TIU CHUN QUC GIA

TCVN 9182 : 2012

THY TNH MU - PHNG PHP PHN TCH HA HC XC NH HM LNG NKEN
OXT
Colour glass - Test method for determination of nickel oxide
Li ni u
TCVN 9182 : 2012 uoc chuyn i t TCXD 141:1985 theo quy jnh tai khon 1 iu 69 ca
Lut Tiu chun v Quy chun k thut v im a khon 1 iu 7 Nghj jnh s 127/2007/N-CP
ngy 1/8/2007 ca Chnh ph quy jnh chi tit ban hnh mt s iu ca Lut Tiu chun v Quy
chun k thut
TCVN 9182 : 2012 do Vin Vt liu xy dung - B Xy dung bin soan, B Xy dung nghj,
Tng cuc Tiu chun o lung Cht luong thm jnh, B Khoa hoc v Cng ngh cng b.
THY TINH MU - PHUONG PHP PHN TCH HA HQC XC [NH HM LUQNG NIKEN
OXIT
Colour glass - Test method for determination of nickel oxide
1. Pham vi p dng
Tiu chun ny quy jnh phuong php phn tch ha hoc xc jnh hm luong niken oxit trong
thy tinh mu v ct sn xut thy tinh.
2. Ti Iiu vin dn
*
Cc ti liu vin dn sau l cn thit khi p dung tiu chun ny. i vi cc ti liu vin dn ghi
nm cng b th p dung bn uoc nu. i vi cc ti liu vin dn khng ghi nm cng b th
p dung phin bn mi nht, bao gm cc bn sa i (nu c).
TCVN 4851-1989 (SO 3696:1987) Nc dng phn tch trong phng th nghi!m - "#u c$u k%
thu&t '( ph)ng ph*p th+,
TCVN 136:1985 Th-. tinh - C*t s/n xu0t th-. tinh - 1h)ng ph*p chu2n 34 m5u trong phng
th ngh!m phn tch h6a h7c '( c*c 8u. 4nh chung,
TC9N :;<= :>?@ Th-. tinh - C*t s/n xu0t th-. tinh - 1h)ng ph*p phn tch h6a h7c x*c 4nh
h(m lAng sBt oxit,
3. Quy [nh chung
Theo TCXD 136:1985.
4. Ha cht, thuc th
4.1. Axit cIohydric (HCI) m c, d = 1,19.
4.2. Axit sunfuric (H2SO4) m c, d = 1,84.
4.3. Axit cIohydric (HCI), dung djch khong 0,5 N.
4.4. Axit sunfuric (H2SO4), pha long (1+1).
4.5. Amoni hydroxyt (NH4OH) m c, d = 0,88.
4.6. Amoni hydroxyt (NH4OH), pha long (1+1).
4.7. EDTA (Na2H2C10H12O8N2.2H2O), dung djch 5 %.
*
Cc tiu chun TCXD, TCN s uoc chuyn i thnh TCVN hoc QCVN
4.8. Natri kaIi tactrat (hoc natri tactrat) (KNaC4H4O6.4H2O), dung djch 20 %.
4.9. Natri hydroxyt (NaOH), dung djch 5 %.
4.10. Natri thiosunfat (Na2S2O3), dung djch 10 %.
4.11. Amoni pesunfat ((NH4)2S2O8), dung djch 5%.
4.12. DimetyI gIyoxin (C4H8N2O2), dung djch 1 %, pha trong dung djch natri hydroxyt 5 %.
4.13. DimetyI gIyoxin (C4H8N2O2), dung djch 1 %, pha trong dung mi etanol.
4.14. CIorofom (CHCI3), d = 1,74 n 1,84.
4.15. Amoni hydroxyt (NH4OH), pha long (1+50).
4.16. Dung d[ch tiu chun gc niken (NiO) 0,2 mg/mL:
Cn 0,4280 gam niken sunfat nung t 400
o
C n 450
o
C vo cc thy tinh dung tch 250 mL,
thm vo cc 15 mL axit clohydric m c (4.1) un n tan trong. ngui chuyn dung djch
vo bnh jnh mc dung tch 1 L, thm nuc n vach jnh mc, lc u.
