Cocoa Butter Specification Is.1263 - 1986

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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.

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Mazdoor Kisan Shakti Sangathan Jawaharlal Nehru
“The Right to Information, The Right to Live” “Step Out From the Old to the New”

IS 1263 (1986): Cocoa Butter [FAD 6: Stimulant Foods]

“!ा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”

Bhartṛhari—Nītiśatakam
“Knowledge is such a treasure which cannot be stolen”
( Reaffirmed 2012 )
IS : 1263- 1986

Indian Standard
SPECIFICATION FOR
COCOA BUTTER

( Third Reoision )

Stimulant Foods Sectional Committee, AFDC 39

Chairman Representing
SHRI A. K. ROY Food Specialities Limited, Moga

Members
DR N. RAMAKRISHNAN( AIternate to
Shri A. K. Roy )
DR B. BANERJEE Tea Research Association, Calcutta
DR M. R. ULLAH ( Alternate )
DEPUTY DIRECTOR ( FI ) Quartermaster General’s Branch, Army Head-
quarters, New Delhi
ASSISTANTDIRECTOR (FI) (Alternate )
DIRECTOR Unit;~o~la$ers’ Association of Southern India,

SHRI V. RANGANATHAN( Alternate )


SHRI D. K. GHOSH Calcutta Tea Traders Association, Calcutta
SHRI S. S. KHA~~AN ( Alternate )
SHRI S. JAYARAMAN Coffee Board, Bangalore
CUP-TASTER ( Alternate )
SHRI S. KASTURI Government Analyst, Madras
DR G. L. KAUL Indian Council of Agricultural Research, New Delhi
SHRI T. A. SRIRAM ( Alternate )
DR S. L. KHOSLA Public Analyst, Government of Haryana, Chandigarh
SHRI S. K. ANAND ( Alternate )
SHRI V. P. MAHAJAN Indian Tea Association, Calcutta
SHRI Y. K. VOHRA ( Alternate )
SHRI R. MANSINGH Brooke Bond India Ltd, Calcutta
DR K. K. MITRA Tea Board, Calcutta
SHRI C. Y. PAL Hindustan Cocoa Products Limited, Bombay
SHRI S. J. KEKOBAD( Alternate )
SHRI K. RAMAKRISHNAPILLAI Kerala State Co-op Marketing Federation Limited,
Cochin
SHRI P. P. BHASKARAN( Alternate )
( Continued on page 2 )

@ Copyright 1987
BUREAU OF INDIAN STANDARDS
This publication is protected under the Indian Copyright Act ( XIV of 1957 ) and
reproduction in whole or in part by any means except with written permission of
the publisher shall be deemed to be an infringement of copyright under the said Act.
AMENDMENT NO. 1 DECEMBER 2009
TO
IS 1263 : 1986 SPECIFICATION FOR COCOA BUTTER
( Third Revision )

[Page 5, clause 3.2, Sl No. (d)] ― Substitute ‘Net quantity’ for ‘Net mass’.

[Page 5, clause 3.2, Sl No. (f)] ― Substitute the following for the existing:

‘Any other requirements as given under the Standards of Weights and Measures
(Packaged Commodities) Rules, 1977 and the Prevention of Food Adulteration
Act, 1955 and the Rules.’

(FAD 6)
Reprography Unit, BIS, New Delhi, India
IS : 1263- 1986

( Continued from page 1 )

Members Representing
DR P. K. RAMAIAH Central Coffee Research Institute, Chikmagalur
SECRETARY( CCFS ) Central Committee for Food Standards, New Delhi
SMT DEBI MUKHERJEE( Alternate )
DR M. L. SHANKARANARAYANA Central Food Technological Research Institute
( CSIR ), Mysore
DR S. B. SINGH Public Analyst, Government of U. P, Lucknow
SHRI DEEPAK SHOURIE Kothari General Foods Corporation Ltd, Madras
SHRI VIREN KAPOOR ( Alternate )
SHRI KAILASH VYAS Kaira District Co-op Milk Producers’ Union Ltd,
Anand
_____--
DR B. NARAIN ( Ahernate )
SHRI T. PURNANANDAM, Director General, BIS ( Ex-officio Member )
Director ( Agri & Food )

Secretary
SHRI S. K. DAS GUPTA
Joint Director ( Agri & Food ), BIS

Cocoa And Its Products Subcommittee, AFDC 39 : 3

Convener
SHRI V. H. SHAH Kaira District Co-operative Milk Producers’ Union
Limited, Anand

Members
SHRI KAILASH VYAS ( Alternate to
Shri V. H. Shah )
DEPUTY DIRECTOR ( FI ) Quartermaster General’s Branch, Army Head-
auarters. New Delhi
ASSISTANT DIRECTOR ( FI ) _ .
( Alternate )
DIRECTOR Central Plantation Crop Research Institute (ICAR),
Kesaragod
SHRI T. A. SRIRAM ( Alternate )
SHRI S. KASTURI Public Analyst, Government of Tamil Nadu, Madras
SHRI C. Y. PAL Hindustan Cocoa Products Ltd, Bombay
SH~I S. J. KEKOBAD ( Alternate )
SHRI M. C. POTHEN Amalgamated Malabar Estates Pvt Ltd, Calicut
SHRI N. G. GOPALAKRISHNARAO Central Food Technological Research Institute
( CSIR ), Mysore
SHRI M. G. SATHE Sathe Biscuit & Chocolate Co Ltd, Pune
THIRU J. S. SUNDERRAJ Agriculture Department, Government of Tamil
Nadu, Madras
THIRU N. SADAVISAM( Alternate )
SHRI E. VELAPPAN Directorate of Cocoa. Arecanut & Soices
Development, Calicut
SHRI M. S. LAKSHMANACHAR
( Alternate )

2
IS : 1263- 1986

Indian Standard
SPECIFICATION FOR
COCOA BUTTER

( Third Reoision )

0. FOREWORD

0.1 This Indian Standard was adopted by the Indian Standards Institution
on 15 April 1986, after the draft finalized by the Stimulant Foods
Sectional Committee had been approved by the Agricultural and Food
Products Division Council.

