SIST EN 1186-14:2003

Materials and articles in contact with foodstuffs - Plastics - Part 14: Test methods for 'substitute tests' for overall migration from plastics intended to come into contact with fatty foodstuffs using test media iso-octane and 95 % ethanol

This European Standard describes test methods for 'substitute tests' performed with volatile test media, iso-octane and 95 % v/v aqueous ethanol, for the determination of overall migration from plastics intended to come into contact with fatty foodstuffs at all temperatures and for any period of time.
These test methods are suitable for plastics samples in a wide variety of forms.
NOTE 1   The iso-octane and 95 % v/v aqueous ethanol volatile test media used in these test methods are those specified for 'substitute tests' in Commission Directive 82/711/EEC [3]and its subsequent amendments [4], [5].  In addition to the use of iso-octane and 95 % v/v aqueous ethanol as test media for 'substitute tests', Commission Directive 82/711/EEC and its subsequent amendments specifies the use of modified polyphenylene oxide as a test medium for use at temperatures of 100 °C and above.  For a test method for overall migration from plastics intended to come into contact with fatty foodstuffs using modified polyphenylene oxide as a test medium, see EN 1186-13.  
NOTE 2   These test methods can also be used for the 'alternative tests' described in Council Directive 82/711/EEC and its subsequent amendments, when the chosen volatile test media are iso-octane and 95 % aqueous ethanol, provided equivalence is shown with olive oil, see prEN 1186-1:2001.

Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Kunststoffe - Teil 14: Prüfverfahren für "Ersatzprüfungen" für die Gesamtmigration aus Kunststoffen, die für den Kontakt mit fettigen Lebensmitteln bestimmt sind, unter Verwendung der Prüfmedien iso-Octan und 95 % Ethanol

Diese Europäische Norm beschreibt Prüfverfahren für ¿Ersatzprüfungen" zur Bestimmung der Gesamtmigration aus Kunststoffen, die für den Kontakt mit fetthaltigen Lebensmitteln bestimmt sind, bei deren Durchführung die flüchtigen Prüfmedien Iso-Octan und 95 % Volumenanteil wässrigem Ethanol bei allen Temperaturen und für jede Prüfzeit angewendet werden.
Diese Prüfverfahren sind für Kunststoffe unterschiedlichster Formgebung geeignet.
ANMERKUNG 1   Die flüchtigen Prüfmedien Iso-Octan und 95 % Volumenanteil wässriger Ethanol, die in diesen Prüfverfahren verwendet werden, entsprechen den in der Richtlinie 82/711/EEC der Europäischen Kommission [3] und deren späteren Änderungen [4],[5] festgelegten Prüfmedien für ¿Ersatzprüfungen". Neben der Verwendung von Iso-Octan und 95 % Volumenanteil wässrigem Ethanol als Prüfmedien für ¿Ersatzprüfungen" legen die Richtlinie 82/711/EEC der Europäischen Kommission und deren spätere Änderungen die Verwendung von modifiziertem Polyphenylenoxid als Prüfmedium für die Anwendung bei Temperaturen von 100 °C und darüber fest. Für ein Prüfverfahren für die Gesamtmigration aus Kunststoffen, die für den Kontakt mit fetthaltigen Lebensmitteln bestimmt sind, unter Verwendung von modifiziertem Polyphenylenoxid als Prüfmedium, siehe EN 1186-13.
ANMERKUNG 2:   Diese Prüfverfahren können auch für die ¿Alternativen Prüfungen" angewendet werden, die in der Richtlinie 82/711/EEC des Rates und deren späteren Änderungen beschrieben sind, wenn die ausgewählten flüchtigen Prüfmedien Iso-Octan und 95 % Volumenanteil wässriges Ethanol sind, vorausgesetzt die Gleichwertigkeit mit Olivenöl wurde nachgewiesen, siehe prEN 1186-1:2001.

