TIU CHUN VIT NAM TCVN 6224 : 1996

ISO 6059 : 1984 (E)

CHT LNG NC- XC NH TNG CANXI V MAGI PHNG PHP CHUN EDTA

Water quality - Determination of the sum of calcium and magnesium - EDTA titrimetric method

TCVN 6224 : 1996 hon ton tng ng vi ISO 6059 : 1984 (E).

TCVN 6224 : 1996 do Ban k thut tiu chun TCVN/TC 147 Cht lng nc bin son. Tng cc Tiu chun - o
lng - Cht lng ngh. B Khoa hc Cng ngh v Mi trng ban hnh.

1 Phm vi p dng

Tiu chun ny quy xc nh phng php chun dng axit etylendiamintetraaxetic (EDTA) xc nh tng nng
canxi v magi trong nc ngm, mt v nc ung

Khng p dng phng php ny cho nc thi v cc loi nc c nng mui cao nh nc bin. Nng ti thiu
c th xc nh c l 0,05 mmol/l.

2. Tiu chun trch dn

ISO 385/1 Dng c thu tinh trong phng th nghim - Buret - Phn 1: Nhng yu cu chung.

ISO 5667 Cht lng nc ly mu.

Phn 1: Hng dn lp chng trnh ly mu

Phn 2: Hng dn k thut ly mu (TCVN 5292:1995)

Phn 3: Hng dn bo qun v x l mu (TCVN 5293 : 1995).

3 Nguyn tc

Chun to phc canxi v magi vi dung dch nc ca mui dinatri ca EDTA pH 10. Dng modan en 11 lm ch
th. Ch th ny to hp cht mu hoc tm vi ion canxi v magi.

Trong qu trnh chun EDTA trc ht phn ng vi cc ion canxi v magi t do, sau im tng ng phn
ng vi cc ion canxi v magi lin kt vi cht th th gii phng ch th v lm mu dung dch i t sang tm sang
xanh.

Kt qu c th hin di dng nng . Nu hm lng canxi c xc nh ring th c th tnh nng magi.

4 Thuc th

Trong phn tch, ch dng cc thuc th tinh khit phn tch v nc ct hoc nc tinh khit tng ng.

4.1 Dung dch m

Ho tan 67,5 g amoni clorua (NH4Cl) trong 570 ml dung dch amoniac [25% (m/m); 20 = 0,910 g/ml]. Sau thm 5,0 g
mui dinatri magi EDTA (C10H12N2O8Na2Mg) ri pha long bng nc thnh 1000 ml.

Bo qun dung dch (bn c hn) trong bnh polyetylen.

Pha long 10 ml dung dch ny bng nc thnh 100ml. Nu dung dch nhn c khng c pH 10 ? 0,1 th phi b
dung dch gc.

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4.2 EDTA, dung dch chun, C(Na2EDTA) 10 mmol/l.

4.2.1 Chun b dung dch

Sau khi mui Na2EDTA (C10H14N2O2Na2, 2H2O) 800C khong hai gi. Ho tan 3,725 g mui kh trong nc v pha
thnh 1000 ml trong bnh nh mc.

Bo qun dung dch EDTA trong bnh polyetylen, v nh k kim tra nng ca n.

4.2.2 Chun ho

Chun ho dung dch (4.2.1) theo dung dch chun canxi (4.3) bng phng php trnh by iu 7.

Dng 20,0 ml dung dch chun canxi (4.3) v pha long thnh 50 ml.

4.2.3 Tnh nng

Nng dung dch EDTA C1, tnh bng milimol trn lt, theo cng thc

trong

C2 l nng ca dung dch tiu chun canxi (4.3(, tnh bng milimol trn lt;

V1 l th tch ca dung dch tiu chun canxi, tnh bng mililit;

V2 l th tch ca dung dch EDTA cn nh chun tnh bng mililit.

4.3 Canxi, dung dch chun, c(CaCO3) = 10 mmol/l.

Sy canxi cacbonat tinh khit rong hai gi 1500C ri ngui n nhit trong phng ht m.

