Disclosure to Promote the Right To Information

Whereas the Parliament of India has set out to provide a practical regime of right to information for citizens to secure access to information under the control of public authorities, in order to promote transparency and accountability in the working of every public authority, and whereas the attached publication of the Bureau of Indian Standards is of particular interest to the public, particularly disadvantaged communities and those engaged in the pursuit of education and knowledge, the attached public safety standard is made available to promote the timely dissemination of this information in an accurate manner to the public.

इंटरनेट मानक

“!ान $ एक न' भारत का +नम-ण”Satyanarayan Gangaram Pitroda

“Invent a New India Using Knowledge”

“प0रा1 को छोड न' 5 तरफ”Jawaharlal Nehru

“Step Out From the Old to the New”

“जान1 का अ+धकार, जी1 का अ+धकार”Mazdoor Kisan Shakti Sangathan

“The Right to Information, The Right to Live”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता है”Bhartṛhari—Nītiśatakam

“Knowledge is such a treasure which cannot be stolen”

“Invent a New India Using Knowledge”

है”ह”ह

IS 4887 (1980): Petroleum Jelly for Cosmetic Industry [PCD19: Cosmetics]

1S :4887-1980

Indian Standard

SPECIFICATION FORPETROLEUM JELLY FOR COSMETIC INDUSTRY

( First Revision).-,I\l~ez First Reprint APRIL 1990

UDC 665.> 772.3 :665.58

....

-.1.1)~-.

@ Copyright 1981

BUREAU OF INDIAN STANDARDSMANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

Gr 5 \ March 1981

— ---— .—— —,,,,..-—. . . .. . .. ......—...—-_—

1$:4887= 19S0

Zndkzn Standard

SPECIFICATION FORPETROLEUM JELLY FOR COSMETIC

( First Revision)

INDUSTRY

Cosmetics Sectional Committee, P(2DC 19

Chairman Rsprsssntilsg

DE S. S. GOTE08KAB Dire~t~r;ta General of Health Services, New

MssnbsrsSHRX N. C. CEAmTn$EX National Test House, CaIcuttaSEmIV. G. DSIEEPANDn Ciba-Geigy of India Ltd, Bombay

DE S. S. KA~HAE~l? ( 4ftSTlUSt6)Snnx W. M. FICSLIUNDSSS Food & Drug Administration, Government of

Maharashtra, BombayBenszal Chemical & Pharmaceutical Works Ltd,Srim GURMW~ISSmwm

SEBI Pnoma ROY ~ Ahrss4)DB S. N. lYm?

SMTUSHA R. JOSHI ( Albrnats )SERI R. C. MEIITA

DB M. A. PATISL( Altunats )DE K. S. NAPAYU

DwA. T. KAJI ( Aftsn@ )SHIU N. A. NISSEALXASSSEEI F. F. PATANWALA

SEEI N. K. SANYU ( ~ )SqBI S, RAMASWAXY

‘Calcutta

Johnson&Johnson Ltd, Bombay

Drugs ‘Control Administration, Government of@ujarat, Ahmadabad. . .

Hindudltan Lever Ltd, Borribay’

Fragtarkce & F1aiwhtt Association, BombayMessrs E, S. ,Pmanwala, Bombay

Dire;tctWat;e~k#ralof Technical Development,

SirExS. N. AOABWAL( XWauts )Sm K. S. RAO Swsstik Household and Industrial Products Pvt

Ltd, Bombayfhmx C, R. KaISEI!SAISOOBTstY ( 4srnst8 )

SrsaI D. J. RIBmXEO Lakme’ Limited, BombaySEstx B.S. BABVB( Al&smuts)

Dn S. K.’RoY Central Dru@”Laboratory, CalcuttaDs P. -C. Ban ( ~~ )

( Cosstiarmdon,@g# 2 )

@) Qsri&hs 19S1

BUREAU OF lNDLW STANWSThis pu~ication” is protacted under the Indiaa Ci&# & ( xv Of 1957 ) adreproductionin wholeor in part by any sneansexcept withwrittenp~mission of thepublishertill W deemed @ haan infris&xnesstof copyright ssnderthe said Act.

.

.

1S :4887-1980 .,

( Cod inued~mn page 1 )

Members Representing

SRRIS. ~. slcN Indian Soap and Toiletries Makers’ Association,Bombay

SIIRI V. S1’1’.4llAll Basic Chemicals, Pharmaceuticals & CosmeticsExport Promotion Council, Bombay

SNRI I. SUNDARESIS ( Alternate)Swr US1[A SUKTIiANKAXi Consumer’s Guidance Society, Bombay

SMT USNA KAMERIKAn ( Alternate)Smu M. S. TII.41HJrt G odrej Soapa Ltd, Bombay

S]lRI N. G, IYER ( Aftemate )SHR1 M. S. SAXENA, Director General, 1S1, ( Ex-oJjcio Member)

