( Reaffirmed 1994 )
IS t 58 - 1976
Indian Standard
SPECIFICATION FOR LITHARGE
( First Revision )
Raw Materials for Paint Industry Sectional Committee, CDC 50
Chairman Representing
DR R. J. RATHI Sudarshan Chemical Industries Ltd, Pune
Members
SHRI K. L. Rathi ( Alternate to
Dr R.J. RATHI)
SIXRIS.K. ABTHALNA Ministry of Defence ( DGI )
SERI S. PANDEY ( Alternate )
S-1 C. J. BHUMKAR Asian Paints ( India ) Ltd, Bombay
SHEI G. C. DESAI Goodlass Nerolac Paints Ltd, Bombay
SERI S. H. DESAI Blundell Eomite Paints Ltd, Bombay
SHRI R. R. SEQTJEIRA( Alternate )
SHRI G.S. GILL Indian Paint Association, Calcutta
DR P. K. BHANDAI~I( Alternate )
JOINT DIRECTOR ( M & C ) Railway Board ( Ministry of Railways )
ASSISTANT RESEARCH OFFICER
SHBI d C$E;~;~,~~~;MtC )
Colour-Chem Ltd, Bombay
SHI& i. M. TILLU ( A&mate )
SHBI T. K S. MANI Addisons Paints & Chemicals Ltd, Madras; and
Paints & Allied Products Sectional Committee,
CDC 8, ISI
SHRI M. B. SATYANARAYANA ( Alternate )
SHRI V. M. NAOHANE Chowgule & Co ( Hind ) Pvt Ltd, Bombay
DR V. S. VIJAYAN NAYAB Travancore Titanium Products Ltd, Trivandrum
SIIRIB. K. NEHETE Jenson & Nicholson ( India ) Ltd, Calcutta
SHRI V. C. PANCIHAYIYA Kamani Metallic Oxides Pvt Ltd, Bombay
DR B. SANYAL Ministry of Defence ( R & D )
SERI K. K. CHOUDHRY ( Alternate)
SHRI P. SATYANAEAYANAN The Development Commissioner, Small Scale
Industries, New Delhi
SHRI K. C. SEAL National Test House, Calcutta
SHRI K. N. R. SH~SMA Directorate General of Technical Development,
New Delhi
SHRI KTJLTARSINQH (Alternate)
( Continued on page 2 )
@ Copyright 1976
INDIAN STANDARDS INSTITUTION
This publication is protected under the Z&an Copyright Act (XIV of 1957) and
reproduction in whole or in part by any means except with written permission of the
publisher shall be deemed to be an infringement of copyright under the said Act*
ISrSS-1976
( Continued from page 1 )
Members Representing
SHRI P. K. SHUNGLU The State Trading Corporation of India Ltd, New
Delhi
SHRI Y. S. SWAMY The Alkali and Chemical Corporation of India Ltd,
Calcutta
SHRI S. BHATTA~HARYA ( Alternate )
SHRI K. S. THAPKAR Hindustan Petroleum Corporation Ltd, Bombay
DR M. K. UNNI National Chemical Laboratory ( CSIR ), Pune
DR A. S. RAO ( Alternate )
DR G. M. SAXENA, Director General, IS1 ( Ex-o&i0 Member )
Director ( Chem )
Secretary
SHRI R. K. SINUH
Assistant Director ( Cbem ), IS1
Pigments and Extenders Subcommittee, CDC 50 : 1
Convener
SHRI K. C. SEAL National Test House, Calcutta
Members
SHRI S. K. ASTHANA Ministry of Defence ( DGI )
SHRI S. PANDEY ( Alternate )
SHRI SUEESH Boaa British Paints ( India) Ltd, Calcutta
SHRI S. H. DESAI Blundell Eomite Paints Ltd, Bombay
SHRI J. N. GHOSAL Sturdia Chemicals Ltd, Bombay
SHRI H. S. VIJAYANATH ( Alternate)
SHRI M. M. GHOEIH Shalimar Paints Ltd, Calcutta
SHRI P. N. KHANNA Asian Paints ( India ) Ltd, Bombay
SHEI K. V. KRISHNAN Colour-Chem Ltd, Bombay
SHRI R. M. TILLU ( Alternate )
SHRI V. C. PANOHAMIYA Kamani Metallic Oxides Pvt Ltd, Bombay
SHRI K. L. RATHI Sudarshan Chemical Industries Ltd, Pune
REPRESENTATIVE Goodlass Nerolac Paints Ltd, Bombay
Ad hoc Panel of Bombay Region, CDC 50 : P 1
Convener
SHRI S. H. DESAI Blundell Eomite Paints Ltd, Bombay
Members
