SIST EN 1186-9:2002

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Materiali in predmeti v stiku z živili - Polimerni materiali - 9. del: Preskusne metode za celotno migracijo v modelno vodno raztopino, s katero je napolnjen predmetWerkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Kunststoffe - Teil 9: Prüfverfahren für die Gesamtmigration in wässrige Prüflebensmittel durch Füllen des GegenstandesMatériaux et objets en contact avec les denrées alimentaires - Matiere plastique - Partie 9: Méthodes d'essai pour la migration globale dans les simulants aqueux par remplissageMaterials and articles in contact with foodstuffs - Plastics - Part 9: Test methods for overall migration into aqueous food simulants by article filling67.250Materiali in predmeti v stiku z živiliMaterials and articles in contact with foodstuffsICS:Ta slovenski standard je istoveten z:EN 1186-9:2002SIST EN 1186-9:2002en01-september-2002SIST EN 1186-9:2002SLOVENSKI
STANDARDSIST ENV 1186-9:19971DGRPHãþD



SIST EN 1186-9:2002



EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 1186-9April 2002ICS 67.250Supersedes ENV 1186-9:1994English versionMaterials and articles in contact with foodstuffs - Plastics - Part9: Test methods for overall migration into aqueous foodsimulants by article fillingMatériaux et objets en contact avec les denréesalimentaires - Matière plastique - Partie 9: Méthodesd'essai pour la migration globale dans les liquidessimulateurs aqueux par remplissageWerkstoffe und Gegenstände in Kontakt mit Lebensmitteln- Kunststoffe - Teil 9: Prüfverfahren für dieGesamtmigration in wässrige Prüflebensmittel durch Füllendes GegenstandesThis European Standard was approved by CEN on 4 January 2002.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,Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2002 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 1186-9:2002 ESIST EN 1186-9:2002



EN 1186-9:2002 (E)2ContentspageForeword.31Scope.52Normative references.53Principle.54Reagents.55Apparatus.66Preparation of test specimens.67Procedure.78Expression of results.99Test report.11Annex A (informative)
Precision data.12Annex ZA (informative)
Relationship of this European Standard with Council Directive 89/109/EECand Commission Directive 90/128/EEC and associated Directives.13Bibliography.15SIST EN 1186-9:2002



EN 1186-9:2002 (E)3ForewordThis document EN 1186-9:2002 has been prepared by Technical Committee CEN/TC 194 “Utensils in contact withfood”, 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 October 2002, and conflicting national standards shall be withdrawn at the latestby October 2002.This document supersedes ENV 1186-9:1994.This European Standard is one of a series of methods of test for plastics materials and articles in contact withfoodstuffs.This document has been prepared under a mandate given to CEN by the European Commission and the EuropeanFree Trade Association, and supports essential requirements of EC Directive(s).For relationship with EC Directive(s), see informative annex ZA, which is an integral part of this document.At the time of preparation and publication of this standard the European Union legislation relating to plasticsmaterials and articles intended to come into contact with foodstuffs is incomplete.
Further Directives andamendments to existing Directives are expected which could change the legislative requirements which thisstandard supports. It is therefore strongly recommended that users of this standard refer to the latest relevantpublished Directive(s) before commencement of any of the test or tests described in this standard.EN 1186-9 should be read in conjunction with EN 1186-1.Further Parts of this standard have been prepared, and others are in preparation, concerned with the determinationof overall migration from plastics materials into food simulants.
Their titles are as follows:EN 1186 Materials and articles in contact with foodstuffs - Plastics –Part 1Guide to the selection of conditions and test methods for overall migrationPart 2Test methods for overall migration into olive oil by total immersionPart 3Test methods for overall migration into aqueous food simulants by total immersionPart 4Test methods for overall migration into olive oil by cellPart 5Test methods for overall migration into aqueous food simulants by cellPart Test methods for overall migration into olive oil using a pouchPart 7Test methods for overall migration into aqueous food simulants using a pouchPart 8Test methods for overall migration into olive oil by article fillingPart 10Test methods for overall migration into olive oil (modified method for use in cases whereincomplete extraction of olive oil occurs)Part 11Test methods for overall migration into mixtures of 14C-labelled synthetic triglyceridePart 12Test methods for overall migration at low temperaturesSIST EN 1186-9:2002



