1、DRAFT FOR DEVELOPMENTDD CEN/TS 13130-17:2005Materials and articles in contact with foodstuffs Plastics substances subject to limitation Part 17: Determination of carbonyl chloride in plasticsICS 67.250g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g4
2、0g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58DD CEN/TS 13130-17:2005This British Standard was published under the authority of the Standards Policy and Strategy Committee on 16 September 2005 BSI 16 September 2005ISBN 0 580 46060 6National fore
3、wordThis Draft for Development is the official English language version of CEN/TS 13130-17:2005.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 not evaluated usin
4、g 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 Development are reque
5、sted 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 the end of its 3-y
6、ear 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 a European Standar
7、d, 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 clause number and pro
8、posing, 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 may be found in t
9、he 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. Users are responsible
10、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 issued.Amendments issued sinc
11、e publicationAmd. No. Date CommentsTECHNICAL SPECIFICATIONSPCIFICATION TECHNIQUETECHNISCHE SPEZIFIKATIONCEN/TS 13130-17February 2005ICS 67.250English versionMaterials and articles in contact with foodstuffs - Plasticssubstances subject to limitation - Part 17: Determination ofcarbonyl chloride in pl
12、asticsMatriaux et objets en contact avec les denresalimentaires - Substances dans les matires plastiquessoumises des limitations - Partie 17: Dtermination duchlorure de carbonyle dans les matires plastiquesWerkstoffe und Gegenstnde in Kontakt mit Lebensmitteln- Substanzen in Kunststoffen, die Beschr
13、nkungenunterliegen - Teil 17: Bestimmung von Carbonylchlorid inKunststoffenThis 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 the members of CEN will be r
14、equested 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 level in an appropriate form
15、. 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 Republic, Denmark, Estonia, Finla
16、nd, 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 NORMALISATIONEUROPISCHES KOMITEE FR NORMU
17、NGManagement 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 13130-17:2005: E2 Contents page Foreword. 3 Introduction 5 1 Scope 6 2 Normative references . 6 3 Principle . 6 4 Reage
18、nts 6 5 Apparatus 8 6 Samples . 9 7 Procedure 11 8 Precision 14 9 Confirmation 14 10 Test report . 15 Bibliography . 16 DD CEN/TS 13130-17:20053 Foreword This document (CEN/TS 13130-17:2005) has been prepared by Technical Committee CEN/TC 194 “Utensils in contact with food”, the secretariat of which
19、 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 series of test methods
20、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. At the time of preparation and publication of this part of EN 13130 the European Un
21、ion 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 strongly recomm
22、ended 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 13130-1. Further parts of EN 13130, under the general title Materials and articles in c
23、ontact 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 plastic
24、s. 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 food simulants Part 2: Determination of terephthali
25、c 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 monoethylene
26、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 simulants Part 11: Determination of 11-aminoundecanoic acid in food simulants Part 12: Dete
27、rmination of 1,3-benzenedimethanamine in food simulants DD CEN/TS 13130-17:20054 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-hydroxyphenyl)-2-indoline in food simulants Part 15: Determination of 1,3-butadiene
28、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-dihydroxybenzene, 1,4-dihydroxybenzene, 4,4-dihydroxybenzophenone and 4,4dihydroxybiphenyl in foo
29、d 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 Part 22: Determination of ethylene oxide and propylene oxide in plastics Part 23: De
30、termination 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 26: Determination of 1-octene and tetrahydrofuran in food simulants Part 27: Determi
31、nation 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 All chemicals are hazardous to health to a greater or lesser extent. It is beyond th
32、e 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 this Technical Specification