* Dung d[ch tiu chun Im vic niken oxit (NiO) 0,01 mg/mL:
Ly 50 mL dung djch tiu chun gc vo bnh jnh mc dung tch 1 L, thm tip 10 mL dung djch
axit clohydric (1+1) (4.4), thm nuc n vach jnh mc, lc u.
* Xy dng th[ chun:
Cch 1:
Ly 11 bnh jnh mc dung tch 100 mL, ln luot cho vo mi bnh mt th tch dung djch tiu
chun niken oxit lm vic (CNiO = 0,01 mg/mL) theo th thu sau: 0 mL; 1 mL; 2 mL; 4 mL; 6 mL; 8
mL; 10 mL; 12 mL; 16 mL; 20 mL; 25 mL, thm vo bnh 5 mL kali natri tactrat 20 % (4.8), dng
dung djch natri hydroxyt 5 % (4.9) trung ha ht axit (theo giy o pH) v cho du thm 10 mL
na. Thm tip vo bnh 10 mL amoni pesunfat 5 % (4.11), 15 mL dung djch thuc th dimetyl
glyoxin 1 % (4.12), 10 ml natri hydroxyt 5 % (4.9). Sau mi ln thm thuc th phi lc u dung
djch. Sau 30 min thm vo bnh 3 mL dung djch EDTA 5 % (4.7), dng dung djch natri hydroxyt 5
% (4.9) jnh mc, lc u.
o hp thu quang ca dung djch mu buc sng = 440 nm. Dung djch so snh l dung
djch mu trng (ly t th nghim trng).
T luong niken oxit c trong mi bnh v gi trj hp thu quang tuong ng xy dung thj
chun.
Cch 2:
Ly 11 cc thy tinh dung tch 100 mL, ln luot cho vo mi cc mt th tch dung djch tiu
chun niken oxit lm vic (CNiO = 0,01 mg/mL) theo th tu sau: 0 mL; 1 mL; 2 mL; 4 mL; 6 mL; 8
mL; 10 mL; 12 mL; 16 mL; 20 mL; 25 mL, thm t 7 mL n 8 mL dung djch kali natri tactrat 20 %
(4.8) nh giot dung djch amoni hydroxyt (1+1) (4.6) vo cc pH at t 8,5 n 9,0, thm tip 5
mL dung djch dimetyl glyoxin 1 % (pha trong dung mi etanol) (4.13). Chuyn dung djch vo
phu chit, thm vo phu 10 mL dung mi clorofom lc manh t 1 min n 2 min, yn cho
dung djch phn lp. Tch lp clorofom vo mt phu chit khc, tin hnh lp lai hai ln na,
mi ln bng 5 mL dung mi clorofom. Gp chung cc phn chit vo mt phu chit khc.
a phn dung mi trong phu chit hai ln, mi ln bng 25 mL dung djch amoni hydroxyt
(1+50) (4.15).
Gii chit niken khi dung mi hu co bng cch lc manh phn dung mi hu co vi 10 mL
dung djch axit clohydric 0,5 N (4.3) t 1 min n 2 min dung djch phn lp, tch phn dung
djch nuc vo bnh jnh mc 100 mL. Tin hnh gii chit 2 ln na mi ln bng 10 mL dung
djch axit clohydric 0,5 N, gp chung phn dung djch gii chit vo bnh jnh mc dung tch 100
mL.
Tin hnh tao phc mu gia niken vi dimetyl glyoxin trong mi trung kim c mt cht oxy
ha v o hp thu quang ca dung djch mu nhu cch 1 (4.16).
T luong niken oxit c trong mi bnh v gi trj hp thu quang tuong ng xy dung thj
chun.