0.2 Since the second revision of this standard in 1980, considerable amount
of developments have taken place in improving quality of cocoa butter. In
this revised version single set of specification for cocoa butter has been
mentioned irrespective of its method of production. The requirement for
free fatty acids and unsaponifiable has been revised keeping in view the
actual ranges in which these values vary. Taking into consideration this
development and other technical changes, it was found necessary to issue
this third revised version of the standard with a view to making it up to
date.
0.3 Cocoa butter is the fat present in cocoa beans which are the seeds of
- Theobroma cacao L. It is generally used for the enhancement of the
organoleptic qualities of the chocolate.

0.4 While formulating this standard, due consideration has been given to
the relevant rules issued by the Government of India under tfie Prevention
of Food Adulteration Act, 1954. This standard is, however, subject to the
restrictions imposed under that Act and the Rules framed thereunder,
wherever applicable.
0.5 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 or analysis, shall be rounded off in accordance with
IS: 2-1960*. The number of significant places retained in the rounded off
value should be the same as that of the specified value in this standard.
*Rules for rounding off numerical values ( revised ).

3
IS : 1263 - 1986

1. SCOPE
1.1 This standard prescribes the requirements and the methods of sampling
and test for cocoa butter.
1.2 This standard applies exclusively to cocoa butter used as ingredient in
the manufacture of chocolate and chocolate products.
2. REQUIREMENTS
2.1 Cocoa butter shall be the fat produced by extraction or expression
from cocoa beans, the fermented and dried seeds of Theobroma cacao L, or
its constituent parts ( except the shell ), or its products, cocoa nib, cocoa
fines, cocoa mass, cocoa press cake or expeller press cake. It shall be free
from rancidity or other off odours, adulterants or other harmful ingredients.
It shall have the colour, odour and taste characteristic of cocoa butter.
2.2 Cocoa butter may be produced by one or more of the following means.
2.2.1 By Hydraulic Pressing - Cocoa butter is obtained by hydraulic
pressing of good quality, commercially shell free nibs that have been
ground to give cocoa mass. The product should be filtered or centrifuged
subsequently. It may also be deodourized.
2.2.2 By Expeller Pressing - Cocoa butter may be obtained by expeller,
extrusion or screw pressing from cocoa beans, cocoa nibs or shell free
cocoa fines (cocoa dust ). The product should be filtered and it may be
refined by one or more of the processes stated in 2.4.
2.2.3 By Solvent Extraction - Cocoa butter may be extracted from cake
residues after the expeller process by means of food grade solvents prescri-
bed in 2.3. It may also be extracted from cocoa beans, cocoa nibs, cocoa
fines ( cocoa dust ), cocoa cake or cocoa powder. The product shall be
refined as described in 2.4 in order to achieve the standard requirements
listed in Table 1.
2.3 Solvents-No solvent other than food-grade Hexane 62 to 82°C and
food grade 1, 1, I-trichloro-ethylene shall be used for extraction of cocoa
butter. The level of residual solvent in the solvent extracted cocoa butter
shall not exceed 5 mg/kg.
2.4 Cocoa butter is refined by subjecting it to:
a) Filtration, centrifugation;
b) ‘Degumming’ with hot water and centrifugal separation followed
by alkali washing (neutralization) and further separation. The
final washings are followed by vacuum drying. This whole process
is also termed ‘lye refining’.
c) Treatment with <fullers earth’ bentoxide or ‘activated charcoal’ to
achieve bbleaching’.
d) <Deodourizing’ with super-heated steam under vacuum.

4
IS : 1263- 1986

2.5 Cocoa butter shall also comply with the requirements given in Table 1.

TABLE 1 REQUIREMENTS FOR COCOA BUTTER

SL CHARACTERISTIC REQUIREMENT METHODOF TEST,


No. REF TO APPENDIX

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

i) Refractive index No., nD, 40°C 1.453-1.458 A

ii) Melting point:

Slip point ( Fincke ) 30-34°C B

Clear melting point 30-34°C

iii) Free fatty acids, expressed as per- 1.5 C


cent m/m olelc acid, MUX

iv) Saponification value, expressed as 188-198 D


mg KOH/g fat

9 Iodine value ( Wijs ) 33-42 E

vi) I&saponifiable matter ( petroleum 1.5 F


ether ) as percent m/m, Max

3. PACKING AND MARKING


3.1 Packing-The material shall be packed in well-closed containers as
agreed to between the purchaser and the vendor.
3.2 Marking - The following particulars shall be legibly and indelibly
marked on each container:

a>Name and type of material;

b) Name and address of the manufacturer;


c) Batch or code number;
4 Net mass;
e>Date of manufacture; and
f) Any other particulars required under the Standards of Weights
and Measures ( Packed Commodities ) Rules, 1977.

5
IS : 1263- 1986

3.2.1 Each container may also be marked with the Standard Mark.
NoTE-T~~ 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 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 are also continuously checked by BIS for conformity 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 Standards.

4. SAMPLING
4.1 The method of drawing representative samples of the material and the
criteria for conformity shall be according to the method prescribed in
Appendix G.

5. TESTS
5.1 Tests shall be carried out as prescribed in the appropriate appendices
specified in 2.3 and in co1 4 of Table 1.
5.2 Quality of Reagents - Unless otherwise specified, pure chemicals or
distilled water ( see IS : 1070-1977* ) shall be employed in tests.
NOTE-‘Pure chemicals’ shall mean chemicals that do not contain impurities which
affect the results of analysis.