33、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, Belgium, Cyprus, Czech Republic
34、, 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 13130-17:20055 Introduction Carbonyl chloride or phosgene,
35、 CCl2O, PM/Ref. No 14380, is a monomer used in the manufacture of certain plastics materials and articles intended to come into contact with foodstuffs. After manufacture, residual carbonyl chloride can remain in the polymer and may migrate into foodstuffs coming into contact with the plastics mater
36、ial or article. The method has been pre-validated by a collaborative trial with two laboratories. DD CEN/TS 13130-17:20056 1 Scope This document, part of EN 13130, specifies an analytical procedure for the determination of carbonyl chloride monomer in polymers. The method is applicable to polycarbon
37、ate as well as to other polymers and copolymers where these are soluble in methylene chloride. The level of carbonyl chloride monomer determined is expressed as milligrams of carbonyl chloride per kilogram of polymer. The method is appropriate for the quantitative determination of carbonyl chloride
38、at a minimum level of 0,3 mg per kilogram of polymer. 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 the referenced document (includi
39、ng 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 determination of substances in plastics an
40、d the selection of conditions of exposure to food simulants. 3 Principle The level of carbonyl chloride in the polymer is determined by dissolution of the polymer and concurrent derivatization with 2-aminophenol. The resulting 2-benzoxazolinone is analyzed by high performance liquid chromatography (
41、HPLC) with ultra violet (UV) detection. Quantification is achieved by standard addition of carbonyl chloride to the test polymer. Confirmation of the identity of carbonyl chloride is carried out by diode array detection. 4 Reagents NOTE 1 Carbonyl chloride reacts rapidly with moisture. Suitable prec
42、autions should be taken to protect carbonyl chloride solutions from moisture. The carbonyl chloride derivative is not sensitive to moisture. NOTE 2 All reagents should be of recognized analytical quality unless otherwise stated. 4.1 Analytes 4.1.1 Carbonyl chloride, CCl2O, molecular weight, 98,9, co
43、mmercially available as a 20 % (w/w) solution in toluene, density at 20 C 0,935 kg per litre, corresponding to a concentration of 1,93 mole per litre or 191 g per litre. Store the commercial carbonyl chloride solution in a closed container for up to 6 months at + 1 C in the dark. DD CEN/TS 13130-17:
44、20057 4.1.2 2-benzoxazolinone, C7H5NO2, molecular weight: 135,1, purity 98 %. 4.2 Chemicals 4.2.1 2-aminophenol (2-hydroxyanilin), C6H7NO, molecular weight: 109,1, purity 98 %. 4.2.2 Dichloromethane (DCM), dried over a bed of molecular sieve (5), H2O 99,5 %. 4.2.3 Toluene, dried over a bed of molecu
45、lar sieve (5), H2O 99,5 %. NOTE The water content of the toluene should be as low as possible. Toluene dried over a molecular sieve can be obtained from chemical suppliers. Alternatively, toluene can be dried before use, in which case the molecular sieve should be activated for maximum water absorpt
46、ion. 4.2.4 Methanol 4.2.5 Acetone 4.2.6 Acetonitrile, purity 99,5 %, HPLC grade 4.2.7 Distilled water, HPLC grade 4.2.8 Sodium dihydrogen orthophosphate, NaH2PO4. 2H2O 4.2.9 Glacial acetic acid 4.2.10 Hydrochloric acid, 1 N 4.2.11 Sodium sulfate, anhydrous 4.2.12 Mobile phase for high performance li
47、quid chromatography, prepared as follows. Dissolve 7,5 g of sodium dihydrogen orthophosphate (4.2.8) in 700 ml of water (4.2.7), add 250 ml acetonitrile (4.2.6) using a measuring cylinder and adjust to pH (3,6 0,1) with glacial acetic acid (4.2.9). NOTE 1 Approximately 5 ml should be sufficient. Mak
48、e up to 1 l with water (4.2.7). NOTE 2 Degassing the mobile phase may be necessary with some HPLC equipment. 4.3 Solutions 4.3.1 Standard solution of carbonyl chloride in toluene, 95,5 mg/l Pipette into a 20 ml vial (5.3) 20,0 0,1ml of toluene (4.2.3) and close with the septum and cap. Using a 10 l
49、syringe (5.5), add 10 l of the 20 % carbonyl chloride solution (4.1.1) by injection through the septum and dispensing after the needle has immersed into the toluene. Remove the syringe and mix. NOTE 1 The exact concentration of this standard solution is 95,5 mg/l. Repeat the procedure to provide a second standard solution. DD CEN/TS 13130-17:20058 NOTE 2 This standard solution can be stored at + 4 C for up to 4 weeks in the dark. 4.3.2 Derivatization reagent solution, 500 g/ml Accurately weigh 25 mg 0,2 mg of 2-aminophenol (4.2.1) into a 50 m