Director ( P & C )

SecwtarySHRI Asssiox KUMAR

Deputy Director ( P & C )

Raw Materials and Gras List Subcommittee, PCDC 19:1

convene?SIiM D. J. RIBEIRO Lakme’ Ltd, Bombay

Members

SHR1 B. S. IIARVE ( Alternate toShri D. J. Ribeiro )

ASSIS’rAN~ COMJMSIONER Food and Drugs Administration, Government ofMaharashtra, Bombay

SENIOTt SCIE~TIBIC OSWICER ( Alferyste 1 .SIiRI V. G. DEWPANDEDn S. N. IYER f%%!!ky;!#%%?%%$

STWTUSHA R: JOSEI ( Alternate )SHRI R. C. MEIiTA Drugs Control Administration, Government of

Gujarat, AhmadabadDn K. S. NARAYAN I-Iindustan Lever Ltd, Bombay

Dn A. T, ICAJI ( Alternate)SHRX K. S. RAO Swastik Household & Industrial prOductJ I%t

Ltd, BombaySNTWC. R. KRXSHNAXKUBTKY ( .4fkfnate )

SHRI K. L. RArHJ Sudarsbaa Chemical Industries Ltd, puneSNXU U. N. LX?dAYIS( Altmafc )

DR S. K. l<OY Central Drugs Laboratory, CalcuttaD~ P. C. &!5~ ( Alt~w:e )

DR N. D. SHAH Ge@ey M:nnem,& Co Ltd, BOmbSYIX M. M. ~oem ( Alt&?sate ).

SBRI NAvINOEANDn-+ R. SEA5i Devar&ss Pvt Ltd; AhmadabadSHRI VINODOHANDBA K. MEETA ( Alternaie)

SHRI M, S. THAKUR ~ Godrej Soaps Ltd, Bombay/ SHRX N. G. IYEB ( Alternate)

,.

2:

.s ;a..m-&

IS t 4887-1980

Indkm Standard

SPECIFICATION FORPETROLEUM JELLY FOR COSMETIC INDUSTRY

(First Revision)

0. FOREWORD

0.1 This Indian Standard ( First Revision) was adopted by the IndianStandards Institution on 24 October 1980, after the draft finalized by theCosmetics Sectional Committee had been approved by the Petroleum,Coal and Related Products Division Council.

0.2 This standard was originally issued in 1968. Initial] y while reviewingthe standard the committee had agreed to indicate separately the essentialand optional requirements. Subsequently, this was found non-implemen-table for certification and therefore a single set of only requirements wasdecided to be specified. In this revision the requirements of kinematicviscosity and relative density have been dropped, A IMWrequirement oflight absorption has been added. Changes have also been made in thedescription, fluorescence and packing of the materiaL All other changesconsidered necessary to align the standard, with others in the series onraw materials fir cosmetics have also been introduced.0.3 Petroleum jelly is a soft, semi-solid material obtained from petroleumoils. It consists essentially of microcrystallh’k waxes in association withsubstantial quantities of oil.

0.4 Petroleum jelly is used in the manufacture of creams, rouges, lipsticks,lubricating creams, hair dressings, foundation creams of greasy type, etc.It is also employed as an emollient for chapped skin.

0.5 The requirement laid down in this standard cover the material for itsvarious application in the cosmetic i~dustry. Product-wise requirementshave not been laid down. ,{

0.6 For the purpose of deciding, whether a particular requirement of this

$standard is complied with, the final value, observed or calculated, express-ing the result of a test r analysis, shall be rounded off in accordance

&with IS : 2-1960*. Th mber of significant places retained in therounded off value should be the same as that of the-specified value in thisstandard.

*Rules for raunding off numerical values ( rdwd.).

/’.5

IS :4887.1980

L SCOPE1.1 This standard pcc~ribes the requirements and methods of samplingand test for petroleum jelly for cosmetic industry.

2. REQUIREMENTS .

2.1 Description — Petroleum jelly shall be in the form of a translucent,soft mass, unctuous to the touch and retaining these characteristics onstorage and also when melted and allowed to cool w“thout stirring. Itshall be not more than slightly fluorescent by daylight, ~en when melted.

2.1.1 It shall be insoluble in water and alcohol but soluble in etherand chloroform.

2.2 Colour — The colour of the material shall be as agreed betweenthe purchaser and the supplier.

2.3 Odour — The material shall be odourless at room temperature whenrubbed on the skin. Further, the material when heated to 95 to 98°C ona boiling water-bath for 30 minutes shall give no disagreeable o,dour.2.4 The material, when tested according to the methods prescribed inAppendix A, shall also comply with the r~s$rcments given in Table 1.Reference to the relevant clauses of App+ndlx A is given in co] 4 of thetable. ,,:

TABLE1 REQUIREMENTSFOR PETROLIWMJELLY‘FORCOSNiETIGl1NDUSTR%

SLNo.