APPENDIX A
( Table 1 )
DETERMINATION OF REFRACTIVE INDEX

A-l. APPARATUS
A-l.1 Refractometer - Abbe or butyro refractometer. The temperature of
the refractometer should be controlled at 40.0 f O.l”C, and for this
purpose it should be provided with a thermostatically controlled waterbath
and a motor-driven pump to circulate water through the instrument. The
instrument should be standardized, following the manufacturer’s instruc-
tions, with a liquid of known purity and refractive index. Distilled water
is a satisfactory liquid for standardization.

*Specification for water for general laboratory use ( second revision ).

6
IS : 1263 - 1986

A-l.2 Light Source - If the refractometer is equipped with a compensator,


a tungsted lamp or a daylight bulb may be used. Otherwise, a monochro-
matic light, such as an electric sodium vapour lamp, shall be used.

A-2. PROCEDURE
A-2.1 Melt the material, if it is not already liquid, and filter through a
filter paper to remove any impurities and the last traces of moisture.
Make sure that this sample of the material is absolutely dry. Adjust the
temperature of the refractometer to 40.0 f O*l”C. Ensure that the prisms
are clean and completely dry, and then place a few drops of the sample on
the lower prism. Close the prisms, tighten firmly with the screw-head, and
allow to stand for one or two minutes. Adjust the instrument and light to
obtain the most distinct reading possible, and determine the refractive
index. If a butyro refractometer is used, convert the readings to refractive
indices ( no ) using Table 2.

A-3. TEMPERATURE CORRECTIONS


A-3.1 It is not possible to determine the refractive index at 4O”C, approxi-
mate corrections shall be made using the following equation:
R = R, + K(T-40)

where
R = the reading of the refractometer reduced to 40°C;
R, = the reading at T”C;
T = the temperature in “C at which the reading R, is taken, and
constant; and
K = O-000 365 (if Abbe refractometer is used ), or 0.55 ( if
butyro refractometer is used ).

7
IS : 1263- 1986

TABLE 2 CONVERSION OF BUTYRO REFRACTOMETER


READINGS (B) TO REFRACTIVE INDICES (ma)

( Chse A-2.1 )

B no B ml B

0.0 1.422 0 4.5 1.425 6 9.0 1,429 2


0.1 9.1
:. ;:; 7
8 :
;:; 3 4.8 9 ;:“4 5

0.5 1.426 0 9.5 6


i ::; 1 9.6
;:; 6 5.2 9.8 8’
0.9 7 5.4 : 9.9 9

1.0 4 10.0 1.430 0


: :::, 5 10.1
::; 1.423 0 6 10.3 :.
1.4 1 5’:; 7 10.4 3

2 6.0 8 IO.5 4
::; 9 10.6
1.7 : 2:; 1.427 0 10.7 ii
1.9 5 6.4 1 10.9 7

2.0 6 2:; 2 11.0


7 11.1 f
f :: 11.3 1.431 0
2.4 ; 2:; :5 11.4 1

1.424 0 ;:y 6 11.5 2


;:; 11.6 3
2.7 : 7.2 i 11.8 4
2.8 3 7.4 9 11.9 5

3.0 4 ;:; 1.428 0 12.0


3.1 12.2 5
3.2 : 7.7 :. 12.3 8
3.3 7 7.9 3 12.4 9

3.5 12.5 1.432 0


3.6 ; 12.7
3.7 1.425 0 6 12.8 :.
3.8 1 ;:g 7 12.9 3

2 8.5 13.0
;:y z 13.2
4.2 fi 8”:; 1.429 0 13.3
4.3 5 8.9 1 13.5

( Continued )

8
IS : 1263- 1986

TABLE 2 CONVERSION OF BUTYRO REFRACTOMETER


READINGS ( B) TO REFRACTIVE INDICES ( no) - Contd

B nD B Ql B nD

13.6 l-432 8 18.8 1.436 8 24.1 1.440 8


13.7 18.9 9
13.8 1.433 ; 19-l l-437 0” ;:: 1.441 0
14.0 1 19.2 1 24.5 1

14.1 2 19.3 2 24.6 2


14.2 19.5 24.7 3
14.4 : 19.6 : 24.8 4
14.5 5 19.7 5 25.0 5

14.6 6 19.8 6 25.1


14.7 7 20.0 7 25.2
14.9 20.1 25.4
15.0 ; 20.3 ti 25.5

15-l 1.434 0 20.4 1.438 0 25.6 1.442 0


15.3 20.5 25.8
15.4 1 20.6 :. 25.9 :
15.5 3 20.8 3 26.1 3

15.6 4 20.9 4 26.2


15.8 21.1 26.3 :
15.9 2 21.2 :, 26.5
16.0 7 21.3 7 26.6 f

16.2 21.4 8 26.7


163 : 21.6 26.9 t
16.4 l-435 0 21.7 I.439 ; 27.0 1443 0
16.6 1 21.8 1 27.1 1

16.7 2 22.0 27.3 2


16.8 22.1 f 27.4 3
17.0 : 22.2 4 27.5
17.1 5 22.4 5 27.7 i

17.2 22.5 6 27.8


17.4
17.5
22.6
22.7 :
27.9
28.1
76
17.6 22.9 9 28.2 ;
17.8 1.436 0 23.0 l-440 0 28.3 1.444 0
17.9 23.2 28.5
18.0 :. 23.3 :. 28.6 :.
18.2 3 23-4 3 28.7 3

18.3 23.5 4 28.9 4


18.4 23.7 29.0
18.5 23.8 : 29.2 i
18.7 23.9 7 29.3 7

( Continued )

