TIU CHUN VIT NAM

TCVN 6533 : 1999

VT LIU CHU LA ALUMOSILICAT - PHNG PHP PHN TCH HA HC
Alumosilicate refractories - Methods of chemical analysis
1. Phm vi p dng
Tiu chun ny quy nh phng php phn tch ha hc xc nh cc thnh phn ch yu
trong vt liu chu la thuc nhm alumosilicat theo TCVN 5441 - 1991. Tiu chun ny cng
c th p dng cho t st, cao lanh lm nguyn liu sn xut vt liu chu la.
2. Tiu chun trch dn
TCVN 4851 - 89 (ISO 3696:1987) Nc dng phn tch trong phng th nghim - Yu cu
k thut v phng php th.
TCVN 5441 - 1991 Vt liu v sn phm chu la - Phn loi.
3. Qui nh chung
3.1. Cn dng trong qu trnh phn tch c chnh xc n 0,000 1 gam.
3.2. Ha cht dng trong phn tch c tinh khit khng thp hn tinh khit phn tch
(TKPT).
Nc dng trong qu trnh phn tch theo TCVN 4851 - 89 (ISO 3696: 1987).
3.3. Ha cht pha long theo t l th tch c t trong ngoc n.
V d: HCl (1+2), ... l dung dch gm 1 th tch HCl m c vi 2 th tch nc ct.
3.4. Khi xc nh chun ca dung dch, h s nng (K), t s nng (k), th ly gi tr
trung bnh cng ca ba kt qu xc nh tin hnh song song cho tng php xc nh.
3.5. Cc ch tiu phn tch c tin hnh trn mu th chun b theo iu 6.
3.6. Vic xy dng li th chun (cho phng php so mu; quang ph hp th nguyn t,
...) tin hnh hai thng mt ln theo cch lm nu trong tiu chun ny.
3.7. Mi ch tiu phn tch c tin hnh song song trn hai lng cn mu th, mt th
nghim trng (bao gm cc lng thuc th nh nu trong tiu chun, nhng khng c
mu th) hiu chnh kt qu.
3.8. Chnh lch gia hai kt qu phn tch song song khng c ln hn gii hn cho php
(c qui nh ring cho mi php th). Nu ln hn phi tin hnh phn tch li.
3.9. Kt qu cui cng l trung bnh cng ca hai kt qu phn tch tin hnh song song.
4. Ha cht, thuc th
4.1. Ha cht rn, thuc th
4.1.1. Natri cacbonat (Na2CO3), khan.
4.1.2. Kali cacbonat (K2CO3), khan.
4.1.3. Natri tetraborat (Na2B4O7), khan.
4.1.4. Kali pyrosunphat (K2S2O7) hoc kali hydrosunphat (KHSO4).
4.1.5. Canxi cacbonat (CaCO3), hm lng khng nh hn 99,5%.
4.1.6. Amoni clorua (NH4Cl), tinh th.
4.1.7. Hn hp nung chy 1: trn u natri cacbonat (4.1.1) vi kali cacbonat (4.1.2) theo t
l khi lng 1:1, bo qun trong bnh nha kn.
4.1.8. Hn hp nung chy 2: trn u ba phn khi lng natri cacbonat (4.1.1) vi mt phn
khi lng natri tetraborat (4.1.3), bo qun trong bnh nha kn.
4.1.9. Ch th mu fluorexon 1%: dng chy ci s nghin mn 0,1 g ch th mu fluorexon vi
10 gam kali clorua (KCl), bo qun trong l thy tinh mu.
4.2. Ha cht lng, thuc th
4.2.1. Axit clohydric (HCl) m c, d = 1,19.
4.2.2. Dung dch axit clohydric, nng 1N:
Ha tan 80 ml HCl m c (4.2.1) vo nc, pha long bng nc thnh 1 000 ml v trn
u.
4.2.3. Axit clohydric, pha long (1 + 1).
4.2.4. Axit sunfuric (H2SO4) m c, d = 1,84.
4.2.5. Axit sunfuric pha long (1 +1): t t axit vo nc ct.
4.2.6. Axit nitric (HNO3) m c, d = 1,40 - 1,42
4.2.7. Axit tartric (H2C4H4O6) hoc mui kali (hoc amoni) tartrat: dung dch 10%.
4.2.8. Axit nitric pha long (1 + 1).
4.2.9. Axit flohydric (HF) m c, d = 1,12; (38 + 40%).
4.2.10. Axit axetic (CH3COOH) m c, d = 1,05 - 1,06.
4.2.11. Amoni hydroxit (NH4OH) m c, d = 0,88 (25%).
4.2.12. Amoni hydroxit pha long (1 + 1).
4.2.13. Dung dch natri hydroxit (NaOH), 30%:
Ha tan 300 g NaOH rn trong nc, ngui, pha long thnh 1 lt, bo qun trong bnh
nha polyetylen.
4.2.14. Dung dch natri hydroxit, 10 %.
4.2.15. Dung dch kali hydroxit (KOH), 25 %.
4.2.16. Dung dch che du kali xianua (KCN) 5%, bo qun trong bnh nha polyetylen.
4.2.17. Dung dch axit sunfosalixylic 10% v 20%.
4.2.18. Metanol (CH3OH), d = 0,792 hoc etanol (C2H5OH), d = 0,789.
4.2.19. Dung dch bc nitrat (AgNO3) 0,5%:
Ha tan 2,5 g bc nitrat vo 500 ml nc c sn 5 ml axit nitric m c (4.2.7) - Bo
qun trong bnh thy tinh mu ti.
