TIU CHUN NGNH

64 TCN 102:1997
PHNG PHP XC NH PHENOL TRONG NC THI
1. PHM VI P DNG, GII HN HM LNG
1.1 Tiu chun ny p dng xc nh hm lng phenol trong nc thi ca cc x nghip
sn xut ho cht, ch bin g (ch to vn dm, vn si p, g dn...) v cc x nghip sn xut
c nc thi cha phenol v cc dn xut ca phenol bng phng php o mu xc nh
phenol vi thuc th p.nitroanilin khi hm lng phenol nh (3mg/lit). Khi hm lng phenol ln
hn 3mg/lit cn pha long mu trc khi phn tch hoc phn tch theo TCVN 4581-88 (phng
php th tch o iot).
1.2 Cc dn xut v ng ng ca phenol c mt trong nc thi nu cng b ct cun v cng
c phn ng vi p-nitroanilin tng t nh phenol c coi l phenol v c tnh quy v
phenol trong kt qu phn tch.
2. NGUYN TC PHNG PHP
Phenol trong nc thi c tch khi nc bng cch ct trong mi trng axit (axit sunfuric,
axit photphoric). Phn ct ra c kim ho bng dung dch natri cacbonat 5% v cho tc dng
vi dung dch p.nitroanilin. Hp cht mu nu vng to thnh s c o mu 450nm. Cng
mu ca dung dch t l vi hm lng ca phenol trong mu nc thi.
tng nhy ca phng php v bn ca hp cht mu, c th dng n-butanol chit v
o mu lp dung mi hu c.
3. PHNG PHP LY MU
3.1 Ly mu nc thi theo TCVN 5992-95 v 5999-95.
3.2 Th tch mu ly xc nh phenol khng di 1000ml.
3.3 Bo qun v x l mu nc thi xc nh phenol theo TCVN 5993-95. Trong trng hp
cn bo qun mu lu hn 24 gi, cn dng natri hidroxit trung ho nc thi n phn ng
trung ho v thm d natri hidroxit vi lng 1g natri hidroxit cho 1 lit nc thi trung ho.
4. DNG C V HO CHT
4.1 Dng c
- B ct phenol (Hnh 1)
- Phu chit dung tch 500ml
- Bi thu tinh (cho vo binh ct)
- Pipet khc vch 2ml
- Cc thu tinh dung tch 500ml
- ng ong dung tch 100ml
- Bnh nh mc dung tch 100ml v 200ml
- My o mu quang in c cuvt 5cm.
4.2 Ho cht v thuc th.
- Cc ho cht s dng u phi l loi tinh khit ho hc (TKHH) hoc tinh khit phn tch
(TKPT)
- Nc ct s dng l nc ct 2 ln theo TCVN 2117-77
- Cc dung dch nu khng c ch gii g thm th coi nh dung mi l nc ct theo TCVN
2117-77

Ho tan 0,69g p.nitroanilin trong 150ml axit clohidric 1M, thm nc n 1 lt, lc k.
- Axit sunfuric, dung dch 1:3 (hoc axit photphoric, dung dch 1:3)
- Natri cacbonat (Na2CO3), dung dch 5%
- Natri nitrit (NaNO2), dung dch bo ho chun b nh sau:
Ho tan 42g natri nitrit trong 50ml nc ct nhit phng.
- ng sunfat (CuSO4), dung dch 10%
- n-Butanol (C4H9OH)
- Clorofom (CHCl3)
- Phenol (C6H5OH). Cc dung dch phenol chun b nh sau:
a/ Dung dch phenol gc: Cn 1,00g phenol ho tan trong nc ct (mi un si ngui). Pha
thnh 1 lit. Dung dch nhn c c chun 1mg/ml. Dung dch bn 1 thng.
b/ Dung dch chun phenol I: Ly 10ml dung dch phenol gc pha long thnh 1 lit bng nc ct
(mi un si ngui). Dung dch nhn c c chun 0,01 mg/ml, c gi l dung dch
chun phenol I.
Dung dch chun phenol I bn 1 ngy t lc chun b.
c/ Dung dch chun phenol II: Ly 50ml dung dch chun phenol I pha long thnh 1 lt bng
nc ct (mi un si ngui). Dung dch nhn c c chun 0,0005 mg/ml, c gi l
dung dch chun phenol II. Dung dch chun phenol II bn 2 gi t lc chun b.
5. CC YU T CN TR
5.1 nh hng ca sunfua v cc sn phm du m.
Sunfua (hidro sunfua, cc mui sunfua tan) v cc sn phm du m cn tr s xc nh v cn
phi loi tr.
5.1.1 Loi tr nh hng ca cc sn phm du m.
Ly 250ml nc thi vo cc thy tinh dung tch 500ml. Dng natri hidroxit ht kim ho mu
nc n pH 12-12,5 (nu mu c bo qun kim th cn kim tra li pH v iu chnh n
pH 12-12,5). Phenol c chuyn thnh natri phenolat. Chuyn dung dch vo phu chit dung
tch 500ml. Chit 2 ln cc sn phm du m bng tng lng 25ml clorofom. Phn dung dch
nc c chuyn li vo cc v chng trn ni cch thu 10-15pht loi clorofom d trc
khi chuyn sang khu x l loi tr nh hng ca sunfua hoc chuyn vo bnh ct ct
phenol sau khi trung ho n pH 4 v cho d 3-5ml axit sunfuric 1:3.
5.1.2 Loi tr nh hng ca sunfua.
Phn dung dch mu nc sau khi x l loi tr nh hng ca cc sn phm du m c
trung ho (bng axit sunfuric hoc axit photphoric 1:3) n pH 4. Thm 10-15ml dung dch ng
sunfat ( kt ta sunfua). Lc b kt ta. Axit ho (n hi tha axit) bng 3-5ml axit sunfuric v
chuyn vo bnh ct ct phenol.
5.2 nh hng ca cc tp cht khng bay hi.
Cc tp cht khng bay hi (k c cn khng tan...) nh hng n php o mu v cn phi
loi tr.
loi tr cc nh hng ny cn ct phenol khi nc thi. V phenol bay hi chm nn th
tch dch ct ra phi ln (c th tch mu ban u, v th trong qu trnh ct cn tip tc b
xung nc dch ct ra t n th tch cn thit).
Cch ct: 250ml (hoc 500ml) nc thi sau khi qua x l loi tr nh hng ca cc sn phm
du m v ca sunfua c axit ho v chuyn vo bnh ct (iu 5.1). Thm 5-10 vin bi thu
tinh vo bnh v ct n khi cn khong 10ml. Thm tip 250ml nc ct vo bnh v li ct tip