9
IS : 1263- 1986

TABLE 2 CONVERSION OF BUTYRO REFRACTOMETER


READINGS ( B ) TO REFRACTIVE INDICES ( nI, ) - Conrd

B nD B nD B no
29.4 1 444 8 35.0 1.448 8 40.6 I.452 8
29.6 35.1 40.7
29.7 1,,445 : 35.3 1.449 0” 40.9 1.453 ;
29.9 1 35.5 1 41.0 1

30.0 35.6 2 41.1 2


30.1 35.1
30.3 35.8 : 41.3
41.4 :
30.4 360 5 41.5 5

30.6 36.1 41.7 6


30.7 36.3 ; 41.8
308 36.4 42.0 ii
30.9 36.5 ; 42.1 9

31.0 1.446 0 36.7 1.450 0 42.3 1.454 0


31.2 1 36.8 1
31.4 37.0 42.4
42.5 :
31.5 : 37.1 42*7 3
31.6 4 37.2 42.8 4
31.8 37.4 43.0
31.9 i 37.5 43.1 2
32.1 I 37.7 43.3 7

32.2 37.8
32.3 ; 37.9 43.6
43.4 i
32.5 1.441 0 38.1 43.7 I.455 0
32.6 1 38.2 43.9 1

32.8 2 38.3 44.0 2


32.9 38.5
33.0 : 38.6 44.3
44.2 :
33.2 5 38,7 44.4 5

33.3 38.9 44.6


33.5 7”
8
39.0
39.2
7”
8
44.7 ;
33.6
33.7 9 39.3 9 z.: fi

33.9 1.448 0 39.5 1.452 0 45.2 1.456 0


34.0 39.6
34.2 :. 39.7 :. 45.5
45.3 :
34.3 3 39.9 3 45.6 3

34.4 4 40.0 4 45,l 4


34.6 5 40.1
34.7 40.3 2 46.0
45.9 :
34.9 7” 40.4 7 46.2 7

( Continued )

10
IS:1263-1986

TABLE 2 CONVERSION OF BUTYRO REFRACTOMETER


READINGS ( B) TO REFRACTIVE INDICES ( n,,) - Contd

B nD B 'ID B nD

46.3 1,456 8 52.2 1.460 8 58.3 1,464 8


46.4 523 58.5
46.6 1.457 ; 52.5 1.461 : 58.6 1.465 :
46.7 1 52.7 1 58.8 1
46.9 2 52.8 2 58.9 2
47.0 53.0 3 59.1
47.2 : 53.1 4 592 ii
47.3 5 53.3 5 594 5
47.5 6 53.4 6 59.5 6
47.6 7 53.6 7 59.7
47.7 8 53.7 59.8 8’
47.9 9 53.9 ; 6@0 9
48.0 1.458 0 54.0 1.462 0 60.2 1.466 0
48.2 54.2 603 1
48.3 : 54.3 : 60.5 z
485 3 545 3 60.6 3
48.6 4 54.6 4 60.8 4
48.8 548 60.9 5
48.9 : 55.0 :, 61.1 f-i
49.1 7 55.1 7 61.2
49.2 55.3 61.4
49.4 9” 55.4 ; 61.5 i
49.5 1.459 0 55.6 1.463 0 61.7 1.467 0
497 I 55.7 1 61.8 1
49.8 2 55.9 2 62.0 2
50.0 56.0 62.2
50.1 i 56.2 : 62.4 ;:
50.2 5 563 5 625 5

50.4 6 565 6 62.6 6


50.5 56.6 7 628
50.7 8’ 56.8 62.9 8’
50.8 9 56.9 9” 63.1 9
51.0 1.460 0 571 1.464 0 63.2 1.468 0
51.1 57.3 1 63.4 1
51.3 1 57.4 63.5
51.4 3 57.6 3” 63.7
51.6 4 57.7 4 63.8
51.7 57.9 640
51.9 2 58.0 2 642
52.0 7 58.2 7 643

( Continued )

11
IS:1263-1986

TABLE 2 CONVERSION OF BUTYRO REFRACTOMETER


READINGS ( B ) TO REFRACTIVE INDICES ( nD ) - Cod

B nD B nD B nD

1.468 8 70.5 1.472 6 16.7 1.476 4


6”%.:
64.8 1.469 :
70.7
70.8
7 76,8
17.0 2
65.0 1 71.0 : 77.2 7

65.1 71.1 1.473 0 77.3


65.3 : 71.3 77.5 ;
65.4 4 71.4 : 77.7 1.477 0
65.6 5 71.6 3 77.9 1

65.7 6 71.8 78.1


65.9 71.9 5” 78.2 z
661 8’ 72.1 6 78.4 4
662 9 72.2 7 78.6 5

66.4 1.470 0 72.4 8 78.7 6


66.5 1 725 78.9
66.7 727 1.474 0” 79.1 8’
66.8 f 72.9 1 79.2 9

4 73.0 79.4 1.478 0


5 73.2 f 79.6
73.3 4 79.8 :
76 73.5 5 80.0 3

67.7 8 73.7 80.1


67.8 73.8 80.3
68.0 1’471’0 740 80.5
68.1 1 741 80.6

68.3 743 1.475 0 80.8


68.4 745 1 81.0 98

68.6 4 74.6 81.2 1.479 0


68.7 748 : 81.3
68.9 2 15.0 4 81.5 :
691 7 75.1 5 81.7 3

69.2 75.3 81.9 4


69.4 z 75.5 : 82.0
695 1.472 0 75.6 8 82.2 2
69.7 1 75.8 9 82.4 7

69.9 2 76.0 1.476 0 82.5


70.0 76.1 82.7 ii
70.2 2 76.3 : 82.9 1.480 0
70.3 5 76.5 3 83.1 1

12

B
1
s
_ .- .”,._.
~..l___. _* .‘._,
IS : 1263- 1986

TABLE 2 CONVERSION OF BUTYRO REFRACTOMETER


READINGS ( B ) TO REFRACTIVE INDICES (no ) - Contd

B nD B no B nD

83.2 1.480 2 88.9 1.483 4 94.7 1.486 6


83.4 89.1 5 94.8
83.6 : 89.2 6 i
83.8 5 89.4 7 ‘9::; 9

83.9 95.4 1.487 0


84.1 7” 8899:: ! 95.6 1
84.3 90.0 1.484 0 95.8
84.5 ii 90.2 1 96.0 :

