TIU CHUN NH NC Nhm I

TCVN 2841-79
THUC TH
AMONI CLORUA
Reagents
Ammonium chloride
C hiu lc t 1-7-1980

Amoni clorua l nhng tinh th nh, mu trng, tan trong nc.
Cng thc ho hc : NH
4
Cl.
Khi lng phn t( theo khi lng nguyn t quc t nm 1969)- 53,49.
I. QUY NH CHUNG
1.1 Nc ct dng trong tiu chun ny ph hp vi TCVN 2117-77.
1.2 Tt c cc php th phi tin hnh song song trn hai mu cn.
1.3 Cc ng so mu phi c kch thc nh nhau, bng thu tinh khng mu, c cng tnh cht
quang hc.
1.4 Cc thuc th dng trong tiu chun ny phi l loi TKHH hoc TKPT.
1.5 Cht lng ca thuc th amoni clorua c nh gi trn c s phn tch cc mu trung bnh
ly c tng l hng.
1.6 L hng l lng sn phm c cng ch tiu cht lng c ng gi v giao nhn trong
cng mt lt.
1.7 Tu thuc vo cch bao gi sn phm, c th tin hnh ly mu theo bng 1.
1.8 Trn mi n vbao gi ly phn tch, tin hnh ly mu nhng v tr khc nhau ( t 3 v
tr tr ln) sao cho khi lng mu trung bnh khng c nh hn khi lng mu trung bnh khng
c nh hn 500 g.
Bng 1

S n v bao gi l hng S n v bao gi ly n v phn
tch

T 1 n 10
T 11 n 50
T 51 n 100
T 101 n 500
T 501 n 700
T 701 n 1000
Ln hn 1000

1
2
4
5
6
7
1%


2.YU CU K THUT
Thuc th amoni clorua phi ph hp vi yu cu k thut ghi trong bng 2.

Bng 2

Mc ( % )


TN CH TIU
Tinh khit
phn tch

Tinh khit

( TKPT) ( TK)

1. Hm lng amoni clorua ( NH
4
Cl) khng c
nh hn

2. Hm lng cn khng tan trong nc, khng
c ln hn


Hm lng cn sau khi nung ( tnh ra SO
4
), khng
c ln hn



5. Hm lng photphat ( PO
4
) khng c ln hn

6. Hm lng st ( Fe ), khng c ln hn

7. Hm lng canxi (Ca), khng c ln hn

8. Hm lng magie ( Mg ), khng c ln hn

9. Hm lng asen (As), khng c ln hn

10. Hm lng kim loi ( tnh ra Pb), khng c
ln hn

11. pH ca dung dch 5 %

0,001

0,0005

0,0015

0,0015

0,00005

0,0005

4,5- 6


0,002

0,0010

0,0050

0,0050

0,00010

0,0010

khng quy nh


3. PHNG PHP TH
3.1 Xc nh hm lng amoni clorua
3.1.1. Thuc th v dung dch
Kali cromat, dung dch 5 %;
Bc nitrat, dung dch 0,1 N.
3.1.2 Tin hnh th
Cn khong 1 g mu chnh xc n 0,0002 g, ho tan bng nc ct ri chuyn dung dch vo
bnh nh mc c dung tch 250 ml, thm nc n vch mc, lc u, ly 25 ml dung dch trn,
dng nc pha long n 50 ml, thm 0,25 ml dung dch kali cromat v chun bng dung dch bc
nitrat n khi mu dung dch bt u chuyn t vng sang gch.
Hm lng amoni clorua ( X ) tnh bng phn trm theo cng thc:

a. 10 . 0,005349 . 100 a . 5,349
X = =
G G

trong :
G- lng mu cn tnh bng g;
a - s ml dung dch bc nitrat tiu tn trong php chun
0,005349- lng amno clorua tnh bng g, tng ng vi 1 ml dung dch bc nitrat.
3.2. Xc nh hm lng cn khng tan trong nc
Cn 50 g mu chnh xc n 0,01 g, cho vo cc c dung tch 500 ml, va un nng va ho tan
bng 200 ml nc si v lc qua cc lc xp loi TPC 4 hoc G
4
( cc c sy kh n khi
lng khng i v cn chnh xc n 0,0002 g). Ra cn trn cc bng 100 ml nc nng chia lm
nhiu ln v sy trong t sy nhit 105 4 110
0
C n khi lng khng i.
Mu t tiu chun nu khi lng cn kh khng ln hn:
2,5 mg i vi loi TKPT;
5,0 mg i vi loi TK.
3.3. Xc nh hm lng cn sau khi nung ( dng sunfat)
Cn 20 g mu chnh xc n 0,01 g, cho vo cc platin hay chn s ( c nung n khi
lng khng i v cn chnh xc n 0,0002 g) v un nng trn bp in. Sau khi mt phn mu
bay hi, cho vo phn cn li 1 ml axit sunfuric ( d=1,84) v un trn bp in n khi bay ht hi
axit sunfuric. Phn mu cn li nung trong l nung nhit 600 4 700
0
C n khi lng khng i.
Mu t tiu chun nu khi lng sau khi nung khng ln hn:
4 mg i vi loi TKPT;
12 mg i vi lai TK
Cn sau khi nung gi li xc nh canxi mc 3.7 v magie mc 3.8.
3.4. Xc nh hm lng sunfat
3.4.1 Thuc th v dung dch
Axit clohidric theo TCVN 1298-78, dung dch 35-38 %;
Bari clorua, dung dch mi chun b, cch chun b nh sau:
Ho tan 20 g bari clorua trong 90 ml nc, nu dung dch c th lc qua giy lc khng tn, thm
2,5 ml axit clohidric v un dung dch n si. Thm vo dung dch cn nng( va thm va khuy
u) 0,25 g h tinh bt c nghin cn thn vi 7,5 ml nc.
Dung dch cha sunfat, chun b theo TCVN 1056-71, pha long n 0,01 mg/ml.
3.4.2. Tin hnh th
Cn 4 g mu chnh xc n 0,01 g, ho tan bng 100 ml nc v lc qua giy lc. Ly 25 ml
dung dch sau khi lc ( ng vi 1 g mu ) i vi loi TKPT hay 6,25 ml ( ng vi 0,25 g mu) i
vi loi TK cho vo ng so mu nt mi, thm 1 ml axit clohidric, 3 ml dung dch bari clorua, lc
u.
Mu t tiu chun nu sau ba mi pht dung dch th khng c hn dung dch so snh. Dung
dch so snh c chun b ng thi vi dung dch th v cha trong cng th tch:
0,05 mg SO
4
i vi loi TKPT
0,05 mg SO
4
i vi loi TK,
v 3 ml dung dch bari clorua, 1 ml axit clohidric.
3.5. Xc nh hm lng photphat
3.5.1. Thuc th v dung dch
Thuc th pht pht, chun b theo TCVN 1055-71;
Dung dch cha pht pht, chun b theo TCVN 1056-71; pha long n 0,01 mg/ml.
3.5.2. Tin hnh th
Cn 5 g mu chnh xc n 0,01 g, cho vo ng so mu nt mi, thm 10 ml nc, 10 ml thuc
th photphat, lc u n khi tan ht mu.
Mu t tiu chun nu sau mi pht, mu ca dung dch th khng m hn mu ca dung
dch so snh. Dung dch so snh c chun b ng thi vi dung dch th v cha trong cng th
tch:
0,05 mg PO
4
i vi loi TKPT;
0,10 mg PO
4
i vi loi TK,
v 10 ml dung dch thuc th pht pht.
3.6. Xc nh hm lng st
3.6.1. Thuc th v dung dch
Axit nitric, dung dch 25 %;
Amoni sunfoxianua, dung dch 5 %;
