CEN/TS 13130-15:2005

Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 15: Determination of 1,3-butadiene in food simulants

This document, part of EN 13130, specifies an analytical procedure for the determination of butadiene monomer in the food simulants water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and olive oil. The level of butadiene monomer determined is expressed as mg butadiene/kg of food. The method is appropriate for the quantitative determination of butadiene at a range of 0,01 mg/kg to 0,1 mg/kg in food simulants.
NOTE   The method should also be applicable to other aqueous food simulants and to the other fatty food simulants such as sunflower oil and a mixture of synthetic triglycerides.

Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen, die Beschränkungen unterliegen - Teil 15: Bestimmung von 1,3-Butadien in Prüflebensmitteln

Diese Technische Spezifikation, Teil der EN 13130, legt ein Analyseverfahren zur Bestimmung von monomerem Butadien in den Prüflebensmitteln Wasser, 3%ige Essigsäure (m/V) in wässriger Lösung, 15%iges Ethanol (Volumenanteil) in wässriger Lösung und Olivenöl fest. Der ermittelte Gehalt an monomerem Butadien wird in Milligramm Butadien je Kilogramm Lebensmittel angegeben. Das Verfahren eignet sich zur quantitativen Bestimmung von Butadien im Bereich von 0,01 mg/kg bis 0,1 mg/kg Prüflebensmittel.
ANMERKUNG   Das Verfahren sollte auch auf andere wässrige Prüflebensmittel sowie weitere fettige Prüflebensmittel, wie z. B. Sonnenblumenöl und eine Mischung synthetischer Triglyceride, anwendbar sein.

Matériaux et objets en contact avec les denrées alimentaires - Substances dans les matières plastiques soumises à des limitations - Partie 15: Détermination du 1,3-butadiène dans les simulants d'aliments

Le présent document qui fait partie de l'EN 13130, spécifie un mode opératoire d'analyse pour la détermination du butadiène dans les quatre simulants d'aliments suivants : eau, solution aqueuse d'acide acétique à 3 % (m/v), solution aqueuse d'éthanol à 15 % (v/v) et huile d'olive. La teneur en butadiène déterminée est exprimée en mg de butadiène par kg de denrée alimentaire. Cette méthode convient pour la détermination quantitative du butadiène dans une gamme de concentrations comprise entre 0,01 mg/kg et 0,1 mg/kg dans les simulants d'aliments.
NOTE   Il convient que cette méthode puisse également être appliquée à d'autres simulants aqueux ainsi qu'à des simulants gras tels que l'huile de tournesol ou un mélange de triglycérides synthétiques.

Materiali in predmeti v stiku z živili - Snovi v polimernih materialih, katerih koncentracija je omejena - 15. del: Določevanje 1,3-butadiena v modelnih raztopinah za živila

General Information

• Status: Published
• Publication Date: 30-May-2005
• ICS: 67.250 - Materials and articles in contact with foodstuffs
• Technical Committee: CEN/TC 194 - Utensils in contact with food
• Drafting Committee: CEN/TC 194/SC 1/WG 2 - Methods of test for monomers
• Current Stage: 6060 - Definitive text made available (DAV) - Publishing
• Start Date: 23-Feb-2005
• Completion Date: 23-Feb-2005
• Ref Project: SIST-TS CEN/TS 13130-15:2005 - Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 15: Determination of 1,3-butadiene in food simulants

Standards Content (Sample)

SLOVENSKI STANDARD
SIST-TS CEN/TS 13130-15:2005
01-april-2005
0DWHULDOLLQSUHGPHWLYVWLNX]åLYLOL6QRYLYSROLPHUQLKPDWHULDOLKNDWHULK
NRQFHQWUDFLMDMHRPHMHQDGHO'RORþHYDQMHEXWDGLHQDYPRGHOQLK
UD]WRSLQDK]DåLYLOD

Materials and articles in contact with foodstuffs - Plastics substances subject to limitation

