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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 Sta
2、ndard 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 It supersedes DD ENV 13130-8:1999 which is withdrawn.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
3、 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 request to i
4、ts 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 Electroni
5、c 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 under
6、stand 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 comprise
7、s 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. DateComments EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 1
8、3130-8 May 2004 ICS 67.250 English version Materials and articles in contact with foodstuffs - Plastics substances subject to limitation - Part 8: Determination of isocyanates in plastics Matriaux et objets en contact avec les denres alimentaires - Substances dans les matires plastiques soumises des
9、 limitations - Partie 8 : Dtermination des isocyanates dans les matires plastiques Werkstoffe und Gegenstnde in Kontakt mit Lebensmitteln - Substanzen in Kunststoffen, die Beschrnkungen unterliegen - Teil 8: Bestimmung von Isocyanaten in Kunststoffen This European Standard was approved by CEN on 24
10、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 lists and bibliographical references concerning such national standards may be o
11、btained 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 responsibility of a CEN member into its own language and notified to the Central S
12、ecretariat 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, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,
13、 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-1050 Brussels 2004 CENAll rights of exploitation in any form and by any means re
14、served worldwide for CEN national Members. Ref. No. EN 13130-8:2004: E EN 13130-8:2004 (E) 2 Contents page Foreword3 1 Scope 6 2 Normative references6 3 Principle6 4 Reagents.6 4.1 Analytes7 4.2 Reagents.7 5 Apparatus .9 5.1 General9 6 Samples 9 7 Procedure .10 7.1 Test sample screening10 7.1.1 Test
15、 sample extraction and derivatization10 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 Quantification of isocyanates by standard addition11 7.2.1 Genera
16、l11 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 Expression of results 13 8.1 Calculation by least squares regre
17、ssion.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 limits15 9 Confirmation.16 9.1 Requirement for confirmation16 9.2 Confirmation by re-analysis on an HPLC column o
18、f different elution characteristics.16 10 Test report16 Annex A (normative) Calibration by standard addition omitting the internal standard 18 Annex B (informative) 19 Annex C (informative) Suggested gradient profile 20 Bibliography21 EN 13130-8:2004 (E) 3 Foreword This document (EN 13130-8:2004) ha
19、s 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 materials and articles in contact with foodstuffs. This Euro
20、pean 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 2004. This document has been prepared under a mandate given to
21、 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 preparation and publication of this part of EN 13130 the Eu
22、ropean 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 requirements which this standard supports. It is therefore strong
23、ly 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 13130, under the general title Materials and articles in cont
24、act 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 determination of specific monomers and additives in plastics.
25、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 exposure to food simulants Part 2: Determination of terephth
26、alic 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 vinylidene chloride in plastics Part 7: Determination of monoethyle
27、ne 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 Part 12: Determination of 1,3-benzenedimethanamine in food
28、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-butadiene in food simulants Part 16 Determination of caprol
29、actam 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 4,4dihydroxybiphenyl in food simulants Part 19: Determination of dimethyla
30、minoethanol 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 plastics Part 23: Determination of formaldehyde and hexamethylenete
31、tramine 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 Part 27: Determination of 2,4,6-triamino-1,3,5-triazine in food
32、 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, “Development of Methods of Analysis for Monomers”. According
33、 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, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
34、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 manufacture of materials and articles intended to come in contact wi
35、th 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 determination of individual and total levels of residual isocyanates
36、 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 given in milligrams of NCO per kilogram of material or article
37、. 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 has not been applied to the analysis of octadecyl isocyanate,
38、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 Normative references This European Standard incorporates by dat
39、ed 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 publications apply to this European Standard
40、 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 limitation - Part 1: Guide to test meth
41、ods 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 parts: screening and, if necessary, quantitative determinati
42、on. 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 derivatization with 9-(methylaminomethyl)anthracene. 1-Naphthyl isoc
43、yanate 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. Materials found to contain residual isocyanates are quantified by st
44、andard 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 standard, as described in annex A. Confirmation of isocyanat
45、e 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 standard to give instructions for the safe handling of all che
46、micals, 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 necessary safety requirements in their own country. NOTE 1 Isocya
47、nates 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, vials should be placed in a desiccator and stored until requir
48、ed. 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 CH3C6H3(NCO)2 4.1.2 diphenylmethane-4,4-diisocyanate OCNC6H4CH2C
49、6H4NCO 4.1.3 2,4-toluene diisocyanate CH3C6H3(NCO)2 4.1.4 hexamethylene diisocyanate OCNC6H12NCO 4.1.5 cyclohexyl isocyanate C6H11NCO 4.1.6 1,5-naphthalene diisocyanate C10H6(NCO)2 4.1.7 diphenylmethane-2,4-diisocyanate OCNC6H4CH2C6H4NCO 4.1.8 2,4-toluene diisocyanate dimer 4.1.9 phenyl isocyanate C6H5NCO 4.1.10 1-naphthyl isocyanate (internal standard, C10H7NCO), which contains no impurity at 1 % by area which will elute at the same rete