1、 g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58substances subject to limitation Part 22: Determination of ethylene oxide and propylene oxide in pl
2、asticsICS 67.250Materials and articles in contact with foodstuffs Plastics DRAFT FOR DEVELOPMENTDD CEN/TS 13130-22:2005DD CEN/TS 13130-22:2005This Draft for Development was published under the authority of the Standards Policy and Strategy Committee on 16 September 2005 BSI 16 September 2005ISBN 0 5
3、80 46064 9a 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 referen
4、ce 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 thi
5、s 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 cont
6、ract. 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 issue
7、d since publicationAmd. No. Date CommentsComments 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 years after it
8、s 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 end of the revi
9、ew period, the responsible BSI Committee will decide whether to support the conversion into National forewordThis Draft for Development is the official English language version of CEN/TS 13130-22:2005.This publication is not to be regarded as a British Standard.It is being issued in the Draft for De
10、velopment 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 experience of its pr
11、actical application may be obtained.TECHNICAL SPECIFICATIONSPCIFICATION TECHNIQUETECHNISCHE SPEZIFIKATIONCEN/TS 13130-22February 2005ICS 67.250English versionMaterials and articles in contact with foodstuffs - Plasticssubstances subject to limitation - Part 22: Determination ofethylene oxide and pro
12、pylene oxide in plasticsMatriaux et objets en contact avec les denresalimentaires - Substances dans les matires plastiquessoumises des limitations - Partie 22 : Dtermination desoxydes dthylne et de propylne dans les matiresplastiquesWerkstoffe und Gegenstnde in Kontakt mit Lebensmitteln- Substanzen
13、in Kunststoffen, die Beschrnkungenunterliegen - Teil 22: Bestimmung von Ethylenoxid undPropylenoxid in KunststoffenThis 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. Afte
14、r 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 availablepromptly
15、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, Cyprus,
16、 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 DE N
17、ORMALISATIONEUROPISCHES 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 13130-22:2005: E2 Contents page Foreword. 3 Introduction 5 1 Scope 6 2 Normativ
18、e references . 6 3 Principle . 6 4 Reagents 7 5 Apparatus 8 6 Samples . 9 7 Procedure 10 8 Precision 12 9 Confirmation 12 10 Test report . 13 Annex A (normative) Calibration via external standardization . 15 Annex B (normative) Manual sample injection . 16 Bibliography . 17 DD CEN/TS 13130-22:20053
19、Foreword This document (CEN/TS 13130-22:2005) 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 M
20、ethods of Analysis 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, 82/71
21、1/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 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 a
22、mendments to 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 st
23、andard. This 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 determi
24、nation of specific 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 s
25、imulants and 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 Par
26、t 5: Determination 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
27、 in food simulants 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 13130-22:20054 Part 13: Determination of 2,2-bis(4-hydroxyphenyl)propane (Bisph
28、enol A) in 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 pla
29、stics Part 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: Deter
30、mination of 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 simul
31、ants Part 25: 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 E
32、uropean 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 of this Technical Specification to give instructions for the safe handling of all chemicals, that meet, in full, the legal obligations in
33、 all countries 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 n
34、ational standards 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, Norwa
35、y, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. DD CEN/TS 13130-22:20055 Introduction Ethylene oxide, C2H4O, PM/Ref. No 17020, and propylene oxide, C3H6O, PM/Ref. No 24010 are monomers used in the manufacture of certain plastics materials and articles intended
36、 to come into contact with foodstuffs. After manufacture residual ethylene oxide can remain in the finished product and may migrate into foodstuffs coming into contact with that product. The method has been pre-validated by collaborative trial with two laboratories. DD CEN/TS 13130-22:20056 1 Scope
37、This document, part of EN 13130, specifies an analytical procedure for the determination of ethylene oxide (EO) or propylene oxide (PO) in polymers. The method is appropriate for the quantitative determination of ethylene oxide or propylene oxide in an analyte concentration range of approximately 0,
38、2 mg/kg to 2 mg/kg of polymer. 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
39、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
40、itions of exposure to food simulants. 3 Principle The level of ethylene oxide and propylene oxide in polymers is determined by headspace gas chromatography. Quantification is achieved using diethyl ether as an internal standard with calibration against polymer samples fortified with ethylene oxide o
41、r propylene oxide according to the standard addition procedure. Confirmation of ethylene oxide is carried out using another column with different polarity. Confirmation of propylene oxide is carried out by combined gas chromatography/mass spectrometry (GC/MS). DD CEN/TS 13130-22:20057 4 Reagents NOT
42、E All reagents should be of recognized analytical quality unless otherwise stated. 4.1 Analytes 4.1.1 Ethylene oxide, C2H4O of purity greater than 99 % (w/w). 4.1.2 Propylene oxide, C3H6O of purity greater than 99 % (w/w). 4.1.3 Diethyl ether, C4H10O containing no impurity greater than 1 % by peak a
43、rea or peak height, which elutes at the same retention time as ethylene oxide or propylene oxide. 4.2 Chemical N,N-dimethylacetamide, distilled, C4H9NO free of any interferences ( 1 % area) with the ethylene oxide or propylene oxide and diethyl ether peak. 4.3 Solutions 4.3.1 Stock solutions of ethy
44、lene oxide or propylene oxide in dimethylacetamide 4.3.1.1 Stock solutions of ethylene oxide in dimethylacetamide (2 mg/ml to 6 mg/ml) Add 50,0 ml dimethylacetamide (4.2) into a 50 ml sample vial and determine the mass including septa and cap to within 0,1 mg. Introduce 0,1g to 0,3 g ethylene oxide
45、(4.1.1) by bubbling the ethylene oxide gas (4.1.1) through the dimethylacetamide. Weigh the vial to an accuracy of 0,1 mg. Calculate the actual concentration in milligrams of ethylene oxide per millilitre of solution. Repeat the procedure to provide a second stock solution. NOTE The stock solution c
46、an be stored at 20 C for up to 3 months protected from light in septum capped glass vials with minimum headspace or at + 4 C for up to 8 weeks. Start by comparing the two stock solutions by making just one dilution of each stock solution. If the response factor, calculated from the detector response
47、, and the concentration of the solution agree to within 5 % of one another, further diluted standards shall be made from only one of the stock solutions. 4.3.1.2 Stock solution of propylene oxide in dimethylacetamide (1 mg/ml) Weigh to the nearest 0,1 mg approximately 50 mg of propylene oxide (4.1.2
48、) into a 50 ml volumetric flask, which contains approximately 30 ml of dimethylacetamide (4.2). Fill the flask to the mark with dimethylacetamide and mix carefully. Calculate the actual concentration in milligrams of propylene oxide per millilitre of solution. Repeat the procedure to provide a secon
49、d stock solution. NOTE The stock solution can be stored at 20 C for up to 3 months protected from light in septum capped glass vials with minimum headspace or at + 4 C for up to 8 weeks. Start by comparing the two stock solutions by making just one dilution of each stock solution. If the response factor, calculated from the detector response, and the concentration of the solution agree to within 5 % of one another, further diluted standards shall be made from only one of the stock solutions. DD CEN/TS 13
