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in order to promote transparency and accountability in the working of every public authority,
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“The Right to Information, The Right to Live” “Step Out From the Old to the New”

IS 13658 (1993): Polyglycerol Esters of Fatty Acids, Food

Grade [FAD 8: Food Additives]

“!ान $ एक न' भारत का +नम-ण”

Satyanarayan Gangaram Pitroda
“Invent a New India Using Knowledge”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता ह”

है”
ह
Bhartṛhari—Nītiśatakam
“Knowledge is such a treasure which cannot be stolen”
 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 STANDARDS
MANAK BHAVAN. 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

JUlIe 1993 Price GroDp 3

 AMENDMENT NO. 1 FEBRUARY 2006
TO
IS 13658: 1993 POLYGLYCEROL ESTERS OF FATIY
ACIDS, FOOD GRADE - SPECIFICATION
(Page 1, clause 2.1 ) - Substitute '1699 : 1995 Methods of sampling and
test for food colours (second revision )' for '1699 : 1974 Methods of sampling
and 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, 81 No. (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 serial
numbers.
[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: 1974 and 18 of68'4: 1973'.

(Page 2, clause S.l, line 5 ) - Substitute '4 of IS 1699 : 1995' for '3 of
IS 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 the
Food 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 of
substances, generally in small quantities, to improve the appearance, flavour, texture or storage
properties and in some cases to enhance the nutritive values of the processed foods. As certain impurities
in these substances have been found to be harmful, it is necessary to have strict quality control of these
food additives. A series of standards is, therefore, being prepared by the Bureau to cover purity and
identification of these substances. These standards would help in checking purity which requires to be
checked at the stage of manufacture, for it is extremely difficult ( and in many cases impossible) to
detect the impurity, once these substances have been added to the processed foods. Besides, these
standards are intended to guide the indigenous manufacturers in making their product conform to
specifications 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 acid
esters are the esters of fatty acids of food fats with a mixture of polyglycerols. They may also be prepa-
red by the transesterification of a mixture of polyglycerols with edible fats in which case the product
may contain residual mono and diglycerides.
Polyglycerol esters of fatty acids are being permitted for use as release agents in bakery industry and
in chocolate manufacture.
Structural Formula
The major components have the following general formula;

OR2
I
.R,O - (CH2-CH - CH2 O)n - R3

where the average value of n is about 3 and RJ , R. and R s each may be a fatty acid moiety or
hydrogen.
In the preparation of this standard due consideration has been given to the provisions of the Prevention
of Food Adulteration Act, 19.5~ and the Rules framed thereunder an~ the Standards of Weights and
Measures ( Packaged Commodittes t Rules. 1977. However, this standard IS subject to the restrictions
imposed under these, wherever applicable.
This standard is based on the BEe Directive No. 78/663/EEC laying down specific criteria of purity for
emulsifiers, stabilizers, thickncrs and gelling agents for use in foodstuffs. Considerable assistance
has 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 Agriculture
Organization 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, the
final value, observed or calculated, expressing the result of a test or analysis, shall be rounded off in
accordance with IS 2: 1960 'Rules for rounding off numerical values (revised )'. The number of
significant places retained in the rounded off value should be the same as that of the specified value in
this standard.
 IS 13658 : 1993

