1、BRITISH STANDARD BS EN 13130-8:2004 Materials and articles in contact with foodstuffs Plastics substances subject to limitation Part 8: Determination of isocyanates in plastics The European Standard EN 13130-8:2004 has the status of a British Standard ICS 67.250 BS EN 13130-8:2004 This British Stand
2、ard was published under the authority of the Standards Policy and Strategy Committee on 17 June 2004 BSI 17 June 2004 ISBN 0 580 43969 0 National foreword This British Standard is the official English language version of EN 13130-8:2004. It supersedes DD ENV 13130-8:1999 which is withdrawn. The UK p
3、articipation 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 request to its
4、 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 BSI Electronic
5、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 enquirers to underst
6、and 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 document comprises
7、a front cover, an inside front cover, the EN title page, pages 2 to 21 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 NORMEEUROPENNE EUROPISCHENORM EN131308
8、May2004 ICS67.250 Englishversion MaterialsandarticlesincontactwithfoodstuffsPlastics substancessubjecttolimitationPart8:Determinationof isocyanatesinplastics Matriauxetobjetsencontactaveclesdenres alimentairesSubstancesdanslesmatiresplastiques soumisesdeslimitationsPartie8:Dterminationdes isocyanate
9、sdanslesmatiresplastiques WerkstoffeundGegenstndeinKontaktmitLebensmitteln SubstanzeninKunststoffen,dieBeschrnkungen unterliegenTeil8:BestimmungvonIsocyanatenin Kunststoffen ThisEuropeanStandardwasapprovedbyCENon24March2004. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipula
10、tetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheCentralSecretariatortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French
11、,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheCentralSecretariathasthesamestatusast heofficial versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,Cyprus,CzechRepublic,Denmark,Estonia,Finland,France, Germany,G
12、reece,Hungary,Iceland,Ireland,Italy,Latvia,Lithuania,Luxembourg,Malta,Netherlands,Norway,Poland,Portugal, Slovakia, Slovenia,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Bru
13、ssels 2004CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN131308:2004:EEN 13130-8:2004 (E) 2 Contents page Foreword3 1 Scope 6 2 Normative references 6 3 Principle6 4 Reagents.6 4.1 Analytes 7 4.2 Reagents.7 5 Apparatus .9 5.1 General9 6 Samples 9 7
14、 Procedure .10 7.1 Test sample screening 10 7.1.1 Test sample extraction and derivatization 10 7.1.2 Preparation of reagent blank sample.10 7.1.3 Preparation of internal standard check sample .10 7.1.4 Preparation of un-derivatized sample blank .10 7.1.5 Chromatographic determination10 7.2 Quantific
15、ation of isocyanates by standard addition11 7.2.1 General11 7.2.2 Preparation of standard solutions for quantification (0 g/ml to 5 g/ml).11 7.2.3 Procedure for standard addition12 7.2.4 Control sample.12 7.2.5 Analysis 12 7.3 Evaluation of data12 7.3.1 General12 7.3.2 HPLC interferences12 8 Express
16、ion of results 13 8.1 Calculation by least squares regression.13 8.2 Graphical determination using internal standard 14 8.3 Precision data and detection limit .15 8.3.1 General15 8.3.2 Repeatability.15 8.3.3 Reproducibility.15 8.3.4 Detection limits 15 9 Confirmation.16 9.1 Requirement for confirmat
17、ion 16 9.2 Confirmation by re-analysis on an HPLC column of different elution characteristics.16 10 Test report 16 Annex A (normative) Calibration by standard addition omitting the internal standard 18 Annex B (informative) 19 Annex C (informative) Suggested gradient profile 20 Bibliography 21 EN 13
18、130-8:2004 (E) 3 Foreword This document (EN 13130-8:2004) 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 of a series of analytical test methods for plastics
19、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 standards shall be withdrawn at the latest by November 20
20、04. 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/EEC 4 and 97/48/EC 5, and 85/572/EEC 6. At the time of
21、 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 are expected which could change the legislative requi
22、rements 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 13130-8 should be read in conjunction with EN 13130-1 Further parts of EN 1
23、3130, 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 materials into foodstuffs and food simulants and the de
24、termination 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 substances in plastics and the selection of conditions of
25、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 5: Determination of vinylidene chloride in food simulants Part 6: Determination of vinylid
26、ene chloride in plastics Part 7: Determination of monoethylene glycol and diethylene glycol in food simulants 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
