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Tiu chun Vit Nam TCVN 6491: 1999

ISO 6060: 1989

CHT LNG NC - XC NH NHU CU OXY HO HC


Water quality - Determination of the chemical oxigen demand
H Ni - 1999

Li ni u
TCVN 6491: 1999 hon ton tng ng vi ISO 6060: 1989.
TCVN 6491: 1999 do Ban K thut TCVN/TC147 "Cht lng nc" bin son, Tng
cc Tiu chun - o lng - Cht lng ngh, B Khoa hc, Cng ngh v Mi
trng ban hnh.

CHT LNG NC - XC NH NHU CU OXY HO HC


Water quality - Determination of the chemical oxigen demand
1. Phm vi
Tiu chun ny quy nh phng php xc nh nhu cu oxy ho hc COD ca
nc.
Tiu chun ny p dng c cho cc loi nc c gi tr COD t 30 mg/l n 700
mg/l Hm lng clorua khng c vt qu 1000 mg/l. Mu nc ph hp vi cc
iu kin ny c s dng trc tip cho phn tch.
Nu gi tr COD vt qu 700 mg/l, mu nc cn c pha long. Gi tr COD
nm khong 300 mg/l n 600 mg/l t c chnh xc cao nht.
Trong iu kin phn ng cho, cc hp cht hu c b oxy ho trit . Ngoi tr
cc cht c cc nguyn t c cu trc nht nh (v d nhn pyridine, cc hp cht
nit bc 4). Mt t cht k nc c th bay hi v thot khi s oxy ho. Cc cht v
c b oxy ho trong iu kin phn ng l,v d:
- cc ion brm, ion it;
- mt s hp cht lu hunh nht nh;
- cc ion nitrit;
- mt s hp cht kim loi.

Mt khc mt s cht nht nh c th tham gia phn ng nh l tc nhn oxy ho.


Tu thuc vo mc ch s dng kt qu php th, cn lu cc tnh hung ny.
Cc cht cn tr, ng ch l clorua, xin xem thm iu 10.
2. Tiu chun trch dn
TCVN 1609: 1999 Dng c o dung tch bng thu tinh dng trong phng th nghim
Buret, hoc ISO 385-1: 1984 Dng c thu tinh phng th nghim - Buret - Phn 1:
Yu cu chung.
ISO 5790: 1979 Sn phm ho cht v c dng trong cng nghip - Phng php
chung xc nh hm lng clorua - Phng php thu ngn.
3. nh ngha
p dng nh ngha sau: Nhu cu oxy ho hc (COD): Nng khi lng ca oxy
tng ng vi lng dicromat tiu tn bi cc cht l lng v ho tan trong mu
nc khi mu nc c x l bng cht oxy ho iu kin xc nh.
4. Nguyn tc
un hi lu mu th vi lng kali dicromat bit trc khi c mt thu ngn (II)
sunfat v xc tc bc trong axit sunfuric c trong khong thi gian nht nh, trong
qu trnh mt phn dicromat b kh do s c mt cc cht c kh nng b oxy
ho. Chun lng dicromat cn li vi st (II) amoni sunfat. Tnh ton gi tr COD
t lng dicromat b kh, 1 mol dicromat (Cr2O7-2) tng ng vi 1,5 mol oxy (O2).
Nu phn mu th c cha clorua ln hn 1000 mg/l cn phi p dng quy trnh
khc.
5. Thuc th v nguyn liu
Cnh bo: phng php ny lin quan n vic x l v un si cc dung dch axit
sunfuric c v dicromat. Cn phi s dng qun o bo h, gng tay v mt n. Khi
xy ra ri rt, nhanh chng ra nhiu ln bng nc sch l cch lm hiu qu v
n gin nht.
Khi thm axit sunfuric c vo nc cn phi lun lun tin hnh rt cn thn v lc
nh bnh cha.
Cn phi cn thn khi chun b v x l dung dch cha bc sunfat v thu ngn
sunfat v y l nhng cht c.
Cc thuc th qua s dng cha mui thu ngn, bc v cromat khi thi ra ngoi
cn phi c x l theo cc quy nh ca quc gia hoc a phng (xem thm
ISO 5790: 1979, ph lc B).
Khi phn tch, ch s dng cc thuc th c tinh khit phn tch c tha
nhn v nc ct hoc nc c tinh khit tng ng.