- Part 15: Determination of 1,3-butadiene in food simulants

Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen,

die Beschränkungen unterliegen - Teil 15: Bestimmung von 1,3-Butadien in
Prüflebensmitteln

Matériaux et objets en contact avec les denrées alimentaires - Substances dans les

matieres plastiques soumises a des limitations - Partie 15: Détermination du 1,3-

butadiene dans les simulants d'aliments
Ta slovenski standard je istoveten z: CEN/TS 13130-15:2005
ICS:
67.250 Materiali in predmeti v stiku z Materials and articles in
živili contact with foodstuffs
SIST-TS CEN/TS 13130-15:2005 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST-TS CEN/TS 13130-15:2005
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SIST-TS CEN/TS 13130-15:2005
TECHNICAL SPECIFICATION
CEN/TS 13130-15
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
February 2005
ICS 67.250
English version
Materials and articles in contact with foodstuffs - Plastics
substances subject to limitation - Part 15: Determination of 1,3-
butadiene 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 15: Détermination du unterliegen - Teil 15: Bestimmung von 1,3-Butadien in

1,3-butadiène 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 13130-15:2005: E

worldwide for CEN national Members.
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Contents
page

Foreword............................................................................................................................................................. 3

Introduction ........................................................................................................................................................ 5

1 Scope...................................................................................................................................................... 6

2 Normative references ........................................................................................................................... 6

3 Principle ................................................................................................................................................. 6

4 Reagents ................................................................................................................................................ 7

5 Apparatus .............................................................................................................................................. 9

6 Samples ............................................................................................................................................... 10

7 Procedure ............................................................................................................................................ 11

8 Expression of results.......................................................................................................................... 12

9 Confirmation........................................................................................................................................ 13

10 Test report ........................................................................................................................................... 14

Bibliography ..................................................................................................................................................... 15

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Foreword

This document (CEN/TS 13130-15:2005) 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
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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.
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Introduction

1,3-butadiene, C H or CH =CH-CH=CH , PM/Ref. No 13630, is a monomer used in the manufacture

4 6 2 2

of certain plastics materials and articles intended to come into contact with foodstuffs. After

manufacture, residual butadiene 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 when carrying out a migration test: From

migration experiments carried out at 10 d for 40 °C it was recognized that a considerable non-reproducible loss of

up to 90 %, due to volatilization of 1,3-butadiene can be obtained when using aqueous food simulants.

The method has been pre-validated by a collaborative trial with three laboratories.

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1 Scope

This document, part of EN 13130, specifies an analytical procedure for the determination of butadiene

monomer in the food simulants water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and

olive oil. The level of butadiene monomer determined is expressed as mg butadiene/kg of food. The

method is appropriate for the quantitative determination of butadiene at a range of 0,01 mg/kg to 0,1

mg/kg in food simulants.

NOTE The method should also be applicable to other aqueous food simulants and to the other fatty food

simulants such as 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 butadiene in a food or a food simulant is determined by headspace gas chromatography

(HSGC) with automated sample injection and using flame ionization detection (FID). Quantification is

achieved using an internal standard (n-pentane) with calibration against relevant food simulants

samples fortified with known amounts of butadiene. Confirmation of butadiene levels is carried out by

combined gas chromatography/mass spectrometry (GC/MS).
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4 Reagents

NOTE All reagents should be of recognized analytical quality unless otherwise stated.

