SIST-TS CEN/TS 13130-9:2005

Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 9: Determination of acetic acid, vinyl ester in food simulants

This document, part of EN 13130, specifies an analytical procedure for the determination of vinyl acetate in the four conventional EU food simulants, water, 10 % (v/v) ethanol aqueous solution; 3 % (w/v) acetic acid aqueous solution and olive oil or an approved substitute. The level of vinyl acetate monomer determined is expressed as milligrams of vinyl acetate per kilogram of food simulant. The method is appropriate for the quantitative determination of vinyl acetate in approximate analyte concentration range of 1,2 mg/kg to 24 mg/kg food simulant.
NOTE 1   The method should also be applicable to other aqueous food simulants as well as to other fatty food simulants such as sunflower oil and a mixture of synthetic triglycerides.
NOTE 2   The suitability of the fat simulant should be assessed prior to setting up migration tests - it may be found necessary to use sunflower oil or a mixture of synthetic triglycerides if unacceptable interferences are found with olive oil.

Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen, die Beschränkungen unterliegen - Teil 9: Bestimmung von Essigsäurevinylester in Prüflebensmitteln

Dieses Dokument, Teil der EN 13130, legt ein Analyseverfahren zur Bestimmung von Vinylacetat in den vier
konventionellen EU-Prüflebensmitteln Wasser, 10 %iges Ethanol (Volumenanteil) in wässriger Lösung, 3 %ige
Essigsäure (m/V) in wässriger Lösung und Olivenöl oder ein zugelassenes Ersatzmittel, fest. Der ermittelte
Gehalt an monomerem Vinylacetat wird in Milligramm Vinylacetat je Kilogramm Prüflebensmittel angegeben.
Das Verfahren eignet sich zur quantitativen Bestimmung von Vinylacetat im angenäherten Konzentrations-
bereich des Analyten von 1,2 mg/kg bis 24 mg/kg Prüflebensmittel.
ANMERKUNG 1 Das Verfahren sollte auch auf andere wässrige Prüflebensmittel sowie weitere fettige Prüflebens-
mittel, wie z. B. Sonnenblumenöl und eine Mischung synthetischer Triglyceride, anwendbar sein.
ANMERKUNG 2 Die Eignung des fettigen Prüflebensmittels sollte vor Beginn der Migrationsprüfungen beurteilt
werden es kann sich als erforderlich herausstellen, Sonnenblumenöl oder eine Mischung synthetischer Triglyceride zu
verwenden, wenn bei der Verwendung von Olivenöl unannehmbare Störwirkungen auftreten.

Matériaux et objets en contact avec des denrées alimentaires - Substances dans les matieres plastiques soumises a des limitations - Partie 9 : Détermination du vinyl ester d'acide acétique dans les simulants d'aliments

Le présent document, constituant une partie de l?EN 13130, spécifie un mode opératoire d?analyse pour la
détermination de l?acétate de vinyle dans les quatre simulants d?aliments conventionnels de l'UE : eau,
solution aqueuse d?éthanol a 10 % (v/v), solution aqueuse d?acide acétique a 3 % (m/v) et huile d?olive ou
substitut approuvé. La teneur en monomere d?acétate de vinyle déterminée est exprimée en milligrammes
d?acétate de vinyle par kilogramme de simulant d?aliment. Cette méthode convient pour la détermination
quantitative de l?acétate de vinyle dans une gamme de concentrations d?analyte comprise approximativement
entre 1,2 mg/kg et 24 mg/kg de simulant d?aliment.
NOTE 1 Il convient que la méthode puisse également etre appliquée a d'autres simulants aqueux ainsi qu?a des
simulants gras tels que l?huile de tournesol ou un mélange de triglycérides synthétiques.
NOTE 2 Il convient d?évaluer l?aptitude a l?emploi du simulant gras avant de conduire les essais de migration.
L?utilisation d?huile de tournesol ou d?un mélange de triglycérides synthétiques peut s?avérer nécessaire en cas
d?identification d?interférences inacceptables avec l?huile d?olive.

