S T D - B S I B S EN IS0 37b.

l-ENGL 2000 Lb2'4bb9 0 8 8 8 2 3 7 700 D

BRITISH STANDARD BS EN IS0
3961:ZOOO
Incorporating
Amendment No. 1 to
BS 684-2.13
(renumbers the BS as
BS EN I S 0 3961)

Animal and vegetable

fats and oils -
Determination of
iodine value
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The European Standard EN IS0 3961:1999 has the status of a

British Standard

IMPORTANT NOTE. This standard should be read in conjunction with

BS 684-0.1 and BS EN IS0 661 (BS 684-0.2).

ICs 67.200.10

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S T D - B S I B S E N IS0 39bL-ENGL 2 0 0 0 P L b 2 q b b S 0 8 8 8 2 3 8 b117 W

BS EN IS0 3961:ZOOO

National foreword
This British Standard is the English language version of EN IS0 3961:1999.
It is identical with IS0 3961:1996.
The UK participation in its preparation was entrusted to Technical Committee
AW/11, Animal and vegetable fats and oils, which has the responsibility to:
- aid enquirers to understand the text;
- present to the responsible internationallEuropean committee any
enquiries on the interpretation, or proposals for change, and keep UK
interests informed;
- monitor related international and European developments and
promulgate them in the UK.

A list of organizations represented on this committee can be obtained on request

to its secretary.
Cross-references
Attention is drawn to the fact that CEN and CENELEC Standards normally
include a n annex which lists normative references to international publications
with their corresponding European publications. The British Standards which
implement international or European publications referred to in this document
may be found in the BSI Standards Catalogue under the section entitled
“International Standards Correspondence Index”, or by using the “ F i n d facility
of the BSI Standards Electronic Catalogue.
A British Standard does not purport to include all the necessary provisions of a
contract. Users of British Standards are responsible for their correct application.
Compliance with a British Standard does not of itself confer immunity
from legal obligations.

This British Standard, having Summary of pages

been DreDared under the
direction-ofthe Consumer This document comprises a front cover, a n inside front cover, pages i and ii,
Products and Services Sector the EN IS0 title page, the EN IS0 foreword page, pages 1t o 5 and a back cover.
Board,was published under the
authority of the Standards The BSI copyright notice displayed in this document indicates when the
Board and comes into effect on document was last issued.
15 October 1996

0 BSI 12-2000
First published November1976
Second edition December 1981 Amendments issued since publication
Fourth edition October 1996 Amd. No. Date Comments

10896 December Renumbers BS 684-2.13 as BS EN IS0 3961 and

2000 adds Annex ZA
The following BSI references
relate to the work on this
standard:
Committee reference AWíl1
Draft for comment 94/504160 DC
~

ISBN O 580 26042 9

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STD.BSI BS E N IS0 ISbL-ENGL 2000 W lb2Libb9 0688237 583 W

BS EN IS0 3961:2000

Contents
Page
National foreword Inside front cover
1 Scope 1
2 Normative references 1
3 Definition 1
4 Principle 1
5 Reagents 1
6 Apparatus 1
7 Sampling 1
8 Preparation of test sample 1
9 Procedure 1
10 Calculation 2
11 Precision 2
12 Test report 2
Annex A (informative) Interlaboratory test 3
Annex B (informative) Bibliography 5
Annex ZA (normative) Normative references to international publications
with their relevant European publications 5
Table 1- Mass of test portion 1
Table 2 - Rounding off of results 2
Table 3 - Repeatability and reproducibility limits 2
Table A.l- Results of interlaboratory tests 4
Table A.2 - Mean determinations of iodine value 4
Table A.3 - Summary of three “error”estimates 4

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STDeBSI BS E N IS0 37bL-ENGL 2000 LbZ'ibbS 08882'iO 2 T 5 D

EUROPEAN STANDARD EN IS0 3961

NORME EUROPÉENNE
EUROPÄISCHE NORM May 1999

ICs 67.200.10

English version

Animal and vegetable fats and oils -

Determination of iodine value
( I S 0 3961:1996)

Corps gras d'origines animale et végétale - Tierische und pflanzliche Fette und Öle -
Détermination de l'indice d'iode Bestimmung der Iodzahl
( I S 0 3961:1996) (IS0 3961:1996)

This European Standard was approved by CEN on 1999-04-15.