Matériaux et objets en contact avec les denrées alimentaires - Matiere plastique - Partie 14: Méthodes de remplacement pour la vérification de la migration globale des matieres plastiques en contact avec des denrées alimentaires grasses dans l'iso-octane et l'éthanol a 95 %

La présente Norme européenne spécifie des méthodes d'essai " de remplacement " réalisées à l'aide de milieux d'essai volatils tels que l'iso-octane et l'éthanol en solution aqueuse à 95 % (v/v) pour la vérification de la migration globale des matières plastiques destinées à entrer en contact avec des denrées alimentaires grasses, à toutes températures et pendant une durée quelconque.
Ces méthodes d'essai conviennent pour des échantillons de plastiques se présentant sous de multiples formes.
NOTE 1   L'iso-octane et l'éthanol en solution aqueuse à 95 % (v/v) utilisés pour les " essais de remplacement " sont les milieux d'essais spécifiés dans la Directive de la Commission 82/711/CEE [3] et ses amendements ultérieurs [4] et [5]. Outre ces milieux, la Directive de la Commission 82/711/CEE et ses amendements ultérieurs prescrivent également l'utilisation d'oxyde de polyphénylène modifié à des températures égales ou supérieures à 100 °C. Voir l'EN 1186-13 pour une méthode d'essai de vérification de la migration globale des matières plastiques destinées à entrer en contact avec les denrées alimentaires grasses à l'aide d'oxyde de polyphénylène modifié.
NOTE 2   Ces méthodes d'essai peuvent également être utilisées pour les " essais de remplacement " décrits dans la Directive du Conseil 82/711/CEE et ses amendements ultérieurs, lorsque les milieux d'essais volatils choisis sont l'iso-octane et l'éthanol à 95 %, à condition de prouver l'équivalence avec l'huile d'olive (voir l'EN 1186-1:2002).

Materiali in predmeti v stiku z živili - Polimerni materiali - 14. del: Preskusne metode za "nadomestne preskuse" za celotno migracijo iz plastičnih mas, ki prihajajo v stik z maščobnimi živili, z uporabo preskusnega medija izooktana in 95-odstotnega etanola

General Information

• Status: Withdrawn
• Publication Date: 31-Dec-2002
• Withdrawal Date: 07-Nov-2022
• ICS: 67.250 - Materials and articles in contact with foodstuffs
• Technical Committee: EPO - Packaging - sales and grouped
• Current Stage: 9900 - Withdrawal (Adopted Project)
• Start Date: 26-Oct-2022
• Due Date: 18-Nov-2022
• Completion Date: 08-Nov-2022
• Ref Project: EN 1186-14:2002 - Materials and articles in contact with foodstuffs - Plastics - Part 14: Test methods for 'substitute tests' for overall migration from plastics intended to come into contact with fatty foodstuffs using test media iso-octane and 95 % ethanol

Relations

• Replaces: SIST ENV 1186-14:2000 - Materials and articles in contact with foodstuffs - Plastics - Part 14: Test methods for 'substitute tests' for overall migration from plastics intended to come into contact with fatty foodstuffs using test media iso-octane and 95% ethanol
• Effective Date: 01-Jan-2003
• Replaced By: SIST EN 1186-3:2022 - Materials and articles in contact with foodstuffs - Plastics - Part 3: Test methods for overall migration in evaporable simulants
• Effective Date: 01-Dec-2022
• Revises: oSIST prEN 1186-14:2006 - Materials and articles in contact with foodstuffs - Plastics - Part 14: Test methods for 'substitute tests' for overall migration from plastics intended to come into contact with fatty foodstuffs using test media iso-octane and 95 % ethanol
• Effective Date: 18-Jan-2023
• Revised: oSIST prEN 1186-14:2006 - Materials and articles in contact with foodstuffs - Plastics - Part 14: Test methods for 'substitute tests' for overall migration from plastics intended to come into contact with fatty foodstuffs using test media iso-octane and 95 % ethanol
• Effective Date: 22-Dec-2008

Standards Content (Sample)