84.6 90.3 96.1 4


84.8
85.0
le4*l
? 90.5
90.7
3’
4
96.3
96.5 2
85.2 : 90.9 5 96.7 7

85.3 4 91-l 6 96.9 8


85.5 91.2 97.0
85.7 2 91.4 i 97.2 1.488 ;
85.9 7 91.6 9 97.4 1

86.0 a 91.8 I.485 0 97.6 2


86.2 92.0 97.8
86.4 1.482 0’ 92.1 : 98.0 ‘i
86.6 1 92.3 3 98.1 5

86.7 92.5 4 98.3 6


86.9 92.7 98.5
87.1 92.9 : 98.7 8’
87.3 93.0 7 98.9 9

87.5 93.2 99.1 1.489 0


87.6 93.4 z 99.2 1
87.8 93.6 1.486 0 99.4 2
88.0 93.8 1 99.6 3

88.2 94.0 2 99.8 4


88.3 94.1 100.0 5
88.5 94.3 i
88.7 94.5 5

13
IS : 1263 - 1986

APPENDIX B
( Table 1 )
DETERMINATION OF MELTING POINT

B-l. APPARATUS
B-l.1 Melting Point Tubes-Thin walled capillary glass tubes open at
both ends and with the following dimensions:
a) Length, 50 to 60 mm;
b) Inside diameter, 0.8 to 1.1 mm; and
c) Outside diameter, 1.2 to I.5 mm.
B-l.2 Standard Thermometer -With 0~2°C subdivisions and a suitable
range. The thermometer should be checked against a standard thermo-
meter which has been calibrated and certified by the National Physical
Laboratory, New Delhi or any other laboratory recognized by the Govern-
ment of India for such work.
B-l.3 Large Test Tube
B-l.4 Glass Beaker - 600 ml capacity.
B-l.5 Heat Source - Gas burner or electric hot-plate with rheostat
control.

B-2. PROCEDURE
B-2.1 Melt the material and filter it through a filter paper to remove the
last traces of moisture. Make sure that this sample of the material is
absolutely dry and mix thoroughly. Insert a clean melting point tube into
the molten product so that a column of the material about IO mm long is
forced into the tube. Cautiously fuse one end of the tube ( where the
sample is located) in a small flame, taking care not to burn the sample.
Place the tube in a beaker and while the sample is still in the liquid state,
transfer to a refrigerator and hold overnight ( about 16 hours ) at a
temperature between 4 and 10°C. Remove the tube from the refrigerator
and attach with a rubberband or by any other suitable means to the
thermometer so that the lower end of the melting point tube is even with
the bottom of the bulb of the thermometer. Suspend the thermometer in
the large test tube containing water and immerse it in the 600-ml beaker
which is about half full of water. Immerse the bottom of the thermometer
in the water about 30 mm below the surface. Adjust the bath temperature
starting from 10°C below the melting point of the sample at the beginning
of the test. Agitate the water in the large test-tube as well as in the beaker

14
IS : 1263 - 1986

with a small stream of air by other means, and apply heat so as to increase
the bath temperature at the rate of ,about 0*5”C per minute. ( As fats
usually pass through an opalescence stage before melting completely, the
heating is continued until the liquid in the tube is completely clear through-
out ). Observe the temperatures at which the sample starts becoming
opalescent and at which the tube liquid becomes clear. Report the average
of the two successive readings separately determined as the slip point and
the clear melting point respectively. The individual readings should not
differ by more than 0.5”C.

APPENDIX C
( Table 1 )

DETERMINATION OF FREE FATTY ACIDS

C-l. REAGENTS
C-l.1 Ethyl Alcohol - 95 percent ( by volume ), or rectified spirit ( see
IS : 323-1959* ) neutral to phenolphthalein indicator.

C-l.2 Phenolphthalein Indicator Solution - One percent ( m/v ) solution in


ethyl alcohol or rectified spirit.

C-l.3 Standard Potassium Hydioxide Solution - Approximately 0.1 N,


accurately standardized.

C-2. PROCEDURE
C-2.1 Mix the material thoroughly, making it entirely liquid before weigh-
ing. Weigh accurately a suitable quantity of the material in a 200 ml
conical flask. The mass of the material taken for the test shall be such
that the volume of alkali required for the titration does not exceed 10 ml
(usually 5.0 g are used ). Add approximately 50 ml of hot ethyl alcohol
and about one millilitre of phenolphthalein indicator solution and titrate
the mixture while hot with standard potassium hydroxide solution. Take
the first pink colouration, persisting for 30 seconds during shaking, as the
end point.
*Specificationfor rectified spirit ( revised ).
.,.
15
IS : 1263 - 1986

C-3. CALCULATION
C-3.1 Free fatty acids ( expressed as oleic acid,
percent by mass = 28.2 ViV
M

where

V = volume in ml of standard potassium hydroxide solution used,


N = normality of standard potassium hydroxide solution, and
M = mass in g of the material taken for the test.

