TIU CHUN VIT NAM TCVN 6200 : 1996

ISO 9280: 1990 (E)

CHT LNG NC - XC NH SUNFAT - PHNG PHP TRNG
LNG S DNG BARI CLORUA
Water quality - Determination of sunfate - Gravimetric method using
barium chloride
Li ni u
TCVN 6200: 1996 hon ton tng ng vi ISO 9280: 1990 (E)
TCVN 6200: 1996 do Ban k thut Tiu chun TCVN/TC F9/SC1 thuc Ban k thut tiu
chun TCVN/TC/F9 ung bin son, Tng cc TC-L-CL ngh, B Khoa hc, Cng
ngh v Mi trng ban hnh.
1. Phm vi p dng
Tiu chun ny quy nh phng php trng lng xc nh sunfat trong nc.
Phng php ny c th p dng phn tch tt c cc loi nc bao gm nc bin v
hu ht nc thi cng nghip. Thng tin v cc cht c kh nng gy nhiu xem iu 8.
C th xc nh c nng sunfat (biu th theo SO 42-) trong khong t 10 mg/l n
5000 mg/l khi dng phn mu th xc nh (6.1). C th xc nh uc nng cao
hn sau khi pha long mu th nghim.
Gii hn ca s pht hin (vi 9 bc t do) l SO 42- = 10 mg/l.
2. Nguyn tc
axit ho mu bng axit clohidric bng cch un si vi dung dch bari clorua t nht 20
pht tng s kt ta bari sunfat lc qua phu lc thu tinh xp, ra ht clorua khi kt
ta, sy 1050C v cn li khi ngui. S tng khi lng ca phu do kt ta bari
sunfat c to thnh do phn ng ca ion bari v ion sunfat c trong mu.
3. Thuc th
Ch s dng cc thuc th loi tinh khit phn tch v nc ct hoc nc c tinh khit
tng ng.
3.1 Axit clohidric c(HCl) = 6mol/l.
Khuy cn thn 500 ml 10 ml axit clohidric m c { (HCl) = 1.18 g/ml} vi nc v
pha long n 1 lit trong bnh ong.
Bo qun trong chai l thu tinh hoc chai polyetylen. Dung dch bn trong thi gian di.
3.2 Bari clorua ngm hai phn t nc dung dch 100 g/l.
Cnh bo - Bari clorua c v c hi nu nut phi.
Ho tan 100 g 1 g bari clorua ngm hai phn t nc (BaCl 2.2H2O) trong khong 800 ml
nc, un nng hn hp ho tan tt. Lm ngui dung dch v thm nc n 1 lit
trong ng ong.
Bo qun trong chai l thu tinh hoc chai polyetylen. Dung dch bn trong thi gian di.
3.3 Dung dch natri hidroxit
c(NaOH) = 5 mol/l
Cnh bo - Dung dch natri hidroxit c hi khi tip xc vi da v mt.
Va cho va khuy ho tan 20.0 g natri hidroxit trong 100.0 ml nc. Bo qun trong
chai polyetylen.
3.4 Metyl da cam, dung dch ch th khong 1 g/l
Ho tan 100 g metyl da cam trong khong 50 ml nc, un nng ho tan tt. Lm
ngui dung dch v pha long n 100 ml bng nc trong ng ong.
Bo qun trong chai l thu tinh hoc chai polyetylen. Dung dch bn trong thi gian di.
3.5 Bc nitrat dung dch khong 0.1 mol/l
Ho tan 17 g 1 g bc nitrat (AgNO 3) trong khong 800 ml nc vpha long n 1 lit
trong ng ong.
Bo qun trong chai mu h phch. Dung dch bn trong thi gian di nu c bo v
khi nh sng.
3.6 Etanola, C2H5OH hoc ru tinh ch (95% etanol, 5% metanol).
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3.7 Ho tan 10.0 g 0.1 g natri clorua, dung dch 100 g/l.
Bo qun trong chai thu tinh hoc chai polyetylen.
3.8 Natri cacbonat, Na2CO3, khan
4. Thit b
Cc thit b phng th nghim thng thng, v
4.1 Phulc thu tinh xp, dung tch khong 30 ml, xp bng 4.
4. 2 Bnh thu tinh c vi (Buchner), c bo him lc chn khng.
4.3 Cn phn tch, c th cn chnh xc n 0.0002 g.
4.4 Bt c bng bch kim dung tch 250 ml.
5. Ly mu v chun b
5.1 Ly mu
Ly mu vo chai thu tinh hoc chai polyetylen v phn tch ngay trong ngy ly mu
hoc bo qun 20C n 50C khng qu mt tun. y chai ng mu loi ht
khng kh v do trnh nguy c b oxy ho mu cha sunfit hoc sunfua.
Ch thch 1 - Cc mu c hm lng cc cht hu c thp c th bo qun lu hn nhng cc php th
cn c tin hnh m bo mu bn.
5.2 Chun b mu th
xc nh sunfat trong dung dch, yn cho cc cht rn l lng lng xung trc khi
rt phn mu th (6.1). C th lc mu th nghim qua giy lc xp mn khng tro
chun b mu th.
6. Cch tin hnh