4.2.20. Dung dch phenolphtalein 0,1% - trong ru etylic.
4.2.21. Dung dch kh:
Ha tan 25 g axit tartric (H2C4H4O6) hoc 5 g axit xitric (H3C6H5O7) v 1 g axit ascorbic vo
100 nc, bo qun trong chai thy tinh mu. Pha dng trong 2 - 3 ngy.
4.2.22. Dung dch amoni molipdat 5%:
Ha tan 25 g (NH4)6Mo7O24.4H2O vo 200 ml nc un m cho tan, (nu c th lc) pha
long thnh 500 ml. Bo qun trong bnh nha polyetylen, sau 4 tun pha dung dch mi.
4.2.23. Dung dch ng sunfat 5%:
Ha tan 5 g CuSO4.5H2O trong 100 ml nc c sn 1 ml axit sunfuric (1+1).
4.2.24. Dung dch axit ascorbic (C6H8O5) 5%. Pha dng trong vi ngy.
4.2.25. Dung dch diantipyrimetan 2%
Ha tan 20 g thuc th vo 300 ml nc c sn 25 ml axit sunfuric m c, thm tip 2 -
3 g axit ascorbic, pha long thnh 1 lt. Bo qun trong chai thy tinh mu.
4.2.26. Dung dch ch th xylenol da cam 0,1%;
Ha tan 0,1 g thuc th trong 100 ml nc.
4.2.27. Dung dch ch th eriocrom T en (ETOO) 0,1%:
Ha tan 0,1 g thuc th trong 100 ml ru etylic 70%, thm 2 - 3 g hydroxylamin hydrocloric
(NH2OH.HCl), Bo qun trong chai thy tinh mu.
4.2.28. Dung dch m pH 5,5:
Ha tan 100 ml amoni hydroxit m c vo 200 - 300 ml nc, thm tip vo 100 ml axit
acetic m c ri thm nc thnh 1 lt.
4.2.29. Dung dch m pH 10,5:
Ha tan 54 g amoni cloruarua vo 500 ml nc, thm tip 350 ml amoni hydroxit m c v
nc thnh 1 lt.
4.2.30. Dung dch tiu chun gc - silic dioxit (SiO2 = 0,4 mg/ml):
Nung chy 0,2 g silic dioxit tinh khit ( c nung 1 000C) trong chn bch kim vi 3 - 4
g hn hp nung chy 1 trong l, nhit 1 000C 50 C trong thi gian 30 - 40 pht.
Chuyn khi nung chy vo cc c sn 200 ml nc v 10 g NaOH, un ti tan trong.
Chuyn dung dch vo bnh nh mc 500 ml. thm nc ti vch mc, lc u.
Bo qun dung dch trong bnh nha polyetylen.
- Dung dch tiu chun lm vic (SiO2 = 0,04 mg/ml):
Ly 25 ml dung dch tiu chun gc vo bnh nh mc 250 ml, thm nc ti vch mc, lc
u. Dung dch pha dng trong ngy.
4.2.31. Dung dch tiu chun gc - st (III) oxit (Fe2O3 = 0,25 mg/ml):
Ha tan 0,25 g st (III) oxit sy kh 100oC - 110oC vo cc c sn 50 ml axit clohydric
(1+1), un si nh ti tan trong.
Chuyn dung dch vo bnh nh mc 1 000 ml, thm nc ti vch mc, lc u.
- Dung dch tiu chun lm vic (Fe2O3 = 0,05 mg/ml)
Ly 50 ml dung dch tiu chun gc vo bnh nh mc 250 ml, thm nc ct ti vch mc,
lc u.
4.2.32. Dung dch tiu chun gc - titan dioxit (TiO2 = 0,1 mg/ml):
Cn 0,3005 g dikali hexafluorotitan (K2TiF8) sy kh vo chn bch kim, thm t 10 ml n
15 ml dung dch axit sunfuric (1+1) lm bay hi trn bp n kh, thm tip 5 ml axit na, lm
bay hi n kh v ngng bc khi trng. Chuyn cc cht trong chn bch kim vo cc thy
tinh bng dung dch axit sunfuric 5%, thm vo cc 5 ml axit sunfuric (1+1) v un ti si.
Chuyn dung dch vo bnh nh mc 1 000 ml, dng axit sunfuric 5% nh mc, lc u.
- Dung dch tiu chun lm vic (TiO2 = 0,04 mg/ml):
Ly 100 ml dung dch tiu chun gc vo bnh nh mc 250 ml, thm axit sunfuric 5% ti
vch mc, lc u.
4.2.33. Dung dch tiu chun gc - natri oxit (Na2O = 0,2 mg/ml):
Ha tan 0,377 2 g natri clorua (NaCl), sy kh 100oC - 110C vo nc, chuyn vo
bnh nh mc 1 000 ml, thm nc ti vch, lc u. Bo qun trong bnh bng polyetylen.
- Dung dch tiu chun lm vic (Na2O = 0,01 mg/ml):
Ly 25 ml dung dch tiu chun gc vo bnh nh mc 500 ml, thm nc ti vch mc, lc
u.
