SIST-TS CEN/TS 14234:2003
(Main)Materials and articles in contact with foodstuffs - Polymeric coatings on paper and board- Guide to the selection of conditions and test methods for overall migration
Materials and articles in contact with foodstuffs - Polymeric coatings on paper and board- Guide to the selection of conditions and test methods for overall migration
This Technical Specification specifies test methods for 'alternative tests' and 'substitute tests' performed with volatile test media, iso-octane and a volume fraction of 95 % aqueous ethanol, for the determination of overall migration from polymeric coatings on paper and board intended to come into contact with fatty foodstuffs.
NOTE 1 It also includes guidance for the application of Council Directive 82/711/EEC [1], as last amended by Commission Directives 93/8/EC and 97/48/EC [2] [3] as regards the determination of the specific and overall migration into fatty food simulants (fat test) and includes a glossary to clarify the terminology used, see annex B.
NOTE 2 The iso-octane and a volume fraction of 95 % aqueous ethanol volatile test media used in these test methods are those specified for 'substitute tests' in Council Directive 82/711/EEC and its subsequent amendments. In addition to the use of iso-octane and 95 % v/v aqueous ethanol as test media for 'substitute tests', Council 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. A test method for overall migration from polymeric coatings intended to come into contact with fatty foodstuffs using modified polyphenylene oxide (MPPO) is in preparation.
Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Polymere Beschichtungen auf Papier und Pappe - Leiftaden für die Auswahl von Prüfbedingungen und Prüfverfahren für die Gesamtmigration
Diese CEN Technische Spezifikation legt mit flüchtigen Prüfmedien, Isooctan und 95%igem (Volumenanteil) wässrigem Ethanol, durchgeführte Prüfverfahren für "alternative Prüfungen" und "Ersatzprüfungen" fest, zur Bestimmung der Gesamtmigration aus polymeren Beschichtungen auf Papier oder Pappe, die dafür vorgesehen sind, in Kontakt mit fetthaltigen Lebensmitteln zu kommen.
ANMERKUNG 1 Sie enthält auch eine Anleitung für die Anwendung der Richtlinie 82/711/EWG des Rates [1], zuletzt geändert durch die Richtlinien 93/8/EWG und 97/48/EU der Kommission [2], [3], was die Bestimmung der spezifischen und Gesamtmigration in fettige Prüflebensmittel (Fetttest) betrifft und enthält ein Wörterverzeichnis zur Erklärung der angewandten Terminologie, siehe Anhang B.
ANMERKUNG 2 Die in diesen Prüfverfahren verwendeten flüchtigen Prüfmedien Isooctan und 95%iges (Volumenanteil) wässriges Ethanol sind die in der Richtlinie 82/711/EWG des Rates und deren nachfolgenden Änderungsrichtlinien für "Ersatzprüfungen" festgelegten. Zusätzlich zu der Verwendung von Isooctan und 95%igem (Volumenanteil) wässrigem Ethanol als Prüfmedien für die "Ersatzprüfungen" wird in der Richtlinie 82/711/EWG des Rates und deren nachfolgenden Änderungsrichtlinien die Verwendung von modifiziertem Polyphenylenoxid als Prüfmedium bei Temperaturen von 100 °C und mehr festgelegt. Ein Prüfverfahren für die Gesamtmigration aus polymeren Beschichtungen, die für den Kontakt mit fettigen Lebensmitteln vorgesehen sind, unter Verwendung von modifiziertem Polyphenylenoxid (MPPO) wird derzeit ausgearbeitet.
Matériaux et objets en contact avec les denrées alimentaires - Revetements polymeres sur papier et carton - Guide pour le choix des conditions et des méthodes d'essai en matiere de migration globale
La présente Spécification Technique spécifie des méthodes d'essai pour des " essais de remplacement " et des " essais de substitution " utilisant des milieux volatiles composés de l'iso-octane et de l'éthanol a 95 % en milieu aqueux, pour la détermination de la migration globale dans les revetements polymeres sur du papier et du carton destinés a entrer en contact avec des aliments gras.
NOTE 1 Elle comprend également des lignes directrices pour l'application de la Directive du Conseil 82/11/CEE [1], ainsi que les Directives 93/8/CE et 97/48/CE [2] et [3] récemment amendées par la Commission en matiere de détermination de migration globale et spécifique dans les simulants gras (essai avec des simulants gras) et comprend un glossaire pour clarifier la terminologie utilisée, voir annexe B.
