tCvn

Tiu chun Vit Nam

tcvn 6179 -1: 1996 ISO 7150-1: 1984 (E)

Cht lng nc - Xc nh amoni Phn 1: Phng php trc ph thao tc bng tay
Water quality - Determination of ammonium Part 1: Manual spectrometric method

H ni - 1996

Li ni u:
TCVN 6179-1:1996 hon ton tng ng vi ISO 7150-1:1984 (E); TCVN 6179-1:1996 do Ban k thut tiu chun TCVN/TC 135/F9/SC1 Nc tinh lc 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 6179-1:1996

Cht lng nc - Xc nh amoni Phn 1: Phng php trc ph thao tc bng tay
Water quality - Determination of ammonium Part 1: Manual spectrometric method

1. Phm vi p dng 1.1 Tiu chun ny qui nh phng php quang ph thao tc bng tay xc nh amoni trong nc. Ch thch - Phng php quang ph t ng xc nh hm lng amoni c qui nh trong ISO 7150/2. 1.2 Loi mu th Phng php c th p dng phn tch nc sinh hot v hu ht nc thi v nc th. Vic p dng phng php ny cho nc c mu hoc nc mn s c tin hnh trc bng chng ct (xem iu 10). Cc cht gy nhiu xem iu 9. 1.3 Khong xc nh Vi hm lng nit dng amoni N ti 1 mg/l, s dng lngmu th ti a l 40 ml xc nh. Nng cao hn so vi nng k trn, c th xc nh c bng cch ly lng mu th nh hn. 1.4 Gii hn pht hin Khi s dng cc cuvet c chiu di ng quang l 40 mm v lng mu th bng 40 ml, gii hn pht hin nm trong khong N t 0.003 n 0.008 mg/l. 1) S liu ly t lin phong th nghim ca Anh bao gm 5 thnh vin. 1.5 nhy S dng lng mu th bng 40 ml v cuvet c chiu di ng quang 40 mm, N = 0.200 mg/l s cho hp th khong 0.69 n v.

S dng lng mu th bng 40 ml v cuvet c chiu di ng quang 10 mm, N = 0.750 mg/l s cho hp th khong 0.65 n v. 2. Tiu chun trch dn TCVN 5988- 1995 (ISO 5664 - 1984) Cht lng nc - Xc nh amoni - Phng php chng ct v phng php chun . 3. Nguyn tc o quang ph bc sng khong 655 nm ca hp cht mu xanh c to bi phn ng ca amoni vi salixylat v ion hypoclorit c s tham gia ca natri nitrosopentaxyano st (III) taxyano st (III) (natri nitroprusiat). Cc ion hypoclorit c to trong situ bng cc thu phn kim ca N, N/ dicloro- 1,3,5triazin 2,4,6 (1H,3H,5H) trion, mui natri (natri diclorosoxyanurat). Phn ng ca cioramin vi natri salixylat xy ra pH 12.6 c s tham gia ca natri nitroprusiat. Bt k cht cloramin no c mt trong mu th cng u c xc nh. Natri xitrat c trong thuc th cn s nhiu do cc cation, c bit l canxi v magi. 4. Thuc th Trong qu trnh phn tch, ch s dng thuc th loi phn tch v nc c chun b nh m t trong mc 4.1. 4.1 Nc Nc khng cha amoni c chun b bng mt trong nhng phng php sau y: 4.1.1 Phng php trao i ion Cho nc ct chy qua ct nha trao i cation c tnh axit mnh (di dng hydro) v thu li dch ra vo trong l thu tinh c nt thu tinh kn. Thm khong 10 g cng loi nha vo mi mt lit dch ra thu c vi mc ch bo qun. 4.1.2 Phng php chng ct Thm 0.10 0.01 ml axit sunfuric ( = 1.84 g/ml) vo 1000 ml 10 ml nc ct v ct li trong thit b chng ct bng thu tinh. Loi b 50 ml nc ct u, v sau thu dch ct trong l thu tinh c nt bng thu tinh y kn. Thm khong 10 g nhatao i cation c tnh axit mnh (di dng hydro) vo mi lit dung dch nc ct thu c. 4.2 Thuc th mu Ho tan 130 g 1 g natri salixylat (C7H6O3Na) v 130 g g 1 g trinatri xytrat ngm hai phn t nc ((C6H5O7Na3.2H2O) trong nc (4.1) trong bnh nh mc 1000 ml. Thm mt lng nc cho