Ch thch 1 - Cht lng nc l yu t rt quan trng i vi chnh xc ca kt qu. Kim tra


cht lng nc bng cch thc hin mu trng (m t trong 8.2) v tin hnh song song mu th
khng un nng nhng gi nguyn cc iu kin khc. Lu s tiu tn ca dung dch st (II) amoni
sunfat (5.4) trong c hai trng hp. S khc nhau ln hn 0,5 ml chng t cht lng nc km.
xc nh gi tr COD di 100 mg/l th s khc bit khng c vt qua 0,2ml. Cht lng ca
nc ct thng c th c ci thin bng cch ct li t dung dch kali dicromat axit ho hoc
dung dch kali pecmanganat, dng thit b chng ct bng thu tinh ton b.

5.1. Axit sunfuric, c(H2SO4) = 4 mol/l


Thm t t v cn thn 220 ml axit sunfuric ( = 1,84 g/ml) vo khong 500 ml nc
ct. ngui v pha thnh 1000 ml.
5.2. Bc sunfat - axit sunfuric
Cho 10 g bc sunfat (Ag2SO4) v 35 ml nc. Cho t t 965 ml axit sunfuric c ( =
1,84 g/ml). 1 hoc 2 ngy cho tan ht. Khuy dung dch tng thm nhanh s
ho tan.
5.3. Kali dicromat
Dung dch chun c nng 0,040 mol/l, cha mui thu ngn.
Ho tan 80 g thu ngn (II) sunfat (HgSO4) trong 800 ml nc. Thm vo mt cch
cn thn 100 ml axit sunfuric ( = 1,84 g/ml). ngui v ho tan 11,768 g kali
dicromat sy kh 1050C trong 2 gi vo dung dch. Chuyn ton b dung dch
vo bnh nh mc v nh mc n 1000 ml.
Dung dch bn t nht 1 thng.
Ch thch 2 - Nu mun, c th s dng dung dch dicromat khng c mui thu ngn. Khi , thm
0,4 g thu ngn (II) sunfat vo phn mu th trc khi thm dung dch dicromat (5.3) vo bnh phn
ng m t trong 8.1 v lc u.

5.4. St (II) amoni sunfat, dung dch chun c nng , c[(NH 4)2Fe(SO4)2 . 6H2O]
0,12 mol/l.
Ho tan 47,0 g st (II) amoni sunfat ngm 6 phn t nc vo trong nc. Thm 20
ml axit sunfuric c ( = 1,84 g/ml). Lm ngui v pha long bng nc thnh 1000
ml.
Dung dch ny phi chun li hng ngy theo cch nh sau:
Pha long 10,0 ml dung dch kali dicromat (5.3) n khong 100 ml vi axit sunfuric
(5.1). Chun dung dch ny bng dung dch st (II) amoni sunfat ni trn s dng
2 hoc 3 git ch feroin (5.6).
Nng , c, ca st (II) amoni sunfat tnh bng mol trn lt, c tnh theo cng thc:

Trong : V l th tch dung dch st (II) amoni sunfat tiu tn tnh bng mililit.

