SIST EN ISO 16035:2005

SLOVENSKI STANDARD
01-december-2005
5DVWOLQVNHLQåLYDOVNHPDãþREHLQROMD±'RORþHYDQMHKDORJHQLUDQLKRJOMLNRYRGLNRY
]QL]NLPYUHOLãþHPYMHGLOQLKROMLK,62
Animal and vegetable fats and oils - Determination of low-boiling halogenated
hydrocarbons in edible oils (ISO 16035:2003)
Tierische und pflanzliche Fette und Öle - Bestimmung von niedrig siedenden
halogenierten Kohlenwasserstoffen in Speiseölen (ISO 16035:2003)
Corps gras d'origines animale et végétale - Dosage des hydrocarbures halogénés a bas
point d'ébullition dans les huiles comestibles (ISO 16035:2003)
Ta slovenski standard je istoveten z: EN ISO 16035:2005
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 16035
NORME EUROPÉENNE
EUROPÄISCHE NORM
August 2005
ICS 67.200.10
English Version
Animal and vegetable fats and oils - Determination of low-boiling
halogenated hydrocarbons in edible oils (ISO 16035:2003)
Corps gras d'origines animale et végétale - Dosage des Tierische und pflanzliche Fette und Öle - Bestimmung von
hydrocarbures halogénés à bas point d'ébullition dans les niedrig siedenden halogenierten Kohlenwasserstoffen in
huiles comestibles (ISO 16035:2003) Speiseölen (ISO 16035:2003)
This European Standard was approved by CEN on 28 July 2005.
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 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 notified to the Central Secretariat has the same status as the official
versions.
CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,
Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,
Slovenia, 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
© 2005 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 16035:2005: E
worldwide for CEN national Members.

Foreword
The text of ISO 16035:2003 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 16035:2005 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 February 2006, and conflicting national
standards shall be withdrawn at the latest by February 2006.

According to the CEN/CENELEC Internal Regulations, the national standards organizations of
the following countries are bound to implement this European Standard: Austria, Belgium,
Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary,
Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,
Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.

Endorsement notice
The text of ISO 16035:2003 has been approved by CEN as EN ISO 16035:2005 without any
modifications.
INTERNATIONAL ISO
STANDARD 16035
First edition
2003-04-15
Animal and vegetable fats and oils —
Determination of low-boiling halogenated
hydrocarbons in edible oils
Corps gras d'origines animale et végétale — Dosage des
hydrocarbures halogénés à bas point d'ébullition dans les huiles
comestibles
Reference number
ISO 16035:2003(E)
©
ISO 2003
ISO 16035:2003(E)
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ii © ISO 2003 — All rights reserved

ISO 16035:2003(E)
Contents Page
Foreword. iv
1 Scope. 1
2 Normative references . 1
3 Terms and definitions. 1
4 Principle . 1
5 Reagents and materials. 1
6 Apparatus. 3
7 Sampling . 4
8 Preparation of samples . 5
8.1 General. 5
8.2 Test solutions. 5
8.3 Calibration solutions . 5
8.4 Blank sample . 5
9 Procedure. 5
9.1 Gas chromatography conditions. 5
9.2 Gas chromatography. 6
10 Calculation and expression of results . 7
10.1 Determination of the ratios from the measurement for the sample and internal standard. 7
10.2 Calculation of regression from calibration solutions . 7
10.3 Calculation of the content of halogenated hydrocarbons. 7
11 Precision . 8
11.1 Results of interlaboratory test. 8
11.2 Repeatability. 8
11.3 Reproducibility . 8
12 Test report. 8
Annex A (informative) Results of interlaboratory test . 9
Bibliography . 12

ISO 16035:2003(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 2.
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 document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 16035 was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 11, Animal
and vegetable fats and oils.
iv © ISO 2003 — All rights reserved

INTERNATIONAL STANDARD ISO 16035:2003(E)

