1、DRAFT FOR DEVELOPMENT DD CEN/TS 13130-15:2005 Materials and articles in contact with foodstuffs Plastics substances subject to limitation Part 15: Determination of 1,3-butadiene in food simulants ICS 67.250 DD CEN/TS 13130-15:2005 This Draft for Development was published under the authority of the S
2、tandards Policy and Strategy Committee on 16 September 2005 BSI 16 September 2005 ISBN 0 580 46070 3 National foreword This Draft for Development is the official English language version of CEN/TS 13130-15:2005. This publication is not to be regarded as a British Standard. It is being issued in the
3、Draft for Development series of publications and is of a provisional nature because 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 experien
4、ce of its practical application may be obtained. Comments arising from the use of this 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
5、after its publication by the European organization so that a decision can be taken on 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
6、 the review period, the responsible BSI Committee will decide whether to support the conversion 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
7、British Standards House, 389 Chiswick High Road, London W4 4AL, giving the document reference 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-references T
8、he British Standards which implement international or European publications referred to in 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 Standa
9、rds Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Summary of pages This document comprises a front cover, an inside front cover, the CEN/TS title page, pages 2 to 15 and a back cover. The BSI copyri
10、ght notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsTECHNICALSPECIFICATION SPCIFICATIONTECHNIQUE TECHNISCHESPEZIFIKATION CEN/TS1313015 February2005 ICS67.250 Englishversion Materialsandarticlesincontactwithfoods
11、tuffsPlastics substancessubjecttolimitationPart15:Determinationof1,3 butadieneinfoodsimulants Matriauxetobjetsencontactaveclesdenres alimentairesSubstancesdanslesmatiresplastiques soumisesdeslimitationsPartie15:Dterminationdu 1,3butadinedanslessimulantsdaliments WerkstoffeundGegenstndeinKontaktmitLe
12、bensmitteln SubstanzeninKunststoffen,dieBeschrnkungen unterliegenTeil15:Bestimmungvon1,3Butadienin Prflebensmitteln ThisTechnicalSpecification(CEN/TS)wasapprovedbyCENon16December2004forprovisionalapplication. TheperiodofvalidityofthisCEN/TSislimitedinitiallytothreeyears.AftertwoyearsthemembersofCENw
13、illberequested tosubmittheir comments,particularlyonthequestionwhethertheCEN/TScanbeconvertedintoaEuropeanStandard. CENmembersarerequiredtoannouncetheexistenceofthisCEN/TSinthesamewayasforanENandtomaketheCEN/TSavailable promptlyatnationallevelinanappropriateform.Itispermissibletokeepconflictingnatio
14、nalstandardsinforce(inparall eltotheCEN/TS) untilthefinaldecisionaboutthepossibleconversionoftheCEN/TSintoanENisreached. CENmembersarethenationalstandardsbodiesofAustria,Belgium,Cyprus,CzechRepublic,Denmark,Estonia,Finland,France, Germany,Greece,Hungary,Iceland,Ireland,Italy,Latvia,Lithuania,Luxembo
15、urg,Malta,Netherlands,Norway,Poland,Portugal, Slovakia, Slovenia,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2005CEN Allrightsofexploitationinanyformandbyanymeansr
16、eserved worldwideforCENnationalMembers. Ref.No.CEN/TS1313015:2005:EDD CEN/TS 13130-15:2005 2 Contents page Foreword. 3 Introduction 5 1 Scope 6 2 Normative references . 6 3 Principle . 6 4 Reagents 7 5 Apparatus 9 6 Samples . 10 7 Procedure 11 8 Expression of results 12 9 Confirmation 13 10 Test rep
17、ort . 14 Bibliography . 15 DD CEN/TS 13130-15:2005 3 Foreword This document (CEN/TS 13130-15:2005) has been prepared by 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 a
18、nd 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 for plastics materials and articles in contact with foodstuffs. This standard is intended to
19、 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 Union legislation relating to plastics materials and articles intended to come into contact wi
20、th 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 standard refer to the latest relevant published Directive(s) before
21、 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 contact with foodstuffs - Plastics substances subject to limitation, have been prepared, and
22、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 plastics. The parts of EN 13130 are as follows. Part 1: Guide to test methods for the specific migr
23、ation 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 terephthalic acid in food simulants Part 3: Determination of acrylonitrile in food and food simulants P
24、art 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 glycol and diethylene glycol in food simulants Part 8: Determination of isocyanates in plast
25、ics 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: Determination of 1,3-benzenedimethanamine in food simulants 4 Part 13: Determination of 2,2-bis(
26、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 in food simulants Part 16: Determination of caprolactam and caprolactam salt in food simulants Part 17: Determinati
27、on 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 food simulants Part 19: Determination of dimethylaminoethanol in food simulants Part 20: Determination of epichlorohyd