CEN members are bound to comply with the CENKENELEC Internal
Regulations which stipulate the conditions for giving this European Standard
the status of a national standard without any alteration. Up-to-date lists and
bibliographical references concerning such national standards may be obtained
on application to the Central Secretariat or to any CEN member.
This European Standard exists in three official versions (English, French,
German). A version in any other language made by translation under the
responsibility of a CEN member into its own language and noti6ed to the
Central Secretariat has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Czech
Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy,
Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and
United Kingdom.

CEN
European Committee for Standardization
Comité Européen de Normalisation
Europäisches Komitee für Normung

C e n t r a l Secretariat: rue de Stassart 36, B-1050Brussels

O 1999 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national
Members.
Ref. No. EN IS0 3961:1999E
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 S T D - B S I BS E N IS0 37bL-ENGL 2000 m 1 b 2 4 b b 7 0888241 131
EN IS0 3961:1999

Foreword
International Standard IS0 3 9 6 1 ~ 9 9 6Animal
, and
vegetable fats and oils -Determination of iodine
ualue, which was prepared by ISOíTC 34,
Agricultural food products, of the International
Organization for Standardization (ISO), has been
adopted by CEN/TC 307, Oilseeds, vegetable and
animal fats and oils and their by-products -
Methods of sampling and analysis, the Secretariat
of which is held by AFNOR, as a European
Standard.
This European Standard shall be given the status of
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a national standard, either by publication of a n

identical text or by endorsement, and conflicting
national standards shall be withdrawn, by
November 1999 a t the latest.
I n accordance with the CENXENELEC Internal
Regulations, the national standards organizations
of the following countries are bound to implement
this European Standard: Austria, Belgium, Czech
Republic, Denmark, Finland, France, Germany,
Greece, Iceland, Ireland, Italy, Luxembourg,
Netherlands, Norway, Portugal, Spain, Sweden,
Switzerland and the United Kingdom.
NOTE Normative references to international publications are
listed in Annex ZA (normative).

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 S T D - B S I B S EN IS0 37bL-ENGL 2000 M l b 2 4 b b 9 0888242 078 M
EN IS0 3961:1999

1 Scope
This International Standard specifies a method for
the determination of the iodine value of animal and
vegetable fats and oils, hereinafter referred to as
fats.
2 Normative references
The following standards contain provisions which,
through reference in this text, constitute provisions
of this International Standard. At the time of
publication, the editions indicated were valid. All
standards are subject to revision, and parties to
agreements based on this International Standard
are encouraged to investigate the possibility of
applying the most recent editions of the standards
indicated below. Members of IEC and I S 0 maintain
registers of currently valid International Standards.
IS0 661:1989, Animal and vegetable fats and oils -
Preparation of test sample.
IS0 3696: 1987, Water for analytical laboratory
use - Specification and test methods.
3 Definition
For the purposes of this International Standard, the
following definition applies.
3.1
iodine value
mass of halogen, expressed as iodine, absorbed by
the test portion following the specified procedure,
divided by the mass of the test portion
iodine value is expressed as grams per 100 g of fat
4 Principle
Dissolution of a test portion in solvent and addition
of Wijs reagent. After a specified time, addition of
potassium iodide and water, and titration of the
liberated iodine with sodium thiosulfate solution.
5 Reagents
Use only reagents of recognized analytical grade,
and water complying with grade 3 of I S 0 3696. -
Expected iodine Mass of test Volume of
5.1 Potassium iodide m),100 gn, not containing value
gI100 g
portion
g
solvent
ml
iodate or free iodine.
Less than 1,5 15,OO 25
5.2 Starch solution 1,5 to 2,5 10,oo 25
Mix 5 g of soluble starch in 30 ml of water and add 2,5to 5 3,OO 20
to 1O00 ml of boiling water. Boil for 3 min and allow 5 to 20 1,oo 20
to cool.
20 to 50 0,40 20
5.3 Sodium thiosulfate, standard volumetric 50 to 100 0,20 20
solution, c(Na2S2O3.5H20) = O, 1mom, standardized 100 to 150 O,13 20
not more than 7 days before use.
150 to 200 0,lO 20
5.4 Solvent, prepared by mixing equal volumes of NOTE The mass of the sample shall be such that there will bi
cyclohexane and glacial acetic acid. an excess of Wijs reagent of between 50 % and 60 % of the
amount added; i.e. 100 % to 150 % of the amount absorbed.

