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IS 14212 (1995): Sodium, Potassium silicate - Method of

test [CHD 1: Inorganic Chemicals]

“!ान $ एक न' भारत का +नम-ण”

Satyanarayan Gangaram Pitroda
“Invent a New India Using Knowledge”

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है”
ह
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“Knowledge is such a treasure which cannot be stolen”
 IS14212:1995
( Reaffirmed 1999 )

Indian Standard

SODIUMANDPOTASSIUMSILICATES-
METHODSOFTEST

UDC 661*833*65 : 661,832.65,543

0 BIS 1995

BUREAU OF INDIAN STANDARDS

MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

July 1995 Price Group 5

- 1
General Inorganic Chemicals Sectional Committee, CHD 003

FOREWORD

This Indian Standard was adopted by the Bureau of Indian Standards, after the draft finalized by the
General Inorganic Chemicals Sectional Committee had been approved by the Chemical Division
Council.
Sodium and potassium silicates are among the most widely used raw materials in the chemical industry.
Sodium silicate is extensively used in soap and detergent, textile, pharamaceuticals and cement
industries.
This standard covers the methods of test for sodium and potassium silicates. This standard does not
deal with the material but prescribes the methods for determining whether they comply with the
requirements of individual standards. Specification for sodium silicate for use in pharmaceutical, toilet
preparations, soap, detergents, textile, welding electrode and cement industry is covered in IS 381 :
1972 ‘Sodium silicate (first revision )‘, whereas the specification for potassium silicate for use in
welding electrode industry is covered in IS 8813 : 1978 ‘Potassium silicate, technical’.
The committee responsible for the formulation of this standard is given at Annex B.
For the purpose of deciding whether a particular requirement of this standard is complied with, the final
value, observed or calculated, expressing the result of a test or analysis, shall be rounded off in accord-
ance with IS 2 : 1960 ‘Rules for rounding off numerical values ( revised)‘. The number of significant
places retained in the rounded off value should be the same as that of the specified value in this
standard.
 IS 14212: 1995

Indian Standard
SODIUM AND POTASSIUM SILICATES -
METHODS OF TEST
1 SCOPE IS No. Tille
I.1 This standard prescribes the methods of test 460 : 1985 Test sieves ( third revision )
for sodium and potassium silicates. 1070 : 1992 Reagent grade water ( third
2 REFERENCES revision )
4905 : 1968 Methods for random sampling
2.1 The Indian Standards listed below are
necessary adjuncts to this standard: 5717 : 1991 Pyknometers (first revision )

IS No. Title 3 METHODS OF TEST

264 : 1976 Nitric acid ( second revision ) 3.1 The methods of test for the determination
265 : 1993 Hydrochloric acid ( fourth of matter insoluble in water, relative density,
revision ) total soluble silica, total alkalinity, total
soluble silicates, loss in mass on ignition, iron
266 : 1993 Sulphuric acid ( third revision ) viscosity, chloride and sulphate are given in
323 : 1959 Rectified sprit Annex A.

ANNEX A
( Clause 3.1 )

METHODS OF TEST FOR SODIUM AND POTASSIUM SILICATES

A-l QUALITY OF REAGENTS 4 kg/ems. Filter and thoroughly wash the filter
paper with freshly boiled water. Transfer both
A-l.1 Unless otherwise specified, pure chemi- the filtrate and the washings to a 500-ml
cals and reagent grade water ( see IS 1070 : volumetric flask and dilute up to the mark.
1992 ) shall be used in tests. Keep this prepared sample solution for test
NOTE - ‘Pure chemicals’ shall mean chemicals that purposes.
do not contain impurities which affect the results of
analysis. A-2.2.2 Neutral Silicate
A-2 PREPARED SAMPLE SOLUTION Crush the material fine enough to pass through
150 micron IS Sieve ( see IS 460 : 1985 ). Digest
A-2.1 Sodium/Potassium Silicates, Liquid about 20 g of the crushed material, accurately
Weigh accurately about 20 g of the material weighed, with twice its weight of water in an
and dissolve in freshly boiled water. Filter and autoclave for 2 hours at a pressure of 4 kg/cm2
thoroughly wash the filter paper with freshly Filter and thoroughly wash the filter paper
boiled water. Transfer both the filtrate and with freshly boiled water. Transfer both filtrate
the washings to a 500-ml volumetric flask and and the washings to a 500-ml volumetric flask
dilute up to the mark. Keep this prepared and dilute up to the mark. Keep this prepared
sample solution for test purposes. sample solution for test purpose.
A-2.2 Sodium/Potassium Silicates, Solid A-3 DETERMINATION OF MATTER
INSOLUBLE IN WATER
NOTE - This material, especially the neutral type,
is very difficult to dissolve and the following A-3.1 Procedure
methods are recommended.
Weigh accurately about 25 g of the material into
A-2.2.1 Alkaline Silicate 400-ml beaker and dissolve in about 250 ml
Digest about 20 g of the material. accurately freshly boiled water ( for the material in the
weighed, with 10 times its weight of water in an solid form, prepare the solution
autoclave for two hours at a pressure of under A-2.2 ). Filter by applying suctiti