4.1 Analytes
4.1.1 1,3-butadiene, CH =CH-CH=CH , purity greater than 99,5 % (GC).
2 2
4.1.2 n-pentane, CH -(CH ) –CH , purity greater than 99,5 % (GC).
3 2 3 3
4.2 Chemicals

4.2.1 N,N-dimethylacetamide (DMAA), CH -CO-N(CH ) , purity greater than 99,5 % (GC); density

3 3 2
d = 0,960 0 - (0,000 94 × T), where T is temperature in °C.
4.2.2 Purified nitrogen (purity 99,999 9 %).
4.3 Solutions

4.3.1 Stock solutions of butadiene in DMAA with defined concentrations of approximately

5mg/g

Weigh a 50 ml sample vial (5.4), including septum and cap, to an accuracy of 1,0 mg. Pipette 50 ml

DMAA (4.2.1) into the vial (5.4), close and weigh again to 1,0 mg. Insert hollow needles equipped with

miniature two-way valves for introducing butadiene and for venting air and weigh again to an accuracy

of 1,0 mg. Introduce, under a fume hood, approximately 0,25 g butadiene (4.1.1) by bubbling through

the DMAA with the valves in the open position. Re-weigh the vial plus needles to an accuracy of

1,0 mg with the valves in the closed position and then remove the needles.

NOTE 1 For safety reasons, the use of hollow needles with miniature two-way valves is recommended but not

necessary. Alternatively, two separate needles can be used.
Calculate the concentration of butadiene in milligrams per gram of solution.
Repeat the procedure to provide a second stock solution.

NOTE 2 The stock solutions can be stored at – 20 °C up to 3 months protected from light in septum-capped

glass vials with minimum headspace; storage at + 4 °C with the exclusion of light should not exceed one week.

4.3.2 Diluted stock solutions of butadiene in DMAA with a defined concentration of

approximately 50 µg butadiene per gram DMAA

Weigh a 20 ml sample vial (5.4), including septum and cap, to an accuracy of 1,0 mg. Pipette 18,0 ml

of DMAA into the sample vial (5.4) and close the vial with the septum and cap. Weigh again to an

accuracy of 1,0 mg. Insert 2,0 ml of the stock solution (4.3.1) through the septum using a syringe (5.5),

mix thoroughly and re-weigh to an accuracy of 1,0 mg. Repeat this procedure taking the 1:10 diluted

stock solution instead of the stock solution (4.3.1) to obtain then the required 50 µg per gram diluted

stock solution.

Calculate the concentration of butadiene in the diluted stock solution in micrograms per gram of

solution.
Repeat the procedure to provide a second diluted stock solution.
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4.3.3 Standard solutions with defined concentrations in the range 1 µg/ml to 10 µg/ml (see

NOTE in 6.3)

Weigh a series of five sample vials (volume 20 ml (5.4)), including septum and cap, to an accuracy of

1,0 mg. Pipette 19,6 ml, 19,2 ml, 18,4 ml, 17,6 ml and 16,0 ml DMAA into the vials, close and weigh

again to 1,0 mg. Add 0,4 ml, 0,8 ml, 1,6 ml, 2,4 ml and 4 ml of the diluted stock solution (4.3.2)

through the septum using a syringe, mix thoroughly and re-weigh to an accuracy of 1,0 mg.

Calculate the concentrations of butadiene in the standard solutions in micrograms per millilitre of

solution and in micrograms per 20 µl solution, using the density according to 4.2.1.

Repeat the procedure using the second diluted stock solution prepared in 4.3.2 to provide a second

set of standard solutions.

NOTE The standard solutions can be stored at – 20 °C for up to 3 months protected from light in septum

capped glass vials with minimum headspace; storage at + 4 °C with the exclusion of light should not exceed one

week.

4.3.4 Internal standard stock solution of n-pentane in DMAA with a defined concentration of

approximately 5 mg/g

Weigh a 50 ml sample vial (5.4) including the septum and cap to an accuracy of 1,0 mg. Pipette 50 ml

DMAA (4.2.1) into the vial (5.4), close and weigh again to 1,0 mg. Insert 0,4 ml n-pentane (4.1.2)

through the septum using a syringe, mix and re-weigh to an accuracy of 1,0 mg.

Calculate the concentration of pentane in the internal standard stock solution in milligrams per gram of

solution.

4.3.5 Diluted internal standard stock solution of n-pentane in DMAA with a defined

concentration of app
...