APPENDIX D
( Table 1 )

DETERMINATION OF SAPONIFICATION VALUE

D-l. APPARATUS
D-l.1 Erlenmeyer Flasks - 250 to 300 ml capacity.
D-l.2 Reflux Air Condensers - At least 65 cm long.
D-l.3 Water-Bath or Electric Hot-Plate with Rheostat Control

D-2. REAGENTS
D-2.1 Alcoholic Potassium Hydroxide Solution - Dissolve 35 to 40 g of
potassium hydroxide in 20 ml of distilled water, and add sufficient
aldehyde-free ethyl alcohol ( 95 percent by volume ) or aldehyde-free
rectified spirit ( see IS: 323-1959* ) prepared as described in C-3.4 of
IS: 323-1959*, to make up to 1000 ml. Allow to stand overnight, decant
the clear liquid and keep in a bottle closed tight with a cork or rubber
stopper.
D-2.2 Phenolphthalein Indicator Solution - One percent ( m/v ) solution in
95 percent ethyl alcohol (by volume), or rectified spirit (see IS : 323-1959*).
D-2.3 Standard Hydrochloric Acid - Approximately 0.5 N.
*Specification for rectified spirit ( revised ).

16
IS : 1263 - 1986

D-3. PROCEDURE
D-3.1 Melt the material if it is not already liquid, and filter through a
filter paper to remove any impurities and the last traces of moisture. Make
sure that sample of the material is absolutely dry. Mix the sample
thoroughly and weigh accurately about 1.5 g of the sample in a tared
Erlenmeyer flask. Add 25 ml of the alcoholic potassium hydroxide solution,
add a few pieces of pumice stone, necessary, and connect the reflux air
condenser to the flask. Heat the flask on a water-bath or an electric hot-
plate for about one hour. Boil gently but steadily until the sample is
completey saponified. After the flask and condenser have cooled some-
what, wash down the inside of the condenser with about 10 ml of hot ethyl
alcohol neutral to phenolphthalein. Add about one millilitre of phenol-
phthalein indicator solution, and titrate with standard hydrochloric acid.
Prepare and conduct a blank determination at the same time.

D-4. CALCULATION
56.1 (B--S) N
D-4.1 Saponification value =
M
where
B = volume in ml of standard hydrochloric acid required for the
blank;
5’ = volume in ml of standard hydrochloric acid required for the
sample;
N = normality of the standard hydrochloric acid; and
M = mass in g of the material taken for the test.

APPENDIX E
( Table 1 )
DETERMINATION OF IODINE VALUE ( WIJS )
E-l. APPARATUS
E-l.1 Thermometer - An engraved stem thermometer calibrated between
10 and 65°C in O*l”C intervals and with the 0°C point marked on the
stem, is recommended. The thermometer shall have an auxiliary reservoir
at the upper end, a total length of about 370 mm and a diameter of about
6 mm.
17
IS : 1263 - 1986

E-2. REAGENTS
E-2.1 Potassium Dichromate - Crystalline.
E-2.2 Concentrated Hydrochloric Acid - sp gr 1.16 (see IS : 265-1976* ).
E-2.3 Potassium Iodide Solution - Prepare a fresh solution by dissolving
10 g of potassium iodide, free from potassium iodate, in 90 ml of water.
E-2.4 Starch Solution - Make a paste of O-5 g of soluble starch in cold
water, pour into 100 ml of boiling water, boil for 5 minutes, cool and
bottle. The solution should be prepared afresh every two or three days.
E-2.5 Standard Sodium Thiosulphate Solution - Approximately O-1 N.
Dissolve approximately 24.8 g of sodium thiosulphate crystals ( Na,S,O,,
5H,O ) in water which has been well boiled to free it from carbondioxide
and make up to 1 000 ml. Store the solution in a cool place in a dark
coloured stock bottle with a guard tube filled with soda lime. After
storing the solution for about two weeks, standardize it as prescribed
in E-2.5.1.
E-2.5.1 Weigh accurately about O-2 g finely ground potassium dichromate
which has been previously dried to a constant weight at 105 f 2”C, in a
clean and dry conical flask, and dissolve in a small quantity of water. Add
60 ml of water, 4 ml of concentrated hydrochloric acid and 20 ml of
potassium iodide solution. Titrate the mixture with the solution of sodium
thiosulphate using starch solution as an internal indicator towards the end.
Take the end point when the blue colour changes to green. Calculate the
normality ( N) of the sodium thiosulphate solution as follows:
t
1 000 m
= 49.03 V

where
m = mass in g of the potassium dichromate, and
Y = volume in ml of sodium thiosulphate solution required for the
titration.
E-2.6 Iodine Crystals - Re-sublimed.
E-2.7 Acetic Acid - Glacial, 99 percent, having a melting point of 14*8”C
and free from reducing impurities. Determine the melting point of the
acetic acid and test it for reducing impurities as follows:
a) Melting Point Determination -Take a 15 cm long test-tube and
fill it to about two-thirds with the acetic acid. Insert into acid a
thermometer satisfying the requirements specified in E-l.1 through
*Specificationfor hydrochloric acid ( revised ).
18
IS : 1263- 1986

a cork stopper fitting the test-tube. The amount of acid should be


at least double the quantity required to cover the bulb of the
thermometer when the bottom of the latter is 12 mm from the
bottom of the test tube.
Suspend this tube within a larger test tube through a cork.
Cool the acid by immersing the assembly in ice water until the
temperature is lO”C, then withdraw the assembly from the ice
water and stir the acid rather vigorously for a few moments, thus
causing the supercooled liquid to crystallize partially and give a
mixture of liquid and solid acid. Take thermometer readings every
15 seconds and consider as the true melting point that temperature
at which the reading remains constant for at least 12 minutes.
b) Test for Reducing Impurities (Potassium Permanganate Test) -
Dilute 2 ml of the acetic acid with a 10 ml of water, add 0.1 ml of
O-1 N potassium permanganate solution and maintain at 27 f 2°C.
The test shall be taken as having been satisfied if the pink colour is
not discharged at the end of two hours.
E-2.8 Chlorine Gas - Dry.
E-2.9 Iodine Trichloride ( ICL, )
E-2.10 Wijs Iodine Monochloride Solution- Prepare this solution by one ‘