4.2.34. Dung dch tiu chun gc kali oxit (K2O = 0,2 mg/ml):
Ha tan 0,3166 g kali clorua (KCl) sy kh 100C -110C vo nc, chuyn vo bnh
nh mc 1 000 ml, thm nc ti vch mc, lc u. Bo qun trong bnh bng polyetylen.
- Dung dch tiu chun lm vic (K2O = 0,01 mg/ml):
Ly 25 ml dung dch tiu chun gc vo bnh nh mc 500 ml, thm nc ti vch mc, lc
u.
4.2.35. Dung dch canxi tiu chun 0,01 M:
Cn 1,0060 g canxi cacbonat (4.1.5) sy 130C trong 2 - 3 gi vo cc thy tinh, tm
t bng nc v thm vo cc 50 ml nc na. y cc bng mt knh ng h, thm t
t 10 ml axit clohydric (1+1), sau khi tan ht, un si nh dung dch 1 - 2 pht. ngui,
chuyn vo bnh nh mc 1 000 ml v thm nc n vch, lc u.
4.2.36. Dung dch tiu chun EDTA 0,01 M:
Ha tan 3,8 - 3,9 g mui dinatri etylendiamin tetraaxetic axit dihydrat (Na2H2C10H12O8N2.2H2O)
vo 200 - 300 ml nc, un m v khuy n tan trong. ngui, pha long thnh 1 lt,
khuy u. Bo qun trong bnh bng polyetylen.
- Xc nh h s nng (K1) ca dung dch EDTA 0,01 M pha c:
Ly 20 ml hoc 25 ml dung dch canxi 0,01 M (4.2.35) vo cc, thm khong 100 ml nc, 20
ml dung dch KOH 25%, 2 ml dung dch KCN 5% v mt t hn hp ch th fluorexon 1%
(4.1.9) - dung dch c mu xanh hunh quang.
t cc ln trn mt nn mu en, dng dung dch EDTA pha c (4.2.36), chun dung
dch khi mu i t xanh hunh quang sang hng; ghi th tch EDTA tiu th (V1).
Tnh h s nng K1 theo cng thc sau:
VCa
K1
V1
trong
VCa l th tch dung dch canxi 0,01 M (4.2.35), tnh bng mililt;
V1 l th tch dung dch EDTA (4.2.36) tiu th, tnh bng mililt.
Tin hnh song song mt th nghim trng, vi tt c cc thuc th (ngoi tr dung dch
canxi tiu chun) hiu chnh kt qu.
4.2.37. Dung dch tiu chun EDTA 0,025 M:
Ha tan 9,5 - 9,7 g mui dinatri etylendiamin tetra acetic axit dihydrat
(Na2H2C10H12O8N2.2H2O) vo 200 - 300 ml nc, un m v khuy n tan trong. ngui,
pha long thnh 1 lt, khuy u. Bo qun trong bnh bng polyetylen.
- Xc nh h s nng (K2) ca dung dch EDTA 0,025 M pha c:
Ly 50 ml dung dch canxi 0,01 M (4.2.35) vo cc, thm khong 100 ml nc, 20 ml dung
dch KOH 25%, 2ml dung dch KCN 5% v mt t hn hp ch th fluorexon 1% - dung dch c
mu xanh hunh quang.
t cc ln trn mt nn mu en, dng dung dch EDTA pha c (4.2.37), chun dung
dch n khi mu i t xanh hunh quang sang hng; ghi th tch EDTA tiu th (V1).
Tnh h s nng K2 theo cng thc sau:

0,4 VCa
K2
V1'
trong
0,4 l t s nng gia dung dch canxi (0,01 M) v dung dch EDTA 0,025 M;
VCa l th tch dung dch canxi 0,01 M (4.2.35), tnh bng mililt;
V1 l th tch dung dch EDTA (4.2.37) tiu th, tnh bng mililt.
Tin hnh song song mt th nghim trng, vi tt c cc thuc th (ngoi tr dung dch
canxi) hiu chnh kt qu.
4.2.38. Dng dch tiu chun km axetat 0,025 M:
Ha tan 5,65 - 5,75 g [Zn(CH3OOH)2].2H2O vo 200 ml nc c sn 2 ml axit acetic m
c, un n tan trong. Pha long bng nc thnh 1 lt, khuy u.
- Xc nh t s nng (k3) gia dung dch EDTA 0,025 M (4.2.37) v dung dch km acetat
0,025 M:
Ly 20 ml dung dch EDTA 0,025 M (4.2.37) vo cc, thm vo cc 100 ml nc v 20 ml
dung dch m pH 5,5, thm 2 - 3 git ch th xylenon da cam (4.2.26). Dng dung dch km
acetat pha c (4.2.38) chun dung dch trong cc n khi chuyn mu t vng sang
hng; ghi th tch dung dch km axetat tiu th (VZn).
Tnh t s nng k3 theo cng thc sau:
20
K3
VZn
trong
20 l th tch dung dch EDTA 0,025 M (4.2.37) ly chun , tnh bng mililt;
VZn l th tch dung dch km acetat (4.2.38) tiu th khi chun , tnh bng mililt.
