IS : 50 - 1980

(Reaffirmed 1999)

Edition 4.1 (1988-01)

Indian Standard
SPECIFICATION FOR LEAD AND SCARLET CHROMES

( Third Revision )
(Incorporating Amendment No. 1)

UDC 667.622.117.628

BIS 2002 BUREAU OF

MANAK BHAVAN , 9 BAHADUR SHAH ZAFAR MARG NEW DELHI 110002

INDIAN

STANDARDS

Price Group 4

IS : 50 - 1980

Indian Standard
SPECIFICATION FOR LEAD AND SCARLET CHROMES

( Third Revision )
Raw Materials for Paints Industry Sectional Committee, CDC 50
Chairman SHRI R. K. MARPHATIA Members SHRI S. G. ARCHICK Indian Paints Association, Calcutta DR P. K. BHANDARI ( Alternate ) SHRI K. M. BANERJEE National Test House, Calcutta SHRI K. J. BHATT State Chemicals & Pharmaceutical Corporation of India Ltd, New Delhi SHRI S. BHATTACHARYYA Alkali and Chemical Corporation of India Ltd, Calcutta SHRI M. L. MALHOTRA ( Alternate ) SHRI H. BHUMKAR Fortuna Chemicals, Thane CHEMIST & METALLURGIST-II Ministry of Railways ASSISTANT RESEARCH OFFICER (CM)-II ( Alternate ) SHRI M. C. CHOKSI Resins & Plastics Pvt Ltd, Bombay DR C. S. VEERA RAGHAVAN ( Alternate ) SHRI A. DANI Asian Paints (India) Ltd, Bombay SHRI S. H. DESAI Garware Paints Ltd, Bombay SHRI R. R. SEQUEIRA ( Alternate ) SHRI O. P. DHAMIJA Export Inspection Council of India, Calcutta SHRI S. N. DUTTA ( Alternate ) DR A. B. KARNIK Colour-Chem Ltd, Bombay SHRI M. E. MARATHE ( Alternate ) SHRI R. D. KAWATRA Directorate General of Technical Development, New Delhi SHRI A. A. KHAN Ministry of Defence (DGI) SHRI R. S. SENGAR ( Alternate ) SHRI A. S. KHANNA Oil Technologists Association of India, Kanpur SHRI T. K. S. MANI Addisons Paints & Chemicals Ltd, Madras SHRI M. B. SATAYANARAYANA ( Alternate ) ( Continued on page 2 ) BIS 2002 BUREAU OF INDIAN STANDARDS This publication is protected under the Indian 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. IVP Limited, Bombay Representing

IS : 50 - 1980
( Continued from page 1 ) Members Representing

SHRI K. C. MEHTA Indian Oil Corporation Ltd, Faridabad SHRI V. C. PANCHAMIYA Kamani Metallic Oxides Pvt Ltd, Bombay SHRI B. RAMAMURTI Travancore Titanium Products Ltd, Trivandrum DR V. S. VIJAYAN NAYAR ( Alternate ) DR R. J. RATHI Sudarshan Chemical Industries Ltd, Pune SHRI K. L. RATHI ( Alternate ) SHRI P. SATYANARAYANAN Development Commissioner (Small Scale Industries), New Delhi DR G. K. SINGHANIA Ministry of Defence (R & D) DR R. SRIVASTAVA Indian Zinc & Lead Oxides Manufacturers Association, Calcutta SHRI M. VAITHYANATHAN Indian Dyestuff Industries Ltd, Bombay SHRI V. R. KARMAKAR ( Alternate ) DR HARI BHAGWAN, Director General, ISI ( Ex-officio Member ) Director (Chem) Secretary SHRI R. K. SINGH Deputy Director (Chem), ISI

Pigments and Extenders Subcommittee, CDC 50 : 1

Convener SHRI K. M. BANERJEE Members SHRI S. BOSE British Paints (I) Ltd, Calcutta SHRI G. C. DESAI Goodlass Nerolac Paints Ltd, Bombay SHRI A. PRABHAKARAN ( Alternate ) SHRI S. H. DESAI Garware Paints Ltd, Bombay DR P. G. CHAUDHARI ( Alternate ) SHRI J. N. GHOSAL M/s Sturdia Chemicals Ltd, Bombay SHRI H. S. VIJAYANATH ( Alternate ) SHRI M. M. GHOSH Shalimar Paints Ltd, Calcutta DR A. B. KARNIK Colour-Chem Ltd, Bombay SHRI M. E. MARATHE ( Alternate ) SHRI A. A. KHAN Ministry of Defence (DGI) SHRI M. R. SRIVATSAN ( Alternate ) SHRI V. C. PANCHAMIYA Kamani Metallic Oxides Pvt Ltd, Bombay SHRI K. L. RATHI Sudarshan Chemical Industries Ltd, Pune SHRI H. J. RATHI ( Alternate ) SHRI P. N. WAGLE Asian Paints (India) Ltd, Bombay ( Continued on page 13 ) National Test House, Calcutta