1
IS 14212 : 1995

through a tared Gooch crucible. Wash the A-5.2 Procedure

beaker and the residue free from alkali with
A-5.2.1 Clean and dry the pyknometer together
freshly boiled water ( no colour with phenol-
with its stopper and weigh to the nearest
phthalein ) and then dry the Gooch crucible in
O*OOl g. Fill the pyknometer with water boiled
an oven maintained at 110 f 5°C. Cool in a
and cooled to 27 * O*S’C and place it in the
desiccator and weigh. Repeat the operation of
till constant mass is water-bath controlled at 27 f 0.5”C. Allow at
heating and cooling
least 30 minutes for the temperature to reach
obtained.
eauilibrium and remove the Dvknometer from
A-3.2 Calculatiou tGe water-bath, holding it by <hk neck; stopper
it, wipe externally and remove the excess water
Matter insoluble in water, from the upper part of the stopper. Weigh the
percent by weight pyknometer and its stopper to the nearest
0.001 g and determine by difference, the mass
where of the water that it contains.

M, = mass in g of the residue, and A-5.2.2 Empty the pyknometer, rinse it with
alcohol or acetone and allow it to dry. Fill it
MS= mass in g of the material taken for
with the sample previously adjtisted to
the test.
27 f 0*5”C, avoiding the formation of air
A-4 DETERMINATION OF SPECIFIC bubbles, especially when the solution has a
GRAVITY high viscosity. Place the pyknometer in the
water-bath at 27 f 0.5%. Allow at least
A-4.1 Apparatus 30 minutes for the temperature lo reach
equilibrium and weigh as in A-5.2.1.
Specific gravity shall be determined with a
NOTE - If, during the procedure, the pyknometer
Twoddell hydrometer. is externaliy soiled by the solution under test, it
should be washed with water at a temperature
A-4.2 Procedure slightly below 27°C and then wiped.
Pour the material to be tested into the clean
hydrometer jar, the diameter of which shall be A-5.3 Calculation
at least 2.5 cm greater than the diameter of the
Relative density, 27127°C = -z- x d
hydrometer used. Remove all air bubbles that
might have formed in the liquid. Keep the jar
where
in a vertical position and in a bath maintained
at 15~5°C. When the sample in the jar attains M1 = mass in g of the sample,
the temperature of the bath, that is, 15.5”C,
lower the hydrometer gently into the material. M = mass in g of the same volume of
When it has settled, depress it about two scale water, and
divisions into the liquid. Keep the unimmersed d= density of water at 27°C.
portion of the stem dry, as any unnecessary
liquid on the stem will change the effective A-6 DETERMINATION OF TOTAL
weight of the instrument and affect the reading SOLUBLE SILICA ( as SiO, )
obtained. Allow the hydrometer to become ( GRAVIMETRIC METHOD )
stationary. Remove all air bubbles that might
have formed during the lowering of the hydro- A-6.1 Reagents
meter. Read the point on the hydrometer A-6.1.1 Concentrated Hydrochloric Acid - See
scale, to which the sample rises, with the eye IS 265 : 1993.
placed at the principle surface of the material.
This reading gives the specific gravity of the A$;;;: Dilute Hydrochloric Acid - 1 : 1 by
material under test.

A-5 RELATIVE DENSITY A-6.1.3 Concentrated Sulphuric Acid - See

IS 266 : 1993.
A-5.1 Apparatus
A-6.1.4 HydroJuoric Acid - about 40 percent
A-5.1.1 Wide Neck Pyknometer ( m/v ).
The channel of the stopper not being a capillary A-6.2 Procedure
tube ( see Types 5 and 6 of IS 5717 : 1991 ).
Take 25 ml ( corresponding to approximately
A-5.1.2 waler Btith -maintained at 27 f 1 g of test sample ) of the test solution
0.5%. ( see A-2 ) and place in a porcelain dish of
 IS 14212:199s