(1)

i)ii)

iii)iv)

v)

vi)vii)

viii)

ix)

4

xi)

xii)

CHARACTIUSXSTIO RBQtJIShUINT METSSODor TSIST( REB TO@ No. IM

APPENDIX A )(2) (3)

Melting range, ‘C 38 to 56Saponifiable matter NilFree acids and alkalis To pass the testArsenic ( as AS,03 ), parts per 2

million, MaxHeavy metals ( as Pb ), parts per 20’

million, MaxIodide value ( Wijs ), Max 1 “5Light absorption ( extinction of 1$0

@1 percent solution), MaxSulphated ash, percent by mass, Max 0“10Organic acids To pais the testSulphur and .wslpbides To pass the testConsistency 100 to 275 as agreed

between the pur-chaser and thesupplier /

Volatile matter, percent by mass, , 5“0Max

(4) -A-2A-3A-4A-5

A-6

A-7A-8

A-9 ‘A-10A-n .A-12

A-13

4.

~...mm-m —-- -...- .-.e _ . .,-, , ,.

1s14s87-1380,,

3. PACKING AND MAEKING

3.1 Pwdcbg — The material shall be packed in mild steeI drumslacquered from inside or as agreed between the purchaser and thesupplier.

Name and mass of the material in the container;

Manufacturer’s name and trade-mark, if any;Batch number in code or otherwise to enable the lot of manu-facture to be traced back from records; and

Year of manufacture.

The containers mtiy also be marked with the 1S1 Certification

3.2 Makking — The containers -shall be securely closed and Ie&iblymarked with the following information:

a)

b)

c)

d)

3.2.1Mark.

NOTn- The use of.the 1S1 Certification Mark is governed by the provisions o fthe Indian Standards Institution ( Certification Marks ) Act and the Rules andRegulations made thereunder. The 1S1 Mark on .f.wuktcts covered by an IndiinStandard conveys the assurance that they have beesvproriuced to comply with therequirements of that standard under a well-deiineds tern of inspection, testing and

rquality control w~lch is devised and supervised y 1S1 and operated by theproducer. 1S1 marked products are also continuously checked by ISI for conformityto that standard as a further safeguard. Details of conditions under which a licencefor the use of the 1S1 Certification Mark may be granted to manufacttirers .orprocessors, may be obtained from the lnd~n Standards Institution.

d. SAMPLING

4.1 The method of preparing representative test samples of the materialand the criteria for conformity shall be as prescribed in Appendix B.

APPENDIX A

( Clam 2.4)

METHODS OF TIZST FOR PETROLEUM JELLYFOR COSMETIC INDUSTRY

!

&lo QUALITY OF REAGENTS

A-1,1 Unless specified otherwise, pure chemicals and distilled water( see IS: 107O-1977* ) shall be used in tests.

NOTE — c Pure chemicals ‘ shall mean chemicals that do not contain impuritieswW1ch affect the results of analysis.

*specification for water for general lab~atory use ( setotid wuision ).

..+ 5

1s:4s87-19s0

A-2. DETERMINATION OF MELTING RANGE

A-2.1 Procedure

A-2.1.1 Melt a quantity of the sample slowly while stirring until itreaches a temperature of 90”C. Remove @e source of heat’ and allowthe molten sample to cool to a temperature of 8 to 10”C above theexpected melting range. Chill the bulb of a thermometer ( range 1 to100”C ) to -5°C, wipe it dry and while it is still cold, dip. it into the moltensample so that approximately half of the bulb is submerged. Withdrawit immediately and hold it vertically away from heat until the waxsurface dulls, then dip it for five minutes into a water-bath having atemperature not higher than 16”C.

A-2.1.2 Fix the thermometer prepared in A-2.1.1 securely in a test-tube so that its lowest point .is about 15 mm above the bottom of thetest-tube. -Suspend the test-tube in a water-bath adjusted at 16°C andraise the temperature of the bath at a rate of 2 deg/min up to ;30°C, thenchange to a rate of rise of 1 deg/min and note the temperature at whichthe first drop of the melted sample leaves -the thermometer. Repeat thedetermination twice on,a ~freshly melted portion of the sample. If thevariation in three detenmkations is less than one degree take the averageof the three as the melting range. If the variation in the three determi-nations is more than one degree, make two additional determinations andtake the average of the five.

A-3. DETERMINATION OF SAPONIFIABLE MATTER

A-3.1 Reagents

A-3.1.1 Methgl Ethyl Ketone — technical grade, stored in amber colouredbottle.

A-3.1.2 Standard Alcoholic Potassium Hydroxide Solution — 0s5 N,standardized before use.

A-3.1.3 Petroleum Ethtr — boiling range 80 to -lOO°C.

A-3.1.4 Standard Hydrochloric Acid — 0s5 N, accurately standardized.