IS : 50 - 1980

Indian Standard
SPECIFICATION FOR LEAD AND SCARLET CHROMES

( Third Revision )
0. FOREWORD
0.1 This Indian Standard (Third Revision) was adopted by the Indian Standards Institution on 31 December 1980, after the draft finalized by the Raw Materials for Paints Industry Sectional Committee had been approved by the Chemical Division Council. 0.2 This standard was first published in 1950 and subsequently revised in 1963 and 1967. In view of the nature and the variety of treating agents used in production of treated chromes it is impracticable to lay down composition of this type of pigments. In this revision, however, limit for lead monoxide in the material has been included. The method for determination of lead monoxide (PbO) content has been replaced by the latest method prescribed in IS : 6947 (Part III)-1975*. Amendment No. 1 issued in July 1975 has also been incorporated in this revision ( see A-2.1 ). 0.3 This standard contains clauses 3.5.1, 4.1 and 4.3 which call for agreement between the purchaser and the supplier. 0.4 This edition 4.1 incorporates Amendment No. 1 (January 1988). Side bar indicates modification of the text as the result of incorporation of the amendment. 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 methods of sampling and test for lead chromes treated lead chromes, and scarlet (molybdated) chromes used as paint pigments.
*Methods of estimation of composite pigments in oil pastes, ready mixed paints and enamels: Part III Estimation of lead chromes, iron blues and zinc compounds. Rules for rounding off numerical values ( revised ).

IS : 50 - 1980 2. TERMINOLOGY
2.1 For the purpose of this standard, the definitions given in IS : 33-1976* and IS : 1303-1963 shall apply.

3. REQUIREMENTS
3.1 Form and Condition The material shall be in the form of dry powder or in such a condition that it is possible to reduce it to the powder form by crushing without grinding action, under a palette knife. 3.2 Composition 3.2.1 The material dried as described under 7.1 of IS : 33-1976* shall consist of chemical precipitates of either normal or basic lead chromate or lead molybdate or mixture of these with or without other co-precipitated insoluble compounds of lead. 3.2.2 The presence of white lead or lead carbonate is not permissible except if formed in situ during the manufacture of the chrome pigments. The amount of white lead or lead carbonate so formed and determined by the method prescribed in Appendix A shall not exceed 5 percent by mass when expressed as lead monoxide (PbO). This limit, however, shall not exceed that for the sample approved against this specification, if any. 3.2.3 The material shall be free from extenders or diluents, such as barium sulphate, clay, whiting, organic dyestuffs, etc. 3.2.4 In case of treated chromes, the pigment may contain other metallic compounds added specifically to improve pigmentary properties. In all such cases, the improvements obtained by way of treatment shall be stated by the supplier. 3.3 Stability of Colour The material shall not be inferior to the approved sample when tested according to the method prescribed in Appendix B. 3.4 Lead Content The total lead content in the material determined as lead monoxide (PbO) shall be minimum 6.1 percent by mass. When tested as prescribed in 5 of IS : 6947 (Part III)-1975.
*Methods of sampling and test for inorganic pigments and extenders for paints ( second revision ). Glossary of terms relating to paints ( revised ). Methods of estimation of composite pigments in oil pastes, ready mixed paints and enamels: Part III Estimation of lead chromes, iron blues and zinc compounds.

IS : 50 - 1980
3.5 For Scarlet Chromes Only 3.5.1 Molybdenum Content If required by the purchaser the molybdenum content of the material shall be determined by the method prescribed in Appendix C and the requirement for same shall be as agreed to between the purchaser and the supplier. 3.6 The material shall also comply with the requirements given in Table 1.
TABLE 1 SL NO. (1) REQUIREMENTS FOR LEAD AND SCARLET CHROMES REQUIREMENT METHOD OF TEST, REF TO CL NO. IN IS : 33-1976* (4) 7 8 9 10

CHARACTERISTIC

(2)

