SIST EN 1186-12:2002
(Main)Materials and articles in contact with foodstuffs - Plastics - Part 12: Test methods for overall migration at low temperatures
Materials and articles in contact with foodstuffs - Plastics - Part 12: Test methods for overall migration at low temperatures
This part of this European Prestandard describes test methods for the determination of the overall migration from plastics intended to come into contact with foodstuffs at low temperatures, for 0.5 h, 1 h, 2 h, 24 h and 10 days at 5 °C or at 20 °C. These test methods are suitable for plastics samples in a wide variety of forms. The fatty food simulant used in these methods is dewaxed sunflower oil since, unlike olive oil, it remains liquid at the lower test temperatures.
Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Kunststoffe - Teil 12: Prüfverfahren für die Gesamtmigration bei tiefen Temperaturen
1 Anwendungsbereich
Dieser Teil dieser Europäischen Norm beschreibt Prüfverfahren für die Bestimmung der Gesamtmigration in fettige Prüflebensmittel aus Werkstoffen und Gegenständen aus Kunststoff durch völliges Eintauchen der Prüfmuster in ein fettiges Prüflebensmittel bei Temperaturen von 5 °C bis einschließlich 20 °C innerhalb ausgewählter Zeiten.
Dieses Verfahren eignet sich am besten für Kunststoffe in Form von Folien und Platten, es kann aber auf ein breites Spektrum an Gegenständen oder Behälter angewandt werden, aus denen Prüfstücke von geeigneter Größe geschnitten werden können.
Das in diesen Prüfverfahren verwendete fettige Prüflebensmittel ist entwachstes Sonnenblumenöl, das, im Unter-schied zu Olivenöl, bei der niedrigeren Prüftemperatur flüssig bleibt.
Das beschriebene Prüfverfahren ist auf die meisten Kunststoffsorten anwendbar, obgleich es einige Kunststoffe gibt, für die es bekanntermaßen nicht anwendbar ist.
Matériaux et objets en contact avec les denrées alimentaires - Matiere plastique - Partie 12: Méthodes d'essai pour la migration globale a basses températures
La présente partie de cette norme européenne spécifie une méthode d'essai de vérification de la migration globale dans les simulants gras des matériaux et objets en matiere plastique par immersion totale d'éprouvettes dans un simulant gras a des températures comprises entre 5 °C et 20 °C inclus 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.
Le simulant gras utilisé pour cette méthode d'essai est de l'huile de tournesol déparaffinée dans la mesure ou cette huile, a la différence de l'huile d'olive, reste liquide a basse température.
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 - 12. del: Preskusne metode za celotno migracijo pri nizkih temperaturah
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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 - 12. del: Preskusne metode za celotno migracijo pri nizkih temperaturahWerkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Kunststoffe - Teil 12: Prüfverfahren für die Gesamtmigration bei tiefen TemperaturenMatériaux et objets en contact avec les denrées alimentaires - Matiere plastique - Partie 12: Méthodes d'essai pour la migration globale a basses températuresMaterials and articles in contact with foodstuffs - Plastics - Part 12: Test methods for overall migration at low temperatures67.250Materiali in predmeti v stiku z živiliMaterials and articles in contact with foodstuffsICS:Ta slovenski standard je istoveten z:EN 1186-12:2002SIST EN 1186-12:2002en01-september-2002SIST EN 1186-12:2002SLOVENSKI
STANDARDSIST ENV 1186-12:19971DGRPHãþD
SIST EN 1186-12:2002
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 1186-12April 2002ICS 67.250Supersedes ENV 1186-12:1995English versionMaterials and articles in contact with foodstuffs - Plastics - Part12: Test methods for overall migration at low temperaturesMatériaux et objets en contact avec les denréesalimentaires - Matière plastique - Partie 12: Méthodesd'essai pour la migration globale à basses températuresWerkstoffe und Gegenstände in Kontakt mit Lebensmitteln- Kunststoffe - Teil 12: Prüfverfahren für dieGesamtmigration bei tiefen TemperaturenThis 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 1186-12:2002 ESIST EN 1186-12:2002
EN 1186-12:2002 (E)2ContentspageForeword.31Scope.52Normative references.53Overall migration into dewaxed sunflower oil by total immersion.54Overall migration into dewaxed sunflower oil by cell.85Overall migration into dewaxed sunflower oil using a pouch.116Overall migration into dewaxed sunflower oil by article filling.14Annex ZA (informative)
Relationship of this European Standard with Council Directive 89/109/EECand Commission Directive 90/128/EEC and associated Directives.17Bibliography.19SIST EN 1186-12:2002
