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TCVN

TIU

CHUN

quc

gia

TCVN : 2009
Xut bn ln 1

x ht l cao phng php phn tch ha hc


Granulated blast furnace slag Methods of chemical analysis

H Ni 2008

TCVN .. : 2009

Li ni u
TCVN. : 2008 do Vin Vt liu xy dng - B Xy
dng bin son, B Xy dng ngh, Tng cc Tiu
chun o lng Cht lng thm nh, B Khoa hc v
Cng ngh cng b.

TCVN : 2009

TCVN .. : 2009

Tiu chun quc gia

TCVN ...... : 2009


Xut bn ln 1

X ht l cao Phng php phn tch ha hc


Granulated blast furnace slag Methods of chemical analysis

Phm vi p dng

Tiu chun ny qui nh phng php phn tch ho hc cho x ht l cao.

Ti liu vin dn

Cc ti liu vin dn sau l cn thit khi p dng tiu chun ny. i vi cc ti liu
vin dn ghi nm cng b th p dng bn c nu. i vi cc ti liu vin dn khng
ghi nm cng b th p dng phin bn mi nht, bao gm cc bn sa i (nu c).
TCVN 141 : 2008 Xi mng poclng - Phng php phn tch ho hc.
TCVN 4315 : 2007 X ht l cao dng sn xut xi mng.
TCVN 4851 : 1989 (ISO 3696 :1987) Nc dng phn tch trong phng th nghim Yu cu k thut v phng php th.

3
3.1

Quy nh chung
Ho 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 - 1989 (ISO 3696 : 1987) hoc nc c tinh khit tng ng (sau y gi l nc).

TCVN : 2009
3.2

Ho cht pha long theo t l th tch c t trong ngoc n. V d HCl

(1 + 3) l dung dch gm 1 th tch HCl m c vi 3 th tch nc.


3.3

Dung dch pha long tnh bng phn trm (%) biu th bng s gam cht tan

trong 100 ml nc. V d kali florua (KF), dung dch 5 % l dung dch gm 5 g kali florua
ho tan trong 100 ml nc.
3.4

Khi lng ring (d) ca thuc th m c c tnh bng gam trn mililit

(g/ml).
3.5 Cc ch tiu phn tch c tin hnh trn mu th c gia cng theo iu
6 ca tiu chun ny.
3.6

Mi ch tiu phn tch c tin hnh song song trn hai lng cn ca mu

th v mt th nghim trng (bao gm cc lng thuc th nh nu trong tiu chun,


nhng khng c mu th) hiu chnh kt qu.
Chnh lch gia hai kt qu xc nh song song khng c vt gii hn cho php (c
qui nh ring cho tng ch tiu th), nu vt gii hn cho php phi tin hnh phn
tch li.
3.7 Vic xy dng li ng chun (cho cc ch tiu th c s dng phng php
trc quang, quang ph hp th nguyn t, quang k ngn la) tin hnh nh k
theo khuyn co ca nh sn xut thit b theo cch lm nu trong tiu chun ny.
3.8 Biu th khi lng, th tch v kt qu.
- Khi lng tnh bng gam.
- Th tch tnh bng mililit.
- Kt qu cui cng tnh bng phn trm (%), l trung bnh cng ca hai kt qu
phn tch tin hnh song song, ly n 2 ch s c ngha sau du phy.

Ho cht, Thuc th

4.1 Ho cht rn
4.1.1 Natri cacbonat (Na 2CO3) khan.
4.1.2 Kali cacbonat (K 2CO 3) khan.
4.1.3 Hn hp nung chy : trn u Na 2CO3 (4.1.1) vi K 2CO3 (4.1.2) theo t l khi
lng 1 : 1, bo qun trong bnh nha kn.
4.1.4 Amoni clorua (NH 4Cl) tinh th.
4.1.5 Kali pyrosunphat (K 2S2O7) khan hoc kali hydrosunphat (KHSO 4) khan.

TCVN .. : 2009
4.1.6 Phenolphtalein tinh th.
4.1.7 Km axetat Zn(CH 3COO)2.2 H 2O.
4.1.8 Silic dioxit (SiO 2) c tinh khit 99,9 %.
4.1.9 Ch th mu fluorexon 1 %: dng chy ci s hoc thu tinh nghin mn 0,1
g ch th mu fluorexon vi 10g kali clorua (KCl), bo qun trong l thu tinh ti mu.
4.2 Ho cht lng, thuc th
4.2.1 Axit clohydric (HCl) m c, d = 1,19.
4.2.2 Axit clohydric (HCl), pha long (1 + 1).
4.2.3 Axit clohydric (HCl), pha long (1 + 9).
4.2.4 Axit flohydric (HF) m c, d = 1,12.
4.2.5 Axit sunfuric (H 2SO4) m c, d = 1,84.
4.2.6 Axit sunfuric (H 2SO4), pha long (1 + 1).
4.2.7 Axit sunfuric (H 2SO4), dung dch 0,10 %: Cho t t 3 ml axit sunfuric m
c (iu 4.2.5) vo 500 ml nc, ngui pha long thnh 1000 ml.
4.2.8 Axit boric (H 3BO3), dung dch bo ho: Ho tan 50 g axit boric (H 3BO 3) trong
500 ml nc nng, pha long thnh 1000 ml.
4.2.9 Axit oxalic (H 2C 2O4), dung dch 2 %, bo qun trong bnh nha polyetylen.
4.2.10 Dung dch kh: Ho tan 15 g axit tartric (H 2C4H 4O6) v 1 g axit ascobic
(C6H 8O6) trong 100 ml nc. Dung dch s dng c trong 2 n 3 ngy, bo qun
trong bnh thu tinh ti mu.
4.2.11 Amoni molipat ((NH 4)6Mo 7O24.4H2O), dung dch 5 %: Ho tan 25 g amoni
molipat ((NH 4)6Mo7O24.4H 2O) vo 200 ml nc, un m cho tan, (nu dung dch c
th phi lc) pha long thnh 500 ml. Dung dch s dng c trong bn tun, bo
qun trong bnh nha polyetylen.
4.2.12 Kali florua (KF), dung dch 5 %, bo qun trong bnh nha polyetylen.
4.2.13 Axit axetic (CH 3COOH) m c, d = 1,05 1,06.
4.2.14 Amoni hydroxit (NH 4OH) m c, d = 0,88 0,91 (25 %)
4.2.15 Urotropin (hecxametylen tetramin (C 6H 12N 4) ), dung dch 10 %, bo qun
trong bnh nha polyetylen.

