Professional Documents
Culture Documents
Is 14212 1995 PDF
Is 14212 1995 PDF
Indian Standard
SODIUMANDPOTASSIUMSILICATES-
METHODSOFTEST
0 BIS 1995
- 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 )
ANNEX A
( Clause 3.1 )
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
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-6.2.1 Transfer the filtrate and the rinsing A-7 DETERMINATION OF TOTAL
water quantitatively into the dish already used ALKALINlTY ( as M,O )
and evaporate to dryness on a boiling water
bath. Heat the residue in the oven at 110 to A-7.1 The principle of the method is based on
120°C for at least 1 hour. After cooling, add titration of the total alkalinity of a test portion
5 ml of the hydrochloric acid solution and with a standard volumetric solution of hydro-
10 ml of water. Place on the boiling water bath chloric acid, in the presence of methyl orange
for 5 to 10 min and stir in order to dissolve as indicator.
the soluble salts. Filter and wash the insoluble A-7.2 Method A
matter on another filter paper by following the
procedure given above for the first filtration. A-1.2.t Reagents
During the analysis, use only reagents of
A-6.2.2 Fold the filter papers containing the recognized analytical grade and only distilled
insoluble matter as obtained in A-6.2 water or water of equivalent purity.
and A-6.2.1 and place them in the platinum cruci- a) Hydrochloric acid, 1 N standard volumetric
ble. Dry in the oven controlled at 100 to 105”C, solution.
then ignite the paper tiith a low flame until the
combustion stops. Allow to cool, and wet the b) Methyl orange , O-5 g/l solution.
residue with a few drops of the sulphuric acid NOTE - The methyl orange may be replaced by any
solution. Place the crucible and its contents on other indicator having the end-point in the same
a hot plate and evaporate the sulphuric acid. pH range.
When the emission of white fumes has ceased, A-7.2.2 Procedure
place the crucible in the furnace, controlled at
950 to 975°C for 15 min in order to calcine its Weigh, to the nearest 0.01 g, 10 f 1 g of the
contents. Allow to cool in a desiccator to test sample. Place the test portion in a 2%ml
ambient temperature and weigh to the nearest one-mark volumetric flask, dissolve with water,
0~000 2 g. dilute to the mark and mix. Take a volume of
the sample solution such that the volume of the
A-6.2.3 Wet the residue with a few drops of the standard volumetric hydrochloric acid solution
sulphuric acid solution and add, with care, required to neutralize it is about 20 ml. Add
2 to 3 ml of the hydrofluoric a.cid solution. 5 drops of the methyl orange solution and
Heat gently on a hot plate in order to volatilize titrate with the standard volumetric hydro-
the hydrofluoric acid and heat more strongly chloric acid solution until the indicator changes
in order to evaporate the sulphuric acid. If any from yellow to orange-pink.
residue remains in the crucible, repeat the A-7.2.3 Calculation
treatment with the sulphuric and hydrofluoric
acids. Finally, calcine in the furnace control- The total alkalinity, expressed as a percentage
led at 950 to 975°C for 15 min. allow to cool in by mass of sodium oxide (Na,O ) or of
a desiccator to ambient temperature and weigh potassium oxide ( K,O ), as appropriate, is
to the nearest O-090 2 g. given by the formulae:
3
IS 14212 : 1995
4
IS 14212 : 1995
6
IS 14212’: 1995
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
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
Boreao of Indian Standards
BIS is a statutory institution established under the Bureau of Indian Standards Act, 1986 to promote
harmonious development of the activities of standardization, marking and quality certification of goods
and attending to connected matters in the country.
Copyright
BIS has the copyright of all its publications. No part of these publications may be reproduced in any
form without the prior permission in writing of BIS. This does not preclude the free use, in the course
of implementing the standard, of necessary details, such as symbols and sizes, type or grade
designations. Enquiries relating to copyright be addressed to the Director ( Publications ), BIS.
Amendments are issued to standards as the need arises on the basis of comments. Standards are also
reviewed periodically; a standard along with amendments is reaffirmed when such review indicates that
no changes are needed; if the review indicates that changes are needed, it is taken up for revision.
Users of Indian Standards should ascertain that they are in possession of the latest amendments or
edition.
This Indian Standard has been developed from Dot No: CHD 3 (0183).
Headquarters:
Manak Bhavan, 9 Bahadur Shah Zafar Marg, New Delhi 110002 Telegrams : Manaksanstha
Telephones : 331 01 31, 331 13 75 ( Common to all offices )