suitable capacity. Carefully add, while stirring, A-6.3 Calculation

5 ml of the hydrochloric acid solution, Cover
the dish with a watch-glass supported by a The silica content, expressed as a percentage
glass triangle and place it on a boiling water by mass of SiO,, is given by the formula:
bath and evaporate to dryness. Heat the residue
in the oven controlled at 110 to 120°C for at ( m, - ma ) x -J$-
least 1 hour. After cooling, add 5 ml of the
hydro-chloric acid solution and 10 ml of water. where
Place on the boiling water bath for 5 to 10 m, is the mass, in grams, of test portion
minutes and stir to dissolve the soluble salts. contained in the volume of the solution
Filter through an ashless lilter paper of medium used;
porosity, and collect the filtrate quantitatively.
Transfer the insoluble product quantitatively m, is the mass, in grams, of the crucible
on to the filter by means of hot water. Wash containing the insoluble product
with hot water, adding the rinsing water to the before the treatment with hydrofluoric
filtrate. Continue washing until 10 ml of filtrate acid; and
from the funnel remain clear 5 min, after the
ma is the mass, in grams, of the crucible
addition of 10 ml of the solution of silver
after the treatment with hydrofluoric
nitrate. ( Discard this portion of the filtrate ).
acid.

A-6.2.1 Transfer the filtrate and the rinsing
water quantitatively into the dish already used
and evaporate to dryness on a boiling water
bath. Heat the residue in the oven at 110 to
120°C for at least 1 hour. After cooling, add
5 ml of the hydrochloric acid solution and
10 ml of water. Place on the boiling water bath
for 5 to 10 min and stir in order to dissolve
the soluble salts. Filter and wash the insoluble
matter on another filter paper by following the
procedure given above for the first filtration.
A-6.2.2 Fold the filter papers containing the
insoluble matter as obtained in A-6.2
and A-6.2.1 and place them in the platinum cruci-
ble. Dry in the oven controlled at 100 to 105”C,
then ignite the paper tiith a low flame until the
combustion stops. Allow to cool, and wet the
residue with a few drops of the sulphuric acid
solution. Place the crucible and its contents on
a hot plate and evaporate the sulphuric acid.
When the emission of white fumes has ceased,
place the crucible in the furnace, controlled at
950 to 975°C for 15 min in order to calcine its
contents. Allow to cool in a desiccator to
ambient temperature and weigh to the nearest
0~000 2 g.
A-6.2.3 Wet the residue with a few drops of the
sulphuric acid solution and add, with care,
2 to 3 ml of the hydrofluoric a.cid solution.
Heat gently on a hot plate in order to volatilize
the hydrofluoric acid and heat more strongly
in order to evaporate the sulphuric acid. If any
residue remains in the crucible, repeat the
treatment with the sulphuric and hydrofluoric
acids. Finally, calcine in the furnace control-
led at 950 to 975°C for 15 min. allow to cool in
a desiccator to ambient temperature and weigh
to the nearest O-090 2 g.
A-7 DETERMINATION OF TOTAL
ALKALINlTY ( as M,O )
A-7.1 The principle of the method is based on
titration of the total alkalinity of a test portion
with a standard volumetric solution of hydro-
chloric acid, in the presence of methyl orange
as indicator.
A-7.2 Method A
A-1.2.t Reagents
During the analysis, use only reagents of
recognized analytical grade and only distilled
water or water of equivalent purity.
a) Hydrochloric acid, 1 N standard volumetric
solution.
b) Methyl orange , O-5 g/l solution.
NOTE - The methyl orange may be replaced by any
other indicator having the end-point in the same
pH range.
A-7.2.2 Procedure
Weigh, to the nearest 0.01 g, 10 f 1 g of the
test sample. Place the test portion in a 2%ml
one-mark volumetric flask, dissolve with water,
dilute to the mark and mix. Take a volume of
the sample solution such that the volume of the
standard volumetric hydrochloric acid solution
required to neutralize it is about 20 ml. Add
5 drops of the methyl orange solution and
titrate with the standard volumetric hydro-
chloric acid solution until the indicator changes
from yellow to orange-pink.
A-7.2.3 Calculation
The total alkalinity, expressed as a percentage
by mass of sodium oxide (Na,O ) or of
potassium oxide ( K,O ), as appropriate, is
given by the formulae:

3
IS 14212 : 1995

Sodium oxide ( in the case of sodium silicates ) A-10.2 Calculation

y&!?!L X 0*0310 =3.10 x $ LOSS in weight on ignition,
m percent by mass = 100 X !!!
Potassium oxide ( in the case of potassium
silicates ) where
100 M = mass in g of the material taken for
VX- X 0.047 1 = 4.71 x -+ the test, and
m
MI = mass in g of the residue after ignition.
where
A-11 DETERMINATION OF IRON ( as Fe )
V is the volume, in millilitres, of the
standard volumetric hydrochloric acid A-11.1 Apparatus
solution used for the titration; A-11.1.1 Nessler Cylinders - 50 ml capacity.
m is the mass, in grams, of the test A-11.2 Reagents
portion ( or the mass, in grams, of test
portion contained in the aliquot part of A-11.2.1 Concentrated Nitric Acid - See IS 264:
the test solution used ); 1976.
A-11.2.2 Ammonium Persulphate - solid.
0.031 0 is the mass, in grams, of sodium
oxide corresponding to 1 ml of exactly 1 A-11.2.3 Butanolic Potassium Thiocyanate
N hydrochloric acid solution;
Dissolve 10 g of potassium thiocyanate in 10 ml
0.047 1 is the mass, in grams, of potassium of water. Add sufficient n-butanol to make up
oxide corresponding to 1 ml of exactly 1 to 100 ml and shake vigorously until the solution
N hydrochloric acid solution. is clear.
NOTE - If the concentration of the standard volu- A-11.2.4 Dilute Sulphuric Acid - approximately
metric solution used is not exactly as specified in the
list of reagents, an appropriate correction shall be 10 percent ( v/v ).
made. A-11.2.5 Standard Iron Solution
A-8 DETERMINATION OF TOTAL Weigh 0.702 g of ferrous ammonium sulphate
SOLUBLE SILICATES [ F&Ok ( NH, ),SO,*6H,O ] and dissolve in
A-8.1 Determine total soluble silica and total 10 ml of dilute sulphurlc acid. Dilute with
alkalinity as given under A-6 and A-7 respecti- water to make up the volume to 1 000 ml.
Transfer 10 ml of this solution and again dilute
vely, and add the percentage of these two
with water to make up the volume to 100 ml.
compo nents to obtain the percentage by weight
One millilitre of this solution is equivalent to
of total soluble silicates.
O-01 mg of iron ( as Fe ).
A-9 DETERMINATION OF RATIO OF A-l 1.3 Procedure
TOTAL ALKALINITY ( AS M,O ) TO TOTAL
SOLUBLE SILICA ( as SiO, ) Take about 5 g of the sample accurately
weighed, dissolve it in water as prescribed
A-9.1 Determine total soluble silica and total in A-2 and make up the solution to exactly
alkalinity as in A-6 and A-7 respectively and 100 ml. Take 10 ml aliquot of this solution, add
find out the ratio of these two components. 1 ml of concentrated nitric acid and boil. Cool,
This ratio also gives the molar ratio in case of transfer the solution to a Nessler cylinder
sodium silicate. Multiply the mass ratio by and add 30 mg of ammonium persulphate
1.567 to obtain molar ratio in the case of and 15 ml of butanolic potassium thiocyanate
Potassium Silicate. solution. Shake for 30 seconds and allow the
A-10 DETRMINATION OF LOSS IN MASS liquid to separate. Carry out a control test in
ON IGNITION the other Nessler cylinder, adding slowly from
a burette a quantity of the standard iron’
A-10.1 Procedure solution in place of the material and the same
quantities of other reagents in the same total
Weigh accurately about 5 g of the material into volume of the reaction mixture until the colours
a clean tared platinum crucible. Heat the of butanol layers in the two cylinders are
crucible with a low flame until the material exactly matched.
melts. Increase the heat gradually as water is A-l 1.4 Calculation
driven off, taking care to aviod sputtering.
Continue heating till constant weight is obtai- 0.001 v
Iron ( as Fe ), percent by weight = - M
ed. Cool in a desiccator and weigh.

