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1、BRITISH STANDARD BS EN 13130-5:2004 Materials and articles in contact with foodstuffs Plastics substances subject to limitation Part 5: Determination of vinylidene chloride in food simulants The European Standard EN 13130-5:2004 has the status of a British Standard ICS 67.250 ? BS EN 13130-5:2004 Th
2、is British Standard was published under the authority of the Standards Policy and Strategy Committee on 17 June 2004 BSI 17 June 2004 ISBN 0 580 43946 1 National foreword This British Standard is the official English language version of EN 13130-5:2004. It supersedes DD ENV 13130-5:1999 which is wit
3、hdrawn. The UK participation in its preparation was entrusted by Technical Committee CW/47, Materials and articles in contact with foodstuffs, to Subcommittee CW/47/1, Migration from plastics, which has the responsibility to: A list of organizations represented on this subcommittee can be obtained o
4、n request to its secretary. Cross-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
5、the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid e
6、nquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This
7、document comprises a front cover, an inside front cover, the EN title page, pages 2 to 18, an inside back cover and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments EUROPEAN STANDA
8、RD NORME EUROPENNE EUROPISCHE NORM EN 13130-5 May 2004 ICS 67.250 English version Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 5: Determination of vinylidene chloride in food simulants Matriaux et objets en contact avec des denres alimentaires
9、- Substances dans les matires plastiques soumises des limitations - Partie 5 : Dtermination du chlorure de vinylidne dans les simulants daliments alimentaires Werkstoffe und Gegenstnde in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen, die Beschrnkungen unterliegen - Teil 5: Bestimmung von V
10、inylidenchlorid in Kunststoffen This European Standard was approved by CEN on 24 March 2004. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date
11、 lists and bibliographical references concerning such national standards may be obtained on application to the Central Secretariat or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the r
12、esponsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, I
13、reland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B
14、-1050 Brussels 2004 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 13130-5:2004: E EN 13130-5:2004 (E) 2 Contents page Foreword3 1Scope 6 2Normative references6 3Principle6 4Reagents.6 4.1Analyte and internal standard7 4.1.1Analyte
15、7 4.1.2Internal standard7 4.2Chemicals.7 4.3Solutions of standards and internal standard7 4.3.1Preparation of stock solutions of vinylidene chloride.7 4.3.2Intermediate solutions of vinylidene chloride 7 4.3.3Internal standard stock solution7 4.3.4Intermediate internal standard solution7 5Apparatus
16、.8 6Samples 9 6.1Laboratory samples.9 6.2Preparation of test samples9 6.2.1General9 6.2.2Aqueous food simulants.9 6.2.3Fatty food simulant9 6.3Preparation of blank samples.9 6.4Preparation of calibration samples9 7Procedure .10 8Expression of results 10 8.1Method of calculation10 8.1.1GC interferenc
17、es10 8.1.2Graphical determination using internal standard 10 8.1.3Graphical determination via external standardization.11 8.1.4Calculation of the concentration using a response factor11 8.1.5Calculation of the specific migration.11 8.2Precision.11 8.2.1Validation11 8.2.2Repeatability and reproducibi
18、lity.12 8.2.3Detection limit12 9Confirmation.13 9.1Requirement for confirmation13 9.2Confirmation by combined gas chromatography-mass spectrometry13 9.3Confirmation by analysis on a GC column of different polarity .13 10Test report13 Annex A (normative) Method of standard addition15 Annex B (normati
19、ve) Manual sample injection.17 Bibliography18 ? EN 13130-5:2004 (E) 3 Foreword This document (EN 13130-5:2004) has been prepared by Technical Committee CEN/TC 194 “Utensils in contact with food”, the secretariat of which is held by BSI. This document was prepared by Subcommittee SC1 of TC 194 as one
20、 of a series of analytical test methods for plastics materials and articles in contact with foodstuffs. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by November 2004, and conflicting national stan
21、dards shall be withdrawn at the latest by November 2004. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. This standard is intended to support Directives 2002/72/EC 1, 89/109/EEC 2, 82/711/EEC 3 and its amendments 93/8/E
22、EC 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 amendments to existing Directives
23、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 standard. EN 13130-5 should be read
24、 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 determination of specific migration from plastics ma
25、terials into foodstuffs and food simulants and the determination of specific monomers and additives in plastics. The other 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 subst
26、ances 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 Part 6: Determination of vinylidene chlori
27、de 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: Determination of 11
