thch hp o tc 40 l/h. 5.11 pH mt , c in cc thch hp. 5.12 My ph k hoc my quang k dng knh lc , thch hp o hp th b c sng

665 nm.

5.13 Cuvet , 1 cm.

TCVN 6637 : 2000

Knh lc

Hnh 1 Bm tim ba vng.

TCVN 6637 : 2000

Hnh 2 Thit b lc mng

TCVN 6637 : 2000

Kch th c tnh bng milimet

Hnh 3 - Thit b phn gii xc nh sunfua ha tan

TCVN 6637 : 2000 6 Ly mu v x l trc ti ni ly mu

Nu khng bit tr c khong nng ca mu, th cc phn ca mu th c lc v l u gi theo 6.1 v 6.2 cho php xc nh vi l ng mu nh hn. Phn mu lc theo 6.1 v 6.2 cn c phn tch trong vng 24 h.

6.1 Ly mu loi n c d lc
Ht bng pipet 5 ml dung dch ascobic (4.5) vo bnh nh mc 50 ml. Ht mu n c vo bm tim 3 vng dung tch 50 ml. Lp ci lc (xem 5.1) v lc n c vo bnh nh mc cho ti khi t vch mc.

6.2 Ly mu loi n c kh lc hn
Ht bng pipet 5 ml dung dch ascobic (4.5) vo bnh nh mc 50 ml. Thi bnh nh mc v my lc p sut bng nit khong 10 min. Lc n c cn xc nh vi p sut nit 2 bar v hng vo bnh nh mc ni trn cho ti vch mc. Vic ni gia my lc p sut v bnh nh mc cn thit k sao cho tip cn khng kh t nht. Thi gian lc khng qu 5 min (xem 1.2).

7 Cch tin hnh

7.1 Xc nh
Rt 25 ml dung dch m phlatat (4.4) vo bnh phn ng (xem hnh 3). Rt 20 ml dung dch km axtat (4.3) vo bnh hp th. Ni my v cho mt dng nit 40 l/h qua dung dch trong 2 min. Chuyn mu thu c t iu 6 vo bnh phn ng qua phu nh git. Trng phu nh git bng l ng nh n c (iu 4) v cho mt dng nit 40 l/h qua dung dch trong 30 min. Tho bnh hp th ra v cho vo 10 ml dung dch thuc th to mu (4.6) v tip theo l 1 ml dung dch amoni st (III) sunfat (4.7). Lm y bnh hp th bng n c (iu 4), y kn, lc v i 10 min.

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TCVN 6637 : 2000

Chuyn dung dch vo bnh nh mc 100 ml, trng cn thn bnh hp th bng l ng nh n c v gp vo bnh nh mc. nh mc bng n c (iu 4) v o hp th b c sng 665 nm so vi n c. Nu nng v t qu 1,5 mg/l sunfua th vic xc nh cn lp li vi l ng mu lc nh hn.

7.2 Th trng
Th mu trng nh mu tht ch khc thay mu tht bng n c (iu 4). hp th ca mu trng khng c lch qu nhiu so vi gi tr tnh ton A SO (xem iu 8).

8 Thit lp ng chun
ng chun thu c khi dng cuvt 1 cm l khng hon ton thng trn ton thang o nng . nh gi ch dng phn thng ca ng chun. Pha long dung dch tiu chun sunfua (4.9) c cc dung dch hiu chun ph kn thang nng cn phn tch. Nng khi l ng cc dung dch hiu chun cn tri u trn khong o. Th d, cho khong nng 0,2 mg/l n 0,7 mg/l (t ng ng vi 0,01 n 0,03 mg sunfua) th lm nh sau: Ly 20 ml dung dch km axetat (4.3) vo 7 bnh nh mc 100 ml. Dng pipet ht 4 ml, 6 ml, 8 ml, 10 ml, 12 ml v 14 ml dung dch tiu chun sunfua (4.9) cho vo 6 bnh. Bnh th 7 dng cho mu trng. Thm 10 ml dung dch thuc th to mu (4.6) v 1 ml dung dch amoni st (III) sunfat (4.7) vo mi bnh, thm n c n khong 40 ml. y cc bnh, lc v nh mc bng n c (iu 4). Sau 10 n 20 min, o hp th 665 nm, so vi n c trong cuvt i chng. Nng sunfua trong cc dung dch hiu chun l: 0 (trng); 0,2 mg/l; 0,3 mg/l; 0,4 mg/l; 0,5 mg/l; 0,6 mg/l; 0,7 mg/l. Xc nh nng chnh xc ca cc dung dch hiu chun bng ph ng php iod (xem ph lc A). Trn trc honh t nng khi l ng sunfua cc dung dch chun. Trn trc tung t gi tr hp th t ng ng.

