SIST EN 1186-2:2002
(Main)Materials and articles in contact with foodstuffs - Plastics - Part 2: Test methods for overall migration into olive oil by total immersion
Materials and articles in contact with foodstuffs - Plastics - Part 2: Test methods for overall migration into olive oil by total immersion
This part of this European Prestandard describes test methods for the determination of the overall migration from plastics intended to come into contact with a fatty foodstuff, by total immersion in olive oil for 10 days, 24 h or for 2 h at 40 °C or 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 a suitable size can be cut. The test method described is applicable to most types of plastics, althoug there are some plastics for which it is known not to be applicable.
Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Kunststoffe - Teil 2: Prüfverfahren für die Gesamtmigration in Olivenöl durch völliges Eintauchen
1 Anwendungsbereich
Dieser Teil der Europäischen Norm beschreibt Prüfverfahren zur Bestimmung der Gesamtmigration aus Werkstoffe und Gegenständen aus Kunststoff in Simulanzlösemittel für fetthaltige Lebensmittel durch völliges Eintauchen der Prüfmuster in das Simulanzlösemittel bei Temperaturen über 20°C bis zu (jedoch nicht einschließlich) 100°C während bestimmter Zeiten.
Dieses Verfahren ist bestens geeignet für Kunststoffe in Form von Folien und Platten, kann aber auch angewendet werden für einen weiten Bereich von Gegenständen und Behältern, aus denen Prüfabschnitte geeigneter Größe geschnitten werden können.
ANMERKUNG Dieses Prüfverfahren wurde beschrieben für die Verwendung von Olivenöl als Simulanzlösemittel für fetthaltige Lebensmittel. Das Prüfverfahren kann mit entsprechender Modifikation auch mit ?anderen Simulanzlösemitteln für fetthaltige Lebensmittel" angewendet werden, dem sogenannten Simulanzlösemittel D - einer synthetischen Mischung von Triglyceriden, Sonnenblumenöl und Maiskeimöl. Diese anderen Simulanzlösemittel für fetthaltige Lebensmittel ergeben für ihre Methylester andere Chromatogramme als für die Methylester des Simulanzlösemittels Olivenöl. Aus den Chromatogrammen der Methylester der anderen Simulanzlösemittel werden geeignete Peaks zur quantitativen Bestimmung des aus dem Prüfmuster extrahierten Simulanzlösemittels ausgewählt.
Das beschriebene Prüfverfahren kann auf die meisten Kunststoffsorten angewendet werden. Es gibt jedoch einige Kunststoffe, von denen bekannt ist, dass es nicht angewendet werden kann.
Matériaux et objets en contact avec les denrées alimentaires - Matiere plastique - Partie 2: Méthodes d'essai pour la migration globale dans l'huile d'olive par immersion totale
La présente partie de cette norme européenne décrit une méthode d'essai de vérification de la migration globale des matériaux et objets en matiere plastique destinés a entrer en contact avec une denrée alimentaire grasse, par immersion totale d'éprouvettes dans un simulant gras a des températures supérieures a 20 °C mais inférieures a 100 °C 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.
NOTE La présente méthode d'essai a été écrite pour l'huile d'olive. Elle peut également etre utilisée, avec les modifications qui s'imposent, pour d'autres simulants gras appelés du terme générique « simulant D », mélange synthétique de triglycérides, d'huile de tournesol et d'huile de mais. Ces autres simulants gras donneront des chromatogrammes des esters méthyliques du simulant utilisé différents de ceux des esters méthyliques de l'huile d'olive. Choisir pour le dosage quantitatif du simulant extrait des éprouvettes les pics de chromatogramme correspondant aux esters méthyliques des autres simulants gras.
La méthode d'essai décrite est applicable a la plupart des types de matieres plastiques, bien qu'il soit connu qu'elle ne le soit pas a certains.