SHRI C. J. BHUMKAR Asian Paints ( India) Ltd, Bombay
SHRI G. C. DESAI Goodlass Nerolac Paints Ltd, Bombay
SHRI K. L. RATHI Sudarshan Chemical Industries Ltd, Pune
SHRI R. M. TILLU Colour-Chem Ltd, Bombay
2
IS:58-1976
Indian Standard
SPECIFICATION FOR LITHARGE
( First Revision)
0. FOREWORD
0.1This Indian Standard (First Revision ) was adopted by the Indian
Standards Institution on 20 September 1976, after the draft finalized by the
Raw Materials for Paint Industry Sectional Committee had been approved
by the Chemical Division Council.
0.2 This standard was first published in 1950 largely based on the interim
co-ordinated draft prepared by the Standing Committee on Specifications
for Paints and Allied Stores of the General Headquarters, India ( now
Army Headquarters ),
0.3 In this revision which has been based on the recommendations of an
ad hoc panel constituted by the concerned Sectional Committee, a require-
ment for colour has been introduced. For analysis of litharge a volumetric
method has been prescribed in place of gravimetric method prescribed
earlier. In addition, EDTA method has been included for routine analysis
of litharge. Amendment No. 1 of January 1962 issued to this standard has
been incorporated and the title of the standard has been simplified in this
revision.
0.4 This standard contains clause 4.1 which calls for agreement between the
purchaser and the supplier.
0.5 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 accordance with
IS : 2-1960*. The number of significant places retained in the rounded off
value should be the same as that of the specified value in this standard.
1.SCOPE
1.1 This standard prescribes requirements and the methods of sampling and
test for the material commercially known as litharge, intended for the use
in the manufacture of paints and-pigments.
*Rules for rounding off numerical values ( revised ).
3
18:58.1976
2. TERMINOLOGY
2.1 For the purpose of this standard, the definitions given under 2 of
IS : 33-1976* shall apply.
3. REQUIREMENTS
3.1 Form and Condition - The material shall be supplied in the form of
dry powder or in such condition that it can be reduced to the powder form
by crushing, without grinding action, under a palette knife.
tzbzh;: material shall also conform to the requirements prescribed in
TABLE 1 REQUIREMENTS FOR LITHARGE
CHARA~ERISTICI REQUIRE- METHOD OB TEST,
&. REF TO CL No. IN
r-----h_-,
Appendix IS : 33-1976*
(1) (2) (3) (4) (5)
4 Volatile matter, percent by 0.2 - 7
mass, Max
ii) Rezis;eM;; sieve, percent by 0.5 - a
iii) Co*our’ Approximate match - 10
to canary yellow
iv) Litharge, as lead monoxide 99.5 A -
( PbO ), percent by mass, Min
v) Matter insoluble in acetic acid, 0.2 B -
percent by mass, Max
*Methods of sampling and test for inorganic pigments and extenders for paints
( second revision ) .
4. PACKING AND MARRING
4.1 Packing - The material shall be packed in suitable containers as
agreed to between the purchaser and the supplier.
4.2 Marking - The containers shall be marked with the following
particulars:
a) Name of the material;
b) Manufacturer’s name or his recognized trade-mark, if any;
*Methods of sampling and test for inorganic pigments and extenders for paints
( second revision ) .