TCVN : 2009
4.2.16 Urotropin (hecxametylen tetramin (C 6H 12N 4) ), dung dch 30 %, bo qun
trong bnh nha polyetylen.
4.2.17 Natri hydroxit (NaOH), dung dch 10 %, bo qun trong bnh nha
polyetylen.
4.2.18 Natri hydroxit (NaOH), dung dch 30 %, bo qun trong bnh nha
polyetylen.
4.2.19 Kali hydroxit (KOH), dung dch 25 %, bo qun trong bnh nha polyetylen.
4.2.20 Kali xyanua (KCN), dung dch 5 %, bo qun trong bnh nha polyetylen.
4.2.21 Natri florua (NaF), dung dch 3 %, bo qun trong bnh nha polyetylen.
4.2.22 Bari clorua (BaCl 2), dung dch 10 %.
4.2.23 Ch th eriocrom T en (ETOO), dung dch 0,10 % : Ho tan 0,10 g ch th ETOO
trong 100 ml cn 90 %, thm tip vo dung dch 3 g Hydroxylamin hydroclorua, bo qun
trong chai thu tinh ti mu.
4.2.24 Ch th xylenol da cam, dung dch 0,10 %.
4.2.25 Ch th phenolphtalein, dung dch 0,10 % trong cn 90 %.
4.2.26 Axit sunfosalixylic (C 6H 4(OH)SO 3H), dung dch 10 %.
4.2.27 EDTA (Na 2H 2C 10H 12O8N 2.2H2O), dung dch 1 %.
4.2.28 Nc brm, dung dch 3 %.
4.2.29 Dung dch tiu chun EDTA 0,01 M: Pha t ng chun (fixanal)
4.2.30 Dung dch tiu chun km axetat (Zn(CH 3COO)2) 0,025 M
Ho tan 5,65 g n 5,75 g Zn(CH 3COO)2.2H 2O trong 200 ml nc ct, cho thm vo 1 ml
axit axetic c, un n tan trong, ngui, pha long thnh 1 lt.
* Xc nh h s K gia dung dich EDTA 0,01 M v dung dch km axetat
0,025 M:
Dng pipet ly 50 ml dung dch EDTA 0,01 M (4.2.29) cho vo cc thu tinh dung tch
250 ml, thm nc n th tch 100 ml v 20 ml dung dch pH = 5,5, thm 2 n 3
git ch th xylenol da cam 0,10 %. un ti nhit 70 0C n 80 0C, chun dung
dch khi cn nng bng dung dch km axetat pha c n khi dung dch trong cc
chuyn t mu vng sang hng, ghi th tch dung dch km axetat tiu th (V Zn).T s
nng K gia hai dung dch c tnh nh sau:

VE
VZn 2,5

TCVN .. : 2009
Trong :

VE l th tch dung dch EDTA ly chun , tnh bng mililit;


