SIST EN ISO 9832:2003

• Abstract:

  This International Standard specifies a method for the determination of the residual technical hexane content of animal and vegetable fats and oils.; The method is suitable for the determination of hexane contents between 10 mg and 1 500 mg per kilogram of fat or oil.; The method is not applicable to marine oils

• Status: Published
• Publication Date: 31-Oct-2003
• ICS: 67.200.10 - Animal and vegetable fats and oils
• Technical Committee: KŽP - Agricultural food products
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 01-Nov-2003
• Due Date: 01-Nov-2003
• Completion Date: 01-Nov-2003
• Ref Project: EN ISO 9832:2003 - Animal and vegetable fats and oils - Determination of residual technical hexane content (ISO 9832:2002)

• Replaces: SIST EN ISO 9832:2001 - Animal and vegetable fats and oils - Determination of residual technical hexane content (ISO 9832:1992, including Amendment 1:1998)
• Effective Date: 01-Nov-2003
• Refers: SIST ISO 661:1995 - Animal and vegetable fats and oils -- Preparation of test sample
• Effective Date: 25-Aug-2026
• Refers: SIST EN 12544-1:2000 - Non-destructive testing - Measurement and evaluation of the X-ray tube voltage - Part 1: Voltage divider method
• Effective Date: 28-Jan-2026

SIST EN ISO 9832:2003 is the Slovenian adoption of EN ISO 9832:2003, published by SIST and based on ISO 9832:2002. It specifies a gas chromatographic method for determining residual technical hexane in animal and vegetable fats and oils, for laboratories and quality staff checking solvent residues in fat processing.

What does SIST EN ISO 9832:2003 specify?

SIST EN ISO 9832:2003 specifies a method for measuring residual technical hexane content in animal and vegetable fats and oils. The method is intended for hexane contents from 10 mg/kg to 1 500 mg/kg, and it is not applied to marine oils.

The document is organized as a short analytical method with clauses for scope, reference material, principle, reagents, apparatus, sampling, test sample preparation, procedure, expression of results, precision, and the test report. It also includes an informative annex with interlaboratory precision data and a normative annex on references used with the European publication.

Annex	What it covers
Annex A	Interlaboratory test results and precision data for the method
Annex ZA	Normative references to international publications with the relevant European publications

What are the key requirements of SIST EN ISO 9832:2003?

SIST EN ISO 9832:2003 measures residual technical hexane by headspace gas chromatography after heating the fat sample in a closed vial. In practice, this means the analyst does not measure the fat directly in the injector; the volatile hydrocarbons are driven into the gas phase and then separated and measured.

Sample range and suitability

The method is suitable only within the stated concentration range of 10 mg/kg to 1 500 mg/kg. That matters because results outside this range are not covered by the stated performance of the method. The scope also excludes marine oils, so a laboratory should choose another method for that matrix.

Sample preparation and handling

Clause 7 points the user to representative sampling and says the sample must be protected from gain or loss of solvent residues. Clause 8 requires preparation of the test sample in accordance with ISO 661. In practice, this means transport, storage, and subsampling must avoid evaporation or contamination before analysis.

Principle of the measurement

Clause 4 states that the volatile hydrocarbons are desorbed by heating at 80 °C in a closed vessel after adding an internal standard. The headspace is then analyzed by gas chromatography, using either packed or capillary columns. This gives the laboratory a direct instrumental route for identifying and quantifying the hexane-related peaks.

Reagents and internal standard

Clause 5 requires analytical-grade reagents and gives technical hexane as the calibration solvent, with n-hexane as an alternative if needed. The internal standard is n-heptane, with cyclohexane allowed when the solvent used has negligible overlap. In practice, the internal standard is what anchors the calculation, so the lab must keep it consistent across calibration and test portions.

