1、DRAFT FOR DEVELOPMENTDD CEN/TS 13130-14:2005Materials and articles in contact with foodstuffs Plastics substances subject to limitation Part 14: Determination of 3,3-bis (3-methyl-4-hydroxyphenyl)-2-indoline ICS 67.250g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g5
2、4g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58in food simulantsDD CEN/TS 13130-14:2005This Draft for Development was published under the authority of the Standards Policy and Strategy Committee on 16 September 2005 BSI 16 Septem
3、ber 2005ISBN 0 580 46072 XNational forewordThis Draft for Development is the official English language version of CEN/TS 13130-14:2005.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 be
4、cause the method 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
5、of this Draft 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 ta
6、ken on its status 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
7、 the conversion 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 docum
8、ent reference 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 referre
9、d 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 Catalogue or of British Standards Online.This publication does not purport to include all the necessary provision
10、s of a contract. 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 15 and a back cover.The BSI copyright notice displayed in this document indicates when the document was last issued.Amend
11、ments issued since publicationAmd. No. Date CommentsTECHNICAL SPECIFICATIONSPCIFICATION TECHNIQUETECHNISCHE SPEZIFIKATIONCEN/TS 13130-14February 2005ICS 67.250English versionMaterials and articles in contact with foodstuffs - Plasticssubstances subject to limitation - Part 14: Determination of 3,3-b
12、is(3-methyl-4-hydroxyphenyl)-2-indoline in food simulantsMatriaux et objets en contact avec les denresalimentaires - Substances dans les matires plastiquessoumises des limitations - Partie 14 : Dtermination de la3,3-bis(3-mthyl-4-hydroxyphnyl)-2-indolinone dans lessimulants dalimentsWerkstoffe und G
13、egenstnde in Kontakt mit Lebensmitteln- Substanzen in Kunststoffen, die Beschrnkungenunterliegen - Teil 14: Bestimmung von 3,3-Bis(3-Methyl-4-Hydroxyphenyl)-2-Indolinon in PrflebensmittelnThis Technical Specification (CEN/TS) was approved by CEN on 16 December 2004 for provisional application.The pe
14、riod of validity of this CEN/TS 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/
15、TS in the same way as for an EN 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.C
16、EN 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, Portugal, Slovakia,Slovenia, Spain, Sweden, Switzerland an
17、d United Kingdom.EUROPEAN COMMITTEE 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-
18、14:2005: E2 Contents page Foreword. 3 Introduction 5 1 Scope 6 2 Normative references . 6 3 Principle . 6 4 Reagents 6 5 Apparatus 8 6 Samples . 9 7 Procedure 10 8 Expression of results 11 9 Confirmation 13 10 Test Report 14 Bibliography . 15 DD CEN/TS 13130-14:20053 Foreword This document (CEN/TS 1
19、3130-14:2005) has been prepared 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”
20、 and has been prepared by Subcommittee (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/
21、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 to existing Directives
22、 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. This part of EN 13130 sh
23、ould 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 migration fro
24、m plastics materials into foodstuffs 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 o
25、f 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 Part 4: Determination of 1,3-butadiene in plastics Part 5: Determination of vinylidene
26、 chloride in food simulants 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 simulants Part 10: Dete
27、rmination 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 DD CEN/TS 13130-14:20054 Part 13: Determination of 2,2-bis(4-hydroxyphenyl)propane (Bisphenol A) in food simulants Part 1
28、4: 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 18: Determination of
29、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 of ethylenediamine and
30、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 25: Determination of 4
31、-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-trimethylolpropane in food simulants Parts 1 to 8 are European Standards. Parts 9 to 28
32、 are Technical Specifications. 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 Tec
33、hnical Specification may be followed. 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
34、of the following countries are 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, Sl
35、ovenia, Spain, Sweden, Switzerland and United Kingdom. DD CEN/TS 13130-14:20055 Introduction 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone, PM/Ref. 13600, C22H19NO3, is a monomer used in the manufacture of certain plastics materials and articles intended to come into contact with foodstuffs. After
36、manufacture residual 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone can remain in the finished product and may migrate into foodstuffs coming into contact with that product. The method has been pre-validated by collaborative trial with two laboratories. DD CEN/TS 13130-14:20056 1 Scope This document
37、, part of EN 13130, specifies an analytical procedure for the determination of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone in the food simulants water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and olive oil or approved substitute. The level of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indo
38、linone determined, is expressed as milligrams of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone per kilogram of food or food simulant. The method is applicable to the quantitative determination of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone in an approximate analyte concentration range of 0,18 mg
39、/kg to 4/ kg of food simulants. NOTE 1 The method should also be applicable to other aqueous food simulants as well as to the other fatty food simulants e.g. a mixture of synthetic triglycerides or sunflower oil. NOTE 2 The suitability of the fat simulant should be assessed prior to setting up migra
40、tion tests. Olive oil has been found to give unacceptable interference in some cases. 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 latest edition of
41、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 and the determinat
42、ion of substances in plastics and the selection of conditions of exposure to food simulants. 3 Principle The level of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone in aqueous food simulants is determined by reverse phase high performance liquid chromatography (HPLC) with UV detection at 235 nm. Fat
43、 simulants are extracted with 80 % aqueous acetonitrile prior to HPLC analysis. Quantification is achieved by calibration against samples of relevant food simulants, fortified with known amounts of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone. The level of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indol
44、inone determined, is expressed as milligrams per kilogram of food simulant. Confirmation of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone is carried out by reverse phase HPLC using an analytical column of different polarity with UV detection at 280 nm. 4 Reagents NOTE All reagents should be of reco
45、gnized analytical quality unless otherwise stated. 4.1 Analyte 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone, (C22H19NO3) purity greater than 98 % w/w. DD CEN/TS 13130-14:20057 4.2 Chemicals 4.2.1 Ethanol, absolute 4.2.2 Acetonitrile, chromatography grade 4.2.3 Water, HPLC grade 4.2.4 Orthophosphor
46、ic acid, 80 % 4.3 Solutions 4.3.1 Stock solution of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone in ethanol (approximately 2 500 mg/l) Weigh to the nearest 0,1 mg approximately 0,06 g of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone (4.1) into a tared 25 ml volumetric flask. Half fill the flask w
47、ith ethanol (4.2.1), shake thoroughly and make the volume up to the mark with ethanol (4.2.1). Calculate the exact concentration of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone in milligrams per litre. Repeat the procedure to provide a second stock solution. NOTE The stock solutions may be stored
48、in the dark at room temperature for up to 3 months in stoppered glass volumetric flasks. 4.3.2 Intermediate standard solutions of 3,3-bis(3-methyl-4 -hydroxyphenyl)-2-indolinone in ethanol Into six 25 ml volumetric flasks, add by pipette 0 ml, 0,1 ml, 0,5 ml, 1,0 ml, 2,0 ml and 4,0 ml of the stock s
49、olution (4.3.1). Dilute to the mark with ethanol (4.2.1) to give standard solutions containing nominal concentrations of approximately 0 mg/l, 10 mg/l, 50 mg/l, 100 mg/l, 200 mg/l and 400 mg per litre of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone. Calculate the exact concentrations of the standard solutions in milligrams per litre. Repeat the procedure using the second stock solution prepared in 4.3.1 to give a second set of intermediate standard solutions. Store the standard solutions of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indolinone stored for up
