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 13658 (1993): Polyglycerol Esters of Fatty Acids, FoodGrade [FAD 8: Food Additives]

IS 13868 : 1993

'IT<<iTlr 1JACf)

emf~ ~ qffurf~ij"m; ~fG(, ~TiT R - f~

Indian Standard

POLYGLYCBROL ESTERS OF FATTY ACIDS,FOOD GRADE - SPECIFICATION

UDC 544'099-6: 547-475-124

o DIS 1993

BUREAU OF INDIAN STANDARDSMANAK BHAVAN. 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

JUlIe 1993 Price GroDp 3

AMENDMENT NO. 1 FEBRUARY 2006TO

IS 13658: 1993 POLYGLYCEROL ESTERS OF FATIYACIDS, FOOD GRADE - SPECIFICATION

(Page 1, clause 2.1 ) - Substitute '1699 : 1995 Methods of sampling andtest for food colours (second revision )' for '1699 : 1974 Methods of samplingand test for foodcolours(first revision)'.

( Page 1, clause 3.2.3, line S ) - Substitute 'isopropanol: water, 90 : 10(v/v) , for 'isopropanol: water 90 : 1 (VN)'.

( Page 1, Table 1, 81No. (vi), col 4 ] - Substitute 'IS of IS 1699 : 1995' for '10

of IS 1699: 1974'.

( Page 1, Table 1 ) - Delete Sl No. (viii)and renumber the subsequent serialnumbers.

[Page 1, Table 1, SI No. (ix), col 4 ] - Substitute 'IS of IS 1699: 1995 and 18 of

IS 6854: 1973' for 'II of IS 1699: 1974and 18 of68'4: 1973'.

(Page 2, clause S.l, line 5 ) - Substitute '4 of IS 1699 : 1995' for '3 ofIS 1699 : 1974'.

(FAD 8)

RoprographyUnit, 81S, New Delhi, India

Food Additives Sectional Committee, FAD 8

FOREWORD

This Indian Standard was adopted by the Bureau of Indian Standards, after the draft finalized by theFood Additives Sectional Committee had been approved by the Food and Agriculture Division Council.

With the increased production of processed foods, manufacturers have started adding a large number ofsubstances, generally in small quantities, to improve the appearance, flavour, texture or storageproperties and in some cases to enhance the nutritive values of the processed foods. As certain impuritiesin these substances have been found to be harmful, it is necessary to have strict quality control of thesefood additives. A series of standards is, therefore, being prepared by the Bureau to cover purity andidentification of these substances. These standards would help in checking purity which requires to bechecked at the stage of manufacture, for it is extremely difficult ( and in many cases impossible) todetect the impurity, once these substances have been added to the processed foods. Besides, thesestandards are intended to guide the indigenous manufacturers in making their product conform tospecifications that are accepted by scientists, health authorities and international bodies.

Polyglycerol esters of fatty acids also known as polyglycerol fatty acid ester and glyceran fatty acidesters are the esters of fatty acids of food fats with a mixture of polyglycerols. They may also be prepa­red by the transesterification of a mixture of polyglycerols with edible fats in which case the productmay contain residual mono and diglycerides.

Polyglycerol esters of fatty acids are being permitted for use as release agents in bakery industry andin chocolate manufacture.

Structural FormulaThe major components have the following general formula;

OR2I

.R,O - (CH2-CH - CH2 O)n - R3

where the average value of n is about 3 and RJ, R. and Rs each may be a fatty acid moiety orhydrogen.

In the preparation of this standard due consideration has been given to the provisions of the Preventionof Food Adulteration Act, 19.5~ and the Rules framed thereunder an~ the Standards of Weights andMeasures ( Packaged Commodittes t Rules. 1977. However, this standard IS subject to the restrictionsimposed under these, wherever applicable.

This standard is based on the BEe Directive No. 78/663/EEC laying down specific criteria of purity foremulsifiers, stabilizers, thickncrs and gelling agents for use in foodstuffs. Considerable assistancehas also been derived from the following publications:

Food and Nutrition Paper N~. ~ 'S~ecificatio,:, ~or identity an.d purity of thickening agents,anticaking agents, antimicrobials, antioxidants, emulsdiers'. Food and AgricultureOrganization of the United 'Natioas, Rome 1978.