tng th tch cht lng bngkhong 950 ml v sau thm 0.970 g 0.005 g natri nitrosopentaxyano st (III) 2 phn t nc [natri nitroprusiat, {Fe(CN)5NO}Na2.2H2O} vo dung dch. Ho tan cht rn trong dung dch, sau pha long bng nc ti vch. Bo qun trong l thu tinh mu h phch, thuc th ny bn t nht trong hai tun. 4.3 dung dch natri diclorosoxyanurat Ho tan 32.0 g 0.1 g natri hydroxit trong 500 ml 50 ml nc (4.1). Lm ngui dung dch n nhit trong phng v thm 2.00 g 0.02 g natri diclorosoxyanurat 2 phn t nc {(C2N3O3 Cl2Na.2H2O) vo dung dch. Ho tan cht rn v chuyn ton b dung dch sang bnh nh mc dung tch 1000 ml. thm nc ti vch. Bo qun trong l thu tinh mu h phch, thuc th ny n nh t nht trong hai tun. 4.4 Nit dng amoni dung dch chun N = 1000 mg/l. Ho tan 3.819 g 0.004 g amoni clorua ( c sy kh 1050C t nht 2 gi) vo khong 800 ml nc (4.1) trong bnh nh mc dung tch 1000 ml. Pha long n vch mc bng nc. 1 ml dung dch chun ny cha 1 mg nit amoni. Bo qun trong l thu tinh nt kn, dung dch bn t nht trong mt thng. 4.5 Dung dch chun nit dng amoni N = 100 mg/l. Dng pipet ly 100 ml dung dch chun nit amoni (4.4) cho vo bnh nh mc dung tch 1000 ml. Pha long bng nc ti vch. Bo qun trong l thu tinh nt kn, dung dch bn t nht trong mt tun. 4.6 Dung dch chun nit dng amoni N = 1 mg/l. Dng pipet ly 1 ml dung dch chun nit amoni (4.5) cho vo bnh nh mc dung tch 100 ml. Pha long bng nc ti vch. 1 ml dung dch chun ny cha 1 g nit amoni. Chun b dung dch ny ngay trc khi s dng.

4.7 Dung dch ra Ho tan 100 g 2 g kali hydroxyt trong 100 ml nc 2 ml nc. Lm ngui dung dch v thm vo 900 ml 50 ml etanol 95% (v/v). Bo qun trong l polyetylen. 5. Thit b Cc thit b th nghim thng thng, v 5.1 Ph k C kh nng hot ng bc sng 655 nm vi cuvet c chiu di ng quang khong t 10 n 50 mm. 5.2 Ni cch thu hoc t m c kh nng duy tr nhit 250C 10C. Lu v ra dng c thu tinh. Tt c dng c thu tinh phi c ra cn thn bng cch s dng dung dch ra (4.7) sau c trng k bng nc (4.1). 6. Ly mu v mu Mu th nghim c ng trong l thu tinh hoc polyetylen. Mu phi c phn tch cng nhanh cng tt hoc phi c bo qun nhit t 20C n 50C cho n khi c phn tch. axit ho bng axit sunfuric ti pH < 2 bo qun nhm trnh s nhim amoni c th xy ra ca mu c axit ho do hp th cc amoniac c trong kh quyn. 7. Cch tin hnh 7.1 Phn mu th Th tch phn mu th ln nht l 40 ml c th c s dng xc nh nng nit dng amoni ti
N

= 1 mg/l.

i vi mu th c hm lng amoni ln hn c th s dng mu th nh hn cho ph hp.Cc mu th nghim c cha cc ht l lng phi lng hoc lc qua bng thu tinh c trng nc trc khi ly mu th, hoc c th chng ct mu (xem iu 10). 7.2 Chun b dung dch th Dng pipet ly phn mu th (7.1) vo bnh nh mc 50 ml v nu cn, pha long bng nc ti 40 ml 1 ml (4.1).

