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1、DRAFT FOR DEVELOPMENT DD CEN/TS 13130-25:2005 Materials and articles in contact with foodstuffs Plastics substances subject to limitation Part 25: Determination of 4-methyl-1-pentene in food simulants ICS 67.250 DD CEN/TS 13130-25:2005 This Draft for Development was published under the authority of
2、the Standards Policy and Strategy Committee on 16 September 2005 BSI 16 September 2005 ISBN 0 580 46067 3 National foreword This 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
3、 the Draft for Development 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 exp
4、erience of its practical 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 y
5、ears after its publication 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 e
6、nd of the review period, 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
7、, at British Standards House, 389 Chiswick High 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-referen
8、ces The British Standards which implement international 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 S
9、tandards Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Summary of pages This document comprises a front cover, an inside front cover, the CEN/TS title page, pages 2 to 14, an inside back cover and a
10、 back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments W - - - - - - - - - 7 - - 7- - - - - 8- - - - - 7 7 8 - - - - - - - - - - - $- - - - - - - - - - - - - - - - - - - - - - - - - - - -
11、 - - - - W W D - - w - - - - 2 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 results11 9 Confirmation 12 10 Test report . 13 Bibliography . 14 DD CEN/TS 13130-25:2005 3 Foreword Thi
12、s 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 An
13、alysis 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
14、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
15、 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
16、 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 sp
17、ecific 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
18、 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: Determi
19、nation 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 sim
20、ulants 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 DD CEN/TS 13130-25:2005 4 Part 13: Determination of 2,2-bis(4-hydroxyphenyl)propane (Bisphenol A) in
21、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
22、18: Determination of 1,2-dihydroxybenzene, 1,3-dihydroxybenzene, 1,4-dihydroxybenzene, 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
23、 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 2
24、5: 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 Sta
25、ndards. 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 countr
26、ies 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 sta
27、ndards 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, P
28、ortugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. DD CEN/TS 13130-25:2005 5 Introduction 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 manufact
29、ure 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 recogn
30、ized 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. DD CEN/TS 13130-25:2005 6 1 Scope This document, part of EN 13130
31、, 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
32、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,
33、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 documen
34、ts 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 subst
35、ances 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 f
36、ood 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 eq
37、uipment 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 recogniz
38、ed analytical quality unless otherwise stated. DD CEN/TS 13130-25:2005 7 4.1 Analytes 4.1.1 4-methyl-1-pentene, 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 Sto
39、ck 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-penten
40、e 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 cycloh
41、exane 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
42、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 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
43、 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 7 ml DMAA. Add with the aid of a microsyringe 100 l of the standard stock solution of 4-methyl-1-pentene (4.3.1). The tip of the syri