Dung dch cha st, chun b theo TCVN 1056-71, pha long n 0,01 mg/ml.
3.6.2. Tin hnh th
Cn 2 g mu chnh xc n 0,01g, ho tan bng 13 ml nc ri chuyn dung dch vo ng so mu
nt mi, thm 1 ml axit nitric, 2 ml amoni sunfoxianua, lc u.
Mu t tiu chun nu sau nm pht mu ca dung dch th khng m hn mu ca dung dch
so snh. Dung dch so snh c chun b ng thi vi dung dch th v cha trong cng th tch:
0,01 mg Fe i vi loi TKPT;
0,02 mg Fe i vi lai TK,
v 1 ml dung dch axit nitric, 2 ml dung dch amoni sunfoxianua
3.7. Xc nh hm lng canxi
3.7.1. Thuc th v dung dch
Axit clohidric theo TCVN 2298-78, dung dch 25 %;
Natri hidroxit, dung dch 1 N;
Murexit, dung dch 0,05 %, dng c trong hai ngy;
Giy o pH ;
Dung dch cha canxi, chun b theo TCVN 1056-71, pha long n 0,01 mg/ml.
3.7.2. Tin hnh th
Thm 1 ml axit clohidric v 10 ml nc vo cn sau khi nung mc 3.3, va ho tan va un trn
bp in. Chuyn dung dch vo bnh nh mc 200 ml, thm nc n vch mc, lc u ( dung dch
A). Gi dung dch xc nh magi mc 3.8.
Ly 5 ml dung dch A( ng vi 0,5 g mu) cho vo ng so mu nt mi, trung ho bng dung dch
natri hidroxxit( theo giy o pH), lc u, thm 1 ml natri hidroxit, 1 ml murexit, lc u.
Mu t tiu chun nu sau mt n hai pht mu hng tm ca dung dch th khng m hn
mu hng tm ca dung dch so snh. Dung dch so snh c chun b ng thi vi dung dch th
v cha trong cng th tch:
0,01 mg Fe i vi loi TKPT
0,02 mg Fe i vi loi TK,
v 1 ml dung dch axit nitric, 2 ml dung dch amoni sunfoxianua
3.7. Xc nh hm lng canxi
3.7.1.Thuc th v dung dch
Axit clohidric theo TCVN 2298-78, dung dch 25 %;
Natri hidroxit, dung dch 1 N;
Murexit, dung dch cha canxi, chun b theo TCVN 1056-71, pha long n 0,01 mg/ml.
3.7.2. Tin hnh th
Thm 1 ml axit clohidric v 10 ml nc vo cn sau khi nung mc 3.3, va ho tan va un trn
bp in. Chuyn dung dch vo bnh nh mc, lc u( dung dch A). G dung dch xc nh
xc nh magi mc 3.8.
Ly 5 ml dung dch A( ng vi 0,5 g mu) cho vo ng so mu nt mi, trung ho bng dung dch
natri hidroxit, 1 ml murexit, lc u.
Mu t tiu chun nu sau mt n hai pht mu hng tm ca dung dch th khng m hn
mu hng tm ca dung dch so snh. Dung dch so snh c chun b ng thi vi dung dch th
v cha trong cng th tch:
0,0075 mg Ca i vi loi TKPT;
0,0250 mg Ca i vi loi TK,
v 1 ml dung dch natri hidroxit, 1ml dung dch murexit
3.8. Xc nh hm lng magi
3.8.1. Thuc th v dung dch
Natri hidroxit, dung dch 10 %;
Titan vng, dung dch 0,05 %, mi chun b ;
Dung dch cha magie, theo TCVN 1056-71, pha long n 0,01 mg/ml.
3.8.2. Tin hnh th
Ly 5 ml dung dch A( chun b mc 3.7, ng vi 0,5 g mu) cho vo ng so mu nt mi c
dung tch 25 ml thm 2 ml dung dch natri hidroxit, 0,2 ml dung dch titan vng, thm nc n vch
mc, lc u.
Mu t tiu chun nu sau mi pht vng hng ca dung dch th khng m hn mu vng
hng ca dung dch so snh. Dung dch so snh c chun b ng thi vi dung dch th v cha
