1、DRAFT FOR DEVELOPMENTDD CEN/TS 13130-19:2005Materials and articles in contact with foodstuffs Plastics substances subject to limitation Part 19: Determination of dimethylaminoethanol in food simulantsICS 67.250g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g
2、50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58DD CEN/TS 13130-19:2005This 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 46062
3、2National forewordThis Draft for Development is the official English language version of CEN/TS 13130-19:2005.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
4、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 Develop
5、ment 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 the
6、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 a Eu
7、ropean 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 clause
8、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 may
9、 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. Users ar
10、e 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 public
11、ationAmd. No. Date CommentsTECHNICAL SPECIFICATIONSPCIFICATION TECHNIQUETECHNISCHE SPEZIFIKATIONCEN/TS 13130-19February 2005ICS 67.250English versionMaterials and articles in contact with foodstuffs - Plasticssubstances subject to limitation - Part 19: Determination ofdimethylaminoethanol in food si
12、mulantsMatriaux et objets en contact avec les denresalimentaires - Substances dans les matires plastiquessoumises des limitations - Partie 19 : Dtermination dudimthylaminothanol dans les simulants dalimentsWerkstoffe und Gegenstnde in Kontakt mit Lebensmitteln- Substanzen in Kunststoffen, die Beschr
13、nkungenunterliegen - Teil 19: Bestimmung vonDimethylaminoethanol 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 the members of CEN
14、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 level in an appropr
15、iate 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 Republic, Denmark, Eston
16、ia, 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 NORMALISATIONEUROPISCHES KOMITEE
17、 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 13130-19:2005: E2 Contents page Foreword. 3 Introduction 5 1 Scope 6 2 Normative references . 6 3 Principle .
18、6 4 Reagents 7 5 Apparatus 8 6 Samples . 9 7 Procedure 11 8 Precision 13 9 Confirmation 13 10 Test report . 14 Bibliography . 15 DD CEN/TS 13130-19:20053 Foreword This document (CEN/TS 13130-19:2005) has been prepared by Technical Committee CEN/TC 194 “Utensils in contact with food”, the secretariat
19、 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 series of test
20、 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. At the time of preparation and publication of this part of EN 13130 the Eu
21、ropean 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 legislative requirements which this standard supports. It is therefore strong
22、ly 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 13130-1. Further parts of EN 13130, under the general title Materials and arti
23、cles 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 determination of specific monomers and additives i
24、n 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 food simulants Part 2: Determination of te
25、rephthalic 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 mono
26、ethylene 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
27、 12: Determination of 1,3-benzenedimethanamine in food simulants DD CEN/TS 13130-19:20054 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-b
28、utadiene 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 4,4dihydroxybiphen
29、yl 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 Part 22: Determination of ethylene oxide and propylene oxide in plastics Pa
30、rt 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 26: Determination of 1-octene and tetrahydrofuran in food simulants Part 27
31、: 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 All chemicals are hazardous to health to a greater or lesser extent. It is
32、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 this Technical Speci
33、fication 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
34、 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 13130-19:20055 Introduction Dimethylaminoethanol
35、(DMAE), C4H11NO, PM/Ref. No 16150, is a monomer used in the manufacture of certain plastics materials and articles intended to come into contact with foodstuffs. After manufacture residual dimethylaminoethanol can remain in the finished product and may migrate into foodstuffs coming into contact wit
36、h that product. The method has been pre-validated by collaborative trial with two laboratories using food simulants. DD CEN/TS 13130-19:20056 1 Scope This document, part of EN 13130, specifies an analytical procedure for the determination of dimethylaminoethanol in food simulants: distilled water, 3
37、 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and rectified olive oil. The method is appropriate for the quantitative determination of dimethylaminoethanol in an approximate analyte concentration range of 3,4 mg/kg to 36 mg per kilogram of food simulant. NOTE The method should also be applica
38、ble to other aqueous food simulants as well as to other fatty food simulants e.g. sunflower oil and 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 app
39、lies. 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 of substances from pla
40、stics to foods and food simulants and the determination of substances in plastics and the selection of conditions of exposure to food simulants. 3 Principle Dimethylaminoethanol (DMAE) is extracted from the food simulants by means of solid phase extraction on a strong cation exchanger. The absorbed
41、DMAE is removed from the absorbent with triethylamine and the resulting solution is submitted to gas chromatography to determine the amount of DMAE in the simulants. For quantification purposes an internal standard is added. Calibration is achieved by analysis of relevant simulants containing known
42、amounts of DMAE. Confirmation of dimethylaminoethanol is established by combined gas chromatography/mass spectrometry. DD CEN/TS 13130-19:20057 4 Reagents NOTE All reagents should be of recognized analytical quality unless otherwise stated. 4.1 Analytes 4.1.1 Dimethylaminoethanol (DMAE), N,N-dimethy
43、lethanol-amine, C4H11NO or (CH3)2NCH2CH2OH molecular weight 89,14; boiling point 134 C; density: 0,886 6 g per millilitre, purity: 99 % (GC). 4.1.2 Diethylaminoethanol (DEAE), (N,N-diethyl-ethanolamine) C6H15NO or (C2H5)2NCH2CH2OH Molecular weight 117,19; boiling point 163 C; density: 0,8921 g per m
44、illilitre, purity: 99 % (GC). 4.2 Chemicals 4.2.1 Water, deionized or HPLC grade. 4.2.2 Acetic acid, 100 %. 4.2.3 Methanol, HPLC grade. 4.2.4 Isopropanol, HPLC grade. 4.2.5 n-Pentane, 95 %. 4.2.6 Triethylamine, 99 %, GC. 4.3 Solid phase extraction cartridges, loaded with 100 mg of a strong cation ex
45、changer (propylsulfonic acid) and a volume of 3 ml. 4.4 Solutions 4.4.1 Triethylamine in methanol, 5 % (v/v) Measure 2,0 ml triethylamine (4.2.6) and add methanol to a final volume of 50 ml in a volumetric flask. 4.4.2 Standard stock solution of DMAE in isopropanol at a defined concentration of appr
46、oximately 2,22 g/l Pipette exactly 0,250 ml or weigh accurately approximately 222 mg of DMAE (4.1.1) into a 100 ml volumetric flask and fill to the mark with isopropanol. Calculate the exact concentration of DMAE in milligrams per millilitre using the specific mass of DMAE or the actual mass taken.
47、Repeat the procedure to obtain a second standard stock solution. NOTE The stock solutions can be stored in a well closed containers in the dark for a maximum period of three months at any temperature between - 20 C and + 20 C. DD CEN/TS 13130-19:20058 4.4.3 Internal standard stock solution of diethy
48、laminoethanol (DEAE) in isopropanol at a defined concentration of approximately 2,22 g/l Pipette exactly 0,250 ml or weigh accurately approximately 222 mg of DEAE (4.1.2) into a 100 ml volumetric flask and fill to the mark with isopropanol. Calculate the exact concentration of DEAE in mg/ml using th
49、e specific mass of DEAE or the actual mass taken. NOTE The stock solutions can be stored in a well closed container in dark for a maximum period of three months at any temperature between - 20 C and + 20 C. 4.4.4 Diluted standard solution of DMAE in isopropanol (0,22 mg/ml) Pipette 2,5 ml of the DMAE standard stock solution 4.4.2 into a 25 ml volumetric flask and fill to the mark with isopropanol. This solution contains approximately 222 g DMAE per millilitre of isopropanol. Calculate the exact concentration of DMAE in micrograms per millilitre o