Food Chemical Codex, 1981 pub. National Academy of Sciences and National Research Council,Washington DC, USA.

For the purpose of deciding whether a .particular requirement of this standard is complied with, thefinal value, observed or calculated, expressing the result of a test or analysis, shall be rounded off inaccordance 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 inthis standard.

IS 13658 : 1993

Indian Standard

POLYGLYCEROL ESTERS OF FATTY ACIDS,FOOD GRADE - SPECIFICATION

1 SCOPE

This standard prescribes the requirementsand methodsof, ~all1pli~~ and test for polyglycerol esters of fattyacids.

% REJ4~EREN(~ES

%.1 The following Indian Standards are necessaryadjuncts to tbis standard: .

IS No. TitleS48 Method of sampling and test for oils and

(part 1): fats: Part 1 Methods of sampling, physi-1964 cal and chemical tests

1070 :1992 Reagent grade water (third revision)1699 :1974 Methods for sampling and tests for food

colours (first revision)6854 :1973 Method of sampling and test for in­

gredients used in media for micro­biological work

11912 :1986 Lime oil, distilled, food grade

3 REQUIREMJ4:NTS

3.1 Description

Polyglycerol esters of fatty acids are yellowish toamberunctuous liquids, senti-solids or waxy solids.

3.% Identification Tests

3.%.1 Solubility

The esters range fro111 very hydrophilic to verylipophilic but as 8 class tend to be dispersible in waterand soluble in organic solvents and oils.3.1.1 The product shall give 8 positive test for fattyacids when determined by the method of test given inAnnexA.3.2.3 Spot 5 to 20 III of tbe aqueous layer obtainedi 11 A-I.I.I alongside control spots of glycerol onpaper such as Whatman No.3 and develop usingdescending chromatography for 36 hours withisopropanol : water 90 : 1 (v/v), The glycerol spotmoves 40 em and the polygJycerols are revealed insuccession below that for glycerol wben the paper issprayed with either permanganate in acetone or am­monlacal silver nitrate.

3.3 Purity Tests

3.3.1 Acids

Acids other tban fatty acids shall not be detectablewhen tested by the method given in Annex B.

3.3.% Polyglycerols

The polyglycerol moiety shall be composed of not lessthan 75 percent of di, lei and tetraglycerols and sballcontain notmore tba1110 percentof polyglycerols equalto or higher tban heptaglyccrol when tested by themethod given in Annex C.3.3.3 The materials shall also conform to the require­lUCIUS given in Table 1.

Table 1 Requirements for Polyglycerol Esters of Fatty Acids, Feed Grade

SINo. (~bar.deristics Requirelnents Method or Test,Ref to

( 1) (2) (3) (4)

i) Total fatty acid ester content, percentby mass, 90 Annex DMill

ii) Free fauyacids (estimatedas oleic acid),percentby 6 7 of IS S48~Part 1) : 1964mass,Max

iii) Totalglycerol and polyglycerol, percent by mass 18-60 Annex C and E

tv) Free glycerol and polyglyeerol, percent by mass, 7 AnnexC and FMax

v) Sulphatedash, percenthy mass,Mea O.S Annex G

vi) Arsenic(as As), m.vkg.Max 3 10 of IS 1699 : 1974

vii) Heavy metals (as Pb), mg/kg. Max 10 Annex B of IS 11912: 1986

viii) Lead (as Ph). Inglkg. MIlX 10 9 of IS 1699 : 1974

ix) Copperand Zinc, mg/kg, Max SO 11 of IS 1699 : 1974 and 18 of6854:1973

x) Zi~c. ma/kg, Max 2S 18 of IS 6854 : 1973

IS 13658: 1993

4 PA(~KIN(;, STORAGE AND MARKIN(~

4.1 PackillR

The mntcrial sll.11I be sccurelv packed III well-filledcontainers with mimmum accessto lightand moisture.The containers shall be such as to preclude contamlna­tion of the contents with metal or other impurities,

4.2 Storage

The material sball be stored in 8 cool and dry place soas to aviod excessive exposure to heat.

