1、DRAFT FOR DEVELOPMENTDD CEN/TS 13130-12:2005Material and articles in contact with foodstuffs Plastics substances subject to limitation Part 12: Determination of 1,3-benzenedimethanamine in food simulantsICS 67.250g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g
2、44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58DD CEN/TS 13130-12:2005This Draft for Development was published under the authority of the Standards Policy and Strategy Committee on 16 September 2005 BSI 16 September 2005ISBN 0 580 460
3、55 XNational forewordThis Draft for Development is the official English language version of CEN/TS 13130-12:2005.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 n
4、ot 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 Deve
5、lopment 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 t
6、he 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 into a
7、 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 clau
8、se 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 document
9、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. Users
10、 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 notice displayed in this document indicates when the document was last issued.Amendments issued since pub
11、licationAmd. No. Date CommentsTECHNICAL SPECIFICATIONSPCIFICATION TECHNIQUETECHNISCHE SPEZIFIKATIONCEN/TS 13130-12February 2005ICS 67.250English versionMaterial and articles in contact with foodstuffs - Plasticssubstances subject to limitation - Part 12: Determination of 1,3-benzenedimethanamine in
12、food simulantsMatriaux et objets en contact avec les denresalimentaires - Substances dans les matires plastiquessoumises des limitations - Partie 12 : Dtermination du1,3-benznedimthanamine dans les simulants dalimentsWerkstoffe und Gegenstnde in Kontakt mit Lebensmitteln- Substanzen in Kunststoffen,
13、 die Beschrnkungenunterliegen - Teil 12: Bestimmung von 1,3-Benzendimethanamin 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. After two years the m
14、embers 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 level
15、 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 NORMALISATIONEUROP
17、ISCHES 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 13130-12:2005: EDD CEN/TS 13130-12:20052ContentspageForeword. 3Introduction 51 Scope 62 Normativ
18、e references . 63 Principle . 64 Reagents 65 Apparatus 96 Samples . 97 Procedure 108 Expression of results 129 Confirmation 1310 Test report . 14Bibliography . 15DD CEN/TS 13130-12:20053Foreword This document (CEN/TS 13130-12:2005) has been prepared by Technical Committee CEN/TC 194 “Utensils in con
19、tact 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 publication
21、 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 sp
24、ecific 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 simula
25、ntsPart 2: Determination of terephthalic acid in food simulants Part 3: Determination of acrylonitrile in food and food simulantsPart 4: Determination of 1,3-butadiene in plasticsPart 5: Determination of vinylidene chloride in food simulantsPart 6: Determination of vinylidene chloride in plasticsPar
26、t 7: Determination of monoethylene glycol and diethylene glycol in food simulantsPart 8: Determination of isocyanates in plastics Part 9: Determination of acetic acid, vinyl ester in food simulantsPart 10: Determination of acrylamide in food simulantsPart 11: Determination of 11-aminoundecanoic acid
27、 in food simulantsPart 12: Determination of 1,3-benzenedimethanamine in food simulants4Part 13: Determination of 2,2-bis(4-hydroxyphenyl)propane (Bisphenol A) in food simulantsPart 14: Determination of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indoline in food simulantsPart 15: Determination of 1,3-butadi
28、ene in food simulantsPart 16: Determination of caprolactam and caprolactam salt in food simulantsPart 17: Determination of carbonyl chloride in plasticsPart 18: Determination of 1,2-dihydroxybenzene, 1,3-dihydroxybenzene, 1,4-dihydroxybenzene, 4,4-dihydroxybenzophenone and 4,4dihydroxybiphenyl in fo
29、od simulantsPart 19: Determination of dimethylaminoethanol in food simulantsPart 20: Determination of epichlorohydrin in plasticsPart 21: Determination of ethylenediamine and hexamethylenediamine in food simulantsPart 22: Determination of ethylene oxide and propylene oxide in plasticsPart 23: Determ
30、ination of formaldehyde and hexamethylenetetramine in food simulantsPart 24: Determination of maleic acid and maleic anhydride in food simulantsPart 25: Determination of 4-methyl-pentene in food simulantsPart 26: Determination of 1-octene and tetrahydrofuran in food simulantsPart 27: Determination o