28、-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 ? EN 13130-5:2004 (E) 4 Part 14: Determination of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indoline in foo
29、d 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- dihydroxybenzene, 4,4
30、- 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: Determination of eth
31、ylene 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: Determination of 1-octene
32、 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-trimethylopropane in food simulants Parts 1 to 8 are European Standards. Parts 9 to 28 are Technical Specifications, prepared within the Standards, Measure
33、ment and Testing project, MAT1-CT92-0006, “Development of Methods of Analysis for Monomers”. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Den
34、mark, 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. ? EN 13130-5:2004 (E) 5 Introduction Vinylidene chloride (VdC) (1,1-dichl
35、oroethylene), H2C=CCl2, is a monomer used in the manufacture of certain plastics films and coatings intended to come into contact with foodstuffs. During the manufacture of vinylidene chloride polymers and copolymers, residual vinylidene chloride monomer can remain in the polymer and can migrate int
36、o food coming into contact with the polymer. The method described in this part of the standard should be used in conjunction with part 1 of this standard which describes the procedures required prior to the determination of vinylidene chloride. ? EN 13130-5:2004 (E) 6 1 Scope This part of this Europ
37、ean Standard specifies a method for the determination of vinylidene chloride monomer in food simulants. The method is applicable to aqueous food simulants, to the fatty food simulant olive oil and other fatty food simulants, simulants D, e.g. a mixture of synthetic triglycerides or sunflower oil or
38、corn oil. The level of vinylidene chloride determined is expressed as milligrams of vinylidene chloride per kilogram of food simulant. The method is appropriate for the quantitative determination of vinylidene chloride at a level of 0,05 mg/kg. NOTE This method was developed for the determination of
39、 vinylidene chloride in 15 % (v/v) aqueous ethanol, as required by the regulations in force at the time the development work was carried out. However, this method, developed for 15 (v/v) aqueous ethanol, should be applicable to the determination in 10 (v/v) aqueous ethanol. 2 Normative references Th
40、is European Standard incorporates by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate places in the text, and the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publ
41、ications apply to this European Standard only when incorporated in it by amendment or revision. For undated references the latest edition of the publication referred to applies (including amendments). EN 13130-1:2004, Materials and articles in contact with foodstuffs - Plastics substances subject to
42、 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 food simulants 3 Principle The level of vinylidene chloride in a food simulant
43、 is determined by headspace gas chromatography with automated sample injection and using either electron capture or flame ionization detection. Quantification is achieved using 1-chloropropane (1-CP) as internal standard with calibration against blank samples of simulant fortified with vinylidene ch
44、loride. If blank samples of simulant cannot be obtained then the method of standard addition described in annex A is employed. If interferences are experienced with the internal standard then calibration is carried out by external standardization. If automated headspace sampling cannot be performed,
45、 manual injection as described in annex B shall be applied. Confirmation of vinylidene chloride levels is carried out either by combined gas chromatography/mass spectrometry (GC/MS) or by re-analysis on a second GC column of different polarity. 4 Reagents WARNING: All chemicals are hazardous to heal
46、th to a greater or lesser extent. It is beyond the scope of this standard to give instructions for the safe handling of all chemicals, that meet, in full, the legal obligations in all countries in which this standard may be followed. Therefore, specific warnings are not given and users of this stand
47、ard shall ensure that they meet all the necessary safety requirements in their own country. ? EN 13130-5:2004 (E) 7 4.1 Analyte and internal standard 4.1.1 Analyte Vinylidene chloride (VdC), H2C=CCl2, of purity greater than 99 %. 4.1.2 Internal standard 1-Chloropropane (1-CP), CH3(CH2)2Cl, of purity
48、 greater than 98 %. 4.2 Chemicals N,N-dimethylacetamide (DMA), CH3CON(CH3)2, of purity greater than 99 %. 4.3 Solutions of standards and internal standard 4.3.1 Preparation of stock solutions of vinylidene chloride a) Stock solution of vinylidene chloride with a defined concentration of approximatel
49、y 2,5 g/kg. To a 20 ml flask or vial with cap, add 20 ml N,N-dimethylacetamide (4.2), close and weigh to an accuracy of 0,1 mg. Add to the N,N-dimethylacetamide a quantity of approximately 40 l (0,048g) vinylidene chloride (4.1.1) and shake the closed flask. Weigh to an accuracy of 0,1 mg. Determine the exact mass of vinylidene chloride added in grams per kilogram. b) Repeat item a) to provide a seco