(3)

i) Volatile matter, percent 1.0 by mass, Max ii) Residue on sieve, 0.5 percent by mass, Max iii) Oil absorption 10 to 40 iv) Colour Close match to IS colours No. 354, 355, 356, 357, or 591, for primrose, lemon, golden yellow, light orange or deep orange, respectively whichever is required OR Close match to the colour of the approved sample, if any Staining power Not inferior to that of the approved sample Tone Equal to that of the approved sample Matter soluble in water, 1.0 percent by mass, Max Acidity (as H2SO4), 0.1 percent by mass, Max Alkalinity (as Na2CO2), 0.1 percent by mass, Max

v) vi) vii) viii) ix)

11 17 18 18

*Methods of sampling and test for inorganic pigments and exteders for pain ( second revision ). This shall, however, be within 10 percent of approved sample, if any. Conforming to IS : 5-1978 Colours for ready mixed paints and enamels ( third revision ).

IS : 50 - 1980 4. PACKING AND MARKING

4.1 Packing The material shall be suitably packed as agreed to between the purchaser and the supplier. 4.2 Marking The containers shall be marked with the following: a) Name of the material and additional information as per 3.2.4 and 3.5.1, wherever applicable; b) Net mass of the material; c) Manufacturers name and his recognized trade-mark, if any; d) Batch number or lot number in code or otherwise; and e) Month and year of manufacture. 4.2.1 Other details of packing and marking shall be in accordance with the instructions given by the purchaser, subject to the conditions given in 4.2.1.1. 4.2.1.1 Each container in which the material is supplied shall be legibly and indelibly marked LEAD PIGMENTS in black or white letters, whichever colour is more prominent, the letters being not less than 25 mm high. 4.2.2 The containers may also be marked with the ISI Certification Mark.
NOTE The use of the ISI Certification Mark is governed by the provisions of the Indian Standards Institution (Certification Marks) Act and the Rules and Regulations made thereunder. The ISI 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 ISI and operated by the producer. ISI marked products are also continuously checked by ISI for conformity to that standard as a further safeguard. Details of conditions under which a licence for the use of the ISI 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 under 4 of IS : 33-1976*. 5.2 Criteria for Conformity A lot shall be declared as conforming to the requirements of this standard, if the test results of the composite sample satisfy the requirement prescribed in 3.
*Methods of sampling and test for inorganic pigments and extenders for paints ( second revision ).

IS : 50 - 1980 6. TEST METHODS

6.1 Tests shall be conducted as prescribed in IS : 33-1976*, IS : 6947 (Part III)-1975 and Appendices A to C of this standard. Reference to the relevant clauses of IS : 33-1976*, IS : 6947 (Part III)-1975 and appendices is given in col 4 of Table 1 and 3.2.2, 3.3, 3.4 and 3.5.1. 6.2 Quality of Reagents Unless specified otherwise, pure chemicals and distilled water ( see IS : 1070-1977 ) shall be employed in tests.
NOTE Pure chemicals shall mean chemicals that do not contain impurities which affect the results of analysis.

APPENDIX A ( Clause 3.2.2 ) DETERMINATION OF WHITE LEAD OR LEAD CARBONATE A-0. GENERAL
A-0.1 Outline of the Method White lead or lead carbonate content is determined by absorbing the carbon dioxide evolved in a potash bulb, when the material is heated in the combustion apparatus.

A-1. PROCEDURE
A-1.1 Weigh accurately about 0.5 g of the dried sample ( see 7.1 of IS : 33-1976* ) in a combustion boat and introduce it into a gas or electrically heated combustion apparatus provided with suitable control to maintain the temperature between 450 and 550C and with a train for the absorption of water and a weighed potash bulb. Pass a slow current of dry air free from carbon dioxide and absorb the carbon dioxide evolved by the sample in the weighed potash bulb. Cool and weigh the potash bulb. The increase in the mass of potash bulb gives the mass of carbon dioxide evolved.
NOTE The experiment takes about an hour to complete. In order to obtain correct and concordant results, it is necessary to carry out a blank test before carrying out the estimation. The water-absorption train and the potash bulb shall not show any increase in mass in the blank test. *Methods of sampling and test for inorganic pigments and extenders for paints ( second revision ). Methods of estimation of composite pigments in oil pastes, ready mixed paints and enamels: Part III Estimation of lead chromes, iron blues and zinc compounds. Specification for water for general laboratory use ( second revision ).

IS : 50 - 1980 A-2. CALCULATION

A-2.1 White lead or lead carbonate expressed in terms of lead monoxide m (PbO), percent by mass = 507.27 ---M where m = mass in g of carbon dioxide evolved, and M = mass in g of the material taken for the test.