7.3 Xc nh 7.3.1 To hp cht hp th Thm 4.00 ml 0.05 ml thuc th mu (4.2) v lc k sau thm 4.00 ml 0.05 ml dung dch natri dicloroxyanuarat (4.3) v li lc k. Ch thch - Sau khi cho thm pH ca dung dch phi l 12.6 0.1. Tnh axit hoc tnh kim qu mnh trong
mu th c th gy ra s sai lch.

Pha long nc ti vch (4.1). Lc k bnh v t vo t m, gi nhit 250C 100C. Ch thch - C th s dng nhit khc ca t m, nhng vic xc nh v hiu chun phi c thc hin
cng mt nhit (sai lch trong khong 1 k)

7.3.2 o ph Sau t nht 60 pht, ly bnh ra khi t m v o hp th ca dung dch ti bc sng c hp th ti a khong 655 nm, trong cuvet c chiu di quang hc thch hp so snh vi nc (4.1) trong cuvet chun. Ch thch - Bc sng c hp th ti a 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. 7.4 Th mu trng Tin hnh nh m t trong iu 7.2 v 7.3, nhng s dng 40 ml 1 ml nc (4.1) thay cho phn mu th. 7.5 Hiu chun 7.5.1 Chun b dy dung dch hiu chun Dng buret cho vo mt dy 9 bnh nh mc 50 ml cc dng dung dch chun nit dng amoni (4.6) c nu ra trong bng 1. Thm nc (4.1) ti dung dch 40ml 1 ml nu cn thit. 7.5.2 To hp cht hp th Xem iu 7.3.1. 7.5.3 o ph

Tin hnh theo iu 7.3.2 s dng cc cuvet c chiu di quang hc c qui nh trong bng 1, o hp th. Bng 1 - Th tch dung dch chun s dng trong dy cc dung dch hiu chun Th tch dung dch chun (4.6) ml 0.00* 2.00 4.00 6.00 8.00 10.00 20.00 30.00 40.00 * Thnh phn ** C th s dng cuvet c chiu di quang 50 mm. 7.5.4 V th chun Ly hp th nhn c ca cc dung dch khc tr i hp th ca thnh phn zero. V th v hp th tng ng vi khi lng nit dng amoni, mN cho mi chiu d quang ca cuvet. th ny phi tuyn tnh v phi i qua im gc to . 8. Biu th kt qu 8.1 Phng php tnh hp th do amoni c trong mu th, Ar c tnh theo cng thc: Ar = As - Ab Khi lng nit amoni, mN g 0 2 4 6 8 10 20 30 40 Chiu di quang ca cuvet mm 10 v 40** 40 40 40 40 10 10 10 10

trong As l hp th ca dung dch th (7.3.2) Ab l hp th ca dung dch th trng (7.4) Ch thch As v Ab phi c o trong cc cuvet c cng chiu di quang cho tng mu c th. Hm lng nit amoni pN, tnh theo miligam trn lit c tnh bng cng thc:

mN V
trong mN l khi lng ca nit dng amoni tnh bng g c xc nh t Ar v th chun (7.5.4) vi cuvet c chiu di quang thch hp. V l th tch mu th, tnh bng mililit. Xem bng 2 chuyn i N sang amoniac v nng amoni. Bng 2 - Bng chuyn i N mg/l N = 1mg/l (NH3) = 1mg/l (NH4)+ = 1mg/l c (NH4)+ = 1 mol/l Th d: Nng ion amoni (NH4)+ l 1 mg/l tng ng vi nng nit l 0.777 mg/l. 8.2 chnh xc Cc lch chun ca lp li v ti lp c xc nh theo bng3. 1 0.823 0.777 0.014 (NH3) mg/l 1.216 1 0.944 0.017 (NH4)+ mg/l 1.288 1.059 1 0.018 c (NH4)+ mol/l 71.4 58.7 55.4 1