6.1 Phn mu th
Th tch phn mu th phi t 10 ml n 200 ml v phi cha khng t hn 50 mg ion
sunfat. Dng pipet ht mt phn mu th t mu lng (xem 5.2).
Ch thch 2 - i vi mu th cha mt lng ln cc cht rn l lng b lng th cn ong lng
mu th bng ng ong nhng c th gim chnh xc ca phng php ny.
6.2 X l s b
6.2.1 ong phn mu th (6.1) cho vo bnh c m dung tch 500 ml v thm 2 git ch th
metyl da cam (3.4). Trung ho phn mu th bng dung dch axit clohidric (3.1) hoc dung
dch natri hidroxit (3.3) tu thuc vo pH ban u. Thm 2 ml 0.2 ml axit clohidric v
sau nu cn th thm nc a tng th tch trong bnh c m n 200 ml 20 ml.
un si cc cht cha trong bnh c m t nht 5 pht.
Nu sau khi si dung dch trong, tin hnh theo 6.3. Nu dung dch c nhng cht khng
tan, tin hnh lc hn hp nng qua giy lc xp mn khng tro v ra giy lc bng mt t
nc nng, gp dch ra vo dch lc. Chuyn ton b dung dch vo cc c m dung tch
500 ml v tin hnh theo 6.3.
6.2.2 Nu nghi ng cc cht khng tan (b gi li trn giy lc) c cha sunfat khng tan
v mun tnh n trong kt qu cui cng th gi li giy lc v tin hnh theo trnh t nu
iu 9.2.
6.2.3 Nu trong phn mu th cha silic vi nng c th gy nhiu (xem iu 8) th
tin hnh x l s b theo phng php nu iu 9.1.
6.2.4 Nu trong phn mu th cha cc cht hu c vi nng c th gy nhiu (xem
iu 8), th tin hnh x l s b theo phng php nu iu 9.1.
6.3 Kt ta
un si dung dch c chun b cui giai on x l s b (6.2) v dng pipet thm
t t 10 ml 1 ml dung dch bari clorua (3,2) nng (khong 80 0C). ung ng dung dch t
nht 1 gi, y np, ngui v yn qua m nhit 50 0C 100C.
Ch thch 3 _ Vic thm bari clorua nng lm gim kh nng ng kt ca kt ta. Vic
un nng tip theo nhm lm ng t cc kt ta v lm cho n kt tinh tt hn ng thi
lm gim s ng kt sau .
6.4 Lc
6.4.1 Cch tin hnh
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Sy phu thu tinh n 1050C trong 1 gi v ngui trong bnh ht m.
Cn ni mt cch chnh xc (chnh xc n 0,0002 g) v sau lp n ln bnh Bunchner
(4.2). Lc kt ta c s dng ht nh. Dng a thu tinh c u bt cao su vt tt c
kt ta cn st li trong bnh c m v trng bng nc lnh vo ni. Ra kt ta trong
ni bng nc lnh khng cha clorua.
6.4.2 Th clorua trong nc ra
Ly khong 5 ml dch lc t 6.4.1 vo mt bnh c m nh cha khong 5 ml dung dch
bc nitrat (3.5). chc chn l dch ra v do kt ta bari sunfat khng c cha
clorua, quan st hn hp nu khng b c l t kt qu. Nu khng th phi tip tc ra.
Ch thnh 4 _ iu quan trng l cn kim tra khng c clorua di y ca ni.
6.5 Sy v cn
Ly ni ra v sy 105 0C 20C trong 1 gii. Cho ni vo bnh ht m, ngui n nhit
phng v em cn bit c khi lng chnh xc. Sy li ni l sy trong 10
pht v li lm ngui v em cn. m bo khi lng cn ln th hai khc vi khi
lng cn ln th nht khng qu 0,0002 g. Nu khng th phi lp li qu trnh sy, lm
ngui v cn cho n khi khi lng gia hai ln cn k tip nhau khng vt qu 0,0002
g.
Ch thch 5 _ C th rt ngn qa trnh sy nu ra kt ta bng 5 ml etanol (3.6) 3 ln.
6.6 Th mu trng
kim tra ni c s dng trong php th, tin hnh nh trong 6.3 n 6.5, nhng
s dng khong 200 ml 20 ml nc.
Ly khi lng ca ni sau khi lc (6.5) tr i khi lng ni trc khi lc c khi
lng trng tnh bng gam.
Ch thch 6 _ Trong qu trnh x l s b mu (6.2) nu cn thit phi lc, th lng nc
dng trong th trng trc tin phi lc nh m t trong on 2 ca 6.2.1, tr khi php
th trc chng t vic lc khng nh hng n th trng.
7 Biu th kt qu
7.1 Tnh ton
Khi lng ca bari sunfat trong mu th, m, tnh bng gam theo cng thc:
m = m 2 - m1 - m0
trong
m0 l khi lng th trng, ghi c theo 6.6, tnh bng gam;
m1 l khi lng ni, ghi c theo 6.4, tnh bng gam;
m2 l khi lng ni, ghi c theo 6.5, tnh bng gam.
Tnh nng sunfat, tnh bng miligam trn lt, theo SO 42- theo cng thc:

trong
m l khi lng ca kt ta bari sunfat, tnh bng gam;
V l th tnh phn mu th, tnh bng mililit, (xem 6.1);
0,4116 l h s trng lng.
Bng 1 _ Cc h s chuyn i theo cc n v nng khc
SO42- c (SO42-) S
mg/l mmol/l mg/l

SO42- = 1 mg/l 1 0,01041 0,3338

c(SO42-) = 1 96,06 1 32,06
mmol/l
7.2 chnh xc
lch chun ca ti lp v lp li c xc nh v ch ra trong bng 2.
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Bng 2 _ lch chun ca lp li v ti lp
Mu Th tch Nng sunfat r CVr R CVR
phn mu mg/l mg/l % mg/l %
th
ml

1 200 50 3,3

2 20 210 3,3 1,6 6,9 3,3

3 20 583 8,4 1,4 12,9 2,1

4 20 1160 9,3 0,8 11,6 1,0

5 20 1500 21,3

6 20 5000 28,4

trong
r l lch chun ca lp li;
CVr l h s bin thin ca lp li;
R l lch chun ca ti lp;
CVR l h s bin thin ca ti lp;
1,5,6: cc dung dch chun, s liu ca Anh, mt phng th nghim, 9 bc t do;
2: s liu ca c, 10 phng th nghim, 37 bc t do;
3: s liu ca c, 10 phng th nghim, 35 bc t do;
4: l s liu ca c, 9 phng th nghim, 32 bc t do;
Bng 3 _ Mc chp nhn i vi cc ion khc
ion Biu th theo Khi lng ti a trong
phn mu th
mg