5. Thit b dng c
5.1. Cn phn tch, c chnh xc n 0,000 1 g.
5.2. L nung c b phn t ng iu chnh nhit ; nhit nung t 1 000 C 50C.
5.3. Chy ci nghin mu bng m no.
5.4. Chn bch kim, dung tch 30 ml v 50 ml.
5.5. My so mu quang in hoc ph quang k UV - VIS, c kh nng o mt quang (
hp th bc sng t 380 - 850 nm.
5.6. My quang ph ngn la hoc my quang ph hp th nguyn t, c trang b thch hp
o kali v natri.
5.7. Giy lc nh lng khng tro cc loi:
- loi chy nhanh, ng knh l trung bnh khong 20 m;
- loi chy trung bnh, ng knh l trung bnh khong 7 m;
- loi chy chm, ng knh l trung bnh khong 2 m.
6. Chun b mu th
Mu th dng cho phn tch ha hc c ly theo cc quy nh v ly v chun b mu theo
cc tiu chun tng ng v nguyn vt liu v sn phm chu la.
Mu th a ti phng phn tch ha hc c khi lng khng t hn 300 g, kch thc ht
khng ln hn 5 mm.
Trn u mu th, dng phng php chia t ly khong 100 g, nghin nh n lt ht qua
sng 0,20 mm; dng phng php chia t ly khong 50 g, tip tc nghin nh n lt ht
qua sng 0,10 mm. Dng phng php chia t ly khong t 12 - 15 g lm mu phn tch
ha hc, phn cn li bo qun lm mu lu.
Khi gia cng mu th, nu s dng dng c bng thp, phi dng nam chm loi st ln
vo mu, sau mi nghin mn mu phn tch ha hc trn ci m no, n lt qua sng
0063.
Mu phn tch ha hc c sy nhit 105 C 5 C, n khi lng khng i.
7. Phng php th
Qu trnh phn tch ha hc c tin hnh theo s hnh 1.
7.1. Xc nh hm lng mt khi nung
7.1.1. Nguyn tc
Nung mu th nhit 1 000C 50C, t s gim khi lng tnh ra hm lng mt khi
nung trong mu th.
7.1.2. Cch tin hnh
Cn 1 g 0,05 g chnh xc n 0,0001g mu (chun b theo iu 6); chuyn vo chn s
nung nhit 1 000C 50C n khi lng khng i. Nung chn c mu nhit
trn khong 1 - 1,5 gi, ngui trong bnh ht m n nhit phng ri cn. Lp li qu
trnh nung nhit trn trong 15 pht, lm ngui v cn n khi c khi lng khng
i.
7.1.3. Tnh kt qu
Hm lng mt khi nung (MKN), tnh bng phn trm, theo cng thc:

m1 m2
MKN 100
m
trong
m1 l khi lng mu v chn trc khi nung, tnh bng gam;
m2 l khi lng mu v chn sau khi nung, tnh bng gam;
m l khi lng mu cn, tnh bng gam.
Chnh lch gia hai kt qu xc nh song song khng ln hn 0,10 %.
7.2. Phn gii mu th
Mu th c phn gii to thnh dung dch phn tch cc thnh phn trong mu, theo
mt trong cc phng php di y:
7.2.1. Phn gii mu bng hn hp kim cacbonat
Phng php ny p dng cho mu c hm lng Al2O3 khng ln hn 45% v mu nguyn
liu.
Cn 0,5000 g mu th (iu 6), chuyn vo chn bch kim c sn t 2 - 3 g hn hp nung
chy 1 (4.1.7), trn u, ph ln trn mt lp mng hn hp nung chy na (khong 2 mm).
Hnh 1 - S phn tch.
Nung mu trong l nhit khong 1 000oC trong thi gian t 45 - 60 pht n tan trong.
Ly chn ra khi l, ngui.
Chuyn ton b cc cht cha trong chn sang bt s c mu bng nc ct nng v axit
clohydric (1+1), trng ra sch chn bch kim.
y bt s bng mt knh ng h, thm t t 20 ml axit clohydric m c vo bt s. Sau
khi mu tan ht, ngng si bt, dng bnh tia nc nng trng ra thnh bt, mt knh; thm
vo bt s 1 ml axit sunfuric (1+1), khuy u.
7.2.2. Phn gii mu bng hn hp kim cacbonat v natri borat
Phng php ny p dng cho mu c hm lng Al2O3 ln hn 45% hoc mu khng tan
hon ton theo phng php qui nh trong iu 7.2.1.
Cn 0,5000 g mu th (iu 6), chuyn vo chn bch kim c sn t 2 - 3 g hn hp nung
chy 2 (4.1.8), trn u; ph ln trn mt lp mng hn hp nung chy na (khong 2 mm).
Nung mu trong l nhit khong 1000oC trong thi gian t 20 - 30 pht, n tan trong.
Ly chn khi l, khi hn hp cn chy lng, nghing thnh chn v xoay trn nh chn,
hn hp cn lng bm thnh mt lp mng trn thnh chn, ngui.
Cho chn vo bt s c sn 40 ml axit clohydric (1+1), t nghing chn bch kim
ngm mu trong axit 15 pht. un m dung dch trong bt s lm tan mu; sau khi mu
tan ht, dng nc nng axit HCl (1+1) ra sch chn bch kim. Thm vo bt s 15 ml axit
clohydric m c (4.2.1) v 1 ml axit sunfuric (1+1), khuy u.
