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Xc nh hm lng Fe2O3 v Al2O3 trong xi mng

NI DUNG

Tng quan v xi mng

S phn tch Fe2O3, Al2O3 trong xi mng

Xc nh hm lng Fe2O3 trong xi mng

Xc nh hm lng Al2O3 trong xi mng

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Xc nh hm lng Fe2O3 v Al2O3 trong xi mng

Tng quan v xi mng

Xi mng l mt cht kt dnh chu nc c kh nng ng rn trong mi trng khng kh v nc. Thnh phn ch yu gm CaO kt hp vi ba oxit chnh SiO2, Al2O3, Fe2O3 to thnh bn khong chnh
*

C3S (3CaO.SiO2)

C2S (2CaO.SiO2)

* C3A

(3CaO.Al2O3)

C4AF (4CaO.Al2O3.Fe2O3)
C3A > 1,5 C4AF C3A = 0,4 1,5 C4AF C3A < 0,4 C4AF

Da vo thnh phn khong C3A v C4AF, ta c Xi mng alumin: Xi mng pooc lng thng: Xi mng xlit:

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Xc nh hm lng Fe2O3 v Al2O3 trong xi mng

Tng quan v xi mng

Thnh phn ha hc xi mng Pooclng gm bn loi oxit ch yu

CaO : 63% - 67%

SiO2 : 21% - 24%

Al2O3 : 4 - 7%
Fe2O3 : 2,5 - 4%

Nguyn nhn gy cho xi mng km bn trong mi trng sunfat l C3A, do nhim v lc thit k phi liu, chun b dy chuyn k thut v nguyn liu sn xut ra clinker th lng C3A phi gim ti thiu v tng lng C4AF. P= Al2O3 =L Fe2O3
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Xc nh hm lng Fe2O3 v Al2O3 trong xi mng

S phn tch Al2O3 v Fe2O3 trong xi mng

Cn 1g 0.05g mu xi mng Nung vi K2CO3 + Na2CO3 Pha ph gia Khng pha ph gia Ha tan vi HCl + NH4Cl

C mu Lc mu SiO2 cha tinh khit c x l vi HF +H2SO4 Nung cn vi KHSO4 hoc K 2 S2 O 7 Nc lc vo bnh nh mc 500 ml dung dch A

25 ml. Xc nh Fe2O3 bng EDTA

100 ml loi canxi,magi, st, titan. nh mc 250 ml lc kh 100ml. Xc nh Al2O3 COMPANY bng Zn(CH COO) LOGO

Xc nh hm lng Fe2O3 trong xi mng

Xc nh hm lng Fe2O3 trong xi mng

1 2

Phng php chun phc cht Phng php chun oxi ha kh

Phng php trc quang vi thuc th SSA

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Xc nh hm lng Fe2O3 trong xi mng

Phng php chun phc cht (TCVN 141:2008)

Phm vi p dng Tiu chun ny quy nh phng php phn tch ha hc cho cc loi xi mng pooclng, clanhke xi mng pooclng. Tiu chun ny khng p dng cho clanhke v xi mng pooclng

cha Bari.
Nguyn tc Chun st (III) bng dung dch EDTA mi trng pH 1,5 n 1,8 vi ch th axit sunfosalixylic. Khi kt thc chun mu dung dch chuyn t tm sang vng rm.
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Xc nh hm lng Fe2O3 trong xi mng

Phng php chun phc cht

1 ml H2O2 30% 2ml axit sunfosalixylic 10% Nh t t HCl (1+1) v NaOH 10% iu chnh pH 1.5 -1.8

25 ml dung dch A

un si nh

Thm nc ct n 100ml

Chun bng EDTA 0.01M

un nng n 50 600C
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Xc nh hm lng Fe2O3 trong xi mng

Phng php chun phc cht

Phng trnh phn ng Phn ng chun : Phn ng ch th: Fe3+ + H2Y2- FeY- + 2H+

FeInd- + H2Y2- FeY- + H2In2-

Cc lu trong quy trnh

Chun st (III) bng dung dch EDTA mi trng pH 1,5

n 1,8 vi ch th SSA, n khi dung dch chuyn t tm sang vng rm (hay dung dch chuyn t mu cam sang

khng mu hoc mu vng nht).