Materiali in predmeti v stiku z živili - Polimerni materiali - 2. del: Preskusne metode za celotno migracijo v olivno olje s popolno potopitvijo
General Information
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Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Materiali in predmeti v stiku z živili - Polimerni materiali - 2. del: Preskusne metode za celotno migracijo v olivno olje s popolno potopitvijoWerkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Kunststoffe - Teil 2: Prüfverfahren für die Gesamtmigration in Olivenöl durch völliges EintauchenMatériaux et objets en contact avec les denrées alimentaires - Matiere plastique - Partie 2: Méthodes d'essai pour la migration globale dans l'huile d'olive par immersion totaleMaterials and articles in contact with foodstuffs - Plastics - Part 2: Test methods for overall migration into olive oil by total immersion67.250Materiali in predmeti v stiku z živiliMaterials and articles in contact with foodstuffsICS:Ta slovenski standard je istoveten z:EN 1186-2:2002SIST EN 1186-2:2002en01-september-2002SIST EN 1186-2:2002SLOVENSKI
STANDARDSIST ENV 1186-2:19971DGRPHãþD
SIST EN 1186-2:2002
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 1186-2April 2002ICS 67.250Supersedes ENV 1186-2:1994English versionMaterials and articles in contact with foodstuffs - Plastics - Part2: Test methods for overall migration into olive oil by totalimmersionMatériaux et objets en contact avec les denréesalimentaires - Matière plastique - Partie 2: Méthodesd'essai pour la migration globale dans l'huile d'olive parimmersion totaleWerkstoffe und Gegenstände in Kontakt mit Lebensmitteln- Kunststoffe - Teil 2: Prüfverfahren für dieGesamtmigration in Olivenöl durch völliges 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 1186-2:2002 ESIST EN 1186-2:2002
EN 1186-2:2002 (E)2ContentspageForeword.31Scope.52Normative references.53Principle.54Reagents.65Apparatus.76Preparation of test specimens.97Procedure.108Expression of results.178.1Method of calculation.179Test report.18Annex A (normative)
Determination of the suitability of olive oil as the fatty food simulant and oftriheptadecanoin as the internal standard.19Annex B (normative)
Determination of the need for sample conditioning.21Annex C (normative)
Determination of the need for sample conditioning and determination of themass of moisture sensitive test specimens, by vacuum drying.22Annex D (normative)
Determination of change in moisture content of test specimens bymeasurement of the transfer of water to, or from olive oil, by Karl Fischer titration.24Annex E (informative)
Typical chromatograms and calibration graph.26Annex F (informative)
Precision data.29Annex ZA (informative)
Relationship of this European Standard with Council Directive 89/109/EECand Commission Directive 90/128/EEC and associated Directives.30Bibliography.32SIST EN 1186-2:2002
EN 1186-2:2002 (E)3ForewordThis document EN 1186-2:2002 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 1186-2:1994.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 1186-2 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 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 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 triglyceridePart 12Test methods for overall migration at low temperaturesSIST EN 1186-2:2002
EN 1186-2:2002 (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 % ethanolAnnexes A, B, C and D to this standard are normative where applicable. The annexes E and F are 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 1186-2:2002
EN 1186-2:2002 (E)51 ScopeThis Part of this European Standard describes test methods for the determination of the overall migration into fattyfood simulants from plastics materials and articles, by total immersion of test specimens in a fatty food simulant attemperatures above 20 °C and up to, but not including, 100 °C for selected 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 a suitable size can be cut.NOTEThis test method has been written for use with the fatty food simulant, olive oil.
The test method can also be usedwith appropriate modifications with 'other fatty food simulants ' called simulant D - a synthetic mixture of triglycerides, sunfloweroil and corn oil.
These other fatty food simulants will produce different chromatograms for the simulant methyl esters to those ofthe methyl esters of olive oil.
