1、DRAFT FOR DEVELOPMENTDD CEN/TS 13130-21:2005Materials and articles in contact with foodstuffs Plastics substances subject to limitation Part 21: Determination of ethylenediamine and hexamethylenediamine in food simulantsICS 67.250g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g4
2、0g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58DD CEN/TS 13130-21:2005This Draft for Development was published under the authority of the Standards Policy and Strategy Committee on 16 September 2005 BSI 16 September 2
3、005ISBN 0 580 46063 0National forewordThis Draft for Development is the official English language version of CEN/TS 13130-21:2005.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
4、 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 practical application may be obtained.Comments arising from the use of th
5、is 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 publication by the European organization so that a decision can be taken o
6、n 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, the responsible BSI Committee will decide whether to support the
7、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 British Standards House, 389 Chiswick High Road, London W4 4AL, giving the document re
8、ference 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 international or European publications referred to i
9、n 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 to include all the necessary provisions of a
10、 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 17 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 13130-21February 2005ICS 67.250English versionMaterials and articles in contact with foodstuffs - Plasticssubstances subject to limitation - Part 21: Determination ofethylenediam
12、ine and hexamethylenediamine in food simulantsMatriaux et objets en contact avec les denresalimentaires - Substances dans les matires plastiquessoumises des limitations - Partie 21 : Dtermination delthylnediamine et de lhexamthylnediamine dans lessimulants dalimentsWerkstoffe und Gegenstnde in Konta
13、kt mit Lebensmitteln- Substanzen in Kunststoffen, die Beschrnkungenunterliegen - Teil 21: Bestimmung von Ethylendiamin undHexamethylendiamin in PrflebensmittelnThis Technical Specification (CEN/TS) was approved by CEN on 16 December 2004 for provisional application.The period of validity of this CEN
14、/TS is limited 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
15、 EN and 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
16、standards 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 CO
17、MMITTEE 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 13130-21:2005: E2 Contents page Fo
18、reword .3 Introduction.5 1 Scope6 2 Normative references6 3 Principle .7 4 Reagents 7 5 Apparatus.9 6 Samples10 7 Procedure.11 8 Precision 14 9 Confirmation 15 10 Test report15 Bibliography17 DD CEN/TS 13130-21:20053 Foreword This document (CEN/TS 13130-21:2005) has been prepared by Technical Commit
19、tee 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 re
22、quirements 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. Furthe
23、r 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 simul
24、ants 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 condi
25、tions 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 o
26、f 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:
27、Determination 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 13130-21:20054 Part 14: Determination of 3,3-bis(3-methyl-4-hydroxypheny
28、l)-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-dih
29、ydroxybenzene, 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: Det
30、ermination 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: Determin
31、ation 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 chemical
32、s 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, sp
33、ecific 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 th
34、is 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 Kingd
35、om. DD CEN/TS 13130-21:20055 Introduction Ethylenediamine (EDA), 1,2-Diaminoethane, C2H8N2or H2N-(CH2)2-NH2, PM/Ref. No 16960, and hexamethylenediamine (HMDA), 1,6-Diaminohexane, C6H16N2or H2N-(CH2)6-NH2, PM/Ref. No 18460 are monomers used in the manufacture of certain plastics materials and article
36、s intended to come into contact with foodstuffs. After manufacture, residual EDA monomer and HMDA monomer can remain in the polymer and may migrate into foodstuffs coming into contact with that plastics article. NOTE Stability tests in olive oil food simulant carried out under test conditions 10 d a
37、t 20 C and 10 d at 40 C indicated that EDA and HMDA cannot be recovered, presumably due to chemical reaction with the olive oil. Therefore, even though this analytical method works in principle with olive oil as a food simulant, the migration test using olive oil or another fat simulant can provide
38、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 is recommended. Alternatively 95 % ethanol or iso-octane could be
39、used as substitute fatty food simulants. The method has been pre-validated by a collaborative trial with two laboratories. DD CEN/TS 13130-21:20056 1 Scope This document, part of EN 13130, specifies an analytical procedure for the determination of EDA monomer and HMDA monomer in the food simulants w
40、ater, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and olive oil as well as in the substitute food simulants 95 % v/v ethanol and iso-octane. The level of EDA monomer and HMDA monomer determined are expressed as milligram EDA per kilogram of food simulant and as milligrams HMDA per kilogram
41、 of food simulant. The method is appropriate for the quantitative determination of EDA at a minimum level of 1 mg per kilogram of food simulants and for the quantitative determination of HMDA at a minimum level of 0,5 mg per kilogram of food simulants. The method should also be applicable to other a
42、queous food simulants as well as to the other fatty food simulants 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. For undat
43、ed 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 plastics to foods
44、and food simulants and the determination of substances in plastics and the selection of conditions of exposure to food simulants. DD CEN/TS 13130-21:20057 3 Principle The level of EDA or HMDA in a food simulant is determined by derivatization of the free diamine, using ethyl chloroformate as derivat
45、ization agent followed by analysis of the resulting diurethane by gas chromatography using automated sample injection and flame ionization detection (FID). Quantification is achieved using propylenediamine (PDA) as an internal standard with calibration against relevant food simulants samples fortifi
46、ed with known amounts of EDA or HMDA. Confirmation of EDA or HMDA levels is carried out by combined gas chromatography/mass spectrometry (GC/MS) of the diurethane. 4 Reagents NOTE All reagents should be of recognized analytical quality unless otherwise stated. 4.1 Analytes 4.1.1 EDA (1,2-diaminoetha
47、ne), H2N-(CH2)2-NH2, purity greater than 99 %. 4.1.2 HMDA (1,6-diaminohexane), H2N-(CH2)6-NH2, purity greater than 97 %. 4.1.3 PDA (1,3-diaminopropane), H2N-(CH2)3-NH2, purity greater than 99 %. 4.2 Chemicals 4.2.1 Ethyl chloroformate, Cl-C(O)-OC2H5, purity greater than 97 %. 4.2.2 Toluene 4.2.3 Die
48、thyl ether 4.2.4 Distilled water 4.2.5 25 % (w/w) aqueous solution of ammonia, NH3(d20= 0,91kg/l). 4.2.6 Sodium sulfate, anhydrous.4.2.7 Sodium hydroxide, NaOH, pellets 99 %. 4.2.8 Acetic acid, glacial 100 %. 4.2.9 Purified nitrogen, 99,999 %. 4.3 Solutions 4.3.1 Solution of NH3in distilled water ap
49、prox. 3 % (w/w) Place 200 ml of distilled water (4.2.4) into a 250 ml Erlenmeyer flask, add 30 ml of 25 % aqueous NH3solution (4.2.5) and mix thoroughly. DD CEN/TS 13130-21:20058 4.3.2 5 M solution of NaOH in distilled water Weigh 50,0 g NaOH (4.2.7) with an accuracy of 0,1 g into a 250 ml volumetric flask and fill up to the mark with distilled water (4.2.4) at room temperature. 4.3.3 3 % (w/v) acetic acid in distilled water Weigh 15,0 g of acetic acid (4.2.8) with an accuracy of 0,1g into a 500 ml volumetric flask and make up to the mark with d