5. Thit b[, dng c
Thit bj, dung cu thng thung trong phng th nghim v:
5.1. Cn phn tch, c chnh xc n 0,0001 g.
5.2. L nung, at nhit 950
o
C 50
o
C c b phn iu chnh nhit .
5.3. T sy, at nhit 300
o
C 5
o
C c b phn iu chnh nhit .
5.4. My ct nuc.
5.5. T ht hoi c.
5.6. My o mu quang in hoc ph quang k UV-VIS, c kh nng o hp thu quang
buc sng t 380 nm n 850 nm.
5.7. Cc thy tinh ch[u nhit, dung tch 100 mL, 250 mL.
5.8. Bnh [nh mc, dung tch 100 mL, 1000 mL.
5.9. Pipet, dung tch 5 mL, 10 mL, 50 mL.
5.10. Giy o pH.
6. Chun b[ v phn gii mu th
Mu th uoc chun bj v phn gii theo TCXD 137-1985 (), thu uoc dung djch A dng xc
jnh hm luong niken oxit.
7. Phuong php th
7.1. Xc [nh hm Iung niken oxit (NiO) bng phuong php o mu trong mi trung
nuc (Khi tap cht 5 0,2 %)
7.1.1. Nguyn tc
Trong mi trung kim c mt cht oxy ha Ni
2+
tao vi thuc th dimetyl glyoxin mt phc cht
mu , cung mu t l vi nng niken c trong dung djch. o mt quang ca dung
djch phc mu buc sng = 440 nm.
7.1.2. Cch tin hnh
7.1.2.1. Khi mu phn tch c hm Iung CuO 5 0,2 %
Ty theo hm luong ng oxit c trong mu, ly mt phn dung djch A (iu 6) vo bnh jnh
mc dung tch 100 mL, thm vo bnh 5 mL kali natri tactrat 20 % (4.6) v dung djch natri
hydroxyt 5 % (4.7) trung ha ht axit (th bng giy o pH) cho du 10 mL na. Thm tip vo
bnh 10 mL amoni pesunfat 5 % (4.8), 15 mL dung djch thuc th dimetyl glyoxin 1 % (4.9) vo
10 mL natri hydroxyt 5 % (4.7). Sau mi ln thm thuc th phi lc u dung djch. Sau 30 min
thm vo bnh 3 mL dung djch EDTA 5 % (4.5), dng dung djch natri hydroxyt 5 % (4.9) jnh
mc, lc u.
o hp thu quang ca dung djch mu buc sng = 440 nm. Dung djch so snh l dung
djch mu trng (ly t th nghim trng).
T gi trj hp thu quang o uoc, dua vo thj chun tm uoc hm luong niken oxit c
trong bnh.
7.1.2.2. Khi mu phn tch c hm Iung CuO > 0,2 %
Ly mt phn dung djch A (iu 6) (th tch ln gp 4 ln so vi th tch cn ly trong trung
hop mu c hm luong CuO 0,2 % (7.1.2.1)) vo cc thy tinh dung tch 100 mL, thm 2 mL
dung djch axit sunfuric (1+1) (4.4), thm nuc n khong 40 mL, thm tip 50 mL dung djch
natri thiosunfat 10 % (4.10) khuy u, un nng dung djch n khong 80
o
C trong thi gian 3
min kt ta hon ton ng sunfat. ngui, chuyn dung djch vo bnh jnh mc dung tch
100 mL, thm nuc n vach jnh mc, lc u. Loc dung djch qua giy loc kh, phu kh vo
bnh nn kh.
Ly 25 mL dung djch trong bnh nn cho vo bnh jnh mc dung tch 100 mL, tin hnh ln mu
v o hp thu quang ca dung djch mu nhu muc 7.1.2.1.
T gi trj hp thu quang o uoc, dua vo thj chun tm uoc hm luong niken oxit c
trong bnh.
7.1.3. Tnh kt qu
Hm luong niken oxit (NiO), tnh bng phn trm (%), theo cng thc:
%NiO =
100
2
1

m
m
Trong :
m1: Luong niken oxit tm uoc trn ung chun, tnh bng gam (g);
m2: Luong mu tuong ng vi th tch mu ly phn tch, tnh bng gam (g).