A-3.1 ..5 Pheno@hthalein Indicator Solutioq — ~ percent solution in !35.pcrcent rectified spirit.

A-3.2 Procedure — Accurat ely weigh ‘in a flask about 5 g of the sampleand add 25 & 1 ml of methyl ethyl ketone, followed by 25 ml of standardalcoholic potassium hydroxide solution from a burette, Connect the flaskto a condenser and heat for 30 minutes after refluxing begins., -Disconn~ctthe condenser, add 50 ml of petroleum ether and titrate the solutlonwhile hot ( without re-heating ) with standard hydrochloric acid, using

~---—=------- —, ,. .!... ,,, ,, i-

Is t 4s07 - 1ss0

3 drops of phenolphthalein indicator. When the indicator colour is dis-charged, add 3 drops more of indicator; if this addition restores the colour,continue the. titration. Proceed in this manner until the end point isreached when the indicator colour is discharged and does not immediatelyreappear upon the addition of 3 more drops of indicator.

A-3.2.1 Run a blank under identical conditions.

A-3.2.2 The sample shall be taken to have passed ~the requirementprescribed in Table 1 if the blank reading does not dilTer from the samplereading by more than 01 ml.

A-4. TEST FOR EREE ACIDS AND ALKALIS

A-4.1 Reagents

A-4.1.1 Phenol~hthaltt% Indicator Solution -- same as in A-3.1.5.

A-4.1.2 Methyl Organge Indicator Solution — dissolve 0°01 g of methylorange in 100 ml of water.

A-4.2 Procedure — Take 35 g of the sample in a 250-ml separatingfunnel. Add to it 100 ml of boiling water and shake vigorously for5 minutes. Draw off the separated water layer in a beaker. Wash thesample further with two 50-mI portions. of boiling water and add thewashings again to the beaker. To the collective” washings, add one drop.of phenolphthalein indicator solution arid boil. If no pink colour isproduced, add 0.1 ml of methyl orange indicator and see if any red orpink colour is produced.

A-4.2.1 The ~ample shall be taken to have passk the test if neither ared colour is produced with phenolphthalein nor a red or pink colourproduced with methyl orange.

A-5. TEST FOR ARSENIC

A-5.1 Reagents

A-5.1.1 Concentrated Jufphuric Acid — see IS :266-1977*.

A-5.1.2 ConcentratedNitric Acid — see IS: 2641976T. u

A-5.2 Procedmre

A-5.2.1 Preparation of Sample — Weigh “2.000 g of the sample in aKjeldahl flask of 500 ml capacity. Add 15 ml of concentrated sulphuricacid followed by 4 ml of concentrated nitric acid. Heat cautiously. Adddrop by drop more nitric acid, if required, from a pipette to speed up the

Specification for sulphuric acid ( secondriun”sion).tSpacification for nitric acid (.wcondrgoision).

IS ~4887-1980

oxidation of the sample. The total amount of .@rie acid shall be notedfor use in the control test. When oxidation is complete, the solution isclear and faint yellow, at that stage, add 2fI ml of water and again boilto fuming. Ensure removal of all nitric acid.

A-5.2.2 Carry out the test for arsenic with the solution preparedin A-5.2.1 as directed in IS : 2088-1971*. Compare the stain obtainedwith that produced with 0-004 g of arsenic tnoxide.

A-6. TEST FOR HEAV#METALS

A-6.1 Apparatus

A-6.1.1 .Nessler Gylinder.s — 50-ml capacity, matched. ~

A-6.2 Reagents

A-6.2.1 Ammonium Acetate Solution — 10 percent,

A-6.2.2 Amnronium Citrate Solution — Dissolve 8.75 g of citric acid inwater, neutralize with ammonia and dilute with water to 100 ml.

A-6.2.3 Ammonium Hydroxide — 10 percent ( mlm ).

A 6.2.4 Potassium Cyarnde Solution — 10 percent ( mltn ).

A-6.2.5 Sodium $k’~hide Solution — 10 percent ( mjm ).

A-6.2.6 Standard Lead Solution — Dissolve 1“600 g of lead nitrate inwater, add 10 ml of concentrate ed nitric acid and dilute to 1000 ml.Pipette out 10 ml of the solution and dilute it again to 1000 ml with ~water. One millilitre of the final solution contains 001 rug of lead(as Pb ). The solution should be freshly prepared.

A-6.3 “Procedure

A-6.3.1 Preparation of Sample — Treat 20000 g of ilm sample asprescribed in A-.5,2.1.

A-6.3.2 Take the solution prepared in A&&l in. a .~--, cyw:er,add 10 ml of ammonium acetate solution* 5 ml of azmrxmiusxz “citratesolution, 5 ml of ammonium hydrom”de W j,# of potassitmx cyanidesolution and dilute to 50 ml with wmteq t$em @ two drops of sodiumsulphide solution and fix well. In ammtltcr l%asler cylinder, carry otita control test using 4 ml of standard lead soltion anrl b same quantitiesof other reagents as used in the test wi~ the material.