NOTE 2 Les milieux d'essai d'éthanol a 95 % en solution aqueuse et d'iso-octane a utiliser dans les présentes méthodes d'essai sont ceux indiqués pour les " essais de substitution " dans la Directive du Conseil 82/711/CEE et ses amendements ultérieurs. En plus de l'utilisation d'iso-octane et d'éthanol a 95 % en milieu aqueux en tant que milieux d'essai pour les " essais de substitution ", la Directive du Conseil 82/711/CEE et ses amendements ultérieurs spécifient l'utilisation d'oxyde de polyphénylene modifié en tant que milieu d'essai devant etre utilisé a des températures supérieures ou égales a 100 °C. Une méthode d'essai pour la migration globale dans les revetements polymeres destinés a entrer en contact avec des aliments gras a l'aide d'oxyde de polyphénylene modifié est en cours d'élaboration.
NOTE 3 Ces méthodes d'essai peuvent également etre utilisées pour les " essais de remplacement " décrits dans la Directive du Conseil 82/711/CEE et ses amendements ultérieurs lorsque les milieux d'essai volatiles choisis sont de l'iso-octane et de l'éthanol a 95 % en milieu aqueux, voir l'ENV 1186-1.
Une suggestion de protocole d'essai est donnée a la Figure A.1. Si les résultats d
Materiali in predmeti v stiku z živili – Polimerne prevleke na papirju in kartonu - Vodilo za izbiro pogojev in preskusnih metod za celotno migracijo
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
SIST-TS CEN/TS 14234:2003
01-julij-2003
Materiali in predmeti v stiku z živili – Polimerne prevleke na papirju in kartonu -
Vodilo za izbiro pogojev in preskusnih metod za celotno migracijo
Materials and articles in contact with foodstuffs - Polymeric coatings on paper and board-
Guide to the selection of conditions and test methods for overall migration
Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln - Polymere Beschichtungen
auf Papier und Pappe - Leiftaden für die Auswahl von Prüfbedingungen und
Prüfverfahren für die Gesamtmigration
Matériaux et objets en contact avec les denrées alimentaires - Revetements polymeres
sur papier et carton - Guide pour le choix des conditions et des méthodes d'essai en
matiere de migration globale
Ta slovenski standard je istoveten z: CEN/TS 14234:2002
ICS:
67.250 Materiali in predmeti v stiku z Materials and articles in
živili contact with foodstuffs
SIST-TS CEN/TS 14234:2003 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST-TS CEN/TS 14234:2003
TECHNICAL SPECIFICATION
CEN/TS 14234
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
October 2002
ICS 67.250
English version
Materials and articles in contact with foodstuffs — Polymeric
coatings on paper and board — Guide to the selection of
conditions and test methods for overall migration
Matériaux et objets en contact avec les denrées Werkstoffe und Gegenstände in Kontakt mit Lebensmitteln
alimentaires – Revêtements polymères sur papier et carton - Polymere Beschichtungen auf Papier und Pappe –
– Guide pour le choix des conditions et des méthodes Leiftaden für die Auswahl von Prüfbedingungen und
d’essai en matière de migration globale Prüfverfahren für die Gesamtmigration
This Technical Specification (CEN/TS) was approved by CEN on 28 July 2002 for provisional application.
The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to submit their
comments, particularly on the question whether the CEN/TS can be converted into a European Standard.
CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS available. It
is permissible to keep conflicting national standards in force (in parallel to the CEN/TS) until the final decision about the possible
conversion of the CEN/TS into an EN is reached.
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 STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels
© 2002 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 14234:2002 E
worldwide for CEN national Members.
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Contents
Foreword.3
1 Scope .4
2 Normative references .5
3 Test conditions .5
4 Total immersion method .6
5 Cell method.9
6 Expression of results .12
7 Test report .13
Annex A (normative) Proposed test scheme for papers with polymeric coatings intended for fatty food
contact. .14
Annex B (informative) Guidance for migration testing of polymeric coatings on cellulosic substrates
(paper and board) .15
Annex ZA (informative) Relationship of this Technical Specification with Council Directive 89/109/EEC
and associated EU Directive(s) .23
Bibliography .25
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Foreword
This document (CEN/TS 14234:2002) has been prepared by Technical Committee CEN/TC 194, "Utensils in
contact with food", the secretariat of which is held by BSI.
This document has been prepared under a mandate given to CEN by the European Commission and the European
Free Trade Association, and supports essential requirements of EU Directive(s).