VZn l th tch dung dch km axetat tiu th khi chun , tnh bng

mililit.
4.2.31 Dung dch m pH = 5,5: Ho tan khong 100 ml amoni hydroxit m
c trong 700 ml nc, thm khong 100 ml axit axetic, khuy u. iu chnh pH =
5,5 bng amoni hydroxit (1 + 1) v axit axetic (1 + 1), thm n c thnh 1 lt, khuy
u.
4.2.32 Dung dch m pH = 10,5: Ho tan 54 g amoni clorua vo 500 ml n c,
thm 350 ml amoni hydroxit m c, khuy u. iu chnh pH = 10,5 bng
amoni hydroxit (1 + 1), thm nc thnh 1 lt, khuy u.
4.2.33 Dung dch tiu chun gc Si 4+ (SiO 2 = 0,2 mg/ml):
Nung chy 0,10 g silic dioxit tinh khit ( c nung 1000 0C n khi lng khng
i) vi 3 g - 4 g hn hp nung chy (4.1.3) trong chn bch kim nhit 950 0C
50 0C trong thi gian t 30 pht - 40 pht. Ly chn ra t nghing, ngui.
Chuyn nh lng khi nng chy vo cc c sn 200 ml nc v 10 g NaOH, ri
un ti tan trong. ngui, thm nc ti 500 ml, lc u. Bo qun trong bnh nha
polyetylen.
* Dung dch tiu chun lm vic Si 4+ (SiO2 = 0,02 mg/ml):
Dng pipet ly 25 ml dung dch tiu chun gc cho vo bnh nh mc dung tch
250 ml, thm nc ti vch mc, lc u. Dung dch s dng c trong 7 ngy.
* Xy dng ng chun:
Ly 11 bnh nh mc dung tch 100 ml (bnh nha polyetylen), ln lt cho vo mi
bnh mt th tch dung dch tiu chun silic dioxit lm vic ( CSiO 2 0,02 mg/ml ) theo
th t sau: 0 ml; 1 ml; 2 ml; 4 ml; 6 ml; 8 ml; 10 ml; 12 ml; 16 ml; 20 ml; 25 ml, thm
dung dch axit sunfuric 0,1 % (4.2.7) n khong 40 ml. Thm vo 5 ml dung dch
Kali florua 5 % (4.2.12), lc u sau 1 pht thm tip 15 ml dung dch axit boric bo
ho (4.2.8), thm tip 10 ml dung dch amoni molipat 5 % (4.2.11) (thi im
khng) v 10 ml dung dch axit oxalic 2 % (4.2.9). Sau 20 pht thm tip 5 ml dung
dch kh (4.2.10), thm dung dch axit sunfuric 0,10 % (4.2.7) n vch nh mc,
lc u. Sau 30 pht (tnh t thi im khng) o hp th quang ca dung
dch mu bc sng = 800 nm - 820 nm. Dung dch so snh l dung dch mu
trng (ly t th nghim trng).
T lng silic dioxit c trong mi bnh v ga tr hp th quang tng ng xy dng
ng chun.
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TCVN : 2009
4.2.34 Dung dch tiu chun gc Fe 3+ (Fe2O3 = 0,2 mg/ml):
Ho tan 0,20 g st (III) oxit sy kh 100 0C - 110 0C vo cc c sn 50 ml
dung dch axit clohydric (1+1) (4.2.2), un si nh ti tan trong. Chuyn dung dch
vo bnh nh mc dung tch 1000 ml, thm nc ti vch mc, lc u.
* Dung dch tiu chun lm vic Fe 3+ (Fe2O3 = 0,02 mg/ml):
Dng pipet ly 25 ml dung dch tiu chun gc cho vo bnh nh mc dung tch
250 ml, thm nc ct ti vch mc lc u.
* Xy dng ng chun:
Ly 11 bnh nh mc dung tch 100 ml, ln l t cho vo mi bnh mt th tch
dung dch tiu chun st (III) oxit lm vic ( C Fe 2O3 0,02 mg/ml ) theo th t 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 n khong
50 ml, thm tip 10 ml dung dch axit sunfosalixylic 10 % (4.2.26), sau va lc
u bnh va nh tng git amoni hydroxit m c (4.2.14) n khi dung dch
xut hin mu vng, cho d t 3 ml n 4 ml amoni hydroxit na, thm nc ti vch
nh mc, lc u.
Sau 15 pht - 20 pht, o hp th quang ca dung dch mu b c sng = 420
nm - 430 nm. Dung dch so snh l dung dch mu trng (ly t th nghim trng).
T lng st (III) oxit c trong mi bnh v ga tr hp th quang t ng ng xy
dng ng chun.

Thit b, dng c

5.1 Cn phn tch c chnh xc n 0,0001 g.


5.2 T sy, t nhit 300 0C 5 0C c b phn iu chnh nhit .
5.3 L nung, t nhit 1200 0C 50 0C c b phn iu chnh nhit .
5.4 My so mu quang in hoc ph quang k UV-VIS, c kh nng o
hp th quang bc sng t 380 nm n 850 nm.
5.5 My o pH, c chnh xc n 0,01 pH.
5.6 My ct nc.
5.7 T ht hi c.
5.8 Chn s, chn bch kim, dung tch 30 ml hoc 50 ml.
5.9 Bp in, bp cch ct, kim sot c 400 0C.

TCVN .. : 2009
5.10 Bnh ht m 140 mm hoc 200 mm.
5.11 Bnh nh mc, dung tch 100 ml, 200 ml, 250 ml, 500 ml, 1000 ml.
5.12 Pipet dung tch 1 ml, 2 ml, 5 ml, 10 ml, 25 ml, 50 ml, 100 ml;
5.13 Buret 10 ml, 20 ml, 25 ml, chnh xc n 0,05 ml.
5.14 Giy lc:
Giy lc nh lng khng tro chy chm (ng knh l trung bnh khong 2
m).
Giy lc nh lng khng tro chy trung bnh (ng knh l trung bnh
khong 7 m).
Giy lc nh lng khng tro chy nhanh (ng knh l trung bnh khong 20
m).
Giy lc nh tnh chy nhanh (ng knh l trung bnh khong 20 m).
5.15 ng ong dung tch 10 ml, 20 ml, 25 ml, 50 ml, 500 ml.
5.16 Chy, ci m no.
5.17 Sng, c kch thc l 0,063 mm; 0,10 mm; 0,20 mm..

Ly mu v chun b mu th

6.1 Ly mu
Theo TCVN 4315 - 5 : 2007.
6.2 Chun b mu th
Mu th mang v phng th nghim c khi lng khng nh hn 400 g. Dng phng
php chia t chia mu thnh hai phn. Mt phn (phn mu A) dng xc nh
m, phn cn li (phn mu B) sy kh mu nhit 105 0C 5 0C dng phn
tch ho. Trn u mu th (phn mu B), 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 (khi gia cng mu th, nu s
dng dng c bng thp, phi dng nam chm loi st ln vo mu). Dng ph ng
php chia t ly khong 15 g n 20 g nghin mn trn ci m no n lt ht qua
sng 0,063 mm lm mu phn tch ho hc, phn cn li bo qun trong l thu tinh
y kn lm mu lu.
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TCVN : 2009
Mu phn tch ho hc c sy nhit 105 0C 5 0C n khi lng khng
i.

