SIST EN 14481:2003

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Kunstoffe - Prüfverfahren zur Bestimmung des fettigen KontaktesMatériaux et articles en contact avec les denrées alimentaires - Plastiques - Méthodes d'essai pour la détermination d'un contact grasMaterials and articles in contact with foodstuffs - Plastics - Test methods for the determination of fatty contact83.080.01Polimerni materiali na splošnoPlastics in general67.250Materiali in predmeti v stiku z živiliMaterials and articles in contact with foodstuffsICS:Ta slovenski standard je istoveten z:EN 14481:2003SIST EN 14481:2003en01-september-2003SIST EN 14481:2003SLOVENSKI
STANDARD



SIST EN 14481:2003



EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 14481May 2003ICS 67.250; 83.080.01English versionMaterials and articles in contact with foodstuffs - Plastics - Testmethods for the determination of fatty contactMatériaux et articles en contact avec les denréesalimentaires - Plastiques - Méthodes d'essai pour ladétermination d'un contact grasWerkstoffe und Gegenstände in Kontakt mit Lebensmitteln- Kunstoffe - Prüfverfahren zur Bestimmung des fettigenKontaktesThis European Standard was approved by CEN on 9 January 2003.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Management Centre or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and UnitedKingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2003 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14481:2003 ESIST EN 14481:2003



EN 14481:2003 (E)2ContentsPageForeword.31Scope.52Principle.53Reagents.54Apparatus.55Preparation of standards and samples.65.1Preparation of standards.65.1.1Stock solution of DPBD at 1mg/ml.61.1.2Working standard solution of DPBD in n-hexane at 1 g/ml.61.1.3Stock solution of DPHT at 1mg/ml.61.1.4Calibration solution of DPHT in n-hexane at 100 g/ml.61.2Preparation of samples.76HPLC analysis.86.1Calibration standards.81.2Analysis.81.3Calibration graph.81.4Check for analytical bias.87Expression of results.97.1Method of calculation.97.2Interpretation.107.3Performance of the method.108Test report.10Annex A (informative)
Typical HPLC chromatogram for standard 1,4-diphenyl-1,3-butadiene and 1,6-diphenyl-1,3,5-hexatriene.11Annex ZA (informative)
Relationship of this European Standard with Council Directive 85/572/EEC.12Bibliography.13SIST EN 14481:2003



EN 14481:2003 (E)3ForewordThis document (EN 14481:2003) has been prepared by Technical Committee CEN /TC 194 "Utensils in contactwith food", the secretariat of which is held by BSI.This European Standard shall be given the status of a national standard, either by publication of an identical text orby endorsement, at the latest by November 2003, and conflicting national standards shall be withdrawn at the latestby November 2003.This document has been prepared under a mandate given to CEN by the European Commission and the EuropeanFree Trade Association.This European Standard contains an informative Annex A.According to the CEN/CENELEC Internal Regulations, the national standards organizations of the followingcountries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal,Slovakia, Spain, Sweden, Switzerland and the United Kingdom.SIST EN 14481:2003



EN 14481:2003 (E)4IntroductionFor certain specified food types, if it can be demonstrated, by means of an appropriate test, that there is no 'fattycontact' with the plastic, the migration test with simulant D (olive oil or alternatives) may be dispensed with.
Themethod described here can be used to determine whether a food makes fatty contact with plastics.NOTE 1The food types are specified in Council Directive 85/572/EEC [1].NOTE 2Guidance on the selection of conditions and test methods for overall migration, and the test methods for the specificmigration of substances from plastics into food and food simulants and the determination of substances in plastics and theselection of conditions of exposure to food simulants is given in EN 1186-1 and EN 13130-1 respectivelySIST EN 14481:2003



