IS 2520 (1984): Zinc Stearate for Cosmetic Industry - Public ...

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IS 2520 (1984): Zinc Stearate for Cosmetic Industry [PCD19: Cosmetics]

IS : 2520 - 1984 (Reaffirmed 1!395)

Indian Standard

SPECIl?ICATION FOR ZINC STEARATE FOR COSMETIC INDUSTRY

( Second Revision )

First Reprint FEBRUARY 1999

UDC 661.847.753 : 665.58

Q Copyright 1984

BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

cl-4 November 1984 ’

IS I 2520-1984

Indian Standard SPECIFICATION FOR

ZINC STEARATE FOR COSMETIC INDUSTRY

( Second Revision )

Cosmetics Sectional Committee, PCDC 19

Choirman RqWrsnling

DB S. S. GOTIWJSKAR Directorate General of Health Services, New Delhi

M&S tt.W.ISTAWT Dm~cxou FoodBo~bsDy”B Administration, Maharashtra State,

DB P. D. PILANKAU ( Al&mate) SEBJ B. S. BULVE Lakm6 Ltd, Eombay

SAEI S. M. SHA~~BEAQ ( Altamata ) Sstm V. G. DESBPANDE Hindustan Ciba-Geigy Ltd, Bombay

Da S. S. KAIMABKAR ( Alternate ) DR A, S. DIVATIA ConsS;reaze;ational & Research Centre,

KUMA~I RANI ADVANI ( Altsmatc ) DB S. N. Ivnx Johnson & Johnson Ltd, Bombay

SBBI G. V. BnaNDAnI ( Allarnala ) SEBNATI T. JACOB Lady Irwin College, New Delhi DE G. L. MADAX Hindustan Lever Ltd, Bombay

SHRI D. CHHIBBA ( Alfmmfc) SERI P. MAZ~D~DAR Nitional Test House, Calcutta

SHRJ P. K. C~AXRABOlrYY ( &eTaalG) Swr R. C. ME~TA DN~S Control Administration, Government of

Gujarat, Ahmadabad Smtr J. P. GANATRA ( Alternate )

SBBI A. M~NHAZUDDIN Millet Rochas Pvt Ltd, Madras KUMARI NASRIN BEQAM ( Alternate )

Dn S. G. PATNEPAP. Perfumes & Flavours Association of India, Bombay SBRI SUDIIIR JAIN ( Alternate )

SHRI K. S. RAO Swastik Household & Industrial Products Pvt Ltd, Bombay

SHRI C. R. KRISIINA~~OOBTIIY ( Altqnafc ) SERI A. C. ROY Indian Soap & Toiletries Makers’ Association,

Bombay DR S. K. ROY Central Drugs Laboratory, Calcutta

DR A. C. Dns GUPTA ( A&s~~~ata )

( Conhued on &y 2 )

@ Ca@ri# 1984 BUREAU OF INDIAN STANDARDS

This publication is protected under the Its&a 0fl@ Act ( XIV of 1957 ) and reproduction in whole or in part by any means except with written permission of the puhlishee shall be deemed to be an infringement of copyright tmder the said Act.

Manbm Representmg SERI P. ROY Bengal chemical & Pharmaceutical Works Ltd,

Calcutta DR A.;N. BAFIU ( Alternate )

SEE1 V. SITARAId Basic Chemicals & Pharmaceuticals & Cosmetics

Srinr I. SUNDABEEH I Alternate 1 Export Promotion Council, Bombay

SEBIXATI UBHA SIJKTHA~~AR ‘Consumer’s Guidance Society, Bombay SHRIYATI USEA KAWEBKAR ( Alterwe )

SHSI M. S. TRAXVB SEUI N. G. IY~B ( Aftmutr )

Godrej Soaps Ltd, Bombay

SEBI R. THANJAXU Directorate General of Technical Development, New Delhi

SEBI S. N. AOABWAL ( Alternate ) SIERI M. S. SAIEIPA,

Director(P&C) Director General, IS1 ( Ex-ofio Member )

