IS 57 : 1989

Indian Standard ( Reaffirmed 1994 )

REDLEADFORPAINTSANDOTHER
-.
4'; PURPOSES-SPECIFICATION
.,
.a
(Second Revfsfon )

UDC 667’622’353

.-• .
, 1
\
._’

..”

I-\
\’ :
l _’ @ BIS 1990

BUREAU OF INDIAN STANDARDS

MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002
March 1990 Price Group 3
Raw Materials for Paint Industry Sectional Committee, CDC 50

FOREWORD

This Indian Standard ( Second Revision ) was adopted by the Bureau of Indian Standards on
15 June 1989, after the draft finalized by the Raw ;\Iaterials for Paint Industry Sectional
Committee had been approved by the Chemical Division Council.

This standard was first published in 1950 and was based largely on the interim co-ordinated draft
compiled by the Co-ordinating Subcommittee No. 5 Standing Committee on ‘Specification for
Paints and Allied Stores’ of the General Headquarters, India ( now Army Headquarters ).
During the first revision in 1965, the requirement for residue on sieve had been lowered to
0’25 percent in the case of Type A and 0’15 percent in the case of Types B and C while the lead
minimum had been revised from 93’15 percent to 95 percent for Type C and the method for
determination of lead dioxide ( PbO,) and lead minimum ( Pbs04 ) in red lead had been
modified.

In this revision, non-setting red lead Type C will now have two grades, namely, high-percentage
red lead and high dispersive red lead. A new requirement on total lead minimum and free lead
monoxide has been added and sodium thiosulphate-iodine method for determination of lead
dioxide ( PbO, ) and lead minimum ( PbsO4) in red lead has been replaced by the hydrogen
peroxide-permanganate method. The title has been suitably modified to cover various uses of
this material.

While’ preparing this standard, assistance has been derived from IS0 510-1977 ‘Red lead for
paints’, issued by the International Organization for Standardization ( IS0 ).

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 ‘Rules for rounding off numerical values (revised)‘. The
number ofsignificant places retained in the rounded off value should be the same as that of the
specified value in this standard.
 IS 57 : 1989

Indian Standard
RED LEAD FOR PAINTS AND OTHER
PURPOSES -SPECIFICATION
( Second Revision )
1 SCOPE 4 TYPES AND GRADES
.
1.1 This standard prescribes the requirements 4.1 Types
and the methods of sampling and test for red
lead used as a pigment and also as rust inhibitor There shall be the following three types of the
in paints, as an ingredient in joining material:
compounds, and as a raw material in battery
making, glass and ceramic industries, etc. 4 Type A, red lead (joining ) used by sugar
mills for steam and water pipe jointing
2 REFERENCES and putty;

2.1 The Indian Standards listed below are b) Type B, red lead ( ordinary ) used in mak-
necessary adjuncts to this standard: ing battery parts and glass and ceramic
industries; and
IS .hfo. Title
4 Type C, red lead, non-setting, used by paint
IS 33 : 1976 Methods of sampling and test industry as rust inhibiting pigment.
for inorganic pigGents and
extenders for paints (second 4.2 Grades
revision )
The material of Type C shall have two grades:
IS 77 : 1976 Specification for linseed oil,
boiled, for paints ( second revision ) a) Grade 1, high-percentage red lead, and
IS 266 : 1977 Specification for sulphuric acid b) Grade 2, high dispersive red lead.
(second revision )
NOTE - High-percentage red lead differs from
IS 323 : 1959 Specification for rectified spirit high-dispersive red lead by, among other factors, its
( revised ) lower sedimentation volume.

