1、DRAFT FOR DEVELOPMENTDD CEN/TS 13130-28:2005Materials and articles in contact with foodstuffs Plastics substances subject to limitation Part 28: Determination of 1,1,1-trimethylolpropane in food simulantsICS 67.250g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54
2、g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58DD CEN/TS 13130-28:2005This Draft for Development was published under the authority of the Standards Policy and Strategy Committee on 16 September 2005 BSI 16 September 2005ISBN 0 580 46
3、056 8National forewordThis Draft for Development is the official English language version of CEN/TS 13130-28:2005.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 method was
4、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 for Dev
5、elopment 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 status at
6、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 conversion into
7、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 and cla
8、use 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 document
9、 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 contract. User
10、s 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.Amendments issued since pu
11、blicationAmd. No. Date CommentsTECHNICAL SPECIFICATIONSPCIFICATION TECHNIQUETECHNISCHE SPEZIFIKATIONCEN/TS 13130-28February 2005ICS 67.250English versionMaterials and articles in contact with foodstuffs - Plasticssubstances subject to limitation - Part 28: Determination of1,1,1-trimethylolpropane in
12、 food simulantsMatriaux et objets en contact avec les denresalimentaires - Substances dans les matires plastiquessoumises des limitations - Partie 28 : Dtermination du1,1,1,-trimthylolpropane dans les simulants dalimentsWerkstoffe und Gegenstnde in Kontakt mit Lebensmitteln- Substanzen in Kunststoff
13、en, die Beschrnkungenunterliegen - Teil 28: Bestimmung von 1,1,1-Trimethylolpropan 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 is limited initially to three years. After two years t
14、he 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 and to make the CEN/TS availablepromptly at national l
15、evel 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 standards bodies of Austria, Belgium, Cyprus, Czech Republ
16、ic, 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 COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONE
17、UROPISCHES 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 13130-28:2005: E2ContentspageForeword. 3Introduction 5 1 Scope 62 Normative references . 63
18、Principle . 64 Reagents 65 Apparatus 86 Samples . 97 Procedure 108 Expression of results 129 Confirmation 1310 Test report . 14Bibliography . 15DD CEN/TS 13130-28:20053Foreword This document (CEN/TS 13130-28:2005) has been prepared by Technical Committee CEN/TC 194 “Utensils in contact with food”, t
19、he 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 Subcommittee (SC 1) of TC 194 “Utensils in contact with food“ as one of a
20、series of test methods for plastics materials and articles in contact with foodstuffs. Informative Annex A details the relationship of this standard with the European Union Directives. At the time of preparation and publication of this part of EN 13130 the European Union legislation relating to plas
21、tics 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 strongly recommended that users of this standar
22、d refer to the latest relevant published Directive(s) before commencement of a test or tests described in this standard. 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. Further parts of EN 13130,
23、 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 determi
24、nation 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 the selection of conditions of exposure to
25、 food simulantsPart 2: Determination of terephthalic acid in food simulants Part 3: Determination of acrylonitrile in food and food simulantsPart 4: Determination of 1,3-butadiene in plasticsPart 5: Determination of vinylidene chloride in food simulantsPart 6: Determination of vinylidene chloride in
26、 plasticsPart 7: Determination of monoethylene glycol and diethylene glycol in food simulantsPart 8: Determination of isocyanates in plastics Part 9: Determination of acetic acid, vinyl ester in food simulantsPart 10: Determination of acrylamide in food simulantsPart 11: Determination of 11-aminound
27、ecanoic acid in food simulantsPart 12: Determination of 1,3-benzenedimethanamine in food simulantsDD CEN/TS 13130-28:20054Part 13: Determination of 2,2-bis(4-hydroxyphenyl)propane (Bisphenol A) in food simulantsPart 14: Determination of 3,3-bis(3-methyl-4-hydroxyphenyl)-2-indoline in food simulantsP
28、art 15: Determination of 1,3-butadiene in food simulantsPart 16: Determination of caprolactam and caprolactam salt in food simulantsPart 17: Determination of carbonyl chloride in plasticsPart 18: Determination of 1,2-dihydroxybenzene, 1,3-dihydroxybenzene, 1,4-dihydroxybenzene, 4,4-dihydroxybenzophe
29、none and 4,4dihydroxybiphenyl in food simulantsPart 19: Determination of dimethylaminoethanol in food simulantsPart 20: Determination of epichlorohydrin in plasticsPart 21: Determination of ethylenediamine and hexamethylenediamine in food simulantsPart 22: Determination of ethylene oxide and propyle