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S T D - B S I B S E N IS0 3 7 b L - E N G L 2 0 0 0 CI L b 2 4 b b 7 0 8 8 8 2 4 3 T O 4 II
EN IS0 3961:1999
9.2 Determination
9.2.1 Place the glass scoop containing the test
portion in a 500 ml flask (6.2) and add the volume of
solvent (5.4) indicated in Table 1.Add 25 ml of the
Wijs reagent (5.5) by pipette. Insert the stopper,
swirl the contents and place the flask in the dark.
CAUTION - Do not use a mouth pipette for
the Wijs reagent.
9.2.2 Prepare a blank with solvent and reagent as
in 9.2.1 but omitting the test portion.
9.2.3 For samples having a n iodine value below 150
leave the flasks in the dark for 1h.
For samples with iodine values above 150, and for
polymerized products and oils containing
conjugated fatty acids (such a s tung oil, dehydrated
castor oil) and any oils containing keto fatty acids
(such as some grades of hydrogenated castor oil) and
products oxidized to a considerable extent, leave the
flasks in the dark for 2 h.
9.2.4 At the end of the reaction time (9.2.3),
add 20 ml of potassium iodide (5.1) and 150 ml of
water.
Titrate with standard sodium thiosulfate
solution (5.3) until the yellow colour due to iodine
has almost disappeared. Add a few drops of the
starch solution (5.2) and continue the titration until
the blue colour just disappears after very vigorous
shaking. Note that potentiometric determination of
the endpoint is permissible.
9.2.5 Carry out the determination using the blank
solution (9.2.2) concurrently.
10 Calculation
The iodine value, wI,expressed in grams per 100 g
of fat, is given by the equation:
1 2 , 6 9 ~ ( V , -V .
WI =
m 12 Test report
where
cis the numerical value of the concentration
of the sodium thiosulfate solution (5.3), in
moles per litre;
VI is the numerical value of the volume, in the
millilitres, of sodium thiosulfate solution
used for the blank test;
V, is the numerical value of the volume, in
millilitres, of sodium thiosulfate solution
used for the determination;
is the numerical value of the mass of the
rn
test portion, in grams.
Round off the result as indicated in Table 2.
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Table 2 - Rounding off of results
Values in grams per 100 g
Round off to
Less than 20
20 to 60
60 and over
11 Precision
Details of a n interlaboratory test on the precision of
the method are summarized in annex A. The values
derived from this interlaboratory test may not be
applicable to concentration ranges and matrices
other than those given.
11.1 Repeatability
The absolute difference between two independent
single test results, obtained using the same method
on identical test material in the same laboratory by
the same operator using the same equipment within
a short interval of time, should not be greater than
the value of r indicated in Table 3.
11.2 Reproducibility
The absolute difference between two single test
results, obtained using the same method on
identical test material in different laboratories with
different operators using different equipment,
should not be greater than the value of R indicated
in Table 3.
Table 3 - Repeatability and reproducibility
WI
g/100g
Less than 20
20 to 50
50 to 100
100 to 135
The test report shall specify
-the method in accordance with which sampling
was carried out, if known;
-the method used;
-the test result(s) obtained; and
- if the repeatability has been checked, the final
quoted result obtained.
It shall also mention all operating details not
specified in this International Standard, or
regarded a s optional (e.g. reaction time, see 9.2.3),
together with details of any incidents which may
have influenced the test result(s).
The test report shall include all information
necessary for the complete identification of the
sample.
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 Annex A (informative)
Interlaboratory test
International collaborative studies carried out
in 1988 to 1990 under the auspices of the IUPAC
Commission for Oils,Fats and Waxes gave the
statistical results shown in Table A . l when
evaluated in accordance with I S 0 5725.
Table A.2 displays the estimated mean
determination for each laboratory, for each of two
analytical methods (that given in the previous
edition of this International Standard and the
present method), and corrected for design imbalance
in the samples analysed. These means were derived
from the entire database, that is by analysing the
average of the A and B determinations
(see Table A.3). Table A.2 also displays the derived
mean difference between the results derived from
the two methods together with the pooled overall
difference and its standard error. The laboratory
mean values were closely similar and the good
agreement between laboratories for both methods is
further demonstrated by the between-laboratory
standard deviations given in Table 3. These are only
a little greater than the within-laboratory variation
with a coefficient of variation of 1,2% for the old
method and 1,3 % for the new cyclohexane/acetic
acid method. There is no consistent bias of one
method over the other from one laboratory to
another and the mean difference (Table A.2) is not
significantly different from zero.
The results of the fish oil collaborative trial confirm
those of the collaborative study of the same two
methods applied to a range of vegetable and animal
oils, including one sample of fish oil with a low
iodine value (Table A.l) in showing that
cyclohexanelacetic acid can be used in place of
carbon tetrachloride without loss of precision. --``,`-`-`,,`,,`,`,,`---

