TIU CHUN NH NC Nhm I

TCVN 3291-80
THUC TH
NG SUNFAT
Reagents
Cuprie sulphate
C hiu lc t 1-1-1982

ng sunfat l nhng tinh th mu xanh tm, tan trong nc, trong dung dch ru long v trong
axit.
Cng thc ho hc: CuSO
4
. 5H
2
O
Khi lng phn t : 249,68 ( theo khi lng nguyn t quc t nm 1961 ).
1. CH DN CHUNG
1.1.Cc thuc th c s dng trong cc phng php phn tch ho hc ca tiu chun ny
phi l loi tinh khit phn tch (TKPT).
1.2..Nc c dng trong cc php th phi l nc ct theo TCVN 2117-77.
1.3.Cc php th phi tin hnh song song trn hai mu cn
1.4.Ly mu theo TCVN 2843-79.
2.YU CU K THUT
Thuc th ng sunfat phi ph hp vi ch tiu v mc quy nh trong bng.

Mc , % Tn ch tiu
Tinh khit phn tch
(TKPT)
Tinh khit ( TK)
1. Hm lng ng sunfat CuSO
4.
5H
2
O khng nh hn
2. Hm lng cn khng tan, trong nc, khng ln hn
3. Hm lng clorua( Cl), khng ln hn
4. Hm lng st(Fe), khng ln hn
5. Cn khng kt ta vi hydrosunfua ( dng mui sunfat), khng ln
hn
6. Hm lng niken (Ni) khng ln hn
7. Hm lng nit tng khng ln hn
99,0
0,005
0,001
0,01
0,1
0,01
0,004
98,5
0,010
0,005
0,03
0,2
0,02
0,008