5.5. Kali hidro phtalat, dung dch chun, c(K 1C8H5O4) = 2,0824 mmol/l.
Ho tan 0,4251 g kali hidro phtalat c sy kh 105 0C, vo trong nc v
nh mc n 1000 ml.
Dung dch ny c gi tr COD l thuyt l 500 mg/l.
Dung dch bn t nht mt tun nu bo qun trong xp x 4 0C.
5.6. Feroin, dung dch ch th
Ho tan 0,7 g st (II) sunfat ngm 7 phn t nc (FeSO 4 . 7H2O) hoc 1 g st (II)
amoni sunfat ngm 6 phn t nc [(NH4)2Fe(SO4)2 . 6H2O] trong nc. Thm 1,50
g 1,10 - phenantrolin ngm mt phn t nc C12H8N2 . H2O v lc cho n khi tan
ht. Pha long thnh 100 ml.
Dung dch ny bn trong vi thng nu c bo qun trong ti. C bn sn cc
dung dch ny trn th trng.
6. Thit b, dng c
Cc dng c thng thng ca phng th nghim, v
6.1. B chng ct hi lu, gm c mt bnh hoc ng phn ng 250 ml c c nhm
ni vi mt ng sinh hn trnh mt mt ng k cc cht bay hi.
C th phi lm mt sinh hn bng nc lnh hoc khng kh lnh.
Lm sch dng c mi bng cch tin hnh mu trng nh c m t trong 8.2.
Lm sch dng c dng xc nh COD bng cch sc vi vi nc ct sau mi
ln chun . Khng c s dng bt k cht ty ra no.
6.2. Bp un hoc cc phng tin t nng khc, c kh nng un si mu trong
vng 10 pht. Phi bo m rng cc dng c lm vic khng gy ra qu nng cc
b cho dung dch ang c un.
6.3. Buret chnh xc, dung tch 10 ml, c vch chia 0,02 ml ph hp vi TCVN 1609:
1988 (hoc ISO 385 - 1).
6.4. Ht si, ht thu tinh th ng knh 2 mm n 3 mm hoc cc loi ht si khc,
c lm sch theo quy trnh c m t trong 6.1.
Lu khi chun b dng c thu tinh
Cc dng c thu tinh cn c ra sch cn thn v gi khng b bm bi v
ch dng ring cho php th COD.
7. Ly mu v bo qun mu
Mu phng th nghim phi c u tin ly vo l thu tinh, mc d l polyethylen
cng thch hp.

Phn tch mu cng sm cng tt v khng qu 5 ngy sau khi ly mu. Nu mu


cn phi c bo qun trc khi phn tch, thm 10 ml axit sunfuric (5.1) cho 1 lt
mu. Gi mu 00C n 50C. Lc cc l mu bo qun v phi m bo chc chn
rng mu trong cc l c ng nht khi ly mt phn mu em phn tch.
8. Cch tin hnh
8.1. Xc nh
Chuyn 10,0 ml mu (pha long nu cn thit) vo bnh phn ng (xem 6.1), thm
5,00 ml 0,01 ml dung dch kali dicromat (5.3). Thm vo vi ht si (6.4) vo phn
mu th (thng l 10 ml) v lc trn u.
Thm t t 15 ml dung dch bc sunfat trong axit sunfuric (5.2) v nhanh chng lp
bnh vo ng sinh hn.
a hn hp phn ng ti si trong vng 10 pht v tip tc un 110 pht na.
Nhit ca hn hp phn ng cn phi t l 148 0C 30C.
Lm ngui ngay bnh phn ng bng nc lnh cho n khong 60 0C v ra ng
sinh hn vi lng nh nc. Tho ng sinh hn v pha long hn hp phn ng
cho n khong 75 ml v lm ngui n nhit phng.
Chun lng d dicromat bng st (II) amoni sunfat (5.4) s dng 1 hoc 2 git
ch th feroin (5.6).
Ch thch
3. cn phi un si nh hn hp phn ng v khng xy ra tro. Hn hp b si tro chng t
dung dch b t qu nng cc b, c th dn n kt qu sai. Hn hp phn ng b tro cn do t
nng qu mnh hoc do ht chng si km hiu qu.
4. mu du lng feroin thm vo khng c ch nh, nhng cn phi cho lng nh nhau cho mi
ln chun . im cui l thi im chuyn mu r rt u tin t xanh lc sang nu , mc d
mu xanh lc c th xut hin tr li sau vi pht.

