SIST EN 1186-3:2002
(Main)Materials and articles in contact with foodstuffs - Plastics - Part 3: Test methods for overall migration into aqueous food simulants by total immersion
Materials and articles in contact with foodstuffs - Plastics - Part 3: Test methods for overall migration into aqueous food simulants by total immersion
This part of this European Prestandard describes a test method for the determination of the overall migration into aqueous based food simulants from plastics which are intended to come into contact with foodstuffs, by total immersion in aqueous food simulant for 10 days, 24 h or 2 h at 40 °C or for 2 h at 70 °C. This method is most suitable for plastics in the form of films and sheets, but can be applied to a wide range of articles or containers from which test pieces of suitable size can be cut.
Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Kunststoffe - Teil 3: Prüfverfahren für die Gesamtmigration in wässrige Prüflebensmittel durch völliges Eintauchen
1 Anwendungsbereich
Dieser Teil der Europäischen Norm beschreibt Prüfverfahren zur Bestimmung der Gesamtmigration in wässrige Lebensmittel aus Kunststoffen, die für den Kontakt mit Lebensmitteln vorgesehen sind, durch völliges Eintauchen der Prüfkörper in ein ausgewähltes Prüflebensmittel bei Prüftemperaturen bis zur Rückflusstemperatur und für ausgewählte Prüfzeiten.
Dieses Verfahren ist am besten geeignet für Kunststoffe in Form von Folien und Platten, es kann jedoch auch für eine große Reihe von Gegenständen oder Behältern angewendet werden, aus denen Prüfabschnitte geeigneter Größe geschnitten werden können.
Matériaux et objets en contact avec les denrées alimentaires - Matiere plastique - Partie 3: Méthodes d'essai pour la migration globale dans les simulants aqueux par immersion totale
La présente partie de cette norme européenne spécifie une méthodes d'essai de vérification de la migration globale des matériaux et objets en matiere plastique destinés a entrer en contact avec les denrées alimentaires par immersion totale d'éprouvettes dans un simulant aqueux choisi a des températures d'essai allant jusqu'au reflux pendant des durées définies.
Cette méthode est plus particulierement applicable aux matieres plastiques sous forme de films et de feuilles, mais peut etre aussi appliquée a une large gamme d'objets ou de récipients a partir desquels des morceaux de taille appropriée peuvent etre prélevés.
Materiali in predmeti v stiku z živili - Polimerni materiali - 3. del: Preskusne metode za celotno migracijo v vodne modelne raztopine s popolno potopitvijo
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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Materiali in predmeti v stiku z živili - Polimerni materiali - 3. del: Preskusne metode za celotno migracijo v vodne modelne raztopine s popolno potopitvijoWerkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Kunststoffe - Teil 3: Prüfverfahren für die Gesamtmigration in wässrige Prüflebensmittel durch völliges EintauchenMatériaux et objets en contact avec les denrées alimentaires - Matiere plastique - Partie 3: Méthodes d'essai pour la migration globale dans les simulants aqueux par immersion totaleMaterials and articles in contact with foodstuffs - Plastics - Part 3: Test methods for overall migration into aqueous food simulants by total immersion67.250Materiali in predmeti v stiku z živiliMaterials and articles in contact with foodstuffsICS:Ta slovenski standard je istoveten z:EN 1186-3:2002SIST EN 1186-3:2002en01-september-2002SIST EN 1186-3:2002SLOVENSKI
STANDARDSIST ENV 1186-3:19971DGRPHãþD
SIST EN 1186-3:2002
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 1186-3April 2002ICS 67.250Supersedes ENV 1186-3:1994English versionMaterials and articles in contact with foodstuffs - Plastics - Part3: Test methods for overall migration into aqueous foodsimulants by total immersionMatériaux et objets en contact avec les denréesalimentaires - Matière plastique - Partie 3: Méthodesd'essai pour la migration globale dans l'huile d'olive parimmersion totaleWerkstoffe und Gegenstände in Kontakt mit Lebensmitteln- Kunststoffe - Teil 3: Prüfverfahren für dieGesamtmigration in wässrige Prüflebensmittel durchvölliges EintauchenThis 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 1186-3:2002 ESIST EN 1186-3:2002
EN 1186-3:2002 (E)2ContentspageForeword.31Scope.52Normative references.53Method A - overall migration into aqueous food simulants by total immersion in an oven orincubator or refrigerator.54Method B - overall migration into aqueous food simulants by total immersion
at reflux.11Annex A (informative)
Precision data.14Annex ZA (informative)
Relationship of this European Standard with Council Directive 89/109/EECand Commission Directive 90/128/EEC and associated Directives.15Bibliography.17SIST EN 1186-3:2002
EN 1186-3:2002 (E)3ForewordThis document EN 1186-3:2002 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 1186-3:1994.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 1186-3 should be read in conjunction with EN 1186-1.Further Parts of this standard have been prepared concerned with the determination of overall migration fromplastics 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 simulants by total immersionPart 4Test methods for overall migration into olive oil by cellPart 5 Test methods for overall migration into aqueous food simulants by cellPart 6Test 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 9Test methods for overall migration into aqueous food simulants 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 triglycerideSIST EN 1186-3:2002