9. Cc cht gy nhiu Mt s cc cht thng gp trong cc mu nc qua th nghim c th gy nhiu theo phng php ny. Chi tit y c a trong ph lc A. Cc cht gy nhiu ng k thng gp l nhiu do anilin v atanolamin, v th hin nhiu ni chung l t cc amin bc 1. Tuy nhin, cc cht nh vy thng t gp trong cc mu nc vi cc nng bnh thng. Tnh axit v tnh kim mnh s gy nhiu bng vic to ra cc hp cht hp th, s c mt ca bt k cht no gy nn vic kh cc ion hypolcorit, mc d cc trng hp ny thng khng chc chn xy ra trong hu ht cc mu nc. Trong cc trng hp nh vy vic tin hnh phi theo iu 10. Trong cc mu nc mn, nhiu do s kt ta ca magi xut hin khi kh nng to phc ca xytrat trong thuc th b vt qu mc. V nguyn nhn ny vic chng ct s b mu th l cn thit (xem iu 10). 10. Cc trng hp c bit Nu nh mu th m mu hoc c mn n mc m cc sai s trong php o hp th hoc l nhiu do nng ca magi hoc clorua cao, mu th nh th cn phi c chun b bng cch chng ct. Trnh t tin hnh s phi thc hin theo TCVN 5988 - 1995 (ISO 5664 - 1984), nhng phi lu rng vic thu thp cc dch ct s c thc hin trong mi trng axit hydrocloric 1% (V/V). Dch ct s c trung ho v lm thnh th tch V2, tnh theo ml. Th tch ca mu th c ly ra chng ct V1, tnh theo ml, cng phi ghi li. Mu th c chun b nh trn, c th c phn tch nh m t trong iu 7. Tuy nhin, kt qu s l nng ca nit dng amoni trong mu th. Nng trong mu gc c tnh bng cng thc sau:

PN1 V 2 V1
trong , N1 l kt qu ca mu th V1 v V2 c xc nh nh nu trn 11. Lu v vic tin hnh th 11.1 Nhng vn chung Vic xc nh nng amoni thp, thc t d b nh hng khng tt do s c mt ca cc vt amoni trong mi trng phn tch. Do vy cn lu ti tt c cc ch dn a ra trong tiu chun ny, phi hn

ch ti a tnh d b nh hng ny, kh nng ca cc thit b nh hng vn cn. Hai phng php ch dn v cc nh hng c th c trnh by nh sau: 11.2 Gim st cc gi hp th ca dung dch hiu chun v dung dch trng Gi tr hp th thc t (c o tng ng trong cuvet chun) nhn c cho dung dch th trng v dy cc dung dch hiu chun phi ghi li trong tng trng hp. Vic ghi li cc gi tr ny s gip cho vic pht hin ra lch. lch nh vy c th do s nhim amoni ca dung dch th trng hoc l dy dung dch hiu chun vi amoni, hoc l do thiu mt hoc nhiu thuc th. Trong c hai trng hp, cc bin php sa li s c thc hin. Ph lc B trch dn cc gi tr in hnh nhn c trong cc thc nghim ca lin phng th nghim. 11.3 Kim tra chnh xc ca kt qu phn tch Khi phng php ny c s dng ln u, vic nh gi lch chun chung (vi t nht l 9 bc t do) phi tin hnh bng cch xc nh dung dch nit dng amoni chun c kim tra vi nng khong 50% nng ca dung dch chun c nng cao nht. Dung dch chun kim tra ny s ng c s dng hiu chun. Mt phn ca dung dch chun kim tra ny phi c phn tch theo tng t xc nh tun t. Vic hiu chun s c thc hin vi dy dung dch hiu chun. Nng xc nh c ca dung dch chun kim tra s nm gia di nng : N2 3s1 trong ,
N2 l