EN 1186-12:2002 (E)3ForewordThis document EN 1186-12:2002 has been prepared by Technical Committee CEN/TC 194 "Utensils in contactwith food", the secretariat of which is held by BSI.This European Standard shall be given the status of a national standard, either by publication of an identical text orby endorsement, at the latest by October 2002, and conflicting national standards shall be withdrawn at the latestby October 2002.This document supersedes ENV 1186-12:1995.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 1186-12 should be read in conjunction with EN 1186-1, EN 1186-2, EN 1186-4, EN 1186-6 and EN 1186-8.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 food simulants by article fillingPart 10Test methods for overall migration into olive oil (modified method for use in cases whereincomplete
extraction of dewaxed sunflower oil occurs)SIST EN 1186-12:2002
EN 1186-12:2002 (E)4Part 11Test methods for overall migration into mixtures of
14C-labelled synthetic triglyceridePart 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 % ethanolAccording 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 1186-12:2002
EN 1186-12:2002 (E)51 ScopeThis Part of this European Standard specifies 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 from 5 °C, up to and including 20 °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.The fatty food simulant used in these test methods is dewaxed sunflower oil since, unlike olive oil, remains liquid atthe lower test temperature.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 food – Plastics – Part 1: Guide to the selection of conditionsand test methods for overall migration.EN 1186-2:2002, Materials and articles in contact with food – Plastics – Part 2: Test methods for overall migrationinto olive oil by total immersion.EN 1186-4:2002, Materials and articles in contact with food – Plastics – Part 4: Test methods for overall migrationinto olive oil by cell.EN 1186-6:2002, Materials and articles in contact with food – Plastics – Part 6: Test methods for overall migrationinto olive oil using a pouch.EN 1186-8:2002, Materials and articles in contact with food – Plastics – Part 8: Test methods for overall migrationinto olive oil by article filling.3 Overall migration into dewaxed sunflower oil by total immersion3.1 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 dewaxed sunflower oil for the exposure time, at temperatures from5 °C up to and including 20 °C, then taken from the dewaxed sunflower oil, blotted to remove oil adhering to thesurface, and reweighed.SIST EN 1186-12:2002
EN 1186-12:2002 (E)6The specimens can usually retain absorbed dewaxed sunflower oil that is extracted and determined quantitativelyby means of gas chromatography 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 dewaxed sunflower oil from the testspecimens.
This ensures that any active or extractable components of the plastics react with the internal standard,as well as with the extracted dewaxed sunflower oil. The internal standard is also subjected to the hydrolysis andmethylation reactions, providing compensation for any inefficiencies in the hydrolysis and methylation processes.Migration into the dewaxed sunflower oil is calculated by subtracting the mass of dewaxed sunflower oil retained bythe test specimen from the mass of the test specimen after removal from the dewaxed sunflower oil, thensubtracting this mass from the initial mass of the specimen.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 dewaxed sunflower oil extracted, see 7.1 of EN 1186-2:2002.
If an unacceptable amountof interference is present then suitability of one of the 'other fatty food simulants' should be examined, see annex A of EN 1186-2:2002 and 9.3 and 9.5 of EN 1186-1:2002.
If an interference is present which would interfere with the triheptadecanoin internalstandard an alternative internal standard should be used, see annex A of EN 1186-2:2002, and 9.3 of EN 1186-1:2002.3.2 ReagentsThe reagents shall be as described in clause 4 of EN 1186-2:2002, except that olive oil, reference simulant D, asspecified in 4.1 of EN 1186-1:2002 is replaced by dewaxed sunflower oil, simulant D.3.3 ApparatusThe apparatus shall be as described in clause 5 of EN 1186-2:2002.3.4 Preparation of test specimensThe test specimens shall be prepared as described in clause 6 of EN 1186-2:2002.3.5 Procedure3.5.1 GeneralDetermine the applicability of the method by carrying out the procedure described in annex A of EN 1186-2:2002.If prior tests have established that the method is applicable then annex A of EN 1186-2:2002 may be omitted.Before weighing, discharge any build up of static electricity with an antistatic gun or other suitable means.3.5.2 Initial weighing of test specimensPerform the initial weighing in accordance with 7.2 of EN 1186-2:2002.SIST EN 1186-12:2002
EN 1186-12:2002 (E)73.5.3 Exposure to food simulantTake six of the glass tubes (5.11 of EN 1186-2:2002), mark them for identification purposes.