EN 1186-3:2002 (E)4Part 12Test methods for overall migration at low temperaturesPart 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 1186-3:2002
EN 1186-3:2002 (E)51 ScopeThis Part of this European Standard specifies test methods for the determination of the overall migration intoaqueous based food simulants from plastics which are intended to come into contact with foodstuffs, by totalimmersion of test specimens in a selected food simulant at test temperatures up to reflux for selected test times.This method is most suitable for plastics in the form of films and sheets, but can be applied to a wide range ofarticles or containers from which test pieces of suitable size can be cut.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 foodstuffs – Plastics – Part 1: Guide to the selection ofconditions and test methods for overall migration.EN 10088-1:1995, Stainless steels - Part 1: List of stainless steels.EN ISO 8442-2:1997, Materials and articles in contact with foodstuffs – Cutlery and table holloware – Part 2:Requirements for stainless steel and silver- plated cutlery (ISO 8442-2:1997).ISO 4788, Laboratory glassware - Graduated measuring cylinders.3 Method A - overall migration into aqueous food simulants by total immersion in anoven or incubator or refrigerator3.1 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 simulant following immersion.The selection of the conditions of test and the food simulant(s) shall be determined by the conditions of use; seeclauses 4, 5 and 6 of EN 1186-1:2002.Test specimens of approximately 1 dm², see clause 8 of EN 1186-1:2002, are immersed in the food simulant for theexposure time at temperatures up to and including the temperature of reflux.
At the end of the test period, eachtest specimen is removed from the food simulant.
The food simulant from each test specimen is evaporated todryness, the mass of the non-volatile residue is determined gravimetrically and expressed as milligrams per squaredecimetre of surface area of test specimen.Overall migration is reported as the mean of three determinations on separate test specimens.3.2 ReagentsNOTEFor details of preparation and quality of these reagents, see clause 4 of EN 1186-1:2002.3.2.1Distilled water or water of equivalent quality (simulant A)3.2.2Acetic acid 3 % (w/v) in aqueous solution (simulant B)3.2.3Ethanol 10 % (v/v) in aqueous solution (simulant C)SIST EN 1186-3:2002
EN 1186-3:2002 (E)63.2.4Alcoholic 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 is carried out with aqueous solutions of ethanol of a similar strength.3.3 Apparatus3.3.1Cutting slab, clean smooth glass, metal or plastics slab of suitable area to prepare test specimens,250 mm ´ 250 mm is suitable.3.3.2Tweezers, stainless steel, blunt nosed.3.3.3Cutting implement, scalpel, scissors or sharp knife or other suitable device.3.3.4Metal template, (100 mm ± 0,2 mm) ´ (100 mm ± 0,2 mm) (square).3.3.5Rule or template, 25 mm ± 1 mm wide.3.3.6Rule, graduated in mm, and with an accuracy of 0,1 mm.3.3.7Analytical balance capable determining a change in mass of 0,1 mg.3.3.8Specimen supports, constructed of stainless steel with cross arms attached by welding or silver soldering,or of glass.
Stainless steel X4 CrNi 18 10 according to EN 10088-1: 1995 or of composition, chromium 17 %,nickel 9 %, carbon 0,04 %, is suitable.
Before initial use thoroughly clean the stainless steel supports. The use of adegreasing solvent and then dilute nitric acid has been found to be suitable.
For the aqueous acetic acid foodsimulant, use supports constructed out of glass, as there is a tendency for the acetic acid to corrode stainless steelsupports, particularly if the joints are silver soldered.NOTE 1However stainless steel supports can be used for acetic acid if it can be demonstrated that when immersed on theirown in simulant, for the test period, at the test temperature, the residue after evaporating the simulant to dryness and drying inan oven or incubator or refrigerator to constant mass at 105 °C to 110 °C is less than 5mg/l, see 4.1 ofEN 1186-1:2002.NOTE 2The method has been written for the supports shown in Figure C.1 of EN 1186-1:2002 which have been found to besuitable for holding thin film and sheet test pieces.
However other supports can be used providing they are capable of holdingand keeping the test pieces apart and at the same time ensuring complete contact with the simulant.
For rigid samples,supports with a single cross arm may be used.3.3.9Gauze, pieces of fine stainless steel gauze, with a mesh size of 1 mm have been found to be suitable,approximately 25 mm ´ 100 mm or, glass rods, 2 mm to 3 mm in diameter and approximately 100 mm long to beused with the acetic acid food simulant, for insertion between the test pieces. Before initial use thoroughly clean thegauze, first with a degreasing solvent and then with dilute nitric acid.3.3.10Glass tubes, ground neck, for retaining the food simulant and test specimens. Tubes with an internaldiameter of approximately 35 mm and length of between 100 mm and 200 mm, excluding the ground neck (see 7.2of EN 1186-1:2002) have been found to be satisfactory.3.3.11Glass beads, 2 mm to 3 mm diameter or glass rods, 2 mm to 3 mm in diameter and approximately 100 mmlong (see 7.2 of EN 1186-1:2002).3.3.12Thermostatically controlled oven or incubator or refrigerator capable of maintaining the set temperaturewithin the tolerances specified in Table B.2 of EN 1186-1:2002.3.3.13Dishes, stainless steel, nickel, platinum, platinum alloy, gold 50 mm to 90 mm diameter and maximummass 100 g, for evaporation of food simulants and weighing of residues.