4
IS t 58 - 1976
c) Mass of the material;
d) Batch number or lot number in code or otherwise; and
e) Date of manufacture.
4.2.1 Each container shall also be marked ‘Lead Pigment’ in letters not
less than 25 mm high.
4.2.2 The containers may also be marked with the IS1 Certification
Mark.
NOTE- The use of the IS1 Certification Mark is governed by the provisions of
the Indian Standards Institution (Certification Marks) Act and the Rules and
Regulations made thereunder. The IS1 Mark on products covered by an Indian
Standard conveys the assurance that they have been produced to comply with the
requirements of that standard under a well-defined system of inspection, testing and
quality control which is devised and supervised by IS1 and operated by the producer.
IS1 marked products are also continuously checked by IS1 for conformity to that
standard as a further safeguard. Details of conditions under which a licence for the
use of the IS1 Certification Mark may be granted to manufacturers or processors, may
be obtained from the Indian Standards Institution.
5. SAMPLING
5.1 Representative samples of the material shall be drawn as prescribed
in 4 of IS : 33-1976*.
6. TEST METHODS
6.1 Tests shall be carried out as prescribed in IS : 33-1976* and Appendices
A and B of this standard. Reference to relevant clauses of IS : 33-1976*
is given in co1 4 of Table 1.
6.2 Quality of Reagents - Unless specified otherwise, pure chemicals and
distilled water ( see IS : 1070-1960t ) shall be employed in tests.
NOTE -’ Pure chemicals ’ shall mean chemicals that do not contain impurities
which affect the results of analysis.
7. CRITERIA FOR CONFORMITY
7.1 A lot shall be declared as conforming to the requirements of this
standard if the test results of the composite sample satisfy the requirements
prescribed under 3.
*Methods of sampling and test for inorganic pigments and extenders for paints
( second revision ).
@pecification for water, distilled quality ( revised ).
5
IS:58-1976
APPENDIX A
[ Table 1, Item ( iv )]
DETERMINATION OF LITHARGE CONTENT
A-O.GENERAL
A-0.1 The percentage of litharge ( as PbO ) shall be determined by either
volumetric or EDTA method. The former method shall be used as a
referee method and the latter for routine analysis,
A-l. VOLUMETRIC METHOD
A-l.1 Reagents
A-1.1.1 Dilute Sulphuric Acid - prepared by diluting 50 ml of concentra-
ted sulphuric acid in a litre of water.
A-1.1.2 Ammonium Acetate Solution - 20 percent ( m/v) .
A-1.1.3 Acetic Acid Solution - 1 : 2 ( v/v ).
A-1.1.4 Potassium Chromate Solution - 4 percent ( m/v).
A-1.1.5 Sodium Acetate Solution - 1 percent ( m/v ).
A-1.1.6 Hydrochloric Acid Solution - 1 : 1 ( v/v ).
A-1.1.7 Potassium Iodide - pure.
A-1.1.8 Sodium Thiosulphate Solution - 0’1 N.
A-1.1-9 Starch Solution - 0’5 percent ( m/v) approximately.
A-l.2 Procedure -Weigh accurately about 0’3 g of the sample and
transfer to a 250-ml beaker. Add 60 to 70 ml of dilute sulphuric acid and
break up agglomerated particles by stirring well with a glass rod. Boil for
2 to 3 minutes taking care to prevent bumping and wash down the sides of the
beaker with about 25 to 30 ml of water. Cool the beaker for 1 hour in ice
cold water ( or allow it to stand overnight ). Then filter the residue through
sintered glass crucible ( No. 4) or Gooch crucible. Transfer the residue to
the crucible and wash it with 10 ml of cold water twice. Keep this residue
under slow suction with hot ammonium acetate solution ( 5 times ) taking
10 ml each time. Wash with 5 ml of acetic acid solution twice and then
2 to 3 times with water. ( The Gooch crucible along with the residue, if
any, should be preserved for examination. ) Transfer the combined filtrate
into the same beaker and make the volume of the solution to about 150 ml
with water and boil the solution. Add drop by drop 10 ml of potassium
6
IS:58-1976
chromate solution, stirring constantly with a glass rod. Boil for 5 to 10
minutes taking care to prevent bumping and then place the beaker on water-
bath for about 30 minutes. Filter the lead chromate precipitate on sintered
glass crucible ( No. 4 ). Transfer the precipitate to the crucible and wash
with sodium acetate solution till it is free from soluble chromate. After
cooling dissolve lead chromate in about 20 ml of cold hydrochloric acid.