A-6.3.3 Th~ material shall be taken as tit having exceeded the limitprescribed in Table 1 if the intensity of dour produced with the materiaJis not greater than that produced in the control test.

●Methods for determination of arsenic (fist rdien ).

8

IS: 4S87 ● Ml@

A-7. DETERMINATION OF IODINE-VALUE

A.7.O Omtline of the Metlmd – The material is treated with a knownexcess of iodine monochloride solution in glacial acetic acid. The excessof iodine monochloride is determined iod~metrically.

A-7.1 Apparatus

A-7.1.1 Thermometer — An engraved stem thermometer, calibratedbetween 10°C and 65°Cl in O-l degree intervals and with the O°C pointmarked on the stem is recommended. The thermometer shall have anauxiliary reservoir at the upper end$ and length of about 370 mrn anddiameter of about 6 mm.

A-7.2.1 Carbon Tetrac/tloride or Chloroform

A-7.2.2 Acetic Acid — glacial, 99 percent, having a melting -point of14S8°C and free from reducing im’purities. Determine the melting pointof the acetic acid and test it for reducing impunities as folbxvs:

a) Melting joint detertiation — Take a 15 crrx’long test-tube and fillit to abouttwo-thirds with the acetic aci& Insert into the-acid athermometer satisfying the requirements specified in A-72.1through a cork stopper fitting the test-tube. The amount of acidshould be at least double the quantity required to cover the bulbof the thermometer when the bottom of the latter is 12 mmfrom the bottoti of the test-tube. Suspend this tube within a“larger test-tube through a cork. Cool the acid by immersingthe assembly in ice water until the temperature is 10”C,then withdraw the assembly fr~m theice water and stir the acidrather vigorously for a few mosncn~. thus causing t&e super-cooled Iiquidto crystallize partially and. gke a mixtme of liquidand solid acid. Take thermometer readi~ every 15 secondsand record that temperature , at which the reading remainsconstant for .at least two minutes, as the true. melting point.

b) Tat for reducing im#rities ( pots.rsium @rnrartgwIata kt-) — Dilute2-ml of the acetic acid with 10 ml of water and add 0.1 ml of0°1 N potassium permanganate solutionana maintain at 27-&2°C.\The test shall be taken aa having ~ satisfied if the pinkcolour is not discharged at the end ofhwo hourt.,.

A-7.23 Potassium Bichromate — finely graynd.

A-7.2.4 Starch Solution — Triturate 5 g of starch and 0“01 g of mercuriciodide with 30 ml of cold. water and. slow]y “p-it with stirring into onelitre of boiling water. Boil for 3 minutes. A.IIow & sol~ion to cool anddecant off the supernatant clear liquid.

...,

r. 9

-—— ._.- -.. -- Im=# 11<lk!~”

IS :4887-1980

A-7.2.5 Slandard Sodium Thiosul~hate Solution — 0.1 N ( see IS: 2316-1968*),

A-7.2.6 Chlorine Gas — dry.

A-7.2.7 Iodine Trichloride

A-7.2.8 Wa’js Iodine Monochlonde Solution— Prepare t~k solution byone of the following two methods, and store in a glass stoppered bottlein a cool place, protected from light and sealed with paraffin untiltakenfor use:

a) Dissolve 13 g of re-sublimed iodine in 1 Iitre of acetic acid, usinggentle heat if necessary, and determine the strength by titrationwith standard sodium thiosulphate solution. Set aside 50 to100 ml of the solution and introduce washed and dried chlorinegas into the remainder until the characteristic colour changeoccurs and the halogen content ‘is nearly doubled as ascertainedagain by titration. If the halogen content has been more thandoubled reduce it by adding the requisite quantity of the iodine-acetic acid solution. A slight excess of iodine does not harm,but avoid an excess of chlorine.

Example:

If the titration of 20 ml of original iodine-acetic -acid solutionrequires 22 ml of standard sodium thiosulphate solution then20 ml of the finished Wijs solution should require-between 43 and44 ml ( and not more than 44 ml ) of the same scdurnthiosulphate solution.

b) As an alternative method for preparing Wijs solution, d~olvc8 g of iodine trichloride in approxiniately 450 ml of acetic acid.Dissolve separately :9 g of iodine in 450 ml of acetic acid usingheat if necessary. Add gradually the iodine solution to the iodinetrichloride solution until the crdour has changed to reddish.brown. Add 50 ml more of iqlinc solution and dilute the mixturewith. acetic acid till 10 ml of the mixture are equivalent to 20 mlof standard sodium thiostdphate solution when the halogencontent is estimated by titration in the presence of an excess ofpotassium iodine and water. Heat the solution at 100°C for20 minutes and cool. Prevent access of water vapour in preparingthe solution.NOTIS— The method prescribed in (a) b referable to that prescr%ed in

i?(b) because of the instability of iodine trichlor e.,

●Methods of pre aration of 8tan&rd eolutiom for ccdorhuetric and volumetrk7analysis ( ,$rst rtiion .

