Determination of major oxide in clinker By EDTA methods

Silica:
Perchloric Methods:
1) 0! "m sam#le in !0 ml $eaker %! ml #erchloric acid &mix to
homo"eno's)
() )eat on hot #late 'ntil *hite f'me s'$sides
+) ,ool the $eaker add (0 ml D-% 1 ml ,onc),l % (.+ dro#s
)/0+% di"est
for 10 min'tes
1) 2'rther dil'te the a$o3e sol'tion $y addin" 10.1! ml distilled *ater
!) 2ilter the sol'tion
4) 2iltrate 'se for 2e(0+5Al(0+5,a0 6 M"0 determination
7) P#t i"nited in Pt cr'ci$le 8 to kno* the silica content
/ote: Determination of silica can $e done $y 's'al method
,ollect the filtrate and *ashin" in a (!0 ml 3ol'metric flask
2e 0
( +
1) (! ml sol'tion %&1:4) /)10) sol'tion till t'r$idity a##ears
() ,lear the t'r$idity *ith minimal dil )cl&1:10)6 add fe* dro#s extra
to
mention #) 1.1!5 shake *ell %add 100 m" of s'l#hosalicylic acid and
titrate *ith 001M EDTA till a colorless or #ale yello* sol'tion a##ears
1 ml of 001M EDTA 9 07:;! m" 2e(0+
< 2e(0+ 9 07:! x = > *
=9 =ol'me of EDTA 'sed
- 9 -ei"ht of sam#le
Al(0+: 2e 0 5 add 1! ml excess EDTA 1)To the conical flask after determination of
( +
%1 ml )+P01 &1:+)%! ml )(S01&1:+) %1 dro# of thymol $l'e
Add ammoni'm acetate sol'tion $y stirrin" 'ntil color chan"es
from () red to yello*
Then 5add (! ml excess ammoni'm acetate to o$tain #) aro'nd
!!.
+)
40
)eat the sol'tion for 1 min'tes to $oilin" %cool the sol'tion 1)
Add !0ml solid xylenol oran"e indicator % Bism'th nitrate
sol'tion
!)
slo*ly till col'r chan"es from yello* to ?ed Add 1.( ml Bism'th
nitrate in excess
Titrate a"ainst 001 M EDTA 5 to chan"e shar#ly yello* from ?ed 4)
1 ml of 001 EDTA 9 0!0:; m" Al(0+
< Al(0+ 9 0!0:; x= > *
-here = 9 =1.=!.&=+ xE)
= 9 3ol'me of EDTA for al'mina in ml
=1 9 total 3ol'me of EDTA 'sed in titration in ml
=(9 =ol'me of EDTA 'sed in determination of 2e(0+
=+9 Total 3ol'me of $ism'th nitrate 'sed in titration in ml
- 9 *ei"ht of am#le in "ms
E 9 E@'i3alence of 1 ml Bism'th nitrate sol'tion
Bism'th nitrate sol'tion to a !00 ml conical flask /ote : E@'i3alence of
and dil'te *ith a$o't 100 ml distilled *aterAdd a fe* dro#s of
thymol $l'e sol'tion 6 ammoni'm aceate sol'tion 'ntil colo'r
chan"es from red to yello* Add !0ml solid xylenol oran"e
indicator
% 01M EDTA sol'tion slo*ly till col'r chan"es from ?ed to
yello*
E 9 =1>-1
=! 9=ol'me of EDTA 'sed
- 1 9 =ol'me of Bism'th nitrate sol'tion 'sed
,a0:
1) 10 ml sol'tion in (!0 ml conical flask %! ml 11 "lycerol %1 ml
triethanol amine %10ml 1 / /a0)%!0ml D- % !0m" P6 ? indicator () Titrate a"ainst 001EDTA sol'tion 5 from *ine red to $l'e 1 ml of 001M EDTA 9 0!40; m" ,a0 ,a0 < 9 0!40; x (! x= >-

= 9 =ol'me of EDTA 'sed
- 9 -ei"ht of sam#le in "ms
M"0
1) Meas're 10 ml of sol'tion in (!0 ml conical flask 5add ! ml of &1:1)
trienthonal amine% (0 ml of ammonia $'ffer
() Add !0 ml of thymol#hathaleone indicator follo*ed $y f'rther
addition of !0
ml distilled *ater
+) Titrate a"ainst 001 M EDTA to o$tain $l'e to #ink
1 ml of 001M EDTA 9 0010+("ms of M"0
M"0 < 9 010+( x (! x&=1. =) >-
= 9 =ol'me of EDTA 'sedin ,ao determination
=193ol'me of EDTA 'sed
- 9 -ei"ht of sam#le in "ms
Sol'tions
ammonium acetate : !0< sol'tion Bismuth Nitrate : *ei"ht 1 "ms in !00 ml $eaker % (0 ml acetic acid %*ater to dil'te % make '# 1 A
Thymol $l'e &01<) 8 Dissol3e 01 "ms Thymol $l'e indicator in
100 ml ethyl alcohol

Thymol#hthalexone . "rind 100m" of indicator *ith 10 "ms Pot
/itrate
Bylenol oran"e : 100 m" indicator in 10 "ms Pot /itrate
A ) Standard Cinc sol'tion : Dissol3e acc'rately *ei"ht 04+7 "ms
"ran'lated
Dinc in minimal @'antity of 1:1 ),l %make '# to 1000 ml
B) Standard Disodi'm acetic acid 8 dissol3e +7((1 "ms %
dissol3e in 100
ml D- 5 later make '#to 1 litre
StandardiDation of EDTA &001M )
Pi#ette o't 10 ml of standard Cinc sol'tion%10.1! ml $'ffer
sol'tion of #) 10
and *arm to !0.40 o, % 3ery small @'ality of EBT and titrate
a"ainst 001M
EDTA till *ine red to $l'e
,alc'latation
Molarity of EDTA 9 001 x 10 >=ol of EDTA 'sed
2actor for EDTA 9 Present molarity >?e@'ired Molarity