EN 1186-9:2002 (E)4Part 13Test methods for overall migration at high temperaturesPart 14Test methods for 'substitute tests' for overall migration from plastics intended to come intocontact with fatty foodstuffs using test media iso-octane and 95 % ethanolPart 15Alternative test methods to migration into fatty food simulants by rapid extraction into iso-octane and/or 95 % ethanolAnnex A is informative.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, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain,Sweden, Switzerland and the United Kingdom.SIST EN 1186-9:2002



EN 1186-9:2002 (E)51 ScopeThis Part of this European Standard specifies test methods for the determination of the overall migration from onesurface only of plastics articles in the form of containers, which are intended to come into contact with foodstuffs,into aqueous based food simulants, by filling articles with a selected food simulant at test temperatures up to andincluding 70 °C for selected test times.This method is most suitable for plastics in the form of containers and articles that can be filled.2 Normative referencesThis European Standard incorporates by dated and undated reference, provisions from other publications.
Thesenormative references are cited at the appropriate places in the text, and the publications are listed hereafter. Fordated references, subsequent amendments to and revisions of any of these publications apply to this EuropeanStandard only when incorporated in it by amendment or revision.
For undated references the latest edition of thepublication referred to applies (including amendments).EN 1186-1:2002, Materials and articles in contact with food – Plastics – Part 1: Guide to the selection of conditionsand test methods for overall migration.ISO 648, Laboratory glassware - One mark pipettes.3 PrincipleThe overall migration of non-volatile substances from a sample of the plastics is determined as the mass of non-volatile residue after evaporation of the food simulants following filling the test specimen.The selection of the conditions of test and the food simulant(s) will be determined by the conditions of use asspecified in clauses 4, 5 and 6 of EN 1186-1:2002 ([3] and [6]).Test specimens are filled with the food simulant for the exposure time at temperatures above up to and including70 °C.
At the end of the test period each test specimen is emptied.
The food simulant from each test specimen isevaporated to dryness, the mass of the non-volatile residue is determined and expressed as milligrams per squaredecimetre of surface area exposed to the food simulant.NOTEIn some circumstances the procedure described in this standard can be used for exposure at temperatures above70 °C.Overall migration is reported as the mean of three determinations on separate test specimens.4 ReagentsFor details of the preparation and purity of these reagents see clause 4 of EN 1186-1:2002.4.1Distilled water or water of equivalent quality (simulant A)4.2Acetic acid 3 % (w/v) in aqueous solution (simulant B)4.3Ethanol 10 % (v/v) in aqueous solution (simulant C)4.4Alcoholic simulants for liquids or beverages of an alcoholic strength exceeding 10 % (v/v).NOTEIn the case of materials and articles intended to come into contact with liquids or beverages of an alcoholic strengthexceeding 10 % (v/v) the test can be carried out with aqueous solutions of ethanol of a similar strength.SIST EN 1186-9:2002



EN 1186-9:2002 (E)65 Apparatus5.1Analytical balance capable of determining a change in mass of 0,1 mg.5.2Lint-free cloth or soft brush.5.3Beaker, 2 l.5.4Glass beads, 2 mm to 3 mm diameter.5.5Thermostatically controlled oven or incubator or refrigerator capable of maintaining the set temperaturewithin the tolerances specified in Table B.2 of EN 1186-1:2002.5.6Dishes, stainless steel, nickel, platinum, platinum alloy, gold 50 mm to 90 mm diameter and maximum mass100 g, for evaporation of food simulants and weighing of residues.
Glass, glass ceramic or ceramic dishes may beused, provided that the surface characteristics are such that the masses of the dishes after evaporation of anyspecified food simulants followed by conditioning in the desiccator used, achieves a constancy of ± 0,5 mg.Stainless steel and nickel dishes are suitable only for distilled water and ethanol solutions.
Glass, glass ceramic,glazed ceramic, platinum, platinum alloy or gold dishes are suitable for all three simulants.5.7Steam bath, hot plate, distillation apparatus or rotary evaporator for evaporation of food simulant at the endof test period.5.8Desiccator with anhydrous calcium chloride or self indicating silica gel.5.9Beakers, 250 ml.5.10Pipette, 200 ml, complying with the minimum requirements of ISO 648.6 Preparation of test specimens6.1 GeneralIt is essential that test specimens are clean and free from surface contamination (many plastics can readily attractdust due to static charges).
Before preparing test specimens, remove any surface contamination from the sampleby gently wiping it with a lint free cloth, or by brushing with a soft brush.
Under no circumstances wash the samplewith water or solvent. If it is specified in the instructions for use of the article that it should be washed or cleanedbefore use see 8.1 of EN 1186-1:2002.
Minimize handling of the samples and, where necessary, wear cottongloves.6.2 Number of test specimens6.2.1 Volume of articlesDetermine and record the volume of food simulant required to fill an article to its nominal foodstuff volume.
If thenominal volume of foodstuff to fill the article is not known, determine the surface area that will be in contact with thefood simulant when filled to 5 mm from the top of the test specimen.6.2.2 Articles with a nominal volume of more than 200 mlFive articles are required to provide five test specimens.
These test specimens are utilized as follows:a) three test specimens for the migration test;b) two test specimens for the determination of surface area.SIST EN 1186-9:2002