27、 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 simulants EN 13130-8:2004 (E) 4 Part 15: Determination of 1,3
28、-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- dihydroxybenzophenone and 4,4dihydroxybi
29、phenyl 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 ethylene oxide and propylene oxide in plastic
30、s 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 and tetrahydrofuran in food simulants Par
31、t 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, Measurement and Testing project, MAT1-CT92-0006,
32、“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, Denmark, Estonia, Finland, France, Germany, G
33、reece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EN 13130-8:2004 (E) 5 Introduction Isocyanates, characterised by the -NCO group, are monomers used for the manufact
34、ure of materials and articles intended to come in contact with food. During manufacture residual isocyanates can remain in the polymer and can migrate into food coming into contact with the polymer. EN 13130-8:2004 (E) 6 1 Scope This part of this European Standard describes a method for the determin
35、ation of individual and total levels of residual isocyanates in plastics materials and articles. This method is applicable to the analysis of polyurethane polymers. The total level of isocyanate monomers in materials and articles determined according to the procedure described in this standard is gi
36、ven in milligrams of NCO per kilogram of material or article. The method is capable of quantitative determination of individual isocyanates measured as NCO at 0,04 mg/kg and total isocyanates at 1,0 mg/kg. NOTE The method has been applied to the analysis of 9 isocyanate monomers listed in 3.1. It ha
37、s not been applied to the analysis of octadecyl isocyanate, diphenylether-4,4-diisocyanate or 3,3-dimethyl-4,4-diisocyanatobiphenyl as samples of these monomers have not been obtained. There is no reason to anticipate that the method may not be suitable for the analysis of these monomers also. 2 Nor
38、mative 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. For dated references, subsequent amendments to or revisions
39、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, Materials and articles in contact with foodstuffs - Plastics s
40、ubstances 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 to food simulants. 3 Principle The procedure consists of two
41、parts: screening and, if necessary, quantitative determination. Quantitative determination is applied only if isocyanates are detected by the screening procedure. Materials and articles are initially screened for residual isocyanates by solvent extraction with dichloromethane and concurrent derivati
42、zation with 9-(methylaminomethyl)anthracene. 1-Naphthyl isocyanate is used during the screening procedure to check that the derivatization procedure has been successful. The resultant fluorescent derivatives are analysed by high performance liquid chromatography with fluorescence detection. Material
43、s found to contain residual isocyanates are quantified by standard addition to the material or article under test, using 1-naphthyl isocyanate as internal standard. If interferences are experienced with the internal standard then calibration is carried out by standard addition omitting the internal
44、standard, as described in annex A. Confirmation of isocyanate levels is carried out by re-analysing the sample extracts on an HPLC column with different elution characteristics. 4 Reagents WARNING: All chemicals are hazardous to health to a greater or lesser extent. It is beyond the scope of this st
45、andard 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 EN 13130-8:2004 (E) 7 not given and users of this standard shall ensure that they meet all the neces
46、sary safety requirements in their own country. NOTE 1 Isocyanates react extremely rapidly with moisture. Suitable precautions should be taken to ensure all glassware is dry. All laboratory glassware should be rinsed with diethyl ether (4.2.2) and baked at 105 C overnight before use. After baking, vi
47、als should be placed in a desiccator and stored until required. Isocyanate standards should be protected from moisture and stored under refrigeration at -20 C. NOTE 2 All reagents should be of recognised analytical quality, unless otherwise specified. 4.1 Analytes 4.1.1 2,6-toluene diisocyanate CH 3
48、 C 6 H 3 (NCO) 24.1.2 diphenylmethane-4,4-diisocyanate OCNC 6 H 4 CH 2 C 6 H 4 NCO 4.1.3 2,4-toluene diisocyanate CH 3 C 6 H 3 (NCO) 24.1.4 hexamethylene diisocyanate OCNC 6 H 12 NCO 4.1.5 cyclohexyl isocyanate C 6 H 11 NCO 4.1.6 1,5-naphthalene diisocyanate C 10 H 6 (NCO) 24.1.7 diphenylmethane-2,4-diisocyanate OCNC 6 H 4 CH 2 C 6 H 4 NCO 4.1.8 2,4-toluene diisocyanate dimer 4.1.9 phenyl isocyanate C 6 H 5 NCO 4.1.10 1-naphthyl isocyanate (internal standard, C 10 H 7 NCO), which contains no impurity at
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