Khi chnh pH c th dng dung dch NH3 m c v dung dch HCl (1:1).
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Xc nh hm lng Fe2O3 trong xi mng

Phng php chun phc cht

Cng thc tnh Hm lng st oxit (Fe2O3) tnh bng phn trm theo cng thc

% Fe2O3 =

0,0007985

100

V l th tch dung dch tiu chun EDTA 0,01M tiu th khi

chun , tnh bng mililit.

0,0007985 l khi lng Fe2O3 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 phn tch,

tnh bng gam. Chnh lch gia hai kt qu song song khng ln hn 0,15%.
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Xc nh hm lng Fe2O3 trong xi mng

Phng php chun oxi ha kh (TCVN 7947:2008)

Phm vi p dng

Phng php ny p dng cho mu c hm lng Fe2O3 ln

hn 2.5%. Nguyn tc Kh st Fe3+ trong dung dch n Fe2+ bng Sn2+ . Sau chun Fe2+ bng dung dch kalidicromat tiu chun vi ch

th baridiphenylamin sunfonat, kt thc chun khi dung

dch chuyn sang mu tm xanh.

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Xc nh hm lng Fe2O3 trong xi mng

Phng php chun oxi ha kh

Tng git SnCl2 Thm d 1 git SnCl2 5ml HgCl2

200 ml dung dch A

C cn dung dch n 25ml 30ml

Pha long n th tch 100ml 15ml hn hp H2SO4 + H3PO4 4-5 git bari diphenylamin sunfonat

Chun bng K2Cr2O7 0.05N

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Xc nh hm lng Fe2O3 trong xi mng

Phng php chun oxi ha kh

Phng trnh phn ng Kh trc Fe3+ Fe2+ bng SnCl2: 2Fe3+ + Sn2+ 2Fe2+ +Sn4+ Loi b lng d SnCl2 bng dung dch HgCl2 SnCl2 + 2HgCl2 Hg2Cl2 + SnCl4

Phn ng chun
6Fe2+ + Cr2O72- + 14H+ 6Fe3+ + 2Cr3+ + 7H2O Cc lu trong quy trnh

Phi chuyn Fe3+ Fe2+ bng SnCl2

Ch c php d rt t SnCl2
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Xc nh hm lng Fe2O3 trong xi mng

Phng php chun oxi ha kh

Cng thc tnh

Hm lng Fe2O3 tnh bng phn trm theo cng thc

% Fe2O3 =
0,0039925

100

0.0039925 l s gam Fe2O3 ng vi 1ml dung dch K2Cr2O7 0.05N. V l th tch dung dch K2Cr2O7 0.05N tiu th, tnh bng mililit. m l khi lng mu ly phn tch, tnh bng gam.

Chnh lch cho php gia hai kt qu xc nh song song 0,20%

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Phng php trc quang vi thuc th SSA (TCVN 7947:2008)

Phm vi p dng

Xc nh hm lng Fe2O3 trong xi mng

Phng php ny p dng cho mu c hm lng Fe2O3 2.5%

Nguyn tc Trong mi trng amoniac, ion Fe3+ to vi thuc th axit sunfosalixylic phc cht mu vng, c cc i hp thu ti bc sng = 420 nm 430 nm, cng mu ca phc t l vi nng Fe3+ c trong dung dch.

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Xc nh hm lng Fe2O3 trong xi mng

Phng php trc quang vi thuc th SSA

10 ml axit sunfosalixylic 10% Tng git amoniac Cho d 1ml amoniac

25 ml dung dch A

Bnh nh mc 100ml

Thm nc n th tch khong 50ml

nh mc thnh 100 ml, lc u

Sau 15 20 pht o quang bc sng 420 nm 430 nm

Tin hnh xy dng ng chun Fe2O3 nh vi mu. T mt quang ca mu v dy chun tnh ra hm lng Fe2O3 c trong mu.
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Xc nh hm lng Fe2O3 trong xi mng

Phng php trc quang vi thuc th SSA

Cng thc tnh Hm lng Fe2O3 tnh bng phn trm theo cng thc

% Fe2O3 =
Trong

100

l khi lng Fe2O3 tm c trn ng chun, tnh bng gam. l khi lng mu ly phn tch, tnh bng gam. Chnh lch cho php gia hai kt qu xc nh song song 0,05%

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Xc nh hm lng Al2O3 trong xi mng