4
 IS 14212 : 1995

where A-13.2.3 Ethanol - approximately 95 percent

( v/v ), see IS 323 : 1959.
Y = volume in ml of standard iron solution
required in the control test, and A-13.2.4 Ethanol - approximately 50 percent
( V/V ) which may be denatured with ether.
M = mass in g of the material present in
the aliquot of prepared sample A-13.2.5 Standard Hydrochloric Acid -- 1 N.
solution. Acid -
A-13.2.6 Hydrochloric approximately
A-12 DETERMINATION OF VISCOSITY 0.1 N solution.
A-13.2.7 Standard Sodium Hydroxide Solution -
A-12.1 Apparatus
1 N.
A-12.1.1 Torsion Viscometer A-13.2.8 iLlethyl Red - 1 g/l solution in 95 per-
The instrument is based on the principle that cent ( v/v ) ethanol.
the torque exerted by a liquid is proportional
to its viscosity. It consists of two cylinders. The A-13.3 Procedure
outer cylinder is connected to a motor and the
inner one is suspended from a torsion spring, A-13.3.1 Blank Test
fitted with a pointer for measuring the torque.
Place in a 250 ml conical flask, 70 ml of water,
A-l 2.2 Procedure 5 ml of the sodium hydroxide solution and
0.30 ml of the methyl red solution. Add, by
Meintain the outer water jacketed cylinder at a means of a graduated pipette, approximately
temperature of 20°C. Place the sample in the 4.5 ml of the hydrochloric acid solution
annular space between the two cylinders. ( A-13.2.5 ) and neutralize with hydrochloric
Revolve the outer cylinder at a constant speed acid solution ( A-13.2.6 ) until the colour of
by the electric motor attached to it. The force the indicator turns from yellow to red. Then
transmitted through the sample exerts a torque add 5 f 0.1 g of the sodium fluoride to
on the inner cylinder. Read the torsion on the the solution thus neutralized. Stir to aid
scale attached to the spindle which is calibrated dissolution of this product, then add a precisely
in terms of viscosity. Report the result in measured volume ( Vs ) of the hydrochloric
centipoises at 20°C. acid solution ( A-13.2.5 ) corresponding to an
A-13 ALTERNATE METHOD FOR excess of about 5 ml after the colour changes to
DETERMINATION OF SILICA CONTENT red. Then add 50 ml of the ethanol ( A-13.2.3 ),
( TITRIMETRIC METHOD ) stir for about 1 min, transfer quantitatively to
a 200-ml one-mark volumetric flask, dilute to
A-13.1 Principle the mark with ethanol ( A-13.2.4 ) and mix.
Neutralization of the alkalinity of a test Filter a little more than 100 ml on a folded,
dry, close grained filter, discarding the first few
portion, previously dissolved, with methyl red
millilitres. Take 100.0 ml of the filtrate and
as indicator. Addition of sodium flouride,
place in a 250-ml conical flask; add 0.30 ml of
which reacts with the silicic acid, forming an
the methyl red solution and titrate the excess
equivalent quantity of sodium hydroxide.
of acid with the sodium hydroxide solution
Addition of a measured volume of standard
( A-13.2.7 ), contained in the burette, until the
volumetric hydrochloric acid solution in excess,
colour changes from red to yellow.
followed by ethanol. Filtration of the silicic
compound thus obtained, which is insoluble A-13.3.2 Determination
under these conditions. Titration of the excess
of acid in the filtrate with standard volumetric Weigh, to the nearest 0.1 mg, a quantity of
sodium hydroxide so!ution with methyl red as laboratory sample corresponding to 2.0 f 0.3 g
indicator. of SiOB and place the test portion in a 250 ml
one-mark volumetric flask, if necessary, dissol-
A-13.1.1 Reactions , ving it in water, dilute to the mark and mix.
H,SiOa + 6 NaF + Hz0 --+ Na,SiFe + 4 NaOH Take 5@0 ml of this solution immediately
NaOH + HCI --f NaCl -t H,O and place in a 250-ml conical flask. Add
0.30 ml of the methyl red solution. Neutralize
A-13.2 Reagents with the hydrochloric acid solution ( A-13.2.5 )
the total alkalinity less about 1 mg equivalent
A-13.2.1 Distilled water or water of equivalent ( if necessary, carry out a preliminary titration
purity shall be used in the test. of this alkalinity on another 50 ml sample ) and
A-13.2.2 Sodium Fluoride - anhydrous, heated neutralize with hydrochloric acid solution
at 600°C and cooled in a desiccator. ( A-13.2.6 ) until the colour of the indicator
IS 14212:1995