10

---- . \-.— ,,, ,.—.—

IS: 40S7-1980

A-7.3 Procedure — Melt the material and filter through the filter paperto remove any impurities and she last traces of moisture. Make sure thatthe glass apparatus used is absolutely clean and dry. Weigh accurately,by difference, about 10 g of the sample, into a clean dry 500 ml glass-stoppered bottle to which 25 ml of carbon tetrachloride or chloroformhave ‘been added, and agitate to dissolve the contents. Add 25 ml-of Wijssolution. ( The quantity of Wijs solution added is 50 to 60 percent morethan the quantity required ) — Replace the glass stopper after wetting withpotassium iodide solution, swirl for intimate mixing, and allow to standin the dark for 45 minutes. Carry out a blank test simultaneously undersimilar experimental conditions. After standing, add 15 ml .of potassiumiodide solution and 100 ml of water, and titrate the liberated iodine withstandard sodium thiosulphate solution, swirling the contents of the bottlecontinuously to avdld any local excess, until the colour of the solution isstraw yellow. Add 05 ml of starch solution and continue the titrationuntil the blue cdour disappears.

A-7.4 Calculation

Iodine value =12 °69(11-S).V

M

where

B = volume in ml of standard sodium thiosulp~ate solutionrequired for the blank,

s = volume in ml of standard sodium thiosulphate solutionrequired for the material,

N = normality of standard sodium thiosulphate solution,and

A4 = mass in g of the material taken for the test.

A-S. DETERMINATION OF LIGHT ABSORPTION

A-O.O General — When radiation is passed through a layer of a solutioncontaining an absorbing substance, part of the radiation is absorbed; theintensity of the radiation emerging from the solution is less than theintensity of the radiation entering it. The magnitude of the absorptionis expressed in terms of the extinction, E which is defined by tile expres-sion, E = log 10 ( ]o/~), where ]0 is “the intensity of the radiation passing ,into the absorbing layer, and 1 is the intensity of the radiation passingout of it.

A-8.O.1 The ?xtincticm depends on the concentration of the absorbingsubstance in the solution and thickness of the absorbing layer talien formeasurement. For convenience of reference and for ease in calculations,the extinction of a l-cm .Iayer of a l-percent m/v solution has beenadopted.

1:1

18 t#87 -1980

A-U Apparatus

A-O.I.I S’ectrophotometer— Comprising of a source of energy, a devicefor selecting the wavelength band, a cell or holder ‘for the sample, adetector of radiant energy and a measuring device.

A-8.2 Procedure — Dissolve 01 g of petrcilemn jelly in 100 ml oftrimethylpentane and measure the extinction of the solution using 1 -cmcell at 290 nm ( 290 x 10-7 cm ).

A-9. DETERMINATION OF SULPHATED ASH

A-9.1 Reagents

A-9.1.1 Dilute Su@huric Acid — ap~ximately 5 N.

A-9.2 Procedure — He+ a porcelain or sillica dish of 30 to 100 mlcapacity lb rednps; cool and weigh. Place .abosst.20 g of the sample,accurately weigh~d, in the dish, Heat the W gesttly by -pmmM of aBunsen burner until the oil can he ignited at the ,xr$ltee. Remove the Iburner and allow the oil to burn completely, -g .eare that all the freecarbon on the sides of the dish is completely lmsmt. Heat the residue witha strong flame or in muffle furnace until all the -carbonaceous matter hasdisappeared. Cool the dish, add a few drctps of dilute sulphunc acid,heat gently to drive off the acid and then heat strarrgly. Cool the dishagain in the desiccator and weigh, Repeat the heating, cooling andweighing until constant mass is obtained.

A-9.3 Cakslatiors

m x 100-Sulphated ash, percent by mass = ~

wherem = mass in g of the residue, and

M = massing of the sample taken for tke test.

A-10. TEST FOR ORGANIC ACUDS

A-10.1 Reagents

A-10.l.l Dilute Rectijied S’irit - ppqxssmd by diluting one volmnt of95 percent rectified spirit with two volumes of water, and neutralized tophenolphthalein indicator.

A-10.I.2 Phenolpltthalein indicator — same as in A~.li?5.

A-10.I.3 St.ndard Sodium -H9droxide Solution — exactly 0°1 N.

A-10.2 Procedure _ To 20 g of the sample, add .100 ml of dilate reetiikdspirit, agitate thoroughly and heat to boiling. Add one milliiitre of

12

-—~-------- n“ ‘

Is s 4887-1980

phenolphthalein indicator and titrate rapidly with- standard sodiumhydroxide solution with vigorous agitation to a sharp p@k end point inthe alcohol water layer.