7.2.3. Phn gii mu bng hn hp axit flohydric v axit sunfuric
Phng php phn gii ny s dng khi phn tch kim loi kim.
Cn 0,2500 g mu th (iu 6), chuyn vo chn bch kim, tm t bng vi git nc,
thm tip vo chn 0,5 ml axit sunfuric (1+1) v 15 ml axit flohydric (4.2.10), lm bay hi t
t trn bp in n kh.
Thm vo chn t 8 - 10 ml axit flohydric na v lm bay hi n kh kit, sau khi chn
ngng bc khi trng. Lm ngui chn, dng nc ct nng v axit clohydric (1+1) chuyn
cc cht cha trong chn bch kim vo cc thy tinh 150 ml. Thm vo cc 5 ml axit
clohydric (1+1) v un si nh t 5 - 10 pht.
7.3. Xc nh hm lng silic dioxit (SiO2)
7.3.1. Nguyn tc
C cn dung dch mu th tch silic dng khng tan trong axit v c; nung kt ta
nhit 1000 C 50 C, ri x l bng dch axit flohydric tch silic dng cht d bay
hi silic tetraflorua xc nh c lng silic dioxit ch yu c trong mu th.
Nu mu c nung chy bng hn hp nung chy 2, cn tin hnh loi ion bo bng
metanol (hoc etanol) dng metyl borac (hoc etyl borac), trc khi tin hnh c cn.
Lng silic cn li trong dung dch c xc nh theo phng php trc quang; cho hin
mu vi amoni molipdat c mt cht kh, to ra cht mu xanh silic molipdat, so mu bc
sng t 800 nm n 820 nm.
7.3.2. Cch tin hnh
7.3.2.1. Xc nh silic dioxit dng cht khng tan trong axit (phng php khi lng)
Lm bay hi dung dch (7.2.1) trong bt s trn bp cch thy hoc cch ct, n kh. i
vi mu phn gii bng hn hp nung chy 2 (7.2.2), thm vo bt s 20 ml metanol khuy
u ri t ln bp c, khi mu cn sn st, thm vo bt 5 ml axit clohydric m c v 20
ml metanol na, khuy u v c n kh.
Khi cc cht trong bt s gn kh kit, dng a thy tinh dm nt cc ht mui mi to ra.
Sau khi mu kh, tip tc c mu thm khong 1 -1,5 gi n kh kit.
Lm ngui bt s, thm vo 15 ml axit clohydric m c, yn 10 pht. Thm vo bt
s 60 ml nc un si, khuy cho tan mui.
Lc dung dch qua giy lc chy trung bnh, nc lc ra thu vo bnh nh mc 500 ml,
dng nc ct nng ra sch bt s v giy lc, n ht ion clo trong nc ra (th bng
dung dch AgNO3 0,5 %).
Cho giy lc c kt ta vo chn bch kim ri t chy giy lc trn bp in. a chn bch
kim vo l nung, tng nhit n 1000 C 50 oC, gi mu nhit ny khong t 1 - 1,5
gi. Lm ngui chn bch kim trong bnh ht m v cn. Lp li qu trnh nung nhit
trn khong 15 pht, lm ngui trong bnh ht m v cn n khi thu c khi lng khng
i (m1).
Tm t kt ta trong chn bng vi git nc, thm vo chn 5 git dung dch axit sunfuric
H2SO4 (1+1) v 10 ml axit flohydric 40 %, lm bay hi cht cha trong chn trn bp in n
kh. Thm tip vo chn t 3 - 4 ml axit flohydric, lm bay hi trn bp in n ngng bc
khi trng. Nung chn bch kim v cn nhit 1000 C 50 C trong 30 pht. Ly chn ra
ngui trong bnh ht m n nhit phng, cn n khi lng khng i (m2).
Tm t kt ta trong chn bch kim bng vi git nc, thm tip t 5 - 6 git axit sunfuric
(1+1) v 10 ml axit flohydric m c ri lm bay hi trn bp in n kh. Thm tip vo
chn 10 ml axit flohydric na, cho bay hi trn bp in n kh kit v ngng bc khi
trng.
Cho chn vo l, nung 1000C 50C trong t 20 - 30 pht, lm ngui trong bnh chng
m n nhit phng v cn. Lp li qu trnh nung 10 pht, lm ngui trong bnh chng
m v cn, n khi thu c khi lng khng i (m3).
Nung cn cn li trong chn bch kim vi t 2 - 3 g kali pyrosunfat (4.1.4) nhit 750C
50C n tan trong.
Lm ngui chn bch kim v ha tan khi nung chy trong cc thy tinh c 50 ml nc ct
v 5 ml axit clohydric (1+1), un ti tan trong; gp dung dch ny vo dung dch trong bnh
nh mc 500 ml, thm nc ct ti vch mc, lc u; thu c dung dch A. Dung dch
ny dng xc nh cc thnh phn silic dioxit cn li trong dung dch, st, nhm, titan,
canxi, magie trong mu.
7.3.2.2. Xc nh hm lng silic dioxit ha tan trong dung dch (theo phng php so mu)
Ly 2,5 ml dung dch A vo bnh nh mc 100 ml, thm nc n khong 50 ml v 10 ml
dung dch amoni molipdat 5% (4.2.22), lc u. Sau 20 pht thm vo bnh 15 ml axit
clohydric (1+1), lc u. Sau 10 pht na thm tip vo bnh 5 ml dung dch kh (4.2.21),
thm nc ti vch mc, lc u.