EN 14481:2003 (E)51 ScopeThis Part of this European Standard specifies a test method to determine whether there is fatty contact and isapplicable to all foods.
Testing some foods can require modifications to the method.
The method is applicable tocontact situations from -20 °C to 100 °C.2 PrincipleFatty contact between a food and a plastic material or article is determined by placing food in contact with apolyethylene film containing a fat-soluble fluorescent dye.
After exposure, the dye is extracted from the food anddetermined by high performance liquid chromatography (HPLC) with fluorescence detection.
The method employs1,6-diphenyl-1,3,5-hexatriene as internal standard.
The degree of transfer is related to the extent of fatty contactmade, and is used to determine whether simulant D be employed or not in subsequent tests of plastics intended tocome into contact with that food.The food used in the test should be the same as, or similar in composition to, the food which will come into contactwith the plastic in actual use.
To allow for possible difficulties encountered in obtaining reproducible film to foodcontact, the test is carried out on five replicate samples of the food.3 ReagentsAll reagents shall be of recognised analytical quality, unless otherwise specified.3.1Low density polyethylene film containing 1,4-diphenyl-1,3-butadiene, fluorescent dye, at 17,3 g/dm2 0,9g/dm2, in the form of a lay-flat tube of width 20 cm, e.g. the certified reference material BCR.593, Plastic film E,certified on the basis of the mass fraction of DPBD (12,58 mg/kg ± 0,63 mg/kg) and on the film thickness (149,7 µm± 0,7 µm).3.21,4-diphenyl-1,3-butadiene (DPBD)3.31,6-diphenyl-1,3,5-hexatriene (DPHT)NOTEAs DPBD and DPHT are slightly light sensitive, the film and standards should be stored with the exclusion of light.3.4n-Hexane, C6H14, HPLC gradeNOTEAs n-hexane is considered to be harmful by inhalation, ingestion and through skin contact, correct safety proceduresshould be followed at all times when using this solvent.3.5Dichloromethane, CH2Cl2, HPLC gradeNOTEAs dichloromethane is considered to be harmful by inhalation, ingestion and through skin contact and as a potentialcarcinogen, correct safety procedures should be followed at all times when using this solvent.4 Apparatus4.1Heat sealer suitable for sealing the polyethylene film (3.1)4.2Dispersion homogenizer4.3Centrifuge, bench-top4.4Centrifuge tubes, 10 ml to 20 ml capacity4.5Filter paper, 15,0 cm diameter circles, Whatman Grade 2 or equivalent4.6Volumetric flasks, 25 ml, 50 ml and 100 ml capacitySIST EN 14481:2003



EN 14481:2003 (E)64.7Glass vials, 2 ml and 20 ml capacity with screw or crimp cap closures and polytetrafluoroethylene (PTFE)lined sealing disks4.8Pasteur pipettes4.9Syringes, glass-barrelled, with needles, 50 l, 100 l, 500 l, 1 ml, 2,5 ml and 10 ml capacity4.10Filter funnels, glass4.11HPLC equipmentNOTEWith a 20 l injection loop and a pumping system capable of generating a gradient at 0,5 ml/min of n-hexane (heldfor 7 min) switched to dichloromethane over 1min (held for 5 min), returned to n-hexane over 1 min and then equilibrated for6 min.4.11.1Fluorescence detector, with excitation wavelength of 346 nm and emission wavelength of 374 nm andlinked to a chromatographic recorder and integrator4.11.2HPLC columnNOTEThe following column has been found suitable. Stainless steel, 100 mm x 3 mm internal diameter, silica, 5mparticle size.4.12Vacuum line with attached needle4.13Beakers, glass, tall form, 400 ml capacity4.14Thermostatically controlled cabinet(s) capable of maintaining a temperature of -20 °C ± 2 °C, 5 °C ± 1 °C,25 °C ± 1 °C and 70 °C ± 2 °C.4.15Food processor4.16Volumetric glass pipette, 5 ml capacity5 Preparation of standards and samples5.1 Preparation of standards5.1.1 Stock solution of DPBD at 1mg/mlWeigh 0,050 g 0,001 g of DPBD (3.2) into a 50 ml volumetric flask and make to the mark with n-hexane (3.4).5.1.2 Working standard solution of DPBD in n-hexane at 1 g/mlPlace approximately 50 ml of n-hexane into a 100 ml volumetric flask.
Add, by syringe, 100 l of the stock solution(5.1.1).
Make to the mark with n-hexane.5.1.3 Stock solution of DPHT at 1mg/mlWeigh 0,050 g
0,001 g of DPHT (3.3) into a 50 ml volumetric flask and make to the mark with dichloromethane(3.5).5.1.4 Calibration solution of DPHT in n-hexane at 100 g/mlPlace approximately 30 ml of n-hexane into a 50 ml volumetric flask.
Add, by pipette (4.16), 5 ml of the stocksolution (5.1.3).
Make to the mark with n-hexane.NOTEAs DPBD and DPHT are sensitive to light, standard solutions should be stored with the exclusion of light.SIST EN 14481:2003



EN 14481:2003 (E)75.2 Preparation of samples5.2.1The reference film is
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