Indian Standard
POLYGLYCEROL ESTERS OF FATTY ACIDS,
FOOD GRADE - SPECIFICATION
1 SCOPE The esters range fro111 very hydrophilic to very
This standard prescribes the requirementsand methods lipophilic but as 8 class tend to be dispersible in water
of, ~all1pli~~ and test for polyglycerol esters of fatty and soluble in organic solvents and oils.
acids. 3.1.1 The product shall give 8 positive test for fatty
% REJ4~EREN(~ES acids when determined by the method of test given in
AnnexA.
%.1 The following Indian Standards are necessary 3.2.3 Spot 5 to 20 III of tbe aqueous layer obtained
adjuncts to tbis standard: . i 11 A-I.I.I alongside control spots of glycerol on
IS No. Title paper such as Whatman No.3 and develop using
S48 Method of sampling and test for oils and descending chromatography for 36 hours with
(part 1): fats: Part 1 Methods of sampling, physi- isopropanol : water 90 : 1 (v/v), The glycerol spot
1964 cal and chemical tests moves 40 em and the polygJycerols are revealed in
succession below that for glycerol wben the paper is
1070 :1992 Reagent grade water (third revision) sprayed with either permanganate in acetone or am-
1699 : 1974 Methods for sampling and tests for food monlacal silver nitrate.
colours (first revision) 3.3 Purity Tests
6854 : 1973 Method of sampling and test for in- 3.3.1 Acids
gredients used in media for micro-
biological work Acids other tban fatty acids shall not be detectable
when tested by the method given in Annex B.
11912 :1986 Lime oil, distilled, food grade
3.3.% Polyglycerols
3 REQUIREMJ4:NTS
The polyglycerol moiety shall be composed of not less
3.1 Description than 75 percent of di, lei and tetraglycerols and sball
Polyglycerol esters of fatty acids are yellowish to contain not more tba111 0 percent of polyglycerols equal
amber unctuous liquids, senti-solids or waxy solids. to or higher tban heptaglyccrol when tested by the
method given in Annex C.
3.% Identification Tests
3.3.3 The materials shall also conform to the require-
3.%.1 Solubility lUCIUS 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, percent by mass, 90 Annex D
Mill
ii) Free fauy acids (estimatedas oleic acid),percentby 6 7 of IS S48~Part 1) : 1964
mass, Max
iii) Total glycerol and polyglycerol, percent by mass 18-60 Annex C and E
tv) Free glycerol and polyglyeerol, percent by mass, 7 AnnexC and F
Max
v) Sulphated ash, percent hy 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 of
6854:1973
x) Zi~c. ma/kg, Max 2S 18 of IS 6854 : 1973
IS 13658 : 1993
4 PA(~KIN(;, STORAGE AND MARKIN(~ t) Any other details required as per the Standards
4.1 PackillR of Weigh's and Measures (Packaged Com-
modities) Rules, 1977/PFA Rules. -
The mntcrial sll.11I be sccurelv packed III well-filled
containers with mimmum accessto light and moisture. 4.3.1 The container may also be marked with the
The containers shall be such as to preclude contamlna- Standard Mark.
tion of the contents with metal or other impurities, S SAMPLING
4.2 Storage 5.1 Representative samples of the ·nutterial shall be
The material sball be stored in 8 cool and dry place so drawn and conformity of the material to the require-
as to aviod excessive exposure to heat. ments of this speciflcation sba IJ be determined accord-
ing to the procedure prescribed in 3 of IS 1699: 1974.
4.3 Marking
, TESTS
Each container shall be legibly marked to give the
following informatiou: 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.
a) Name oftbe material including the words 'food
grade'; 6.1 Quality of Reagents
b) Source of manufacture; Unless specified otherwise, pure chemicals altd dis-
c) Minimum net n18SS of the contents; tilled water (see IS 1070 : 1992) shall be employed in
d) Balch or code number; tests.
e) Date of 111ai,ufacture; and N01'E - 'Pure chemicals' shall mean chemicals that
do not contain impurities which affect the test results.

ANNEX A
(Clause 3.2.2)

A-I PROCEll(JRE produced which is soluble inS ml of hexane.

A-I.I Reflux 1 g of sample with 15 lui of 0.5 N A-I.I.1 Rel110Ve tbe hexane layer. Extract again with
ethanolic potassium hydroxide for 1 hour. Add 15 lui 5 lui or hexane and again remove the hexane layer. Use'
of water, acidify with about 6 lui of dilute hydrochloric the aqueous layer for detection of acids other than fatty
acid. Oily drops or a white to yellowish while solid is acids.