Measure100 ml ± 5 ml of dewaxed sunflower oil (4.1 of EN 1186-2:2002, see 3.2) into each tube by measuring cylinder andstopper the tube.NOTE.1If the procedure described in annex D of EN 1186-2:2002 is used, it can be necessary to dry all of the dewaxedsunflower oil used for the migration test, see D.3.2.of EN 1186-2:2002.Alternatively mark the tubes for a volume of 100 ml and fill with dewaxed sunflower oil to the mark.
Place into oneof the tubes a thermometer or thermocouple and stopper the tubes.
Two extra tubes with a minimum of 50 ml ofdewaxed sunflower oil are required as blank simulant, if the procedure described in annex D of EN 1186-2:2002 isused.
Place the six or eight tubes, and two empty tubes, in the thermostatically controlled oven or incubator (5.12of EN 1186-2:2002) set at the test temperature.
Leave until the dewaxed sunflower oil has attained the testtemperature, using the thermometer or thermocouple to monitor the temperature.
Take all tubes from the oven andplace into four of the tubes containing dewaxed sunflower oil, weighed test specimens prepared as in clause 6 andconditioned if necessary. Stopper the tubes.
Ensure that the test specimens are totally immersed in dewaxedsunflower oil; if they are not, then add either glass beads or glass rods (5.22 of EN 1186-2:2002) to raise the levelof the dewaxed sunflower oil until total immersion is achieved.NOTE 2The dewaxed sunflower oil in the fifth tube is used as a reference standard in constructing the calibration graph andif the procedure described in annex D of EN 1186-2:2002 is used, as the third blank sample for Karl Fischer titrations. Thedewaxed sunflower oil in the sixth tube is used to check the temperature of the oil.
If glass beads or glass rods have been usedto raise the level of the dewaxed sunflower oil to achieve total immersion, then similar glass beads or glass rods should beadded to the sixth tube.Place the remaining two test specimens into the empty tubes and stopper.NOTE 3These two test specimens are used to check whether the sample loses mass from the evaporation of volatiles, suchas water, solvents and oligomers, during the test period.
If the vacuum drying procedure described in annex C ofEN 1186-2:2002 is applicable these test specimens are not required as during the vacuum drying volatiles will have beenremoved from the test specimens.Replace all eight or ten tubes in the thermostatically controlled oven or incubator set at the test temperature.
Thispart of the operation should be carried out in the minimum time possible to prevent undue heat loss.
Observe thetemperature of the thermostatically controlled oven or incubator or the dewaxed sunflower oil (see NOTE 5) in thesixth tube and leave the tubes for the selected test period, taking into account the tolerances specified in Table B.1of EN 1186-1:2002, after the dewaxed sunflower oil in the sixth tube has reached a temperature within thetolerance specified in Table B.2 of EN 1186-1:2002.NOTE 4Annex 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.NOTE 5For exposure times of 24 h or more it is acceptable to monitor the temperature of the air bath of the thermostaticallycontrolled oven or incubator or refrigerator, instead of the temperature of the simulant.Take the tubes from the oven or incubator and immediately remove the test specimens from the tubes.
For thosespecimens which have been in dewaxed sunflower oil, allow the oil to drain.
Remove any adhering dewaxedsunflower oil by gently pressing between filter papers (5.13 of EN 1186-2:2002).
Repeat the pressing procedureuntil the filter paper shows no spots of dewaxed sunflower oil.
For test specimens on supports, remove theindividual test pieces from the supports to carry out this operation.
Clean the supports of oil by washing with theextraction solvent and replace the test pieces on them.NOTE 6If the procedure described in annex D of EN 1186-2:2002 is followed, the tubes containing the oil should beretained. The tubes should be capped to prevent further change in the moisture content of the oil and the Karl Fischerdetermination of water content should be carried out as soon as possible.3.5.4 Final weighing of test specimensPerform the final weighing in accordance with 7.4 of EN 1186-2:2002.SIST EN 1186-12:2002
EN 1186-12:2002 (E)83.5.5 Extraction of absorbed dewaxed sunflower oilExtract the dewaxed sunflower oil in accordance with 7.5 of EN 1186-2:2002.3.5.6 Determination of extracted dewaxed sunflower oilDetermine the extracted dewaxed sunflower oil in accordance with 7.6 of EN 1186-2:2002.3.6 Expression of results3.6.1 Method of calculationExpress the results in accordance with 8.1 of EN 1186-2:2002.3.6.2 PrecisionSee annex F of EN 1186-2:2002.3.7 Test reportPrepare the test report in accordance with clause 9 of EN 1186-2:2002.4 Overall migration into dewaxed sunflower oil by cell4.1 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 3, 4 and 5 of EN1186-1:2002.Test specimens of known mass are exposed in a cell to dewaxed sunflower oil for the exposure time, attemperatures above 5 °C and below 20 °C, then taken from the cell, blotted to remove oil adhering to the surface,and reweighed.The specimens will usually retain absorbed dewaxed sunflower oil that is extracted and determined quantitativelyby means of gas chromatography 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 dewaxed sunflower oil from the testspecimens.
