TIU CHUN QUC GIA

TCVN 9178 : 2012

THY TNH MU - PHNG PHP XC NH HM LNG ST OXT
Colour glass - Test method for determination of ferric oxide
Li ni u
TCVN 9178:2012 duoc chuyn di t TCXD 137:1985 theo quy djnh tai khon 1 iu 69 ca
Lut Tiu chun v Quy chun k thut v dim a khon 1 iu 7 Nghj djnh s 127/2007/N-CP
ngy 1/8/2007 ca Chnh ph quy djnh chi tit ban hnh mt s diu ca Lut Tiu chun v Quy
chun k thut.
TCNV 9178:2012 do Vin Vt liu xy dung - B Xy dung bin soan, B Xy dung d nghj,
Tng cuc Tiu chun o lung Cht luong thm djnh, B Khoa hoc v Cng ngh cng b.
THY TINH MU - PHUONG PHP XC [NH HM LUQNG SAT OXIT
Colour glass - Test method for determination of ferric oxide
1. Pham vi p dng
Tiu chun ny quy djnh phuong php phn tch ha hoc xc djnh hm luong st () oxit trong
thy tinh mu.
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 duoc 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 di (nu c).
TCVN 4851-1989 (SO 3696:1987), Nc dng phn tch trong phng th nghim - !"u c#u
$% thu&t '( ph)ng ph*p th+,
TCXD 136:1985 Th-. tinh - C*t s/n xu0t th-. tinh - 1h)ng ph*p chu2n 34 m5u trong phng
th nghim phn tch h6a h7c - 8u. 4nh chung,
3. Quy [nh chung
Theo TCXD 136:1985.
4. Ha cht, thuc th
4.1. KaIi pyrosunfat (K2S2O7), khan.
4.2. Amoni cIorua (NH4Cl), tinh th.
4.3. Axit fIohydric (HF) dm dc, d = 1,12.
4.4. Axit cIodydric (HCl) dm dc, d = 1,19.
4.5. Axit sunfuric (H2SO4) dm dc, d = 1,84.
4.6. Axit nitric (HNO3) dm dc, d = 1,52.
4.7. Axit cIohydric (HCI), pha long (1+1).
4.8. Axit sunfuric (H2SO4), pha long (1+1).
4.9. Axit nitric (HNO3), pha long (1+1).
4.10. Axit tactric (H2C4H4O6), dung djch 20 %, bo qun trong chai thy tinh ti mu.
*
Cc tiu chun TCXD, TCN s duoc chuyn di thnh TCVN hoc QCVN
4.11. Amoni hydroxit (NH4OH) dm dc, d = 0,88.
4.12. Amoni hydroxit (NH4OH), pha long (1+1).
4.13. HydroxyIamin cIohydrat (NH2OH.HCI), dung djch 10 %.
4.14. Para nitrophenoI (C6H5NO3), dung djch 0,5 % pha trong hn hop (ruou etylic:nuc) (1+1).
4.15. 1,1 phenantroIin (C12H8N2), dung djch 0,25 %.
4.16. Phn nhm amoni ((NH4)2SO4.12H2O), dung djch 5 %.
4.17. Dung d[ch tiu chun gc st (III) oxit (Fe2O3) 0,1 mg/mL:
Cn 0,1005 gam st () oxit (hoc luong cn tuong ng ca mt mui st ()) d sy 105
o
C
5
o
C vo cc thy tinh dung tch 250 mL, thm vo cc 10 mL axit clohydric dc (4.4), dun dn
tan trong. ngui chuyn dung djch vo bnh djnh mc dung tch 1 L, thm nuc dn vach djnh
mc, lc du.
* Dung d[ch tiu chun Im vic st (III) oxit (Fe2O3) 0,01 mg/mL:
Ly 50 mL dung djch tiu chun gc vo bnh djnh mc dung tch 500 mL thm nuc ti vach
mc, lc du.
* Xy dng th[ chun:
Ly 11 bnh djnh mc dung tch 100 mL, ln luot cho vo mi bnh mt th tch dung djch tiu
chun st () oxit lm vic (CFe2O3 = 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, pha long dn khong 50 mL, thm tip 5 mL dung
djch axit tactric 20% (4.10), 3 mL dung djch hydroxylamin clohydrat 10 % (4.13), 2 giot chi thj
para nitrophenol 0,5 % (4.14). Sau d va lc du bnh va nh tng giot dung djch amoni
hydroxit (1+1) (4.12) dn khi dung djch xut hin mu vng, dng dung djch axit clohydric (1+1)
(4.7) v dung djch amoni hydroxit (1+1) (4.12) diu chinh dung djch dn mt mu vng (hoc cn
thong vng). Sau 15 min thm tip 10 mL dung djch 1,1 phenantrolin 0,25 % (4.15), thm nuc
ti vach djnh mc, lc du.
o d hp thu quang ca dung djch mu buc sng t 500 nm dn 520 nm. Dung djch so
snh l dung djch mu trng (ly t th nghim trng).