ANNEX B
(Clause 3.3.1)

8-1 PROCEDlJRE (see A-t.l.l) and a drop of 8 0.5% solution of am-

B-l.1 AceticAcid monium chloride a ud several mgof zinc powderinto a
micro test tube.
D-l.l.l Transfer about- 5 ml of tbe aqueous layer
(see A-I.I.I) into a dish. Add excess calcium carbonate
and eY~i()rate until dry. Transfer the major part of the
residue 111M a glass tube. Place a filter paper, moistened
with reaS-1l1 for acetone (8 saturated solution of 0- METAL SPIRAL
nitrobcll1J'ldehyde in sodium hydroxide, freshly
prepared) 011 the top of the tube. Heal .as indicated in
Fig. I.
ASBESTOS ----==:.:..=....... =.:.
The yellow colour of tbe paper changes into greenish
blue by reaction of the reagent for acetone, with the
calcium acetate formed, MICRO FLAME
8-1.% Succinic Acid
B-l.2.1 Transfer one drop of the aqueous layer .
FIG. 1 HEATING ARRANGEMENT
.

2

8-1.%.% The mouth·of the tube is covered with II disk
of filter paper moistened with II solution, in benzene, of
5% p-dimethylamiuobeuzaldehydc and 20(~
trichloroacetic acid. The bottom of the test tube is
healed vigorously with a micro flame (Fig.I) for about
1 I1UllUtC. Depending on the 8111oU11t of succinic acid or
succinimlde.e red-violet or pinkstainappears onthe paper.
0-1.3 FUDlaric Acid
Transfer 1 1111 of the aqueous layer (see A-I.l.l) with
l ml of2N sodium carbonate into 8 test tube. Add 2 or
3 drops of 0.1 N potassium pennauganate. The solution
is promptly discoloured. . into a test tube and place for 2 minutes in hoiling
8-1.4 'rartaric Acid
Evaporate about 5 lui of'the a(IUCOUS layer (see A-I.I.I)
in a porcelain disb until dry. Add 2 lui of concentrated
sulphuric acid containing O.5(~ of pyrogallol and heat
011 a steam bath. An intense violet colour is produced.
B-l.5 Cltrie Acid
B-I.!.1 To 3 ml of tbe aqueous layer (see A-I.I.I) add
a few drops of 1% potassium permanganatc and warm
IS 13658 : 1993
until the colour has disappeared. Then add an eXl"CSS of
bromine solution. A white precipitate (pen-
tabromoacetone) is formed immediately on cooling.
11-1..5.2 Evaporate Inti of the aqueous layer resulting
from test in a porcelain dish, add 1 ml of II mixture of
1 volume acetic anhydride and 5 volume of pyridine
into the wann dish, A violet colour is produced. (Tar-
taric acid produces it green colour.)
0-1.6 Laetle Acid
n-l.6.1 Transfer 0.2 ml of tbe aqueous layer
(see A-I.I.I) add 2 lui of concentrated sulfuric acid
water. Cool and add t or 2 drops of it 5(~J guaiacol
solution in ethanol. A red colour is immediately
produced.
1)-1.6.2 If tartaric acid is present according to lest 5, it
must be removed as follows:
Transfer 3 1111 of the aqueous layer (see A-I.I.I)
and an excess of calcium hydroxide- as a powder
into a 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)]

