1、BRITISH STANDARD BS EN 13130-2:2004 Materials and articles in contact with foodstuffs Plastics substances subject to limitation Part 2: Determination of terephthalic acid in food simulants The European Standard EN 13130-2:2004 has the status of a British Standard ICS 67.250 BS EN 13130-2:2004 This B
2、ritish Standard was published under the authority of the Standards Policy and Strategy Committee on 16 June 2004 BSI 16 June 2004 ISBN 0 580 43932 1 National foreword This British Standard is the official English language version of EN 13130-2:2004. It supersedes DD ENV 13130-2:1999 which is withdra
3、wn. The UK participation in its preparation was entrusted by Technical Committee CW/47, Materials and articles in contact with foodstuffs, to Subcommittee CW/47/1, Migration from plastics, which has the responsibility to: A list of organizations represented on this subcommittee can be obtained on re
4、quest to its secretary. Cross-references The 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
5、 Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirer
6、s to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This documen
7、t comprises a front cover, an inside front cover, the EN 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 publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENO
8、RM EN131302 May2004 ICS67.250 Englishversion MaterialsandarticlesincontactwithfoodstuffsPlastics substancessubjecttolimitationPart2:Determinationof terephthalicacidinfoodsimulants Matriauxetobjetsencontactaveclesdenres alimentairesSubstancesdanslesmatiresplastiques soumisesdeslimitationsPartie2:Dter
9、minationde lacidetrphtaliquedanslessimulantsdaliments WerkstoffeundGegenstndeinKontaktmitLebensmitteln SubstanzeninKunststoffen,dieBeschrnkungen unterliegenTeil2:BestimmungvonTerephtalsurein Prflebensmitteln ThisEuropeanStandardwasapprovedbyCENon24March2004. CENmembersareboundtocomplywiththeCEN/CENE
10、LECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheCentralSecretariatortoanyCENmember. ThisEuropeanStandardexistsinth
11、reeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheCentralSecretariathasthesamestatusast heofficial versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,Cyprus,CzechRepublic,Denmark
12、,Estonia,Finland,France, Germany,Greece,Hungary,Iceland,Ireland,Italy,Latvia,Lithuania,Luxembourg,Malta,Netherlands,Norway,Poland,Portugal, Slovakia, Slovenia,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG Managem
13、entCentre:ruedeStassart,36B1050Brussels 2004CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN131302:2004:EEN 13130-2:2004 (E) 2 Contents Foreword3 1 Scope 6 2 Normative references 6 3 Principle6 4 Reagents.6 5 Apparatus .7 6 Samples 8 7 Procedure .8
14、7.1 Preparation of standards 8 7.2 Preparation of calibration graphs 9 7.3 Validation of preparation of standard solutions.9 7.4 Suitability of orthophthalic acid as an internal standard 9 7.5 Extraction of olive oil simulant migration test samples 9 7.6 Preparation of aqueous simulant migration sam
15、ples10 7.7 Injection of samples 10 8 Expression of results 10 8.1 Method of calculation10 8.2 Precision.10 9 Confirmation of terephthalic acid 12 9.1 Requirement for confirmation 12 9.2 Re-analysis using an ion exchange column .12 9.3 Multi-wavelength measurements/diode array spectra analysis .12 10
16、 Test report 13 Annex A (normative) Reagents for confirmation of terephthalic acid14 A.1 Reagents for confirmation of terephthalic acid14 Bibliography 15 EN 13130-2:2004 (E) 3 Foreword This document (EN 13130-2:2004) has been prepared by Technical Committee CEN/TC 194 “Utensils in contact with food”
17、, the secretariat of which is held by BSI. This document was prepared by Subcommittee SC1 of TC 194 as one of a series of analytical test methods for plastics materials and articles in contact with foodstuffs. This European Standard shall be given the status of a national standard, either by publica
18、tion of an identical text or by endorsement, at the latest by November 2004, and conflicting national standards shall be withdrawn at the latest by November 2004. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. This sta
19、ndard 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 Union legislation relating to plastics materials and articles intended to
20、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 recommended that users of this standard refer to the latest relevant published
21、 Directive(s) before commencement of a test or tests described in this standard. EN 13130-2 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 prepa
22、red, 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 plastics. The other parts of EN 13130 are as follows. Part 1: Guide to test methods for th
23、e 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 3: Determination of acrylonitrile in food and food simulants Part 4: Determination of 1,3-butadiene in plast
24、ics 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 plastics Part 9: Determination of acetic acid, viny
25、l ester in food simulants Part 10: Determination of acrylamide in food simulants Part 11: Determination of 11-aminoundecanoic acid in food simulants EN 13130-2:2004 (E) 4 Part 12: Determination of 1,3-benzenedimethanamine in food simulants Part 13: Determination of 2,2-bis(4-hydroxyphenyl)propane (B
26、isphenol 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: Determination of carbonyl chloride in
27、 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 epichlorohydrin in plastics Part 21
28、: 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 maleic anhydride in foo