8.2. Php th trng


Tin hnh hai php th trng song song cho mi ln xc nh theo quy trnh m t
trong 8.1, nhng thay th mu th bng 10,0 ml nc. Cn xem thm ch thch
trong iu 5.
8.3. Th kim chng
Mi ln xc nh cn kim tra k thut v tinh khit ca ho cht bng cch phn
tch 10,0 ml dung dch chun (5.5) theo cng quy trnh tin hnh nh vi phn mu
th.
Nhu cu oxy l thuyt ca dung dch ny l 500 mg/l, quy trnh th nghim t yu
cu nu kt qu ca th kim chng t nht t 96% gi tr ny.
Th trng phi c tin hnh nh nu ra trong 8.2

9. Biu th kt qu
9.1. Tnh ton
Nhu cu oxy ho hc COD, tnh bng miligam oxy trn lt, c tnh theo cng thc:

Trong :
c l nng ca st (II) amoni sunfat nh c tnh trong 5.4, tnh
bng mol trn lt;
Vo l th tch ca phn mu th trc khi pha long (nu c), tnh
bng mililit;
V1 l th tch ca st (II) amoni sunfat s dng khi chun mu trng,
tnh bng mililit;
V2 l th tch ca st (II) amoni sunfat s dng khi chun mu th,
tnh bng mililit;
8000 l khi lng mol ca 1/2 O2, tnh bng miligam trn lt.
Kt qu c tnh chnh xc n miligam trn lt.
Nu cc gi tr COD di 30 mg/l phi ghi trong bo co l "< 30 mg/l".
9.2. ti lp
S liu nhn c vi mt quy trnh rt gin nhau (1) thc hin bng cc phng th
nghim khc nhau vi cng mu nc thi c bn sn cho thy lch chun nh
hn 10 mg/l.
----------------1) Nhu cu xy ho hc cho nc thi v nc b nhim. London, Her Majesty's Stationery Office,
1978.

--------Khong 40 phng th nghim khc nhau phn tch mt s mu c gi tr COD =


500 mg/l. lch chun l 20 mg/l cho dung dch kali phtalat v 25 mg/l cho nc
thi cng nghip ly t nh my giy v bt giy. mc 50 mg/l, lch chun l
10 mg/l cho loi nc thi tng t.
Trong nghin cu khc, 2 mu nc thi cng nghip c 32 phng th nghim
phn tch. Mc COD l 140 mg/l v 160 mg/l, lch chun gia cc phng th
nghim l gn 14 mg/l cho c 2 mu.

10. Yu t cn tr
Php th nhy vi vi yu t cn tr, v nguyn l l vi clorua. Cc tc nhn kh
v c nh nitrit, sunfua v st (II) s lm tng kt qu. Thc t c th chp nhn
rng nhu cu oxy bao gm c cc tc nhn ny v coi nh mt phn ca gi tr COD
tng s ca mu.
Gim s cn tr ca clorua (nhng khng loi tr c hon ton) bng cch thm
thu ngn (II) sunfat. Cht ny cng vi ion clo hnh thnh phc tan thu ngn clorua
(II). Khi hm lng ion clorua vt qu 1000 mg/l, phi p dng mt quy trnh c
ci bin cho ph hp.
Cc hidro cacbon thm v pyridin b oxy ho khng ng k. Mt vi cht hu c d
bay hi c th trnh khi s oxy ho do bay hi. Cc cht bo mnh thng b oxy
ho mnh bi bc sunfat-axit sunfuric (5.2).
11. Bo co kt qu
Bo co kt qu cn phi c cc thng tin sau:
a) trch dn tiu chun ny;
b) s nhn bit chnh xc mu th;
c) kt qu, c biu th bng miligam trn lt O2;
d) bt k s thao tc no khc vi quy trnh quy nh hoc bt k tnh hung no
c th lm nh hng n kt qu.

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