e-l PRINCIPLE ilazane, shake, add 0.2 lui trimcthylchlorosllane and

PolygJycerol estersare saponitied withalcoholicpotas- shake again. Stand 011 a warn, plate (about 80) for 3-5
sium hydroxide solution a nd the fatty acids removed minutes, Check that white fumes arc present indicating
by extraction. The polyols are converted to uimethyl- an CXl"'CSS of reagent.
silyl ( TMS ) derivatives and analysed hy gas liquid C.2,.3 (ias-IJitluid l~hronlat{)graphy
chromatography. (~-Z.3.1 Any suitable gas chromatograph may be used
C-Z ))ROCEllURE equivalent to It Pyc Model 104 lilted witb a flame
e-l.l Pre parado 11 ot the Polyol Sample ionization detector and a column (1.5 In X 4 I11IU 1.0.)
packed with 3% OVI on Diatomite CO (100-120 mesh)
Weigh about 0.5 g of sample and reflux with 20 ml of or on Gas Chrom 0 (100-120 mesh).. Recommended
cthanolic potassium hydroxide solution (tN) for 2 conditions are: oven temperature, progranuned from
bourse Reduce tbe volume of ethanol hy evaporation at 90 ll to 330 0 at 4-6°/nlin; nitrogen currier gasflow rate,
45-50° in a stream of nitrogen, Add 10 1111 of water and 86 IUI/IUiu; injection blocktemperature, 275 0 ; detector
convert the soaps to free fatty acids by acidifying with blocktemperature, 350°.
concentrated hydrochJoric acid. Extract the fatty acids Inject a 2.0 III sample of TMS derivatives of polyoJs.
from the aqueous phase with successive20 11t1 portions The resultant chromatograph displays the following
of light petroleum extracts with water (20 ml) and sequence of peaks:
combine the wash with the aqueous phase.
Elution Identity Description (lind
Adjust the aqueous polyol solution to pH 7.0 wirb Sequence Typical Attenua-
aqueous potassium hydroxide solution with tbe aid of of Peaks tion Settings)
apH-lnetcr. Evaporate to a-snwll volume (2-311\1) under
reduced pressure and extract three times with 30 lui of 1. Solvent Overloaded
boiling ethanol. Filter off any residue: and evaporate the .2. Glycerol Sillglc.~eak
ethanol under reduced pressure to yield a viscous liquid (2 x 10·)
sample of polyols. 3. Cyclic diglycerols Single ~eak
Dissolve It 0.1 g sample of polyol ill 0.5 ml of warm (2 X 10-)
pyridine (previously dried over potassium hydroxide) 4. Diglyecrols Single peak
ill a 10 ml capped phial. Add 0.2 ml hexamethyl dis- (32 X 10")

3
IS 13658 : 1993

Elution Identity Description (lind Ellltion ldentity Description (lind

Sequence Typical Attenua- Sequence Typical Attenua-
of Peaks lion Settings} ofPetlks lion Seuings)
5. Cyclic triglycerols Single ~cak 12. Octaglycerols Single ~enk
(2 X 10-) (t x 10') .
13o N01UtgIYl~Cr()ls Barely discern-
6. Triglyccrols Single peak
(16 X lO-~) ible in the taiI of
peak 12.
7. Cyclic tetraglycerols Single ~eak
C-Z.3.3 Caiculation
(2 x 10·)
Measure each peak area by a suitable method and
8. 'Ictraglycerols Multiple peak correct for attenuation cha nges.
(8 X l()-~)
(~ di-, tri- and tetraglycerols
9. Peuraglycerols Single ~eak Sunlof corrected areas of peaks 3 to 8 xlOO
(4 X 10")
- Sum of corrected areas of peaks 3 to 13
to. Hexaglycerols Single ~cak
~) polygJycerols equaI to or greater tha11 hcptaglycerol
(2 )( lO·)
SUlll of corrcl1Otcd areas of peaks It to 13 X 100
11. Hcptaglycerols Single ~eak
(2 X 10') SUIl) of corrected areas of peaks 3 to 13

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

I).:l~":I~MINArrI()N or rorxr, J4A'I'''Y ACII) ES1"EI(S coxrsxr

1)-0 PI{IN( ~11)I.jE Erlenmeyer flask with 30 ml chloroform and transfer
A distribution of t.he starting material between II In the separating funnel. Then add tRO ml Witter and
chloroform and a water phase is established, and the mix the contents of the separating funnel.' Let the two
,..tauy aciids nrc extracted Ily l' hioro toouu, and id
estunate phases separate from CH("h other, Extract chloroform
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. Wash
1)-1.1 Chloroform tbe combined water phase, once, in a 500-1111 separating
D-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 bas heen removed, treat the flask further for
D-Z.~ Sepal-stil1g ."unnel- 1 litre 20 minutes at tbe distilling rotator. Dry the llask for 20
D-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 - I f 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-4 (~AL(~lJLATI()N
D-Z.7 Water Jet I-ump f
D-%.8 Heatillg CUpbOB.-d
Total fatty acid ester content, =~ X 100
D-1.9 Desiccator percent by 111HSS
D-3 PR()(~EDlIRE
where
D-3.1 Take 20 g ofa homogenoussample ofemulsifier
in a l-litre Erlenmeyer flask. Dissolve in 100 ml M = nU1SS, in g, of material taken for the test;
chloroform. Add to it 200 lui methanol and mix the Hnd
blend with a magnetic stirrer. After mixing, add another X = 111a~S, in g, of the material remaining in the
100 ml chloroform find continue the mixing. Transfer 500-lul round bouomed flask alter cooling
the solution into a t-litre separuting funnel, Wa~b tbe in the desiccator, .