Apparatus and operating conditions

Clause 6 specifies septum vials, inert septa, gas-tight syringes, and a gas chromatograph with a flame ionization detector. It also sets the column options and the main temperatures: injector and detector at 100 °C, oven at 50 °C, and the vial bath at 80 °C ± 2 °C. These settings matter because the separation and response depend on keeping the chromatographic system stable and comparable from run to run.

Calibration and determination

Clause 9 requires a seven-vial calibration set built from calibration fat and known additions of technical hexane. The analyst then calculates a calibration factor from the chromatograms and uses that mean factor for sample results. For the sample itself, two test portions are analyzed in rapid succession, which helps check whether the result is repeatable before it is reported.

Result reporting and precision

Clause 10 gives the calculation of residual technical hexane content from the sample chromatogram and the mean calibration factor. The final result is the mean of the two determinations, provided the repeatability requirement is met. Clause 11 ties the method to interlaboratory precision data in Annex A, so users can judge whether two results agree closely enough for routine reporting or dispute comparison.

What terms does SIST EN ISO 9832:2003 define?

Clause 3 defines residual technical hexane content as the content of volatile hydrocarbons remaining in fats after processing with hydrocarbon solvents, expressed in milligrams of hexane per kilogram of sample. In practice, that is the reported value the laboratory is trying to obtain.

An internal standard is the reference compound added at a known amount before analysis, so the chromatographic response can be compared with the sample peaks. The method uses n-heptane, or cyclohexane when suitable.

A calibration fat is a freshly refined and deodorized vegetable fat with negligible technical hexane content. It provides the base matrix for preparing calibration samples that behave like real test samples.

The headspace is the gaseous phase above the heated fat in the sealed vial. The gas chromatograph measures that gas phase, which is where the volatile hydrocarbons are collected.

A test portion is the weighed part of the prepared sample taken for analysis. The method uses duplicate test portions so the laboratory can check repeatability.

Repeatability is the agreement between two results from the same laboratory under the same conditions, while reproducibility is the agreement between results from different laboratories. These terms matter because the method sets precision expectations for routine use and interlaboratory comparison.

Who uses SIST EN ISO 9832:2003?

SIST EN ISO 9832:2003 is used by analytical laboratories testing fats and oils, especially in the edible oils and fats sector. It also supports quality control teams in processing plants that need to verify residual solvent levels after extraction or refining.

Buyers, suppliers, and inspectors may use the results when they need a common test method for comparing product lots. The method is most relevant where animal or vegetable fats and oils may retain technical hexane after solvent-based processing.

What changed in SIST EN ISO 9832:2003 from the previous edition?

The foreword states that this second edition cancels and replaces ISO 9832:1992 and that it is a minor revision incorporating Amendment 1:1998. The European version, EN ISO 9832:2003, supersedes EN ISO 9832:2000.

Which standards are used with SIST EN ISO 9832:2003?

ISO 661:1989, Animal and vegetable fats and oils - Preparation of test sample, is the main normative reference. It supplies the sample preparation step used before the hexane determination.

ISO 5555:1991, Animal and vegetable fats and oils - Sampling, is cited as the recommended sampling method. It helps users obtain a representative sample before the test sample is prepared.

ISO 5725:1986 and the later parts ISO 5725-1:1994 and ISO 5725-2:1994 are named in connection with the precision data in Annex A. They provide the statistical basis for evaluating repeatability and reproducibility.

What does the SIST EN ISO 9832:2003 document contain?

The document contains the full analytical procedure, from sample handling through gas chromatographic measurement to calculation of the final result. It includes the reagent list, the apparatus list, the calibration procedure, the test procedure, and the calculation approach for converting chromatographic response into mg/kg.

It also gives an example chromatogram that identifies the relevant peaks, including the hexane-related peaks and the internal standard. That helps analysts see which signals to measure and which ones to ignore.

Annex A contains the collaborative-test data used to support the stated precision, including results from sunflowerseed oil and soyabean oil samples. These data support practical decisions on whether a result is close enough to be accepted.