29、d 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-trimethylopropane in food simulants Parts 1 to 8
30、are European Standards. Parts 9 to 28 are Technical Specifications, prepared within the Standards, Measurement and Testing project, MAT1-CT92-0006, “Development of Methods of Analysis for Monomers”. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the follow
31、ing countries are bound to implement this European Standard: 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,
32、 Switzerland and United Kingdom. EN 13130-2:2004 (E) 5 Introduction Terephthalic acid (TA) is a comonomer used in the manufacture of polyester plastics. Residues of terephthalic acid can be present in the plastics after processing to form materials and articles intended to come into contact with foo
33、dstuffs. When these plastics are in contact with foodstuffs, the residual terephthalic acid monomer can migrate into the foodstuff. EN 13130-2:2004 (E) 6 1 Scope This part of this European Standard specifies methods for the determination of the monomer terephthalic acid in food simulants; distilled
34、water, 3 % (w/v) acetic acid aqueous solution, 15 % (v/v) ethanol aqueous solution and olive oil and other fatty food simulants, simulants D, e.g. a mixture of synthetic triglycerides or sunflower oil or corn oil. The methods are capable of determining terephthalic acid in the food simulants at the
35、level of the specific migration limit of 7,5 mg of terephthalic acid per kilogram of food simulants. NOTE This method was developed for the determination of terephthalic acid in 15 % (v/v) aqueous ethanol, as required by the regulations in force at the time the development work was carried out. Howe
36、ver, this method, developed for 15 (v/v) aqueous ethanol, should be applicable to the determination in 10 (v/v) aqueous ethanol. 2 Normative references This European Standard incorporates by dated or undated reference, provisions from other publications. These normative references are cited at the a
37、ppropriate places in the text, and the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in it by amendment or revision. For undated references the latest edition of the p
38、ublication referred to applies (including amendments). 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 determinati
39、on of substances in plastics and the selection of conditions of exposure to food simulants EN ISO 1042; Laboratory glassware One-mark volumetric flasks (ISO 1042:1998). ISO 385 (all parts); Laboratory glassware Burettes. ISO 648; Laboratory glassware One-mark pipettes. ISO 835 (all parts); Laborator
40、y glassware Graduated pipettes. ISO 4788, Laboratory glassware Graduated measuring cylinders. 3 Principle The aqueous simulant test samples are directly analysed by high performance liquid chromatography (HPLC) with ultraviolet (UV) detection. The olive oil test samples are extracted with dilute sod
41、ium hydrogen carbonate and the resultant aqueous solution is acidified and analysed by HPLC. 4 Reagents WARNING: All chemicals are hazardous to health to a greater or lesser extent. It is beyond the scope of this standard to give instructions for the safe handling of all chemicals, that meet, in ful
42、l, the legal obligations in all countries in which this standard can be followed. Therefore, specific warnings are not given and users of this standard shall ensure that they meet all the necessary safety requirements in their own country. NOTE During the analysis, unless otherwise stated, only reag
43、ents of recognized analytical grade and only distilled water of equivalent purity should be used. EN 13130-2:2004 (E) 7 4.1 Methanol (HPLC grade). 4.2 Sodium acetate, trihydrate. 4.3 Orthophthalic acid. 4.4 Terephthalic acid. 4.5 Orthophosphoric acid 85 % (w/v). 4.6 Water (HPLC grade). 4.7 Sodium hy
44、drogen carbonate solution 0,1 % (w/v). 4.8 Acetic acid, 50 % (v/v) in water. 4.9 Propan-2-ol. 4.10 Heptane. 4.11 pH 3,6 buffer solution. Dissolve 25,0 g of sodium acetate, trihydrate in 350 ml of water, add 5,0 ml 0,1 ml of orthophosphoric acid and adjust to pH (3,6 0,2) with glacial acetic acid (ap
45、proximately 50 ml). Make up to 500 ml with water. 4.12 Weigh accurately about 0,05 g terephthalic acid and, by continuous stirring, dissolve in about 90 ml of methanol. Make up to 100 ml with methanol in a volumetric flask. Prepare a second terephthalic acid standard stock solution for validation pu
46、rposes, see 7.3. NOTE The solution can be warmed to 50 C to facilitate dissolution of the terephthalic acid, which takes at least 1 h. 4.13 Orthophthalic acid internal standard stock solution. Weigh about 0,1 g of orthophthalic acid and dissolve in propan-2-ol. Make up to 100 ml with propan-2-ol in
47、a volumetric flask. 4.14 Mobile phase for high performance liquid chromatography. Using a measuring cylinder add 150 ml of methanol to 150 ml of pH 3,6 buffer and dilute to 1 l with water. NOTE Degassing the mobile phase can be necessary with some HPLC equipment. 5 Apparatus 5.1 Analytical balance c
48、apable of weighing accurately to 0,1 mg. 5.2 pH meter with an accuracy of pH 0,1. 5.3 Volumetric flasks, of 25 ml, 50 ml and 100 ml capacity, conforming to the minimum requirements of EN ISO 1042. 5.4 Measuring cylinders, of 5 ml, 25 ml, 50 ml, 100 ml and 250 ml capacity, conforming to the minimum requirements of ISO 4788. 5.5 Pipettes, of 5 ml and 50 ml capacity, conforming to the minimum requirements of ISO 648. 5.6 Graduated pipette, of 2 ml capacity, conforming to the minimum requirements of
