CEN/TS 13130-25:2005

SLOVENSKI STANDARD
01-april-2005
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Materials and articles in contact with foodstuffs - Plastics substances subject to limitation
- Part 25: Determination of 4-methyl-1-pentene in food simulants
Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen,
die Beschränkungen unterliegen - Teil 25: Bestimmung von 4-Methyl-1-Penten in
Prüflebensmitteln
Matériaux et objets en contact avec les denrées alimentaires - Substances dans les
matieres plastiques soumises a des limitations - Partie 25 : Détermination du 4-méthyl-1
pentene dans les simulants d'aliments
Ta slovenski standard je istoveten z: CEN/TS 13130-25:2005
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 13130-25
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
February 2005
ICS 67.250
English version
Materials and articles in contact with foodstuffs - Plastics
substances subject to limitation - Part 25: Determination of 4-
methyl-1-pentene 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 25 : Détermination du 4- unterliegen - Teil 25: Bestimmung von 4-Methyl-1-Penten in
méthyl-1 pentène dans les simulants d'aliments 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.
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. CEN/TS 13130-25:2005: E
worldwide for CEN national Members.

Contents
page
Foreword. 3
Introduction . 5
1 Scope. 6
2 Normative references . 6
3 Principle . 6
4 Reagents . 6
5 Apparatus . 8
6 Samples . 8
7 Procedure . 10
8 Expression of results. 11
9 Confirmation. 12
10 Test report . 13
Bibliography . 14

Foreword
This document (CEN/TS 13130-25:2005) 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
4-methyl-1-pentene, C H , PM/Ref. No 22150 is a monomer used in the manufacture of certain
6 12
plastics materials and articles intended to come into contact with foodstuffs. After manufacture
residual 4-methyl-1-pentene can remain in the finished product and may migrate into foodstuffs
coming into contact with that product.
NOTE However, the following should be taken into account when carrying out a migration test. From
migration experiments carried out at 10 d for 40 °C it was recognized that there was an irreproducible and
considerable loss of 4-methyl-1-pentene, 35 % to 98 %, due to volatilization when using aqueous food simulants.
The method has been pre-validated by collaborative trials with two laboratories.
1 Scope
This document, part of EN 13130, specifies an analytical procedure for the determination of 4-methyl-
1-pentene in food simulants distilled water, 3 % (w/v) aqueous acetic acid aqueous solution, 15 %
(v/v) aqueous ethanol aqueous solution and rectified olive oil. The level of
4-methyl-1-pentene monomer determined is expressed as milligrams per kilogram of food simulant. In
principle, the method is appropriate for the quantitative determination of 4-methyl-1-pentene at a
minimum level of 0,005 mg/kg in all of the four food simulants. However, in the case of interferences,
which have been observed for some olive oil batches, the detection limit can be compromised
correspondingly.
NOTE The method should also be applicable to other aqueous food simulants as well as to other fatty food
simulants such as corn oil, sunflower oil and 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 Principle
The level of 4-methyl-1-pentene in food simulants is determined by headspace gas chromatography
(HSGC). Quantification is achieved using an internal standard, cyclohexane. Calibration is realized by
analysis of relevant food simulant samples containing known amounts of 4-methyl-1-pentene and
cyclohexane.
NOTE If automatic headspace equipment is applied, the use of an internal standard is not required.
Repeatability may even be improved without use of the internal standard.
Confirmation of 4-methyl-1-pentene is carried out by combined gas chromatography/mass
spectrometry (GC/MS).
4 Reagents
NOTE All reagents should be of recognized analytical quality unless otherwise stated.
4.1 Analytes
4.1.1 4-methyl-1-pentene, C H , molecular weight: 84,16, purity ≥ 98 %.
6 12
4.1.2 Cyclohexane, C H , molecular weight: 84,16, purity ≥ 99,5 %.
6 12
4.2 Chemical
N,N-dimethylacetamide - distilled (DMAA)
4.3 Solutions
4.3.1 Stock solution of 4-methyl-1-pentene (1 mg/ml)
Weigh to the nearest 0,1 mg approximately 25 mg of 4-methyl-1-pentene into a 25 ml volumetric flask,
which contains approximately 20 ml of DMAA. Make up to the mark with DMAA and mix carefully.
Calculate the concentration in milligrams of 4-methyl-1-pentene per millilitre of solution.
Repeat the procedure to obtain a second stock solution.
NOTE The stock solution can be stored in a well closed container, with the exclusion of light, for a maximum
of 3 weeks at any temperature between - 20 °C and + 10 °C.
4.3.2 Internal standard stock solution of cyclohexane in DMAA (1 mg/ml)
Weigh to the nearest 0,1 mg, approximately 25 mg of cyclohexane into a 25 ml volumetric flask.
Make up to the mark with DMAA.
Calculate the concentration in milligrams of cyclohexane per millilitre of solution.
NOTE The solution can be stored in a well closed container, with the exclusion of light, for a maximum of
2 weeks at any temperature between - 20 °C and + 10 °C.
4.3.3 Diluted internal standard solution of cyclohexane in DMAA (50 µg/ml)
Transfer with a microsyringe 500 µl of the internal standard stock solution (4.3.2) into a 10 ml
volumetric flask and make up to the mark with DMAA.
Calculate the concentration in micrograms of cyclohexane per millilitre of solution.
NOTE The solution can be stored in a well closed container, with the exclusion of light, for a maximum of
2 weeks at any temperature between - 20 °C and + 10 °C.
4.3.4 Diluted standard solution (10 µg/ml)
Transfer into a 10 ml volumetric flasks approximately 7 ml DMAA. Add with the aid of a microsyringe
100 µl of the standard stock solution of 4-methyl-1-pentene (4.3.1). The tip of the syringe shall be
submerged into DMAA at the moment the syringe is emptied. Make up to the mark with DMAA.
The standard solution thus obtained contains 10 µg of 4-methyl-1-pentene/ml DMAA.
Repeat the procedure using the second standard stock solution.
NOTE The solution can be stored in a closed container, with the exclu
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