SLOVENSKI STANDARD
01-november-2003
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SIST EN ISO 9832:2001
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,62
Animal and vegetable fats and oils - Determination of residual technical hexane content
(ISO 9832:2002)
Tierische und pflanzliche Fette und Öle - Bestimmung des Gehaltes an technischem
Resthexan (ISO 9832:2002)
Corps gras d'origines animale et végétale - Dosage de l'hexane technique résiduel (ISO
9832:2002)
Ta slovenski standard je istoveten z: EN ISO 9832:2003
ICS:
67.200.10 5DVWOLQVNHLQåLYDOVNH Animal and vegetable fats
PDãþREHLQROMD and oils
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EUROPEAN STANDARD
EN ISO 9832
NORME EUROPÉENNE
EUROPÄISCHE NORM
July 2003
ICS 67.200.10 Supersedes EN ISO 9832:2000
English version
Animal and vegetable fats and oils - Determination of residual
technical hexane content (ISO 9832:2002)
Corps gras d'origines animale et végétale - Dosage de Tierische und pflanzliche Fette und Öle - Bestimmung des
l'hexane technique résiduel (ISO 9832:2002) Gehaltes an technischem Resthexan (ISO 9832:2002)
This European Standard was approved by CEN on 10 July 2003.
CEN members are bound to comply with the CEN/CENELEC 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 Management Centre 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 notified to the Management Centre 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,
Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and United
Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36  B-1050 Brussels
© 2003 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 9832:2003 E
worldwide for CEN national Members.

Foreword
The text of ISO 9832:2002 has been prepared by Technical Committee ISO/TC 34 "Agricultural
food products” of the International Organization for Standardization (ISO) and has been taken
over as EN ISO 9832:2003 by Technical Committee 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.
This European Standard shall be given the status of a national standard, either by publication of
an identical text or by endorsement, at the latest by January 2004, and conflicting national
standards shall be withdrawn at the latest by January 2004.
This document supersedes EN ISO 9832:2000.
According to the CEN/CENELEC 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, Hungary, Iceland, Ireland, Italy,
Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and
the United Kingdom.
Endorsement notice
The text of ISO 9832:2002 has been approved by CEN as EN ISO 9832:2003 without any
modifications.
NOTE Normative references to International Standards are listed in annex ZA (normative).
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 (including amendments).
NOTE Where an International Publication has been modified by common modifications, indicated
by (mod.), the relevant EN/HD applies.
Publication Year Title EN Year
ISO 661 1989 Animal and vegetable fats and oils - EN ISO 661 1995
Preparation of test sample
INTERNATIONAL ISO
STANDARD 9832
Second edition
2002-02-15
Animal and vegetable fats and oils —
Determination of residual technical hexane
content
Corps gras d'origines animale et végétale — Dosage de l'hexane technique
résiduel
Reference number
ISO 9832:2002(E)
©
ISO 2002
ISO 9832:2002(E)
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ii © ISO 2002 – All rights reserved

ISO 9832:2002(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO
member bodies). The work of preparing International Standards is normally carried out through ISO technical
committees. Each member body interested in a subject for which a technical committee has been established has
the right to be represented on that committee. International organizations, governmental and non-governmental, in
liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical
Commission (IEC) on all matters of electrotechnical standardization.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3.
The main task of technical committees is to prepare International Standards. Draft International Standards adopted
by the technical committees are circulated to the member bodies for voting. Publication as an International
Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this International Standard may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 9832 was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 11, Animal and
vegetable fats and oils.
This second edition cancels and replaces the first edition (ISO 9832:1992), of which it constitutes a minor revision
to incorporate Amendment 1:1998.
Annex A of this International Standard is for information only.