28、rin 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: Determination of formaldehyde and hexamethylenetetramine in food simulants Part 24: Determination of maleic acid and
29、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: Determination of 2,4,6-triamino-1,3,5-triazine in food simulants Part 28: Determination of 1,1,1-trimethylolpropane in foo
30、d 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 the scope of this Technical Specification to give instructions for the safe handling of all chemicals, that meet, in
31、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 should ensure that they meet all the necessary safety requirements in their own country. According to the CEN/CENEL
32、EC Internal Regulations, the national standards organizations of the following countries are bound to announce this CEN Technical Specification: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembou
33、rg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. DD CEN/TS 13130-15:2005 5 Introduction 1,3-butadiene, C 4 H 6or CH 2 =CH-CH=CH 2 , PM/Ref. No 13630, is a monomer used in the manufacture of certain plastics materials and articles in
34、tended to come into contact with foodstuffs. After manufacture, residual butadiene monomer can remain in the polymer and may migrate into foodstuffs coming into contact with that plastics article. NOTE However, the following should be taken into account when carrying out a migration test: From migra
35、tion experiments carried out at 10 d for 40 C it was recognized that a considerable non-reproducible loss of up to 90 %, due to volatilization of 1,3-butadiene can be obtained when using aqueous food simulants. The method has been pre-validated by a collaborative trial with three laboratories. DD CE
36、N/TS 13130-15:20056 1 Scope This document, part of EN 13130, specifies an analytical procedure for the determination of butadiene monomer in the food simulants water, 3 % w/v aqueous acetic acid, 15 % v/v aqueous ethanol and olive oil. The level of butadiene monomer determined is expressed as mg but
37、adiene/kg of food. The method is appropriate for the quantitative determination of butadiene at a range of 0,01 mg/kg to 0,1 mg/kg in food simulants. NOTE The method should also be applicable to other aqueous food simulants and to the other fatty food simulants such as sunflower oil and a mixture of
38、 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. For undated references, the latest edition of the referenced document (including any amendments) applies.
39、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 and the selection of condition
40、s of exposure to food simulants. 3 Principle The level of butadiene in a food or a food simulant is determined by headspace gas chromatography (HSGC) with automated sample injection and using flame ionization detection (FID). Quantification is achieved using an internal standard (n-pentane) with cal
41、ibration against relevant food simulants samples fortified with known amounts of butadiene. Confirmation of butadiene levels is carried out by combined gas chromatography/mass spectrometry (GC/MS). DD CEN/TS 13130-15:2005 7 4 Reagents NOTE All reagents should be of recognized analytical quality unle
42、ss otherwise stated. 4.1 Analytes 4.1.1 1,3-butadiene, CH 2 =CH-CH=CH 2 , purity greater than 99,5 % (GC). 4.1.2 n-pentane, CH 3 -(CH 2 ) 3CH 3 , purity greater than 99,5 % (GC). 4.2 Chemicals 4.2.1 N,N-dimethylacetamide (DMAA), CH 3 -CO-N(CH 3 ) 2 , purity greater than 99,5 % (GC); density d T= 0,9
43、60 0 - (0,000 94 T), where T is temperature in C. 4.2.2 Purified nitrogen (purity 99,999 9 %). 4.3 Solutions 4.3.1 Stock solutions of butadiene in DMAA with defined concentrations of approximately 5mg/g Weigh a 50 ml sample vial (5.4), including septum and cap, to an accuracy of 1,0 mg. Pipette 50 m
44、l DMAA (4.2.1) into the vial (5.4), close and weigh again to 1,0 mg. Insert hollow needles equipped with miniature two-way valves for introducing butadiene and for venting air and weigh again to an accuracy of 1,0 mg. Introduce, under a fume hood, approximately 0,25 g butadiene (4.1.1) by bubbling t
45、hrough the DMAA with the valves in the open position. Re-weigh the vial plus needles to an accuracy of 1,0 mg with the valves in the closed position and then remove the needles. NOTE 1 For safety reasons, the use of hollow needles with miniature two-way valves is recommended but not necessary. Alter
46、natively, two separate needles can be used. Calculate the concentration of butadiene in milligrams per gram of solution. Repeat the procedure to provide a second stock solution. NOTE 2 The stock solutions can be stored at 20 C up to 3 months protected from light in septum-capped glass vials with min
47、imum headspace; storage at + 4 C with the exclusion of light should not exceed one week. 4.3.2 Diluted stock solutions of butadiene in DMAA with a defined concentration of approximately 50 g butadiene per gram DMAA Weigh a 20 ml sample vial (5.4), including septum and cap, to an accuracy of 1,0 mg.
48、Pipette 18,0 ml of DMAA into the sample vial (5.4) and close the vial with the septum and cap. Weigh again to an accuracy of 1,0 mg. Insert 2,0 ml of the stock solution (4.3.1) through the septum using a syringe (5.5), mix thoroughly and re-weigh to an accuracy of 1,0 mg. Repeat this procedure taking the 1:10 diluted stock solution instead of the stock solution (4.3.1) to obtain then the required 50 g per gram diluted stock solution. Calculate the concentration of butadiene in the d