4.3 Marking

Each container shall be legibly marked to give thefollowing informatiou:

a) Name oftbe material including the words 'foodgrade';

b) Source of manufacture;c) Minimum net n18SS of the contents;d) Balch or code number;e) Date of 111ai,ufacture; and

t) Any other details required as per the Standardsof Weigh's and Measures (Packaged Com­modities) Rules, 1977/PFARules. -

4.3.1 The container may also be marked with theStandard Mark.

S SAMPLING

5.1 Representative samples of the ·nutterial shall bedrawn and conformity of the material to the require­mentsof this speciflcation sba IJ be determined accord­ing to the procedure prescribed in 3 of IS 1699: 1974.

, TESTS

6.1 Tesl~ shaII be carried out by tbe methods -8S

specified in 3.2.2, 3.2.3,3.3 and l'014 of Table 1.

6.1 Quality of Reagents

Unless specified otherwise, pure chemicals altd dis­tilled water (see IS 1070 : 1992) shall be employed intests.

N01'E - 'Pure chemicals' shall mean chemicals thatdo not contain impurities which affect the test results.

ANNEX A(Clause 3.2.2)

A-I PROCEll(JRE

A-I.I Reflux 1 g of sample with 15 lui of 0.5 Nethanolic potassium hydroxide for 1 hour. Add 15 luiof water, acidify with about 6 lui of dilute hydrochloricacid. Oily drops or a white to yellowish while solid is

produced which is soluble inS ml of hexane.

A-I.I.1 Rel110Ve tbe hexane layer. Extract again with5 lui or hexaneand again remove the hexane layer. Use'the aqueous layer for detection of acids other than fattyacids.

ANNEX B(Clause 3.3.1)

8-1 PROCEDlJRE

B-l.1 AceticAcid

D-l.l.l Transferabout- 5 ml of tbe aqueous layer(see A-I.I.I) into a dish. Add excess calcium carbonateand eY~i()rate until dry. Transfer the major part of theresidue 111M a glass tube. Place a filter paper, moistenedwith reaS-1l1 for acetone (8 saturated solution of 0­nitrobcll1J'ldehyde in sodium hydroxide, freshlyprepared) 011 the top of the tube. Heal .as indicated inFig. I.The yellow colour of tbe paper changes into greenishblue by reaction of the reagent for acetone, with thecalcium acetate formed,

8-1.% SuccinicAcid

B-l.2.1 Transfer one drop of the aqueous layer

2

(see A-t.l.l) and a drop of 8 0.5% solution of am­monium chloride audseveral mgof zinc powderinto amicro test tube.

METAL SPIRAL

ASBESTOS ----==:.:..=.......=.:.

MICRO FLAME. .FIG. 1 HEATING ARRANGEMENT

IS 13658 : 1993

8-1.%.% The mouth·of the tube is covered with II diskof filter paper moistened with II solution, in benzene,of5% p-dimethylamiuobeuzaldehydc and 20(~trichloroacetic acid. The bottom of the test tube ishealed vigorously with a micro flame (Fig.I) for about1 I1UllUtC. Depending on the 8111oU11t of succinic acid orsuccinimlde.e red-violet or pinkstainappears onthe paper.

0-1.3 FUDlaric Acid

Transfer 1 1111 of the aqueous layer (see A-I.l.l) withl ml of2N sodium carbonate into 8 test tube. Add 2 or3 drops of 0.1N potassium pennauganate. Thesolutionis promptlydiscoloured. .

8-1.4 'rartaric Acid

Evaporate about 5 luiof'the a(IUCOUS layer(seeA-I.I.I)in a porcelain disb until dry. Add 2 lui of concentratedsulphuric acid containing O.5(~ of pyrogallol and heat011 a steam bath. An intense violet colour is produced.

B-l.5 Cltrie Acid

B-I.!.1 To 3 ml of tbe aqueous layer (seeA-I.I.I) adda few drops of 1% potassiumpermanganatc and warm

until thecolour hasdisappeared. Then add an eXl"CSS ofbromine solution. A white precipitate (pen­tabromoacetone) is formed immediately on cooling.11-1..5.2 Evaporate Inti of the aqueous layer resultingfrom test in a porcelain dish, add 1 ml of II mixture of1 volume acetic anhydride and 5 volume of pyridineinto the wann dish, A violet colour is produced. (Tar­taric acid produces it green colour.)

