CEN/TS 13130-26:2005

SLOVENSKI STANDARD
01-april-2005
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Materials and articles in contact with foodstuffs - Plastics substances subject to limitation
- Part 26: Determination of 1-octene and tetrahydrofuran in food simulants
Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen,
die Beschränkungen unterliegen - Teil 26: Bestimmung von 1-Octen und Tetrahydrofuran
in Prüflebensmitteln
Matériaux et objets en contact avec les denrées alimentaires - Substances dans les
matieres plastiques soumises a des limitations - Partie 26 : Détermination du 1-octene et
du tétrahydrofurane dans les simulants d'aliments
Ta slovenski standard je istoveten z: CEN/TS 13130-26:2005
ICS:
67.250 Materiali in predmeti v stiku z Materials and articles in
živili contact with foodstuffs
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

TECHNICAL SPECIFICATION
CEN/TS 13130-26
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
February 2005
ICS 67.250
English version
Materials and articles in contact with foodstuffs - Plastics
substances subject to limitation - Part 26: Determination of 1-
octene and tetrahydrofuran in food simulants
Matériaux et objets en contact avec les denrées Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln
alimentaires - Substances dans les matières plastiques - Substanzen in Kunststoffen, die Beschränkungen
soumises à des limitations - Partie 26 : Détermination du 1- unterliegen - Teil 26: Bestimmung von 1-Octen und
octène et du tétrahydrofurane dans les simulants d'aliments Tetrahydrofuran in Prüflebensmitteln
This Technical Specification (CEN/TS) was approved by CEN on 16 December 2004 for provisional application.
The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to submit their
comments, particularly on the question whether the CEN/TS can be converted into a European Standard.
CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS available
promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the CEN/TS)
until the final decision about the possible conversion of the CEN/TS into an EN is reached.
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.
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EUROPÄISCHES KOMITEE FÜR NORMUNG
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© 2005 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 13130-26:2005: E
worldwide for CEN national Members.

Contents
page
Foreword. 3
Introduction . 5
1 Scope. 6
2 Normative references . 6
3 Method A – Determination of 1-octene in food simulants . 6
4 Method B – Determination of tetrahydrofuran in food simulants . 15
Bibliography . 25