Phng php th

7.1 Xc nh hm lng m (W)


7.1.1 Nguyn tc
Mu th c sy 105 0C 5 0C n khi lng khng i. T s gim khi lng tnh
ra c hm lng m c trong mu.
7.1.2 Cch tin hnh
Cn khong 10 g mu (phn mu A) chnh xc n 0,0001 g c chun b theo
iu 6, chuyn vo hp lm m c sy nhit 105 0C 5 0C v cn n khi
thu c khi lng khng i. Sy hp c mu nhit trn khong 1 gi n 1,5
gi, ngui trong bnh ht m n nhit phng ri cn. Lp li qu trnh sy
nhit trn trong 15 pht, lm ngui v cn n khi thu c khi lng khng
i.
7.1.3 Tnh kt qu
Hm lng m, tnh bng phn trm, theo cng thc;

%W

m1 m 2
100
m

Trong :
m 1 l khi lng mu v hp lm m trc khi sy, tnh bng gam;
m 2 l khi lng mu v hp lm m sau khi sy, tnh bng gam;
m l khi lng mu ly phn tch, tnh bng gam.
Chnh lch gia hai kt qu xc nh song song khng ln hn 0,10 %.
7.2

Xc nh hm lng mt khi nung (MKN)

7.2.1 Nguyn tc
Mu th c nung 950 0C 50 0C n khi lng khng i. T s gim khi lng khi
nung mu ti nhit trn v hm lng sunfua xc nh theo iu 7.9, tnh ra lng
mt khi nung.
7.2.2 Cch tin hnh

TCVN .. : 2009
Cn khong 1 g mu (phn mu B) chnh xc n 0,0001 g c chun b theo
iu 6, chuyn vo chn s c nung nhit 950 0C 50 0C v cn n khi
thu c khi lng khng i. Nung chn c mu nhit trn khong 1 gi n
1,5 gi , ly mu ra ngui trong bnh ht m n nhit phng v cn. Nung
li nhit trn trong 15 pht, lm ngui v cn n khi thu c khi lng khng
i.
7.2.3 Tnh kt qu
Lng mt khi nung, tnh bng phn trm, theo cng thc:

% MKN

m1 m 2
100
m

Trong :
m 1 l khi lng mu v chn trc khi nung, tnh bng gam;
m 2 l khi lng mu v chn sau khi nung, tnh bng gam;
m l khi lng mu ly phn tch, tnh bng gam.

12

TCVN : 2009

TCVN .. : 2009
Chnh lch gia hai kt qu xc nh song song khng ln hn 0,10 %.
7.2.4 Xc nh hm lng MKN qui i
Trong x ht l cao, hm lng sunfua (S 2-) trong mu gy sai lch m n kt qu
xc nh hm lng MKN. Nn hm lng MKN c hiu chnh theo hm lng sunfua (S 2-)
trong mu nh sau:
% MKN qui i = % MKN (thu c mc 7.2.3) + 1,996 x % S

7.3

2-

(iu 7.9)

Xc nh hm lng silic dioxit (SiO 2)

7.3.1 Xc nh hm lng silic dioxit dng kt ta silisic (phng php khi lng)
7.3.1.1 Nguyn tc
Ho tan mu x trong axit clohydric m c, c cn dung dch tch n c ca
axit silisic, lc, ra, v nung kt ta 1000 0C 50 0C, dng dung dch axit flohydric
tch silic dng silic tetra florua, nung, cn, lng mt i tng ng vi hm lng
silc ioxit.
7.3.1.2 Cch tin hnh
Cn khong 1 g mu (phn mu B) chnh xc n 0,0001 g c chun b theo
iu 6 vo bt s, tm t mu bng nc ct. y bt bng mt knh ng h, cho t
t 15 ml axit clohydric m c qua ming bt. C cn dung dch trn bp cch ct
( nhit t 100 0C n 110 0C) n khng cn git nc trn mt knh ng h.
Trong qu trnh c mu, dng a thu tinh dm nh cc cc mui to thnh n c
ht khng ln hn 2 mm, tip tc c mu nhit trn trong thi gian t 1 gi n
1,5 gi. ngui mu th, thm vo bt s 15 ml axit clohydric m c, yn 10
pht, thm tip t 90 ml n 100 ml nc un si, khuy u cho tan ht mui.
Lc dung dch cn nng qua giy lc khng tro chy trung bnh. Dng dung dch axit
clohydric (1+9) (4.2.3) un nng, ra kt ta v thnh bt, lc gn 3 ln, sau
chuyn kt ta vo giy lc, dng giy lc khng tro chy trung bnh lau sch
a thu tinh v thnh bt. Tip tc ra bng nc un si n ht axit (th bng
giy o pH). Thu nc lc v nc ra vo bnh nh mc dung tch 500 ml. Chuyn
giy lc c kt ta v giy lau vo chn bch kim, sy v t giy lc trn bp in.
Nung chn nhit 1000 0C 50 0C trong 1 gi 30 pht. Ly chn ra ngui
trong bnh ht m n nhit phng. Nung li nhit trn n khi thu c
khi lng khng i. Ghi khi lng chn v kt ta thu c (m 1).