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Kunststoffe - Teil 14: Prüfverfahren für "Ersatzprüfungen" für die Gesamtmigration aus Kunststoffen, die für den Kontakt mit fettigen Lebensmitteln bestimmt sind, unter Verwendung der Prüfmedien iso-Octan und 95 % EthanolMatériaux et objets en contact avec les denrées alimentaires - Matiere plastique - Partie 14: Méthodes de remplacement pour la vérification de la migration globale des matieres plastiques en contact avec des denrées alimentaires grasses dans l'iso-octane et l'éthanol a 95 %Materials and articles in contact with foodstuffs - Plastics - Part 14: Test methods for 'substitute tests' for overall migration from plastics intended to come into contact with fatty foodstuffs using test media iso-octane and 95 % ethanol67.250Materiali in predmeti v stiku z živiliMaterials and articles in contact with foodstuffsICS:Ta slovenski standard je istoveten z:EN 1186-14:2002SIST EN 1186-14:2003en01-januar-2003SIST EN 1186-14:2003SLOVENSKI
STANDARDSIST ENV 1186-14:20001DGRPHãþD

EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 1186-14September 2002ICS 67.250English versionMaterials and articles in contact with foodstuffs - Plastics - Part14: Test methods for 'substitute tests' for overall migration fromplastics intended to come into contact with fatty foodstuffs usingtest media iso-octane and 95 % ethanolMatériaux et objets en contact avec les denréesalimentaires - Matière plastique - Partie 14: Méthodesd'essai pour des 'tests de substitution' pour la migrationglobale des matières destinées au contact avec lesdenrées alimentaires gras en utilisant des liquidessimulateurs tels que l'isooctane et l'éthanol à 95 %Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln- Kunststoffe - Teil 14: Prüfverfahren für “Ersatzprüfungen”für die Gesamtmigration aus Kunststoffen, die für denKontakt mit fettigen Lebensmitteln bestimmt sind, unterVerwendung der Prüfmedien Iso-Octan und 95 %igemEthanolThis European Standard was approved by CEN on 29 April 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 1186-14:2002 ESIST EN 1186-14:2003

Example of a pouch holder.17Annex ZA (informative)
Relationship of this European Standard with Council Directive 89/109/EECand Commission Directive 90/128/EEC and associated Directives.18Bibliography.20SIST EN 1186-14:2003

Take care to ensure that thetest specimens are well stoppered, closed and covered to prevent solvent volatilizing into the interior ofthe oven, incubator or refrigerator and generating an explosive mixture.
Care should be taken at all timeswhen handling these solvents to prevent contact with sources of ignition.EN 1186-14 should be read in conjunction with EN 1186-1, EN 1186-3, EN 1186-5, EN 1886-7, and EN 1186-9.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 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 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 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 triglyceridePart 12Test methods for overall migration at low temperaturesPart 13Test methods for overall migration at high temperaturesSIST EN 1186-14:2003

In addition to the use of iso-octane and 95 % v/v aqueous ethanol as test media for 'substitute tests', Commission Directive 82/711/EEC and its subsequentamendments specifies the use of modified polyphenylene oxide as a test medium for use at temperatures of 100 °C and above.For a test method for overall migration from plastics intended to come into contact with fatty foodstuffs using modifiedpolyphenylene oxide as a test medium, see EN 1186-13.NOTE 2These test methods can also be used for the 'alternative tests' described in Council Directive 82/711/EEC and itssubsequent amendments, when the chosen volatile test media are iso-octane and 95 % aqueous ethanol, provided equivalenceis shown with olive oil, see EN 1186-1:2002.2 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 1186-3:2002, Materials and articles in contact with foodstuffs – Plastics – Part 3: Test methods for overallmigration into aqueous food simulants by total immersion.EN 1186-5:2002, Materials and articles in contact with foodstuffs – Plastics – Part 5: Test methods for overallmigration into aqueous food simulants by cell.EN 1186-7:2002, Materials and articles in contact with foodstuffs – Plastics – Part 7: Test methods for overallmigration into aqueous food simulants using a pouch.EN 1186-9:2002, Materials and articles in contact with foodstuffs – Plastics – Part 9: Test methods for overallmigration into aqueous food simulants by article filling.EN 10088-1:1995, Stainless steels - Part 1: List of stainless steels.ISO 648, Laboratory glassware - One mark pipettes.ISO 4788, Laboratory glassware - Graduated measuring cylinders.SIST EN 1186-14:2003

