tCvn

Tiu chun Vit Nam

tcvn 6198 : 1996 ISO 6058: 1984 (E)

Cht lng nc- Xc nh hm lng canxiPhng php chun EDTA

Water quality - Determination of calcium content - EDTA titrimetric method

H Ni - 1996

TCVN 6198:1996

Li ni u
TCVN 6198:1996 hon ton tng ng vi ISO 6058:1984(E); TCVN 6198:1996 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.

TCVN 6198:1996

Tiu chun Vit Nam

TCVN 6504:1999

Cht lng nc- Xc nh hm lng canxiPhng php chun EDTA

Water quality - Determination of calcium content - EDTA titrimetric method

1. Phm vi p dng Tiu chun ny qui nh phng php chun xc nh hm lng canxi trong nc ngm, nc b mt v nc ung s dng axit etylendiamintetra axetic (EDTA). Phng php ny cng c th s dng i vi nc th v nc nguyn liu dng cho cng nghip, vi iu kin l chng khng cha cc cht gy nhiu ca kim loi nng. Phng php ny khng p dng i vi nc bin v cc loi nc khc tng t c hm lng mui cao. Phng php ny c th p dng i vi nc c hm lng canxi t 2 n 100 mg/l (0.05 n 2.5 mol/l). i vi nc c hm lng canxi ln hn 100 mg/l, mu phi pha long khi phn tch. 2. Tiu chun trch dn ISO 385/1 Dng c thu tinh ca phng th nghim - Buret- Phn 1: Qui nh chung. ISO 5667 Cht lng nc - Ly mu Phn 1 - Hng dn xy dng cc phng n ly mu. Phn 2 - Hng dn k thut ly mu. TCVN : 1995. Hng dn bo qun v x l mu. 3. Nguyn tc

TCVN 6198:1996
Chun phc cht ca cc ion canxi vi dung dch mui dinatri EDTA th nc pH gia 12 v 13. HSN kt hp vi canxi to nn hn hp mu , c s dng nh cht ch th. Magie b kt ta di dng hidroxit v khng lm nh hng n vic xc nh. Trong khi chun , EDTA trc ht phn ng vi cc ion canxi t do v sau vi cc ion canxi kt hp vi cht ch th. Sau cht ch th i mu sang mu xanh sng. 4. Thuc th Ch dng cc loi thuc th thuc loi phn tch v nc ct hoc nc c tinh khit tng ng trong sut qu trnh phn tch. 4.1 Dung dch natri hidroxit, 2 mol/l. Ho tan 8 g natri hidroxit trong 100 ml nc mi chng ct. Bo qun trong chai polyetylen. Ch thch - phng b nhim bi cacbon dioxit ca khng kh. 4.2 Dung dch chun EDTA, c (Na2EDTA) 10 nmol/l. 4.2.1 Chun b Sy kh mt lng mui dinatri ca EDTA ngm 2 phn t nc (C10H14N2O8Na2.2H2O) 800C trong 2 gi, ho tan 3,725 g ca mui kh trong nc v pha long ti 1000 ml trong mt bnh cu. Bo qun dung dch EDTA trong chai polyethylen v thnh thong kim tra nng trong cc khong thi gian u n. 4.2.2 Chun ho Chun ho dung dch (4.2.1) da vo dung dch chun canxi (4.3) theo trnh t m t iu 7. S dng 20.0 ml dung dch chun (4.3) v pha long ti 50 ml. 4.2.3 Tnh nng Nng ca dung dch EDTA, c1 tnh bng milimol trn lit theo cng thc:

TCVN 6198:1996
trong c2 l nng ca dungdch chun canxi (4.3), milimol trn lit; V1 l th tch ca dung dch chun canxi, mililit; V2 l th tch ca dung dch EDTA s dng cho vic chun ho, mililit. 4.3 Canxi, dung dch i chiu chun, c(CaCO3) = 10 mmol/l. Sy mu canxi cacbonat tinh khit trong 2 gi 1500C, v lm ngui trong bnh ht m ti nhit phng. Ly 1.001 g cho vo bnh nn dung dch 500 ml, v lm m bng nc. Thm tng git axit clohydric 4 mol/l n khi ho tan ht cacbonat. Khng c axit d. Thm 200ml nc v un si trong vi pht ui ht cacbon dioxit. Lm ngui ti nhit phng v thm vi git dung dch ch th metyl . Thm dung dch amoniac 3 mol/l cho ti khi dung dch chuyn sang mu da cam. Chuyn lng dung dch sang bnh nh mc mt vch dung tch 1000 ml v thm nc cho ti vch. 1 ml dung dch ny cha 0.4008 mg (0.01 mmol) canxi. Ch thch - C th dng cc dung dch c sn trong thng mi. 4.4 Cht ch th, HSN Trn k 0.2 g HSN {axit 2hydroxy-1(2-hydroxi-4isunfua-1-naphtylazo)-3naphtoic}