nng ca dung dch

s1 l sai lch chun trc khi xc nh i vi dung dch chun kim tra Nu tiu chun ny khng t yu cu trong bt k t phn tch so snh no, phi nguyn cu nguyn nhn gy ra cc sai lch v lp li qu trnh phn tch. Sau t nht l trn 20 ln xc nh dung dch chun kim tra, vi tt c cc gi tr km theo vi cc tiu chun nu trn, cc gi tr s c s dng tnh ton li gi tr s1 cho ln s dng tip theo. Bng 3 - lch chun ca lp li v ti lp Mu ** Nng nit amoni N Chiu di quang ca cuvet lch chun, s lp li ti lp

mg/l Dung dch chun Dung dch chun Dung dch chun Nc ging Nc thi sinh hot * S liu ly ca Anh 0,150 1,00 5,00 0,217 0,877

mm 40 10 10 40 10

mg/l 0,002 *** 0,005 - 0,025+ 0,036*** 0,002+ 0,007 - 0,027+

mg/l 0,015 - 0,038+ 0,004 - 0,010+ 0,009 - 0,027+

** Ton b cc th tch mu th c ly l 40 ml ngoi tr dung dch chun 5,00 mg/l l 5 ml *** Kt qu t mt phng th nghim: 9 bc t do + Gi tr cao nht v thp nht ly t cc thc hnh ca lin phng th nghim vi s tham gia ca 5 thnh vin. Tt c cc gi tr u c 9 bc t do. 12. Bo co kt qu Bo co kt qu gm cc thng tin sau: a. tham kho tiu chun ny; b. tt c cc thng tin cn thit cho vic nhn bit hon ton mu th; c. chi tit v lu kho v bo qun cc mu th phng th nghim trc khi phn tch; d. cng b v lp li t c; e. kt qu v phng php biu th c s dng; f. chi tit ca bt k thao tc no khng nm trong phn ny ca tiu chun, hoc c coi l t chn, cng vi cc tnh hung bt k no khc c th nh hng n kt qu th.

Ph lc A nh hng ca cc cht khc ln N * Cht Nng trong 40 ml mu th (mg/l) Thc t *** N (mg/l) B ** Natri clorua Natri bicarbonat Natri octtophotphat Natri sunfat Kali florua Kali nitrat Natri silicat Natri thiosunfat Kali cyanua Canxi clorua Magi axetat St (III) sunfat Nhm sunfat ng sunfat Km sunfat Ch axetat Cl HCO3 PO4 SO4 F N SiO2 S2O3 CN Ca Mg Fe Al Cu Zn Pb mg/l 1000 1000 100 500 5 50 50 10 5 500 50 10 5 5 5 5 0,000 +0,002 +0,002 0,000 0,000 +0,002 +0,006 +0,003 -0,001 +0,002 0,000 +0,004 +0,001 0,000 +0,003 +0,003 +0,001 0,200 +0,013 +0,002 -0,001 +0,001 -0,001 +0,002 0,000 +0,007 +0,019 +0,013 -0,009 +0,003 +0,008 +0,011 +0,006 +0,016 0,500 +0,033 -0,025 -0,015 +0,016 -0,001 +0,002 +0,011 nh hng ca cht ln N

Anilin Etanolamin

C6H5NH2 NH2C2H4OH

1 1

0,040 + 0,164

0,040 + 0,114

* S liu ly ca Anh ** Np ion, (nu c), b b qua *** Nu cc cht khc khng gy nhiu, 95% gii hn tin s l Nng quy c N (mg/l) 95% gii hn tin cy (mg/l) 0,000 0,003 Ph lc B Gi tr hp th in hnh * i vi dung dch chun v dung dch mu trng Dung dch c nng mg/l Chiu di quang ca cuvet mm Phng th nghim 1 0,000 0,050 0,500 * S liu ly ca Anh ** Gi tr hp th trung bnh nhn c trong qu trnh thc hnh ca lin phng th nghim trong 5 ngy 40 40 10 0,07 0,26 0,50 Phng th nghim 2 0,12 0,48 Phng th nghim 3 0,09 0,22 0,38 Phng th nghim 4 0,06 0,24 0,45 hp th ** 0,200 0,014 0,500 0,021