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IS 1917-3 (1992): Chemical analysis of quartzite and high

silica sand, Part 3: Determination of silica [MTD 13: Ores
and Raw Materials]

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 IS 1917 ( Part 3 ) : 1992
(Reaffirmed 2005)

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Indian Standard
CHEMICAL ANALYSIS OF QUARTZITE
AND HIGH SILICASAND
PART 3 DETERMINATION OF SILICA

( First Revision )

UDC 553.57 : 553 [ 546.28 ]

@ BIS 1992

BUREAU OF INDIAN STANDARDS

MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

March 1992 Price Group 1

Methods of Chemical Analysis of Ores, Minerals and Allied Materials for Metallurgical Industry
Sectional Committee, MTD 29

FOREWORD
This Indian Standard ( Part 3 ) ( First Revision ) was adopted by the Bureau of Indian Standards,
after the draft finalized by the Methods of Chemical Analysis of Ores, Minerals and Allied
Materials for Metallurgical Industry Sectional Committee had been approved by the Metallur-
gical Engineering Division Council.
IS 1917 : 1962 <Methods of chemical analysis of quartzite and high silica sand’ covers the
methods for the determination of silica and other constituents of quartzite and high silica sand.
The committee decided to revise this standard into different parts and covering determination
of each element in a separate part, which on publication would supersede the determination of
that element given in IS 1917 : 1962. The determination of loss on ignition, silica, sodium,
potassium, aluminium, iron, calcium, magnesium and titanium oxide in quartzite and high silica
sand have been covered in this series.
This part covers the determination of silica. The other parts in this series are:
Part 1 Determination of loss on ignition
Part 2 Determination of sodium and potassium
Part 4 Determination of aluminium
Part 5 Determination of iron
Part 6 Determination of calcium and magnesium
Part 7 Determination of titania
In this revision the determination of total silica by gravimetric method has been replaced by
determination of major silica by gravimetric method and residual silica by photometric method.
In reporting the result of a test or analysis made in accordance with this standard, if the final
value, observed or calculated, is to be rounded off, it shall be done in accordance with
IS 2 : 1960 ‘Rules for rounding off numerical values ( revised)‘.
 Is I917 (Pqrt 3. ), : 1992

Indian Standard
CHEMICAL ANALYSIS OF QUARTZITE
AND HIGH SILICA SAND
PAfiT 3 DETERMINATION OF SILICA

( First Revision )
1 SCOPE acid. The silica is rendered insoluble through
dehydration and baking. The maior sX:a thus
: Ti%is standard ( Part 3 ) covers the methods obtained by filtration, is h3drofluorlsed and
for determination of silica in the range above determined by d;&rence. The residual silica is
.90 percent in quartzite and high silica sand. determined yhoto:netri~:aily and added to the
major silica to get ‘total silica.
2 REFERENCES
5.2 Reagents
The following Indian Standards are necessary
adjuncts to this standard. 5.2.1 Fusion Mixture
Mix 6 g of sodium carbonate with 4 g of
IS No. Title potassium carbonate.
1070 : 1977 Water for general laboratory
5.2.2 Dilute Sulphuric Acid, 1 : 1 ( v/v )
use ( second revision )
1811 : 1984 Methods of sampling foundry 5.2.3 Potassium Bisulphate, solid
sand ( jirst revision )
5.2.4 Dilute Hydrochlo7z Acid, 1 : 2 ( v/v )
2245 : 1962 Methods of sampling quartzite
5.2.5 Hydrojuoric Acid, 48 percent
3 SAMPLING
5.3 Procedure
3.1 The sample shall be drawn and prepared
5.3.1 Weigh accurately O-5 g of the finely ground
after quartering in accordance with IS 2245 :
test sample in a platinum crucible. Add 3 to 4 g
1962 or IS 1811 : 1984, as the case may be.
of anhydrous fusion mixture and mix thoroughly
3.2 Grind 3 to 5 g of the sample so that it with a platinum rod. Heat the crucible gently
passes through IS Test Sieve No. 15 ( 149 at first and finally at 950” to 1000°C for at least
microns ). Dry the sample in a weighing bottle half an hour with occasional swriling of the
at 105” to 110°C for 2 h. Keep the weighing melt with platinum tipped tongs to get a clear
bottle stoppered in a desiccator and cool to melt. Cool and observe that a transparent mass
room temperature. The sample is ready for is obtained. Place the crucible and the lid into
chemical analysis. a platinum dish containing 75 to 100 ml of
dilute hydrochloric acid ( 1 : 2 ) and 2 drops of
4 QUALITY OF REAGENTS dilute sulphuric acid ( 1 : 1 ). Cover the dish
with the watch glass. When the reaction
Unless specified otherwise, analytical grade ceases, wash the crucible and the lid thoroughly
reagents and distilled water ( see IS 1070 : 1977 ) with water. Evaporate the solution over a
shall be employed for the test. steam bath until the smell of hydrochloric acid
is no longer detected. Finally cover the dish
5 DETERMINATION OF MAJOR SILICA RY with the watch glass and bake the mass for an
hour in an air oven at 105” to 110°C. Cool and
GRAVIMETRIC METHOD
digest the contents of platinum dish with about
5.1 Outline of the Method 50 ml of dilute hydrochloric acid ( 1 : 2 ).
Filter through fine textured filter paper. Transfer
The sample is fused with fusion mixture and quantitatively all the residue by hot water to
the fused mass extracted with hydrochloric the filter paper. Wash the residue five times