T hm luong st () oxit c trong mi bnh v gi trj d hp thu quang tuong ng xy dung d
thj chun.
5. Thit b[, dng c
Thit bj, dung cu thng thung trong phng th nghim v:
5.1. Cn phn tch, c d chnh xc dn 0,0001 g.
5.2. L nung, c b phn diu chinh nhit d dn 950
o
C 50
o
C.
5.3. T sy, c b phn diu chinh nhit d dn 300
o
C 5
o
C.
5.4. My ct nuc.
5.5. T ht hoi c.
5.6. Chn bach kim, dung tch 30 mL hoc 50 mL.
5.7. Bp in, bp cch ct, kim sot duoc 400
o
C.
5.8. My o mu quang in hoc ph quang k UV-VIS, c kh nng do d hp thu quang
buc sng t 380 nm dn 850 nm.
5.9. Cc thy tinh ch[u nhit, dung tch 250 mL.
5.10. Pipet, dung tch 5 mL, 10 mL, 50 mL.
5.11. Bnh [nh mc, dung tch 100 mL, 500 mL.
5.12. Giy Ic, chy nhanh (dung knh l trung bnh khong 20 m).
5.13. Giy pH.
6. Chun b[ v phn gii mu th
6.1. Chun b[ mu th
Theo TCXD 136:1985.*
6.2. Phn gii mu th
Cn khong 2,0 g mu (6.1) chnh xc dn 0,0001 g vo chn bach kim, tm ut mu bng vi
giot nuc thm vo chn t 2 mL dn 3 mL axit nitric (1+1) (4.9) v t 8 mL dn 10 mL axit
lohydric 40 % (4.3), lm bay hoi cc cht trong chn trn bp dn kh, thm tip 5 mL axit
lohydric 40 % (4.3), cho bay hoi tip dn kh, lp lai qu trnh trn mt ln na. Thm tip 2 mL
dn 3 mL axit sunuric (1+1) (4.8), cho bay hoi trn bp din dn ngng bc khi trng. ngui,
thm vo chn t 4 g dn 5 g kali pyrosunat. Cho chn mu vo l nung nhit d khong 750
o
C 50
o
C trong thi gian 10 min, nung mu dn tan trong. Ha tan khi nung chy bng nuc
nng c khong 10 mL axit clohydric (1+1) (4.7), dun dn tan trong. Chuyn ton b dung djch
vo bnh djnh mc dung tch 250 mL d ngui, thm nuc dn vach djnh mc, lc du.
Dung djch thu duoc dng d xc djnh cc oxit Fe2O3, TiO2, CuO, CoO, NiO c trong mu (dung
djch ).
Luong cn mu th cn ly d phn tch do mu cho tng chi tiu phn tch theo Bng 1:
Bng 1: Lung cn mu th cn Iy phn tch
Hm Iung oxit trong mu
(%)
Lung mu cn Iy phn tch
(g)
T 0,005 dn 0,01
T 0,01 dn 0,05
T 0,05 dn 0,10
Trn 0,10
T 0,5 dn 0,25
T 0,2 dn 0,1
T 0,1 dn 0,05
dui 0,05
7. Phuong php th
7.1. Xc [nh hm Iung st (III) oxit (khi tap cht 5 0,5 %)
7.1.1. Nguyn tc
Kh ion Fe
3+
v ha trj 2 bng hydroxylamin, trong mi trung axit ion Fe
2+
tao vi thuc th 1,1
phenantrolin mt phc cht mu d, cung d mu t l vi nng d st c trong dung djch. o
d hp thu quang ca dung djch phc mu d buc sng t 500 nm dn 520 nm.
7.1.2. Cch tin hnh
Ly mt phn dung djch theo bng 1 (6.2) vo bnh djnh mc dung tch 100 mL, pha long dn
khong 50 mL, thm tip 5 mL dung djch axit tactric 20% (4.10), 3 mL dung djch hydroxylamin
clohydrat 10 % (4.13), 2 giot chi thj para nitrophenol 0,5 % (4.14). Sau d va lc du bnh va
nh tng giot dung djch amoni hydroxit (1+1) (4.12) dn khi dung djch xut hin mu vng, dng
dung djch axit clohydric (1+1) (4.7) v dung djch amoni hydroxit (1+1) (4.12) diu chinh dung djch
dn mt mu vng (hoc cn thong vng). Sau 15 min thm tip 10 mL dung djch 1,1
phenantrolin 0,25 % (4.15), thm nuc ti vach djnh mc, lc du.
o d hp thu quang ca dung djch mu buc sng t 500 nm dn 520 nm. Dung djch so
snh l dung djch mu trng (ly t th nghim trng). T gi trj d hp thu quang do duoc, dua
vo dung chun tm duoc hm luong st () oxit c trong bnh.