SHRIYATI V~JAY MALIK As&ant Director ( P & C ), IS1

Raw Materials and GRAS List Subcommittee, PCDC 19 : 1

DE G. L. MA~AX Members

Hindustan Lever Ltd, Bombay

.SEBI D. CEHIsBA ( Afternute to Dr G. L. Madan )

AauumAler ~OXS~~~IO~R Food 8 Drug Administration, Maharashtra State,

( 2zzz2xTm.m omc!m Bombay

CnaesI(Cn~~) (A&,) SHBI B. S. BABVE LakmC

SBBI S. M. SlIAl’?BHAQ ( Alterwe > Ltd, Bombay

S-1 V. G. I)~~~HPANDE SEEI J. P. GANATBA

~~~m~~~oi;“ip 14trl, Bofl~y .g . Acinmutra~on, Government of

S-1 R D. DIEODEAR ( Al&m&c ) ularat, Alunadabad

DBS.N.IYW Johnson h Johnson Ltd. Bombay S-TX USEA R. JOSHI ( Ati )

SW1 K. S. RAO Swastik Household h Industrial Products Pvt Ltd, Bombay

S-I C. R. KB~SFRJAU~OO~TI~P ( Al&n& ) SE& K. L. RATEI

&IBI U. N. LlYAYB ( dUR& ) Sudershan Chemical Industries Ltd, P~FM

DF&. K:RoY? DBP. C. BOSE ( Afrmrok )

Central Drug Laboratory, Calcutta

DE N. D. !%k D~M.h¶.Dortn AlkrncrcI)

Geoffrey Mannera (It Co Ltd, Bombay

SEIU NA~OEAI~DBA 6 . SHAH Devarwns Pvt Ltd, Ahmadabad 8~~1 VLIIODOHABIDBA K.

MmnTA(‘&m-) 8sNA4.8.Tl?AxuB

8~uxN.G.h’xa(~) Godrej Soaps Ltd, Bombay

2

ISr2520.1984

Indian Standard SPECIFICATION FOR

ZINC STEARATE FOR COSMETIC INDUSTRY

( Second Revision )

0. FOREWORD

0.1 This Indian Standard ( Second Revision ) was adopted by the Indian Standards Institution on 16 August 1984, after the draft finalized by the Cosmetics Sectional Committee had been approved by the Petroleum, Coal and Related Products Division Council.

0.2 This standard was first published in 1963 and subsequently revised in 1977. In the first revision of this standard, two sets of requirements, namely, the essential and the optional requirements had been prescribed. Subsequently this was found non-implementable for certification and therefore the Sectional Committee after due consideration decided to stipulate only a single set of requirement.

0.3 Zinc stearate is used in face powders, after-shave powders; baby powders, foot powders etc, to which it is said to impart improved pro- perties of smoothness and adhesion. It has mild antisepticand astrin- gent properties. It is also used as a local smoothing application in inflammatory and irritating skin diseases and as a water-in-oil emulsifier in hair-grooming preparations.

0.4 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*. The number of significant places retained in the rounded off value should be the same as that of the specified valuein this standard.

1. SCOPE

1.1 This standard prescribes the requirements and the methods of sampling and test for zinc stearate for cosmetic industry.

*Rules for rounding off numerical values ( rcuiscd ).

3

IS : 2520 - 1984

2. REQUIREMENTS

2.1 Description - The material shall be in the form of a fine white bulky powder, free f.om rancid odour. It shall be insoluble in alcohol, water and ether.

2.2 The material shall also comply with the requirements given in Table 1, when tested according to the methods prescribed in Appendix A. Reference to the relevant clauses of Appendix A is given in co1 4 of the table.

TABLE I REQUIREMBNTS FOR ZINC STEARATE FOR COSMETIC INDUSTRY

SL No.

(1)

i)

ii)

iii)

iv)

v)

vi)

vii)

ix)

4

xi)

(2)

Zinc ( as ZnO ), percent by mass

T$; of separated fatty acids ( “C ),

Arseuic ( as As,O, ), ppm, Max

Heavy metals ( as Pb ), ppm, Max

Sieve analysis )

Bulk density 1 Moisture, percent by mass, Max

Total nsb, percent by mass

Iodine MUX

value of separated fatty

Frgafatty matter, percent by mass,

PH, Ma.v

REQUUUZXIWT

(3)

130 to 15-5

54

2

10

As agreed to between the purchaser and the supplier

4-O

Shall not differ from zinc content by more than 05

3.0

1-O

9'0

METHODOBTEST ( REP TO CL No. IN APF-J~NDIX A )

(4)

A-2

A-3

A-4

A-5

A-8

A-7

A-8

A-9

A-10

A-11

3. PACKING AND MARRING