APPENDIX ( Clause 3.3 )

DETERMINATION OF STABILITY OF COLOUR B-0. GENERAL

B-0.1 Outline of the Method Stability of colour is determined by finding the change in colour of the dried painted tin plate panels with the sample after subjecting them to the action of ultraviolet light in a fadeometer.

B-1. PROCEDURE
B-1.1 Convert the material into a paint by the method prescribed under 10 of IS : 33-1976*. Determine the stability of colour by the method of test for fastness to light as prescribed in 12 of IS : 101-1964.

APPENDIX C ( Clause 3.5.1 ) DETERMINATION OF MOLYBDENUM IN SCARLET (MOLYBDATED) CHROMES C-0. GENERAL
C-0.1 Outline of the Method The procedure is based on the reduction of hexavalent molybdenum to trivalent form by passing its
*Methods of sampling and test for inorganic pigments and extenders for paints ( second revision ). Methods of test for ready mixed paints and enamels ( second revision ).

IS : 50 - 1980
acidified solution through a coloumn of amalgamated zinc. The reduced compound is added in excess of ferric solution, whereupon an equivalent amount of ferric compound is reduced to ferrous state. Titration of the reduced iron by means of standard potassium permanganate establishes the amount of molybdenum reduced by zinc.

C-1. APPARATUS
C-1.1 Jones Reductor Suitable dimensions for the reductor are as shown in Fig. 1. A perforated porcelain plate or platinum gauze covered with purified asbestos or glass wool, supports the zinc column and also acts as a filtering pad. The reductor shall contain at least 350 mm column of amalgamated zinc which is prepared as given in C-1.1.1. C-1.1.1 Take 300 g of pure, 20 to 30 mesh zinc and wash the same with 1 N hydrochloric acid for one minute. The quantity of hydrochloric acid added shall be just sufficient to cover all the zinc. Afterwards cover the zinc metal with 2 percent mercuric chloride solution. The quantity of mercuric chloride shall be sufficient to give an amalgam containing 1 percent mercury. Stir the mixture thoroughly for 5 minutes. Decant off the solution and wash well with water. Add this amalgamated zinc in the reductor.
NOTE When not in use the reductor shall be kept filled with water, otherwise its effectiveness will be reduced due to formation of basic salts with oxygen from atmosphere.

C-2. REAGENTS
C-2.1 Dissolving Solution Prepare 1 000 ml of a saturated solution of sodium chloride. Filter through a sintered glass funnel. Add 150 ml of water and 10 ml of concentrated hydrochloric acid ( see IS : 265-1976* ). C-2.2 Rectified Spirit See IS : 323-1959. C-2.3 Ammonium Hydroxide Solution 20 percent ( m/m ). C-2.4 Concentrated Sulphuric Acid see IS : 266-1977. C-2.5 Hydrogen Sulphide gas, from Kipps apparatus. C-2.6 Dilute Sulphuric Acid (One Percent) Saturated with Hydrogen Sulphide C-2.7 Concentrated Nitric Acid see IS : 264-1976.
*Specification for hydrochloric acid ( second revision ). Specification for rectified spirit ( revised ). Specification for sulphuric acid ( second revision ). Specification for nitric acid ( second revision ).

IS : 50 - 1980

FIG. 1

JONES REDUCTOR 10

IS : 50 - 1980
C-2.8 Bromine C-2.9 Dilute Sulphuric Acid Approximately 12 N. C-2.10 Ferric Ammonium Sulphate Solution Dissolve 20 g of Fe2(SO4)3.(NH4)2SO424H2O in 200 ml of water to which has been added 50 ml of concentrated sulphuric acid and 20 ml of phosphoric acid (85 percent), and dilute to one litre. C-2.11 Standard Potassium Permanganate Solution 0.1 N ( see 27 of IS : 2316-1963 )*.

