1、DRAFT FOR DEVELOPMENTDD CEN/TS 13130-9:2005Materials and articles in contact with footstuffs Plastics substances subject to limitation Part 9: Determination of acetic acid, vinyl ester in food simulantsICS 67.250g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g4
2、4g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58DD CEN/TS 13130-9:2005This Draft for Development, having been prepared under the direction of the Consumer Products and Services Sector Committee, was published under the authority of the
3、Standards Policy and Strategy Committee on 31 October 2005 BSI 31 October 2005ISBN 0 580 46074 6National forewordThis Draft for Development is the English language version of CEN/TS 13130-9:2005.This publication is not to be regarded as a British Standard. It is being issued in the Draft for Develop
4、ment series of publications and is of a provisional nature because the method was not evaluated using recognized ring trial procedures. As a consequence there are no reproducibility data for the method. It should be applied on this provisional basis, so that information and experience of its practic
5、al application may be obtained. Comments arising from the use of this Draft for Development are requested so that UK experience can be reported to the European organization responsible for its conversion to a European standard. A review of this publication will be initiated 2 years after its publica
6、tion by the European organization so that a decision can be taken on its status at the end of its 3-year life. Notification of the start of the review period will be made in an announcement in the appropriate issue of Update Standards.According to the replies received by the end of the review period
7、, the responsible BSI Committee will decide whether to support the conversion into a European Standard, to extend the life of the Technical Specification or to withdraw it. Comments should be sent in writing to the Secretary of BSI Subcommittee CW/47/1, Migration from plastics, at 389 Chiswick High
8、Road, London W4 4AL, giving the document reference and clause number and proposing, where possible, an appropriate revision of the text.A list of organizations represented on this subcommittee can be obtained on request to its secretary. Cross-referencesThe British Standards which implement internat
9、ional or European publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online.This publication does not purport
10、to include all the necessary provisions of a contract. Users are responsible for its correct application.Summary of pagesThis document comprises a front cover, an inside front cover, the CEN/TS title page, pages 2 to 15 and a back cover.The BSI copyright date displayed in this document indicates whe
11、n the document was last issued.Amendments issued since publicationAmd. No. Date CommentsTECHNICAL SPECIFICATIONSPCIFICATION TECHNIQUETECHNISCHE SPEZIFIKATIONCEN/TS 13130-9February 2005ICS 67.250English versionMaterials and articles in contact with foodstuffs - Plasticssubstances subject to limitatio
12、n - Part 9: Determination of aceticacid, vinyl ester in food simulantsMatriaux et objets en contact avec des denresalimentaires - Substances dans les matires plastiquessoumises des limitations - Partie 9 : Dtermination duvinyl ester dacide actique dans les simulants dalimentsWerkstoffe und Gegenstnd
13、e in Kontakt mit Lebensmitteln- Substanzen in Kunststoffen, die Beschrnkungenunterliegen - Teil 9: Bestimmung von Essigsurevinylesterin PrflebensmittelnThis Technical Specification (CEN/TS) was approved by CEN on 16 December 2004 for provisional application.The period of validity of this CEN/TS is l
14、imited initially to three years. After two years the members of CEN will be requested to submit theircomments, 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
15、to make the CEN/TS availablepromptly 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 standard
16、s 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
17、FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2005 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. CEN/TS 13130-9:2005: E2 Contents page Foreword .3
18、 Introduction.5 1 Scope6 2 Normative references6 3 Principle .6 4 Reagents 6 5 Apparatus.7 6 Samples9 7 Procedure.11 8 Expression of results12 9 Confirmation 13 10 Test report14 Bibliography15 DD CEN/TS 13130-9:20053 Foreword This document (CEN/TS 13130-9:2005) has been prepared by Technical Committ
19、ee 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
20、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
21、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 req
22、uirements 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
23、 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 simula
24、nts 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 condit
25、ions 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
26、 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: D
27、etermination 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 DD CEN/TS 13130-9:20054 Part 14: Determination of 3,3-bis(3-methyl-4-hydroxyphenyl)
28、-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-dihyd
29、roxybenzene, 4,4-dihydroxybenzophenone and 4,4dihydroxybiphenyl 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: Deter
30、mination 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: Determinat
31、ion 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
32、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, spec
33、ific 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
34、 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
35、. DD CEN/TS 13130-9:20055 Introduction Acetic acid, vinyl ester (vinyl acetate) CH3CO2CH=CH2, PM/Ref. No 10120, is a monomer used in the manufacture of certain materials and articles intended to come into contact with foodstuffs. After manufacture, residual vinyl acetate can remain in the polymer an
36、d 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 4
37、0 C. Vinyl acetate is stable in olive oil. The method has been validated by a collaborative trial with three laboratories. DD CEN/TS 13130-9:20056 1 Scope This document, part of EN 13130, specifies an analytical procedure for the determination of vinyl acetate in the four conventional EU food simula
38、nts, 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 det
39、ermination 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 T
40、he 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 ind
41、ispensable 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 subj
42、ect 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 i
43、s 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
44、. 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 us
45、ed 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. DD CEN/TS 13130-9:20057 4.1 Analytes 4.1.1 Vinyl acetate, CH3CO2C
46、H=CH2, purity greater than 99 %. 4.1.2 Methyl propionate, CH3CH2CO2CH3, purity greater than 99 %, which is free of interfering substances 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 sol
47、ution 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 acetat
48、e 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 propioni
49、c 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 contain