For relationship with EU Directive(s), see informative annex ZA, which is an integral part of this document.
In this standard the Annex A is normative and Annex B is informative.
Guidance for migration testing of polymeric coatings on cellulosic substrates (paper and board) is given in the
informative annex B.
At the time of preparation and publication of this Technical Specification the European Union legislation relating to
resinous and polymeric coatings on paper and board has not been formulated.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to announce this Technical Specification: Austria, Belgium, Czech Republic, Denmark,
Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal,
Spain, Sweden, Switzerland and the United Kingdom.
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1 Scope
This Technical Specification specifies test methods for 'alternative tests' and 'substitute tests' performed with
volatile test media, iso-octane and a volume fraction of 95 % aqueous ethanol, for the determination of overall
migration from polymeric coatings on paper and board intended to come into contact with fatty foodstuffs.
NOTE 1 It also includes guidance for the application of Council Directive 82/711/EEC [1], as last amended by Commission
Directives 93/8/EC and 97/48/EC [2] [3] as regards the determination of the specific and overall migration into fatty food
simulants (fat test) and includes a glossary to clarify the terminology used, see annex B.
NOTE 2 The iso-octane and a volume fraction of 95 % aqueous ethanol volatile test media used in these test methods are
those specified for 'substitute tests' in Council Directive 82/711/EEC and its subsequent amendments. In addition to the use of
iso-octane and 95 % v/v aqueous ethanol as test media for 'substitute tests', Council 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.
A test method for overall migration from polymeric coatings intended to come into contact with fatty foodstuffs using modified
polyphenylene oxide (MPPO) is in preparation.
NOTE 3 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 a volume fraction of 95 % aqueous ethanol,
see ENV 1186-1.
A suggested test scheme is given in Figure A.1. If the test result obtained by the total immersion method, described
in clause 4 of this Technical Specification, exceeds the allowed overall migration limit the single-sided migration
test using a cell, see clause 5, if technically feasible; may be used. If it is not possible to use the single sided cell
method, e.g. because of pinholes, use adsorption by modified polyphenylene oxide, (MPPO).
Iso-octane is used as a test medium for test samples coated with non polar food contact layers, such as
polyolefins. For test samples coated with polar food contact polymers such as polyamide and polyethylene
terephthalate, a volume fraction of 95 % aqueous ethanol is used. For polystyrenes, plasticised polyvinyl chloride
and other polymers where the identification or polarity of the polymer is not clear, two parallel tests shall be
conducted using both of the proposed test media and taking the higher value obtained as the relevant result.
NOTE 4 The nature of the food contact layer determines the selection of the test medium(a).
NOTE 5 The overall migration limit for materials and articles of an all polymeric construction is specified in Commission
Directive 90/128/EEC [4] and the conditions of test in Council Directive 82/711/EEC [1] and its subsequent amendments, [2],[3].
There is an expectation that the scope of this directive will be extended to cover polymeric coatings on paper and board.
The 'substitute tests' described in this Technical Specification are by total immersion, see clause 4 and in a
migration cell, see clause 5.
NOTE 6 The test conditions are those described in Council Directive 82/711/EEC [1] and its subsequent amendments,
[2],[3].
The 'alternative test' methods described here specifies a rapid extraction test with a 'more severe' test character,
for the assessment of the overall migration into fatty food simulants. The method differs from the substitute test
methods only in the combination of test time and test temperature. The method is based on the determination of
the extraction of migrateable substances from polymeric coated paper or board, which are intended to come into
contact with foodstuffs, by total immersion in non-polar, iso-octane, and/or polar, ethanol, solvents depending on
the polarity of the polymeric coating. According to the results obtained by this method, see [5],[6],[7],[8],[9] and
taking physio-chemical considerations into account, the obtained extraction efficiency has, generally, been found to
be equivalent to or higher than overall migration results obtained using fat simulant D,under the test conditions, 10
days at 40 °C, 2 h at 70 °C, 1 h at 100 °C, 30 min at 121 °C and 30 min at 130 °C.
NOTE 7 This method is not applicable to test materials intended for applications over 130 °C. Test materials intended for
applications over 70 °C have to be checked for their physical suitability at the intended time and temperature of use.
The test method should be applied to polymer coated packagings where the polymer layer is less than 300 μm in
thickness. However, if this extraction test is applied to materials with coatings with higher thickness than 300 μm
and the result does not exceed any allowed overall migration limit then the method is considered to be suitable for
those materials.