C-3. PROCEDURE
C-3.1 Weigh about 1 g of the sample accurately, dried as prescribed under 7 of IS : 33-1976 into a clean dry beaker. Add 150 ml of dissolving solution and stir well until the pigment is completely dissolved. Add 5 ml of rectified spirit. Cover the beaker and boil the contents gently to reduce the chromates, which is noted by a change in the colour of the solution to green. If any insolubles remain, filter and wash the same thoroughly with hot water. Collect the filtrate and washings and add ammonium hydroxide solution until the formation of a faint precipitate takes place. Add 15 ml of concentrated sulphuric acid and dilute to 400 ml. Boil and pass a rapid stream of hydrogen sulphide gas for 10 to 15 minutes. Dilute this solution further with 400 ml of hot water and again pass hydrogen sulphide gas till the preciptation is complete. Allow the precipitate to settle, filter and wash well with dilute sulphuric acid saturated with hydrogen sulphide. C-3.2 Transfer the precipitate from the filter paper into the beaker and add 20 ml of concentrated nitric acid and 5 ml of concentrated sulphuric acid. Treat the filter paper separately with bromine and filter. Add the filtrate to the beaker. Cover and boil on a hot plate until fumes are evolved and cool. Add 10 ml of concentrated nitric acid and heat again to fumes until the solution is clear. Wash the sides, cover the beaker and boil to remove nitric acid. Repeat the operation to ensure complete removal of nitric acid. Dilute to 300 ml with water and neutralize with ammonium hydroxide solution and finally add 10 ml of dilute sulphuric acid. Cool this solution and pass through the Jones reductor, at a rate not exceeding 100 ml per minute. Collect the reduced solution under 200 ml of ferric ammonium sulphate solution. Titrate the ferric ammonium sulphate solution with standard potassium permanganate solution. Carry out the blank determination in the same way.
*Methods of preparation of standard solutions for colorimetric and volumetric analysis ( first revision ). Methods of sampling and test for inorganic pigments and extenders for paints ( second revision ).

11

IS : 50 - 1980 C-4. CALCULATION

( V1 V 2 ) N Molybdenum, percent by mass = 3.2 ----------------------------M where V1 = volume in ml of standard potassium permanganate solution used for the sample, V2 = volume in ml of standard potassium permanganate solution used in the blank, N = normality of standard potassium permanganate solution, and M = mass in g of the material taken for the test.

12

IS : 50 - 1980
( Continued from page 2 )

Panel for Inorganic Pigments, CDC 50 : 1 : 1

Convener SHRI G. C. DESAI Members SHRI A. PRABHAKARAN ( Alternate to Shri G. C. Desai ) SHRI K. M. BANERJEE National Test House, Calcutta SHRI S. BHATTACHARYYA Alkali and Chemical Corporation of India Ltd, Calcutta SHRI M. L. MALHOTRA ( Alternate ) SHRI T. K. S. MANI Addisons Paints & Chemicals Ltd, Madras SHRI V. C. PANCHAMIYA Kamani Metallic Oxides Pvt Ltd, Bombay SHRI K. L. RATHI Sudarshan Chemical Industries Ltd, Pune SHRI H. J. RATHI ( Alternate ) DR V. S. VIJAYAN NAYAR Travancore Titanium Products Ltd, Trivandrum SHRI D. V. WITTENBAKER Waldies Limited, Calcutta Representing Goodlass Nerolac Paints Ltd, Bombay

13

Bureau 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. Review of Indian Standards 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 by referring to the latest issue of BIS Catalogue and Standards : Monthly Additions. This Indian Standard has been developed by Technical Committee : CDC 50 Amendments Issued Since Publication Date of Issue January 1988

Amend No. Amd. No. 1

BUREAU OF INDIAN STANDARDS Headquarters: Manak Bhavan, 9 Bahadur Shah Zafar Marg, New Delhi 110002. Telephones: 323 01 31, 323 33 75, 323 94 02 Regional Offices: Central Eastern : Manak Bhavan, 9 Bahadur Shah Zafar Marg NEW DELHI 110002 : 1/14 C. I. T. Scheme VII M, V. I. P. Road, Kankurgachi KOLKATA 700054 Telegrams: Manaksanstha (Common to all offices) Telephone
323 76 17 323 38 41 337 84 99, 337 85 61 337 86 26, 337 91 20 60 38 43 60 20 25 235 02 16, 235 04 42 235 15 19, 235 23 15 832 92 95, 832 78 58 832 78 91, 832 78 92

Northern : SCO 335-336, Sector 34-A, CHANDIGARH 160022 Southern : C. I. T. Campus, IV Cross Road, CHENNAI 600113 Western : Manakalaya, E9 MIDC, Marol, Andheri (East) MUMBAI 400093

BANGALORE. BHOPAL. BHUBANESHWAR. COIMBATORE. Branches : AHMEDABAD. FARIDABAD. GHAZIABAD. GUWAHATI. HYDERABAD. JAIPUR. KANPUR. LUCKNOW. NAGPUR. NALAGARH. PATNA. PUNE. RAJKOT. THIRUVANANTHAPURAM. VISHAKHAPATNAM