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 EN IS0 3961:1999 S T D - B S I B S E N IS0 3 ï b L - E N G L 2 0 0 0 1111111 L b 2 V b b 7 O d ô 8 2 V 5 a 8 7 W

1 tble A.1- Results of ir ierlaboratory tests

Sample No. of laboratories Mean iodine value
g/100 g
Palm kernel oil 8 18,3
Beef fat 10 46,9
Crude palm oil 9 52,6
Refined palm oil 10 53,2
Hardened fish oil 17 72,8
Hardened soyabean oil 17 74,8
Hardened soyabean oil 17 102,3
Sunflower seed oil 10 132,9

Table A 2 - Mean determinations of iodine value

Values in grams per 100
~~

Method given in
Laboratory Mean difference
IS0 3961:1989 IS0 3961:1996
using carbon tetrachloride using cyclohexanelacetic
acid (Vi)

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1 155,43 154,22 1,21
3 156,OZ 155,74 0,28
5 154,59 154,87 -0,28
6 154,64 155,61 -0,97
7 154,OO 154,29 -0,29
8 154,70 153,56 1,15
10 154,88 156,86 -1,98
Overall: -0,13 to +0,16

Table A3 - Summary of three “error” estimates

Values in grams per 100 g
Method $ven in
IS0 3961:1989 IS0 3961:1996
using carbon tetrachloride using cyclohexanelacetic acid (Vi)
Mean determinations of iodine value 154,9 155,O
i Standard deviation (percentage
of mean value) estimated from:
Open duplicates 1,08 (0,70) 0,66 (0,43)
Hidden duplicates Aa 1,71 (1,lO) 1,55 (1,OO)
Ba 1 , O l (0,65) 1,29 (0,83)
Between laboratories A 1,81(1,17) 1,98 (1,28)
B 1,43 (0,92) 1,79 (1,15)
a Comparison of hidden duplicate results in the first analysis of the samples (A) and hid en duplicates in second analysis of the
same samples (l3).

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 Annex B (informative)
Bibliography
[i]IS0 5555:1991,Animal and vegetable fats and oils - Sampling.
[2]IS0 5725:1986,Precision of test methods - Determination of repeatability and reproducibility by
interlaboratory tests (now withdrawn), was used to obtain the precision data.

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Annex ZA (normative)
Normative references to international publications with their relevant
European publications
This European Standard incorporates by dated or undated reference, provisions from other publications.
These normative references are cited at the appropriate places in the text and the publications are listed
hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply
to this European Standard only when incorporated in it by amendment or revision. For undated references
the latest edition of the publication referred to applies.

Publication Year Title EN Year

IS0 661 1989 Animal and vegetable fats and oils - EN IS0 661 1995
Preparation of test sample
IS0 3696 1987 Water for analytical laboratory use - EN IS0 3696 1995
Specification and test methods

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 3961:ZOOO
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