Select suitable chromatogram peaks of the methyl esters of the other fatty food simulants for thequantitative determination of the simulant extracted from the test specimens.The test method described is applicable to most types of plastics, although there are some plastics for which it isknown not to be applicable.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, 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 648, Laboratory glassware - One mark pipettes.ISO 4788, Laboratory glassware - Graduated measuring cylinders.3 PrincipleThe overall migration from a sample of the plastics is determined as the loss in mass per unit of surface areaintended to come into contact with foodstuffs.The selection of the conditions of test will be determined by the conditions of use, see clauses 4, 5 and 6 of EN1186-1:2002.Test specimens of known mass are immersed in olive oil for the exposure time, at temperatures above 20 °C andbelow 100 °C, then taken from the olive oil, blotted to remove oil adhering to the surface, and reweighed.The specimens will usually retain absorbed olive oil that is extracted and determined quantitatively by means of gaschromatography after conversion to methyl esters.
Methylation is carried out by reacting a borontrifluoride/methanol complex with fatty acids formed by hydrolysing the oil with potassium hydroxide.
An internalstandard, triheptadecanoin, is added prior to the extraction of the absorbed olive oil from the test specimens.
ThisSIST EN 1186-2:2002
EN 1186-2:2002 (E)6ensures that any active or extractable components of the plastics react with the internal standard, as well as withthe extracted olive oil. The internal standard is also subjected to the hydrolysis and methylation reactions, providingcompensation for any inefficiencies in the hydrolysis and methylation processes.Migration into the olive oil is calculated by subtracting the mass of olive oil retained by the test specimen from themass of the test specimen after removal from the olive oil, then subtracting this mass from the initial mass of thespecimen.The total loss in mass is expressed in milligrams per square decimetre of surface area of the specimen and theoverall migration is reported as the mean of a minimum of three determinations on separate test specimens.To allow for inaccuracies which may arise during the procedure and which may be difficult to detect, due forexample to contamination or loss of oil during the sample handling stages, four determinations are carried out onthe sample allowing for the result from one specimen to be discarded.This method includes variations that are applicable to certain plastics.NOTEBefore starting a migration exercise, the test sample should be examined for the presence of components interferingin the determination of the amount of olive oil extracted, see 7.1.
If an unacceptable amount of interference is present thensuitability of one of the 'other fatty food simulants' should be examined, see annex A and 9.3 and 9.5 of EN 1186-1:2002.
If aninterference is present which would interfere with the triheptadecanoin internal standard an alternative internal standard shouldbe used, see annex A and 9.3 of EN 1186-1:2002.4 ReagentsNOTEAll reagents should be of recognized analytical quality, unless otherwise specified.4.1Olive oil, reference simulant D, as specified in 5.2 of EN 1186-1:2002.4.2Extraction solvent (see 10.1 of EN 1186-1:2002).4.2.1For non-polar plastics, such as polyethylene and polypropylene:- Pentane 98 % boiling point 36 °C.For polar plastics, such as polyamide and polyacetal:- 95/5 by volume azeotropic mixture of pentane 98 % and ethanol 99 %.NOTE 1Pentane is a very volatile and highly flammable solvent.
Care should therefore be taken when handling this solventto prevent contact with sources of ignition.
Ethanol is also a flammable solvent.
It is not recommended that extractions witheither pentane or the pentane/ethanol mixture be left unattended, particularly overnight.NOTE 2Due to the low boiling points of these solvents, cooled condenser water can be required to prevent undue loss of thesolvent from the condenser.4.2.2Other suitable solvent.NOTE 1In previous methods for determining overall migration into olive oil the extraction solvent used has been 1,1,2-trichloro-trifluoroethane.
For environmental reasons the use of this solvent should be avoided where possible, see 9.1 of EN1186-1.
Experience has shown that this solvent, although effective for most plastics requires longer periods of extraction.NOTE 2Some solvents can contain non-volatile substances which, after hydrolysis and methylation processes, produce gaschromatography peaks with retention times similar to the retention times of olive oil methyl esters and methyl heptadecanoatefrom the internal standard.