0-1.6 Laetle Acid

n-l.6.1 Transfer 0.2 ml of tbe aqueous layer(seeA-I.I.I) add 2 lui of concentrated sulfuric acidinto a test tube and place for 2 minutes in hoilingwater. Cool and add t or 2 drops of it 5(~J guaiacolsolution in ethanol. A red colour is immediatelyproduced.1)-1.6.2 If tartaricacid is present according to lest 5, itmustbe removed as follows:

Transfer 3 1111 of the aqueous layer (see A-I.I.I)and an excess of calcium hydroxide- as a powderintoa test tube, place in boiling water for 5 minutes,shaking several times, cool and filter.

ANNEX C[Clause 3.3.2, Table 1, Sl N(). (iii) and (iv)]

Description (lindTypical Attenua­tion Settings)Overloaded

Sillglc.~eak

(2 x 10·)

Single ~eak

(2 X 10-)Single peak(32 X 10")

Diglyecrols

Cyclic diglycerols

SolventGlycerol

3.

4.

ilazane, shake, add 0.2 lui trimcthylchlorosllane andshake again. Stand 011 a warn, plate (about 80) for 3-5minutes,Check that white fumes arc present indicatingan CXl"'CSSof reagent.

C.2,.3 (ias-IJitluid l~hronlat{)graphy

(~-Z.3.1 Any suitable gas chromatograph may beusedequivalent to It Pyc Model 104 lilted witb a flameionization detector and a column (1.5 In X 4 I11IU 1.0.)packedwith3% OVI on Diatomite CO (100-120 mesh)or on Gas Chrom 0 (100-120 mesh)..Recommendedconditions are: oven temperature, progranuned from90ll to 3300 at 4-6°/nlin; nitrogen currier gasflow rate,86 IUI/IUiu; injection blocktemperature, 2750

; detectorblocktemperature, 350°.Inject a 2.0 III sample of TMS derivatives of polyoJs.The resultant chromatograph displays the followingsequence of peaks:Elution IdentitySequenceof Peaks

1..2.

e-l PRINCIPLEPolygJycerol estersaresaponitied withalcoholicpotas­sium hydroxide solution and the fatty acids removedby extraction. The polyols are converted to uimethyl­silyl ( TMS ) derivatives and analysed hy gas liquidchromatography.

C-Z ))ROCEllURE

e-l.l Preparado 11 ot the Polyol Sample

Weigh about 0.5 g of sample and reflux with 20 ml ofcthanolic potassium hydroxide solution (tN) for 2bourse Reduce tbe volume of ethanol hyevaporation at45-50° in a stream of nitrogen, Add 10 1111 of water andconvert the soaps to free fatty acids by acidifyingwithconcentrated hydrochJoric acid. Extract the fatty acidsfrom the aqueous phase with successive20 11t1 portionsof light petroleum extracts with water (20 ml) andcombine the wash with the aqueous phase.Adjust the aqueous polyol solution to pH 7.0 wirbaqueous potassium hydroxide solution with tbe aid ofapH-lnetcr.Evaporate to a-snwll volume(2-311\1) underreduced pressure andextract three times with 30 lui ofboiling ethanol. Filteroff any residue: and evaporate theethanol under reduced pressure to yielda viscous liquidsample of polyols.

Dissolve It 0.1 g sample of polyol ill 0.5 ml of warmpyridine (previously dried over potassium hydroxide)ill a 10 ml capped phial. Add 0.2 ml hexamethyl dis-

3

C-Z.3.3 Caiculation

Measure each peak area by a suitable method andcorrect for attenuation cha nges.