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Tm t kt ta trong chn bng vi git nc, thm vo 0,5 ml dung dch axit sunfuric (1 +
1) (4.2.6) v 10 ml axit flohydric 40 % (4.2.4). Lm bay hi cht cha trong chn trn bp
in n kh. Thm tip t 3 ml n 4 ml axit flohydric, lm bay hi trn bp in
n ngng bc khi trng. Nung chn bch kim v cn nhit 1000 0C 50 0C trong
30 pht. Ly chn ra ngui trong bnh ht m n nhit phng. Nung li nhit
trn n khi thu c khi lng khng i. Ghi khi lng chn v cn thu c (m2).
Nung cn cn li trong chn bch kim vi t 2 g n 3 g kali pyrosulfat (4.1.5) nhit
750 0C 50 0C n tan trong. Lm ngui chn bch kim v ho tan khi nung
chy trong cc thu tinh c sn 50 ml nc v 5 ml axit clohydric (1+1) (4.2.2), un
ti tan trong. Gp dung dch ny vo dung dch trong bnh nh mc 500 ml, thm
nc ti vch mc, lc u thu c "dung dch A". Dung dch ny dng xc nh
cc thnh phn silic dioxit ho tan trong dung dch, nhm, st, canxi, magi, titan,
mangan trong mu.
7.3.1.3 Tnh kt qu
Hm lng silic dioxit, tnh bng phn trm, theo cng thc:

% SiO2

m1 m2
100
m

Trong :
m 1 l khi lng chn bch kim v kt ta trc khi x l bng axit flohydric, tnh bng
gam;
m 2 l khi lng chn bch kim v kt ta sau khi x l bng axit flohydric, tnh bng
gam;
m l khi lng mu ly phn tch, tnh bng gam.
Chnh lch gia hai kt qu xc nh song song khng ln hn 0,25 %.
7.3.2

Xc nh silic dioxit (SiO 2) ha tan trong dung dch (phng php o

mu)
7.3.2.1 Nguyn tc
Trong mi trng axit (pH=1,0 - 1,5) Si 4+ ha tan tc dng vi amoni molipat to
thnh phc mu vng, kh phc ny sang dng mu xanh bng axit ascobic. o
hp th quang ca dung dch phc mu xanh bc sng = 800 nm - 820 nm.
7.3.2.2 Cch tin hnh
Dng pipet ly 25 ml "dung dch A" (7.3.1) cho vo bnh nh mc dung tch 100 ml
(bnh nha polyetylen), thm dung dch axit sunfuric 0,10 % (4.2.7) n khong 40

TCVN .. : 2009
ml. Tip tc lm theo cc thao tc mc (4.2.33) trong phn xy dng ng chun
t Thm vo 5 ml kali florua 5 % (4.2.12) n Dung dch so snh l dung dch
mu trng (ly t th nghim trng).
T gi tr hp th quang o c, da vo ng chun tm c hm lng silic dioxit c
trong bnh.
7.3.2.3 Tnh kt qu:
Hm lng silic dioxit ho tan, tnh bng phn trm, theo cng thc:

% SiO 2(Ha tan)

m1
100
m2

Trong :
m 1 l lng silic dioxit tm c trn ng chun, tnh bng gam;
m 2 l khi lng mu tng ng vi th tch mu ly phn tch, tnh bng gam;
Chnh lch gia hai kt qu xc nh song song khng ln hn 0,04 %.
7.3.3 Xc nh hm lng SiO2 tng
Hm lng SiO 2 tng l tng hm lng SiO 2 xc nh theo iu 7.3.1 v iu 7.3.2
7.4

Xc nh hm lng st (III) oxit (Fe2O3)

7.4.1 Xc nh hm lng st (III) oxit theo phng php chun phc cht
Phng php ny p dng khi hm lng st (III) oxit ln hn 2 %
7.4.1.1 Nguyn tc
Chun ion st (III) bng dung dch EDTA mi tr ng pH 1,5 n 1,8 vi ch th
mu axit sunfosalixylic. Khi kt thc chun mu dung dch chuyn t tm
sang vng rm.
7.4.1.2 Cch tin hnh
Dng pipet ly 25 ml dung dch A (7.3.1) cho vo cc thu tinh dung tch 250 ml,
thm 2 ml dung dch axit sunfosalixylic 10 % (4.2.26), thm n c ct n khong 100
ml. Dng dung dch axit clohydric (1 + 1) (4.2.2) v dung dch natri hydroxit 10 %
(4.2.17) nh t t tng git iu chnh pH t 1,5 n 1,8 (dung dch chuyn
sang mu tm ). un nng dung dch n 50 0C 60 0C, chun bng dung
dch tiu chun EDTA 0,01 M n khi dung dch chuyn t mu tm sang vng
rm.
7.4.1.3 Tnh kt qu
Hm lng st (III) oxit, tnh bng phn trm, theo cng thc
16

TCVN : 2009
% Fe 2 O 3

0,0007985 V
100
m

Trong :
V l th tch dung dch tiu chun EDTA 0,01 M tiu th khi chun , tnh bng
mililit;
0,0007985 l khi lng Fe2O3 tng ng vi 1 ml dung dch tiu chun EDTA 0,01 M, tnh
bng gam;
m l khi lng mu tng ng vi th tch mu ly phn tch, tnh bng gam.
Chnh lch gia hai kt qu xc nh song song khng ln hn 0,15 %.
7.4.2 Xc nh hm lng st (III) oxit theo phng php o mu.
Phng php ny p dng khi hm lng st (III) oxit nh hn 2 %
7.4.2.1 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
hp th quang ca dung dch phc mu vng bc sng = 420 nm - 430 nm.
7.4.2.2 Cch tin hnh
Dng pipet ly 25 ml dung dch A (7.3.1) cho vo bnh nh mc dung tch 100 ml.
Tip tc lm theo cc thao tc mc (4.2.34) trong phn xy dng ng chun t
pha long n khong 50 ml n Dung dch so snh l dung dch mu trng
(ly t th nghim trng).
T gi tr hp th quang o c, da vo ng chun tm c hm lng st (III)
oxit.
7.4.2.3 Tnh kt qu
Hm lng st (III) oxit, tnh bng phn trm, theo cng thc:

% Fe 2 O 3

m1
100
m2

Trong :
m 1 l lng st (III) oxit tm c t ng chun, tnh bng gam;
m 2 l khi lng mu c trong dung dch ly em xc nh st (III) oxit, tnh bng
gam;
Chnh lch cho php gia hai kt qu xc nh song song khng ln hn 0,04 %.