Materiali in predmeti v stiku z živili - Snovi v polimernih materialih, katerih koncentracija je omejena - 9. del: Določevanje vinilacetata v modelnih raztopinah za živila

General Information

• Status: Published
• Publication Date: 31-Mar-2005
• ICS: 67.250 - Materials and articles in contact with foodstuffs
• Technical Committee: EPO - Packaging - sales and grouped
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 01-Apr-2005
• Due Date: 01-Apr-2005
• Completion Date: 01-Apr-2005
• Ref Project: CEN/TS 13130-9:2005 - Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 9: Determination of acetic acid, vinyl ester in food simulants

Standards Content (Sample)

SLOVENSKI STANDARD
SIST-TS CEN/TS 13130-9:2005
01-april-2005
0DWHULDOLLQSUHGPHWLYVWLNX]åLYLOL6QRYLYSROLPHUQLKPDWHULDOLKNDWHULK
NRQFHQWUDFLMDMHRPHMHQDGHO'RORþHYDQMHYLQLODFHWDWDYPRGHOQLKUD]WRSLQDK
]DåLYLOD
Materials and articles in contact with foodstuffs - Plastics substances subject to limitation
- Part 9: Determination of acetic acid, vinyl ester in food simulants
Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen,
die Beschränkungen unterliegen - Teil 9: Bestimmung von Essigsäurevinylester in
Prüflebensmitteln
Matériaux et objets en contact avec des denrées alimentaires - Substances dans les
matieres plastiques soumises a des limitations - Partie 9 : Détermination du vinyl ester
d'acide acétique dans les simulants d'aliments
Ta slovenski standard je istoveten z: CEN/TS 13130-9:2005
ICS:
67.250 Materiali in predmeti v stiku z Materials and articles in
živili contact with foodstuffs
SIST-TS CEN/TS 13130-9:2005 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 13130-9:2005

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SIST-TS CEN/TS 13130-9:2005
TECHNICAL SPECIFICATION
CEN/TS 13130-9
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
February 2005
ICS 67.250
English version
Materials and articles in contact with foodstuffs - Plastics
substances subject to limitation - Part 9: Determination of acetic
acid, vinyl ester in food simulants
Matériaux et objets en contact avec des denrées Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln
alimentaires - Substances dans les matières plastiques - Substanzen in Kunststoffen, die Beschränkungen
soumises à des limitations - Partie 9 : Détermination du unterliegen - Teil 9: Bestimmung von Essigsäurevinylester
vinyl ester d'acide acétique dans les simulants d'aliments 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.
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 13130-9:2005: E
worldwide for CEN national Members.

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SIST-TS CEN/TS 13130-9:2005
CEN/TS 13130-9:2005 (E)
Contents
page
Foreword .3
Introduction.5
1 Scope.6
2 Normative references.6
3 Principle .6
4 Reagents .6
5 Apparatus.7
6 Samples.9
7 Procedure.11
8 Expression of results.12
9 Confirmation .13
10 Test report.14
Bibliography.15

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SIST-TS CEN/TS 13130-9:2005
CEN/TS 13130-9:2005 (E)
Foreword
This document (CEN/TS 13130-9:2005) 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
3

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SIST-TS CEN/TS 13130-9:2005
CEN/TS 13130-9:2005 (E)
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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SIST-TS CEN/TS 13130-9:2005
CEN/TS 13130-9:2005 (E)
Introduction
Acetic acid, vinyl ester (vinyl acetate) CH CO CH=CH PM/Ref. No 10120, is a monomer used in the
3 2 2,
manufacture of certain materials and articles intended to come into contact with foodstuffs. After manufacture,
residual vinyl acetate can remain in the polymer and may migrate into foodstuffs coming into contact with the
plastic material or product.
NOTE The following should be taken into account when carrying out a migration test. Vinyl acetate is known to
hydrolyze in aqueous media. In acetic acid solutions the hydrolysis is almost complete after 10 d at 40 °C. Vinyl acetate is
stable in olive oil.
The method has been validated by a collaborative trial with three laboratories.
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SIST-TS CEN/TS 13130-9:2005
CEN/TS 13130-9:2005 (E)