Sau khi thm dung dch kh 30 pht, o mt quang (hoc hp th) ca dung dch mu
bc sng t 800 - 820 nm; dung dch so snh l mu trng. T tr s mt quang o
c, da vo th chun tm ra lng silic dioxit c trong 25 ml dung dch A (m).
Xy dng th chun:
Ly 6 bnh nh mc 100 ml, cho vo tng bnh ln lt mt th tch dung dch tiu chun
lm vic silic dioxit (SiO2 = 0,04 mg/ml) theo th t sau: 0; 1; 2; 4; 6 v 7 ml. Thm nc ct
vo tng bnh n khong 50 ml. Nh mt git phenolphtalein 0,1% v dng axit clohydric
(1+1) nh git n mt mu hng, thm d 2 ml axit na. Thm tip vo bnh 10 ml amoni
molipdat 5% (4.2.22), lc u, tip tc lp li thao tc trn.
T hm lng SiO2 trong tng bnh v gi tr mt quang tng ng, xy dng th
chun.
7.3.3. Tnh kt qu
Hm lng silic dioxit (SiO2) tnh bng phn trm, theo cng thc:
m1 m2 20m3
SiO2 100
m
trong
m1 l khi lng chn bch kim v kt ta trc khi x l bng axit flohydric (7.3.2.1), tnh
bng gam;
m2 l khi lng chn bch kim v kt ta sau khi x l bng axit flohydric (7.3.2.1), tnh
bng gam;
m3 l khi lng silic dioxit cn li trong 25 ml dung dch A - tm c trn th chun
(7.3.2.2), tnh bng gam;
m l khi lng mu cn tnh bng gam.
Chnh lch cho php gia hai kt qu xc nh song song khng ln hn 0,40 %.
7.4. Xc nh hm lng st (III) oxit (Fe2O3)
7.4.1. Xc nh hm lng st (III) oxit theo phng php so mu
Phng php ny p dng khi hm lng Fe2O3 nh hn 2,0%
7.4.1.1. Nguyn tc
Trong mi trng kim amoniac, ion st (III) to vi thuc th axit sunfosalixylic mt phc
cht mu vng; cng mu t l vi nng st c trong dung dch. o mt quang
ca dung dch bc sng khong t 420 - 430 nm.
7.4.1.2. Cch tin hnh
Ly 25 ml dung dch A vo bnh nh mc 100 ml, thm nc n khong 50 ml, thm tip 5
ml dung dch amoni tartrat 10% (4.2.7) v 20 ml dung dch axit sunfosalixylic 20 % (4.2.17).
Va lc u bnh va nh git amoni hydroxit m c n khi dung dch xut hin mu
vng, cho d t 3 - 4 ml amoni hydroxit na, thm nc ti vch mc, lc u.
o mt quang ca dung dch mu bc sng t 420 - 430 nm, dung dch so snh l
dung dch mu trng. T tr s mt quang o c, da vo th chun tm ra lng st
oxit c trong 25 ml dung dch A (m)
Xy dng th chun:
Ly 6 bnh nh mc 100 ml, ln lt thm vo mi bnh mt th tch dung dch tiu chun
lm vic st oxit (Fe2O3 = 0,05 mg/ml) theo th t sau: 0, 1, 2, 4, 8 v 10 ml, thm nc ct
n khong 50 ml, thm tip 5 ml dung dch amoni tartrat 10%, tip tc thc hin thao tc
trn.
T hm lng st oxit trong mi bnh v tr s mt quang tng ng xy dng th
chun.
7.4.1.3. Tnh kt qu
Hm lng st (III) oxit (Fe2O3) tnh bng phn trm, theo cng thc:
m
Fe2O3 100
mx
trong
m l khi lng st oxit tm c t th chun, tnh bng gam;
mx l khi lng mu c trong 25 ml dung dch A ly em xc nh st, tnh bng gam.
Chnh lch cho php gia hai kt qu xc nh song song khng ln hn 0,10 %.
7.4.2. Xc nh hm lng st oxit theo phng php chun phc cht.
Phng php ny p dng khi hm lng Fe2O3 ln hn 1,5%.
7.4.2.1. Nguyn tc
Chun ion st (III) bng dung dch EDTA mi trng pH khong 1,5 vi ch th mu l
axit sunfosalisilic, kt thc chun khi dung dch mt mu tm .
7.4.2.2. Cch tin hnh
Ly 50 ml dung dch A vo cc thy tinh, thm vo 60 ml nc v t 2 - 3 ml dung dch
axit sunfosalixylic 10% (4.2.17); dng amoni hydroxit (1+1) iu chnh dung dch n chuyn
mu t sang .. Thm vo cc 10 ml dung dch axit clohydric 1 N (4.2.2), un nng dung
dch n khong 70C.
Chun t t dung dch khi cn nng bng EDTA 0,01 M n khi dung dch mt mu tm
, ghi th tch EDTA tiu th (V).