3. PHNG PHP TH
3.1.Xc nh hm lng ng sunfat
3.1.1 Thuc th
Kali iodua, dung dch 20 % trong nc;
H tinh bt, dung dch 0,5 % trong nc, dung dch mi pha theo TCVN 1055-71;
Axit axetic bng;
Natri thiosunfat, dung dch chun 0,1 N, nu khng c ng chun th chun b theo TCVN 1056-71.
3.2.1. Tin hnh phn tch
Cn chnh xc n 0,0002 g khong 1 gam ng sunfat vo bnh nn 250 ml v ho tan mu vo
50 ml nc. Cho vo dung dch 5 ml axit axetic, 15 ml dung dch kali iodua, y kn bnh bng nt
nhm, lc k v yn trong ch ti nm pht. Sau , chun lng iot thot ra bng dung dch natri
thiosunfat, cho h tinh bt vo gn cui php chun lm ch th.
Hm lng ng sunfat CuSO
4
5H
2
O (X) tnh bng phn trm theo cng thc:
(V V
0
) . 0,02497 . 100
X =
m
trong :
V- th tch dung dch natri thiosunfat 0,1 N dng chun , tnh bng ml;
V
0
- th tch dung dch natri thiosunfat 0,1 N dng chun mu trng cha 15 ml dung
dch kali iodua v 5 ml axit axetic, ( ml )
m- lng cn ng sunfat CuSO
4
.5 H
2
O tng ng vi 1 ml dung dch natri thiosunfat chun
0,1 N , ( g/ml )
3.2. Xc nh hm lng cn khng tan trong nc
3.2.1 Thuc th
Axit sunfuric, dung dch 20 %.
3.2.2. Tin hnh phn tch
Cn chnh xc n 0,01 g khong 50 g mu vo cc dung dch 250 ml, ho tan mu vo 100 ml
nc c un nng n 60 470
0
C v c axit ho bng 1 ml dung dch axit sunfuric. Lc
dung dch qua phu lc loi s 4 c sy n khi lng khng i v c cn chnh xc n
0,0002 g. Cn trn phu cvj ra bng 150 ml nc nng. Sau , sy phu cha cn nhit
105 4 110
0
C n khi lng khng i. Mu t tiu chun ny nu khi lng cn khng vt qu :
2,5 mg - i vi loi THPT;
5,0 mg - i vi loi TK.
3.3. Xc nh hm lng clorua
3.3.1. Thuc th
Axit nitric, dung dch 25 % v dung dch 1 %;
Bc nitrat, dung dch 0,1 N;
Dung dch ng sunfat khng cha clorua;
chun b nh sau:
Cn chnh xc n 0,01 g khong 5 g ng sunfat vo bnh nh mc dung tch 100 ml, ho tan
vo 50 ml nc, thm 10 ml dung dch axit nitric 25 %, 5 ml dung dch bc nitrat, nh mc bng
nc n vch, lc k v yn dung dch trong ch ti mi hai gi. Sau n lc dung dch qua
giy lc c ra bng dung dch axit ntic 1 % nng. Dung dch nhn c khng cha clorua v
dng chun b cc dung dch so snh.
Dung dch tiu chun cha clorua, chun b theo TCVN 1056-71, khi dng pha long n 0,01
mg/ml.
3.3.2 Tin hnh phn tch
Cn chnh xc 0,01 g khong 5 g mu vo bnh nh mc dung tch 100 ml, ho tan mu trong 50
ml nc, thm dung dch axit nitric 25 %. Sau , nh mc dung dch bng nc v lc k. em lc
dung dch qua giy lc, giy lc c tm t trc bng dung dch axit nitric 1 %.
Dng pipet ht 20 ml dung dch lc ( tng ng 1 g mu) vo ng so mu c vch mc 50 ml,
pha long dung dch bng nc n khong 45 ml, thm vo 1 ml dung dch bc nitrat v thm nc
n vch mc, lc k.
Mu t tiu chun ny, nu qua hai mi pht, dung dch mu khng c hn dung dch dung
dch so snh c chun b cng thi gian trong cng mt loi ng so mu c cng th tch v cha:
0,01 mg Cl - i vi loi TKPT;
0,05 mg Cl - i vi loi TK,
v 20 ml dung dch ng sunfat khng cha clorua, 1 ml dung dch bc nitrat v cc thuc th nh
trn.
3.4. Xc nh hm lng cht khng kt ta vi hydrosunfua.
3.4.1. Thuc th
Axit sunfuric, dung dch 20 %;
Hydrosunfua.
3.4.2. Tin hnh phn tch
Cn chnh xc n 0,01 g khong 10 g mu vo bnh nn, dung tch 250 ml c vch mc n 200
ml. Ho tan mu trong 150 ml nc, thm 10 ml dung dch axit sunfuric v un dung dch n
khong 60 4 70
0
C. Sau , nh mc n vch 200 ml v lc k.
Lc dung dch qua giy lc gp np, y dung dch vo phu trnh kh nmg oxy ho ng
sunfua v do ng c th lt qua gi lc. Dung dch nhn c chia lm hai, mt phn gi li
lm st.
C n kh 100 ml dung dch ny ( tng ng 5 g mu ) trong bt s c khi lng khng i
v c cn chnh xc n 0,0002 g. u tin c mu trn bp chc thu, sau c trn bp cch
ct n khi ngng bay hi khi ca axit sunfuaric. Nung cn nhit 500 4600
0
C n khi lng
khng i.
Mu t tiu chun ny nu khi lng cn khng vt qu :
5 mg - i vi loi TKPT;
10 mg - i vi loi TK,
gi cn li xc nh hm lng niken.
3.5. Xc nh hm lng niken
3.5.1. Thuc th
Amoni hidroxit, dung dch 25 %;
Amoni xitrat, dung dch 10 %;
Nc brom bo ho;
Dimetylglyoxim, dung dch 1 %;
Axit clohidric, dung dch c v 25 %;
Dung dch tiu chun cha niken, chun b theo TCVN 1056-71, khi dng pha long dn 0,01 mg/
ml;
Nc cng thu, mt th tch axit nitric v ba th tch axit clohidric c.
3.5.2. Tin hnh phn tch
Ho tan cn gi li mc 3.4.2. v 4 ml nc cng thu v c n kh trn bp cch thu. Sau
ho tan cn vo 1 ml dung dch axit clohidric 25 % v 19 ml nc, lc dung dch qua giy lc
khng tn. Ht 1ml dung dch ny, cho vo ng so mu, va lc va thm 2 ml dung dch amoni
xitrat, 1 ml nc brm, 7 ml dung dch amoni hydroxit v 3 ml dung dch dimetylglyoxim.
Qua 10 pht, so mu hng da cam ca dung dch mu vi mu ca dung dch so snh.
Mu t tiu chun ny nu mu ca dung dch mu khng m hn mu ca dung dch so snh
c chun b ng thi cng thi gian trong cng mt th tch v cha:
0,05 mg niken 0,05 ml dung dch axit clohidric 25 %, 2 ml dung dcha mni xitrat, 1 ml nc
brom, 7 ml dung dch amoni hydroxit v 3 ml dimetylglyoxim.
3.6. Xc nh hm lng st
3.6.1. Thuc th
Axit sunfosalisilic, dung dch 10 %;
Dung dch tiu chun cha st, chun b theo TCVN 1056-71, khi dng pha long n 0,01 mg/ml;
Amoni hydroxit, dung dch 25 %.
3.6.2. Tin hnh phn tch
Ht 5 ml dung dch thu dc t mc 3.4.2 vo ng so mu dung dch 100 ml . Thm 2 ml dung
dch axit sunfosalilic, lc u, thm 5 ml dung dch amoni hydroxit, nh mc, lc u, sau nm pht
em so mu.
Mu t tiu chun ny, nu mu vng ca dung dch mu khng m hn mu ca dung dch so
snh c chun b trong cng thi gian v cha trong cng mt th tch :
0,025 mg st - i vi loi TKPT;
0,075 mg st - i vi loi TK,
3.7. Xc nh hm lng nit tng
Xc nh theo TCVN 2317- 78 Thuc th. Phng php xc nh tng hm lng tp cht nit
mc 3. Phng php so mu bng mt.
Cn chnh xc n 0,01 g khong 1 g mu, cho vo bnh ct vacda v 10 ml dung dch natri
hydroxit, sau phn tch theo TCVN 2317- 78.
Mu t tiu chun nu sau 10 pht mu vng nu ca dung dch mu nht hn mu ca dung
dch so snh cng c b nh trn cha :
0,2 mg nit - i vi loi TKPT;
0,4 mg nit - i vi loi TK,
4. BAO GI V GHI NHN
4.1. Bao gi
Thuc th ng sunfat phi ng trong cc chai nha hoc chai thu tinh, ming rng c nt xoy
hoc hai ln nt.
Khi lng khng b ca thuc th khng qu 0,5 kg; 1 kg. Cc chai l ng gi phi kh, sch v
khng nh hng n cht lng ca thuc th.
4.2. Ghi nhn
Trn cc chai l phi gn nhn ph hp vi iu 4.2 ca tiu chun ny
Trn nhn cn ghi r;
C quan ch qun ca c s sn xut;
Tn c s hoc x nghip sn xut;
Tn gi ca thuc th v cng thc ho hc;
Cc ch tiu phn loi sn phm ( TKPT, TK ) theo TCVN . . .
Khi lng khng b;
S l hng.