This ensures that any active or extractable components of the plastics react with the internal standard,as well as with the extracted dewaxed sunflower oil. The internal standard is also subjected to the hydrolysis andmethylation reactions, providing compensation for any inefficiencies in the hydrolysis and methylation processes.Migration into the dewaxed sunflower oil is calculated by subtracting the mass of dewaxed sunflower oil retained bythe test specimen from the mass of the test specimen after removal from the dewaxed sunflower oil, thensubtracting this mass from the initial mass of the specimen.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 which are applicable to certain plastics.SIST EN 1186-12:2002
EN 1186-12:2002 (E)9NOTEBefore starting a migration exercise, the test sample should be examined for the presence of components interferingin the determination of the amount of dewaxed sunflower oil extracted, see 7.1 of EN 1186-2:2002.
If an unacceptable amountof interference is present then suitability of one of the 'other fatty food simulants' should be examined, see annex A of EN 1186-4:2002 and 9.3 and 9.5 of EN 1186-1:2002.
If an interference is present which would interfere with the triheptadecanoin internalstandard an alternative internal standard should be used, see annex A of EN 1186-4:2002, and 9.3 of EN 1186-1:2002.4.2 ReagentsThe reagents shall be as described in clause 4 of EN 1186-4:2002, except that olive oil, reference simulant D, asspecified in 4.1 of EN 1186-1:2002 is replaced by dewaxed sunflower oil, simulant D.4.3 ApparatusThe apparatus shall be as described in clause 5 of EN 1186-4:2002.4.4 Preparation of test specimensThe test specimens shall be prepared as described in clause 6 of EN 1186-4:2002.4.5 Procedure4.5.1 GeneralDetermine the applicability of the method by carrying out the procedure described in annex A of EN 1186-4:2002.If prior tests have established that the method is applicable then annex A of EN 1186-4:2002 may be omitted.Before weighing, discharge any build up of static electricity with an antistatic gun or other suitable means.4.5.2 Initial weighing of test specimensPerform the initial weighing in accordance with 7.2 of EN 1186-4:2002.4.5.3Exposure to food simulantTake four type A cells (5.6 of EN 1186-4:2002), mark them for identification purposes.
Place in the thermostaticallycontrolled oven or incubator (5.9 of EN 1186-4:2002), which is set at the test temperature and leave until the testtemperature has been attained.Take five glass tubes (5.8 of EN 1186-4:2002), measure 125 ml ± 5 ml of dewaxed sunflower oil (4.1 ofEN 1186-4:2002) into each tube by measuring cylinder and stopper the tubes.NOTE 1If the procedure described in annex D of EN 1186-4:2002 is used, it can be necessary to dry all of the dewaxedsunflower oil used for the migration test, see D.3.2 of EN 1186-4:2002.Alternatively mark the tubes for a volume of 125 ml and fill with dewaxed sunflower oil to the mark.
Place into oneof the tubes a thermometer or thermocouple and stopper the tubes.
Two extra tubes with a minimum of 50 ml ofdewaxed sunflower oil are required as blank simulant, if the procedure in annex D of EN 1186-4:2002 is used.Place the five or seven tubes, and two empty tubes, in the thermostatically controlled oven or incubator (5.9 of EN1186-4:2002) set at the test temperature.
Leave until the dewaxed sunflower oil has attained the test temperature,using the thermometer or thermocouple to monitor the temperature.Remove the cells from the thermostatically controlled oven or incubator, dismantle the cells and place on the baseof each cell one of the test specimens.
Reassemble the cells, ensuring that the clamping screw wheel is welltightened down.Remove four tubes containing 125 ml of dewaxed sunflower oil from the thermostatically controlled oven orincubator or refrigerator and transfer the dewaxed sunflower oil from each tube to each of the cells through the fillerSIST EN 1186-12:2002
EN 1186-12:2002 (E)10hole.