(~ di-, tri- and tetraglycerols

Sunlof corrected areas of peaks3 to 8 xlOO- Sum of corrected areas of peaks 3 to 13

~) polygJycerols equaI to or greater tha11 hcptaglycerolSUlll of corrcl1Otcd areas of peaks It to 13 X 100

SUIl) of corrected areas of peaks 3 to 13

IS 13658 : 1993

Elution Identity Description (lindSequence Typical Attenua-ofPeaks lion Settings}

5. Cyclic triglycerols Single ~cak

(2 X 10-)

6. Triglyccrols Single peak(16 X lO-~)

7. Cyclic tetraglycerols Single ~eak

(2 x 10·)

8. 'Ictraglycerols Multiple peak(8 X l()-~)

9. Peuraglycerols Single ~eak

(4 X 10")

to. Hexaglycerols Single ~cak

(2 )( lO·)

11. Hcptaglycerols Single ~eak

(2 X 10')

Ellltion ldentitySequenceofPetlks

12. Octaglycerols

13o N01UtgIYl~Cr()ls

Description (lindTypical Attenua­lion Seuings)

Single ~enk(t x 10') .Barely discern-ible in the taiI ofpeak 12.

ANNEXO[Table 1,51N(). (i)]

f

Total fatty acid ester content, =~ X 100percent by 111HSS

D-4 (~AL(~lJLATI()N

where

M = nU1SS, in g, of material taken for the test;Hnd

X = 111a~S, in g, of the material remaining in the500-lul round bouomed flask alter coolingin the desiccator, ..

D-3.1 Take 20 g ofa homogenoussample ofemulsifierin a l-litre Erlenmeyer flask. Dissolve in 100 mlchloroform. Add to it 200 lui methanol and mix theblend with a magnetic stirrer. After mixing, add another100 ml chloroform find continue the mixing. Transferthe solution into a t-litre separuting funnel, Wa~b tbe

I).:l~":I~MINArrI()N or rorxr, J4A'I'''Y ACII) ES1"EI(S coxrsxr1)-0 PI{IN( ~11)I.jE Erlenmeyer flask with 30 ml chloroform and transferA distribution of t.he starting material between II In the separating funnel. Then add tRO ml Witter andchloroform and a water phase is established, and the mix the contents of the separating funnel.' Let the two,.. id d I hi to did phases separate from CH("h other, Extract chloroformtauy aci s nrc extracte ly l' oro ouu, an estunate I, I'

after distilling off tlll~ chloroform. phase two times with a lfl-ml mixture of 9 : 10-1)-1 1{1~(;~N'rS water: methanol.Alter separating, the water: methanol

mix is combined with the original water phase. Wash1)-1.1 Chloroform tbecombined waterphase, once, in a 500-1111 separatingD-l.2 Methanol funnel with 50 ml chloroform.

()-1.3 MagnesiuDI Chleride Solution in Water 1).3.1 Transfer the chloroform phase which contains-1 Molar. the fatty acid ester to a 500-0\1 round bouomed flask{)-2 AI»))l\ltATlJS and distil off the solvent in a rotational distilling ap-D 2 ElF"" paratus under vacuum ("CCUll a water jet JlUIUp. After tbe

-.1 sr enmeyer llsk- 1 litre chloroform basheen removed, treat the flask further forD-Z.~ Sepal-stil1g ."unnel- 1 litre 20 minutesat tbe distilling rotator. Dry the llask for 20D-2.3 Separatin" Funl1el- 500 ml minutes in a healing cupboard at 105°C and after C()oJ-

D-2.4 Round-Bottomed Flask - 500 lui ing in a desiccator weigh.1)-2.5 Magnetic Stirrer NOTE-If an emulsion is formed in the solvent,add 1 ml of a

I molarmagnesium chloride. solution.D-2.6 Rotatioll I~YDI)C)rat()r

D-Z.7 Water Jet I-ump

D-%.8 Heatillg CUpbOB.-dD-1.9 DesiccatorD-3 PR()(~EDlIRE

4

IS 13658 : 1993

ANNEXE[Table 1, 51 No. (iii)]

(lJ4:TERMINATI()N ()F TOTALGLYCEROL

E-O PRINCIPLE

The material is saponified with alcoholic potassiumhydroxide solution and the water soluble componentsof the neutralized solutions are purified and determinedgravimetrically,

E-l REA(-;ENTS

E-I.l AloohoUc Pota.4\Sium Hydroxide Solutiolt-0.5 N.E-l.Z Hydrochloric Acid- 0.5 N..:-1.3 Hexane (for analysis)E-l.4 Z-Propollol (for analysis).:-Z AI»))AI{Al'llS

E-Z.l Erlenmeyer ....Iask - 300-1111.

