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1、DRAFT FOR DEVELOPMENT DD CEN/TS 13130-22:2005 Materials and articles in contact with foodstuffs Plastics substances subject to limitation Part 22: Determination of ethylene oxide and propylene oxide in plastics ICS 67.250 DD CEN/TS 13130-22:2005 This Draft for Development was published under the aut
2、hority of the Standards Policy and Strategy Committee on 16 September 2005 BSI 16 September 2005 ISBN 0 580 46064 9 National foreword This 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
3、 issued in the Draft for Development 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 informati
4、on and experience of its practical application may be obtained. Comments 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 ini
5、tiated 2 years after its 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 receive
6、d by the end of the review period, the responsible BSI Committee will decide whether to support the 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 fro
7、m plastics, at British Standards House, 389 Chiswick High Road, London W4 4AL, giving the document reference 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. Cro
8、ss-references The British Standards which implement international or European publications referred to in 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
9、 British Standards Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Summary of pages This document comprises a front cover, an inside front cover, the CEN/TS title page, pages 2 to 17 and a back cover.
10、 The BSI copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments W - - - - - - - - - 7 - - 7- - - - - 8- - - - - 7 - - 78 8 - - 8- - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -
11、- W W D - - w - - - - 2 Contents page Foreword. 3 Introduction 5 1 Scope 6 2 Normative 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 (
12、normative) Manual sample injection.16 Bibliography . 17 DD CEN/TS 13130-22:2005 3 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
13、 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 food“ as one of a series of test methods for plastics materials and articles in contact with foodstuffs.
14、 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 of this part of EN 13130 the European Union legislation relating to plastics materials and articles int
15、ended 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 supports. It is therefore strongly recommended that users of this standard refer to the latest relevant
16、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 general title Materials and articles in contact with foodstuffs - Plastics substances subject to limitat
17、ion, 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 specific monomers and additives in plastics. The parts of EN 13130 are as follows. Part 1: Guide to test
18、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 simulants Part 2: Determination of terephthalic acid in food simulants Part 3: Determination of acrylonitrile
19、 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 plastics Part 7: Determination of monoethylene glycol and diethylene glycol in food simulants Part 8: Determin
20、ation 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-aminoundecanoic acid in food simulants Part 12: Determination of 1,3-benzenedimethanamine in food simulants DD CEN/
21、TS 13130-22:2005 4 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 simulants Part 15: Determination of 1,3-butadiene in food simulants Part 16: Determination of caprolactam and ca
22、prolactam 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-dihydroxybenzophenone and 4,4dihydroxybiphenyl in food simulants Part 19: Determination of dimethylaminoethanol in
23、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 and propylene oxide in plastics Part 23: Determination of formaldehyde and hexamethylenetetramine in food
24、 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 tetrahydrofuran in food simulants Part 27: Determination of 2,4,6-triamino-1,3,5-triazine in food simulants Part
25、 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 of this Technical Specification to give instructions f
26、or 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 ensure that they meet all the necessary safety requirem
27、ents 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, Estonia, Finland, France, Germany, Greece, Hungary
28、, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. DD CEN/TS 13130-22:2005 5 Introduction Ethylene oxide, C2H4O, PM/Ref. No 17020, and propylene oxide, C3H6O, PM/Ref. No 24010 are
29、monomers used in the manufacture of certain plastics materials and articles intended 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-valid
30、ated by collaborative trial with two laboratories. DD CEN/TS 13130-22:2005 6 1 Scope 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 et
31、hylene oxide or propylene oxide in an analyte concentration range of approximately 0,2 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 refe
32、rences, 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 and foo
33、d simulants and the determination of substances in plastics and the selection of conditions 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 inter
34、nal standard with calibration against polymer samples fortified with ethylene oxide or 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
35、gas chromatography/mass spectrometry (GC/MS). DD CEN/TS 13130-22:2005 7 4 Reagents NOTE 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
36、% (w/w). 4.1.3 Diethyl ether, C4H10O containing no impurity greater than 1 % by peak area 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
37、or propylene oxide and diethyl ether peak. 4.3 Solutions 4.3.1 Stock solutions of ethylene 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
38、mass including septa and cap to within 0,1 mg. Introduce 0,1g to 0,3 g ethylene oxide (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 soluti
39、on. Repeat the procedure to provide a second 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
40、 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. 4.3.1.2 Stock solution of propylene oxide in dimethylacetami
41、de (1 mg/ml) Weigh to the nearest 0,1 mg approximately 50 mg of propylene oxide (4.1.2) 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
42、of propylene oxide per millilitre of solution. Repeat the procedure to provide a second 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
43、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 13130-22:2005 8 4.3.2 Diluted standard solution of ethylene oxide or propylene oxide in dimethylacetamide 4.3.2.1 Diluted standard solutions of ethylene oxide in dimethylacetamide (4 g