Solvents found to contain such substances should be redistilled before use.SIST EN 1186-2:2002
EN 1186-2:2002 (E)74.3Internal standard, triheptadecanoin (glyceryl trimargarate) CAS No. 2438-40-61) of a quality such that theproducts from hydrolysis and methylation processes do not contain substances giving detectable gaschromatography peaks (see 9.3 of EN 1186-1) with similar retention times to the olive oil methyl ester peaks.Prepared as a solution containing 2,0 mg/ml in cyclohexane.4.4Potassium hydroxide solution, 11,0 g/l in methanol.4.5Boron trifluoride, methanol complex, approximately 150 g/l BF3.4.6n -Heptane.4.7Sodium sulfate.4.7.1Sodium sulfate, anhydrous, Na2SO4.4.7.2Sodium sulfate, saturated solution.4.8Diethyl ether.4.9Karl Fischer solvent, commercially prepared, methanol and chloroform based, water capacity of 5 mg/ml.4.10Karl Fischer titrant (for volumetric apparatus only), commercially prepared, water capacity of 2 mg/ml.5 Apparatus5.1Cutting slab, clean smooth glass, metal or plastics slab of sufficient area to prepare test specimens,250 mm ´ 250 mm is suitable.5.2Tweezers, stainless steel, blunt nosed.5.3Cutting implement, scalpel, scissors, sharp knife or other suitable device.5.4Metal templates (100 mm ± 0,2 mm) ´ (100 mm ± 0,2 mm) (square).5.5Rule or template, 25 mm ± 1 mm wide.5.6Rule, graduated in millimetres, and with an accuracy of 0,1 mm.5.7Analytical balance capable of determining a change in mass of 0,1 mg.5.8Specimen supports, constructed of stainless steel with cross arms attached by welding or silver soldering.Stainless steel X4 CrNi 18 10 according to EN 10088 or of composition, chromium 17 %, nickel 9 %, carbon0,04 %, is suitable.
Before initial use thoroughly clean the steel supports. The use of a degreasing solvent andthen dilute nitric acid has been found to be suitable.NOTEThe 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 can be used.5.9Gauze, pieces of fine stainless steel gauze, with a mesh size of 1 mm have been found to be suitable,approximately 25 mm ´ 100 mm for insertion between the test pieces on the supports.
Before initial use thoroughlyclean the gauze, first with a degreasing solvent and then with dilute nitric acid.
1) The source of this is the Chemical Abstracts published by the American Chemical Society.SIST EN 1186-2:2002
EN 1186-2:2002 (E)85.10Conditioning containers, for conditioning test specimens at 50 % ± 5 % relative humidity and 80 % ± 5 %relative humidity at 20 °C ± 5 °C.NOTEFor 50 % relative humidity, 43 % w/v sulphuric acid solution in water is suitable and for 80 % relative humidity, 27 %w/v sulphuric acid solution is suitable. The solutions should be freshly prepared by adding a weighed amount of acid to asuitable volume of water, cooling to room temperature and making up to the required volume.It is recommended that relative humidity and temperature be maintained during the conditioning period.
Therefore thecontainers should be placed in a thermostatically controlled room or oven, at a temperature of approximately 20 °C, the settemperature should not vary by more than ± 1 °C.5.11 Glass tubes, ground neck and stoppers, for retaining the olive oil and test specimens. Tubes with an internaldiameter of approximately 35 mm and length in the range of 100 mm to 200 mm, excluding the ground neck, see7.2 of EN 1186-1:2002, have been found to be satisfactory.5.12Thermostatically controlled oven or incubator capable of maintaining the set temperature, within thetolerances specified in Table B.2 of EN 1186-1:2002.5.13Filter paper, lint-free.5.14Anti-bumping beads.5.15Soxhlet type extractors, capable of holding test specimens on the supports, with 250 ml or 500 ml roundbottom flasks to fit.NOTEAlternative extractors capable of satisfactorily extracting absorbed olive oil from the test specimens can be used.5.16Water bath, capable of holding the flasks of soxhlet type extractors (5.15)5.17Rotary evaporator or distillation apparatus, for evaporation and collection of the extraction solvent.NOTEArtificially cooled water can be necessary for efficient condensation of a low boiling point solvent.5.18Steam bath or water bath.5.19Flasks, 50 ml, long neck with condensers to fit, for methyl ester preparations.5.20Measuring cylinders, complying with the minimum requirements of ISO 4788, 500 ml, 250 ml, 100 ml, 25 ml,and 10 ml.