changes from yellow to red. Then add to the A-14.2 Reagents

neutralized product 5 f 0.1 g of the sodium
fluoride. Stir to aid dissolution of this product The following reagents are required and shall
and then add a precisely measured volume (V,) be of reccgnized analytical quality. Water
of the hydrochloric acid solution ( A-13.2.5 ) complying with the requirements of
corresponding to an excess of about 5 ml after IS 1070 : 1960 shall be used throughout.
the colour changes to red. Add 50 ml of the A-14.2.1 Nitrobenzene
‘ethanol ( A-13.2.3 ), stir for about 1 min, trans-
fer to a 200-ml one-mark volumetric flask, WARNING - Serious risk of poisoning by
dilute to the mark with the ethanol ( A-13.2.4 ) inhalation, swallowing or skin contact.
and mix. Avoid breathing vapour. Prevent contact
with skin and eyes.
Filter a little more than 100 ml on a folded,
dry, close grained filter, discarding the first few A-14.2.2 Nitric acid, approximately 5 N solution.
millilitres. Take 100.0 ml of the filtrate and A-14.2.3 Silver nitrate, O-1 N standard volu-
place in a 250-ml conical flask; add 0.30 ml of metric solution.
the methyl red solution and titrate the excess
of acid with the sodium hydroxide solution A-14.2.4 Ammonium thiocyanate, 0 1 N stan-
( A-13.2.7 ) contained in the burette until the dard volumetric solution.
colour changes from red to yellow. A-14.2.5 Ammonium iron ( III ) sulphate
A-13.4 Calculation indicator solution, 100 g/l. Dissolve 25 g of
ammonium iron ( III ) sulphate in 250 ml of
Silica content is given, as a percentage by mass, water. Allow the solution to settle and decant,
by the formula: if necessrry. If the solution is still not clear,
add a few drops of approximately 5 N nitric
[ Y, - 2V, ) - ( VIJ - 2V, ) ] x o-015 02 X
acid solution.
250
__ ~ 100
50x m A-14.3 Procedure
Weigh, to the nearest O-1 g: 10 g of the sample.
= [ ( VI - 2V, ) - ( Vs - 2V, )] x F Transfer to a 500-ml stoppered flask. Add
250 ml of water and 25 ml of the nitric acid
where solution. Prepare a blank solution from 250 ml
Vl is the volume, in millilitres, of the hydro- of water and 25 ml of the nitric acid solution
chloric acid solution ( A-13.2.5 ) added in a second, similar flask. To each flask, add
for the determination (A-13.3.2 ); 10 ml of the silver nitrate solution from a
pipette, followed by 2 ml of the nitrobenzene
V!2is the volume, in millilitres, of the
and 1 ml of the ammonium iron ( III ) sulphate
sodium hydroxide solution ( A-13.2.7 )
used for the back titration in the deter- indicator solution. Stopper the flasks and shake
mination; them for about 30 s. Titrate the blank solution
with the ammonium thiocyanate solution until
VB is the volume, in millilitres, of the hydro- a faint pink brown colour just persists through.
chloric acid solution ( A-13.2.5 ) added out the solution. Similarly, titrate the test
for the blank test; solution to a matching end-point.
v4 is the volume, in mill:litres, of the sodium A-14.4 Calculation
hydroxide solution used for the back
titration in the blank test; The chloride content, expressed as a percentage
by mass of sodium chloride ( NaCl ), is given
O-015 02 is the mass, in grams, of SiO, by the formula:
corresponding to 1 ml of the hydrochloric
acid solution; and ( VI - V, x 0.005 8 x 100
10
m is the mass, in grams, of the test portion.
= ( VI - V, ) x 0.058
A-14 DETERMINATION OF CHLORIDE where
CONTENT
Vl is the volume of the ammonium thiocya-
A-14.1 Principle nate solution required for the blank test,
in ml;
A solution of the test portion is mixed with
silver nitrate solution and the excess of silver VZ is the volume of the ammonium thiocya-
nate solution required for the test
nitrate is titrated with ammonium thiocyanate solution, in ml; and
solution using ammonium iron ( III ) sulphate
solution as indicator. 10 is the mass of the test portion, in g.

6
 IS 14212’: 1995

A-15 DETERMINATION OF SULPHATE chloric acid solution and add an excess of 25 ml

CONTENT of this acid. Boil for 2 min. turn off the heat
and add very slowly, while stirring, 50 ml of
A-15.1 Principle
the barium chloride solution.
Dissolution of a test portion, either directly or
Rinse down the internal walls of the beaker
after alkaline fusion, depending on whether the
with about 20 ml of water, without stirring, so
product is readily or sparingly soluble in water
as to maintain a layer of water on the liquid
respectively. Separation of the insoluble matter.
surface and thus prevent solids climbing up the
Precipitation while boiling, of the sulphate ions
walls during heating. Cover the beaker with a
in the form of barium sulphate, in an acid
watch glzss and allow to stand for 2 h on a
medium. Filtration, washing and calcination of
boiling water bath and then for 24 h at room
the precipitate. Weighing of the barium sulphate
after treatment with hydrofluoric acid in order
temperature. Filter the precipitate through an
to remove any silica which may be present.
ash-free fine grade filter paper B42. Wash the
filter paper and precipitate with boiling water
A-l 5.2 Reagents until 10 ml of the liquid passing through the
filter remains clear for 5 min after the addition
During the analysis, use only reagents of of 10 ml of the silver nitrate solution. If
recognized analytical reagent grade and only
chloride ion is detected, the precipitate should
distilled water or water of equivalent purity.
be washed a further two or three times with
A-15.2.1 Hydrochloric acid, approximately 2N small quantities of water until the chloride ion
soluticn. has completely disappeared from the wash
water. Place the filter paper and precipitate
A-15.2.2 Sulphuric acid, P approximately carefully in the crucible, previously heated to
1.84 g/ml, about 96 percent ( m/m ) solution or red heat, cooled in the desiccator and weighed
approximately 36 N. to the nearest, 0.1 mg. Place the crucible and
A-15.2.3 Hydrofiuoric acid, P approximately, its contents in the oven, controlled at
1.15 g/ml, about 40 percent ( m/m ) solution. 110 st 2”C, until completely dry.

