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tCvn

Tiu chun Vit Nam

tcvn 6178 : 1996 ISO 6777: 1984 (E)

Cht lng nc - Xc nh nitrit Phng php trc ph hp th phn t


Water quality - Determination of nitriteMolecular absorption spectrometric method

H Ni - 1996

TCVN 6178: 1996

Li ni u
TCVN 6178: 1996 hon ton tng ng vi ISO 6777: 1984 (E) TCVN 6178: 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.

TCVN 6178: 1996

Tiu chun Vit Nam

TCVN 6178:1996

Cht lng nc - Xc nh nitrit Phng php trc ph hp th phn t


Water quality - Determination of nitriteMolecular absorption spectrometric method

1. Phm vi p dng Tiu chun ny quy nh phng php trc ph hp th phn t xc nh nitrit trong nc sinh hot, nc thi v nc th. 2. Lnh vc p dng 2.1 Khong xc nh Nng nit dng nitrit a (40 ml). 2.2 Gii hn pht hin Khi s dng cc cuvet c chiu di ng quang 40 mm v lng mu th 40 ml, gii hn pht hin c xc nh nm khong gia N = 0.001 n 0.002 mg/l. 2.3 nhy S dng 40 ml lng mu th v cuvet c chiu di ng quang 40 mm, cho hp thu vo khong 0.66 n v. S dng 40ml lng mu th v cuvet c chiu di ng quang 10mm, pN = 0,25 mg/l s cho hp thu vo khong 0,67 n v. 2.4 Cc cht gy nhiu Nu kim ca mu cao, c th gp mt vi cht loi nhiu (xem iu 9).
N N

ti 0.25 mg/l c th xc nh c khi s dng th tch mu th ti

= 0.062 mg/l s

TCVN 6178: 1996


Mt s cc cht thng gp trong cc mu nc c th nghim v kh nng gy nhiu. Chi tit y c nu trong ph lc. T nhng cht qua th, ch c cloramin, clo, thiosufat, natri polyphotphat v st (III) l gy nhiu mt cch ng k. 3. Nguyn tc Phn ng ca nitrit trong mu th vi thuc th 4 -aminobenzen sufonamid vi s c mt ca axit octhophosphoric pH bng 1.9 to mui diazo, m mui ny s to thuc nhum mu hng vi N-(1 naphtyl)- 1.2 diamonietan dihidroclorua (c thm vo bngthuc th 4 aminobenzen sufonamid. o hp thu 540 nm. 4. Thuc th Trong qu trnh phn tch, ch dng thuc th thuc loi phn tch v ch dng nc ct hoc nc c tinh khit tng ng. 4.1 Axit octhophosphoric, dung dch 15 mol/l. ( = 1.70 g/ml). 4.2 Axit octhophosphoric, dung dch 1.5 mol/l. Dng pipet ly 25 ml axit octhophosphoric (4.1) vo150 ml 25 ml nc. Khuy u v lm ngui ti nhit trong phng. Chuyn dung dch sang bnh nh mc dung tch 250 ml v pha long vi nc ti vch. Bo qun trong l thu tinh mu h phch, dung dch bn t nht trong vng 6 thng. 4.3 Thuc th mu Cnh bo - Thuc th ny l cht c. Trnh tip xc vi da hoc nut phi cc thuc th thnh phn ca n. Ho tan 40.0 g 0.5 g 4 -aminobenzen sufonamid (NH2C6H4SO2NH2) trong hn hp ca 100 ml 1 ml axit octophotphoric (4.1) v 500 ml 50 ml nc trong cc thu tinh c m. Ho tan 2.00 g 0.02 g N (1 naphtyl) 1.2 diamonietan dihidroclorua (C10H7- NH-CH2-CH2-NH22HCl) trong dung dch to thnh. Chuyn sang bnh nh mc dung dch 1000 ml v pha long vi nc ti vch. Lc u. Bo qun trong l thu tinh mu h phch, dung dch bn trong vng 1 thng nu gi nhit t 20C n 50C.