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TCVN 6637 : 2000

Tnh ng hi qui tuyn tnh. Bit nng v hp th ca cc dung dch hiu chun c th da vo thng k tnh ton hm chun. dc b ca ng chun l nhy, tnh bng l/mg. im ng chun ct trc tung l hp th A SO ca mu trng. im ct trc tung v dc cn c kim tra th ng xuyn, nht l khi dng l thuc th mi. Mi my o ph, mi cuvt u c ng chun ring, hm chun ring.

9 Tnh ton
Nng ca sunfua ha tan trong mu n c, tnh bng mg/l, c tnh bng cng thc

( Al A l ,0 ) f bV
trong Al A l, 0 l f b V l hp th ca mu n c (xem 7.1); l hp th ca mu trng (xem 7.2); l k hiu ch di quang ca cuvet; l h s chuyn, f = 100 ml; l nhy thu c theo iu 8, tnh bng lit trn miligam; l th tch mu lc dng phn tch, V = 45 ml.

Khi tnh kt qu, mi b c pha long cn tnh n.

10 Biu th kt qu
Nng sunfua ha tan trong mu n c c lm trn n 0,01 mg nh ng khng qu 2 s c ngha. Th d sunfua ha tan: 0,55 mg/l.

11 c tnh ca ph ng php
V lc cc mu khng n nh l mt phn ca tiu chun ny, v s vn chuyn mu l kh khn do tnh khng bn ca sunfua ha tan nn mt nghin cu so snh c tin hnh thay cho php th

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TCVN 6637 : 2000

lin phng th nghim. Nghin cu so snh ny c lm bi cc nh phn tch trong 1 phng th nghim. Dung dch sunfua cha 1 mg sunfua trn lt c dng xc nh. Hm chun c xc nh l y = 0,010 79 x + 0,022 8 c tnh ca ph ng php cho bng 1. Ch thch 1 - i vi cc thnh vin c bo co hn bn gi tr trng bn gi tr u tin c dng
nh gi.

12 Bo co kt qu
Bo co kt qu cn gm nhng thng tin sau: a) trch dn tiu chun ny;

b) nhn dng mu; c) d) e) biu th kt qu, ph hp vi mc 10; x l mu tr c; mi s lch khi ph ng php ny hoc mi tnh hung c th gy nh h ng n kt qu. Bng 1 c tnh ca ph ng php

Thng s

na %

x mg/l 1,152

r
mg/l 0,020 6

VC r % 1,8

R
mg/l 0,020 9

VC R % 1,8

Mu

28

0,0

l n na x

l s thnh vin; l s gi tr o; phn trm loi b; l gi tr trung bnh; l lch chun lp li; l h s lch lp li;

r
VC r

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TCVN 6637 : 2000

R
VC R l lch chun ti lp; l h s lch ti lp;

Ph lc A (qui nh) nh chun dung dch gc sunfua

Dng pipet ht 25 ml dung dch iot ( c = 0,05 mol/l) vo bnh nn 250 ml v thm n c n khong 100ml. Thm 10 ml axit axtic v dng pipet ht 50 ml dung dch gc sunfua (4.8) cho vo dung dch iot. hn hp phn ng khong 3 pht. Chun l ng d iot bng dung dch thiosunfat ( c = 0,1 mol/l) n mu vng nht. Thm h tinh bt v chun tip n khng mu. Tnh nng dung dch gc sunfua, tnh bng mg/l, bng cng thc sau:

(V1 V2 ) 1,604 100 50

trong

V1 V2 1,604

l th tch dung dch iot, tnh bng mililit; l th tch dung dch thiosunfat tiu tn, tnh bng mililit; l h s hp thc ca phn ng.

___________________________

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