E-Z.Z Separating J4~unnel-SOD-lui.E·Z.3 Round-Bottomed ....Iask - 200-n1l, with NS29.E-Z.4 Round-Bottomed Flask - l00-IUI, with NS79.E·Z.S Water Bath•:-1.6 Rotatioll EvaporatorE-Z.7 Wilter .Jet )lun1pE-Z.S ~eatil1g Cupboard

E·Z.9 Desiccator

.:-1.10 Condenser

.:-3 PR()(:EIj.lfRE

The analysis arc carried out in duplicate, Weigh 1 g ofthe polyglycerol ester in a 300-1111 Erlenmeyer flask,Add 25 ml of 0.5 N alcoholic potassium hydroxide

solution and saponify the sample for 30 minutes byboiling under reflux.

After saponification neutralize, the sample with anequivalent amount of 0.5 N hydrochloric acid. Furtheradd 0.5 ml hydrochloric acid. Distil off the alcohol inthe rotating evaporator. Transfer the contents of theflask to a 500-nllseparating funnel with 100 In) hexaneand 25 1111 distilled water. Shake. After the separation,transfer the water phase to a 200-1l11 flask fitted withNS 29. Wash the hexane phase two times with 25 mldistilled water each time, Both the water phases areunited with the first phase in tbe flask. Distil the waterin the rotating evaporator. Dissolve the remainingglycerol in 2- propanol and filter through a Whatmanfilter paper No.41 of9 em diameter into a 100-nll flaskfitted with NS 29. Wash the flask and filters with2-propanol inorder to transferthe samplequantitative­ly. After distilling off the 2-propanol in the rotatingevaporator on a water bath, apply full vacuum from thewater jet pump for 20 minutes followed by drying for20 minutes in the beating cupboard and finally cool inthe desiccator, Weigh.

NOTE- The tOO-1ll1 round-bottomed flaskwith NS 29 is firstdriedalI05°<: and after coolingin a desiccatorweighedwith anaccuracyof 0.000 S g.

.:-4 (~AL(~lJtAl~)()N

1J X 100Total glycerol, percent by mass =--­

a

where

b = mass, in S, of the dried polyalcohol phase; andII =mass, in g, of the ester.

ANNEX F[Table 1, Sl No. (iv)]

F·O A distrioution of tbe starting material betwen achloroform phase and a water phase is established, tbe

, free glycerol collected front the water phase and es­timated after drying the water phase.

•"'-1 Rt;A(iEN1'S

F-l.l C1110rofoml

....·1.2 MethanolJ...·l.3 Magnesiunl OllorideSolution illWater--l-Molar...·Z AIIPARXflJS

5

F-Z.I Erlenmeyer Flask -I-litre.

F-2.2 Separatin~ Funnel-r-: l-litre.F·2.3 Separating .'unnel- 500-1111..~·Z.4 Rcund-Bottemed Flask - 500-1111.F·Z.5 Ma~netic Stirn.·

F-Z.' .Rotutiul\ t:,'uJlurutor

f4""-Z.7 Water .Iet PumpF·Z.H Heatlng CupboardF-Z.9 Deslecator

IS 13658 : 1993

F-J PROCEDlJRE

Proceedas given under D-3.1. Transfer the water phaseinto a weighed 500-1111 round-bottomed flaskand distiloff the solvent in a rotating evaporator under vacuumfrom a W8 ter jet pU111p. A'i soon as the cblorofonn andtbe methanol has been distilled off, treat the flaskfurther full vacuum in the rotating evaporator. Dry theflask for 20 minutes illa heatingcupboard at 105°C andalter cooling ill a desiccator, weigh, .

NOTE-If there is a tendency to emulsion formation, add 1 ml

of a 1 molar magnesium chloridesolution.

F·4 CALClJLATION

. MtFreeglycerol, percent by 1l18SS='Ai x 100

where

M 1 = 1118SS, in g, of material remauung ill the500 -ml round- bottomed flask; Bud

M =1118SS,in g, of tbe material taken for tbe test.