4
 IS 13658 : 1993

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

(lJ4:TERMINATI()N ()F TOTALGLYCEROL

E-O PRINCIPLE solution and saponify the sample for 30 minutes by

The material is saponified with alcoholic potassium boiling under reflux.
hydroxide solution and the water soluble components After saponification neutralize, the sample with an
of the neutralized solutions are purified and determined equivalent amount of 0.5 N hydrochloric acid. Further
gravimetrically, add 0.5 ml hydrochloric acid. Distil off the alcohol in
E-l REA(-;ENTS the rotating evaporator. Transfer the contents of the
flask to a 500-nll separating funnel with 100 In) hexane
E-I.l AloohoUc Pota.4\Sium Hydroxide Solutiolt-0.5 N. and 25 1111 distilled water. Shake. After the separation,
E-l.Z Hydrochloric Acid- 0.5 N. transfer the water phase to a 200-1l11 flask fitted with
.:-1.3 Hexane (for analysis) NS 29. Wash the hexane phase two times with 25 ml
distilled water each time, Both the water phases are
E-l.4 Z-Propollol (for analysis) united with the first phase in tbe flask. Distil the water
.:-Z AI»))AI{Al'llS in the rotating evaporator. Dissolve the remaining
E-Z.l Erlenmeyer ....Iask - 300-1111. glycerol in 2- propanol and filter through a Whatman
filter paper No. 41 of9 em diameter into a 100-nll flask
E-Z.Z Separating J4~unnel-SOD-lui. fitted with NS 29. Wash the flask and filters with
E·Z.3 Round-Bottomed ....Iask - 200-n1l, with NS 2-propanol in order to transferthe sample quantitative-
29. ly. After distilling off the 2-propanol in the rotating
E-Z.4 Round-Bottomed Flask - l00-IUI, with NS evaporator on a water bath, apply full vacuum from the
79 . wa ter jet pump for 20 minutes followed by drying for
20 minutes in the beating cupboard and finally cool in
E·Z.S Water Bath the desiccator, Weigh.
•:-1.6 Rotatioll Evaporator NOTE- The tOO-1ll1 round-bottomed flask with NS 29 is first
E-Z.7 Wilter .Jet )lun1p dried alI05°<: and after cooling in a desiccatorweighedwith an
E-Z.S ~eatil1g Cupboard accuracy of 0.000 S g.
E·Z.9 Desiccator .:-4 (~AL(~lJtAl~)()N

.:-1.10 Condenser 1J X 100

Total glycerol, percent by mass =---
.:-3 PR()(:EIj.lfRE a
The analysis arc carried out in duplicate, Weigh 1 g of where
the polyglycerol ester in a 300-1111 Erlenmeyer flask, b = mass, in S, of the dried polyalcohol phase; and
Add 25 ml of 0.5 N alcoholic potassium hydroxide II =mass, in g, of the ester.

