1、DRAFT FOR DEVELOPMENTDD CEN/TS 13130-23:2005Materials and articles in contact with foodstuffs Plastics substances subject to limitation Part 23: Determination of formaldehyde and hexamethylenetetramine in food simulantsICS 67.250g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40
2、g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58DD CEN/TS 13130-23:2005This Draft for Development was published under the authority of the Standards Policy and Strategy Committee on 16 September 2005 BSI 16 September 20
3、05ISBN 0 580 46065 7National forewordThis Draft for Development is the official English language version of CEN/TS 13130-23:2005.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
4、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 of thi
5、s 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 taken on
6、 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 the c
7、onversion 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 re
8、ference 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 i
9、n 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 provisions of a
10、 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 16, an inside back cover and a back cover.The BSI copyright notice displayed in this document indicates when the document was l
11、ast issued.Amendments issued since publicationAmd. No. Date CommentsTECHNICAL SPECIFICATIONSPCIFICATION TECHNIQUETECHNISCHE SPEZIFIKATIONCEN/TS 13130-23February 2005ICS 67.250English versionMaterials and articles in contact with foodstuffs - Plasticssubstances subject to limitation - Part 23: Determ
12、ination offormaldehyde and hexamethylenetetramine in food simulantsMatriaux et objets en contact avec les denresalimentaires - Substances dans les matires plastiquessoumises des limitations - Partie 23 : Dtermination duformaldhyde et de lhexamthylnettramine dans lessimulants dalimentsWerkstoffe und
13、Gegenstnde in Kontakt mit Lebensmitteln- Substanzen in Kunststoffen, die Beschrnkungenunterliegen - Teil 23: Bestimmung von Formaldehyd undHexamethylentetramin in PrflebensmittelnThis Technical Specification (CEN/TS) was approved by CEN on 16 December 2004 for provisional application.The period of v
14、alidity 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/TS in the
15、 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.CEN member
16、s 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 and United
17、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 13130-23:2005:
18、E2 Contents page Foreword .3 Introduction.5 1 Scope6 2 Normative references6 3 Principle .6 4 Reagents 6 5 Apparatus.8 6 Samples9 7 Procedure.10 8 Precision 12 9 Confirmation 13 10 Test report15 Bibliography16 DD CEN/TS 13130-23:20053 Foreword This document (CEN/TS 13130-23:2005) has been prepared b
19、y 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 Subcomm
20、ittee (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/
21、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 change
22、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 with
23、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 foodstu
24、ffs 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 the
25、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 Part
26、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 food s
27、imulants Part 11: Determination of 11-aminoundecanoic acid in food simulants Part 12: Determination of 1,3-benzenedimethanamine in food simulants Part 13: Determination of 2,2-bis(4-hydroxyphenyl)propane (Bisphenol A) in food simulants DD CEN/TS 13130-23:20054 Part 14: Determination of 3,3-bis(3-met
28、hyl-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-dihydro
29、xybenzene, 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 simu
30、lants 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 simulants
31、 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. WA
32、RNING 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 follo
33、wed. 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 are bo
34、und 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, Switzerlan
35、d and United Kingdom. DD CEN/TS 13130-23:20055 Introduction Formaldehyde, CH2O, PM/Ref. No 17260, and hexamethylenetetramine, C6H12N4, PM/Ref. No 18670, are monomers used in the manufacture of certain plastics materials and articles intended to come into contact with foodstuffs. After manufacture re
36、sidual formaldehyde or residual hexamethylenetetramine (HMTA) can remain in the finished product and may migrate into foodstuffs coming into contact with that product. Since migration of HMTA is limited as formaldehyde, this method allows the determination of formaldehyde, liberated from HMTA, in fo
37、od simulants water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and rectified olive oil. The chemical conversion of HMTA to formaldehyde is as follows: C6H12N4+ 6 H2O 6 CH2O + 4 NH3The method allows the determination of HMTA and formaldehyde at the same time. The method has been pre-valida
38、ted by collaborative trial with two laboratories. The confirmation procedure was found to be quantitative. In collaborative trials with three laboratories comparable results using the chromotropic acid method and the acetyl acetone method were found for the detection limits, repeatability, recovery
39、and migration of formaldehyde. Therefore the method of determination and the confirmation procedure are interchangeable. DD CEN/TS 13130-23:20056 1 Scope This document, part of EN 13130, specifies an analytical procedure for the chemical conversion of HMTA to formaldehyde and the determination of fo
40、rmaldehyde in food simulants water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and rectified olive oil. The method is appropriate for the quantitative determination of formaldehyde in approximate analyte concentration range of 3,0 mg to 30 mg formaldehyde per kilogram of food simulant, wh
41、ich corresponds to 2,3 mg to 23,3 mg hexamethylenetetramine per kilogram of food simulant. NOTE The method should also be applicable to other aqueous food simulants as well as to other fatty food simulants e.g. sunflower oil, corn oil or a mixture of synthetic triglycerides. 2 Normative references T
42、he 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 (including any amendments) applies. EN 13130-1:2004, Materials and articles in contact
43、 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 and the selection of conditions of exposure to food simulants. 3 Principle HMTA
44、is treated with acid and heated to release formaldehyde. Formaldehyde in food simulant is determined by spectrophotometry. Formaldehyde reacts with chromotropic acid in the presence of sulfuric acid. This solution is measured in a spectrophotometer at the wavelength of 574 nm, with cells of an optic
45、al path length of 10 mm. Quantification is achieved using an external standard. Confirmation of formaldehyde is carried out by spectrophotometer. Formaldehyde reacts with pentane-2,4-dione in the presence of ammonium acetate to form 3,5-diacetyl-1,4-dihydrolutidine. The absorption of this extract is
46、 measured at 410 nm, with a spectrophotometer with cells of an optical path length of 10 mm. NOTE The confirmation procedure is also a quantitative method and can therefore be used as the method of determination. In that case the method with chromotropic acid should be used as the confirmation proce
47、dure. 4 Reagents NOTE All reagents should be of recognized analytical quality unless otherwise stated. 4.1 Analyte Formaldehyde solution, CH2O, minimum 37 % (w/v), stabilized with approximately 10 % methanol. DD CEN/TS 13130-23:20057 4.2 Chemicals 4.2.1 Water, deionised. 4.2.2 Acetic acid, glacial 1
48、00 %. 4.2.3 Ethanol, absolute. 4.2.4 Olive oil, rectified (according to Directive 93/8/EEC) 4.2.5 Chromotropic acid disodium salt (dihydrate), 4,5-dihydroxy-2,7-naphthalene-disulfonic acid, C10H6Na2O8S2.2H2O. 4.2.6 Sulfuric acid, density 1,84 g/cm3. 4.2.7 Acetone 4.2.8 Starch, soluble 4.2.9 n-pentan
49、e 4.3 Solutions 4.3.1 90 % Acetone Measure 900 ml of acetone (4.2.7) and make up with water (4.2.1) to 1 000 ml. 4.3.2 Stock solution of formaldehyde in water containing approximately 1,5 mg formaldehyde per millilitre Weigh to the nearest 1 mg approximately 0,8 g formaldehyde solution (4.1.1) into a 200 ml volumetric flask and make up to the mark with water (4.2.1). Determine the strength of this solution as follows. Pipette 10,0 ml formaldehyde stock solution into a beaker, add 25,0 ml of a 0,05 mol standard iodine solution (4.3.5) and 10,0 ml of