EN 1186-9:2002 (E)76.2.3 Articles with a nominal volume of less than 200 mlThe number of articles required to provide a test specimen is dependent on their volume.
A test specimen shall bemade up of sufficient articles to contain a minimum of 200 ml of the food simulant.Five test specimens are required.
These test specimens are utilized as follows:a) three test specimens for the migration test;b) two test specimens for the determination of surface area.Record the number of articles used to provide the test specimen.6.3 Surface area of test specimen exposed to food simulantDetermine and record the surface area of the test specimen which is intended to come into contact with its nominalvolume of foodstuff.
If the nominal volume of foodstuff to fill the article is not known, determine the surface areawhich will be in contact with the food simulant when filled to 5 mm from the top of the test specimen.NOTE 1For some articles it is recognized that it is impractical to measure the surface area intended to come into contactwith foodstuff.
For such articles the overall migration is measured as milligrams of substance released per kilogram of foodsimulant.NOTE 2In the case of articles with a volume of less than 200 ml this will be the surface area of one article multiplied by thenumber of articles used to provide a test specimen.6.4 Articles with a capacity of not less than 500 ml and not more than 10 lIt is not necessary to determine the volume of these articles since the migration is expressed in mg/kg of foodsimulant.7 Procedure7.1 Exposure to food simulantMark each test specimen for identification, and where more than one article has been used for a test specimen,also mark individually.Place, in a beaker, a sufficient volume of the food simulant to fill the three test specimens to the nominal volume, ifknown, or to 5 mm from the top and to provide two 200 ml blanks.
Insert a thermometer or thermocouple, ifapplicable see NOTE 3, in the simulant.
Place the beaker in the thermostatically controlled oven or incubator orrefrigerator set at the test temperature and leave until the simulant has attained the test temperature.Remove the beaker containing the food simulant from the thermostatically controlled oven or incubator orrefrigerator.
Fill the three test specimens with simulant to the nominal volume of the article or to 0,5 cm from thetop.
If the container has a specified nominal volume of contents see 8.2 of EN 1186-1:2002.
Insert thethermometer or thermocouple in one of the test specimens containing simulant, if applicable see NOTE 3.
Coverthe test specimens and the remaining simulant with an inert material to prevent evaporation.
This part of theoperation should be carried out in the minimum time to prevent undue heat loss from the simulant.Place the test specimens and food simulant in the thermostatically controlled oven or incubator or refrigerator set atthe test temperature.
Observe the temperature and leave the test specimens and food simulant for the selectedperiod of time after the temperature of the simulant has reached a temperature within the permitted tolerance fortemperature, see Tables B.1 and B.2 of EN 1186-1:2002 for permitted tolerances on test times and temperature.NOTE 1Where the surface of simulant is large, a check should be made to ensure that excessive loss of simulant byevaporation does not occur.SIST EN 1186-9:2002



EN 1186-9:2002 (E)8NOTE 2Annex B of EN 1186-1:2002 includes tolerances on a wide range of contact times and contact temperatures.
All ofthese contact times and contact temperatures are not necessarily relevant to this Part of the standard.Take the test specimens and food simulant
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