A-10.2.1 The material shall be taken to have passed the test if notmore than 0“4 ml of standard sodium hydroxide solution ii required forthe titration.

A-11. TEST FOR SULPHUR AND SULPHIDES

A-11.l Reagent

A-11.1.1 Cop}er-Stri@ — One ccntixneqe, in width, and freshly, polished.

A-11.2 Procedure - Melt in a beaker about 100 g of the, sample andkeep on a water-bath at a temperature of 95”C. Then place a strip ofcopper in the melted sample so that it is partially immersed and allow itto remain for 10 minutes.

A-11.2.1 The material shall be taken to have passed the test if thecopper strip used in the test shows ,no tarnishing when compared withanother similar freshly polished copper strip.

A-12. DETERMINATION OF CONSISTENCY

A-12.O Outline of the Method — Determination of consistency of thematerial is made by measuring the rmmtration of a standard cone at25-0 ~ 0°50C. “

.

A-12.1 Apparatus

A-12.1.1 Penetrometer — Any suitable pene~ometersDecified cone to droIJ vertically without amweciab]e~0 mm and which i~dicates achrately th< ~epth ofnearest 0“1 mm. The instrument shall have a table-to carry the test

which permits thefriction for at leastpenetration to the

sample, which may be adjusted horizontal bef- making the test. Amechanism for rekasing the clamp of the loade,d cone shall be provided.

A-12.1.2 Cone — Consisting of a conical body of brass. or corrosionresistant steel with detachable hardened ‘steel tip, constructed to cdnformto the dimensions and tolerances shown in Fig. 1. The total mbving mass,namely, that of the cone and its movable attachments, shall be 150”0+0” 1 g. The attachments consist of a rigid shaft having a suitable deviceat its lower end for engaging the cone. The outer surface should bepolished to a very smooth finish.

13

\

.— 4, :p -

1st 4@7’=1980 .

A-12.1.3 Constant TemperatureBath — A water-bath capable of regulationat 25(I + 05°C and of suitable design for conveniently bringing thesample container to the test temperature. The bath should be providedwith a cover to maintain tle temperature of the air above the” sample -at25°C.

A-12.1.4 Timing Device —-A stop-watch or other suitable instrumentcapable of measuring an interval of 5 seconds to within O‘2 second.

A-12.L5 Sample Container— Flat-bottomed, metal or glass cylinders thatare 100 + 5 mm in diameter and not less than 60 mm m height,

A-12.2 Procedsme — Melt the quantity of the s~ple at 82s0 & 2050C,pour into one or more of the sample containers, filling to within 6 mm ofthe brim. Cool at 25’0 & 2“5°C over a period of not ‘less than 16 hours,protecting from draughts. Two hours before the test, place the containersin a water-bath at 250 + 0*5”G. If tbe room temperature is below23°50C, or above 26”5°C, adjust the temperattme of the cone to 25oO+ 0“5°C by placing it in the water-bath. .

I/,.

‘OETACiASI “TIP-

N.G

ALTkRNArEW51GNFoRacos w

All dimensions in rnillimetrea.

FIG. 1 PENItTROM~TERCONR

I1

1SS4SS7.19S0

A-12.2.1 Without disturbing the surface bf the sample; place thecontainer on the penetrometer table, and lower the cone until the tip justtouches the top surface of the sample at a spot 25 to 38 mm from theedge of the container. Adjust the zero setting and quickly release theplunger, then hold it free for 5 seconds. Secure the plunger and readthe total penetration from the scale. Make 3 or more trials each so. spacedthat there is no overlapping of the areas of penetration. Where thepenetration exceeds 20 mm use a separate container of the sample foreach trial. Read the penetration to the nearest 0s 1 mm. Calculate theaverage of the three or more readings and conduct further trials to a totalof 10 if the individual results differ from the average by more than& 3 percent.

A-12.3 Calculation*

Consistency = 10A

where\

A = is the mean of all the values of penetration in mm.

A-13. DETERMINATION OF VOLATILE MATTER

A-13.O Outline of the Method

A-13.O.I The sample is weighed in petri/glass dish and kept in an ovenmaintained at 105 + l,oC. The loss in mass is calculated as a percentageof the mass of the sample taken.

A-13.1 APPARATUS

A-13.1.1 Petri/Glass Dishfs — made of heai-resistant glass, 90 to 100 mmin diameter and 7 to 10 mm in height ( sue IS: 2626-1972*).

A.13.I.2 Thermometer — Any suitabl$ thermometer having a range/from O to 1l~C.

A-13.1.3 Air-Oven — an electrically or gas-heated air--oven capable ofmaintaining temperature at 105 + l“C. :!!

A-13.2 PROCEDURE‘t “-”

A-13.2.1 Weigh about 10 g of the sample, accurately to the nearest0.1 g, in a tared petri/glass dish, distributing the sample in as uniform alayer as possible-with the help of spatula over the whole of’ the bottom ofthe dish. Keep it in the oven, maintained at 105+ 1°C. COO1 andweigh the petri/glass dish to a constant mass.

t

*Specificationfor petri dishes.