A-15.2 4 Barium chloride, approximately 1N Char the filter paper in air, at a low tempera-
solution. Dissolve 122 g of barium chloride ture, then calcine at red heat for 15 min using
dihydrate ( BaC1,.2H,O) in a I 000 ml one-mark Maker Burner.
volumetric flask, dilute to the mark and mix. After cooling, add a few drops of the sulphuric
A-15.2.5 Silver nitrate, 5 g/l solution in Nitric acid solution and 5 ml of the hydrofluoric acid
Acid. solution. Evaporate to dryness on an air bath
or hot-plate, then calcine again for 15 min,
A-15.2.6 Methyl orange, 0.5 g/l solution. under the same conditions as before.
A-15.2.7 Potassium Sodium Carbonate Allow to cool in the desiccator to room tempe-
( KNuC03 ) - Having a maximum sulphate con- rature and weigh to nearest O*l mg.
tent of 0.005 percent ( m/m ). 1 percent NOTE - The filtration of the harium sulphnte pre-
solution in water. cipitate can be accelerated by first lining the filter
with ash-free cellulose powder.
A-15.3 Procedure
A-15.5 Calculation
Weigh, to the nearest 0.01 g, a quantity of test
sample equal to 10 g of liquid product. In a The sulphntes content, expressed as a percen-
1 000 ml beaker, dilute it with 200 ml of water tage by mass of sulphate ( SO1 ), is given by the
and allow to stand for 1 h. Ifthe resultant formula:
solution is clear, dilute it to 400 ml and proceed
as specified in A-15.4. If the resultant solution nTi,
” x 0.411 57 x “0 - --41.157 ml
is turbid, filter it and then wash the filter paper m0 m0
five times with potassium sodium carbonate
( A-15.2.7 ) solution, heated to approximately where
7O”C, collecting the filtrate and washings in a mO is the mass, in grams; of the test portion
second 1 000 ml beaker. Dilute to 400 ml and ( A-15.3 );
then proceed as in A-15.4.
ml is 11le mass, in gram?, of barium sulphate
A-15.4 Determination precipitate weighed; and
Add 5 drops of the methyl ornng~ soluiion to 0.41 I 57 is Ihe Conversion factor from
the test solution, neutralize it with 11~chydro- 13aSO., tq so,.

7
IS 14212: 1995

ANNEX B
( Foreword )
COMMITTEE COMPOSITION
General Inorganic Chemicals Sectional Committee, CHD 003