1
IS 1917 ( Part 3 ) : 1992

with hot dilute hydrochloric acid ( 1 ; 20 ) and 6.2.2.2 Prepare a standard working solution
then with hot water until free from chloride. containing O-04 mg/mI of silica solution
Preserve the filtrate and washings ( Main filtrate immediateIy before use by diluting the above
A ) in a 500 ml beaker for the subsequent solution. Store in a high density poIythene
determination of residual silica by the bottle.
photometric method. 6.2.3 Ascorbic Acid Solufion, 10 percent ( mfv ).
5.3.2 Ignite the paper with the residue in a Store in an amber bottle ( stable up to 5 days ).
weighed platinum crucible raising the temper-
ature gradually and finally at 950” to 1000°C 6.2.4 Oxalic Acid Solution, 10 percent ( m/v ).
for 30 minutes. Cool in a desiccator and 6.2.5 EDTA Solution ( @OS M )
weigh. Moisten the residue with a few ml of
water, add 1 drop of dilute sulphuric acid and Dissolve 18.6 g of disodium saIt of EDTA in
10 ml of hydrofluoric acid. Keep the crucible water and dilute to 1 btre.
covered at room temperature for 10 minutes.
Then remove the lid and place the crucible on 6.3 Procedure
a sandbath for evaporation and continue up to 6.3.1 Fuse the residue as obtained under 5.3.2
copious fuming. Cool the crucible, add further with 1 g of potassium bisulphate. Dissolve the
5 ml of hydrofluoric acid and repeat the process. melt in water containing few drops of hydro-
Lastly, drive out all the acid to obtain a dry chloric acid. Add the solution to the main
residue. Finally, ignite the residue at 1000°C filtrate obtained as under 5.3.1. Cool and dilute
for 30 minutes. Repeat heating, cooling and to 500 ml in a volumetric flask. Take an aliquot
weighing until constant mass is obtained. of 10 ml into a 100 ml volumetric flask. Add 5 ml
of EDTA solution, a drop of phenolphthalein
.5.4 Calculation solution and then ammonia solution dropwise
-B until the colour changes to red. Add 10 ml of
Major silica, percent by mass=‘7 X 100
ammonium molybdate solution and allow to
where stand f;,r 10 minutes. Now add 5 ml of oxalic
acid followed by 5 ml of ascorbic acid and
A = mass in g, of impure silica, dilute to 100 ml. Allow the soIution to stand
B = mass in g, of residue after hydrofluori- for half an hour for development of full colour.
sation, and Measure the absorbance at 810 nm in 10 mm
cell against a test blank soIution prepared in
C = mass in g, of the sample taken. the same way, but without the sample. Compute
the silica content from the calibration curve.
6 DETERMINATION OF RESIDUAL SILICA
BY PHOTOMETRIC METHOD 6.4 Calibration

6.1 Outline of the Method 6.4.1 Establish a calibration curve by taking

0, 1, 2, 3, 4 and 5 ml of standard silica solution
Soluble silica is converted into heteropolysili- in 100 ml calibrated flasks. Carry out the entire
comolybdate by the addition of ammonmm stage of procedure as given in 6.3 without the
molybdate. The complex is reduced to molyb- main solution. Measure the absorbance of the
denum blue and measured at 810 nm. above aliquots against the reagents blank.
Draw a calibration curve by plotting absor-
6.2 Reagents bance against amount of silica in mg. Compare
6.2.1 Ammonium Molybdate Solution and convert the absorbance of the test solution
to the amount of silica with the help of the
Dissolve 10 g ammonium molybdate, in 100 ml calibration curve.
of water, filter, if necessary.
6.5 Calculation
6.2.2 Standard Silica Solution Residual silica, =fiZ, x 100
6.2.2.1 Fuse 0.2 g of powdered ( 200 mesh ) percent by mass M
and dried ( 105” to 110 C ) pure silica with 5 g where
of fusion mixture in a .platinum crucible. Cool
and dissolve the melt in 300 ml of water A~1 - mass in mg, of the residual sibca pre-
containing 2 g of sodium hydroxide in a sent in 10 ml aliquot of the main
polythene beaker. Warm the solution on a filtrate A ( 5.3.1 ), and
water bath and dilute to 500 ml in a volumetric M = mass in mg, of the sample represented
flask-. by the aliquot.

2
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Revision of Indian Standards

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Dot ; No MTD 29 ( 3809 )

Amendments Issued Since Publication

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