1、DRAFT FOR DEVELOPMENTDD CEN/TS 13130-25:2005Materials and articles in contact with foodstuffs Plastics substances subject to limitation Part 25: Determination of 4-methyl-1-pentene in food simulantsICS 67.250g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50
2、g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58DD CEN/TS 13130-25:2005This Draft for Development was published under the authority of the Standards Policy and Strategy Committee on 16 September 2005 BSI 16 September 2005ISBN 0 580 46067 3N
3、ational forewordThis Draft for Development is the official English language version of CEN/TS 13130-25:2005.This publication is not to be regarded as a British Standard.It is being issued in the Draft for Development series of publications and is of a provisional nature because the method was not ev
4、aluated 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 practical application may be obtained.Comments arising from the use of this Draft for Developme
5、nt 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 publication by the European organization so that a decision can be taken on its status at the en
6、d 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, the responsible BSI Committee will decide whether to support the conversion into a Euro
7、pean 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 British Standards House, 389 Chiswick High Road, London W4 4AL, giving the document reference and clause nu
8、mber 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 international or European publications referred to in this document may b
9、e 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 to include all the necessary provisions of a contract. Users are
10、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 14, an inside back cover and a back cover.The BSI copyright notice displayed in this document indicates when the document was last issued.Amendments
11、 issued since publicationAmd. No. Date CommentsTECHNICAL SPECIFICATIONSPCIFICATION TECHNIQUETECHNISCHE SPEZIFIKATIONCEN/TS 13130-25February 2005ICS 67.250English versionMaterials and articles in contact with foodstuffs - Plasticssubstances subject to limitation - Part 25: Determination of 4-methyl-1
12、-pentene in food simulantsMatriaux et objets en contact avec les denresalimentaires - Substances dans les matires plastiquessoumises des limitations - Partie 25 : Dtermination du 4-mthyl-1 pentne dans les simulants dalimentsWerkstoffe und Gegenstnde in Kontakt mit Lebensmitteln- Substanzen in Kunsts
13、toffen, die Beschrnkungenunterliegen - Teil 25: Bestimmung von 4-Methyl-1-Penten inPrflebensmittelnThis 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
14、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 to make the CEN/TS availablepromptly at national leve
15、l 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,
16、 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 STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEURO
17、PISCHES 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 13130-25:2005: E2 Contents page Foreword. 3 Introduction 5 1 Scope 6 2 Normative references . 6
18、 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 DD CEN/TS 13130-25:20053 Foreword This document (CEN/TS 13130-25:2005) has been prepared by Technical Committee CEN/TC 194 “Utensils in contact
19、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“
20、 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 t
21、his 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 suppo
22、rts. 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 gener
23、al 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 specif
24、ic 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
25、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 Pa
26、rt 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
27、acid in food simulants Part 12: Determination of 1,3-benzenedimethanamine in food simulants DD CEN/TS 13130-25:20054 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
28、 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-dihydroxybenzophe
29、none 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: Determination of ethylene oxide and pro
30、pylene 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 tetrahydrofura
31、n 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 great
32、er 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 us
33、ers 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: Aust
34、ria, 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. DD CEN/TS 13130-25:20055 Introdu
35、ction 4-methyl-1-pentene, C6H12, PM/Ref. No 22150 is a monomer used in the manufacture of certain 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 int
36、o 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 volat
37、ilization when using aqueous food simulants. The method has been pre-validated by collaborative trials with two laboratories. DD CEN/TS 13130-25:20056 1 Scope This document, part of EN 13130, specifies an analytical procedure for the determination of 4-methyl-1-pentene in food simulants distilled wa
38、ter, 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 determin
39、ation 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 aque
40、ous 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
41、. 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 plastic
42、s 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 interna
43、l 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
44、 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. DD CEN/TS 13130-25:20057 4.1 Analytes 4.1.1 4-methyl-1-pentene,
45、C6H12, molecular weight: 84,16, purity 98 %. 4.1.2 Cyclohexane, C6H12, molecular weight: 84,16, purity 99,5 %. 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-penten
46、e 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 ca
47、n 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
48、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 int
49、ernal standard solution of cyclohexane in DMAA (50 g/ml) Transfer with a microsyringe 500 l 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 g/ml) Transfer into a 10 ml volumetric flasks approximately
