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tCvn

Tiu chun Vit Nam

TCVN 5988 : 1995 Iso 5664 : 1984

Cht lng nc
Xc nh amoni Phng php chng ct v chun

H Ni 1995

tcvn 5988 - 1995

Li ni u
TCVN 5988 - 1995 hon ton tng ng vi ISO 5664 1984; TCVN 5988 - 1995 do Ban K thut Tiu chun Cht lng nc TCVN/TC 147 bin son, Tng cc Tiu chun - o lng - Cht lng ngh v c B Khoa hc, Cng ngh v Mi trng ban hnh.

tcvn 5988 - 1995

Tiuchunvitnam

TCVN 1984 - 1994


ISO 5664-1984 (E)

Cht lng nc Xc nh amoni Phng php chng ct v chun


Water quality Determination of aminonium Distillation and titration method 1 Phm vi p dng
Tiu chun ny qui nh phng php chng ct v chun xc nh amoni trong ngun nc cha x l, nc ung v nc thi.

2 Lnh vc p dng
2.1 Khong nng Phng php cho php xc nh amoni tnh theo nit ti hm lng 10mg trong mu th. Nu th tch mu th l 10ml th hm lng ny tng ng vi nng mu CN = 1000 mg/l. 2.2 Gii hn pht hin Gii hn pht hin thc nghim (bc t do 4), dng 250 ml mu th l CN = 0,2 mg/l. 2.3 nhy nhy khi dng 100ml mu th, 1,0ml axit clohidric 0,02 mol/l tng ng vi CN = 2,8 mg/l. 2.4 Cc yu t cn tr Cht cn tr chnh l ure v n cng b chng ct di dng amoniac trong cc iu kin tng t v lm cao kt qu. Cc amin d b bay hI cng b chng ct v phn ng vi axit trong qu trnh chun , v nh vy lm cao kt qu. Cc cloramin c trong mu nc c clo ha b xc nh bng phng php tng t.

tcvn 5988 - 1995 3 Nguyn tc


iu chnh pH ca phn mu th n khong 6,0 7,4. Them magi oxit to mi trng kim yu, chng ct amoniac c gii phng v thu vo bnh cha c sn dung dch axit boric. Chun amoni trong phn ct c bng dung dch chun axit boric/ch th.

4 Thuc th
Trong phn tch ch dng cc thuc th tinh khit phn tch v nc c chun b theo mc 4.1.

4.1 Nc khng cha amoni, iu ch bng mt trong cc phng php sau: 4.1.1 Phng php trao i ion Cho nc ct chy qua ct nha cationit axit mnh (dng H+). Cha nc thu c trong bnh thy tinh c nt thy tinh kn. Thm vo bnh cha khong 10 g cationit cng loi cho mi lt nc thu c ( bo qun). 4.1.2 Phng php chng ct Thm 0,10 0,01 ml axit sunfuric (d = 1,84 g/ml) vo 1000 10ml nc ct v ct li trong my hon ton bng thy tinh. Nc thu c b i 50ml u tin, sau cha vo bnh thy tinh c nt thy tinh kn. Thm khong 10g cationit axit mnh cho mi lt nc thu c.

4.2 Axit clohidric, d= 1,18g/ml

4.3 Dung dch axt clohidric tiu chun, c(HCl) = 0,10 mol/l Pha ch dung dch ny bng cch pha long axit clohidric (4.2) v nh chun bng phng php thng thng. C th dng dung dch chun c bo m trn th trng.

4.4 Dung dch axit clohidric tiu chun, c(HCl) = 0,02 mol/ Pha ch dung dch ny bng cch pha long axit clohidric (4.2) v nh chun bng phng php thng thng. Cng c th pha long t dung dch 4.3 hoc mua trn th trng.

4.5 Dung dch axit boric/ ch th 4.5.1 Ha tan 0,5 0,1 g metyl loi tan trong nc vo khong 800 ml nc ri pha long thnh 1 lt. 4.5.2 Ha tan 1,5 0,1 g xanh metylen vo khong 800ml nc ri pha long thnh 1 lt. 4.5.3 Ha tan 20 1g axit boric (H3BO3) vo nc m. ngui n nhit phng. Thm 10 0,5 ml dung dch metyl (4.5.1) v 2,0 0,1 dung dch xanh metylen (4.5.2) ri pha long thnh 1 lt. 4

tcvn 5988 - 1995

4.6 Dung dch ch th xanh bromothymol 0,5 g/l Ha tan 0,5 0,02g xanh bromothyonol vo nc v pha long thnh 1 lt. 4.7 Dung dch axit clohidric 1% (theo th tch) Pha long 10 1ml axit clohydric (4.2) bng nc thnh 1 lt. 4.8 Dung dch natri hidroxit 1 mol/l Ha tan 40 2 g natri hidroxit vo khong 500 ml nc. Lm ngui n nhit phng v pha long thnh 1 lt.

