TIU CHUN NH NC Nhm 1

TCVN 2307-78 CHT CH TH

CREZOLA
Indicators
Cresol red

Khuyn khch p dng
Tiu chun ny p dng cho cht ch th crezola ( octocrezolsunfoftalein). Ch th l mt
cht bt nh mu ti hay mu gch nh xanh, kh tan trong nc, d tan hn trong ru
etylic; d tan trong cc dung dch kim long v mui cacbonat ca kim loi kim.
Ch th chuyn mu hai khong pH: 0,2-1,8, chuyn t mu sang vng v 7,2-8,8,
chuyn t mu vng sang thm.
Cng thc phn t:
C
21
H
18
O
5
S
Cng thc cu to

khi lng phn t(theo khi lng nguyn t quc t nm 1969)-382,44 g.
1.YU CU K THUT
1.1 Cc ch tiu l ho ca cresola phi tng ng vi yu cu v mc cho trong bng.

Mc Tn gi cc ch tiu
Tinh khit phn
tch
1. Cresola C
21
H
18
O
5
S tnh bng phn trm khng nh hn.
2.Mt quang ca dung dch c 0,01 g/l pH 11 ti cc i ng cong hp
th nh sng khng nh hn
3.Cc cht khng tan trong ru,tnh bng phn trm, khng ln hn
4. Khong pH chuyn mu vng sang thm
5. nhy khi thay i pH

6.Hm lng nc tnh bng phn trm khng ln hn
7. Phn cn li sau khi nung di dng sunfat, tnh bng phn trm, khng ln
hn.
75
0,550

0,2
7,2-8,8
Bin i mu
theo hng
thm
2,0
0,2
2.PHNG PHP TH
2.1 Khi lng mu trung bnh khng nh hn 10 g
2.2 Xc nh hm lng crezola v mt quang ca dung dch ch th ( 0,004 g/l)
pH=11 ti cc i ca ng cong hp th nh sng
2.2.1 Thuc th, dng c v dung dch
Amoni hidroxit, dung dch 0,5%( pH 11 ) nc ct khng cha cacbon dioxit.Axit
clohidric, dung dch 1 N ( pH 0,1)
My so mu n sc vi cuvet hp th nh sng c chiu dy 10 mm.
Nc ct khng cha cacbon dioxit
2.2.2 Tin hnh th
Cn 0,05 g cht pha ch c tn nh vi chnh xc n 0,0002 g, cho vo bnh nh
mc dung tch 250 ml v ho tan vo 10ml amoni hidroxit,thm nc n vch mc, lc u-
dung dch 1.
Dng pipet hoc microburet chia n 0,02 ml ly 2 ml dung dch 1vo bnh nh mc
dung tch 100 ml, thm dung dch axit clohidric n vch mc, lc u-dung dch 2. Dung
dch 2 dng xc nh hm lng crezola .
o mt quang ca dung dch 2 so vi nc trong khong di sng 530-630 nm. Qua
10 nm xc nh mt gi tr , gn im cc i qua 5 nm o mt gi tr v gi tr mt
quang ti cc i ca ng cong hp th nh sng( l=520 65 nm)
o mt quang ca dung dch 2 so vi nc trong khong di sng 490-550 nm, qua
10 nm o mt gi tr v gi tr mt quang ti cc i ca ng cong hp th nh sng ( l=
57065 nm).
Dng pipet hoc microburet chia n 0,02 ml ly 2 ml dung dch 1vo bnh nh mc
dung tch 100 ml, thm dung dch amoni hidroxit n vch mc, lc u-dung dch 3. Sau ,
o mt quang ca dung dch 3 so vi nc di sng 530-610 nm, qua 10 nm o mt
gi tr, gn im cc i qua 5 nm o mt gi tr, ghi ly mt quang im cc i ca
ng cong hp th nh sng( l=57065 nm).
Xem cht pha ch l tng ng vi yu cu ca tiu chun ny, nu mt quang ca
dung dch 3 khng nh hn 0,550.
2.2.3 Tnh ton kt qu
Hm lng crezola ( x) tnh bng phn trm theo cng thc:
D.382,44 .100 .250 .100
x =
68500 .0,05 .2 . 1000
trong :
D- Mt quang ca dung dch 2 ti cc i hp th nh sng;
68500- h s hp th phn t ca dung dch crezola pH 0,1;
Chnh lch cho php gia cc kt qu ca hai php xc nh song song khng c vt
qu 1 % ( tuyt i).
2.3 Xc nh hm lng cc cht khng tan trong ru
2.3.1. Thuc th, dung dch v dng c
Nc ct
Ru etylic tinh ct k thut,96 v 50 %.
Chn lc
2.3.2 Tin hnh th
Cn 0,5 g cht pha ch c tn cn thn vi chnh xc n 0,01 g, cho vo cc dung
tch 300-400 ml, thm 150 ml ru 96 %. Dng knh ng h y li, cho ln bnh cch thu,
un 30 pht 60-70
0
C v khng cho dung dch si. Sau , rt vo cc 150 ml nc un
nng n 46-50
0

C v lc u. Ngay sau , lc lng cha qua chn lc s l s b n
khi lng khng i v cn vi chnh xc n 0,0002 g.
Gi ly dch lc xc nh nhy khi thay i pH theo iu 2,5.
Dng 100-150 m dung dch ru 50 % un nng n 40-50
0
C ra phn cn li trn
giy lc, sy trong t sy 105-110
0
C n khi lng khng i.
Xem cht pha ch l tng ng vi yu cu ca tiu chun ny, nu khi lng phn cn
li sau khi sy khng qu 1 mg.
2.4. Khong pH chuyn mu xc nh theo TCVN 1057-72
2.5 Th nhy qua vic thay i pH
2.5.1Thuc th v dung dch
Nc ct khng cha cacbon dioxit
Natri hidroxit, dung dch 0,02 N
2.5.2Tin hnh th
Cho 100 ml nc vo bnh nn dung tch 250 ml, thm 0,2 ml dch lc gi li iu 2.3.
Thm vo dung dch mu vng thu c 0,1 ml dung dch natri hidroxit.
Xem cht pha ch l tng ng vi cc yu cu ca tiu chun ny, nu mu ca dung dch
bin i theo hng thm.
2.6Xc nh hm lng nc
Tin hnh xc nh theo phng php sy trong my iu nhit v ly lng cn l 1 g.
2.7. Xc nh phn cn li sau khi nung
2.6.1. Thuc th v dung dch
Axit sunfuric
Axit nitric
2.6.2. Tin hnh th
Cn 2 g cht pha ch vi chnh xc n 0,01 g, cho vo chn s x nung trc n khi
lng khng i v cn vi chnh xc n 0,0002 g. Dng 0,5 ml axit sunfuric thm t
v un trn bnh cch ct n ht hi axit sunfuric.
Sau khi lm ngui chn, thm vo phn cn li 1,5 ml axit nitric, sy phn cn li trn bnh
cch ct v t cn thn. Sau , em nung trong l Mup 800-900
0
C n khi lng khng
i.
Xem cht pha ch l tng ng vi yu cu ca tiu chun ny, nu khi lng phn cn
li sau khi nung khng vt qu 4 mg.