A 10 ml graduated syringe may be used in place of the 10 ml measuring cylinder.5.21Pipettes, complying with the minimum requirements of ISO 648, 5 ml and 10 ml.5.22Glass beads, 2 mm to 3 mm in diameter or glass rods, 2 mm to 3 mm in diameter and approximately100 mm long (see 7.2 of EN 1186-1:2002).5.23Gas chromatograph, with flame ionisation detector equipped with an appropriate column.
When using apolar column, the major peaks of olive oil, such as C16:0, methyl hexadecanoate (methyl palmitate), C16:1, methyl9-hexadecenoate (methyl palmitoate), C18:0, methyl octadecanoate (methyl stearate), C18:1, methyl 9-octadecenoate (methyl oleate), C18:2, methyl 9,12-octadecadienoate (methyl linoleate) and the internal standardC17:0, methyl heptadecanoate (methyl margarate) shall demonstrate baseline separation. Optionally, a non-polarcolumn can be used which shall give baseline separation of the methyl esters with 16 and 18 carbon numbers andthe internal standard with 17 carbon number.NOTEThe following columns have been found to be suitable:- Column 1, polar column, WCOT fused silica column, length 50 m, internal diameter 0,25 mm, coated with a 0,21micrometre film of cyanopropyl silicone;- Column 2, non polar column, BP1, length 25 m, internal diameter 0,32 mm, with a 1 micron film thickness;- Column 3, polar column, stainless steel column 2 mm to 3 mm internal diameter and 2 m to 3 m length with a packing of10 % to 20 % by mass of polyestersuccinate on a stationary phase of diatomaceous earth 80 mesh to 100 mesh.SIST EN 1186-2:2002
EN 1186-2:2002 (E)95.24Glass tubes with ground glass necks and stoppers, of a volume of approximately 10 ml, for storing theheptane layer if necessary.5.25Vacuum oven or vacuum desiccator, capable of maintaining a temperature of 60 °C ± 2 °C.
The vacuumoven or vacuum desiccator shall be equipped with or connected to a vacuum pump capable of achieving a vacuumof 1,3 kPa or less.
The vacuum pump shall be provided with a time controller to switch on the vacuum pump everyhour for 15 min.NOTEIf a vacuum oven is not available, a vacuum desiccator placed in an oven at 60 °C can be used.5.26Desiccator containing self indicating silica gel or anhydrous calcium chloride.5.27Balance, capable of determining a change of mass of 10 mg.5.28Disposable plastic syringes with luer fitting. 1 ml or 10 ml size.5.29Wide gauge luer needles (80 mm ´ 1.2 mm).5.30Karl Fischer apparatus, either an automated volumetric titrator, or an automated coulometric titrator.
TheKarl Fischer titrator shall be capable of measuring the water content of the simulant with a precision
(standarddeviation) of 10 mg/kg or less (equivalent to 1 mg/dm2 plastic).
An automated volumetric or coulometric instrumentshall be used.
Manual titration procedures do not give the required accuracy or precision.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.
Minimise handling of the samples and, where necessary, wear cottongloves.To ensure that test pieces are well separated and that their surfaces are freely exposed to olive oil during theperiod of the test, for thin films insert a piece of fine stainless steel gauze (5.9) between the test pieces or for thicksamples not placed on the supports, insert glass rods between the test pieces after immersion in the olive oil.Where specimen supports are used, label the supports with a tag bearing the test specimen identification.When preparing test specimens measure the surface area according to 8.3 of EN 1186-1:2002.6.2 Number of test specimensSeven test specimens are required for samples, in the form of thin films, sheets, cut sections from containers orsimilar articles.