IS 1303 : 1983 Glossary of terms relating to

5 REQUIREMENTS
paints ( second revision )
IS 2080 : 1980 Specification for stabilized 5.1 Form and Condition
hydrogen peroxide (jirst revision )
The material shall be in the form of dry
3 TERMINOLOGY powder or in such a condition that it can be
reduced to the powder form by crushing,
3.1 For the purpose of this standard, the without grinding action, under a palette knife.
definitions given in IS 1303 : 1983 ahd under 2
of IS 33 : 1876, in addition to the following, 5.2 Description
shall apply.
The material shall be red to orange-red in colour
3.2 Red Lead and consist of lead orthoplumbate (Pb,O* )
( probably PbOz. 2PbO ) and lead monoxide
A red to orange-red pigment which consists of ( PbO ), and shall be free from added colouring
lead orthoplumbate ( Pb304) and lead monoxide matter organic colour and other adulterants
( PbO ), and in which no impurities other than except those arising from normal manufacturing
those arising from normal manufacturing processes.
processes are present.
5.2.1 Colouring Matter/Organic Colour
3.3 Non-setting Red Lead, High-Percentage
Red Lead a) Boil 2 g of the sample with 25 ml of
95 percent ethyl alcohol, let it settle.
Red lead which, when mixed with linseed oil, Decant the supernatant liquid. Boil the
does not cause undue thickening: residue with 25 ml of distilled water and

1
IS57:1989

decant as before. Again boil the residue to between the manufacturer and the
with 25 ml of diluted amonia ( 1 : 4 ) and purchaser.
again decant the supernatant liquid.
6.2 Marking
Boil another 2 g portion of the sample
with 25 ml of chloroform, let it settle and
The containers/packs shall be marked with the
decant the supernatant liquid.
following particulars:
If any one of the above solutions is
coloured, presence of organic colour 4 Name of the material;
matter is indicated. If the solutions
remain colourless, organic colours are b) Type and grade;
probably absent. cl Net mass;
5.3 The material shall also comply with the 4 Name of the manufacturer or his recog-
requirements given in Table 1, when tested nized trade-mark, if any;
according to the methods referred to in Annex
A in co1 8 of the Table 1. 4 Batch No. or lot No in code or otherwise;
and
5.4 Specific Requirements for Type C
f) Month and year of manufacture.
5.4.1 N&setting Properties

The material for both the grades of Type C 7. SAMPLING

shall also satisfy the test as prescribed in
Annex B. 7.1 Preparation of Test Samples

5.4.2 Sedimentation Volume Kepresentative samples of the material shall be

prepared as prescribed under 3 of IS 33 : 1976.
The material for Grade 2 of Type C ( non-
setting red-high dispersive ) shall have minimum
8 QUALITY OF REAGENTS
30 ml sedimentation volume when tested by the
method given in Annex C.
8.1 Unless otherwise specified, pure chemicals
6. PACKING AND MARKING and distilled water shall be employed in tests.

6.1 Packing NOTE - ‘Pure chemicals’ shall mean chemicals that do

not contain impurities which af%ect the results of
The material shall be suitably packed as agreed analysis.

Table 1 Requirements for Red Lead for Paints and Other Purposes
(Clause 5.3 )

61 Characteristic Requirement Ref to

No. ~-----__-* --------_- ,-------A ------
Type B Type C ’ ’ Clause No. in Annex ’
c__*-_-7 IS 33 : 1976 of this
Grade 1 Grade 2 Standard

(1) (2) (3) (4) (5) (6) (7) (8)

Lead dioxide, PbOs, l!vl-25’1 25’2-33’2 33’3 Min 33’5 Min - A

i)
percent by mass

ii) Lead orthoplumbate, Pb,O,, 43.0-72’0 72’ l-95.0 95’1 Min 96’0 Min - A
percent by mass

iii) Total lead orthoplumbate and 99’5 99’5 99’5 99’5 - A

Ea;iea$znmonoxide, percent by
,
iv) Violatile matter at 105’C, 0’2 0’2 0’2 0’2 7 -
percent by mass, Max I

v) Residue on sieve ( 63 micron ), 0’25 0’15 0’15 0’15 8 -

percent by mass, Max

vi) Oil absorption* 5toll 5toll 5to 11 510 11 9 -

vii) Matter soluble in water, 0’3 0’3 0’3 0’3 17

percent by mass, Max

*This shall, however, be within f: 10 percent by the approved sample, if any.