TCVN .. : 2009
7.5

Xc nh hm lng nhm oxit (Al 2O3)

7.5.1 Nguyn tc
Loi Ca2+, Mg 2+

ra khi dung dch cha Al 3+ bng dung dch urotropin 30 %, tch

nhm khi cc nguyn t nh hng bng kim mnh. To phc gia nhm v EDTA d
pH = 5,5. Chun lng d EDTA bng dung dch km axetat theo ch th xylenol da
cam. Dng natri florua gii phng EDTA khi phc complexonat nhm, dng dung
dch tiu chun km axetat chun lng EDTA c gii phng, t tnh ra hm lng nhm.
7.5.2 Cch tin hnh
Dng pipet ly 100 ml dung dch A (7.3.1) cho vo cc thu tinh dung tch 250 ml,
thm vo cc khong 2 g amoni clorua (4.1.6), un nng, trung ho bng amoni
hydroxyt m c (4.2.14) n khi bt u xut hin kt ta hydroxyt, ho tan
kt ta tr li bng vi git dung dch axit clohydric (1+1) (4.2.2). Cho t t dung
dch urotropin 30 % (4.2.16) n kt ta hon ton. Cho d 20 ml dung dch urotropin
30 % na, un nng dung dch trong cc n gn si trong 10 pht. Lc dung dch
cha kt ta khi cn nng qua giy lc chy nhanh, ra kt ta v cc thu tinh 5 ln
n 7 ln bng dung dch urotropin 10 % (4.2.15). Ho tan kt ta trn giy lc bng
dung dch axit clohydric (1+1) (4.2.2), hng dung dch vo cc tin hnh kt ta.
Ra giy lc bng nc nng n ht phn ng axit (th bng giy o pH). Thm vo n c
lc 5 ml dung dch axit clohydric (1+1) (4.2.2), un si 3 pht. Thm vo cc 30 ml
dung dch natri hydroxit 30 % (4.2.18), khuy u, un si dung dch 1 pht n 2
pht, ly ra ngui ri chuyn dung dch trong cc vo bnh nh mc dung tch
250 ml, thm nc ti vch mc, lc u. Lc dung dch qua giy lc th (kh), phu
(kh) vo bnh nn dung tch 250 ml (kh). Dung dch lc dng xc nh hm l ng
nhm oxit.
Dng pipet ly 100 ml dung dch lc trn cho vo cc thu tinh dung tch 250 ml, thm
vo cc 10 ml dung dch EDTA 1 %( iu 4.2.27), thm tip vo cc 1 git - 2 git ch
th phenolphtalein 0,10 % ( 4.2.25) dng dung dch axit clohydric (1+1) (4.2.2) v dung
dch natri hydroxit 10 % (4.2.17) iu chnh dung dch ti mi trng trung tnh (dung
dch mt mu hng), thm vo cc 15 ml dung dch m pH = 5,5 (4.2.31). un nng
dung dch trong cc n khong 80 0C, thm vo cc vi git ch th xylenol da cam
0,10 % (4.2.24) v dng dung dch tiu chun km axetat 0,025 M (4.2.30) chun
n khi dung dch chuyn t mu vng sang hng. Thm vo cc 15 ml dung dch
natri florua 3 % (4.2.21), un si trong 3 pht, dung dch lc ny c mu vng,
ngui dung dch n 70 0C - 80 0C ri chun bng dung dch tiu chun km axetat

18

TCVN : 2009
0,025 M (4.2.30) n khi dung dch chuyn t vng sang hng. Ghi th tch km axetat
tiu th khi chun ln th hai (V Zn).
7.5.3 Tnh kt qu
Hm lng nhm oxit, tnh bng phn trm, theo cng thc:

% Al 2 O 3

0,0012745 VZn K
100
m

Trong :
0,0012745 l h s gam Al 2O3 ng vi 1 ml dung dch tiu chun km axetat 0,025
M;
VZn l th tch dung dch km axetat 0,025 M tiu th khi chun l ng EDTA c gii
phng ra khi phc, tnh bng ml;
K l h s nng gia dung dch tiu chun km axetat 0,025 M v dung dch
tiu chun EDTA 0,01 M;
m l khi lng mu tng ng vi th tch mu ly phn tch, tnh bng gam;
Chnh lch cho php gia hai kt qu xc nh song song khng ln hn 0,15 %.
7.6

Xc nh hm lng canxi oxit (CaO)

7.6.1 Nguyn tc
Fe3+, Al3+, Ti 4+ v cc ion cn tr khc c tch khi Ca 2+ v Mg 2+ bng amoni hydroxit.
Chun Ca 2+ bng dung dch EDTA tiu chun pH ln hn 12 vi ch th fluorexon,
im tng ng dung dch chuyn t mu xanh hunh quang sang mu hng.
7.6.2 Cch tin hnh
Dng pipet ly 100 ml dung dch A (7.3.1) cho vo cc thu tinh dung tch 250 ml,
thm 1 g amoni clorua (4.1.4), un dung dch n 60 0C - 70 0C, nh t t dung dch
amoni hydroxit m c (4.2.14) v khuy u n khi xut hin kt ta hydroxit,
cho d 1 git amoni hydroxit. un nng dung dch 70 0C 80 0C trong thi gian t 45
pht n 60 pht ng t kt ta v loi amoni hydroxit d. ngui dung dch,
chuyn dung dch trong cc vo bnh nh mc dung tch 250 ml, thm n c ti vch
mc, lc u. Lc dung dch qua giy lc chy nhanh (kh), phu (kh) vo bnh
nn dung tch 250 ml (kh) (dung dch B).
Dng pipet ly 25 ml dung dch B, thm 80 ml nc, 20 ml dung dch kali hydroxit 25 %
(4.2.19), 2 ml dung dch kali xyanua 5 % (4.2.20) v mt t ch th fluorexon 1 %
(4.1.10), t cc trn nn mu en, dng dung dch tiu chun EDTA 0,01 M (4.2.29),

