1、DRAFT FOR DEVELOPMENTDD CEN/TS 13130-26:2005Materials and articles in contact with foodstuffs Plastics substances subject to limitation Part 26: Determination of 1-octene and tetrahydrofuran in food simulantsICS 67.250g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g5
2、4g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58DD CEN/TS 13130-26:2005This Draft for Development was published under the authority of the Standards Policy and Strategy Committee on 16 September 2005 BSI 16 September 2005ISBN 0 58
3、0 46068 1National forewordThis Draft for Development is the official English language version of CEN/TS 13130-26:2005.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
4、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 practical application may be obtained.Comments arising from the use of this Draft for
5、 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 publication by the European organization so that a decision can be taken on its status
6、 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, the responsible BSI Committee will decide whether to support the conversion i
7、nto 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 British Standards House, 389 Chiswick High Road, London W4 4AL, giving the document reference and
8、 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 international or European publications referred to in this docu
9、ment 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 to include all the necessary provisions of a contract.
10、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 25 and a back cover.The BSI copyright notice displayed in this document indicates when the document was last issued.Amendments issued sinc
11、e publicationAmd. No. Date CommentsTECHNICAL SPECIFICATIONSPCIFICATION TECHNIQUETECHNISCHE SPEZIFIKATIONCEN/TS 13130-26February 2005ICS 67.250English versionMaterials and articles in contact with foodstuffs - Plasticssubstances subject to limitation - Part 26: Determination of 1-octene and tetrahydr
12、ofuran in food simulantsMatriaux et objets en contact avec les denresalimentaires - Substances dans les matires plastiquessoumises des limitations - Partie 26 : Dtermination du 1-octne et du ttrahydrofurane dans les simulants dalimentsWerkstoffe und Gegenstnde in Kontakt mit Lebensmitteln- Substanze
13、n in Kunststoffen, die Beschrnkungenunterliegen - Teil 26: Bestimmung von 1-Octen undTetrahydrofuran in 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 limited initially to three years.
14、 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 to make the CEN/TS availableprom
15、ptly 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, Cy
16、prus, 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 STANDARDIZATIONCOMIT EUROPEN
17、 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 13130-26:2005: E2 Contents page Foreword. 3 Introduction 5 1 Scope 6 2 Nor
18、mative references . 6 3 Method A Determination of 1-octene in food simulants 6 4 Method B Determination of tetrahydrofuran in food simulants 15 Bibliography . 25 DD CEN/TS 13130-26:20053 Foreword This document (CEN/TS 13130-26:2005) has been prepared by Technical Committee CEN/TC 194 “Utensils in co
19、ntact 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
20、 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 publicatio
21、n 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
22、 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
23、 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
24、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 simu
25、lants 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 plast
26、ics 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-aminoundec
27、anoic acid in food simulants Part 12: Determination of 1,3-benzenedimethanamine in food simulants DD CEN/TS 13130-26:20054 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 simulant
28、s 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-dihydroxybe
29、nzophenone 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 a
30、nd 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 tetrahyd
31、rofuran 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
32、 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
33、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
34、: 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. DD CEN/TS 13130-26:20055 I
35、ntroduction 1-octene, C8H16or CH2=CH-(CH2)5CH3, PM/Ref. No 22660, and tetrahydrofuran (THF), C4H8O, PM/Ref. No 25150, are monomers used in the manufacture of certain plastics materials and articles intended to come into contact with foodstuffs. After manufacture, residual monomer can remain in the p
36、olymer and may migrate into foodstuffs coming into contact with that plastics article. NOTE However, the following should be taken into account at carrying out a migration test for 1-octene. From migration experiments carried out for 10 d for 40 C it was recognized that irreproducible loss of 1-octe
37、ne, 11 % to 69 %, due to volatilization, can arise when using aqueous food simulants. Method A describes the determination of 1-octene in food simulants. Method B describes the determination of tetrahydrofuran in food simulants. The methods have been pre-validated by collaborative trials with two la
38、boratories. DD CEN/TS 13130-26:20056 1 Scope This document, part of EN 13130, specifies analytical procedures for the determination of 1-octene and THF in food simulants water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and olive oil. The level of 1-octene and THF monomer determined is ex
39、pressed as milligrams of monomer per kilogram of food simulant. The methods are appropriate for the quantitative determination of 1-octene in the range of 2 mg/kg to 30 mg/kg in food simulants and of THF in the range of 0,06 mg/kg to 1,5 mg/kg in food simulants. NOTE The method should also be applic
40、able to other aqueous food simulants as well as to the other fatty food simulants e.g. sunflower oil, corn oil or 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 edi
41、tion 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 subst
42、ances 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 Method A Determination of 1-octene in food simulants 3.1 Principle The level of 1-octene in a food or a food simulant is determined by head
43、space gas chromatography (HSGC) of the food simulant sample, sealed in headspace glass vials. Headspace gas chromatography is carried out applying automatic injection and flame ionization detection. Quantification is achieved using iso-octane as internal standard with calibration against food simula
44、nt samples fortified with known amounts of 1-octene. Confirmation of 1-octene levels is carried out by combined gas chromatography/mass spectrometry (GC/MS). 3.2 Reagents NOTE All reagents should be of recognized analytical quality unless otherwise stated. 3.2.1 Analytes 3.2.1.1 1-octene, CH2=CH-(CH
45、2)5CH3, purity greater than 97,5 % (GC). 3.2.1.2 Iso-octane, (CH3)2-CH-CH2-C(CH3)3, purity greater than 99 % (GC). 3.2.2 Chemical N,N-dimethylacetamide (DMAA), CH3-CO-N(CH3)2, purity greater than 99 %. DD CEN/TS 13130-26:20057 3.2.3 Solutions 3.2.3.1 Stock solutions of 1-octene with a defined concen
46、tration of approximately 2 mg/ml in DMAA Weigh a 50 ml volumetric flask, including cap, filled with about 45 ml of DMAA (3.2.2), to an accuracy of 0,1 mg. Add approximately 100 mg of 1-octene (about 150 l), then reweigh to an accuracy of 0,1 mg. Make up to 50 ml with DMAA. Close and shake. Calculate
47、 the exact concentration of the stock solution in milligrams of 1-octene per millilitre of solution. Repeat the procedure to provide a second stock solution. NOTE These stock solutions can be stored at + 4 C, with the exclusion of light, for up to 3 months. 3.2.3.2 Standard solutions of 1-octene in
48、DMAA with a defined concentration of approximately 200 g/ml Place 1,0 ml of the 1-octene stock solution (3.2.3.1) in a 10 ml volumetric flask and make up to the mark with DMAA (3.2.2). Close and mix thoroughly. Calculate the exact concentration of the standard solution in milligrams of 1-octene per
49、millilitre of solution. Repeat the procedure using the second stock solution prepared in 3.2.3.1 to provide a second standard solution. NOTE These standard solutions can be stored at + 4 C and with the exclusion of light for up to 3 months. 3.2.3.3 Stock solution of internal standard iso-octane in DMAA at a defined concentration of approximately 2 mg/ml Weigh a 50 ml volumetric flask, including cap, filled with about 45 ml of DMAA (3.2.2), to an accuracy of 0,1 mg. Add approximately 100 mg of iso-octane (about 150 l), then reweigh to an ac