2
 IS 57 : 1989

ANNEX A
[ Table 1, hems (i) to (iii) ]
ANALYSIS OF RED LEAD

A-l DETERMINATION OF LEAD conical flask, add 25 to 50 ml of water, 5 g of

DIOXIDE ( PbO, ) AND LEAD sodium bicarbonate and 2 ml of starch solution.
ORTHOPLUMBATE (Pb,Or 1 IN RED Swirl the solution carefully until the
LEAD BY SODIUM THIOSULPHATE - bicarbonate has dissolved. Then titrate slowly
IODINE METHOD with the iodine solution, contained in a burette,
to the first blue colour. Calculate the exact
A-1.0 Principle strength of iodine.
The method involves the interaction of lead A-1.2 Procedure
peroxide with sodium thiosulphate and a
titration of the excess of the latter by standard Weigh to the nearest 1 mg, 1 g of the sample
iodine. and transfer to a 250-ml conical flask. Add
successively 25 ml of the sodium thiosulphate
A-l.1 Reagents
solution ( A-1.1.1 ), accurately measured with a
A-1.1.1 Sodium Thiosulphate Solution, 0’2 fl pipette, 30 ml of the sodium acetate-acetic acid
bufIer (A-1.1.2). S wirl gently to dissolve the
Dissolve 50 g of sodium thiosulphate penta- test portion. Rub down coarse particles of the
hydrate ( Na, S,Oc, 5H,O ) in water and dilute pigment by means of a glass rod flattened at
to 1 litre with water. the end. ( After this, carefully rinse the rod.
Use of few glass beads accelerates dissolution ).
A-1.1.2 Sodium Acetate-Acetic Acid Bu$er Solution If the last traces of pigment are difficult to
dissolve, the addition of not more than 0’5 g of
Dissolve. 85 g of sodium acetate trihydrate potassium iodide is recommended. When the
( CHsCOONa. 3Hz0 ) in 750 ml water. Add to lead oxides are completely dissolved, titrate the
it, 75 ml of glacial acetic acid. Dilute to 1 litre excess sodium thiosulphate with iodine solution
with water. using starch as indicator.

A-1.1.3 Iodine Solution, 0’1 N ( Approximate ) A-1.2.1 Blank Test

Dissolve 12’8 g of re-sublimed iodine in 200 ml In parallel with the determination, carry out a
of water containing 20 g of potassium iodide. blank test following the same procedure and
When the dissolution is complete, filter through using the same quantity of all the reagents but
glass wool and collect the filtrate in a 1 litre omitting the test portion.
volumetric flask. Wash the glass wool and
collect the washings in the flask. Dilute to A-l.3 Calculation
1 litre with water.
Lead dioxide ( PbOz ), percent by mass,
A-1.1.4 Standard Arsenite Solution, 0’1 JV

Dissolve 4’946 g of pure arsenious oxide in a 11’96 ( V2---VI > Jv

a=
solution of 2 to 3 g pure sodium hydroxide in ml
30 to 40 ml of water. Dilute the solution to
about 250 ml and neutralize the excess alkali Lead orthoplumbate ( PbsOd), percent by
with dilute sulphuric acid until a few drops of mass, b=2’866 1a
phenolphthalene indicator are just decolourized.
where
Transfer it quantitatively in a 1 litre volumetric
flask. Add 4 to 5 g of sodium bicarbonate, and
VI = volume in ml of standard iodine
when the dissolution is complete, dilute to the
solution used for the red lead
mark and shake well.
titration,
A-1.1.5 Starch Indicator Solution
Vz = volume in ml of standard iodine
solution used for the blank titration,
Dissolve 10 g of soluble starch and 10 mg of
mercurous [mercury (II)] iodide in 1 litre Jv - normality of the standard iodine
boiling water. solution, and
A-1.1.6 Standardization of Iodine ml = mass in g of the test portion.