Foreword
This document (CEN/TS 13130-26:2005) has been prepared by Technical Committee CEN/TC 194
“Utensils in contact with food”, the secretariat of which is held by BSI.
This part of EN 13130 has been prepared within the Standards, Measurement and Testing project,
MAT1-CT92-0006, “Development of Methods of Analysis for Monomers” and has been prepared by
Subcommittee (SC 1) of TC 194 "Utensils in contact with food" as one of a series of test methods for
plastics materials and articles in contact with foodstuffs.
This standard is intended to support Directives 2002/72/EC [1], 89/109/EEC [2], 82/711/EEC [3] and
its amendments 93/8/EEC [4] and 97/48/EC [5], and 85/572/EEC [6].
At the time of preparation and publication of this part of EN 13130 the European Union legislation
relating to plastics materials and articles intended to come into contact with foodstuffs is incomplete.
Further Directives and amendments to existing Directives are expected which could change the
legislative requirements which this standard supports. It is therefore strongly recommended that users
of this standard refer to the latest relevant published Directive(s) before commencement of a test or
tests described in this standard.
This part of EN 13130 should be read in conjunction with EN 13130-1.
Further parts of EN 13130, under the general title Materials and articles in contact with foodstuffs -
Plastics substances subject to limitation, have been prepared, and others are in preparation,
concerned with the determination of specific migration from plastics materials into foodstuffs and food
simulants and the determination of specific monomers and additives in plastics. The parts of
EN 13130 are as follows.
Part 1: Guide to test methods for the specific migration of substances from plastics to foods and food
simulants and the determination of substances in plastics and the selection of conditions of exposure
to food simulants
Part 2: Determination of terephthalic acid in food simulants
Part 3: Determination of acrylonitrile in food and food simulants
Part 4: Determination of 1,3-butadiene in plastics
Part 5: Determination of vinylidene chloride in food simulants
Part 6: Determination of vinylidene chloride in plastics
Part 7: Determination of monoethylene glycol and diethylene glycol in food simulants
Part 8: Determination of isocyanates in plastics
Part 9: Determination of acetic acid, vinyl ester in food simulants
Part 10: Determination of acrylamide in food simulants
Part 11: Determination of 11-aminoundecanoic acid in food simulants
Part 12: Determination of 1,3-benzenedimethanamine in food simulants
Part 13: Determination of 2,2-bis(4-hydroxyphenyl)propane (Bisphenol A) in food simulants
Part 14: Determination of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indoline in food simulants
Part 15: Determination of 1,3-butadiene in food simulants
Part 16: Determination of caprolactam and caprolactam salt in food simulants
Part 17: Determination of carbonyl chloride in plastics
Part 18: Determination of 1,2-dihydroxybenzene, 1,3-dihydroxybenzene,
1,4-dihydroxybenzene, 4,4’-dihydroxybenzophenone and 4,4’dihydroxybiphenyl in food simulants
Part 19: Determination of dimethylaminoethanol in food simulants
Part 20: Determination of epichlorohydrin in plastics
Part 21: Determination of ethylenediamine and hexamethylenediamine in food simulants
Part 22: Determination of ethylene oxide and propylene oxide in plastics
Part 23: Determination of formaldehyde and hexamethylenetetramine in food simulants
Part 24: Determination of maleic acid and maleic anhydride in food simulants
Part 25: Determination of 4-methyl-pentene in food simulants
Part 26: Determination of 1-octene and tetrahydrofuran in food simulants
Part 27: Determination of 2,4,6-triamino-1,3,5-triazine in food simulants
Part 28: Determination of 1,1,1-trimethylolpropane in food simulants
Parts 1 to 8 are European Standards. Parts 9 to 28 are Technical Specifications.
WARNING All chemicals are hazardous to health to a greater or lesser extent. It is beyond
the scope of this Technical Specification to give instructions for the safe handling of all
chemicals, that meet, in full, the legal obligations in all countries in which this Technical
Specification may be followed. Therefore, specific warnings are not given and users of this
Technical Specification should ensure that they meet all the necessary safety requirements in
their own country.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to announce this CEN Technical Specification: 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.
Introduction
1-octene, C H or CH =CH-(CH ) –CH , PM/Ref. No 22660, and tetrahydrofuran (THF), C H O,
8 16 2 2 5 3 4 8
PM/Ref. No 25150, are monomers used in the manufacture of certain plastics materials and articles
intended to come into contact with foodstuffs. After manufacture, residual monomer can remain in the
polymer and may migrate into foodstuffs coming into contact with that plastics article.
NOTE However, the following should be taken into account at carrying out a migration test for 1-octene.
From migration experiments carried out for 10 d for 40 °C it was recognized that irreproducible loss of 1-octene,
11 % to 69 %, due to volatilization, can arise when using aqueous food simulants.
Method A describes the determination of 1-octene in food simulants.
Method B describes the determination of tetrahydrofuran in food simulants.
The methods have been pre-validated by collaborative trials with two laboratories.
1 Scope
This document, part of EN 13130, specifies analytical procedures for the determination of 1-octene
and THF in food simulants water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and olive
oil. The level of 1-octene and THF monomer determined is expressed as milligrams of monomer per
kilogram of food simulant. The methods are appropriate for the quantitative determination of 1-octene
in the range of 2 mg/kg to 30 mg/kg in food simulants and of THF in the range of 0,06 mg/kg to 1,5
mg/kg in food simulants.
NOTE The method should also be applicable to other aqueous food simulants as well as to the other fatty
food simulants e.g. sunflower oil, corn oil or a mixture of synthetic triglycerides.
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.
EN 13130-1:2004, Materials and articles in contact with foodstuffs – Plastics substances subject to
limitation – Part 1: Guide to test methods for the specific migration of substances from plastics to
foods and food simulants and the determination of substances in plastics and the selection of
conditions of exposure to food simulants.
3 Method A – Determination of 1-octene in food simulants
3.1 Principle
The level of 1-octene in a food or a food simulant is determined by headspace gas chromatography
(HSGC) of the food simulant sample, sealed in headspace glass vials. Headspace gas
chromatography is carried out applying automatic injection and flame ionization detection.
Quantification is achieved using iso-octane as internal standard with calibration against food simulant
samples fortified with known amounts of 1-octene. Confirmation of 1-octene levels is carried out by
combined gas chromatography/mass spectrometry (GC/MS).
3.2 Reagents
NOTE All reagents should be of recognized analytical quality unless otherwise stated.
3.2.1 Analytes
3.2.1.1 1-octene, CH =CH-(CH ) –CH , purity greater than 97,5 % (GC).
2 2 5 3
3.2.1.2 Iso-octane, (CH ) -CH-CH -C(CH ) , purity greater than 99 % (GC).
3 2 2 3 3
3.2.2 Chemical
N,N-dimethylacetamide (DMAA), CH -CO-N(CH ) , purity greater than 99 %.
3 3 2
3.2.3 Solutions
3.2.3.1 Stock solutions of 1-octene with a defined concentration of approximately 2 mg/ml in
DMAA
Weigh a 50 ml volumetric flask, including cap, filled with about 45 ml of DMAA (3.2.2), to an accuracy
of 0,1 mg. Add approximately 100 mg of 1-octene (about 150 µl), then reweigh to an accuracy of
0,1 mg. Make up to 50 ml with DMAA. Close and shake.
Calculate the exact concentration of the stock solution in milligrams of 1-octene per millilitre of
solution.
Repeat the procedure to provide a second stock solution.
NOTE These stock solutions can be stored at + 4 °C, with the exclusion of light, for up to 3 months.
3.2.3.2 Standard solutions of 1-octene in DMAA with a defined concentration of
approximately 200 µg/ml
Place 1,0 ml of the 1-octene stock solution (3.2.3.1) in a 10 ml volumetric flask and make up to the
mark with DMAA (3.2.2). Close and mix thoroughly.
Calculate the exact concentration of the standard solution in milligrams of 1-octene per millilitre of
solution.
Repeat the procedure using the second stock solution prepared in 3.2.3.1 to provide a second
standard solution.
NOTE These standard solutions can be stored at + 4 °C and with the exclusion of light for up to 3 months.
3.2.3.3 Stock solution of internal standard iso-octane in DMAA at a defined concentration of
approximately 2 mg/ml
Weigh a 50 ml volumetric flask, including cap, filled with about 45 ml of DMAA (3.2.2), to an accuracy
of 0,1 mg. Add approximately 100 mg of iso-octane (about 150 µl), then reweigh to an accuracy of
0,1 mg. Make up to the mark with DMAA close and mix.
...