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 This
2、 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 withd
3、rawn. 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 on
4、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 the B
5、SI 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 enquir
6、ers 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 docum
7、ent 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. Date CommentsEUROPEANSTANDARD NOR
8、MEEUROPENNE EUROPISCHENORM EN131305 May2004 ICS67.250 Englishversion MaterialsandarticlesincontactwithfoodstuffsPlastics substancessubjecttolimitationPart5:Determinationof vinylidenechlorideinfoodsimulants Matriauxetobjetsencontactavecdesdenres alimentairesSubstancesdanslesmatiresplastiques soumises
9、deslimitationsPartie5:Dterminationdu chloruredevinylidnedanslessimulantsdaliments alimentaires WerkstoffeundGegenstndeinKontaktmitLebensmitteln SubstanzeninKunststoffen,dieBeschrnkungen unterliegenTeil5:BestimmungvonVinylidenchloridin Kunststoffen ThisEuropeanStandardwasapprovedbyCENon24March2004. C
10、ENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheCentralSecretariatortoanyC
11、ENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheCentralSecretariathasthesamestatusast heofficial versions. CENmembersarethenationalstandardsbodiesofAust
12、ria,Belgium,Cyprus,CzechRepublic,Denmark,Estonia,Finland,France, Germany,Greece,Hungary,Iceland,Ireland,Italy,Latvia,Lithuania,Luxembourg,Malta,Netherlands,Norway,Poland,Portugal, Slovakia, Slovenia,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISA
13、TION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2004CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN131305:2004:EEN 13130-5:2004 (E) 2 Contents page Foreword3 1 Scope 6 2 Normative references 6 3 Principle6 4 Reagents
14、.6 4.1 Analyte and internal standard 7 4.1.1 Analyte 7 4.1.2 Internal standard7 4.2 Chemicals .7 4.3 Solutions of standards and internal standard 7 4.3.1 Preparation of stock solutions of vinylidene chloride.7 4.3.2 Intermediate solutions of vinylidene chloride 7 4.3.3 Internal standard stock soluti
15、on 7 4.3.4 Intermediate internal standard solution 7 5 Apparatus .8 6 Samples 9 6.1 Laboratory samples.9 6.2 Preparation of test samples9 6.2.1 General9 6.2.2 Aqueous food simulants.9 6.2.3 Fatty food simulant9 6.3 Preparation of blank samples.9 6.4 Preparation of calibration samples9 7 Procedure .1
16、0 8 Expression of results 10 8.1 Method of calculation10 8.1.1 GC interferences10 8.1.2 Graphical determination using internal standard 10 8.1.3 Graphical determination via external standardization.11 8.1.4 Calculation of the concentration using a response factor11 8.1.5 Calculation of the specific
17、migration.11 8.2 Precision.11 8.2.1 Validation11 8.2.2 Repeatability and reproducibility.12 8.2.3 Detection limit 12 9 Confirmation.13 9.1 Requirement for confirmation 13 9.2 Confirmation by combined gas chromatography-mass spectrometry13 9.3 Confirmation by analysis on a GC column of different pola
18、rity .13 10 Test report 13 Annex A (normative) Method of standard addition 15 Annex B (normative) Manual sample injection.17 Bibliography 18 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 secreta
19、riat of which is held by BSI. This document was prepared by Subcommittee SC1 of TC 194 as one 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 id
20、entical text or by endorsement, at the latest by November 2004, and conflicting national standards 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 inte
21、nded 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 intended to come into con
22、tact 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 published Directive(s)
23、 before commencement of a test or tests described in this standard. EN 13130-5 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 other
24、s 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 other parts of EN 13130 are as follows. Part 1: Guide to test methods for the specific mig
25、ration 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 in food and food simulants
26、Part 4: Determination of 1,3-butadiene in plastics 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 in food
27、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 Part 13: Determination of 2,2-bis(4-hydroxyphenyl)propane (Bisphenol A) in food simulants EN 13130
28、-5:2004 (E) 4 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 plastics Part 1
29、8: 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: Determination
30、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 simulants Part
31、 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-trimethylopropane in food simulants Parts 1 to 8 are European St
32、andards. Parts 9 to 28 are Technical Specifications, prepared within the Standards, Measurement 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 a
33、re bound to implement this European Standard: 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 an
34、d United Kingdom. EN 13130-5:2004 (E) 5 Introduction Vinylidene chloride (VdC) (1,1-dichloroethylene), H 2 C=CCl 2 , 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 c
35、opolymers, residual vinylidene chloride monomer can remain in the polymer and can migrate into 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
36、determination of vinylidene chloride. EN 13130-5:2004 (E) 6 1 Scope This part of this European 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
37、food simulants, simulants D, e.g. a mixture of synthetic triglycerides or sunflower oil or 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
38、 chloride at a level of 0,05 mg/kg. NOTE This method was developed for the determination of 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, shoul
39、d be applicable to the determination in 10 (v/v) aqueous ethanol. 2 Normative references This 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
40、hereafter. For dated references, subsequent amendments to or revisions of any of these publications 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
41、-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 conditions of
42、 exposure to food simulants 3 Principle The level of vinylidene chloride in a food simulant 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 intern
43、al standard with calibration against blank samples of simulant fortified with vinylidene chloride. 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 ca
44、rried out by external standardization. If automated headspace sampling cannot be performed, 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 seco
45、nd GC column of different polarity. 4 Reagents WARNING: All chemicals are hazardous to health 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 s
46、tandard may be followed. Therefore, specific warnings are not given and users of this standard 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), H 2 C=CCl 2 , of pur
47、ity greater than 99 %. 4.1.2 Internal standard 1-Chloropropane (1-CP), CH 3 (CH 2 ) 2 Cl, of purity greater than 98 %. 4.2 Chemicals N,N-dimethylacetamide (DMA), CH 3 CON(CH 3 ) 2 , of purity greater than 99 %. 4.3 Solutions of standards and internal standard 4.3.1 Preparation of stock solutions of
48、vinylidene chloride a) Stock solution of vinylidene chloride with a defined concentration of approximately 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 second stock so