IS t 4887-1980

A-13.3 CALCULATION AND REPORT

A-13.3.1 Calculate and report the evaporation loss as follows:

Volatile matter percent = 100 (Ml — ~s )by mass, Max MI

where

Ml = mass in g of the sample taken for the test, andM2 = mass in g of the sample after the test.

APPENDIX B( Clause 4.1 )

SAMPLING OF PETROLEUM JELLY

H. GENER& REQUIREMENTS OF SAMPLING

B-1.O ln drawing, pre~aring, storing and handling test samples, thefollowing precautions and directions shall be Observed.

E-1.1 Samples shalI not be taken in an exposed place.

B-1.2 The sampling instrument shall be clean and diy.

B-1.3 Precautions shall be taken to protect the sam.plcs, the materialbeing sampled, the sampling instrument and the containers for samplesfrom adventitious contamination.

B-1.4 Tb draw a representative sample, the contents of each container’selected for sampling shall be mixed as thoroughly as possible by suitablemeans.

B-1.5 The samples shall be placed in ciean, dry, air-tight glaas or othersuitable means.

B-1.6 The sample containers shall be of SUC%size that they are almostcompletely filled by the sample. IB-1.7 Each sample con@iner shall be sealed air-tight with a suitablestopper after filling and marked with full details of sampling, the date ofsampling and the’year of manufacture of the material.

\

B-2. SCALE OF SA_N~ 1

IB-2.1 Lot — Alr the “containers in a single consignment of the materialdrawn from a single batch of manut%cture shall’ cxanstitute a lot. If ,a

l@

~__ -...--– . . . -—.——---III“-—..——

.

n;4tw.19d0

consignment is declared or known to consist of dtierent batches of manu-facture, the containers belonging to the same batch shall be groupedtogether and each such group shall constitute a separate lat.

B-2.1.1 Samples shall be tested from each lot for ascertainingconformity of the m?terial to the requirements of this specification.

B-2.2 The number of containers (n) to be chosen from the lot shall dependon the size of the lot (W) and shall be as gi,ven in Table 2.

B-2.3 The containers to be selected for sampling shall be chosen atrandom. In order to ensure randomness of selection, random numbertables shall be used. For gpidance and use of random number tables,IS: 4905-1968* may .be referred. In the absence of random numbertables, the following procedure may be adopted:

Starting from any container in the lot, cou~t them as 1, 2, 3,...up to r and so on in one order, where r is tie integral part of N/n. ~being the lot size and n the sample size. Every rth container thuscounted shall be withdrawn from the lot so -as to constitute therequired sample size.

TABLE2 NUMBEROF CONTAINERSTO BESELECTEDFOR SAMPLING

( Clause B-2.2)

LOT SJZE

(N)

(1)

up to 50

51 to 100

101 ,, 300 “301 ,, 500.501,, 1000

1001 and above

NUMBER or CONTAINEBSTO BE SELEG~ED

(n)

(2)

-345678

B-3. TEST SAMPLES AND REFEREE SAMPLE

B-%1 Preparation of Test Samples

B-3.1.1 Draw with an appropriate sampling instrument a small portionof “the material from different parts of each container selected ( seeTable 2 ). The total quantity of the material drawn from each containershall be .sullicient to conduct the tests for all the characteristics givenunder 2 and shall be not less than 250 g.

●Methods ”for random sampling.

17

\. . ... .—————.:.-m

k5:#e7-19d0

B-3.1.2 Thoroughly mix all portions of the materitd&awn &om thesame container. Out Of these portions, equal quantities shall be takenfrom each selected container and shall be well mixed up together so as toform a composite sample weighhg not less than 500 g. This compositesample shall be divided into three equal parts, one for the purchaser,another for the supplier and the third for the referee.

..

B-3.2 Referee Sample — The referee sample shall consist of a co~po-site sample marked for thh purpose and shall bear the seals. of thepurchaser and the supplier. It shall be kept at a place a@eed betweenthe purchaser and the supplier and shall be used in case of disputebetween the two.

B-40 NUMBER OF TESTS

B-4.l Tests for all the characteristics given in 2 and Table 1 shall beconducted on the composite sample. ,

B-5. CRITERIA FOR CONFORMITY “‘,,

‘ B-5.1 A lot shall be declared as con formkt@@~composite sample satisfies the requirements for &listed in 2 and in Table 1. If the requireruds @s*.~istics are not met, the lot shall be decla@ed. %$ -w~-~~crequirements of the specification. ,..

~

,, II

t

BUREAU OF INDIAN ST AN DA R-DS

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I

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[

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231083

{

6347169832

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62305~621 04\621 17

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-.. w —a-.. — ..=.., ___ ,___