7.4.2.3. Tnh kt qu
Hm lng st (III) oxit (Fe2O3) tnh bng phn trm, theo cng thc:
0,0007985 K1 V
Fe2O3 100
mx
trong
0,0007985 l khi lng Fe2O3 tng ng vi 1 ml dung dch EDTA 0,01 M, tnh bng gam;
K1 l h s nng EDTA 0,01 M (4.2.36);
V l th tch dung dch EDTA 0,01 M tiu th khi chun , tnh bng mililt;
mx l khi lng mu c trong 50 ml dung dch A ly em xc nh st oxit, tnh bng gam.
Chnh lch cho php gia hai kt qu xc nh song song khng ln hn 0,20 %.
7.5. Xc nh hm lng nhm oxit (Al2O3)
7.5.1. Nguyn tc
Tch nhm khi cc thnh phn khc bng kim mnh. To phc gia nhm vi EDTA d
pH 5,5; chun lng d EDTA bng dung dch km acetat theo ch th xylenon da cam, t
tnh ra hm lng nhm oxit.
7.5.2. Cch tin hnh
Thm t t 100 ml dung dch A vo cc cha sn 30 ml dung dch natri hydroxit 30% v
1 g natri cacbanat (4.1.1), khuy u. un si dung dch 5 pht, lm ngui, chuyn vo bnh
nh mc 250 ml, thm nc ti vch mc, lc u. Lc dung dch qua giy lc chy nhanh
kh, phu kh, vo bnh nn kh; dung dch lc ny dng xc nh nhm.
Ly 100 ml dung dch lc vo cc, thm tip vo cc:
- 25 ml dung dch EDTA 0,025 M (4.2.37) khi hm lng Al2O3 45%;
- 40 ml dung dch EDTA 0,025 M (4.2.37) khi hm lng Al2O3 > 45%.
Thm tip vo cc 1 git ch th phenolphtalein 0,1%, dng axit clohydric (1+1) v natri
hydroxit 10% iu chnh dung dch n ht mu hng. Thm vo cc t 20 - 25 ml dung dch
m pH 5,5 v un si dung dch t 3 - 5 pht.
Ly cc khi bp un, ngui, thm vo cc vi git ch th xylenon da cam, chun dung
dch trong cc bng dung dch km acetat 0,025 M (4.2.38), n khi dung dch chuyn t mu
vng sang hng; ghi th tch dung dch km acetat tiu th (VZn).
7.5.3. Tnh kt qu
Hm lng oxit nhm (Al2O3) tnh bng phn trm, theo cng thc:

0,0012745 .K 2 . V k 3 .VZn
Al2O3 100
mx
trong
0,0012745 l s gam nhm oxit tng ng vi 1 ml EDTA 0,025 M;
K2 l h s nng dung dch EDTA 0,025 M (4.2.37);
V l th tch dung dch EDTA 0,025 M (4.2.37) ly to phc vi nhm, tnh bng mililt;
k3 l t s nng gia dung dch Zn(CH3COO)2 0,025 M v dung dch EDTA 0,025M;
7.6.3. Tnh kt qu
Hm lng titan dioxit (TiO2) tnh bng phn trm, theo cng thc:
m
TiO 2 100
mx
trong
m l Ing titan dioxit tm c t th chun, tnh bng gam;
mx l khi lng mu c trong 25 ml dung dch A ly em xc nh titan, tnh bng gam.
Chnh lch cho php gia hai kt qu xc nh song song khng ln hn 0,10 %.
7.7. Xc nh hm lng canxi oxit (CaO)
7.7.1. Nguyn tc
Loi st, nhm, titan, ... khi dung dch cha canxi v magie bng amoni hydroxyt; chun
lng canxi bng EDTA theo ch th fluorexon trong mi trng kim ca kali hydroxit.
7.7.2. Cch tin hnh
Ly 100 ml dung dch A vo cc, thm khong 2 g amoni clorua (4.1.6), un nng dung dch
n 70 - 80 C, nh git dung dch amoni hydroxit (1+1) n khi bt u xut hin kt ta
hydroxit, cho d t 1 - 2 git na.
un nng dung dch nhit trn khong t 10 - 15 pht. Lc dung dch qua giy lc chy
nhanh vo bnh nh mc 250 ml, ra kt ta v cc bng dung dch amoni nitrat (NH4NO3)
2% nng t 3 - 4 ln, sau ra bng nc ct nng n ht ion clorua trong nc ra;
thm nc ti vch mc, lc u, c dung dch B dng xc nh canxi v magie.
Ly 100 ml dung dch B vo cc, thm 20 ml dung dch kali hydroxit 25%, 2 ml dung dch
kali xianua 5 % v mt t hn hp ch th fluorexon 1 % (4.1.9), dung dch c mu vng xanh
hunh quang. t cc trn mt nn mu en, dng dung dch EDTA 0,01 M (4.2.36) chun
dung dch trong cc n khi dung dch chuyn mu t xanh hunh quang sang hng; ghi th
tch EDTA tiu th (V1).
7.7.3. Tnh kt qu
Hm lng canxi oxit (CaO) tnh bng phn trm, theo cng thc:
0,00056 K1 V1
CaO 100
mx
trong
0,00056 l khi lng canxi oxit tng ng vi 1 ml dung dch EDTA 0,01 M, tnh bng gam;
K1 l h s nng dung dch EDTA 0,01 M (4.2.36);
V1 l th tch dung dch EDTA 0,01 M tiu th chun lng canxi, tnh bng mililt;
mx l khi lng mu c trong 100 ml dung dch B ly em xc nh canxi, tnh bng gam.