3.1 Packing - The size and material of construction of the containers shall be subject to agreement between the purchaser and the supplier.

3.2 Marking - The containers shall be securely closed and marked with the name and mass of the material in the container; manufacturer’s name and trade-mark, if any; batch number in code or otherwise; and the year of manufacture.

4

IS : 2529 - 1984

3.2.1 The product may also be marked with Standard mark.

3.3 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 details of conditions under which the licence for the use of Standard Mark may be granted to manufacturers or producers may be obtained from the Bureau of Indian Standards.

4. SAMPLING

41 Preparation of Test Samples - Representative test samples of the material shall be prepared as prescribed in Appendix B.

4.2 Number of Tests

4.2.1 Tests for the determination of zinc shall be conducted on each of the individual samples constituting the set of test sample ( see B-3.1.3 ).

4.2.2 Tests for the remaining characteristics, namely, sieve analysis, bulk density, moisture, total ash titre of separated fatty acids, iodine value of separated fatty acids, arsenic, heavy metals, free fatty matter, and PH shall be conducted on composite sample.

4.3 Criteria for Conformity

4.3.1 For Individual Samples - The mean and the range for .the test results for the determination of zinc shall be calculated as follows:

Mean ( X) = the sum of the test results divided by the number of test results, and

Rang ( R ) = the difference between the maximum and the minimum value of the test results.

4.3.1.1 The lot shall be declared to have satisfied the requirements for zinc if:

a) X- 0.6 R is equal to or greater than 13.0, and

b) 2 + 0 6 R is equal to or less than 15.5.

43.2 For Composite Sample - The test results on the composite sample shall meet the corresponding requirements specified in 2 and in Table 1.

5

II3 I 2520 - 1984

APPENDIX A ( Claw? 2.2 )

AbfALYSIS OF ZINC STBARATE FOR cosMETx INDUSTRY

A-1. QUALITY OF REAGENTS

A-l.1 Unless specified otherwise, pure chemicals and distilled water ( se6 IS : 1070-19778 ) shall be employed in the tests.

NOTE- Pure chemicals ’ shall mean chemicals that do not contain impurities which affect the results of analysis.

A-2. DETERMINATION OF ZINC

A-2.1 Reagents

A-21.1 Concentrated Hydrochltiric Acid - See IS : 265-1962t.

A-2.1.2 Ammtiium Hydrogett Phosphate Solution - 10 percent and 1 percent.

A-2.1.3 Ethyl Alcohol - 50 percent ( v/v ).

A-21.4 Methyl Red Indkator - Dissolve 0.15 g of methyl red in 500 ml of water.

A-2.2 Procedure - Weigh accurately about 1 g of the material into a

P latinum dish and ignite to light grey ash at 600 to 650°C. DO not heat

anger than necessary. Cool and take up the ash in about 10 ml of water. Add methyl red indicator and neutralize with concentrated h drochloric acid and make up to about 200 ml. Bring to boil on a hot p ate and add 60 ml of ammonium hydrogen phosphate solution ( 10 per- r cent ) and continue to heat at just below boiling for 30 minutes. Remove from the hot plate and allow to cool to room temperature. Filter through a tared Gooch crucible. Wash with freshly prepared ammonium hydrogen phosphate solution ( 1 percent ) and finally with 50 ml of ethyl alcohol. Discard the filtrate. Place the crucible in a porcelain crucible of suitable size and dry over a low flame. Increase the temperature and ignite at full heat to constant mass.

*Specification for water for general laboratory use ( second revision ) . f?Specification for’hydrochloric acid ( rroisti ).

6

A-2.3 Calculation

Zinc ( as Z,O ), percent by mass = q

where

m - mass in g of the residue, and

1M I mass in g of the material taken for the test.

A-3. DETERMINATION OF TlTItE OF SEPARATab FATTY ACIDS

