1、DRAFT FOR DEVELOPMENTDD CEN/TS 13130-27:2005Materials and articles in contact with foodstuffs Plastics substances subject to limitation Part 27: Determination of 2,4,6-triamino-1,3,5-triazine in food simulantsICS 67.250g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g
2、54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58DD CEN/TS 13130-27:2005This Draft for Development was published under the authority of the Standards Policy and Strategy Committee on 16 September 2005 BSI 16 September 2005ISBN 0 5
3、80 46069 XNational forewordThis Draft for Development is the official English language version of CEN/TS 13130-27:2005.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
4、 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 fo
5、r 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 statu
6、s 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 conversion
7、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 and
8、 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 docu
9、ment 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.
10、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 14, an inside back cover and a back cover.The BSI copyright notice displayed in this document indicates when the document was last issued.
11、Amendments issued since publicationAmd. No. Date CommentsTECHNICAL SPECIFICATIONSPCIFICATION TECHNIQUETECHNISCHE SPEZIFIKATIONCEN/TS 13130-27February 2005ICS 67.250English versionMaterials and articles in contact with foodstuffs - Plasticssubstances subject to limitation - Part 27: Determination of2
12、,4,6-triamino-1,3,5-triazine in food simulantsMatriaux et objets en contact avec les denresalimentaires - Substances dans les matires plastiquessoumises des limitations - Partie 27 : Dtermination de la2,4,6-triamino-1,3,5-triazine dans les simulants dalimentsWerkstoffe und Gegenstnde in Kontakt mit
13、Lebensmitteln- Substanzen in Kunststoffen, die Beschrnkungenunterliegen - Teil 27: Bestimmung von 2,4,6-Triamino-1,3,5-Triazin 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
14、 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 and to mak
15、e 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 standards bodi
16、es 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 COMMITTEE FOR ST
17、ANDARDIZATIONCOMIT 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 13130-27:2005: E2 Contents page Foreword. 3 Intr
18、oduction 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 12 10 Test report . 13 Bibliography . 14 DD CEN/TS 13130-27:20053 Foreword This document (CEN/TS 13130-27:2005) has been prepared by Techn
19、ical 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 Subcommittee (
20、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 85/572/EEC 6.
21、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 change the leg
22、islative 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 with EN 1313
23、0-1. 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 foodstuffs and
24、 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 the selecti
25、on 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 Part 6: Dete
26、rmination 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 food simulant
27、s Part 11: Determination of 11-aminoundecanoic acid in food simulants Part 12: Determination of 1,3-benzenedimethanamine in food simulants DD CEN/TS 13130-27:20054 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-h
28、ydroxyphenyl)-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-dihydroxybenze
29、ne, 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 simulants P
30、art 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 simulants Part 2
31、6: 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. WARNING A
32、ll 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 followed. Th
33、erefore, 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 are bound to
34、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, Switzerland and U
35、nited Kingdom. DD CEN/TS 13130-27:20055 Introduction 2,4,6-triamino-1,3,5-triazine, (C3H6N6), PM/Ref. No 25420, is a monomer used in the manufacture of certain plastics materials and articles intended to come into contact with foodstuffs. Other frequently used names for 2,4,6-triamino-1,3,5-triazine
36、 are melamine and 2,4,6-triamino-s-triazine. After manufacture residual 2,4,6-triamino-1,3,5-triazine can remain in the finished product and may migrate into foodstuffs coming into contact with that product. The method has been pre-validated by a collaborative trial with two laboratories. DD CEN/TS
37、13130-27:20056 1 Scope This document, part of EN 13130, specifies an analytical procedure for the determination of 2,4,6-triamino-1,3,5-triazine in food simulants distilled water, 3 % (w/v) acetic acid aqueous solution, 15% (v/v) ethanol aqueous solution and rectified olive oil. The level of 2,4,6-t
38、riamino-1,3,5-triazine monomer determined is expressed as milligrams per kilogram food simulant. The method is appropriate for the quantitative determination of 2,4,6-triamino-1,3,5-triazine in approximate analyte concentration range of 2 mg/kg to 60 mg/kg food simulant. NOTE The method should also
39、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. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, onl
40、y the edition cited applies. For 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
41、 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 level of 2,4,6-triamino-1,3,5-triazine in food simulants is determined by high performance liquid chromatography (HPL
42、C) using UV detection at 230 nm. The aqueous food simulants are analyzed directly by HPLC. The olive oil test samples are extracted with water/isopropanol and the resultant solutions analyzed by HPLC. Quantification is achieved by means of external standard calibration using relevant food simulant s
43、amples fortified with known amounts of 2,4,6-triamino-1,3,5-triazine. Confirmation of 2,4,6-triamino-1,3,5-triazine is carried out by diode array detection and peak ratio measurement at various wavelengths. 4 Reagents NOTE All reagents should be of recognized analytical quality unless otherwise stat
44、ed. 4.1 Analyte 2,4,6-triamino-1,3,5-triazine, (C3H6N6), purity 99 %. DD CEN/TS 13130-27:20057 4.2 Chemicals 4.2.1 Acetonitrile, HPLC grade. 4.2.2 Isopropanol 4.2.3 Iso-octane 4.2.4 Water deionized, HPLC quality, 4.2.5 Sodium dihydrogen phosphate monohydrate 4.2.6 Sodium hydroxide 4.3 Solutions 4.3.
45、1 Stock solution of 2,4,6-triamino-1,3,5-triazine in water (1 mg/ml) Weigh to the nearest 0,1 mg approximately 50 mg of 2,4,6-triamino-1,3,5-triazine (4.1) in a 50 ml volumetric flask and add 40 ml water (4.2.4). Place the flask for 15 min to 30 min in an ultrasonic water-bath at 70 C to dissolve th
46、e 2,4,6-triamino-1,3,5-triazine. Cool the solution to room temperature and fill the volumetric flask up to the mark with water (4.2.4). Calculate the actual concentration in milligrams of 2,4,6-triamino-1,3,5-triazine per millilitre of solution. Repeat the procedure to obtain a second stock solution
47、. Store the solution in a well closed container in dark for a maximum period of 3 months at any temperature between - 20 C and + 20 C. 2,4,6-triamino-1,3,5-triazine is only slightly soluble in water, therefore assure that all 2,4,6-triamino-1,3,5-triazine is dissolved. Preparation of more concentrat
48、ed stock solutions is not feasible. 4.3.2 Diluted standard solutions of 2,4,6-triamino-1,3,5-triazine in aqueous food simulants (0,1 mg/ml) Pipette 5 ml of the stock solution (4.3.1) into a 50 ml volumetric flask. Make up to the mark with the appropriate food simulant. Calculate the actual concentra
49、tion in milligrams of 2,4,6-triamino-1,3,5-triazine per millilitre of solution. Repeat the procedure using the second standard stock solution to obtain a second set of diluted standard solutions. 4.3.3 Standard solution of 2,4,6-triamino-1,3,5-triazine in isopropanol/water Pipette, into a series of 25 ml volumetric flasks, 0 ml, 0,5 ml, 1 ml, 2 ml, 4 ml and 8 ml of the stock solution (4.3.1). Add 12,5 ml isopropanol (4.2.2) and make up to the mark with water (4.2.4). The standard solutions thus obtained contain 0 g/ml, 20 g/ml, 40 g/ml, 80 g/ml, 16