Measure out from a burette 25 ml of the NOTE - 0.119 6 is the number of grams of lead dioxide
arsenite solution ( A-1.1.4 ) into a 250 ml equivalent to 1 ml of 1 .N iodine solution.

3
IS 57 : 1989

A-2 DETERMINATION OF TOTAL LEAD 110 f 5°C for one hour. Cool in a desiccator
CONTENT BY SULPHATE METHOD and weigh as lead sulphate. Repeat the
operation till constant mass is obtained.
A-2.0 Principle
NOTE - If the sample contains soluble barium and/or
The material is dissolved by warming in dilute calcium salts, the lead sulphate will also contain barium
nitric acid and hydrogen peroxide. Lead is sulphate and/or calcium sulphate and should, therefore,
be treated with acidic ammonium acetate solution,
precipitated by sulphuric acid as lead sulphate filtered and lead re-precipitated as lead sulphide in the
which is dried and weighed. filtrate by passing hydrogen sulphide gas ( to eliminate
calcium sulphate ). Lead sulphide is fumed with
A-2.1 Reagents sulphuric acid and few drops of nitric acid and lead
sulphate is estimated as above.
A-2.1.1 Dilute Nitric Acid 1 : 1 ( v/v ),
A-2.3 Calculation
A-2.1.2 Hydrogen Peroxide ( IS 2080 : 1962 ).
Total lead content, c, expressed as a percentage
A-2.1.3 ConcentratedSul#huric Acid ( IS 266 : 1961 ). by mass of lead,

A-2.1.4 EthyL Alcohol ( 95 percent) or rectified 68’32 (MS - Mq )

IT=
spirit ( IS 323 : 1959). M2

A-2.2 Procedure where

Weigh accurately 1 g of the sample, dried as MS = mass in g of the first precipitate,

prescribed under 7 of IS 33 : 1976 and transfer M4 = mass in g of the residue after
to a beaker. Add 20 ml of dilute nitric acid extraction with ammonium acetate,
and hydrogen peroxide drop by drop with and
gentle heating until all the red lead has
dissolved. Boil the solution gently for 5 minutes n/i, = mass in g of the test portion.
to decompose any excess of hydrogen peroxide. NOTE - 0’683 2 is the factor for the conservation of
If any insoluble matter is present, add 25 ml of sulphate to lead.
water, boil, filter and wash the precipitate with
water. Add 25 ml of concentrated sulphuric A-3 CALCULATION OF SUM OF FREE
acid to the original solution of filtrate and LEAD MONOXIDE AND LEAD ORTHO-
evaporate until copious fumes of sulphuric acid PLUMBATE CONTENTS
are evolved. Cool the solution and dilute with
water. If brown fumes are observed, this A-3.1 The sum of the free lead monoxide
would indiczlte incomplete removal of nitric ( PbO ) and the lead orthoplumbate ( Pb,Oa )
acid. In that case refume the solution. Cool contents, expressed as a percent by mass, is
and add 150 ml each of water and 95 percent given by the formula:
ethyl alcohol or rectified spirit. Keep the
1.077 (b - 2’5999 a) + 2’866 a
beaker in ice-cold water for an hour and filter
through a tared Gooch crucible and wash with where
95 percent ethyl alcohol or rectified spirit till
the filterate is free from sulphuric acid. Keep a = lead dioxide content, and
the crucible in an oven maintained at b = total lead content.