Chnh lch gia hai kt qu xc jnh song song khng ln hon 0,04 %.
7.2. Xc [nh hm Iung niken oxit (NiO) bng phuong php chit, o mu (khi tap cht >
0,2 %)
7.2.1. Nguyn tc
Trong mi trung kim amoniac c mt dung mi hu co Ni
2+
uoc chit khi cc ion cn tr,
ra sn phm chit bng amoni hydroxyt long loai ng, gii chit bng dung djch axit
clohydric. Trong mi trung kim c mt cht oxy ha Ni
2+
tao vi thuc th dimetyl glyoxin mt
phc cht mu . o mt quang ca dung djch phc mu buc sng = 440 nm.
7.2.2. Cch tin hnh
Ty theo hm luong ng oxit c trong mu, ly mt phn dung djch A (iu 6) vo cc thy tinh
dung djch 100 mL, thm 8 mL dung djch kali natri tactrat 20 % (4.8), nh giot dung djch amoni
hydroxyt (1+1) (4.6) vo cc pH at t 8,5 n 9,0 (th bng giy o pH), thm tip 5 mL
dung djch dimetyl glyoxin 1 % (pha trong dung mi etanol) (4.13). Chuyn dung djch vo phu
chit, thm vo phu 10 mL dung mi clorofom lc manh t 1 min n 2 min, yn cho dung
djch phn lp. Tch lp clorofom vo mt phu chit khc, tin hnh lp lai hai ln chit na, mi
ln bng 5 mL dung mi clorofom, gp chung cc phn chit vo mt phu chit khc.
a phn dung mi trong phu chit hai ln, mi ln bng 25 mL dung djch amoni hydroxyt
(1+50) (4.15).
Gii chit niken khi dung mi hu co bng cch lc manh phn dung mi hu co vi 10 mL
dung djch axit clohydric 0,5 N (4.3) t 1 min n 2 min dung djch phn lp, tch phn dung
djch nuc vo bnh jnh mc dung tch 100 mL, tin hnh gii chit 2 ln na mi ln bng 10
mL dung djch axit clohydric 0,5 N, gp chung phn dung djch gii chit vo bnh jnh mc dung
tch 100 mL.
Tin hnh tao phc mu gia niken vi dimetyl glyoxin trong mi trung kim c mt cht oxy
ha v o hp thu quang ca dung djch mu nhu muc 7.1.2.1.
T gi trj hp thu quang o uoc, dua vo thj chun tm uoc hm luong niken oxit c
trong bnh.
7.2.3. Tnh kt qu
Theo muc 7.1.3.
8. Bo co th nghim
Bo co th nghim bao gm t nht cc thng tin sau:
- Cc thng tin cn thit nhn bit mu th mt cch y ;
- Vin dn tiu chun ny;
- Cc buc tin hnh th khc vi quy jnh ca tiu chun ny (ghi r ti liu vin dn);
- Cc kt qu th;
- Cc tnh hung c nh hung n kt qu th;
- Ngy, thng, nm tin hnh th nghim.
MUC LUC
Li ni u
1. Pham vi p dung
2. Ti liu vin dn
3. Quy jnh chung
4. Ha cht, thuc th
5. Thit bj, dung cu
6. Chun bj v phn gii mu th
7. Phuong php th
7.1. Xc jnh hm luong niken oxit (NiO) bng phuong php o mu trong mi trung nuc (khi
tap cht 0,2 %)
7.1.1. Nguyn tc
7.1.2. Cch tin hnh
7.1.3. Tnh kt qu
7.2. Xc jnh hm luong niken oxit (NiO) bng phuong php chit, o mu (khi tap cht 0,2 %)
7.2.1. Nguyn tc
7.2.2. Cch tin hnh
7.2.3. Tnh kt qu
8. Bo co th nghim