SILICA

1) Transfer 0.5 gms of the sample into a 100 ml beaker,moisten with

10 ml of distilled water at room temperature to prevent lumping ,
add 10 ml of hydrochloric acid, and digest with the aid of gentle
heat and agitation until the sample is completely dissolved.
2) Dissolution may be aided by light pressure with the flattened end
of a glass rod.
3) Evaporate the solution to dryness on a stream bath.
4) Without heating the residue any further treat it with 5 to 10 ml of
hydrochloric acid and then,equal amount of water, or pour at once
upon the residue 10 ml to 20 ml of hydrochloric acid (1:1).
5) Then cover the beaker and digest for 10 minute on the water bat or
hot plate.
6) Dilute the solution with the equal volume of hot water immediately
filter through an ashless filter paper ( Whatman No.40 or its
equivalent ), and wash the separated silica (SiO2) ,thoroughly with
hot water and reserve the residue.
7) Again evaporate the filtrate to dryness baking the residue in an
oven for one hour at 105 -110 oC
8) Then treat the residue with 10 -15 ml of hydrochloric acid (1:1)
and heat the solution on water bath or hot plate.
9) Dilute the solution with equal of hot water catch and wash the
small amount of silica it contains on other filter paper.
10) Reserve the filtrate and washing for the determination of combined
alumina and ferric acid.
11) Transfer the paper containing the residues to weighed platinum crucible
12) Dry and ignite the papers, first at a low heat untill the carbon of the filter
paper is completely consumed without inflaming , and finally at 1100 to
1200 deg.C until weight remains constant.
13) Treat the ignited residue thus obtained ,which will contain small amount
impurities , with 1 to 2 ml of distilled water, about 10 ml of HF and 2
drops of sulphuric acid and evaporate cautiously to dryness.
14) Finally heat the small residue at 1050oC to 1100oC for a minute or two ,
cool and weigh.
15) The difference between the weight and the weight of ignite sample
represents the amount of silica
Silica percent = 200 ( w 1 w2)
W1= weight of silica +(insoluble residue)
W2 = weight of impurities.

FERRIC OXIDE
To the amount of silica , add the amount of silica recovered from the residue
derived from the combined precipitates of alumina and ferric acid , as under
1) Add 0.5 of sodium or potassium persulphate to the crucible and heat
until the small residue of impurities is dissolved in the melt.
2) Cool and dissolve the fused mass in water and add it to the filtrate and
washing reserved for the determination of the combined alumina and
ferric oxide.
3) The mix filtrate make up the volume in a 250 ml volumetric flask.
4) Take 25 ml of solution above, add dilute Ammonium hydroxide (1:6) till
turbidity appears.
5) Clear the turbidity with minimum amount of dilute hydrochloric acid
(1:10) and add a few drops in excess to adjust the pH to approximately 1
to 1.5 .
6) Shake well.
7) Then , add 100 mg of sulphosalicyclic acid and titrate with 0.01 M
EDTA ,solution carefully to a colorless or pale yellow solution.
Calculation Calculate the percentage of Fe2O3 , as below
1 ml of 0.01 M EDTA = 0.7985 mg of Fe2O3
Fe2O3) % = 0.7985 x Volume of EDTA used in ml,
Weight of the sample in gms.

ALUMINA
8) Add 15 ml EDTA solution ,followed by 1 ml H3PO4 (1:3) , 5ml of
sulphuric acid (1:3) and one drop of thymol blue into the titration flask .
9) Add ammonium acetate solution by stirring until the colour changes
from red to yellow.
10) Add 25 ml of ammonium acetate in excess to obtain pH approximately 6.
11) Heat the solution to xylenol orange boiling for one minute and then cool.
12) Add 50 mg of the solid indicator and bismuth nitrate solution slowly
with stirring until the colour of the solution changes from yellow to red.
Add 2 to3 ml of bismuth nitrate solution in excess .Titrate with 0.01 M
EDTA solution to a sharp yellow end point red colour.
Calculation:Calculate the % of Al2O3 as below
V= V1 V2-(V3XE)
Where
V =Volume of EDTA for alumina in ml.
V1 = total volume of EDTA used in the titration.
V2 = Volume of the EDTA used in the IRON in ml.
V3 = Total volume of the bismuth nitrate solution used in the titration in
ml, and
E =equivalence of 1 ml of bismuth nitrate solution
1 ml of 0.01M EDTA = 0.5098mg of the Al2O3
Aluminium oxide (Al2O3) % = 0.5098 x Calculated Volume/Wt. ,,,,,
Note equivalence of bismuth solution is obtained as follows
Transfer 25 ml of bismuth nitrate solution to a 500 ml flask and dilute
with about 100 ml of distilles water .add a few drops of thymol blue

solution and ammonium acetate solution until the colur change from red
to yellow.The equivalence ( ml of the EDTA ) of 1ml od bismuth nitrate is
calculate as follow
E = Volume of the EDTA solution in ml./25

CALCIUM OXIDE
1) Take 10 ml of the solution reserved in a 250 ml conical flask .
2) Add 5 ml of 1: 1 glyerol with constant stiring and 5 ml of TEA
3) To the above add 10 ml of 4N NaOH solution and shake well to adjust
pH to highly alkaline range of 12 or slightly more.
4) Add approximately 50 ml of distilled water and 50 mg of solid PattonReeders indicator.
5) Titrate against 0.01 M EDTA solution to a sharp change in colour
from wine red to clear blue.
Notes Mangnase interfers with the estimation of CaO.In presence of
manganese,the alternate procedure specified
CALCULATION
1ml of the 0.01 M EDTA=0.5608 mg of CaO
CaO % =Volume of EDTA in ml x 25 x 0.5608
Weight of the sample

MAGNESIA
1) Take 10 ml of solution in 250 ml conical flask.
2) Add 5 ml of TEA (1:1) and 20 ml of buffer solution pH 10.
3) Add approx. 50 ml of EBT indicator
4) Followed by 50ml distilled water
5) titrate against 0.01M EDTA, untill blue to clear Pink.
6) This titration gives the sum of calcium and magnesium oxide
present in the solution.
7) Titre value of Magnesium oxide is obtained by subtracting the titre
value of CaO from Total titre value.
Note ;- take 10 ml solution , initially add 1ml less than titre value of
CaO, followed by step 3 to 7, this will correct results.

CALCULATION

1ml of the 0.01 M EDTA=0.4032 mg of MgO

MgO % =Volume of EDTA in ml(total titre value titre value of CaO) x
25 x 0.4032 divide by Weight of the sample