of the following two methods, and store in a glass-stoppered bottle in a


cool place, protected from light:
a) Dissolve 13 g of iodine in one litre of acetic acid, using gentle heat,
if necessary, and determine the strength by titration with standard
sodium thiosulphate solution. Set aside 50 to 100 ml of the
solution and introduce chlorine gas into the remainder until the
characteristic colour change occurs and the halogen content is
nearly doubled as ascertained again by titration. If the halogen
content has been more than double, 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 solution
requires 22 ml of standard sodium thiosulphate, 20 ml of the
finished Wijs solution should require between 43 and 44 ml (and
not more than 44 ml ) of the same sodium thiosulphate solution.
b) As an alternative method for preparing Wijs solution, dissolve 8 g
of iodine trichloride in approximately 450 ml of acetic acid.
Dissolve separately 9 g of iodine in 450 ml of acetic acid using
heat, if necessary. Add gradually the iodine trichloridc until the

19
* _I._ -~ll------____ _ -__.. _

IS : 1263- 1986

colour has changed to reddish-brown. Add 50 ml more of iodine


solution and dilute the mixture with acetic acid till 10 ml of the
mixture is equivalent to 20 ml of standard thiosulphate solution
when the halogen content is estimated by titration in the presence
of an excess of potassium iodide and water. Heat the solution to
100°C for 20 minutes, and cool. Prevent the access of water
vapour in preparing the solution.
E-2.11 Carbon Tetrachloride or Chloroform - Inert to Wijs solution.

E-3. PROCEDURE
E-3.1 Melt the material and filter through a filter paper to remove any
impurities and the last traces of moisture. Make sure that this sample of
the material as well as the glass apparatus used is absolutely clean and dry.
Weigh accurately, by difference, 0.530 0 to 0.660 0 g to an accuracy of
0.000 2 g of the sample, into a clean, dry 500 ml glass-stoppered bottle to
which 25 ml of carbon tetrachloride or chloroform have been added, and
agitate to dissolve the contents. ( The mass of the sample shall be such
that there is an excess of Wijs solution 50 to 60 percent of the amount
added). Add 25 ml of the Wijs solution and replace the glass stopper
after wetting with potassium iodide solution, swirl for intimate mixing and
. allow to stand in the dark for 30 minutes. Carry out a blank test simul-
taneously under similar experimental conditions. After standing, add 15 ml
of potassium iodide solution and 100 ml of water, and titrate the liberated
iodine with standard sodium thiosulphate solution, swirling the contents of
the bottle continuously to avoid any local excess until the colour of the
solution is straw yellow. Add 0.5 ml of the starch solution and continue
the titration until the blue colour formed disappears.

E-4. CALCULATION

12.69 (B-S) N
E-4.1 Iodine Value =
M

where

B = volume in ml of standard sodium thiosulphate solution required


for the blank,
S = volume in ml of standard sodium thiosulphate solution required
for the sample,
N = normality of the standard sodium thiosulphate solution, and
M = mass in g of the sample taken for the test.

20
IS : 1263 - 1986

APPENDIX F
( Table 1 )
DETERMINATION OF UNSAPONIFIABLE MATTER

F-l. GENERAL
F-l.1 The material is completely saponified with alcoholic potassium
hydroxide solution and extracted with petroleum ether. The petroleum
ether extract is washed with aqueous alcohol and then again with water.
The washed ether extract is evaporated and the residue weighed. Un-
saponifiable matter is this residue minus the fatty acid present in it, which
is determined by titration with sodium hydroxide solution in alcoholic
medium.

F-2. APPARATUS
F-2.1 Separating Funnel - 250 ml capacity.
F-2.2 Flat Bottomed or Erlenmeyer Flasks - 250 to 300 ml capacity.
F-2.3 Reflux Air or Water Condenser - At least 65 cm long.

F-3. REAGENTS
F-3.1 Concentrated Potassium Hydroxide Solution - Dissolve 60 g of KOH
in 40 ml of water.
F-3.2 Dilute Potassium Hydroxide Solution - Dissolve 10 g KOH in 1 litre
of water.
F-3.3 Diethyl Ether - Peroxide free.
F-3.4 Ethyl Alcohol - Rectified spirit or 95 percent alcohol ( v/v).
F-3.5 Phenolphthalein Indicator - Dissolve 1 g of phenolphthalein in
100 ml of ethyl alcohol.
F-3.6 Standard Sodium Hydroxide - 0.02 N.

F-4. PROCEDURE
F-4.1 Weigh accurately about 35 g of well mixed sample into the flask.
Add 25 ml of alcohol and 1.5 ml of potassium hydroxide. Saponify by
boiling with occasional swirling, on steam-bath for 30 minutes under reflux
air condenser or water condenser ( no loss of alcohol should occur during
saponification ). Transfer alcoholic soap solution while still warm to
250 ml separatmg funnel using about 50 ml of water. Rinse the flask with
50 ml ether and add to separating funnel. Shake vigorously and let layers