A-3.1 Reagents

A-3.1.1 Dilute Sulphuric Acid - 1 : 3.

Ad.2 Procedure - Heat 50 g of the material with 400 ml of water and 50 ml of dilute eulphuric acids until the fatty acidr have separated a6 a layer. Wabh the fatty acids with boiling water until ‘free of sulphate. Warm the fatty acid6 on a steam-bath until the water is separated and the acid6 arc clear. Allow the acid6 to cool, melt and filter into a dry hot beaker and dry for 20 minutes at 100°C. Thsre fatty acids are also ured for test in A*9. Determine the titre a6 directed in 16 of IS : 266-1966*.

A-4. TEST FOR ARSENIC

A-4.1 Preparation of Solutioa - Place 1’000 g of the material .in a platinum dish and incinerate for about 2 hours at 525 to 550°C. COOI and treat with a mixture of 5 ml of concentrated sulphuric acid and 5 ml of concentrated nitric acid. Take to fumes on a hot plate, cool and make up the volume to exactly 100 ml.

A-4.2 Take 10 ml of the solution of the material a6 obtained in A-4.1 and carry out the test for arsenic as prescribed in IS : 2088-1971t. Corn are the stain obtained with that produced by 0’000 2 mg of arsenic triox P de ( As606 ).

A-5.’ TEST FOR HEAVY METALS

A-5.1 Apparatus

A&I.1 Nesster Cylindrrs - 50 ml capacity.

A-5.2 Reagents

A-3.2.1 Concentrated Hydrochloric Acid - Sor IS : 265.1962#.

*Methods of sampling and test for soaps ( i;rJt r#OiJbn ).

tMethods of the determination of arsenic ( Ji*sl w&ion ). Jspecification for hydrochloric acid ( ftiJed ).

7

IS: 2520 - 1984

A-5.2.2 Dilute Hydrochloric Acid - 1 : 1.

A-5.2.3 Ammonium Chloride

A-5.2.4 Acetic Acid - 1 N.

A-5.2.5 Standard Lead Solution - Dissolve I.60 g of Iead nitrate in water, add 1 ml of concentrated nitric acid ( See IS : 261-1968* ) and make up the volume to 1 000 ml. Pipette out 10 ml of solution and dilute again to 1 000 ml with water. One millilitre of this solution contains 0’01 mg of lead ( as Pb ).

A-5.2.6 Hydrogen &&hide Solution - Freshly prepared, saturated solution.

A-S.3 Procedure - Heat 0.500 g of the material in a silica crucible in a muffle furnace at 475 to 500°C. Cool and treat the residue with 3 drops of concentrated hydrochloric acid. Evaporate to dryness over a low flame and heat again in the furnace for 20 to 30 minutes. A clean white ash should result, otherwise, the treatment may be repeated. Dissolve the white ash in 1 ml of dilute hydrochloric acid and wash with several portions of water into an evaporating dish. Evaporate to dryness on steam bath and dissolve the residue in about 30 ml of water. Transfer the solution to a Nessler cylinder and add 1 g of ammonium chloride and I ml of acetic acid. Carry out a control test in another Nessler cylinder using 0.5 ml of standard lead solution in place of the material. Add 1 g of ammonium chloride and 1 ml of acetic acid to each Nessler cylinder add 10 ml of hydrogen sulphide solution, dilute to the mark and shake well. Compare the intensity of colour produced in the two cylinders.

A-5.3.1 The limit prescribed in Table 1 shall be taken as not having been exceeded if the intensity of the colour obtained with the material is not greater than that obtained in the control test.

A-6. DETERMINATION OF SIEVE ANALYSIS AND BULK DENSlTY

A-6.1 Sieve Analysis

A-6.1.1 Procedure - Place about 10 g of the material, accurately weighed, in the agreed sieve and wash by means of a slow stream of running tap water ( see Note 1 ) and finally with fine stream from a wash bottle until all the material that is capable of passing through the sie.ve has passed ( see Note 8 ). Let the water drain from the sieve and then dry the sieve contaming the residue on a steam-bath. If there is any

*Specification for nitric acid (JFrsr reuision ).

8

IS : 2520 - 1984

residue, carefully transfer it on to a tared watch-glass and dry to constant mass at 105 f 2°C.