Chnh lch cho php gia hai kt qu xc nh song song khng ln hn 0,20 %.
7.8. Xc nh hm lng magi oxit (MgO)
7.8.1. Nguyn tc
Xc nh tng hm lng canxi v magi oxit trong dung dch B bng EDTA pH 10,5 theo
ch th mu eriocrom T en (ET00), tnh lng magie t hiu s lng EDTA tiu th
chun tng lng canxi - magie v ch ring lng canxi.
7.8.2. Cch tin hnh
Ly 100 ml dung dch B vo cc, thm 20 ml dung dch m pH 10,5, 2 ml dung dch kali
xianua 5 % v vi git dung dch ch th mu eriocrom T en 1 % (4.2.27).
Chun dung dch bng dung dch EDTA 0,01 M, n khi mu chuyn t tm sang xanh
nc bin, ghi th tch EDTA tiu th (V2).
7.8.3. Tnh kt qu
Hm lng magi oxit (MgO) tnh bng phn trm, theo cng thc;

0,000403 K1 V2 V1
MgO 100
mx
trong
0,000403 l khi lng magi oxit tng ng vi 1 ml dung dch EDTA 0,01 M, tnh bng
gam;
K1 l h nng dung dch EDTA 0,01 M (4.2.36);
V2 l th tch dung dch EDTA 0,01 M tiu th chun tng lng canxi v magie, tnh
bng mililt;
V1 l th tch dung dch tiu chun EDTA 0,01 M tiu th chun ring lng canxi
(7.7.2), tnh bng mililt;
mx l khi lng mu c trong 100 ml dung dch B ly xc nh magi, tnh bng gam.
Chnh lch cho php gia hai kt qu xc nh song song khng ln hn 0,20 %.
7.9. Xc nh hm lng kali oxit (K2O) v natri oxit (Na2O)
7.9.1. Nguyn tc
Ha tan mu th thnh dung dch v loi bt cc nguyn t cn tr (st, nhm, titan,) bng
cch kt ta trong mi trng kim amoniac, thu ly dung dch lc. Xc nh hm lng cc
oxit kim loi kim c trong dung dch lc bng mt trong hai loi thit b sau:
- quang ph hp th nguyn t vi cc ngun bc x n sc ng vi bc sng 766,5 nm
(cho kali) v 539,0 nm (cho natri);
- quang ph ngn la vi cc knh lc sng ng vi bc sng 768 nm (cho kali) v bc
sng 589 nm (cho natri).
7.9.2. Cch tin hnh
un dung dch mu th c phn gii bng axit flohydric (7.2.3) n khong 70C; nh git
amoni hydroxit (1+1) n xut hin kt ta, cho d t 1 git n 2 git amoni hydroxit na,
un dung dch ti si.
Lc dung dch khi cn nng qua giy lc chy nhanh vo bnh nh mc 250 ml, dng nc
ct ra sch cc v kt ta n ht ion clo trong nc ra (th bng dung dch bc nitrat
0,5%); ngui, thm nc ti vch mc, lc u thu c dung dch C.
Ly 25 ml dung dch C vo bnh nh mc 250 ml, thm nc ti vch mc, lc u; thu
c dung dch pha long 10 ln: dung dch D.
1 ml dung dch D cha: 0,0001 g mu (0,1 mg/ml).
Thc hin thao tc o kali trong dung dch D trn my quang ph ngn la (hoc my
quang ph hp th nguyn t) theo ng hng dn s dng ca nh sn xut thit b, dng
dung dch mu trng lm dung dch so snh. Ghi li gi tr o c (tr s in k hoc
hp th,). Da vo th chun tm ra nng K2O trong dung dch mu th (Cm).
Xy dng th chun
Ly 6 bnh nh mc 100 ml, ln lt thm mt th tch dung dch tiu chun kali oxit lm vic
(K2O = 0,01 mg/ml) theo th t sau: 0; 2; 5; 10; 15 v 20 ml, thm nc ct ti vch mc v
lc u. Nng kali oxit trong cc bnh ny ln lt l: 0,0000; 0,0002; 0,0005; 0,0010;
0,0015; 0,0020 mg/ml.
Thc hin thao tc o kali trong tng bnh trn my quang ph ngn la (hoc my quang
ph hp th nguyn t) nh thc hin phn trn, dng dung dch trong bnh khng cha
kali lm dung dch so snh. Ghi li gi tr o (tr s in k hoc hp th;...) ca tng bnh.
T nng kali oxit trong mi bnh v gi tr o c trn my tng ng, xy dng th
chun.
- Tin hnh tng t phn tch natri oxit t dung dch D v xy dng ng chun
xc nh hm lng natri oxit.
7.9.3. Tnh kt qu
Hm lng kali oxit (K2O) hoc natri oxit (Na2O) trong mu, tnh bng phn trm, theo cng
thc:
Cm
K2O (hoc Na2O) = 100
C
trong
C l nng mu th trong dung dch D em o trn my, tnh bng mg/ml;
Cm l nng kali oxit (hoc nairi oxit) tm c trn ng chun, tnh bng mg/ml.
Chnh lch cho php gia hai kt qu xc nh song song, khng ln hn 0,10%.