21
IS : 1263- 1986

separate and clarify. Drain lower layer and pour ether layer through top
into second separating funnel. Rinse the pouring edge with.ether through
top into second separating funnel. Rinse the pouring edge with ether
adding rinsings to second separating funnel. Make additional extractions
of soap solution with 50 ml portions of ether in same manner.
F-4.2 Rotate combined ether extracts gently with 40 ml of water (violent
shaking at this stage may cause trouble some emulsions). Let layers
separate and drain aqueous layer. Wash with two additional 40 ml
portions of water, shaking vigorously. Then wash ether solution 3 times
with alternate 20 ml portions of 0.5 N aqueous, potassium hydroxide and
water, shaking vigorously each time. If emulsion forms during washing,
drain as much aqueous layer as possible leaving emulsion in separating
funnel with ether layer and proceed with next washing. Wash ether solu-
tion successively with 40 ml of water until washings are no longer alkaline
to phenolphthalein.
F-4.3 Transfer the ether layer through a funnel containing cotton and
anhydrous sodium sulphate to a tared flask containing a few pieces of
pumic stone and evaporate to dryness on a water-bath under a gentle
stream of clear dry air. To remove the last trace of ether, place the flask
in an air oven at 80” to 90°C for about an hour. Cool in a desiccator and
weigh. Repeat heating, cooling and weighing until constant weight is
obtained. After weighing, dissolve the residue in 50 ml of warm neutral
ethyl alcohol, containing a few drops of phenolphthalein indicator solution
and titrate with standard sodium hydroxide solution.

F-5. CALCULATION
F-5.1 Mass in g of fatty acids in the extract as oleic acid =
B = 0.056 4 VN

where

V = volume in ml of standard sodium hydroxide,


N = normality of standard sodium hydroxide solution,

100 (A-B)
Unsaponifiable matter = M

A z mass in g of residue,

B = mass in g of fatty acids in the extract, and

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

22

,.._
my r-“rrr*,^“.
IS : 1263 - 1986

APPENDIX G
( Czuuse 5.1 )
SAMPLING OF COCOA BUTTER

G-l. GENERAL REQUIREMENTS OF SAMPLING


G-1.0 In drawing, preparing, storing and handling samples, the following
precautions and directions shall be observed.
G-l.1 Samples shall be taken in a protected place not exposed to damp-air,
dust or soot.
G-l.2 The sampling instrument shall be clean and dry when used.
G-l.3 Precautions shall be taken to protect the samples, the material being
sampled, the sampling instrument and the containers for samples from
adventitious contamination.
G-l.4 The samples shall be placed in clean and dry glass containers. The
sample containers shall be of such a size that they are almost completely
filled by the sample.
G-l.5 Each container shall be sealed air-tight after filling and marked with
full details of sampling, batch or code number, name of the manufacturer
and other important particulars of the consignment.
G-l.6 Samples shall be stored in such a manner that the temperature of
the material does not vary unduly from the normal temperature.

G-2. SCALE OF SAMPLlNG


G-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 the
consignment is declared to consist of different batches of manufacture, the
batches shall be marked separately and the group of containers in each
batch shall constitute a separate lot.
G-2.1.1 From each lot, samples shall be tested to ascertain the confor-
mity of the material.
G-2.2 The number of containers to be selected shall depend on the size N
of the lot and shall be in accordance with co1 1 and 2 of Table 3.
G-2.2.1 These containers shall be chosen at random from the lot. For
this purpose ( 3.1 ) simple random sampling or ( 3.3) systematic sampling
specified in IS : 4905-1968* shall be followed.

*Methods for random sampling.

23
IS : 1263 - 1986

TABLE 3 NUMBER OF CONTAINERS TO BE SELECTED


FOR SAMPLING

( Clause G-2.2)

LOT SIZE SAMPLE SIZE

N n

(1) (2)
5 to 100 3
101 to 300 5

301 to 500 7

501 and above 9

G-3. PREPARATION OF TEST SAMPLES AND REFEREE SAMPLE


G-3.1 About 250 g of the material shall be taken from each of the selected
containers using a sampling scoop (see Fig. 1 ), if the material is a solid
and a sampling tube (see Fig. 2 ), if the material is a liquid at the tempera-
ture prevailing the time of sampling. The material so taken shall be heated
to 40°C and shall be mixed thoroughly.
G-3.2 Preparation of Composite Sample - Equal quantities of material
( about 100 g ) shall be taken from the sample as obtained in G-3.1 and
mixed thoroughly to constitute a composite sample of size 300 g. This
sample shall be divided into three equal parts, one for the purchaser, one
for the vendor and the third for the referee. The test samples so obtained
shall be transferred immediately to thoroughly clean and dry containers
and sealed air-tight. These shall be labelled with particulars of sampling
given in G-1.5.
G-3.3 Preparation of Individual Sample - The remaining portions of the
material from each of the selected containers (after the required quantity
needed for formation of the composite sample ) shall be divided into three
equal parts. These parts shall be immediately transferred to thoroughly
dried containers which are then sealed air-tight and labelled with all the
particulars given in G-1.5.
G-3.4 Referee Samples - Referee samples shall consist of the composite
sample (see G-3.2) and a set of individual test samples (see G-3.3) marked
for this purpose and shall bear the seals of the purchaser and the vendor.
These shall be kept at a place agreed to between the two.
G-4. NUMBER OF TESTS
G-4.1 Tests for description ( 3.1), treatment ( 3.2 ) and solvents (3.3) shall
be conducted on each of the individual test samples ( see G-3.3 ).
24
IS : 1263- l!H6

- - 5T0 IO DIA

I J 0

--- - 20 TO 40 DIA

-5T0 10 DIA

All dimensionsin millimetres.

FIG. 1 SAMPLING SCOOP FIG. 2 SAMPLING TUBE

25
IS : 1263 - 1986

G-4.2 Tests for the determination of remaining characteristics shall be


conducted on the composite test sample as prepared under G-3.2.

G-5. CRITERIA FOR CONFORMITY


G-5.1 A lot shall be declared as conforming to the requirements of this
standard if G-5.1.1 and G-5.1.2 are satisfied.
G-5.1.1 Each of the test results obtained for various characteristics from
individual testing ( see G-4 ) shall satisfy the corresponding requirements
as given in 3.
G-5.1.2 The test results on the composite sample for the characteristics
specified in Table 1 shall satisfy the corresponding requirements given in
Table 1.

26

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