ANNEX G[Table 1,Sl Nt). (v)]

()ETERMINATION OF SlJLPHATED ASH

0-1 DETERMINATI()N os SlJLPHA1'ED ASH

G-I.l Reagents

G-I.I.I Dilute Sulphuric Acid- 10percent (mlv)

G-l.2 Procedure

Transfer about 2 g of tbe sample, accurately weigbed,to a tared 50-u1l to 100-lul platinum dish or othersuitable container and add sufficient diluted sulpburicacid to moisten the entire S8111ples. Heat gently, untilthe sample is dry and thoroughlycharred, tbencontinueheating until all tbe sample bas been volatilized ornearly all of tile carbon bas been oxidized. Cool.

6

Moisten the residue with 0.1 1111 of sulphuric acid,and heat in the same manner until tbe remainder ofthe sample and any excess sulphuric acid havebeen volatilized. Finally ignite ill a muffle furnaceat 800± 25°C for 15 minutes. Cool in a desiccatorand weigh.G-l.3 Caleulatlen

- MSulphated ash, percentby mass=~ x 100

whereM1 =mass, in g, of residue; andM = IU8SS, in g, of the material taken for the test.

IStallard MulEI The use of the Standard Mark is governed by the provisions of the Bureau 01 IndianI 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 ofinspection, testing and quality control which is devised and supervised by BIS and operatedby the producer. Standard marked products arc also continuously checked by DIS for con­formity to that standard as a further safeguard. Details of conditions under which a licencefor the use of the Standard Mark may be granted to manufacturers or producers may beobtained from the Bureau of Indian Standardl.

Bureau of IndiaD StaDdards

BIS is a statutory institution eltablished under the Bureau o/I"dla" Standa,tb Act, 1986 to promoteharmonioul development of the activities of standardization. marking and quality certification ofgoods and attendinl to connected matters in the country.

COPJrilbt

BIS has the copyrilht of all its publications. No part of these publications may be reproduced in anyform without the prior permission in writius of BIS. This does not preclude the free use, in the course ofimplementing the standard, of necessary details, such as symbols and sizes, type or grade desilDatioDs.Enquiries relatiDl to copyriaht be addressed to the Director ( Publications ), BIS.

Review of ladiaD Sta.dards

Amendments are issued to standards as the need arises on the basis of comments. Standards are an)'reviewed periodically; a standard along with amendments is reaffirmed when such review indicates thatno changes are needed; if the review indicates that changes are needed, it is taken up for revisioneUsers of Indian Standards should ascertain that they are in possession of the latest amendments oredition by referring to the latest issue of cBIS Handbook' and CStandards MODthly AdditioD.'.Comments OD this Indian Standard may be sent to BIS giving the following reference:

Doc: No. FAD 8 ( 0028 )

Amead_eau Illued 8lDce PublicatiOD

Amend No. Date of Issue Text Affected

BUREAU OP INDIAN STANDARDS

( 53 38 43,l 53 23 84

~ 235 02 16, 235 04 42l 235 IS 19, 235 23 IS

{632 92 9S, 632 78 58632 78 91. 632 78 92

Telegrams: Mandsaostha( Common to all offices )

Telephone

~ 331 01 31l 331 13 75

~ 37 84 99, 37 85 61l 37 86 26, 37 86 62

53 16 40

Headquarters:

Manak Bbavan, 9 Bahadur Shah War Marg, New Delhi 110002Telephones: 331 01 31. 331 13 75

Regional Offices :

Central: Manak Bhavan, 9 Babadur Shah zafar MarsNEW DELHI 110002

Eastern: 1/14 C. I. T. Scheme VII M, V. I. P. Road, ManiktolaCALCUTTA 700054

Norther. : sce 445·446, Sector 3S-e, CHANDIGARH 160036

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

Western: Manakalaya, E9 MIDC, Marol, Andheri ( East)BOMBAY 400093

Branches: AHMADABAD. BANGALORB. BHOPAL. BHUBANESHWAR.COIMBATORE. FARIDABAD. OHAZIABAD. GUWAHATT. HYDERABAD.JAIPUR. KANPUR. LUCKNOW. PATNA. THIRUVANANTHAPURAM.

Prla&ed at New IDdI. PdDt•• Pr••• Kbar'a. IAdI.