1、BRITISH STANDARD BS EN 13130-3:2004 Materials and articles in contact with foodstuffs Plastics substances subject to limitation Part 3: Determination of acrylonitrile in food and food simulants The European Standard EN 13130-3:2004 has the status of a British Standard ICS 67.250 BS EN 13130-3:2004 T
2、his 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 43948 8 National foreword This British Standard is the official English language version of EN 13130-3:2004. It supersedes DD ENV 13130-3:1999 which is wi
3、thdrawn. 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
4、on 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 th
5、e 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 enq
6、uirers 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 do
7、cument 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
8、NORMEEUROPENNE EUROPISCHENORM EN131303 May2004 ICS67.250 Englishversion MaterialsandarticlesincontactwithfoodstuffsPlastics substancessubjecttolimitationPart3:Determinationof acrylonitrileinfoodandfoodsimulants Matriauxetobjetsencontactavecdesdenres alimentairesSubstancesdanslesmatiresplastiques sou
9、misesdeslimitationsPartie3:Dterminationde lacrylonitriledanslesalimentsetlessimulantsdaliments WerkstoffeundGegenstndeinKontaktmitLebensmitteln SubstanzeninKunststoffen,dieBeschrnkungen unterliegenTeil3:BestimmungvonAcrylnitrilin LebensmittelnundPrflebensmitteln ThisEuropeanStandardwasapprovedbyCENo
10、n24March2004. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheCentralSecr
11、etariatortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheCentralSecretariathasthesamestatusast heofficial versions. CENmembersarethenationalstanda
12、rdsbodiesofAustria,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 COMITEUR
13、OPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2004CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN131303:2004:EEN 13130-3:2004 (E) 2 Contents page Foreword3 1 Scope6 2 Normative references6 3 Principl
14、e6 4 Reagents.6 5 Apparatus.7 6 Samples8 6.1 Laboratory samples.8 6.2 Test sample preparation .8 7 Procedure.9 7.1 GC preparation.9 7.2 Performance of GC measurements .10 8 Expression of results10 8.1 General10 8.2 Method of calculation10 8.3 Precision data and detection limit .12 9 Confirmation.12
15、9.1 Requirement for confirmation 12 9.2 Confirmation by combined gas chromatography-mass spectrometry12 9.3 Confirmation by re-analysis on a GC column of different polarity.13 10 Test report13 Annex A (normative) Method of standard addition .14 Annex B (normative) Calibration via external standardiz
16、ation 16 Annex C (normative) Manual sample injection 17 Bibliography 18 EN 13130-3:2004 (E) 3 Foreword This document (EN 13130-3:2004) 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 Subcommit
17、tee 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 identical text or by endorsement, at the latest by November 2004, and c
18、onflicting 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 intended to support Directives 2002/72/EC 1, 89/109/EEC 2, 82/711/EEC 3 a
19、nd 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 amendments
20、 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 standard. E
21、N 13130-3 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 determination of specific mi
22、gration 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 migration of substances from plastics to foods and food simulants and the
23、 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 4: Determination of 1,3-butadiene in plastics Part 5: Determination of vinylidene chloride in food simulants Part 6: Determination
24、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 simulants Part 11:
25、 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 Part 14: Determination of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indoline in food si
26、mulants EN 13130-3:2004 (E) 4 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- dihy
27、droxybenzene, 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 Part 22: Det
28、ermination 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 26: Determin
29、ation 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 Standards. Parts 9 to 28 are Technical Specifications, prepared within the S
30、tandards, 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 are bound to implement this European Standard: Austria, Belgium, Cyprus, Cz
31、ech 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. EN 13130-3:2004 (E) 5 Introduction Acrylonitrile, CH 2 =
32、CH-CN, is a monomer used in the manufacture of certain plastics materials and articles intended to come into contact with foodstuffs. During the manufacture of acrylonitrile copolymers, residual acrylonitrile monomer can remain in the polymer and can migrate into food coming into contact with the po
33、lymer. 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 acrylonitrile. The method has been validated by collaborative trial using fruit juice, wine and sunflower oil. EN
34、13130-3:2004 (E) 6 1 Scope This part of this European Standard specifies a method for the determination of acrylonitrile monomer in foods and 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 m
35、ixture of synthetic triglycerides or sunflower oil or corn oil, as well as to liquid and solid foodstuffs such as beverages and soft margarine. The level of acrylonitrile monomer determined is expressed as milligrammes of acrylonitrile per kilogram of food or food simulant. The method is appropriate
36、 for the quantitative determination of acrylonitrile monomer at minimum levels of down to 0,01 mg/kg to 0,005 mg/kg, or lower, in food simulant, depending on the applied test conditions (see NOTE in 8.2.3). With regard to the performance in the mentioned foodstuffs, in general, a direct detection li
37、mit of 0,02 mg/kg is achievable. NOTE This method was developed for the determination of acrylonitrile 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 applic
38、able 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 hereafter.
39、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 13130-1:2004, Ma
40、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 t
41、o food simulants 3 Principle The level of acrylonitrile (AN) in a food, or a food simulant, is determined by headspace gas chromatography with automated sample injection, using nitrogen specific detection. Quantification is achieved using propionitrile (PN) as an internal standard with calibration a
42、gainst blank samples fortified with acrylonitrile. If blank samples 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 as described in annex
43、B. If automated headspace sampling cannot be performed, manual injection as described in annex C shall be applied. Confirmation of acrylonitrile 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 Reag
44、ents 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 standard may be followed. Therefore, specif
45、ic EN 13130-3:2004 (E) 7 warnings are not given and users of this standard shall ensure that they meet all the necessary safety requirements in their own country. 4.1 Acrylonitrile, CH 2 =CH-CN, purity greater than 99% (w/w). 4.2 Propionitrile, CH 3 -CH 2 -CN, containing no impurity at 1 % by area w
46、hich will elute at the same GC retention time as acrylonitrile. 4.3 Propylene carbonate, CH 3 -CH-OCOO-CH 2 , boiling point 240 C to 243 C at normal pressure, free of any interferences ( 1 % area) with the acrylonitrile and propionitrile peaks. 4.4 Nitrogen, purified to 99,9999 %. 4.5 Standard solut
47、ions of acrylonitrile in propylene carbonate with defined concentrations in the range 25 g/ml to 25 g/ml, prepared as described in 4.5.1 and 4.5.2. 4.5.1 Prepare concentrated standard acrylonitrile solutions at approximately 12,5 mg/ml as follows: a) Fill a 100 ml volumetric flask with 50 ml propyle
48、ne carbonate (4.3), close and weigh to an accuracy of 0,2 mg. Add to the propylene carbonate a quantity of approximately 1,5 ml (1,25 g) acrylonitrile (4.1) and shake the closed flask. Determine the exact mass of acrylonitrile added by re-weighing to an accuracy of 0,2 mg. Fill the flask to the 100 ml mark. b) Repeat item a) to provide a second concentrated standard solution. 4.5.2 Prepare dilute standard acrylonitrile solutions as follows: a) With an accuracy of 0,1 ml throughout, dilute one of the solu