INTERNATIONAL STANDARD ISO 9832:2002(E)

Animal and vegetable fats and oils — Determination of residual
technical hexane content
1 Scope
This International Standard specifies a method for the determination of the residual technical hexane content of
animal and vegetable fats and oils (referred to as fats hereinafter).
The method is suitable for the determination of hexane contents between 10 mg and 1 500 mg per kilogram of fat.
The method is not applicable to marine oils
2 Normative reference
The following normative document contains provisions which, through reference in this text, constitute provisions of
this International Standard. For dated references, subsequent amendments to, or revisions of, any of these
publications do not apply. However, parties to agreements based on this International Standard are encouraged to
investigate the possibility of applying the most recent edition of the normative document indicated below. For
undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC
maintain registers of currently valid International Standards.
ISO 661:1989, Animal and vegetable fats and oils — Preparation of test sample
3 Term and definition
For the purposes of this International Standard, the following term and definition applies.
3.1
residual technical hexane content
content of volatile hydrocarbons such as those remaining in fats following processing involving the use of
hydrocarbon solvents, when determined by the method specified in this International Standard
NOTE The content is expressed as milligrams of hexane per kilogram of sample.
4 Principle
Desorption of volatile hydrocarbons by heating at 80 °C in a closed vessel after addition of an internal standard.
Determination of the particular volatile hydrocarbons content of the headspace by gas chromatography using
packed or capillary columns.
5 Reagents
Use only reagents of recognized analytical grade, unless otherwise stated, and distilled or demineralized water or
water of equivalent purity.
ISO 9832:2002(E)
5.1 Technical hexane, with a composition similar to that of hexane used in industrial processing or, if this is not
available, n-hexane.
It is recommended that technical hexane be used for the calibration. This reagent usually has an n-hexane content
of 50 % (by mass) and consists mainly of C isomers but may include C and C hydrocarbons.
6 5 7
5.2 Internal standard, n-heptane.
If this is not available, cyclohexane may be used, provided that the solvent (5.1) used for the extraction or
calibration has a negligible content of cyclohexane and/or n-heptane or components with similar retention times.
5.3 Carrier gas, e.g. hydrogen, nitrogen or helium, etc., thoroughly dried and with an oxygen content of less
than 10 mg/kg.
5.4 Auxiliary gases, hydrogen (99,9 % pure, free from organic impurities) and air (free from organic impurities).
5.5 Calibration fat, freshly refined and deodorized vegetable fat, the technical hexane content of which is
negligible.
This material should be free from peroxides or other components likely to decompose with the formation of volatile
material which could be confused with hydrocarbons during the test.
6 Apparatus
Usual laboratory equipment and, in particular, the following.
6.1 Septum vials, of 20 ml capacity.
6.2 Septa, inert to fats and solvents, made of a material such as butyl rubber or red rubber free from
hydrocarbon solvent residues and of a suitable quality that they will not swell under the conditions of use,
aluminium caps suitable for use with the vials (6.1) and crimping pliers.
6.3 Tongs, suitable for holding the vials (6.1).
6.4 Syringes, of 10 µl capacity, used only for the analysis of residual technical hexane. They shall not be
cleaned with hydrocarbon solvent.
6.5 Syringes, of 1 µl capacity, used only for the analysis of residual technical hexane. They shall not be cleaned
with hydrocarbon solvent.
6.6 Syringes, of 1 000 µl capacity, gas-tight, used only for the analysis of residual technical hexane. They shall
not be cleaned with hydrocarbon solvent.
6.7 Gas chromatograph, with a flame ionization detector and an integrator and/or recorder, equipped with
either
a) a packed glass column, 2 m to 4 m long and of internal diameter 3,2 mm approximately, packed with an acid-
washed and silanized diatomaceous earth support of particle size 150 µm to 180 µm (Chromosorb P NAW
1)
60-80 mesh is suitable), and coated with 10 % squalane or any other phase permitting the chromatographic
separation required, or
b) a glass capillary column, approximately 30 m long and of 0,3 mm internal diameter, coated with
methylpolysiloxane of film thickness 0,2 µm.

1) Chromosorb P NAW 60-80 is an
...