(C21H14N2O7S.3H2O) v 100 g natri clorua (NaCl). Ch thch - Cht ch th ny cng c bit di tn "axit cancon cacboxylic" Cht ch th khc c th c s dng nh cancein {2.7 - bis {N,N-di (cacbonxymetyl) aminometyl}- fluorescein} (C30H26N2O13). 5. Thit b Cc thit b ca phng th nghim thng thng, v Buret c dung tch 25 ml, c chia theo cc khong 0.05 ml, ph hp vi qui nh ca ISO 385/1, Loi A, hoc dng c tng t. 6. Ly mu Ly mu theo cc phn tng ng ca ISO 5667. 7. Cch tin hnh

TCVN 6198:1996
7.1 Chun b mu th Phn mu th nn c nng canxi trong khong 2 v 100 mg/l (0.05 v 2.5 mmol/l). Nu nng vt qu 100 mg/l (2.5 mmol/l), pha long mt th tch bit trcca dung dch th sao cho nng nm trong khong qui nh v ghi h s pha long F. Nu cc mu th c axit ho bo qun, trung ho chng vi cc lng dung dch natri hidroxit c tnh ton (4.1). Trong phn tnh ton kt qu phi tnh ti vic pha long mu hoc mu th bng axit hoc kim. 7.2 Xc nh Dng pipet, chuyn 50.0 ml dung dch th sang bnh nn 250ml. Thm 2 ml dung dch natri hidroxit (4.1) v khong 0.2 g cht ch th HSN (4.4). Lc u v chun ngay lp tc. Thm dung dch EDTA (4.2) bng buret (4.2) (xem iu 5) v lc lin tc. Chun nhanh lc ban u v sau chm dn. im kt thc l khi mu sc i sang mu xanh r rt. V mu khng i khi thm mt git ca dung dch EDTA. 8. Biu th kt qu Hm lng canxi, Cca tnh bng mmol/l , theo cng thc:

C Ca =
trong

C1V3 V0

c1 l nng ca dung dch EDTA, tnh theo milimol trn lit; V0 l th tch ca mu th, tnh theo mililit; V3 l th tch ca EDTA dng chun , tnh theo mililit; Nu cn,hm lng canxi r Ca tnh bng miligam trn lit, theo cng thc:

Ca =
trong A l nguyn t lng ca canxi (40.08).

C1V3 A V0

TCVN 6198:1996
Nu s dng mu th pha long th phn tnh ton kt qu phi s dng h s pha long F. 10. Cc cht gy nhiu Cnh bo - Natri xyanua c. Cn thn khi vn chuyn v thi b ho cht. Cc dung dch c cha natri xyanua khng c axit ho. Cc ion kim loi nh nhm, bari, ch, st, coban, ng, mangan, thic v km lm nhiu vic xc nh, hoc bi v chng chun nh canxi, hoc bi v chng lm m i vic chuyn mu im cui. Nng ca orthophotphat ln hn 1 mg/l lm kt ta canxi pH chun , Nu vic xc nh thc hin qu chm hoc nu hm lng canxi cao (ln hn 100 mg/l hay 2.5 mmol/l) c th canxi cacbonat b kt ta. Cc ion kim loi gy nhim c th khng th hin. S gy nhiu ca st c nng 30 mg/l hoc t hn c th b che nu trc khi chun thm hoc l 250 mg natri xyanua hoc vi mililit trietanolamin gim s nhiu do nhm gy ra. Phi m bo dung dch c kim ho trc khi thm natri xyanua. Nu nh khn loi b c s nhiu, s dng phng php hp th nguyn t. Mt phng php thch hp s c xy dng thnh tiu chun sau ny. 11. Bo co kt qu Bo co kt qu gm nhng thng tin sau: a) tham kho tiu chun ny; b) nhn bit mu; c) kt qu tnh bng miligam trn lit, ghi chnh xc ti 1mg/l, hoc tnh bng mmol/l ghi chnh xc ti 0.02 mmol/lit; d) chun b mu th (nu c); e) ch ra cc thao tc khng ghi trong trnh t ca tiu chun ny hoc cc chi tit bt thng c th lm nh hng ti kt qu,

TCVN 6198:1996

Ti liu tham kho

[1] Hip hi Y t M, Hip hi nghin cu nc ca M, Lin on kim tra s nhim nc, lin hip bo ch. Cc phng php kim tra nc v nc thi, xut bn ln th 15., Denver, Colorado, USA, 1980, p.185. [2] SCHWARZENBACH, G v H. Chun phc, xut bn ln th 2, New york, Barnes v Noble, 1969. [3] WHO. Cc tiu chun Quc t v nc ung, Geneva, T chc Y t th gii, 1971. -------------------------------------------------