1、DRAFT FOR DEVELOPMENTDD CEN/TS 13130-24:2005Materials and articles in contact with foodstuffs Plastics substances subject to limitation Part 24: Determination of maleic acid and maleic anhydride in food simulantsICS 67.250g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g
2、44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58DD CEN/TS 13130-24:2005This Draft for Development was published under the authority of the Standards Policy and Strategy Committee on 16 September 2005 BSI 16 September 2005ISBN
3、0 580 46066 5National forewordThis Draft for Development is the official English language version of CEN/TS 13130-24:2005.This publication is not to be regarded as a British Standard.It is being issued in the Draft for Development series of publications and is of a provisional nature because the met
4、hod was not evaluated using recognized ring trial procedures. As a consequence there are no reproducibility data for the method. It should be applied on this provisional basis, so that information and experience of its practical application may be obtained.Comments arising from the use of this Draft
5、 for Development are requested so that UK experience can be reported to the European organization responsible for its conversion to a European standard. A review of this publication will be initiated 2 years after its publication by the European organization so that a decision can be taken on its st
6、atus at the end of its 3-year life. Notification of the start of the review period will be made in an announcement in the appropriate issue of Update Standards.According to the replies received by the end of the review period, the responsible BSI Committee will decide whether to support the conversi
7、on into a European Standard, to extend the life of the Technical Specification or to withdraw it. Comments should be sent in writing to the Secretary of BSI Subcommittee CW/47/1, Migration from plastics, at British Standards House, 389 Chiswick High Road, London W4 4AL, giving the document reference
8、 and clause number and proposing, where possible, an appropriate revision of the text.A list of organizations represented on this subcommittee can be obtained on request to its secretary.Cross-referencesThe British Standards which implement international or European publications referred to in this
9、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 Catalogue or of British Standards Online.This publication does not purport to include all the necessary provisions of a contra
10、ct. Users are responsible for its correct application.Summary of pagesThis document comprises a front cover, an inside front cover, the CEN/TS title page, pages 2 to 16, an inside back cover and a back cover.The BSI copyright notice displayed in this document indicates when the document was last iss
11、ued.Amendments issued since publicationAmd. No. Date CommentsTECHNICAL SPECIFICATIONSPCIFICATION TECHNIQUETECHNISCHE SPEZIFIKATIONCEN/TS 13130-24February 2005ICS 67.250English versionMaterials and articles in contact with foodstuffs - Plasticssubstances subject to limitation - Part 24: Determination
12、 ofmaleic acid and maleic anhydride in food simulantsMatriaux et objets en contact avec les denresalimentaires - Substances dans les matires plastiquessoumises des limitations - Partie 24 : Dtermination delacide malique et de lanhydre malique dans lessimulants dalimentsWerkstoffe und Gegenstnde in K
13、ontakt mit Lebensmitteln- Substanzen in Kunststoffen, die Beschrnkungenunterliegen - Teil 24: Bestimmung von Maleinsure undMaleinanhydrid in PrflebensmittelnThis Technical Specification (CEN/TS) was approved by CEN on 16 December 2004 for provisional application.The period of validity of this CEN/TS
14、 is limited initially to three years. After two years the members of CEN will be requested to submit theircomments, particularly on the question whether the CEN/TS can be converted into a European Standard.CEN members are required to announce the existence of this CEN/TS in the same way as for an EN
15、 and to make the CEN/TS availablepromptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the CEN/TS)until the final decision about the possible conversion of the CEN/TS into an EN is reached.CEN members are the national sta
16、ndards bodies of 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 and United Kingdom.EUROPEAN COMMI
17、TTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2005 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. CEN/TS 13130-24:2005: E2 Contents page Forew
18、ord. 3 Introduction 5 1 Scope 6 2 Normative references . 6 3 Principle . 6 4 Reagents 6 5 Apparatus 8 6 Samples . 9 7 Procedure 11 8 Expression of results 12 9 Confirmation 13 10 Test report . 15 Bibliography . 16 DD CEN/TS 13130-24:20053 Foreword This document (CEN/TS 13130-24:2005) has been prepar
19、ed by Technical Committee CEN/TC 194 “Utensils in contact with food”, the secretariat of which is held by BSI. This part of EN 13130 has been prepared within the Standards, Measurement and Testing project, MAT1-CT92-0006, “Development of Methods of Analysis for Monomers” and has been prepared by Sub
20、committee (SC 1) of TC 194 “Utensils in contact with food“ as one of a series of test methods for plastics materials and articles in contact with foodstuffs. 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/
21、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 are expected which could cha
22、nge 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. This part of EN 13130 should be read in conjunction w
23、ith 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 materials into foo
24、dstuffs and food simulants and the determination of specific monomers and additives in plastics. The 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
25、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 5: Determination of vinylidene chloride in food simulants P
26、art 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 simulants Part 10: Determination of acrylamide in fo