Ly 1,001 g vo bnh nn c 500 ml, tm t bng nc. Thm tng git axit clohidric HCl 4 mol/l n tan hon ton.
Trng thm d axit. Thm 200 ml nc v un si vi pht ui kh CO2. Lm ngui n nhit phng v thm vi
git dung dch metyl . Thm dung dch amoniac 3 mol/l cho n dung dch chuyn sang mu da cam. Chuyn nh
lng vo bnh nh mc 1000 ml nh mc bng nc.

1 ml dung dch ny cha 0,4008 mg (0,01 mmol) canxi.

Ch thch - C th dng dung dch bn trn th trng.

4.4 Modan en 11, ch th

Ho tan 0,5 g modan en 11, dng mui natri ca axit 1 (1-hydroxy-2-naphtylazo)_6-nitro-2-naphtol-4-sunfonic

(C20H12N3O7SNa) trong 100 ml trietanolamin [(HOCH2CH2)3N]

C th thay 25 ml trietanolamin bng th tch n 25 ml etanol gim nht dung dng.

Ch thch - d nhn im cui, c th thm vo dung dch ch th 0,17 g mui metanil (natri ca 4-anilidoazobenzen
sunfonic). Mu ca ch th nh vy s chuyn t sng xm nht hoc xanh l cy.

5 Thit b dng c

Cc thit b th nghim thng thng v buret, dung tch 25 ml, vch chia n 0,05 ml. ph hp vi yu cu ca ISO
385/1, loi A hoc tng ng.

6 Ly mu

Ly mu theo cc phn c lin quan ca ISO 5667.

7 Cch tin hnh

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7.1 Chun b phn mu th

Khng cn x l mu trc, tr trng hp mu cha cc ht th th phi lc qua ci lc c kch thc l 0,45 m ngay
sau khi ly. Lc c th lm mt mt phn canxi v magi.

Nu nng tng canxi v magi trong mu vt qu 3,6 mmol/l th pha long mu v ghi h s pha long F.

Nu mu c axit ho bo qun th cn trung ho phn mu th bng mt th tch dung dch natri hidroxit NaOH 2
mol/l tnh ton trc. Khi tnh kt qu, cn ch n mi s pha long mu, v phn mu th do thm axit hoc kim.

7.2 Xc nh

7.2.1 Dng pipet ly 50,0 ml dung dch mu vo bnh nn dung tch 250 ml. Thm 4 ml dung dch m (4.1) v 3 git ch
th modan en 11 (4.4). Dung dch phi c pH 10,0 ? 0,1 v phi c mu hoc tm.

Tin hnh chun ngay bng dung dch EDTA (4.2) t burt (mc 5) ng thi khuy trong khi lc u. Chun
nhanh lc u v chm dn khi gn n cui. Tip tc thm dung dch EDTA khi mu ca dung dch bt u chuyn t
mu hoc tm sang mu xanh. im cui chun l lc nh cui cng cng bin mt. Sc thi mu dung dch
khng thay i nu thm mt git EDTA na.

7.2.2 Chun mt ln na theo cch sau:

Ly 50,0 ml dung dch mu vo bnh nn. Thm vo bnh mt th tch dung dch EDTA t hn 0,5 ml so vi th tch tiu
tn trong chun ln u (7.2.1). Thm 4 ml dung dch m (4.1) v 3 git ch th (4.4). Chun bng tng git EDTA
n im cui.

7.2.3 Nu th tch EDTA tiu tn trong chun nh hn 4,5 ml th cn tng th tch phn mu th v tng th tch dung
dch m (4.1) tng ng.

Nu th tch EDTA tiu tn trong chun ln hn 20 ml th gim th tch phn mu th v thm nc cho 50 ml.

8 Biu th kt qu

Hm lng tng canxi v magi, CCa+Mg, tnh bng milimol trn lt theo cng thc:

trong

C1 l nng ca dung dch EDTA, tnh bng milimol trn lt

V0 l th tch phn mu th (thng l 50 ml), tnh bng mililit.

V3 l th tch dung dch EDTA tiu tn trong chun (xem 7.2.2), tnh bng mililit

Nu c pha long mu th cn a thm h s pha long F vo tnh ton.