30、ne oxide in plasticsPart 23: Determination of formaldehyde and hexamethylenetetramine in food simulantsPart 24: Determination of maleic acid and maleic anhydride in food simulantsPart 25: Determination of 4-methyl-pentene in food simulantsPart 26: Determination of 1-octene and tetrahydrofuran in foo
31、d simulantsPart 27: Determination of 2,4,6-triamino-1,3,5-triazine in food simulantsPart 28: Determination of 1,1,1-trimethylolpropane in food simulants Parts 1 to 8 are European Standards. Parts 9 to 28 are Technical Specifications. WARNING All chemicals are hazardous to health to a greater or less
32、er 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 followed. Therefore, specific warnings are not given and users of thi
33、s 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 are bound to announce this CEN Technical Specification: Austria, Belgiu
34、m, 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. DD CEN/TS 13130-28:20055Introduction 1,1,1-
35、trimethylolpropane (TMP), C6H14O3, PM/Ref. No 25600, is a monomer used in the manufacture of certain plastics materials and articles intended to come into contact with foodstuffs. After manufacture residual 1,1,1-trimethylolpropane can remain in the finished product and may migrate into foodstuffs c
36、oming into contact with that product. NOTE 1 The analytical method described in this part of EN 13130 is the result of a study on the determination of the migration of 1,1,1-trimethylolpropane from plastics materials into food simulants. In the course of the study several problems were encountered a
37、nd solutions for these problems were incorporated in the final method. The most suitable method is described in this part of EN 13130. The method was successfully pre-validated by the developing laboratory tests, using the four official EU food simulants, to establish the precision data at the restr
38、iction criterion. Also migration tests were performed with samples containing 1,1,1-trimethylolpropane as monomer in contact for 10 d at 40 C with 15 % v/v aqueous ethanol and olive oil. NOTE 2 During the testing of the method by a second laboratory it appeared that the testing laboratory was not ab
39、le to reproduce the precision data as obtained by the developing laboratory. Based on the problems encountered by the testing laboratory the method description was modified to make critical points more clear. Within the scope of the project “Development of Methods of Analysis for Monomers” it was no
40、t possible to re-test the method and therefore the method described should be considered as a useful analytical method, with limited validation data. Further testing is required to demonstrate that the method can be applied with the required accuracy. The method has been pre-validated in a validatio
41、n experiment only by one laboratory, the developing laboratory. DD CEN/TS 13130-28:2005DD CEN/TS 13130-28:200561 ScopeThis document, part of EN 13130, specifies an analytical procedure for the determination of 1,1,1-trimethylolpropane in food simulants distilled water, 3 % (w/v) acetic acid aqueous
42、solution, 15 % (v/v) ethanol aqueous solution and rectified olive oil. The method is appropriate for the quantitative determination of 1,1,1-trimethylolpropane in approximate analyte concentration range of 0,6 mg/kg to12 mg/kg food simulant. NOTE The method should also be applicable to other aqueous
43、 food simulants as well as to the other fatty food simulants e.g. sunflower oil, corn oil or a mixture of synthetic triglycerides. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. F
44、or undated references, the latest 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 t
45、o foods and food simulants and the determination of substances in plastics and the selection of conditions of exposure to food simulants.3 PrincipleAqueous food simulants are saturated with potassium carbonate and extracted with ethanol/ethyl acetate. After evaporation of the solvent, the extracted
46、TMP is silylated with trimethylsilylimidazole in pyridine. The amount of 1,1,1-trimethylolpropane silyl ethers are determined by gas chromatographywith flame ionization detection. 1,4-butanediol is used as an internal standard. Fat simulant is extracted with water prior to derivatization. Confirmati
47、on of the identity of 1,1,1-trimethylolpropane is established by combined gaschromatography/mass spectrometry. 4 ReagentsNOTE All reagents should be of recognized analytical quality unless otherwise stated. DD CEN/TS 13130-28:200574.1 Analytes4.1.1 1,1,1-trimethylolpropane (TMP), C6H14O3or CH3CH2C(C
48、H2OH)3, molecular weight 134,18; boiling point: 297 C; solubility: W, al; purity: 97 % (GC). 4.1.2 Internal standard: 1,4-butandiol (BUG) or tetramethyleneglycol, C4H10O2or HOCH2CH2CH2CH2OH, molecular weight: 90,12; boiling point: 235,12 C; density: 1,0171 g/ml; solubility: W, al; purity: 98 % (GC).
49、 4.2 Chemicals4.2.1 Water, deionized or HPLC grade. 4.2.2 Acetic acid, 100 %. 4.2.3 Ethanol, absolute. 4.2.4 n-Pentane, 95 %. 4.2.5 Ethyl acetate, 99,5 %. 4.2.6 Derivatizing reagent, trimethylsilylimidazole, TMSI in dry pyridine, in 1 ml ampoules. 4.2.7 Potassium carbonate, 99,9 %. 4.2.8 Cation exchange resin, strong acidic, sulfonated polystyrene resins with spherical particles, capacity 1,7 meq/ml, size 50 mesh to 100 mesh). The cation exchange resin shall be washed with methanol before use. 4.2.9 Sodium hydroxide, 99 %. 4.3 Solutions4.3.1 Stock sol