Remove the thermometer or thermocouple from the tube and insert, if applicable see NOTE 5, in one of thecells and replace the filler plugs.NOTE 2The dewaxed sunflower oil in the fifth tube is used as a reference standard in constructing the calibration graph (see7.6.6 of EN 1186-4:2002) and if the procedure in annex D of EN 1186-4:2002 is used, as the third blank sample for Karl Fischertitrations.
The dewaxed sunflower oil in the sixth tube is used to check the temperature of the oil.
If glass beads or glass rodshave been used to raise the level of the dewaxed sunflower oil to achieve total immersion, then similar glass beads or glassrods should be added to the sixth tube.Remove the two empty tubes from the thermostatically controlled oven or incubator or refrigerator and place ineach tube one of the remaining two test specimens and stopper.NOTE 3These two test specimens are used to check whether the sample loses mass from the evaporation of volatiles, suchas water, solvents and oligomers, during the test period.
If the vacuum drying procedure in annex C of EN 1186-4:2002 isapplicable these test specimens are not required as during the vacuum drying volatiles will have been removed from the testspecimens.Replace the four cells and the two tubes in the thermostatically controlled oven or incubator set at the testtemperature. This part of the operation should be carried out in the minimum time to prevent undue heat loss fromthe cells and dewaxed sunflower oil.
Observe the temperature of the thermostatically controlled oven or incubatoror the dewaxed sunflower oil (see NOTE 5) in the one of the cells and leave the cells and tubes for the selectedtest period, taking into account the tolerances specified in Table B.1 of EN 1186-1:2002, after the dewaxedsunflower oil in the cell has reached a temperature within the tolerance specified in Table B.2 of EN 1186-1:2002.NOTE 4Annex 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.NOTE 5For exposure times of 24 h or more it is acceptable to monitor the temperature of the air bath of the thermostaticallycontrolled oven or incubator or refrigerator, instead of the temperature of the simulant.Take the cells and tubes from the oven or incubator and immediately remove the test specimens from the cells.For those specimens which have been in dewaxed sunflower oil, allow the oil to drain.
Remove any adheringdewaxed sunflower oil by gently pressing between filter papers (5.10 of EN 1186-4:2002).
Repeat the pressingprocedure until the filter paper shows no spots of dewaxed sunflower oil.NOTE 6If the procedure in annex D of EN 1186-4:2002 is followed, the tubes containing the oil should be retained. Thetubes should be capped to prevent further change in the moisture content of the oil and the Karl Fischer determination of watercontent should be carried out as soon as possible.4.5.3 Final weighing of test specimensPerform the final weighing according to 7.4 of EN 1186-4:2002.4.5.4 Extraction of absorbed dewaxed sunflower oilExtract the dewaxed sunflower oil in accordance with 7.5 of EN 1186-4:2002.4.5.5 Determination of extracted dewaxed sunflower oilDetermine the extracted dewaxed sunflower oil in accordance with 7.6 of EN 1186-4:2002.4.6 Expression of results4.6.1 Method of calculationExpress the results in accordance with 8.1 of EN 1186-4:2002.SIST EN 1186-12:2002
EN 1186-12:2002 (E)114.6.2 PrecisionSee annex F of EN 1186-4:2002.4.7 Test reportPrepare the test report in accordance with clause 9 of EN 1186-4:2002.5 Overall migration into dewaxed sunflower oil using a pouch5.1 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 3, 4 and 5 ofEN 1186-1:2002.Test specimens of known mass and in the form of pouches are filled with dewaxed sunflower oil for the exposuretime, at temperatures from 5 °C up to and including 20 °C, then the dewaxed sunflower oil is removed, the pouchescut open and the dewaxed sunflower oil adhering to the surface is removed by blotting.
The cut portion of eachpouch is then reweighed,The specimens will usually retain absorbed dewaxed sunflower oil that is extracted and determined quantitativelyby means of gas chromatography 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 dewaxed sunflower oil from the testspecimens.
This ensures that any active or extractable components of the plastics react with the internal standard,as well as with the extracted dewaxed sunflower oil. The internal standard is also subjected to the hydrolysis andmethylation reactions, providing compensation for any inefficiencies in the hydrolysis and methylation processes.Migration into the dewaxed sunflower oil is calculated by subtracting the mass of dewaxed sunflower oil retained bythe test specimen from the mass of the test specimen after removal from the dewaxed sunflower oil, thensubtracting this mass from the initial mass of the specimen.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 conta
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