V tnh ton cng xem ph lc

9 chnh xc ca phng php

chnh xc ca phng php l ? 0,04 mmol/l, tng ng vi khong 2 git dung dch EDTA.

10 Cc cht cn tr

Cnh bo - natri xianua NaCN l cht c. Cn rt thn trng khi lm vic vi n. Khng c axit ho dung dch natri
xianua NaCN !

Cc ion nhm, bari, ch, st, coban, ng, mangan, thic, km cn tr vic xc nh bi chng hoc cng b chun vi
canxi v magi hoc chng cn tr s chuyn mu ca ch th im cui. Ion photphat v cacbonat c th kt ta canxi
pH chun . Mt s cht hu c cng c th cn tr vic xc nh.

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Khi nng st bng hoc nh hn 10 mg/l c th che bng cch thm vo 250 mg canxi xianua NaCN vo phn mu
th. Xianua cng loi tr c cn tr ca cc ion km, ng v coban. Cn chc chn dung dch c mi trng kim
trc khi thm natra xianua.

Nu khng loi tr c ht cc cht cn tr th phi dng phng php trc ph hp th nguyn t.

11 Bo co kt qu

Bo co kt qu cn c nhng thng tin sau:

a) trch dn tiu chun ny;

b) nhn dng y v mu;

c) kt qu, tnh bng milimol trn lt chnh xc n 0,02 mmol/l;

d) chun b phn mu th (nu c);

e) nhng khc bit so vi phng php nu trong tiu chun ny, hoc nhng tnh hung c th nh hng n kt qu.

TI LIU THAM KHO

[1] Hip hi bo v sc kho M, Hip hi cc Cng trnh v nc ca M, Hip hi kim tra nhim nc. Cc phng
php Tiu chun dng kim tra nc v nc thi. XB ln th 15, Denver, Colorado, USA, 1980, tr.185.

[2] Schawarzenbach, G v Flaschka, H. Chun Compiexon, XB ln th 2, New York, Bames & Noble, 1969.

Ph lc A

(Tham kho)

NHNG KHI NIM V CNG CA NC

A.0 M u

cng ca nc l mt khi nhim dng biu th hm lng ca canxi v magi trong nc. Ngi ta phn bit
nhiu loi cng ca nc ( cng chung, cng cacbonat...) v mi quc gia li theo mt nh ngha khc. iu
A.1 cho mt s th d v nh ngha .

A.1 nh ngha

A.1.1 cng tng: Nng tng s ca canxi v magi.

A.1.2 cng cacbonat: mt phn ca cng chung, tng ng vi hm lng cacbonat v hidro cacbonat trong
nc.

A.2 Cc thang cng

A.2.1 cng c

1 cng c (10HD) l gy ra bi mt hm lng canxi oxit 10 mg/l hoc mt nng canxi oxit 0,178 mmol/l.

Ch thch - cng c khng c dng na.

A.2.2 cng Anh

1 cng Anh (10Clark) l cng gy ra bi 1 Gren trong 1 imperial galng, tc l hm lng canxi cacbonat 14,3
mg/l hoc mt nng canxi cacbonat 0,143 mmol/l.

A.2.3 cng Php

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1 cng Php l cng gy ra bi mt hm lng canxi cacbonat 10 mg/l hoc nng canxi cacbonat 0,1 mmol/l.

A.2.4 cng M

cng M c biu din bng phn triu (ppmm) canxi cacbonat, hoc bng miligam canxi cacbonat trn lt, 1 mg/l
canxi cacbonat tng ng vi nng 0,01 mmol/l.

A.3 Bng tnh chuyn

tnh chuyn cng gia cc thang nu trn, dng bng A3 sau:

Bng 3

mmol/l c Anh Php M

0 0
DH Clark F ppm

mmol/l 1 5,61 7,02 10 100

0
c DH 0,178 1 1,25 1,78 17,8
0
Anh Clark 0,143 0,80 1 1,43 14,3

Php F 0,1 0,56 0,70 1 10

M ppm 0,01 0,056 0,070 0,1 1

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