31、f 2,4,6-triamino-1,3,5-triazine in food simulantsPart 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 o
32、f 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 en
33、sure 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
34、, 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 13130-12:20055Introduction 1,3-benzenedimethanamine (also known as 3
35、-(aminomethyl)-benzylamine or m-xylylene diamine (m-XDA), C8H12N2, PM/Ref-No. 13000, hereinafter referred to as m-XDA, is a monomer used in the manufacture of certain plastics materials and articles intended to come into contact with foodstuffs. After manufacture, residual m-XDA monomer can remain i
36、n the polymer and may migrate into foodstuffs coming into contact with the plastics material or article. NOTE However the following should be taken into account when carrying out a migration test: Stability tests in spiked olive oil food simulant carried out under test conditions 10 d at 40 C indica
37、ted that m-XDA is not stable in the fat simulant, presumably due to chemical reaction with the olive oil and/or oxygen. Typically a recovery of only 25 % was obtained under these test conditions. Therefore, even though this analytical method works in principle with olive oil as a food simulant, the
38、migration test using olive oil or another fat simulant can provide false-negative results. Therefore, the method should only be applied in case of short exposure periods with olive oil and if applied, a recovery check with spiked olive oil applying the same time/temperature migration test conditions
39、 is recommended, see also the NOTE in Clause 1. The method has been tested by a second laboratory. DD CEN/TS 13130-12:200561 Scope This document, part of EN 13130, specifies a procedure for the determination of 1,3-benzenedimethanamine (also known as 3-(aminomethyl)-benzylamine or m-xylylene diamine
40、 (m-XDA) monomer, hereinafter referred to as m-XDA, in the food simulants water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and olive oil. The level of m-XDA monomer determined is expressed as milligrams of m-XDA per kilogram of food simulant in the above mentioned food simulants. NOTE In
41、 addition to the instability of m-XDA observed in olive oil, the test laboratory could not detect any m-XDA peak from the olive oil work-up procedure. Based on some control checks, the assumption of the test laboratory was that the extraction from the olive oil does not work. Therefore, it is recomm
42、ended that the food simulant 95 % ethanol or iso-octane be applied as substitute fatty simulants instead of olive oil. It is believed that 95 % ethanol and iso-octane can be treated in the same way as 15 % v/v aqueous ethanol and olive oil simulant, respectively. Corresponding investigations were no
43、t possible within the project. 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) appl
44、ies. 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 cond
45、itions of exposure to food simulants. 3 Principle m-XDA in aqueous simulant test samples is determined, following bis-derivatization with fluorescamine, by high performance liquid chromatography (HPLC) with fluorescence detection. m-XDA in olive oil test samples is extracted with 3 % w/v aqueous ace
46、tic acid and determined in the same way. Quantification is relative to external standards. The identity of m-XDA is confirmed by mono-derivatization with less fluorescamine leading to a second peak in the HPLC chromatograms obtained from samples, and by comparison with authentic samples. 4 Reagents
47、NOTE All reagents should be of recognized analytical quality unless otherwise stated. 4.1 Analyte 1,3-benzenedimethanamine (also known as 3-(aminomethyl)-benzylamine or m-xylylene diamine (m-XDA), C8H12N2, purity 99 %. DD CEN/TS 13130-12:200574.2 Other chemicals 4.2.1 Distilled water (HPLC grade), s
48、aturated with nitrogen (4.2.10). 4.2.2 Methanol (HPLC grade). 4.2.3 Tetrahydrofuran (HPLC grade). 4.2.4 Acetone 4.2.5 Heptane 4.2.6 Fluorescamine, C17H10O4, purity 98 %. 4.2.7 Disodium tetraborate 10-hydrate, Na2B2O7.10H2O. 4.2.8 Sodium hydroxide 4.2.9 Acetic acid glacial 100 % 4.2.10 Purified nitro
49、gen, 99,9999 %. 4.3 Solutions 4.3.1 3 % w/v acetic acid in distilled water Weigh 15,0 g of acetic acid (4.2.9) with an accuracy of 0,1 g into a 500 ml volumetric flask and make up to the mark with distilled water (4.2.1). 4.3.2 90 % (v/v)Tetrahydrofuran Pour 90 ml of tetrahydrofuran (4.2.3) into a 100 ml volumetric flask and make up to the mark with water (4.2.1). 4.3.3 Fluorescamine solution, 2 mg/ml Weigh 10 mg of fluorescamine (4.2.6) into a 5 ml volumetric flask and make up to the mark with acetone (4.2.4). NOTE The solution can be stored for up