TCVN .. : 2009
chun cho n khi dung dch chuyn t mu xanh hunh quang sang hng. Ghi
th tch dung dch tiu chun EDTA 0,01 M tiu th (V 1).
Lm song song mt th nghim trng hiu chnh kt qu. Ghi th tch dung
dch tiu chun EDTA 0,01 M tiu th (V 01 ).
7.6.3 Tnh kt qu
Hm lng canxi oxit, tnh bng phn trm, theo cng thc:

% CaO

0,00056 (V1 V01 )


100
m

Trong :
V01 l th tch dung dch tiu chun EDTA 0,01 M tiu th khi chun mu trng,
tnh bng mililit;
V1 l th tch dung dch tiu chun EDTA 0,01 M tiu th khi chun mu th, tnh
bng mililit;
0,00056 l khi lng canxi oxit CaO tng ng vi 1 ml dung dch tiu chun EDTA 0,01
M, tnh bng gam;
m l khi lng mu tng ng vi th tch mu ly xc nh canxi oxit, tnh bng
gam;
Chnh lch gia hai kt qu xc nh song song khng ln hn 0,30 %.
7.7

Xc nh hm lng magi oxit (MgO)

7.7.1 Nguyn tc
Chun tng lng Ca2+ v Mg 2+ trong mu bng dung dch tiu chun EDTA 0,01 M
theo ch th eriocrom T en pH = 10,5. Xc nh hm lng magi oxit theo hiu s
th tch dung dch tiu chun EDTA tiu th.
7.7.2 Cch tin hnh
Dng pipet ly 25 ml dung dch B (7.6.2) thm 80 ml nc ct, 15 ml dung dch m
pH = 10,5 (4.2.32) v 2 ml dung dch kali xyanua 5 % (4.2.20) cng vi vi git
eriocrom T en 0,10 % (4.2.23), chun tng lng Ca2+ v Mg 2+ bng dung dch
tiu chun EDTA 0,01 M (4.2.29) n khi dung dch chuyn t mu ru nho sang
xanh nc bin. Ghi th tch dung dch tiu chun EDTA 0,01 M tiu th (V 2).
Lm song song mt th nghim trng hiu chnh kt qu. Ghi th tch dung
dch tiu chun EDTA 0,01 M tiu th (V 02 ).
7.7.3 Tnh kt qu

20

TCVN : 2009
Hm lng magi oxit, tnh bng phn trm, theo cng thc:

% MgO

0,000403 (V2 V02 ) (V1 V01 )


100
m

Trong :
V01 l th tch dung dch tiu chun EDTA 0,01 M tiu th khi chun ring l ng
canxi trong mu trng, tnh bng mililit;
V1 l th tch dung dch tiu chun EDTA 0,01 M tiu th khi chun ring l ng canxi
trong dung dch mu th, tnh bng mililit;
V02 l th tch dung dch tiu chun EDTA 0,01 M tiu th khi chun tng l ng
canxi v magi trong mu trng, tnh bng mililit;
V2 l th tch dung dch tiu chun EDTA 0,01 M tiu th khi chun tng l ng
canxi v magi trong dung dch mu th, tnh bng mililit;
0,000403 l khi lng magi oxit MgO tng ng vi 1 ml dung dch EDTA 0,01 M, tnh
bng gam;
m l khi lng mu tng ng vi th tch mu ly xc nh magi oxit, tnh bng
gam;
Chnh lch gia hai kt qu xc nh song song khng ln hn 0,25 %.
7.8 Xc nh hm lng anhydric sunfuric (SO 3)
7.8.1 Nguyn tc
Kt ta sunfat di dng bari sunfat. T bari sunfat thu c tnh ra khi lng anhydric
sunfuric.
7.8.2 Cch tin hnh
Cn khong 1 g mu (phn mu B) chnh xc n 0,0001 g chun b theo iu
6, cho vo cc dung tch 100 ml, thm 50 ml dung dch axit clohydric (1+9) (4.2.3),
dng a thu tinh dm cho tan ht mu, un si nh trn bp cch ct trong 30
pht. Lc gn vo giy lc khng tro chy trung bnh. Ra bng n c si n ht axit
(th bng giy o pH). un si dung dch lc ng thi un si dung dch bari
clorua 10 % (4.2.22). Cho t t 10 ml dung dch bari clorua 10 % khuy u, tip tc
un nh trong 5 pht. yn kt ta ni m (40 0C n 50 0C) t 4 gi n 8 gi
kt ta lng xung.
Lc kt ta qua giy lc khng tro chy chm, ra kt ta v giy lc 5 ln bng dung
dch axit clohydric (1+9) (4.2.3) un nng. Tip tc ra vi nc un si cho n
ht axit (th bng giy o pH). Cho kt ta v giy lc vo chn s nung v cn

TCVN .. : 2009
n khi thu c khi lng khng i (m 2). Sy v t chy giy lc, nung nhit
t 800 0C n 850 0C trong 60 pht.
Ly ra ngui trong bnh ht m n nhit phng, cn, nung li nhit trn
n khi thu c khi lng khng i (m1).
7.8.3 Tnh kt qu
Hm lng anhydric sunfuric, tnh bng phn trm, theo cng thc:

% SO 3

0,343 (m1 m 2 )
100
m

Trong :
m 1 l khi lng chn c kt ta, tnh bng gam;
m 2 l khi lng chn khng, tnh bng gam;
m l khi lng mu tng ng vi th tch mu ly xc nh anhydric sunfuric,
tnh bng gam;
0,343 l h s chuyn i t BaSO 4 sang SO3;
Chnh lch gia hai kt qu xc nh song song khng ln hn 0,05 %.
7.9 Xc nh hm lng sunfua (S2-)
7.9.1 Nguyn tc
Oxy ho lu hunh dng sunfua thnh sunfat bng nc brm. Sau kt ta di dng bari
sunfat, lc ra, nung v cn t xc nh c hm lng sunfua c trong mu.
7.9.2 Cch tin hnh
Cn khong 1 g mu (phn mu B) chnh xc n 0,0001 g chun b theo iu
6 vo cc dung tch 250 ml, tm t mu bng nc. Thm vo cc t 70 ml n 80 ml
nc brm (4.2.28), khuy u, yn t 2 gi n 3 gi. Sau thm t t 20 ml
dung dch axit clohydric m c (4.2.1) v khuy. Sau t 10 pht n 15 pht
chuyn ton b dung dch sang bt s, c mu trong bt s n kh kit tch
loi silic. Lm ngui bt s, thm vo 5 ml axit clohydric m c (4.2.1), yn
10 pht, thm tip 45 ml nc un si khuy cho tan mui. Lc dung dch qua giy lc
chy trung bnh, nc lc ra thu vo cc dung tch 250 ml, dng nc ct nng ra sch
bt s v giy lc n ht axit (th bng giy o pH). Tip tc lm theo cc thao tc
mc (7.8.2) t " un si dung dch lc ng thi un si dung dch bari clorua 10
% (4.2.22)..." n " Ly ra ngui trong bnh ht m n nhit phng, cn,
nung li nhit trn n khi thu c khi lng khng i."

22

TCVN : 2009
7.9.3 Tnh kt qu
Hm lng sunfua, tnh bng phn trm, theo cng thc:

% S2

0,1373 (A B)
100
m

Trong :
A l khi lng BaSO 4 tng ng vi lu hunh tng s xc nh theo 8.9, tnh bng gam;
B l khi lng BaSO 4 tng ng vi lu hunh dng sunfua xc nh theo 8.8, tnh bng
gam;
0,1373 l h s chuyn t BaSO 4 sang S2-;
m l khi lng mu ly phn tch, tnh bng gam;
Chnh lch gia hai kt qu xc nh song song khng ln hn 0,05 %.
7.10 Xc nh hm lng kali oxit (K2O) v natri oxit (Na2O) tng
Vin dn t mc 7.15 tiu chun TCVN 141: 2008
7.11 Xc nh hm lng titan oxit (TiO2)
Vin dn t mc 7.17 tiu chun TCVN 141: 2008
7.12 Xc nh hm lng mangan oxit (MnO)
Vin dn t mc 7.18 tiu chun TCVN 141: 2008

8. Bo co kt qu th nghim
Bo co kt qu th nghim bao gm t nht cc thng tin sau:
- Tn tiu chun p dng;
- Cc thng tin cn thit nhn bit mu th mt cch y ;
- Cc bc tin hnh th khc vi quy nh ca tiu chun ny (ghi r ti liu
vin dn);
- Cc kt qu th;
- Cc tnh hung c nh hng n kt qu th;
- Ngy, thng, nm tin hnh th nghim.
_________________________________

TCVN .. : 2009

Mc lc
Trang
1

Phm vi p dng.............................................................................................................. 5

2 Ti liu vin dn............................................................................................................. 5


3 Quy nh chung............................................................................................................. 5
4 Ho cht, Thuc th......................................................................................................... 6
4.1 Ho cht rn.............................................................................................................. 6
4.2 Ho cht lng, thuc th............................................................................................. 7
5

Thit b, dng c......................................................................................................... 10

Ly mu v chun b mu th..................................................................................... 11
6.1 Ly mu................................................................................................................... 11
6.2 Chun b mu th................................................................................................... 11

Phng php th............................................................................................................ 11


7.1 Xc nh hm lng m (W)..................................................................................... 11
7.2 Xc nh hm lng mt khi nung (MKN)................................................................12
7.3 Xc nh hm lng silic dioxit (SiO2)......................................................................14
7.3.1 Xc nh hm lng silic dioxit dng kt ta silisic (phng php khi lng)....14
7.3.2 Xc nh silic dioxit (SiO2) ha tan trong dung dch (phng php o mu). 15
7.3.3 Xc nh hm lng SiO2 tng..........................................................................16
7.4 Xc nh hm lng st (III) oxit (Fe2O3).................................................................16
7.4.1 Xc nh hm lng st (III) oxit theo phng php chun phc cht.........16
7.4.2 Xc nh hm lng st (III) oxit theo phng php o mu............................16
7.5 Xc nh hm lng nhm oxit (Al2O3).....................................................................17
7.6 Xc nh hm lng canxi oxit (CaO).......................................................................18
7.7 Xc nh hm lng magi oxit (MgO).....................................................................19
7.8

Xc nh hm lng anhydric sunfuric (SO3)..........................................................20

7.9

Xc nh hm lng sunfua (S2-)............................................................................. 21

7.10 Xc nh hm lng kali oxit (K2O) v natri oxit (Na2O) tng..................................22


7.11 Xc nh hm lng titan oxit (TiO2)........................................................................22
7.12 Xc nh hm lng mangan oxit (MnO)..................................................................22
8. Bo co kt qu th nghim.......................................................................................... 22
24

TCVN : 2009