Animal and vegetable fats and oils — Determination of
low-boiling halogenated hydrocarbons in edible oils
1 Scope
This International Standard specifies a method for the determination of low-boiling halogenated hydrocarbons
by means of static headspace gas chromatography. Halogenated hydrocarbon solvents are ubiquitously
distributed toxic compounds. The method is applicable to all edible fats and oils to determine these
compounds in the range 0,01 mg/kg to 0,2 mg/kg.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
ISO 661:1989, Animal and vegetable fats and oils — Preparation of test sample
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
halogenated hydrocarbons content
content of low-boiling halogenated hydrocarbons in the products determined by the method specified in this
International Standard
NOTE 1 The halogenated hydrocarbons content is expressed in milligrams per kilogram.
NOTE 2 For the purposes of this International Standard, the term low-boiling halogenated hydrocarbons covers those
specified in 5.1.
4 Principle
The contents of halogenated hydrocarbons in the test sample are determined by manual or automatic static
headspace gas chromatography of a sample drawn from the vapour space above the heated test sample. A
capillary column is used for separation, and detection is carried out by means of an electron capture detector
(ECD). An internal standard is used to obtain a quantitative evaluation. For the purpose of calibration,
calibration curves are obtained by the addition of various halogenated hydrocarbon calibration solutions to a
blank sample.
5 Reagents and materials
WARNING — Attention is drawn to the regulations which prescribe the handling of dangerous matter.
Technical, organizational and personal safety measurements shall be followed.
Use only reagents of recognized analytical grade unless otherwise stated.
ISO 16035:2003(E)
5.1 Standard substances, of appropriate purity as required by the nature and number of components to be
determined, for example, the following.
5.1.1 1,1,1-Trichloroethane, density = 1,34 g/ml.
5.1.2 Tetrachloromethane, density = 1,59 g/ml.
5.1.3 1,1,2-Trichloroethene, density = 1,46 g/ml.
5.1.4 Tetrachloroethene, density = 1,63 g/ml.
5.1.5 2-Bromo-1-chloropropane (internal standard), density = 1,54 g/ml.
5.1.6 Dichloromethane (methylene chloride), density = 1,32 g/ml.
5.1.7 Trichloromethane (chloroform), density = 1,47 g/ml.
5.1.8 Bromodichloromethane, density = 1,98 g/ml.
5.1.9 Dibromochloromethane, density = 2,45 g/ml.
5.1.10 Tribromomethane (bromoform), density = 2,89 g/ml.
5.1.11 1,1,2-Trichloro-1,2,2-trifluoroethane, density = 1,57 g/ml.
5.2 Isooctane, suitable for haloform analysis. Check the isooctane for its halogenated hydrocarbons
content.
5.3 Nitrogen (extra purified), helium or hydrogen, as carrier gas.
5.4 Argon/methane or nitrogen, as purge gas for the ECD.
Use in accordance with the manufacturer's instructions.
5.5 Halogenated hydrocarbons stock solutions
Add 10 µl of each of the standard substances (5.1) to be determined to a 100 ml volumetric flask that contains
40 ml of isooctane, using an injection syringe and make up to the mark. However, only add 5 µl of
tetrachloromethane since its detection sensitivity is very high, but add 500 µl of dichloromethane since its
detection sensitivity is very low.
These stock solutions contain:
 1,1,1-trichloroethane: 13,40 mg/100 ml;
 tetrachloromethane: 7,95 mg/100 ml;
 1,1,2-trichloroethene: 14,60 mg/100 ml;
 tetrachloroethene: 16,30 mg/100 ml;
 dichloromethane: 660,00 mg/100 ml;
 trichloromethane: 14,70 mg/100 ml;
 bromodichloromethane: 19,80 mg/100 ml;
 dibromochloromethane: 24,50 mg/100 ml;
 tribromomethane: 28,90 mg/100 ml;
 1,1,2-trichloro-1,2,2-trifluoroethane: 15,70 mg/100 ml.
2 © ISO 2003 — All rights reserved

ISO 16035:2003(E)
5.6 Halogenated hydrocarbons standard solutions I, II, III and IV
Use the stock solution (5.5) to prepare standard solutions (I, II, III, IV) of appropriate concentrations by adding,
for example, 200 µl, 400 µl, 1 000 µl and 2 000 µl of the stock solution to 10 ml volumetric flasks that contain a
little isooctane, and make up to the mark with isooctane.
The internal standard (5.7) may also be added to the halogenated hydrocarbon standard solutions.
5.7 Internal standard solution (2-bromo-1-chloropropane solution).
Add 200 µl 2-bromo-1-chloropropane to a little isooctane in a 50 ml volumetric flask using an injection syringe
and make up to the mark with isooctane (concentration by mass = 308 mg/50 ml).
In order to obtain a suitable dilution, add 400 µl of the above solution to a little isooctane in a 10 ml volumetric
flask and make up to the mark with isooctane. The conc
...