n khi thu c thm 200ml dch ct na. Gp dung dch ct v xc nh th tch, ghi s ml dch
ct thu c.
6. DNG NG CHUN
6.1 Dng ng chun gii hn nng phenol cao
(0-30 g phenol/100ml)
Chun b mt dy dung dch chun cha phenol trong bnh nh mc dung tch 100ml c cha
sn 80ml nc ct theo bng 1.
Bng 1
Dung dch s

Th tch dung dch chun phenol I, ml

0,0

0,2

0,5

1,0

1,5

2,0

3,0

Lng phenol tng ng, g

10

15

20

30

Thm vo mi bnh 2ml dung dch natri cacbonat 5%, lc trn cn thn. Chun b ng thi dung
dch p.nitroanilin diazo ho bng cch thm vo 35ml p.nitroanilin 7 git natri nitrit bo ho v lc
trn cn thn. Thm 5ml dung dch p.nitroanilin diazo ho vo mt bnh nh mc v thm
nc n vch. Lc trn cn thn v yn 15 pht. o mt quang ca cc dung dch mu
vi cuvet 5cm, knh lc mu tm (=450nm). Dung dch so snh l dung dch s 0. Dng giy k
ly biu din quan h gia lng phenol (trc honh) v mt quang dung dch (trc tung).
Nhn c ng chun s 1.
6.2 Dng ng chun gii hn nng phenol thp
(0-0,5 g phenol/100ml)
Chun b mt dy dung dch chun cha phenol trong bnh nh mc dung tch 200ml c cha
sn 180ml nc ct theo bng 2.
Bng 2
Dung dch s

Th tch dung dch chun phenol II, ml

0,0

0,2

0,5

1,0

1,5

2,0

Lng phenol tng ng, g

0,00

0,10

0,25

0,50

0,75

1,00

Thm vo mi bnh 2ml dung dch natri cacbonat 5%, 5ml dung dch p.nitroanilin diazo ho
(iu 6.1). nh mc n 200ml bng nc ct. Lc trn cn thn v yn 15 pht. Chuyn
ton b dung dch mu t bnh nh mc vo phu chit dung tch 50ml. Thm vo mi phu
chit 30ml n.butanol, y nt v lc phu chit 1 pht. yn phu chit 20-30 pht tch lp
n lc lp hu c tr nn trong sut. Tch b lp nc bn di, lp hu c bn trn c
chuyn vo cuvet 5cm.
o mu lp dung mi hu c trn my o mu knh lc mu tm (=450nm). Dung dch so snh
l lp dung mi hu c ng vi dung dch s 0 (bng 2).
Dng giy k li ng ng chun nh iu 6.1 v nhn c ng chun s 2.
7. TIN HNH XC NH
7.1 Nc thi cha phenol hm lng cao.
Ly 80ml hoc mt phn thch hp th tch dung dch ct ra (iu 5.2) c cha lng phenol
khng ln hn 30 g. Dng nc ct a th tch chung ca dung dch n 80ml trong bnh nh
mc dung tch 100ml.
Chun b ng thi mt dy mu chun nh bng 1 (iu 6.1)
Thm vo dung dch v dy mu chun ln lt:

- 2ml dung dch natri cacbonat 5%

- 5ml dung dch p.nitro anilin diazo ho (iu 6.1), lc trn cn thn yn 15 pht.
o mt quang dy mu chun v mu phn tch vi cuvet 5cm, knh lc mu tm ( = 450nm),
mu so snh l mu trng (s 0 bng 1)
Xy dng ng chun v t mt quang o c ca mu phn tch m tm ra hm lng
phenol trong mu.
7.2 Nc thi cha phenol hm lng thp
Ly 200ml dung dch ct ra (iu 5.2) cho vo phu chit dung tch 500ml. Ln lt thm:
- 2ml dung dch natri cacbonat 5%.
- 5ml dung dch p.nitroanilin diazo ho. Lc trn cn thn yn 15 pht.
- Thm 30ml n.butanol. Lc phu chit 1 pht. yn 30 pht cho lp hu c hon ton trong.
- Tch b lp nc v chuyn lp hu c vo cuvet 5cm.
Chun b ng thi mt dy mu chun nh iu 6.2
o mt quang dy mu chun v mu phn tch vi cuvet 5cm, knh lc mu tm (=450nm),
mu so snh l mu trng (s 0 bng 2).
Xy dng ng chun v t kt qu mt quang o c ca mu phn tch m tm ra hm
lng phenol trong mu.
7.3 Tnh ton kt qu.
Hm lng phenol trong mu nc thi c tnh theo cng thc:
X=

m
V

Trong :
X : hm lng phenol trong nc thi, mg/lit
m : lng phenol tm c theo ng chun, mg
V : th tch nc thi ban u tng ng vi lng m (mg) phenol, lit.
Hnh 1. B CT PHENOL