Xc nh hm lng Al2O3 trong xi mng

Phng php chun phc cht

Phng php chun phc cht k thut chun thay th

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Xc nh hm lng Al2O3 trong xi mng

Phng php chun phc cht (TCVN 141:2008)

Nguyn tc Loi canxi v magie c trong dung dch bng cch dng NH4OH 25% kt ta nhm sau ha tan li kt ta bng HCl (1+1). Tch nhm ra khi cc nguyn t nh hng nh st, titan bng

kim mnh. To phc nhm vi EDTA d pH= 5,5. Chun

lng d EDTA bng Zn(CH3COO)2 vi ch th xylenol da cam. Dng natri florua gii phng EDTA khi phc complexonat nhm, dng dung dch tiu chun Zn(CH3COO)2 0,01 M chun lng EDTA c gii phng, t tnh ra hm lng nhm.
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Xc nh hm lng Al2O3 trong xi mng

Phng php chun phc cht

100 ml dd A 1-2 g NH4Cl Metyl Cho d 1 git NH4OH 25% Lc khi cn nng Khuy u Khuy u HCl v NaOH chnh pH = 7

un si nh Ra ta bng nc ct 2 3 ln. Ha tan ta bng HCl

15 ml dd m pH=5,5

Thm 20ml dd EDTA + 1-2 git PP

30 ml NaOH 30%

100 ml dung dch lc

nh mc thnh 250ml

un si ngui
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Xc nh hm lng Al2O3 trong xi mng

Phng php chun phc cht

Xylenol da cam 0.1% Zn(CH3COO)2 0,01M 10 ml NaF 3%

un nng n 800 C un si 3 pht Zn(CH3COO)2 0,01M

ngui n 70 -800 C
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Xc nh hm lng Al2O3 trong xi mng

Phng php chun phc cht

Phng trnh phn ng Loi canxi v magie: Al3+ + 3NH3 + 3H2O Al(OH)3 + 3NH4+

Al(OH)3 + 3HCl AlCl3 + 3H2O

To phc nhm vi EDTA d pH= 5,5 Al3+ + H2Y2- AlY- + 2H+ Phn ng chun Phn ng ch th Zn2+ + H2Y2- Zn2+ + H2Ind2- ZnY2- + 2H+ ZnIn2-

Cc lu trong quy trnh

Cn phi ra ta k n ht Cl- (th bng dung dch AgNO3)
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Xc nh hm lng Al2O3 trong xi mng

Phng php chun phc cht

Cng thc tnh Hm lng Al2O3 tnh bng phn trm theo cng thc % Al2O3 =
0,0005098

100

VZn l th tch dung dch tiu chun Zn(CH3COO)2 0.01 M tiu th khi

chun .
0.0005098 khi lng Al2O3 tng ng vi 1ml Zn(CH3COO)2 0.01M. K l h s nng gia dung dch Zn(CH3COO)2 0.01 M v dung dch

EDTA tiu chun 0.01 M.

m l khi lng mu tng ng vi th tch mu ly phn tch. Chnh lch cho php gia hai kt qu xc nh song song 0,15%
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Phng php chun phc cht - k thut chun thay th (TCVN 7947:2008)
Nguyn tc

Xc nh hm lng Al2O3 trong xi mng

Tch nhm khi cc thnh phn khc ri cho Al3+ to phc vi

EDTA d pH= 5,5. Chun lng d EDTA bng dung dch Zn(CH3COO)2 vi ch th xylenol da cam (ln th nht).

Cho NaF tc dng vi phc cht ca nhm y ra mt lng

EDTA tng ng vi nhm. Chun (ln th hai) lng EDTA b y ra bng dung dch Zn(CH3COO)2 tiu chun, t tnh ra hm lng nhm oxit c trong mu.