NOTE I-Tap water is usually sufficiently free from suspended particles to be utilized directly as i&_comesfrom the faucet. If the water is turbid, it is necessary to place a large bottle of&&d water above the working sink and to siphon the water through a clean rubher tube to the level of the sieve. It is a good plan to insert a small rubber stopper carrying a short glass tube about 5 cm in length and W6 cm in internal dia- meter in the faucet outlet. A thin flexible piece of clean rubber tubing ( new tubing should first be thoroughly washed ) about 60 cm in length is then attached to the glass tube. The faucet is turned [on slowly until a thin stream of water is coming through the rubber tube. By processing the end of the rubber tube between the fingers, the steam of water can be varied in intensity and directed to any section of the sieve. Experience has shown that the best practice is to alternately tip the sieve from one side to another, washing the sample from the higher level of the sieve to the lower and then reversing the sieve and repeating the operation.

NOTE 2 - In order to obtain comparable results, it is essential to continue washing the residue on the sieve until one is satisfied that all the material fine enough to pas through the sieve has been removed. At least one-half hour of washing is essential in most cases. It is a good plan to catch the last washes in a beaker. By viewing the contents of the beaker against a dark coloured background, it is possible to accurately gauge the progress of the washing operations.

A-6.1.2 Calculation

Material retained on the specified sieve, 1OOm percent by mass

~ M

where m = mass in g of the residue retained on the specified sieve,

and M =- mass in g of the material taken for the test.

A-6.2 Bulk Density A-6.2.1 Apparatus

A-6.2.1.1 Assemble the apparatus as shown in Fig. 1. The base of measuring cylinder A shall be ground flat and the emply measuring cylinder A together with the rubber bung shall weigh 250 f 5 g. It shall be accurately calibrated to 250 ml with an error, if any, of less than one millilitre. The distance between zero and 250 ml graduation on the measuring cylinder A shall be not less than 220 mm and not more than 250 mm. The distance between the flat-ground part of the base of measuring clyinder A and the rubber base pad B, when the measuring cylinder A is raised to full height shall be 25 f 2 mm.

A-6.2.1.2 Rubber base pad - The rubber base pad B shall have a shore hardness of 42 to 50.

A-6.2.1.3 Balance - Pans of the balance shall be at least 10 cm in diameter and the balance shall be sensitive to less than 0.1 g.

A-6.2.2 Procedure - Sieve about 40 g of the material through 250 micron IS Sieve on to a tared glazed paper and weigh it accurately.

9

-

15:2520-1984

Slip the powder should be held

gently and smoothly into the measuring cylinder which at 45” to the vertical, without knocking or squeezing.

Assemble the apparatus as shown in Fig. 1. With the thumb and four fingers of one hand, gently grasp the upper part of cylinder and within one second, lift it about 25 mm ( takihg care not to jerk the cylinder by knocking it against the upper stop ) and let it drop. Note the volume after dropping it once. Continue lifting and dropping 50 complete drops have been given to the cylinder. During this operation, give a gentle turn of about 10” in the clockwise direction to the cylinder afier every two drops. As soon as 50 drops are completed, raise the cylinder to eye level and read the volume of the material.

FIQ. 1

AI1 dimensions in milHmetres.

APPARATUS FOR DETERMINATION OF BULK DENSITY

A-6.2.3, Calculation

Bulk density, g/ml:

a) After one tap - F 1

b) After 50 taps - -F .n

where

m = mass in g of the material taken for the test,

