1、BRITISH STANDARD BS EN 13130-7:2004 Materials and articles in contact with foodstuffs Plastics substances subject to limitation Part 7: Determination of monoethylene glycol and diethylene glycol in food simulants The European Standard EN 13130-7:2004 has the status of a British Standard ICS 67.250 B
2、S EN 13130-7:2004 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 21 June 2004 BSI 21 June 2004 ISBN 0 580 43967 4 National foreword This British Standard is the official English language version of EN 13130-7:2004. It supersedes DD ENV 13130
3、-7:1996 which is withdrawn. 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 subcommitt
4、ee can be obtained on request 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 “Sea
5、rch” 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 for its correct application. Compliance with a British Standard does not of itself confer immunity from legal o
6、bligations. aid enquirers 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. Summa
7、ry of pages This document comprises a front cover, an inside front cover, the EN 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 since publication Amd. No. Date Commen
8、tsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN131307 May2004 ICS67.250 Englishversion MaterialsandarticlesincontactwithfoodstuffsPlastics substancessubjecttolimitationPart7:Determinationof monoethyleneglycolanddiethyleneglycolinfoodsimulants Matriauxetobjetsencontactaveclesdenres alimentairesSu
9、bstancesdanslesmatiresplastiques soumisesdeslimitationsPartie7:Dterminationdu monothylneglycoletdudithylneglycoldansles simulantsdaliments WerkstoffeundGegenstndeinKontaktmitLebensmitteln SubstanzeninKunststoffen,dieBeschrnkungen unterliegenTeil7:BestimmungvonMonoethylenglykol undDiethylenglykolinLe
10、bensmittelSimulantien ThisEuropeanStandardwasapprovedbyCENon24March2004. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchn
11、ational standardsmaybeobtainedonapplicationtotheCentralSecretariatortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheCentralSecretariathasthesamest
12、atusast heofficial versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,Cyprus,CzechRepublic,Denmark,Estonia,Finland,France, Germany,Greece,Hungary,Iceland,Ireland,Italy,Latvia,Lithuania,Luxembourg,Malta,Netherlands,Norway,Poland,Portugal, Slovakia, Slovenia,Spain,Sweden,Switzerlandand
13、UnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2004CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN131307:2004:EEN 13130-7:2004 (E) 2 Contents
14、 page Foreword3 1 Scope 6 2 Normative references 6 3 Principle6 4 Reagents.6 5 Apparatus .7 6 Samples 8 7 Procedure .8 7.1 Preparation of standards 8 7.1.1 Intermediate standards .8 7.1.2 Internal standard, 800 mg/l butan-1,4-diol 8 7.1.3 Working standards for aqueous simulants.8 7.1.4 Working stand
15、ards for olive oil9 7.2 Preparation of calibration graphs 9 7.2.1 Injection of standards .9 7.2.2 Validation of stock monoethylene glycol/diethylene glycol solution 9 7.3 Extraction of olive oil simulant migration test samples 9 7.4 Preparation of aqueous simulant migration test samples 10 7.5 Injec
16、tion of samples 10 8 Expression of results 10 8.1 Method of calculation10 8.1.1 As milligrams of monoethylene glycol and diethylene glycol per kilogram of food simulant 10 8.1.2 As milligrams of monoethylene glycol and diethylene glycol per square decimetre of surface area of plastic material or art
17、icle10 8.1.3 Calculation of the specific migration.10 8.2 Precision.10 8.2.1 Validation10 8.2.2 Repeatability and reproducibility.11 8.2.3 Detection limit 12 9 Confirmation of monoethylene glycol and diethylene glycol .12 9.1 Requirement for confirmation 12 9.2 Confirmation by re-analysis using conf
18、irmed by gas chromatography - mass spectrometry 12 10 Test report 12 Annex A (informative) 14 Annex B (informative) 15 Bibliography 16 EN 13130-7:2004 (E) 3 Foreword This document (EN 13130-7:2004) has been prepared by Technical Committee CEN/TC 194 “Utensils in contact with food”, the secretariat o
19、f 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 publication of an identica
20、l 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 standard is intended t
21、o 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 w
22、ith 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) befor
23、e commencement of a test or tests described in this standard. EN 13130-7 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 others are
24、 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 the specific migratio
25、n 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 Part
26、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 8: Determination of isocyanates in plastics Part 9: Determination of acetic acid, vinyl ester in food simulants Part 10: Determin