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

F·O A distrioution of tbe starting material betwen a F-Z.I Erlenmeyer Flask -I-litre.
chloroform phase and a water phase is established, tbe F-2.2 Separatin~ Funnel-r-: l-litre.
, free glycerol collected front the water phase and es-
F·2.3 Separating .'unnel- 500-1111.
timated after drying the water phase.
.~·Z.4 Rcund-Bottemed Flask - 500-1111.
•"'-1 Rt;A(iEN1'S
F·Z.5 Ma~netic Stirn.·
F-l.l C1110rofoml
F-Z.' . Rotutiul\ t:,'uJlurutor
....·1.2 Methanol
f4""-Z.7 Water .Iet Pump
J...· l.3 Magnesiunl OllorideSolution illWater--l-Molar
F·Z.H Heatlng Cupboard
...·Z AIIPARXflJS
F-Z.9 Deslecator

5
IS 13658 : 1993

F-J PROCEDlJRE F·4 CALClJLATION

Proceed as given under D-3.1. Transfer the water phase . Mt
into a weighed 500-1111 round-bottomed flask and distil =
Freeglycerol, percent by 1l18SS 'Ai x 100
off the solvent in a rotating evaporator under vacuum
from a W8 ter jet pU111p. A'i soon as the cblorofonn and
tbe methanol has been distilled off, treat the flask where
further full vacuum in the rotating evaporator. Dry the
flask for 20 minutes ill a heating cupboard at 105°C and M1 = 1118SS, in g, of materialremauung ill the
alter cooling ill a desiccator, weigh, . 500 -ml round- bottomed flask; Bud
NOTE-If there is a tendency to emulsion formation, add 1 ml
of a 1 molar magnesium chloridesolution. 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- 10 percent (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 other
suitable container and add sufficient diluted sulpburic
acid to moisten the entire S8111ples. Heat gently, until
the sample is dry and thoroughlycharred, tben continue
heating until all tbe sample bas been volatilized or
nearly all of tile carbon bas been oxidized. Cool.
Moisten the residue with 0.1 1111 of sulphuric acid,
and heat in the same manner until tbe remainder of
the sample and any excess sulphuric acid have
been volatilized. Finally ignite ill a muffle furnace
at 800± 25°C for 15 minutes. Cool in a desiccator
and weigh.
G-l.3 Caleulatlen
- M
=
Sulphated ash, percent by mass ~ x 100
where
=
M 1 mass, in g, of residue; and
M = IU8SS, in g, of the material taken for the test.

6
IStallard
I
MulE
The use of the Standard Mark is governed by the provisions of the Bureau 01 Indian
I Standards Act, 1986 and the Rules and Regulations made thereunder. The Standard Mark on
. products covered by an Indian Standard conveys the assurance that they have been
produced to comply with the requirements of that standard under a well defined system of
inspection, testing and quality control which is devised and supervised by BIS and operated
by the producer. Standard marked products arc also continuously checked by DIS for con-
formity to that standard as a further safeguard. Details of conditions under which a licence
for the use of the Standard Mark may be granted to manufacturers or producers may be
obtained 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 promote
harmonioul development of the activities of standardization. marking and quality certification of
goods 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 any
form without the prior permission in writius 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 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 that
no changes are needed; if the review indicates that changes are needed, it is taken up for revisione
Users of Indian Standards should ascertain that they are in possession of the latest amendments or
edition 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

Headquarters:
Manak Bbavan, 9 Bahadur Shah War Marg, New Delhi 110002 Telegrams: Mandsaostha
Telephones: 331 01 31. 331 13 75 ( Common to all offices )
Regional Offices : Telephone
Central: Manak Bhavan, 9 Babadur Shah zafar Mars ~ 331 01 31
NEW DELHI 110002 l 331 13 75
Eastern: 1/14 C. I. T. Scheme VII M, V. I. P. Road, Maniktola ~ 37 84 99, 37 85 61
CALCUTTA 700054 l 37 86 26, 37 86 62
Norther. : sce 445·446, Sector 3S-e, CHANDIGARH 160036 ( 53 38 43, 53 16 40
l 53 23 84
Southern: C. I. T. Campus, IV Cross Road, MADRAS 600113 ~ 235 02 16, 235 04 42
l 235 IS 19, 235 23 IS
Western: Manakalaya, E9 MIDC, Marol, Andheri ( East) 632 92 9S, 632 78 58
BOMBAY 400093 { 632 78 91. 632 78 92

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.