At the end of the test period, each test specimen is removed from the testmedium.
The test medium from each test is evaporated to dryness, the mass of the non-volatile residue isdetermined gravimetrically and expressed as milligrams per square decimetre of surface area of test specimen.Overall migration is reported as the mean of three determinations on separate test specimens.3.2 Reagents3.2.1Iso-octane, (2,2,4-trimethyl pentane), purity 98,5 % (v/v) or greater, CAS No. 540-84-11.3.2.2Ethanol, purity 96 % (v/v) or greater, 95 % (v/v) in aqueous solution.WARNING — Both these solvents are flammable.
Take care at all times when handling these solvents toprevent contact with sources of ignition.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 x 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 %, nickel9 %, carbon 0,04 %, is suitable.
Before initial use thoroughly clean the stainless steel supports. The use of adegreasing solvent and then with dilute nitric acid has been found to be suitable.NOTEThe method has been written for the supports shown in Figure C.1 of prEN 1186-1:2002 which have been found tobe suitable for holding thin film and sheet test pieces.
However other supports can be used providing they are capable of
1The source of this is the Chemical Abstracts published by the American Chemical SocietySIST EN 1186-14:2003

For rigidsamples, supports with a single cross arm can 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 forinsertion between the test pieces.
Before initial use thoroughly clean the gauze, first with a degreasing solvent andthen with dilute nitric acid.3.3.10Glass tubes, ground neck with stoppers, for retaining the test medium and test specimens.
Tubes with aninternal diameter of approximately 35 mm and length in the range of 100 mm to 200 mm, excluding the groundneck, see 8.2 of 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 approximately100 mm long, see 8.2 of EN 1186-1:2002.3.3.12Thermostatically controlled oven, incubator or refrigerator capable of maintaining a temperature within therange of 5 °C to 60 °C and within the tolerances specified in Table B.2 of EN 1186-1:2002.WARNING — The interior/sample space of the oven, incubator or refrigerator should not have any exposedheating elements, to minimise safety hazards arising from any loss of the flammable test media from thetubes during the test period.3.3.13Dishes, stainless steel, nickel, platinum, platinum alloy, gold 50 mm to 90 mm diameter and maximumweight 100 g, for evaporation of test media and weighing of residues.
Glass, glass ceramic or ceramic dishes maybe used provided that the surface characteristics are such that the weights of the dishes after evaporation of anyspecified test media followed by conditioning in the desiccator used achieves a constancy of ± 0,5 mg.3.3.14Steam bath, hot plate, distillation apparatus or rotary evaporator for evaporation of test medium 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 4788.3.3.17Thermometer or electronic temperature measuring instrument with thermocouple, capable of measuringtemperature in the range 5 °C to 60 °C, with a precision of 0,1 °C.3.4Preparation of test specimensPrepare the test specimens in accordance with 3.4 of EN 1186-3:2002.3.4 Procedure3.4.1 Exposure to test mediaTake 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 test medium into each tube and stopper the tube.
If the evaporation method is to beused measure into a further two tubes, by measuring cylinder, 120 ml ± 2 ml of the test medium, to provide blanks.If the distillation method is to be used measure into those further two tubes by measuring cylinder 100 ml ± 2 ml ofthe test medium to provide blanks. Insert a thermometer or thermocouple in one of the tubes containing 100 ml oftest medium, then stopper all five tubes. Place the five tubes in the thermostatically controlled oven, incubator orrefrigerator, set at the test temperature, and leave until the test medium has attained the test temperature.Place a test specimen into each of the three tubes containing 100 ml of test medium, re-insert the thermometer orthermocouple and re-stopper the tubes.
Mark the tubes for identification.
Ensure that the test specimens aretotally immersed in the test medium; if they are not then add either glass beads or rods to raise the level of the testmedium until total immersion is achieved.
This part of the operation should be carried out in the minimum time toprevent undue heat loss from the test medium.SIST EN 1186-14:2003

