1、DRAFT FOR DEVELOPMENTDD CEN/TS 13130-16:2005Materials and articles in contact with foodstuffs Plastics substances subject to limitation Part 16: Determination of caprolactam and caprolactam salt in food simulantsICS 67.250g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g
2、44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58DD CEN/TS 13130-16:2005This Draft for Development was published under the authority of the Standards Policy and Strategy Committee on 16 September 2005 BSI 16 September 2005ISBN
3、0 580 46071 1National forewordThis Draft for Development is the official English language version of CEN/TS 13130-10:2005.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 met
4、hod 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
5、 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 on its st
6、atus 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 conversi
7、on 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 reference
8、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 in this d
9、ocument 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 contrac
10、t. 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 16, an inside back cover and a back cover.The BSI copyright notice displayed in this document indicates when the document was last issu
11、ed.Amendments issued since publicationAmd. No. Date CommentsTECHNICAL SPECIFICATIONSPCIFICATION TECHNIQUETECHNISCHE SPEZIFIKATIONCEN/TS 13130-16February 2005ICS 67.250English versionMaterials and articles in contact with foodstuffs - Plasticssubstances subject to limitation - Part 16: Determination
12、ofcaprolactam and caprolactam salt in food simulantsMatriaux et objets en contact avec les denresalimentaires - Substances dans les matires plastiquessoumises des limitations - Partie 16: Dtermination ducaprolactame et des sels de caprolactame dans lessimulants dalimentsWerkstoffe und Gegenstnde in
13、Kontakt mit Lebensmitteln- Substanzen in Kunststoffen, die Beschrnkungenunterliegen - Teil 16: Bestimmung von Caprolactam undCaprolactamsalz 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 13130-16:2005: E2 Contents page Fo
18、reword. 3 Introduction 5 1 Scope 6 2 Normative references . 6 3 Principle . 6 4 Reagents 6 5 Apparatus 8 6 Samples . 9 7 Procedure 10 8 Precision 12 9 Confirmation 13 10 Test report . 14 Bibliography . 16 DD CEN/TS 13130-16:20053 Foreword This document (CEN/TS 13130-16:2005) has been prepared by Tec
19、hnical 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 Analysis for Monomers” and has been prepared by Subcommittee
20、 (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 its amendments 93/8/EEC 4 and 97/48/EC 5, and 85/572/EEC 6
21、. 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 existing Directives are expected which could change the l
22、egislative 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 part of EN 13130 should be read in conjunction with EN 13
23、130-1. 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 specific migration from plastics materials into foodstuffs a
24、nd 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 the determination of substances in plastics and the selec
25、tion 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: Determination of vinylidene chloride in food simulants Part 6: De
26、termination 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 simulants Part 10: Determination of acrylamide in food simula
27、nts Part 11: Determination of 11-aminoundecanoic acid in food simulants Part 12: Determination of 1,3-benzenedimethanamine in food simulants DD CEN/TS 13130-16:20054 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
28、-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 18: Determination of 1,2-dihydroxybenzene, 1,3-dihydroxyben
29、zene, 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 ethylenediamine and hexamethylenediamine in food simulants
30、 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 25: Determination of 4-methyl-pentene in food simulants Part
31、 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 Standards. Parts 9 to 28 are Technical Specifications. WARNING
32、 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 countries in which this Technical Specification may be followed.
33、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 standards organizations of the following countries are bound t
34、o 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, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and
35、 United Kingdom. DD CEN/TS 13130-16:20055 Introduction Caprolactam, C6H11NO, PM/Ref. No. 14200, is a monomer used in the manufacture of certain plastics materials and articles intended to come into contact with foodstuffs. After the manufacture residual caprolactam can remain in the finished product
36、 and may migrate into foodstuffs coming into contact with that product. Caprolactam sodium salt, C6H10NO Na, PM/Ref. No 14230, is a monomer used as a catalyst in the anionic polymerisation of caprolactam. After the manufacture residual caprolactam sodium salt can remain in the finished product and m
37、ay migrate into foodstuffs coming into contact with that product. Caprolactam sodium salt hydrolyzes instantly when in contact with aqueous media. The method has been pre-validated by a collaborative trial with five laboratories. DD CEN/TS 13130-16:20056 1 Scope This document, part of EN 13130, spec
38、ifies an analytical procedure for the determination of caprolactam in the food simulants distilled water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and rectified olive oil. The level of caprolactam monomer determined is expressed as mg caprolactam/kg of food or food simulant. The method
39、is appropriate for the quantitative determination of caprolactam in an approximate analyte concentration range of 1,5mg/kg to 30 mg per kilogram of food simulant. This method is also applicable to the determination of the specific migration of caprolactam sodium salt, PM/Ref No 14230, as caprolactam
40、 sodium salt instantaneously hydrolyzes to caprolactam when in contact with aqueous media. NOTE The method should also be applicable to other aqueous food simulants as well as to other fatty food simulants e.g. sunflower oil, a mixture of synthetic triglycerides and volatile substitutes for fat simu
41、lants. 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) applies. EN 13130-1:2004, Ma
42、terials 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 conditions of exposure to fo
43、od simulants. 3 Principle The level of caprolactam in aqueous food simulants is determined by gas chromatography. Olive oil test samples are extracted with a mixture of water/ethanol and the resultant solutions analyzed by gas chromatography. Quantification is achieved using an internal standard, ca
44、prylolactam. Calibration is achieved by analysis of relevant simulants containing known amounts of caprolactam and caprylolactam. Confirmation of caprolactam levels is established by gas chromatography using a column of different polarity. Alternatively, confirmation can also be carried out by combi
45、ned gas chromatography/ mass spectrometry (GC/MS). 4 Reagents NOTE All reagents should be of recognized analytical quality unless otherwise stated. DD CEN/TS 13130-16:20057 4.1 Analytes 4.1.1 Caprolactam, (6-Caprolactam; e-Caprolactam; Aza-2-cycloheptanone), C6H11NO molecular weight: 113,16, purity
46、98 % (GC). 4.1.2 Aza-2-cyclononanone, (8-aminooctanoic acid lactam; 8-Caprylolactam), C8H15NO molecular weight 141,2, purity 99 %. 4.2 Chemicals 4.2.1 Ethanol, absolute 4.2.2 n-Heptane 4.2.3 Methanol 4.2.4 Water, deionized 4.3 Solutions 4.3.1 Ethanol/water = 1:2 Measure 200 ml ethanol (4.2.1) and ma
47、ke up with water (4.2.4) to 600 ml. 4.3.2 Standard stock solution of caprolactam in methanol (0,5 mg/ml) Weigh to the nearest 0,1 mg approximately 50 mg of caprolactam (4.1.1) into a 100 ml volumetric flask. Dissolve the caprolactam in methanol and make up to the mark with methanol (4.2.3). Calculat
48、e the exact concentration in milligrams of caprolactam per millilitre solution. Repeat the procedure to obtain a second stock solution. NOTE The solution can be stored in a well-closed container in the dark for a maximum period of 3 months at any temperature between - 20 C to + 20 C. 4.3.3 Internal
49、standard stock solution of caprylolactam in methanol (0,35 mg/ml) Weigh to the nearest 0,1 mg approximately 70 mg of caprylolactam (4.1.2) into a 200 ml volumetric flask. Dissolve the caprylolactam in methanol and make up to the mark with methanol (4.2.3). Calculate the exact concentration in milligrams caprylolactam per millilitre of solution. NOTE The solution can be stored in a well-closed container in the dark for a maximum period of 3 months at any temperature between - 20 C and + 20 C. 4.3.4 Diluted internal standard solution of caprylolactam in