27、ation 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 Part 13: Determination of 2,2-bis(4-hydroxyphenyl)propane (Bisphenol A) in food simulants Part 14: Determination of 3,3-bis(3
28、-methyl-4-hydroxyphenyl)-2-indoline in food simulants EN 13130-7:2004 (E) 4 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-dih
29、ydroxybenzene, 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: Determination of ethylenediamine and hexa
30、methylenediamine 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 food simulants Part 25: Determination of 4-met
31、hyl-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 are European Standards. Parts 9 to 28 are
32、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 following countries are bound to implement this
33、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, Switzerland and United Kingdom. EN 13130-
34、7:2004 (E) 5 Introduction Monoethylene glycol (MEG) and diethylene glycol (DEG) are monomers used in the manufacture of plastics materials and articles intended to come into contact with foodstuffs. Residues of monoethylene glycol and diethylene glycol can remain in the plastic after processing to f
35、orm materials and articles for food contact use, and can migrate into foodstuffs. NOTE Commission Directive 2002/72/EC lists a combined specific migration limit of 30 mg/kg (T) of monoethylene glycol and diethylene glycol in foods or food simulants. EN 13130-7:2004 (E) 6 1 Scope This part of this Eu
36、ropean Standard specifies methods for the determination of monoethylene glycol and diethylene glycol in the food simulants; water, 3 % (w/v) acetic acid, 15 % (v/v) ethanol and olive oil and other fatty food simulants, simulants D, e.g. a mixture of synthetic triglycerides or sunflower oil or corn o
37、il. The methods are capable of determining monoethylene glycol and diethylene glycol in food simulants separately, or combined, at the specific migration limit SML (T) of 30 mg/kg. NOTE This method was developed for the determination of monoethylene glycol and diethylene glycol in 15 % (v/v) aqueous
38、 ethanol, as required by the regulations in force at the time the development work was carried out. However, 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
39、 or undated reference, provisions from other publications. These normative references are cited at the appropriate 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 o
40、nly when incorporated in it by amendment or revision. For undated references the latest edition of the publication 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 method
41、s 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. EN ISO 1042; Laboratory glassware One-mark volumetric flasks (ISO 1042:1998). ISO 385 (all parts), Labor
42、atory glassware Burettes. ISO 835 (all parts); Laboratory glassware Graduated pipettes. ISO 4788, Laboratory glassware Graduated measuring cylinders. 3 Principle After addition of an internal standard the aqueous food simulants or the olive oil water extract is directly injected for gas chromatograp
43、hic analysis using a cold on-column injector. Detection limits are approximately 1 mg/kg in the food simulants. The concentrations of monoethylene glycol and diethylene glycol are measured by comparison of peak height or area ratios against standards. 4 Reagents WARNING: All chemicals are hazardous
44、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 full, the legal obligations in all countries in which this standard may be followed. Therefore, specific warnings are not given and users of thi
45、s standard shall ensure that they meet all the necessary safety requirements in their own country. 4.1 Methanol 4.2 Monoethylene glycol EN 13130-7:2004 (E) 7 4.3 Diethylene glycol 4.4 Butan-1,4-diol, internal standard 4.5 Water (HPLC or deionized) 4.6 Heptane 4.7 Prepare a monoethylene glycol and di
46、ethylene glycol standard stock solution as follows: Weigh accurately about 0,75 g each of monoethylene glycol and diethylene glycol into a beaker, dissolve in methanol and transfer with washings to a 100 ml volumetric flask. Dilute to the mark with methanol. This solution is stable for 1 month if st
47、ored in the dark at 5 C in a stopped flask. Prepare a second stock solution for validation purposes, see 7.2.2. 4.8 Prepare a butan-1,4-diol internal standard stock solution as follows: Weigh about 1 g of butan-1,4-diol into a beaker, dissolve in methanol and make up to 100 ml mark with methanol in
48、a volumetric flask. This solution is stable for 1 month if stored in the dark at 5 C in a stoppered flask. 5 Apparatus 5.1 Analytical balance capable of weighing to 0,1 mg. 5.2 Graduated pipettes, conforming to the minimum requirements of ISO 835 and of 1 ml and 2 ml capacity. 5.3 Burette, conforming to the minimum requirements of ISO 385 and of 25 ml capacity. 5.4 Volumetric flasks, conforming to the minimum requirements of EN ISO 1042 and of 25 ml, 50 ml and 100 ml capacity. 5.5 Separating funnels w