Glass, glass ceramic or ceramic dishesmay be used provided that the surface characteristics are such that the masses of the dishes after evaporation ofany specified 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 or, platinum alloy or gold dishes are suitable for all three simulants.SIST EN 1186-3:2002
EN 1186-3:2002 (E)73.3.14Steam bath, hot plate, distillation apparatus or rotary evaporator for evaporation of food simulant at the endof test period.3.3.15Desiccator with anhydrous calcium chloride or self indicating silica gel.3.3.16Measuring cylinder, 100 ml, complying with the minimum requirements of ISO 4788.3.4 Preparation of test specimens3.4.1 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.
Minimise handling of the samples and where necessary, wear cottongloves.To ensure that test pieces are well separated and that the surfaces are freely exposed to the food simulant duringthe period of the test, for thin films, insert a piece of fine stainless steel gauze, or glass rods with the acetic acidsimulant, between the test pieces or for thick samples not placed on the supports, insert glass rods between thetest pieces after immersion in the food simulant.
Where specimen supports are used, label the supports with a tagbearing the test specimen identification.When preparing test specimens measure the surface area according to 8.3 of EN 1186-1:2002.3.4.2 Number of test specimensThree test specimens are required for samples, in the form of thin films, sheets, cut sections from containers orsimilar articles.
Five test specimens, similar dimensionally one to another, are required for samples of articles ofirregular shape.
These test specimens are utilized as follows:a) three test specimens for the migration test;b) two test specimens for determination of the surface area, in the case of samples of irregular shape(3.4.5).3.4.3 Films and sheetsLay the sample on the cutting slab (3.3.1) and cut the test specimens of 1 dm² (see 9.3 of EN 1186-1:2002), usingthe 100 mm ´ 100 mm template (3.3.4).
Check, using the rule (3.3.6), that the dimensions of the specimen arewithin the specified tolerance (± 1 mm).Cut each test specimen into four test pieces 25 mm ´ 100 mm using the rule (3.3.5).
Assemble one test specimenonto the support (3.3.8) by piercing suitable holes in the test pieces and placing two test pieces on each side of thecross arms of the support. Repeat this procedure for all remaining test specimens.3.4.4 Containers and other articlesCut sections from the walls of the container or article to give test specimens each of area approximately 1 dm².
Forarticles with individual areas less than 1 dm², use a number of articles to provide each test specimen.
Measure thedimensions of each test specimen to the nearest 1 mm, using the rule.
Calculate only the surface area of thesample which is intended to come into contact with foodstuffs, see 8.3 of EN 1186-1:2002.Calculate the area of each test specimen to the nearest 0,01 dm² and record. If necessary, cut each test specimeninto smaller pieces to enable them to fit into the glass tubes (3.3.10).
The test specimens or pieces are placed onthe specimen supports if these are appropriate or, if the test specimens or pieces are sufficiently rigid, they can betested unsupported.SIST EN 1186-3:2002
EN 1186-3:2002 (E)83.4.5 Articles of irregular shapeSelect representative portions of the article, or multiples of the article for small articles, to give five dimensionallysimilar test specimens each with a known total surface area of at least 1 dm².
Measure only the surface areaintended to come into contact with foodstuffs of two of these test specimens to the nearest 0,05 dm² using theSchlegel Method, as described in EN ISO 8442-2:1997, annex B, or any other suitable method.
Record the surfacearea of each test specimen.3.5 Procedure3.5.1 Exposure to food simulantTake three of the glass tubes, for the test specimens and a further two to provide blanks, measure by measuringcylinder 100 ml ± 2 ml of the food simulant into each tube and stopper the tube.
Insert a thermometer orthermocouple, if applicable see NOTE 2, in one of the test specimen tubes, and stopper all five tubes.
Place thefive tubes in the thermostatically controlled oven, incubator or refrigerator, set at the test temperature, and leaveuntil the simulant has attained the test temperature.Place a test specimen into each of the three tubes containing 100 ml of simulant, re-insert the thermometer orthermocouple and stopper the tubes.
Mark the tubes for identification.
Ensure that the test specimens are totallyimmersed in the simulant; if they are not then add either glass beads or rods to raise the level of the simulant untiltotal immersion is achieved.
This part of the operation should be carried out in the minimum time to prevent undueheat loss from the simulant.Mark the liquid level on the outside of each tube with a suitable marker.Replace all of the tubes in the thermostatically controlled oven, incubator or refrigerator, set at the test temperature.Observe the temperature and leave the tubes for the selected period of time after the temperature of the simulanthas reached a temperature within the permitted tolerance for the test temperature, see Tables B.1 and B.2 ofEN 1186-1:2002 for permitted tolerances on test times and temperature.NOTE 1Annex B of EN 1186-1:2002 inc
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