Va = volume in ml of the material after one tap, and

Vg = volume in ml of the material after 50 taps.

10

IS : 2529 - 1984

A-7. DETERMINATION OF MOISTURE

A-7.1 Procedure - Weigh accurately about 3 g of the material and dry in an oven at 105 f 2°C for 3 hours and weigh to constant mass.

A-7.2 Calculation

100 MI Moisture, percent by mass = -

M2

where

Ml = loss in mass in g on drying, and MS = mass in g of the material taken for the test.

A-8. DETERMINATION OF TOTAL ASH

-A-9.1 Procedure - Weigh accurately about 1’5 g of the material in a platinum dish and gently heat until the organic matter is burnt away. Increase the temperature to about 550°C until all carbon residue is burnt away. Allow to cool and weigh. Repeat the operation of heating, cooling and weighing until constant mass is obtained.

A-0.2 Calculation

Total ash, percent by mass lOO& _ M2

where

Ml = mass in g of the ash, and

M2 = mass in g of the material taken for the test.

A-9. DETERMINATION OF IODINE VALUE OF SEPARATED FATTY ACIDS

A-9.1 Procedure - Weigh accurately about 3.0 g of the fatty acids as obtained in A-3.2 and determine iodine value by Wijs method as directed in 18 of IS : 286.1966*.

A-10. DETERMINATION OF FREE FATl’Y MATTER

A-10.1 Reagent

A-10.1.1 EthTl Ether - set IS : 336-1973t.

A-10.2 Prpcedurc - Weigh accurately about 5 g of the material and mix it with 100 ml of ether in a beaker. Shake for about half an hour

*Methods of sampling and tat for soap0 (fir: r&ion ). tspecification for ether ( aond rmisien ).

11

IS : 2528 - 1984 .

and filter. Take the filtrate in a tared porcelain dish and evaporate slowly on a steam-bath. Cool and weigh the residue.

A-10.3 Calcolation

100 Ml Free fatty matter, percent by mass = -

Ma where

Ml = mass in g of the residue, and

Ma - mass in g of the material taken for the test.

A-11. $3 DETERMINATION

A-11.1 Apparatus - pH Meter

A-11.2 Procedure - Weigh about 2 g of the material and wet it with 5 ml of neutralized ethyl alcohol and 45 ml of water. Filter the susDension through G 3 sintered glass funnel and determine the pH of the filtrate at 27°C.

APPENDIX ( Clause 4.1 )

OF ZINC STEARATE PREPARATION OF TEST SAMPLES FOR COSMETIC INDUSTRY

B

B-I. GENERAL REQ-MENTS OF SAMPLING

B-1.0 In drawing, preparing, storing and handling test samples, the following precautions and directions as directed in IS : 8883 ( Part 1 )- 1978* shall be observed.

B-2. SCALE OF SAMPLING

B-2.1 Lot - All the containers in a single consignment of the material drawn from a single batch of manufacture shall constitute a lot. If a consignment is declared or known to consist of different batches of manufacture, the containers belonging to the same batch shall be group- ed together and each such group shall constitute a separate lot.

B-2.1.1 Samples shall be tested from each lot for ascertaining conformity of the material to the requirements of this specification.

*Methods of sampling chemicals and chemical products: Part 1 General require- ments and precautions.

12

IS:2520-1984

B-2.2 The number of containers ( n ) to be chosen from the lot shall depend on the size of the lot ( .N) and shall be as given in Table 2.

TABLE 2 NUMBEB OF CONTAINERS TO BE SELECTED FOR SAMPLING

LOTSIZE NO. OB COXTMNRRS TO BE SELECTED

N n

(1) (2)

up to 50 3 51 to 150 4

151 to 300 5 301 to 500 7 501 and above IO

B-2.3 The containers to be selected for sampling shall be chosen at random from the lot and for this purpose random number tables ( see IS : 49051968; ) shall be used. In case such tables are not avail- able, the following procedure may be adopted:

Starting from any container, count them 1, 2, 3 ,...... . . . . r and so on in a systematic manner, where r is the integral part of N/n. Every rth container thus counted shall be withdrawn from the lot.