1 Scope
This document, part of EN 13130, specifies an analytical procedure for the determination of vinyl acetate in
the four conventional EU food simulants, water, 10 % (v/v) ethanol aqueous solution; 3 % (w/v) acetic acid
aqueous solution and olive oil or an approved substitute. The level of vinyl acetate monomer determined is
expressed as milligrams of vinyl acetate per kilogram of food simulant. The method is appropriate for the
quantitative determination of vinyl acetate in approximate analyte concentration range of 1,2 mg/kg to 24
mg/kg food simulant.
NOTE 1 The method should also be applicable to other aqueous food simulants as well as to other fatty food simulants
such as sunflower oil and a mixture of synthetic triglycerides.
NOTE 2 The suitability of the fat simulant should be assessed prior to setting up migration tests - it may be found
necessary to use sunflower oil or a mixture of synthetic triglycerides if unacceptable interferences are found with olive oil.
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 vinyl acetate in food simulants is determined by headspace capillary gas chromatography, using
flame ionization detection. Quantification is achieved using propionic acid, methyl ester (methyl propionate),
as an internal standard with calibration against relevant food simulants samples, fortified with known amounts
of vinyl acetate.
Confirmation of vinyl acetate levels is carried out by combined headspace gas chromatography/mass
spectrometry, or by repeating the analytical procedure using a gas chromatograph capillary column of different
polarity.
If automated headspace sampling cannot be performed, manual injection may be used ensuring that the gas
syringe and needle are preheated to the same temperature as the headspace vials before the headspace is
sampled.
4 Reagents
NOTE All reagents should be of recognized analytical quality unless otherwise stated.
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CEN/TS 13130-9:2005 (E)
4.1 Analytes
4.1.1 Vinyl acetate, CH CO CH=CH , purity greater than 99 %.
3 2 2
4.1.2 Methyl propionate, CH CH CO CH , purity greater than 99 %, which is free of interfering substances
3 2 2 3
which elute at the same retention time as vinyl acetate.
4.2 Chemicals
4.2.1 Water, HPLC grade.
4.2.2 N,N-dimethylacetamide (99,9 %)
4.3 Solutions
4.3.1 Stock solution of vinyl acetate in dimethylacetamide (6 mg/ml)
Weigh accurately approximately 0,15 g of the vinyl acetate into a tared stoppered 25 ml volumetric flask
containing about 10 ml of dimethylacetamide, and dilute to the mark with dimethylacetamide. Calculate the
exact concentration of vinyl acetate in milligrams per litre.
Repeat the procedure to provide a second standard stock solution.
NOTE The stock solutions can be stored in a well closed containers in the dark for a maximum period of three
months at any temperature between 5 °C and 20 °C.
4.3.2 Internal standard stock solution of propionic acid, methyl ester (methyl propionate) in
dimethylacetamide (6 mg/ml)
Weigh approximately 0,6 g of propionic acid methyl ester (methyl propionate), into a tared stoppered 100 ml
volumetric flask containing about 20 ml of dimethylacetamide, and dilute to the mark with dimethylacetamide.
NOTE The stock solutions can be stored in well closed containers in the dark for a maximum period of three months
at any temperature between 5 °C and 20 °C.
4.3.3 Standard solutions of vinyl acetate in dimethylacetamide
Into six 25 ml volumetric flasks, each containing approximately 5 ml of dimethylacetamide, add by pipette 0 ml,
0,5 ml, 1,0 ml, 2,0 ml, 3,0 ml and 5,0 ml of the stock solution (3.3.1). Pipette in 5,0 ml of internal standard
solution (4.3.2). Dilute to the mark with dimethylacetamide to give standard solutions containing a nominal
concentration of 0 mg/l, 120 mg/l, 240 mg/l, 480 mg/l, 720 mg/l and 1200 mg/l vinyl acetate. Shake thoroughly
to mix.
Calculate the exact concentrations of the standard solutions in milligrams per litre.
Repeat the procedure using the second stock solution prepared in 4.3.1 to give a second set of standard
solutions.
NOTE The standard solutions can be stored in well closed containers in the dark for a maximum period of three
months at any temperature between 5 °C and 20 °C.
5 Apparatus
NOTE An instrument or item of apparatus is listed only where it is special or made to a particular specification, the
usual laboratory glassware and equipment being assumed to be available.
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SIST-TS CEN/TS 13130-9:2005
CEN/TS 13130-9:2005 (E)
5.1 Gas chromatograph, fitted with a capillary column capable of resolving vinyl acetate and the internal
standard from each other and other compounds present in the food simulants.
Appropriate operating conditions shall be established for the specific equipment used for the determination.
NOTE The following chromatographic column and conditions have been found to be satisfactory.
System 1
GC analytical column and temperature program for ethanol, water and olive oil food simulants.
Column:   25 m x 0,32 I.D dimethylsiloxane 5 µm film thickness
Temperature program:  50 °C held for 1 min, raised to 90 °C at 5 °C/min
    raised at 30 °C/min to 120 °C, held for 5 min.
Carrier gas:   Helium 2 ml/min.
Carrier gas split ratio  1 : 10
Run time:   20 min
Flame ionization detector  200 °C
Injector:   125 °C

System 2
GC analytical column and temperature program for 3 % w/v aqueous acetic acid food simulant.
Column:   25 m x 0,32 I.D polyethylene glycol 1 µm film thickness.
Temperature program:  54 °C held f
...