trong cng th tch:
0,0075 mg Mg i vi loi TKPT;
0,0250 mg Mg i vi loi TK,
v 2 ml dung dch natri hidroxit, 0,2 ml dung dch titan vng.
3.9. Xc nh hm lng asen
3.9.1. Thuc th v dung dch
Giy tm thu ngn bromua chun b theo TCVN 1055-71;
Axit sunfuric, d=1,84, pha long 1:4;
Giy tm ch axetat, chun b theo TCVN 1055-71;
Thic diclorua, dung dch 10 %, chun b theo TCVN 1055-71;
Km kim loi dng ht, hm lng asen khng ln hn 1,5 . 10
5
%.
Dung dch cha asen, chun b theo TCVN 1056-71, pha long n 0,001 mg/ml.
Dng c xc nh asen theo hnh v
3.9.2. Tin hnh th
Cn 10 g mu chnh xc n 0,01 g, cho vo bnh 1 ca dng c xc nh asen, ho tan bng
30 ml nc, thm 20 ml dung dch axit sunfuric, 0,5 ml thic diclorua, lc, cho nhanh 10 g km v lp
tip phn trn ca dng c xc nh asen vo bnh phn ng, lc u.
Mu t tiu chun, nu sau mt gi mu ca giy tm thu ngn bromua bnh th khng m
hn mu ca giy tm thu ngn bromua bnh so snh. Bnh so snh c chun b ng thi vi
bnh th v cha trong cng th tch:
0,005 mg As i vi TKPT;
0,010 mg As i vi loi TK,
v 20 ml dung dch axit sunfuric, 0,5 ml dung dch thic diclorua, 10 g km ht.
3.10. Xc nh hm lng kim loi (Pb)
3.10.1. Thuc th v dung dch
Kali-natri-tatrat, dung dch 20 %;
Natri hidroxit, dung dch 10 %;
Thioaxetamit, dung dch 2 %, lc qua giy lc khng tn, dng c trong ba ngy;
Dung dch cha ch theo TCVN 1056-71, pha long n 0,01 mg/ml.
3.10.2. Tin hnh th
Cn 5,0 g mu chnh xc n 0,01 g cho vo ng so mu nt mi, ho tan bng 15 ml nc ct,
thm 1 ml dung dch kal-natri-tatrat, 2 ml dung dch natri hidroxit, 1ml dung dch thioaxetamit, lc
u.
Mu t tiu chun nu sau 10 pht mu ca dung dch th khng m hn mu ca dung dch so
snh. Dung dch so snh c chun b ng thi vi dung dch th v cha trong cng th tch:
0,025 mg Pb i vi loi TKPT;
0,05 mg Pb i vi loi TK,
v 1 ml dung dch kali-natri-tatrat, 2 ml dung dch natri hidroxit, 1 ml dung dch thioaxetamit.
3.11. Xc nh pH ca dung dch 5 %
Cn 5 g mu chnh xc n 0,01 g, cho vo cc c dung tch 200 ml, ho tan bng 95 ml nc
khng cha cacbon dioxit v o pH trn my pH c in cc thu tinh.
4.BAO GI, BO QUN, NHN HIU
4.1. Bao gi v bo qun
4.1.1. Amoni clorua c ng trong nhng chai thu tinh nt mi hoc chai nha c hai ln c
khi lng khng b 0,5 4 1 kg. Nhng bao gi ny phi ng vo hm g hoc cactng v gn nhn
ph hp vi iu 4.2 ca tiu chun ny.
4.1.2. Amoni clorua cn c th ng vo nhng ti cht do c hai lp vi khi lng theo yu cu
khch hng. Nhng bao gi ny phi ng vo hm g hoc hp cactng, bn ngoi gn nhn ph
hp vi iu 4.2 ca tiu chun ny.
4.1.3 Nhng bao gi ny phi phi kh, sch, khng gy nh hng n cht lng sn phm v
ni kh, mt.
4.2. Nhn hiu
Trn mi bao gi ng amoni clorua phi gn nhn ghi r:
Tn B, Tng cc;
Tn x nghip sn xut;
Tn x nghip sn xut;
Tn thuc th v cng thc ho hc;
Mc tinh khit v cc ch tiu cht lng;
K hiu v s tiu chun( TCVN 2842-79)
Khi lng khng b