This 20 ml of hydrochloric acid solution should be added in 3 instahnents
( 10, 5 and 5 ml ) under slow suction. Then wash the crucible 3 to 4 times
with cold water. Transfer the solution to the same beaker and adjust the
volume with water to about 150 to 200 ml. Add 2 g of potassium iodide
and titrate the liberated iodine with standard sodium thiosulphate solution
using starch as indicator.
NOTE-Lead chromate may also be filtered over a small filter paper ( Whatman
No. 30 ), the precipitate along with the filter paper transferred to the beaker and
treated with 20 ml of hydrochloric acid solution for titration.
A-l.3 Calculation
Litharge content ( expressed as PbO ), = V x Jv x 0.007 43 x 100
percent by mass M
where
V = volume in ml of standard sodium thiosulphate solution used,
Jv = normality of standard sodium thiosulphate solution used,
and
M = mass of the pigment taken for analysis.
A-2. EDTA METHOD
A-2.1 Reagents
A-2.1.1 Standard zinc Sulphate Solution - 0’02 M.
A-2.1.2 Ethylene Diamine Tetra Acetate ( EDTA ) Solution- 0.02 M.
A-2.1.3 Bufer Solution - Prepare by dissolving 30 g of ammonium
chloride in 300 ml of water and add 250 ml of ammonia and mix.
A-2.1.4 Erichrome Black T (EBT ) Indicator-Dissolve 0.2 g of EBT
powder in 15 ml of triethanolamine and add 5 ml of ethyl alcohol.
A-2.1.5 Double Distilled Water
A-2.1.6 Acetic Acid- 5 percent solution.
A-2.2 Procedure - Weigh accurately about 0’4 to 0.5 g of the sample in
a 100 ml beaker. Add 50 ml of acetic acid and dissolve it completely by
slight warming on water-bath. Make volume to 500 ml. Take 25 ml of
the diluted solution. Add 50 ml of EDTA solution, 50 ml of double distilled
7
IS : 58 - 1976
water and 2 ml of buffer solution ( PH should be adjusted to 10 ), Then
titrate against standard zinc sulphate solution using two drops of EBT
indicator. At the end point the colour changes from wine red to sky blue.
Take one blank reading using all the reagents but excluding the sample.
A-2.3 Calculation
Litharge ( as PbO ), = (B - I’) x Jv x 11’16 x 2
percent by mass M
where
B - volume in ml of standard zinc sulphate solution used in
blank titration,
V = volume in ml of standard zinc sulphate solution used in
titration with sample,
.N = normality of standard zinc sulphate solution used, and
M - mass in g of the sample used,
APPENDIX B
[ Tabte 1, Item ( v ) ]
DETERMINATION OF MATTBR INSOLUBLE IN ACETIC ACID
B-l. PROCEDURE
B-l.1 Stir 50 g of the material with 400 ml of hot water to which 50 ml of
glacial acetic acid has been added. Heat the mixture nearly to boiling,
allow it to settle, filter through a tared filter paper, dry the filter paper at
110 f 5°C weigh to constant mass and calculate the matter insoluble in
acetic acid.
NOTIU -Constant mass may be deemed to have been attained when the change
in mass of dried filter paper which has been redried for at least 30 minutes does not
exceed by O*OOO 5 g.