4.9 Magie oxi nh khng cacbonat Nung magie oxit 5000C ui ht cacbonat.

4.10

Ht chng si bn ( bt) Cht chng to bt, th d cc mnh sp parafin

4.11

5 Thit b, dng c
Cc thit b thng thng trong phng th nghim, v cc thit b dng c sau: My chng ct, gm mt bnh ct dung dch 800 1000 ml, ni vi ng mao qun (capillave) v vi mt ng sinh hn thng ng, u ra ca sinh hn phi nhng ngp vo dung dch hp th. Ch thch v lm sch my chng ct: Cn lm sch my chng ct bng phng php sau y mi khi my ngng lm vic trong t ngy: Ly khong 350ml nc khng amoni (4.1) vo bnh ct. Thm vi ht bt (4.10), ni lp my v tin hnh ct n khi thu c t nht 100ml nc. b phn ct c v phn d trong bnh ct.

6 Ly mu v mu
Ly mu vo bnh bng polyetylen hoc thu tinh. Mu ly xong cn phn tch cng sm cng tt, nu lu gi cn 2-50C. Axit ho mu bng axit sunfuric n pH <2 gip cho lu gi mu tt, nhng phi ht sc trnh mu axit ho hp th amoniac t khng kh.

7 Cch tin hnh

tcvn 5988 - 1995


7.1 Chn th tch phn mu th Nu bit s b hm lng amoni gn ng trong mu, chn th tch phn mu th theo bng 1. Bng 1 Nng amoni CN, mg/l cho n 10 10-20 20-50 50-100 Th tch phn mu th * ml 250 100 50 25

* Khi dng dung dch chun axit clohidric (4.3) chun

7.2 Xc nh 7.2.1 Ly 50 5ml dung dch axit boric/ ch th (4.5) vo bnh hng ca my chng ct. Cn u mt ca ng chy ra t sinh hn ngp trong dung dch axit boric. Ly phn mu th (7.1) vo bnh ct. Ch thch: Nu mu cha clo, ui clo bng cch thm vi tinh th natri thiosunfat. Thm vi git dung dch ch th xanh bromothymol (4.6), v nu cn th iu chnh pH n khong t 6,0 (ch th c mu vng) n 7,4 (ch th c mu xanh) bng dung dch natri hidroxit (4.8) hoc axit clohidric (4.7). Sau thm nc khng amoni (4.1) vo bnh ct n th tch tng cng khong 350ml. Thm vo bnh ct 0,25 0,05 magie oxit nh (4.9) v vi ht bt (4.10). [Thm cht chng to bt (4.11) c th cn vi mt s mu nc thi]. Lp ngay bnh ct vo my. 7.2.2 un nng bnh ct sao cho tc chy vo bnh hng khong 10ml/pht. Dng ct khi

thu c khong 200ml bnh hng. 7.2.3 Chun dung dch trong bnh hng bng axit clohidric chun (4.4) n mu hng.

Ghi th tch HCl dng.

tcvn 5988 - 1995


Ch thch: 1) Axit clohidric tiu chun (4.3) c th dng chun mu c hm lng amoni cao. 2) Amoniac c th c chun khi ct vo bnh hng. Nu vic ct amoniac cn phi ko di chng t c nhng cht ngn cn ang b thu phn chm to ra amoniac. 7.3 Th trng Tin hnh th trng nh mc 7.2 nhng thay mu th bng 250 ml nc khng cha amoni (4.1).

8 Th hin kt qu
Nng amoni tnh theo nit, CN, tnh bng mg/l, c tnh theo cng thc

CN =

V1 V2 x c x 14,01 x 1000 V0

trong : V0 l th tch ca phn mu th (7.1), ml; V1 l th tch ca axit clohidric chun tiu tn trong chun mu, ml; V2 l th tch ca axit clohidric chun tiu tn trong chun mu trng (7.3), ml; C l nng chnh xc ca dung dch axit clohidric dng chun , mol/l; 14,01 l khi lng nguyn t ca nit, g/mol; Kt qu c th th hin bng nng khi lng (miligam trong lt) ca nit CN, ca amoniac CNH3, hoc ca ion amoni CNH4+ hoc bng micromol trong lt ca ion amoni, c(NH4+). H s chuyn i gia cc nng ny c trnh by bng 2. Bng 2 CN mg/l CN = 1mg/l CNH3= 1mg/l CNH4+ = 1mg/l c(NH4+) = 1mg/l Th d: Nng ion amoni CNH4+ 1mg/l tng ng vi nng nit l 0,777mg/l. 7 1 0, 823 0,777 0,014 CNH3 mg/l 1,216 1 0,944 0,017 CNH4+ mg/l 1,288 1,059 1 0,018 c(NH4+) g 71,4 58,7 55,4 1

tcvn 5988 - 1995


8.2 lp li lch chun c xc nh nh nu trong bng 3. Bng 31) Mu Hm lng amoni, CN, mg/l Dung dch chun Dung dch chun Nc cng lng Nc cng chy
1)

Th tch phn mu th, ml 250 250 100 25

lch chun, mg/l 0,23 0,56 0,70 0,16

Bc t do

4,0 40 35 1,8

10 11 16 11

S liu t Vng quc Anh

9 Bo co kt qu
Trong bo co kt qu cn c nhng thng tin sau: a) Trch dn tiu chun ny; b) mi chi tit nhn dng mu; c) cch lu gi mu trc khi phn tch; d) lp li phng th nghim khi dng phng php ny; e) kt qu v phng php th hin kt qu; f) chi tit v nhng khc bit so vi cch lm trong tiu chun ny, hoc nhng bt thng c th nh hng n kt qu. _____________________________________