ANNEX B
( Clause 5.4.1 )
DETERMINATION OF NON-SETTING PROPERTY

B-O PRINCIPLE ( by mass ) of oil, and further thinning the paste

with the same oil, to paint consistency. Pour
B-0.1 The material ground with linseed oil into the paint into a tin of capacity 200 ml and
a suitable consistency for application as a paint, diameter 74 mm ( approximately ) so that it is
is exposed to air for 14 days. After this period, filled to within approximately 12 mm of the top.
the mixed material is retested as to whether the Cover the tin with muslin cloth. Without
consistency suitable for painting has been placing a lid on the tin, leave the paint exposed
retained. to the air for 14 days at ambient temperature.
At the end of this period, remove the skin
B-l PROCEDURE
formed at the surface of the paint, stir the paint
B-l.1 Prepare at least 200 ml of paint by and note whether it has thickened unduly.
thoroughly grinding the sample in the linseed Apply the stirred paint to a non-absorbent
oil ( IS 77 : 1976 ) having an acid value of 8 to surface and note whether it is still suitable for
10 to form a paste containing 8 to 10 percent application by brush.

4
 IS 57 : X&9-

(‘Clazise 5.43 )
‘“DEi’~Rbl$A+IOti OF THE .SEDftiElkTA-fIOhI VOLUME

k-1 kE&EN+ ‘C-3 ,PROCEDURE

‘C-l;1 “R&&d ’ Spirit, 95 i bercent ( is C-3.1 Weigh 50’0 f 0’1 g of the material into
323 : 1959). the cylinder, add 35 ml of rectified spirit and
‘c-2 APPARATUS shake the mixture for exactly 15 minutes.
After this period, make up to the 50-ml mark
‘C-2.1 bags-Stoppered Graduated Cylinder, with the rectified spirit. Allow to stand for
‘capacity 50 ml, internal height to 50 ml 24 hours at room temperature. After 24 hours,
‘of graduation lines extending over a height read the sedimentation volume to the nearest
6f 150 f 3 mm. ml.

5
Standard Mark

The use of the Standard Mark is governed by the provisions of the Bureau of Indian Standards
Act, 1986 and the Rules and Regulations made thereunder. The Standard 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 BlS and operated by the producer. Standard marked
products are also continuously checked by BIS for conformity to that standard as a further safe-
guard. Details of conditions under which a licence for the use of Standard Mark may be granted
to manufacturers or producers may be obtained from the Bureau of Indian Standards.
 \ \
Bureau of Indian Standards ‘6
I
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.

Revision of Indian Standards

Indian Standards are reviewed periodically and revised, when necessary and amendments, if any,
are issued from time to time. Users of Indian Standards should ascertain that they are in
possession of the latest amendments or edition. Comments on this Indian Standard may be sent
to BIS giving the following reference:

Dot : No. CDC 50 (9635 )

Amendments Issaed Since Publication

Amend No, Date of Issue Text Affected

BUREAU OF INDIAN STANDARDS

Headquarters:

Manak Bhavan, 9 Bahadur Shah Zafar Marg, New Delhi 110002

Telephones : 331 01 31,331 13 75 Telegrams : Manaksanstha
( Common to all Offices )

Regional Offices:

Central : Manak Bhavan, 9 Bahadur Shah Zafar Marg

NEW DELHI 110002

Eastern : l/14 C.I.T. Scheme VII M, V.I.P. Road, Maniktola 37 86 62

CALCUTTA 700054

Northern : SC0 445-446, Sector 35-C, CHANDIGARH 160036 2 1843

Southern : C.I.T. Campus, IV Cross Road, MADRAS 600113 41 29 16

Western : Manakalaya, E9 MIDC, Marol: Andheri (East) 6 32 92 95

XMBAY 400093

Branches : AHMADABAD. BANGALORE. BHOPAL. BHUBANESHWAR.

COIMBATORE. FARIDABAD. GHAZIABAD. GUWAHATI.
HYDERABAD. JAIPUR. KANPUR. PATNA. TRIVANDRUM.

Printed at Arcte Preu, Now Delhi, India

 AMENDMENT NO. 1 NOVEMBER 1993
TO
IS 57 : 1989 RED LEAD FOR PAINTS AND OTHER
PURPOSES - SPECIFICATION
(SecondRevision)

( Page 4, clause A-3.1 ) - Substitute ‘c’ for ‘b’ wherever it occurs in the
clause. .

( CHD 021)
Reprography Unit, BIS, New Delhi, India