27、od simulants Part 11: Determination of 11-aminoundecanoic acid in food simulants Part 12: Determination of 1,3-benzenedimethanamine in food simulants DD CEN/TS 13130-24:20054 Part 13: Determination of 2,2-bis(4-hydroxyphenyl)propane (Bisphenol A) in food simulants Part 14: Determination of 3,3-bis(3
28、-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 18: Determination of 1,2-dihydroxybenzene, 1,3-dih
29、ydroxybenzene, 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 of ethylenediamine and hexamethylenediamine in food
30、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 25: Determination of 4-methyl-pentene in food simul
31、ants 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-trimethylolpropane in food simulants Parts 1 to 8 are European Standards. Parts 9 to 28 are Technical Specifications
32、. WARNING All chemicals are hazardous to health to a greater or lesser extent. It is beyond the scope of this Technical Specification to give instructions for the safe handling of all chemicals, that meet, in full, the legal obligations in all countries in which this Technical Specification may be f
33、ollowed. Therefore, specific warnings are not given and users of this Technical Specification should ensure that they meet all the necessary safety requirements in their own country. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries ar
34、e bound to announce this CEN Technical Specification: 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, Switze
35、rland and United Kingdom. DD CEN/TS 13130-24:20055 Introduction Maleic acid, C4H4O4, PM/Ref. No 19540, and maleic anhydride, C4H2O3, PM/Ref. No 19960, are monomers used in the manufacture of certain plastics materials and articles intended to come into contact with foodstuffs. After manufacture resi
36、dual maleic acid and maleic anhydride can remain in the finished product and may migrate into foodstuffs coming into contact with that product. This method describes the determination of the specific migration of maleic anhydride as maleic acid. The method has been pre-validated by a collaborative t
37、rial with three laboratories. DD CEN/TS 13130-24:20056 1 Scope This document, part of EN 13130, specifies an analytical procedure for the determination of maleic acid in the four conventional food simulants, water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and olive oil or approved subst
38、itute. The level of maleic acid determined is expressed as milligrams of maleic acid per kilogram of food or food simulant. The method is appropriate for the quantitative determination of maleic acid in approximate analyte concentration range of 5 mg/kg to 60 mg/kg in the above mentioned food simula
39、nts. This method is also suitable for the determination of maleic anhydride in the four food simulants as the anhydride is hydrolyzed rapidly and completely to maleic acid during sample preparation. The level of maleic anhydride is then expressed as milligrams of maleic acid per kilogram of food sim
40、ulant. NOTE The method should also be applicable to other aqueous food simulants as well as to the other fatty food simulants, e.g. sunflower oil, corn oil or a mixture of synthetic triglycerides. The suitability of the fat simulant should be assessed prior to setting up migration tests - it may be
41、found necessary to use sunflower oil or HB 307 if unacceptable interferences are found with olive oil. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the l
42、atest edition of the referenced document (including any amendments) applies. EN 13130-1:2004, 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 a
43、nd the determination of substances in plastics and the selection of conditions of exposure to food simulants. 3 Principle The level of maleic acid is determined by reverse phase, ion pair high performance liquid chromatography (HPLC) with UV detection at 220 nm. Maleic anhydride hydrolyzes rapidly a
44、nd completely to maleic acid during sample preparation. Quantification of maleic acid is achieved using citraconic acid, as an internal standard, with calibration against relevant food simulants samples, fortified with known amounts of maleic acid. Confirmation of the maleic acid level is carried ou
45、t by ion exchange chromatography with UV detection at 245 nm. 4 Reagents NOTE All reagents should be of recognized analytical quality unless otherwise stated. DD CEN/TS 13130-24:20057 4.1 Analytes 4.1.1 Maleic acid, HO2CCH=CHCO2H purity greater than 98 %. 4.1.2 Citraconic acid, HO2CC(CH3)=CHCO2H of
46、purity greater than 98 % w/w and not containing maleic acid. 4.1.3 Mesaconic acid, HO2CH=C(CH3).CO2H of purity greater than 98 % w/w and not containing maleic acid. NOTE Mesaconic acid may be used as an alternative internal standard. 4.2 Chemicals 4.2.1 Ethanol, absolute. 4.2.2 Sodium hydrogen carbo
47、nate 4.2.3 Water, HPLC grade. 4.2.4 Dipotassium hydrogen orthophosphate, K2HPO4.3 H2O. 4.2.5 Potassium dihydrogen orthophosphate, KH2PO4.4.2.6 Orthophosphoric acid (85 %) 4.2.7 Sodium hydroxide, 2 mol/l solution in water. 4.2.8 Cetyl trimethyl ammonium bromide, HPLC grade. 4.2.9 Disodium tetraborate
48、 4.2.10 Ammonium chloride 4.2.11 Acetonitrile 4.3 Solutions 4.3.1 Stock solution of maleic acid in ethanol (7 500 mg/l) Weigh accurately approximately 0,75 g of the maleic acid (4.1.1) into a tared 100 ml volumetric flask. Half fill the flask with ethanol (4.2.1), shake thoroughly and make the volum
49、e up to the mark with ethanol (4.2.1). Calculate the actual concentration of maleic acid in milligrams per litre. Repeat the procedure to provide a second stock solution. NOTE The stock solutions can be stored at 20 C for up to 2 months in stoppered glass volumetric flasks. DD CEN/TS 13130-24:20058 4.3.2 Preparation of an internal standard solution of citraconic acid in ethanol (7 500 mg/l) Weigh approximately 0,75 g of citraconic acid (4.1.2) into a tared 100 ml volumetric flask. Dissolve in ethanol (4.2.1) and make the volume up to the mark wit