7.1.3. Tnh kt qu
Hm luong st () oxit (Fe2O3), tnh bng phn trm (%), theo cng thc:
%Fe2O3
100
2
1
=
m
m
Trong d:
m1: Luong st oxit tm duoc trn dung chun, tnh bng gam (g);
m2: Luong mu tuong ng vi th tch mu ly d phn tch, tnh bng gam (g).
Chnh lch cho php gia hai kt qu xc djnh song song khng ln hon 0,04 %.
7.2. Xc [nh hm Iung st (III) oxit (khi tap cht > 0,5 %)
7.2.1. Nguyn tc
Tch luong nh st khi mt luong ln Cu
2+
, Co
2+
bng cch kt ta vi l
3+
trong amoni
hydroxyt, ha tan kt ta. Kh ion Fe
3+
v ha trj 2 bng hydroxylamin, trong mi trung axit ion
Fe
2+
tao vi thuc th 1,1 phenantrolin mt phc cht mu d, cung d mu t l vi nng d
st c trong dung djch. o d hp thu quang ca dung djch phc mu d buc sng t 500
nm dn 520 nm.
7.2.2. Cch tin hnh
Ly mt phn dung djch ln gp hai ln quy djnh bng 1 (6.2) thm vo dung djch 3 g amoni
clorua (4.2), 2 mL dung djch phn nhm 5 % (4.16), thm nuc dn khong 50 mL. un nng
dung djch dn 70
o
C, nh t t dung djch amoni hydroxyt (1+1) (4.12), tip tuc dun dung djch dn
70
o
C d dng tu kt ta. Loc dung djch qua giy loc chy nhanh v ra t 2 ln dn ln bng
nuc dun si, b phn nuc loc ra.
Ha tan kt ta trn giy loc bng dung djch axit clohydric (1+1) (4.7) vo bnh djnh mc dung
tch 100 mL, dng nuc dun si ra giy loc dn ht axit (th bng giy do pH). Lm ngui phn
dung djch ra, thm nuc ti vach djnh mc, lc du (dung djch B).
Ly 5 mL dung djch B vo bnh djnh mc dung tch 100 mL, thm nuc dn khong 50 mL, thm
tip 5 mL dung djch axit tactric 20 % (4.10), 3 mL dung djch hydroxylamin clohydrat 10 % (4.13),
2 giot chi thj para nitrophenol 0,5 % (4.14). Sau d va lc du bnh va nh tng giot dung djch
amoni hydroxit (1+1) (4.12) dn khi dung djch xut hin mu vng, dng dung djch axit clohydric
(1+1) (4.7) v dung djch amoni hydroxit (1+1) (4.12) diu chinh dung djch dn mt mu vng
(hoc cn thong vng). Sau 15 min thm tip 10 mL dung djch 1,1 phenantrolin 0,25 % (4.15),
thm nuc ti vach djnh mc, lc du.
o d hp thu quang ca dung djch mu buc sng t 500 nm dn 520 nm. Dung djch so
sch l dung djch mu trng (ly t th nghim trng). T gi trj d hp thu quang do duoc, dua
vo dung chun tm duoc hm luong st () 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 d nhn bit mu th mt cch dy d;
- Vin dn tiu chun ny;
- Cc buc tin hnh th khc vi quy djnh ca tiu chun ny (ghi r ti liu vin dn);
- Cc kt qu th;
- Cc tnh hung c nh hung dn kt qu th;
- Ngy, thng, nm tin hnh th nghim.
MUC LUC
Li ni du
1. Pham vi p dung
2. Ti liu vin dn
3. Quy djnh chung
4. Ha cht, thuc th
5. Thit bj, dung cu
6. Chun bj v phn gii mu th
6.1. Chun bj mu th
6.2. Phn gii mu th
7. Phuong php th
7.1. Xc djnh hm luong st () oxit (khi tap cht 0,5 %)
7.1.1. Nguyn tc
7.1.2. Cch tin hnh
7.1.3. Tnh kt qu
7.2. Xc djnh hm luong st () oxit (khi tap cht 0,5 %)
7.2.1. Nguyn tc
7.2.2. Cch tin hnh
7.2.3. Tnh kt qu
8. Bo co th nghim