TCVN 6178: 1996


4.4 Ni trit, dung dch chun, N = 100 mg/l Ho tan 0.4922 g 0.0002 g natri nitric (sy kh nhit 1050C trong thi gian t nht l 2 gi) trong khong 750 ml nc. Chuyn ton b dung dch sang bnh nh mc dung tch 1000 ml v pha long vi nc ti vch. Bo qun trong l thu tinh mu nu c nt kn nhit t 20C n 50C. Dung dch ny bn t nht l mt thng. (Xem iu 10). 4.5 Nitrit, dung dch chun, N = 1,00 mg/l Dng pipet chuyn 10 ml dung dch nitrit chun (4.4) sang bnh nh mc dung tch 1000 ml v pha long vi nc ti vch mc. Chun b dung dch ny khi dng v loi b sau khi s dng. 5. Thit b Tt c dng c thu tinh phi c lm sch cn thn bng axit clohidric 2 mol/l v sau trng k vi nc. Cc thit b th nghim thng thng v Quang ph k thch hp cho vic o bc sng 540 nm, cng vi cc cuvet c chiu di ng quang trong khong t 10 nm n 50 nm. 6. Ly mu Mu phng th nghim c ng trong l thu tinh v phi c phn tch cng sm cng tt trong vng 24 gi sau khi ly mu. Bo qun mu nhit t 20C n 50C th c th bo qun nhiu loi mu th, nhng iu phi c kim tra. 7. Cch tin hnh 7.1 Phn mu th Th tch phn mu th ln nht l 40 ml. Lng mu ny thch hp cho vic xc nh nng nitrit ti = 0.25 mg/l. Phn mu th nh hn c th c s dng xc nh nitrit c nng cao hn. Nu mu th nghim c cha cc cht l lng, th phi lng hoc phi lc qua bng thu tinh trc khi ly phn mu th. 7.2 Xc nh

TCVN 6178: 1996


Dng pipet chuyn phn mu th c ly vo bnh nh mc dung dch 50 ml, v nu cn thit, pha long vi nc ti 40 ml 2ml. Ch thch: - iu thit yu l phi iu chnh th tch ti 40 ml + 2 ml m bo chnh xc t
c (sau khi thm thuc th) cho phn ng.

Dng pipet thm 1.0 ml thuc th mu (4.3). Lc u v pha long vi nc ti vch. Lc v yn. pH trong giai on ny phi t 1.9 0.1. (xem iu 9). t nht 20 pht sau khi thm thuc th, o hp thu ca dung dch bc song c hp thu ln nht, khong 540 nm, trong cuvet c chiu di ng quang thch hp, s dng nc lm dung dch i chiu. Ch thch: - Bc sng c hp thu ln nht phi c kim tra khi phng php ny c s dng ln u v phi c s dng trong tt c cc ln xc nh tip theo. 7.3 iu chnh mu Nu mu ca mu th l mu c th lm nhiu vic o d hp thu, x l mu p nh m t trong iu 7.2, nhng thay thuc th mu (4.3) bng 1 ml dung dch axit octophotphoric (4.2). 7.4 Th mu trng Tin hnh th mu trng nh m t 7.2, nhng thay phn muth bng 40 ml 2 ml nc. 7.5 Chun b th chun Dng buret ly cc th tch ca dung dch nitrit chun (4.5) c a trong bng 1 vo dy chnh gm 9 bnh nh mc dung dch 50 ml. Pha long lng dung dch cha trong mi bnh trn vi nc cho th tch ca dung dch t ti 40 ml 2 ml v tin hnh nh m t trong 7.2, t on th 2 n cui, s dng cc cuvet c chiu di ng quang c quy nh trong bng 1. hp thu ca cc dung dch khc tr i hp thu ca bnh zezo v v th ca hp thu tng ng vi khi lng nitrit tnh theo nit, i vi tng chiu di ng quang. th phi tuyn tnh v phi i qua im gc to . 8. Biu th kt qu 8.1 Phng php tnh hp thu c hiu chnh, Ar, ca dung dch th c tnh theo cng thc:

TCVN 6178: 1996


Ar = As - Ab Hoc, nu vic hiu chnh mu c thc hin, tnh theo cng thc: Ar = As - Ab - Ac Trong : As l hp thu o c ca dung dch th; Ab l hp thu ca dung dch th trng; Ac l hp thu ca dung dch c chun b hiu chun. Ch thch - iu cn thit l cc gi tr As, Ab v Ac c o trong cc cuvet c cng chiu di ng
quang i vi mt mu ring bit.

T hp thu c hiu chnh Ar, xc nh trn th chun (7.5) i vi chiu di ng quang thch hp ca cuvet, hm lng nitrit tnh theo nit bng microgam trn lt c tnh theo cng thc:

mN V
Trong : MN l khi lng ca nit dng ni trit tng ng vi hp thu c iu chnh (Ar), tnh bng microgam; V l th tch ca phn mu th, tnh bng mililit. Kt qu c th c biu th bng nng khi lng nit
N 2

hoc ni trit

NO2

tnh bng

miligam trn lit, hoc tng nng cc cht cha ion ni trit c(NO ), tnh bng micromol trn lit. Cc h s chuyn i thch hp c a trong bng 2.

TCVN 6178: 1996


Bng 1 Th tch dung dch ni trit chun (4.5) ml 0.00 0.50 1.00 1.50 2.00 2.50 5.00 7.50 10.00 g 0.00 0.50 1.00 1.50 2.00 2.50 5.00 7.50 10.00 Khi lng nit ni trit mN Chiu di ng quang ca cuvet mm 10 v 40 * 40 10 v 40 40 40 10 v 40 10 10 10

* c th s dng cuvet 50 mm Bng 2 pN mg/l PNO2mg/l pN=1 mg/l pNO2=1mg/l C(NO2-)= 1mol/l 1 0.304 0.014 3.29 1 0.046 C(NO2-) mol/l 71.4 21.7 1

Th d: Nng nit mg/l tng ng vi nng nitrit 3.29 mg/l.

TCVN 6178: 1996


8.2 chnh xc lch chun ca lp li v ti lp c xc nh nh ch dn trong bng 3. Bng 3*
Mu th Hm lng nitrit N Th tch phn mu th Chiu di ng quang ca cuvet mm 40 40 10 10 10 lp li 0,001 0,003 0,002 0,008 0,0011 0,0054 0,002 0,026 0,002 0,020 ti lp _ 0,002 0,0018 0,003 0,009 0,007 0,040 0,004 0,021 lch chun**

Mg/l Dung dch chun Dung dch chun Dung dch chun Dung dch chun Nc thi sinh hot Nc bin Nc sng 0,20 0,30 0,000 0,040 0,40 1,60 1,01

ml 40 40 40 5 5

40 25

10 10

0,0003 0,0026 0,008 0,0116

0,001 0,004 0,002 0,012

* Thng tin nhn c t kt qu trc nghim ca lin phng th nghim ca Anh c 5 thnh vin tham gia. ** Gi tr cao nht v thp nht t thc nghim ca lin phng th nghim. Tt c cc gi tr c 14 bc t do. 9. Cc trng hp c bit Nu mu th c tnh kim cao, pH khng t 1,9 0,1 sau khi x l phn mu th v pha long ti 40 ml, dung dch axit octophotphoric b sung (4.2) s c thm vo trc khi pha long, nh vy s t c pH quy nh. Tuy nhin, phng php s lm sai lch kim ca hidro cacbonat, t nht l 300 mg/l trong mt phn mu th l 40 ml ngoi sai lch vi pH c xc nh.