B-3. TEST SAMPLES AND REFEREE SAMPLE

B-3.1 Preparation of Test Samples

B-3.1.1 Draw with an appropriate sampling instrument a small portion of the material from different parts of each container selected ( see Table 2 ). The total quantity of the material drawn from each container shall be sufficient to conduct the tests for all the characteristics given under 2 and shall not exceed 1 kg.

B-3.1.2 Thoroughly mix all portions of the material draw’n from the same container. Out of these portions, equal quantity shall be taken from each selected container and shall be well mixed up together so as to form a composite simple weighing not less than 1 kg. This composite sample shall be divided into three equal parts, one for the purchaser, another for the supplier and the third for the referee.

B-3.1.3. The remaining portion of the material from each container ( after the quantity needed for the formation of composite sample has been taken ) be divided into three equal parts, each part weighing not less than 100 g. These parts shall be immediately transferred to thoroughly dried bottles which are then sealed air-tight with stoppers and labelled with all the particulars of sampling given under B-1.0.

*Methods for random sampling.

13

lSt2520-19s4

The material in each test sample. These

such sealed bottle shall constitute an individual individual samples shall be separated into three

identical sets of samples in such a way that each set has an individual test sample representing each container selected. One of these three sets shall be sent to the purchaser, another to the supplier and the third shall be used as referee sample.

B-3.2 Referee Sample - The referee sample shall consist of the composite sample ( see B-3.1.2 ) and a set of individual samples ( SIC B-S.13 ) marked for this purpose and shall bear the seals of the purchaser and the supplier. These shall be kept at a place agreed to between the purchaser and the supplier and shall be used in case of dispute between the two.

14

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AMENDMENT NO. 1 DECEMBER 1995 TO

IS 2520 : 1984 SPECIFICATION FOR ZINC STEARATE FOR COSMETIC INDUSTRY

( Second Revision )

[ Page 4, Table 1, SINo. (i), coZ3 ] -Substitute ‘12.5 to 14.5’ for ‘13.Oto 15.5’.

( Page 6, clause A-2, Determination of Zinc ) - Substitute the following for the existing:

‘A-2.1 Reagents

A-2.1.1 Sulplluric Acid - 0.1 N.

A-2.1.2 Strong Ammonia - Ammonium Chloride solution - Dissolve 67.5 g of Ammonium Chloride in 740 ml of Ammonia solution (25% w/w) and add sufficient water to produce 1000 ml.

A-2.1.3 Erichome Black T Solution - Dissolve 0.20 g of Erichrome Black T and 2 g of Hydroxylamine hydrochloride in sufficient methyl alcohol to produce 50 ml. This solution must be freshly prepared.

A-2.1.4 Standard Disodium Ethylenediamine Tetra Acetate Solution - 0.05 M.

A-2.2 Procedure - Weight accurately about 1 g of material and boil with 50 ml of O.lN Sulphuric acid until the fatty acid layer which separates is clear, adding mote water as necessary to maintain the original volume; cool and filter. Wash thoroughly with water until the last washing is not acid to litmus paper. Add to the combined filtrate and washings, 15 ml of strong Ammonia - Ammonium Chloride solution and 0.2 ml of Erichrome Black T Solution. Heat the solution to about 40°C and titrate with 0.05M Disodium Ethylenediamine tetra acetate until the solution is deep blue in colour.

A-2.3 Calculation

Zinc as ZnO, percent by mass = 8.138xVx M

m where

V = volume in ml of Disodium Ethylenediamine tetra acetate solution,

M = molarity of Disodium Ethylenediamine tetra acetate solution, and

m = weight of the material in g.

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