Chairman Representing
DR M. S. VAIDYA The Dharamsi Morarji Chemical Co Ltd, Amhernath
Members
( Alternate to
SHRI R. S. VYA~
Dr M. S. Vaidya )
SERI B. M. Ac~cawa~ Central Glass and Ceramics Research Institute, Calcutta
Da S. K. ROY ( Alternate )
DR A. N. BHAT Hindustan Lever Ltd, Bombay
Dn S. N. K. CHAUDEARI ( Alternate )
DR N, RAVI BIUJSHAN Bharat Electronics Ltd, Bangalore
DAR.M. BWATNAQAR projects and Drvelopment India Ltd, Sindri
SHllIR. M.CURSETJI The Associated Cement Companies Ltd, Bombay
SHRI C. H. Paon ( Alternate )
SHRIA.K.DASGUPTA Deepak Nitriee Ltd, Vadodara
Sau D. P. GUPTA (Alternate )
SHltIA.K.DAs Indian Oxygen Ltd, Crlcutta
SHRI P.R. DESAI Sarabbai RI. Chemicals, Vadodara
DR A. N. Soar ( Alternate )
SHRIS.K.DJWAN Federation of Associations of Small Industries of India, New Delhi
DIRECTOR(CRPY) Development Commissioner ( SSI ), New Delhi
SHRI R. MUKHOPADHYAY ( Alternafe )
DR P. C. GUPTA Indian ( hemicals Manufacturers’ Association, Calcutta
SHRI S. C. GULATI Oil and Natural Gas Commission, Debra Dun
DR S.H.IQ~AL National Chemical Laboratory, Pune
DRC. GOPJNATHAN( Alternate)
DR Morn ZAFAR JAWL Indian Institute of Chemical Technology, Hyderabad
SHIII P.JOYKUMAI~AN Directorate General of Supplies and Disposals. New Delhi
SHRI N. K. KAU~HAL ( Alternafc )
SURI P.Mazr~~an National Test House, Calcutta
SHRI B. M. SOOI, ( Alternate )
SHRIA.K.MEHRA Shriram Foods and Fertilizers Industries, New Delhi
SBRI S. 1..DEWAN ( Alternate )
Pnor P. NATARAJAN Central Salt and Marine Chemicals Research Institute, Bhavnagar
Dn 0. K. SRIVASTAVA (Alternate)
SRRl ‘1‘. c. Pz4TEL Tata Chemicals Ltd, Bombay
Die Ii. C. PATRAK ( Altertratd)
SHRI P.G. PRADHAN Golden Chemicals Ltd, Bomhav
SHRI P. I. BIJAGAT ( Alternate )
SHRI G.M. RAO Indian Bureau of Mines, Nagpur
SHRI S. R. BHAISARE (Afternate)
DR S. S. RATHI Ministry of Defence ’ DGQA )
SHRI P. Das ( Alternate )
DRS.K.KAPOOR Ministry of Defence ( R & D )
DR R. K SBTHI ( Alternate)
SHRI C.R.SANT!TANAXRISHNAN Travancore Chemicals & Mfg Co Ltd, Mettur Dam
SHIII R. V. MANI ( AItewafe )
Snnr R. C. SHAI~MA Director‘ite General of Technical Development, New Delhi
SHRI A. K. CHATTIERJEE (Alternate)
SHRI L. B. SHI{IVASTAVA Shriram Instittue for Industrial Research, Delhi
SHRI V. K. VEITMA ( dlternofe)
SERI V. B.Soi-41 Union Carbide of India Ltd, Bombay
SHRI V. K.CHAKRAWARTY (Alternate )
SHXI YUnHlSTIllR Geological Survey of India, Calcutta
DR K. N. MATHUR ( Alrernate)
DR R.K SINGH, Director General, BIS ( Ex-officio Member )
Director ( Chem )

Member Secretory
DR R. K. JHA
Deputy Director (Chem ),BIS

( Continued on page 9 )

8
 IS 14212: 1995

Continued from page 8 )

Composition of Minerals for Chemicals and Allied Industries

Subcommittee, CHD 003 : 04

Convener Representing
%~uIV.B. SON1 Electrolytic Mangane Company, Division of Union Carbide of
Indian Ltd, Thane
Members
Sanr A. K. CHAKRAVARTS ( Alternate to Electrolytic Mangane Company, Division of Union Carbide of
Shri V. B. Soni ) India Ltd Thane
SHRI B. H. PATEL Deepak Nitiite Ltd, Vadodara
SHRI H. li. SHAH ( Alternate )
REPRESENTATIVE Development Commissioner, Small Scale Industries, New Delhi
REPRESENTATIVE Geological Survey of India, Calcutta
SHRS S. S. SINGEANIA Indian Council of Small Industries, Calcutta
Smr B. L. KANODIA ( Altcrnutc)
DR P. G. PRADHAN Golden Chemicals Pvt Ltd, Bombay
SHIZI P. I. BHAGAT ( Ahrnatc )
DR H. C. SHAH 3 K Chemicals Company, Thane
SHRIMATI K. H. SEAH ( Alternate)
DE R. M. BHATNAQAH Projects and DevrlopmFnt India Ltd, Sindri
SHRI B. MUKEIERJBB ( Alternate )
SHRI S. BALASUBRAIANIAN Tamil Nadu Chemicals Products Ltd, Madras
SHRI K. SUBRAHANIAN ( Alternate )
Snrtr P. c. GoPlNATtIAN The Travancore-Cochin Chemicals Ltd, Udyogamandal
SRRI K. NAFUBOOWIIRI ( Alternate )
SHRI S. K. BARAT Waldies Ltd, Calcutta
SHRI S, BANERJEE ( Altern&)

9
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