TCVN 6178: 1996


10. Cc lu khi tin hnh th V dung dch nitrit chun c th tr nn mt n nh, nng ca dung dch chun (4.4) c s dng c th c kim tra bng phng php sau y: Dng pipet ly 50 ml dung dch chun kali pemanganat, c(1/5 KMnO4) = 0,01 mol/l vo bnh nn 250 ml. Thm 10 ml 1ml dung dch axit sunfuric 2,5 mol/l v khuy u. Rt y dung dch nitrit chun (4.4) vo buret 50 ml v iu chnh sao cho u ca buret ngp di b mt ca dung dch pemanganat trong mi trng axit trong bnh. Tin hnh chun n mt mu. Khi va t n im cui, lm m dung dch ln n khong 400C v tip tc chun t t cho n khi mu ca pemaganat bin mt. Ghi li th tch ca dung dch nitrit chun s dng trong chun . 50 ml dung dch th tch chun kali pemanganat c(1/5 KmnO4) = 0,01 mol/l tng ng vi 3,502 mg nit. Do vy, i vi dung dch nitrit chun (4.4), th tch s dng chun phi l 35,02 ml. Dung dch nitrit chun ch thch hp nu th tch s dng chun nm khong 35,02 ml 0,40 ml. 11. Bo co kt qu Bo co kt qu phi bao gm cc thng tin sau: a) tham kho tiu chun ny; b) tt c cc chi tit cn thit nhn bit hon ton mu; c) cc chi tit lin quan n bo qun mu th nghim trc khi phn tch; d) cng b v lp li do phng th nghim t c khi s dng phng php; e) kt qu v phng php biu th s dng; f) cc chi tit v tt c cc s sai lch cch tin hnh th quy nh trong tiu chun ny hoc l bt k trng hp no khc c th nh hng n kt qu th.

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TCVN 6178: 1996


Ph lc A nh hng ca cc cht khc n kt qu th Cht Mui s dng Axetat Clorua Clorua Clorua Clorua Natri Khi lng cht * g 1000 100 1000 100 1000 6100 (HCO3) 12200 (HCO3) 1000 (N) 100 (N) 100 100 100 10 100 100 100 100 (SiO2) 100 100 (S2O3) 1000 (S2O3) 2 (Cl2) 20 (Cl2) 2 (Cl2) 20 (Cl2) 100 50 500 nh hng ** theo s xc nh ca mN = 0 g mN = 1,00 g mN = 0 g 0,00 0,00 -0,07 0,00 0,00 -0,07 0,00 -0,03 -0,13 0,00 0,00 -0,02 0,00 -0,01 -0,13 0,00 +0,03 +0,01 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 -0,06 0,00 0,00 0,00 0,00 0,00 0,00 -0,01 _ -0,01 0,00 0,00 0,00 +0,03 0,00 -0,01 -0,03 -0,04 +0,04 +0,04 -0,06 -0,06 0,00 0,00 +0,04 -0,03 0,00 -0,22 -1,01 -0,06 -0,30 0,00 -0,03 -0,80 +0,06 -0,06 -0,03 -0,03 0,00 -0,03 -0,03 -0,51 -0,07 -0,03 _ -0,09 -0,82 -0,07 -0,25 -2,81 -0,07 -2,78 -0,01 -0,82 -8,10

Magi Kali Kali Natri Natri Hidro cacbonat Hidro Natri cacbonat Nitrat Kali Amoni Clorua Cadmi Clorua Km Axetat Mangan Clorua St (III) Clorua St (III) Clorua ng Axetat Nhm Sunfat Silicat Natri Ur _ Thiosunfat Natri Thiosunfat Natri Clo _ Clo _ Cloramin _ Cloramin _ Hidroxylamoni Natri polyphotphat (hexametaphotphat) Natri polyphotphat (hexametaphotphat)

* Khi lng cht c mt trong mu th. Khi lng cho l mt thnh phn hoc hp cht tr khi c ch r trong ngoc kp. ** nh hng ln nht c coi l khng nhiu l cc gi tr sau: 0,00 g 0,02 g; 1,00 g 0,08 g; 10,00 g 0,14 g (gii hn tin cy 95%).

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