Take care to ensure that thetubes are well stoppered to prevent solvent volatilizing into the interior of the oven, incubator orrefrigerator and generating an explosive mixture.WARNING
2 — If possible place the tubes in a drip container capable of holding the total volume of volatilesimulant in case of accident.WARNING
3 — To minimise hazards arising due to the volatile and flammable nature of the two test mediathe maximum test temperature is 60 °C. Do not conduct the tests at temperatures above 60 °C.Take the tubes from the oven, incubator or refrigerator and check the level of test medium in each, if this has fallento more than 10 mm below the mark, or has exposed any part of the test pieces, repeat the test using fresh testspecimens.NOTEFor exposure times of more than 24 h it is acceptable to monitor the temperature of the airbath of thethermostatically controlled oven or incubator, instead of the temperature of the simulant.If the level of test medium in a tube is less than 10 mm below the mark, remove the test specimen from the tube,and allow the test medium adhering to the test specimen and support to drain back into the tube. Recover at least90 % of the original volume of test medium or repeat the test.3.4.2 Determination of migrating substancesDetermine the migrating substances in accordance with 3.5 of EN 1186-3:2002.WARNING — Both iso-octane and ethanol are volatile and flammable solvents. Take care when evaporatingthese test media to prevent vapours contacting sources of ignition, particularly when using a hot plate tocarry out the evaporation.
The evaporation should be carried out in a fume cupboard.3.5 Expression of resultsCalculate the results in accordance with 3.6 of EN 1186-3:2002.3.6 Test reportThe test report shall include the following, see clause 12 of EN 1186-1:2002:a) reference to this European Standard and to the Part used for the test procedure;b) all information necessary for complete identification of the sample such as chemical type, supplier, trademark, grade, batch number, thicknesses;c) conditions of time and temperature of exposure to test media;d) departures from the specified procedure, and reasons for these;e) individual test results, and the mean of these, expressed as milligrams of residue per square decimetreof sample;f) relevant comments on the test results.SIST EN 1186-14:2003

At the end of the test period, each test specimen is removed from contact with the test medium. Thetest medium from each test is evaporated to dryness, the mass of the non-volatile residue is determinedgravimetrically and expressed as milligrams per square decimetre of surface area of test specimen, which hadbeen in contact with the test medium.Overall migration is reported as the mean of three determinations on separate test specimens.4.2 Reagents4.2.1Iso-octane (2,2,4-trimethyl pentane), purity 98,5 % (v/v) or greater, CAS No. 540-84-1.4.2.2Ethanol, purity 96 % (v/v) or greater, 95 % (v/v) in aqueous solution.WARNING — Both these solvents are flammable.
Take care at all times when handling these solvents toprevent contact with sources of ignition.4.3 Apparatus4.3.1Cutting slab, clean smooth glass, metal or plastics slab of suitable area to prepare test specimens, 250 mm ´ 250 mm is suitable.4.3.2Tweezers, stainless steel, blunt nosed.4.3.3Cutting implement, scalpel, scissors or sharp knife or other suitable device.4.3.4Rule, graduated in mm, and with an accuracy of 0,1 mm.4.3.5Analytical balance capable of determining a change in mass of 0,1 mg.4.3.6Cell type A, as shown in Figure C.3 of EN 1186-1:2002, either the all aluminium (anodised) cells or thecells with the stainless steel (316 grade) lids and rings. The internal diameter of the rib of the sealing ring shall be178,4 mm ± 0,1 mm, to give an area of the test specimen exposed to the test medium of 2,5 dm².
It is necessary tomodify the filler plug on one of the cells to allow a thermometer or thermocouple to be inserted into the testmedium, whilst maintaining an effective seal to prevent loss of test medium during the test period.NOTEThe cell type A is constructed with a rubber mat in the base plate.
It is advised that a disc of aluminium foil is placedon the mat before inserting the test specimen.
The use of these discs will prevent any substances from the mat influencing themigration result.For details of equivalent cells see 8.3 of EN 1186-1:2002.4.3.7Pipettes, complying with the minimum requirements of ISO 648, 50 ml and 100 ml.4.3.8Glass tubes, ground neck, and stoppers, for retaining the test medium.
Tubes with an internal diameter ofapproximately 35 mm and length of approximately 100 mm to 200 mm, excluding the ground neck, see 8.2 ofEN 1186-1:2002, have been found to be satisfactory.SIST EN 1186-14:2003
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