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Phng php chun phc cht - k thut chun thay th

1 -2 g NH4Cl Tng git NH4OH (1:1) 1-2 git HCl 30 ml (1:1) urotropin 30%

Xc nh hm lng Al2O3 trong xi mng

25 ml dd A un nng dung dch Nh t t HCl (1+1) v NaOH 10% 25 ml EDTA 1 % 2 git PP 0,1 % un nng dung dch n gn si

Ra bng nc nng

Ra cc v kt ta 5-7 ln bng urotropin 10%

Ha tan kt ta bng HCl (1:1)

Lc nng dung dch

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Phng php chun phc cht - k thut chun thay th

15 ml m acetat pH=5 Vi git XO

Xc nh hm lng Al2O3 trong xi mng

Zn(CH3COO)2 0,015M

un si 5 pht Zn(CH3COO)2 0,015M

ngui n nhit phng Vi git XO 15 ml NaF 3 %

un si 3 pht, ngui
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Phng php chun phc cht - k thut chun thay th

Phng trnh phn ng To phc nhm vi EDTA d pH= 5,5

Xc nh hm lng Al2O3 trong xi mng

Al3+ + H2Y2- AlY- + 2H+

Phn ng chun Phn ng ch th Zn2+ + H2Y2- Zn2+ + H2Ind2- mu vng ZnY2- + 2H+ ZnIn2mu hng tm

Cho NaF tc dng vi phc cht ca nhm y ra mt lng

EDTA tng ng vi nhm

AlY- + 6F- AlF63- + Y
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Phng php chun phc cht - k thut chun thay th

Cng thc tnh Hm lng Al2O3 tnh bng phn trm theo cng thc

Xc nh hm lng Al2O3 trong xi mng

% Al2O3 =

0,0007647

100

0,0007647 l s gam Al2O3 ng vi 1 ml Zn(CH3COO)2 0,015M VZn l th tch Zn(CH3COO)2 0,015M tiu th khi chun ln th hai. K l h s nng dung dch Zn(CH3COO)2 0,015M m l khi lng mu ly phn tch, tnh bng gam.

Chnh lch cho php gia hai kt qu xc nh song song

Khng ln hn 0,35% khi hm lng Al2O3 45% Khng ln hn 0,50% khi hm lng Al2O3 > 45%
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Xc nh hm lng Fe2O3 v Al2O3 trong xi mng

Tng kt
Xc nh hm lng Fe2O3 v Al2O3 trong xi mng

Xc nh hm lng Fe2O3
Phng php chun phc cht (TCVN 141:2008) Phng php chun oxi ha kh (TCVN 7947:2008) Phng php trc quang vi thuc th SSA (TCVN 7947:2008) Xc nh hm lng Al2O3

Phng php chun phc cht (TCVN 141:2008)

Phng php chun phc cht k thut chun thay th (TCVN 7947:2008)
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Cht cn xc nh

Phng php

Phm vi p dng Xi mng poc lng

Tng kt

Dung dch chun v Mu dung cht ch th dch Dung dch EDTA mi trng pH =1.51.8 vi ch th SSA

Xc nh hm lng Fe2O3 v Al2O3 trong xi mng

Cng thc tnh

Chun phc cht (TCVN 141:2008)

Dung dch chuyn t tm sang vng rm.

% Fe2O3 =

0,0007985

100

Fe2O3

Chun oxi ha kh (TCVN 7947:2008)

Xi mng alumin hm lng Fe2O3 > 2.5% Xi mng alumin hm lng Fe2O3 2.5 % Xi mng poc lng Xi mng alumin

Dung dch K2Cr2O7 vi ch th bari diphenylamin sunfonat

Mu tm xanh

% Fe2O3 =

0,0039925

100

Trc quang (TCVN 7947:2008) Chun phc cht (TCVN 141:2008) Al2O3 Chun thay th (TCVN 7947:2008)

Mi trng amoniac Fe3+ To vi SSA phc cht mu vng

Mu vng

% Fe2O3 =

100

to vi EDTA d pH =5,5. Chun lng d EDTA bng Zn2+vi ch th XO Al3+

Dung dch chuyn t vng sang hng tm

% Al2O3 =

0,0005098 100

% Al2O3 =

0,0007647 100

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Xc nh hm lng Fe2O3 v Al2O3 trong xi mng

Ti liu tham kho

1. Gio trnh phn tch cng nghip, Trng i hc Cng Nghip

Thnh ph H Ch Minh, 2009, (trang 47 - 50).

2. Bi ging mn ha k thut, i hc Nng. (trang 28-31). 3. Bi ging mn Ha k thut, Trng i hc Cng Nghip Thnh

ph H Ch Minh.
4. TCVN 141 : 2008 Xi mng poc lng. Phng php phn tch ha hc, (trang 18 - 19). 5. TCVN 7947 : 2008 Xi mng alumin. Phng php phn tch ha hc, (trang 15 - 18).
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