cromat CrO42- 10

photphat PO42- 10

nitrat NO32- 100

silicat SiO22- 2,5

canxi Ca2+ 100

st (III) Fe3+ 50
8 Cc cht gy nhiu
Sunfua v sunfit c th gy nhiu nu mu b tip xc vi khng kh qu mc gy nn s
oxi ho thnh sunfat trc khi phn tch. Do , s c mt ca sunfua v sunfit, khi bt
u phn tch cn phi c chuyn thnh kh hidrosunfua v sunfua dioxyt bng cch
un si trong khi x l s b (6.2).
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Cc hp cht hu c vi lng ng k (th d mu c ch s pemanganat > 30 mg/l O 2)
c th gy nhiu bng cch hp th hoc ng kt ta. Lm theo quy trnh nu trong iu
9 th khc phc c tr ngi ny.
Cc ion v c khc trong mu th di mc nu trong bng 3 th khng gy nhiu.
9 Cc trng hp c bit
9.1 Loi b cc hp cht hu c
ong mt phn mu th (6.1) cho vo bt bay hi bng bch kim (4.4) v thm 2 git
ch th metyl da cam.
Trung ho phn mu th bng axit clohidric (3.10 hoc natri hidroxit tu thuc vo pH
lc u, sau thm 2,0 ml axit clohidric. Lm bay hi n gn kh trn bnh cch thu v
sau thm 5 git dung dch natri clorua (3.7) gi lng.
Bay hi n kh hon ton v sau un nng a cho n khi t nng m (khong
7000C) trn ngn la bunsen hoc trong l nung n khi to thnh tro.
ngui v sau lm m tro vi khong 10 ml nc. Thm 5 git axit clohidric (3.1) v
lm bay hi trn ni cch thu cho n kh. Sau n hi ngui, thm 3 ml 1 ml
nc v un hn hp trong ni (basin) n gn si. Sau tin hnh theo m t trong
6.2, bt u t "... lc hn hp nng ..." trong on th 2 ca 6.2.1.
9.2 Xc nh sunfat trong cht khng tan
9.2.1 t giy lc t 6.2.2 vo a bch kim (4.4), y np v t cho n khi ngn la
bunsen thp hoc cho vo l nung nhit phng v nng nhit n 500 0C t
chy ht giy lc. Trn cn nung vi 4 g 0,1 g natri cacbonat khan (3.8) v t mnh cho
n khi hn hp nng chy, gi trng thi nng chy trong 15 pht. ngui.
Thm 50 ml nc vo a bch kim, un nng ho tan hn hp nng chy v sau
lc dung dch qua giy lc th. Ra giy lc bng 20 ml nc. Gp dch ra vo dch
lc, tin hnh theo m t t 6.2 n 6.6 bt u t "... thm 2 git ch th metyl da cam..."
trong cu th nht ca 6.2.1.
Ch thm axit vo s c s bay hi mnh ca cacbon dioxit.
9.2.2 Tnh nng sunfat thm vo SO 42- (miligam trn lt) theo m t iu 7 v thm n
vo sunfat ho tan c xc nh trong dch lc khi x l s b (6.2) nhn c
nng sunfat tng s.
10 Ch khi tin hnh th
Lm sch ni thu tinh sau khi dng.
Bari sunfat c th loi b khi ni sau khi phn tch bng cch ngm n qua m trong
dung dch cha khong 5 g natri etylen diamin tetraaxetat (EDTA mui dinatri EDTA) v
khong 25 ml etanolamin [CH 2(OH)CH2NH2] trong 1 lt nc. Sau khi ngm ra ni bng
cch ht nc qua phn di trc khi sy v s dng li cho phn sau.
11 Bo co kt qu
Bo co kt qu phi bao gm cc thng tin sau:
a) tham kho tiu chun ny;
b) s nhn bit y v mu;
c) kt qu lm trn n 1 mg/l (gi tr di 100 mg/l) nhng khng qu 3 ch s c
ngha (gi tr trn 100 mg/l lm trn n 10 mg/l) hoc s liu chnh xc;
d) tnh hnh lp li t c;
e) cc chi tit chun b mu th (xem iu 5);
f) bt k trnh t c bit no c s dng;
g) mi thao tc khng quy nh trong phng php ny hoc cc tnh hung bt thng
khc lin quan n trnh t s dng c th nh hng n kt qu.