Nine test specimens, similar dimensionally one to another, are required for samples of articles ofirregular shape.These test specimens are utilized as follows:a) four test specimens for the migration test;b) two test specimens to check for possible loss of volatiles;c) one test specimen to determine the suitability of olive oil as the fatty food simulant and triheptadecanoinas the internal standard (see annex A);SIST EN 1186-2:2002
EN 1186-2:2002 (E)10d) two test specimens for determination of the surface area, in the case of samples of irregular shape (see6.5).If the conditioning test in annex C is used, one additional test specimen is required.NOTEThe two test specimens, b), are used to check whether the sample losses mass from the evaporation of volatiles,such as solvents, during the test period.
If the vacuum drying procedure in annex C is used these test specimens are notrequired as during the vacuum drying any volatiles will have been removed from the test specimens.If previous testing has established that interference in the gas chromatography procedure is unlikely and annex A isomitted, one fewer test specimen will be required.A minimum of three valid test results is required to calculate the mean.
Testing in triplicate is allowed but in thiscase if one test result is invalid repeat the entire procedure.6.3 Films and sheetsLay the sample on the cutting slab (5.1) and cut test specimens of 1 dm², see 8.3 of EN 1186-1:2002, using the100 mm ´ 100 mm template (5.4).
Check, using the rule (5.6), that the dimensions of the test specimen are withinthe specified deviation (± 1 mm).Cut each test specimen into four test pieces 25 mm ´ 100 mm using the rule (5.5).
Assemble one test specimenonto the support by piercing suitable holes in the test pieces and placing two test pieces on each side of the crossarms of the support. Repeat this procedure for all remaining test specimens.6.4 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 the dimensions of each test specimen to the nearest 1 mm, using the rule, 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 (5.11). The test specimens or pieces are placed on thespecimen supports if these are appropriate or, if the test specimens or pieces are sufficiently rigid, they can betested unsupported.NOTECutting the test specimens into smaller pieces will increase the area of cut edges, so that the area of cut edgesexceeds 10 % of the of the test specimen area.
In this case see 8.3 of EN 1186-1:2002.6.5 Articles of irregular shapeSelect representative portions of the article, or multiples of the article for small articles, to give nine 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.7 Procedure7.1 GeneralDetermine the applicability of the method by carrying out the procedure described in annex A.
If prior tests haveestablished that the method is applicable then annex A may be omitted.Before weighing, discharge any build up of static electricity with an antistatic gun or other suitable means.SIST EN 1186-2:2002
EN 1186-2:2002 (E)117.2 Initial weighing of test specimens7.2.1Determine the need for conditioning of the test specimens by carrying out the procedure described inannex B or in annex C.
If prior tests have established that sample conditioning is not required then annex B andannex C
may be omitted.
If prior tests have established that the procedure described in annex D is applicable tothe sample, then annex B or annex C may be omitted.7.2.2If the tests described in annex B or annex C show that conditioning is not necessary, determine and recordthe mass of each test specimen.7.2.3If the tests described in annex B or annex C show that conditioning is necessary, follow the directions inthe relevant annex to determine the initial mass of the sample.7.2.4If the tests described in annex B show that conditioning is necessary, but constant mass cannot beachieved within five days then carry out the conditioning procedure described in C.3.1 or annex D.NOTE 1Long conditioning periods are not satisfactory due to oxidation of the olive oil which can occur upon prolongedconditioning.NOTE 2The conditioning procedures described in annex C and annex D may be used if it has been established that theseprocedures are more suited to the
polymer type under test.7.3 Exposure to food simulantTake six of the glass tubes (5.11), ma
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