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In those cases where the rapid extraction test by total immersion, yields total extraction values that exceed the
overall migration limit or may be technically unsuitable a cell test method using the same time and temperature
conditions is applicable. This cell test method should primarily only be applied to packagings with a physical barrier
layer (for instance of aluminium or other material to prevent penetrative loss of test medium) and which have a
thinner food contact layer than 300 μm. This test method can not be applied if the polymeric coating is shown to
have pinholes.
2 Normative references
This Technical Specification incorporates by dated and undated reference, provisions from other publications.
These normative references are cited at the appropriate places in the text and the publications are listed hereafter.
For dated references, subsequent amendments to and revisions of any of these publications apply to this Technical
Specification only when incorporated in it by amendment or revision. For undated references the latest edition of
the publication referred to applies (including amendments).
ENV 1186-1:1994 Materials and articles in contact with foodstuffs – Plastics - Guide to the selection of
conditions and test methods for overall migration
ISO 648 Laboratory glassware – One-mark pipettes
ISO 4788 Laboratory glassware - Graduated measuring cylinders
3 Test conditions
3.1 ´Substitute test´ methods
For substitute tests, the conditions of test will be determined by the conditions of use, see clauses 4, 5 and 6 of
ENV 1186-1:1994.
3.2 ´Alternative test’ methods
For alternative tests, the test medium (a) and test conditions are to be selected according to the nature of the
polymeric coating as given by Table 1.
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Table 1 — Use of test media and test conditions for alternative tests
Polymer type of food contact layer Test medium to be applied Test conditions to be applied
Polyolefins and copolymers iso-octane 24 h at 40 °C
Polyamides 95 % ethanol 24 h at 40 °C
Polystyrene iso-octane and 95 % ethanol 24 h at 40 °C
Polyethylene terephthalate 95 % ethanol 24 h at 50 °C
Polyvinyl chloride (plasticised) iso-octane and 95 % ethanol 24 h at 40 °C
Polyvinyl chloride (rigid) 95 % ethanol 24 h at 50 °C
In case of doubt or unknown iso-octane and 95 % ethanol 24 h at 50 °C
4 Total immersion method
4.1 Principle
The migrateable substances extracted from a sample of the polymer coated paper or board is determined as the
mass of non-volatile residue after evaporation of the solvent following immersion.
Test specimens of at least 1 dm² (single side considered) are immersed in the test medium for set periods of time
and at set temperatures and then removed. The test medium is evaporated to dryness, the mass of the non-
volatile residue is determined and expressed as milligrams per square decimetre of surface area of the test
specimen.
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4.2 Apparatus
4.2.1 Cutting slab, clean smooth glass, metal or plastics slab of suitable area to prepare test specimens,
250 mm x 250 mm is suitable.
4.2.2 Tweezers, stainless steel, blunt nosed.
4.2.3 Cutting implement, scalpel, scissors or sharp knife or other suitable device.
4.2.4 Metal template, 100 mm ± 0,2 mm x 100 mm ± 0,2 mm (square).
4.2.5 Rule, graduated in mm, and readable to the nearest 0,1 mm.
4.2.6 Analytical balance, capable of determining a change in mass of 0,1 mg.
4.2.7 Extraction containers; glass weighing jars with ground joints, tall form, of a capacity of approximately
60 ml.
4.2.8 Thermostatically controlled oven or incubator capable of maintaining a temperature within the range of
+ 40 °C to + 50 °C and meeting temperature tolerance values within those specified for the test temperature, see
annex B of ENV 1186-1: 1994.
WARNING The interior/sample space of the oven or incubator should not have any exposed heating elements, to
minimise safety hazards arising from any loss of flammable test media during the test period.
4.2.9 Dishes, stainless steel, nickel, platinum, platinum alloy or gold, 50 mm to 90 mm diameter and maximum
weight 100 g, for evaporation of solvents and weighing of residues. Glass, glass ceramic, ceramic or aluminium
dishes may be used provided that the surface characteristics are such that the weights of the dishes after
evaporation of any specified solvent followed by conditioning in the desiccator used achieves a constancy of
0,5 mg.
4.2.10 Steam bath, hot plate, distillation apparatus or rotary evaporator.
4.2.11 Desiccator with anhydrous calcium chloride or self indicating silica gel.
4.2.12 Measuring cylinder, of a capacity of 50 ml, complying with the minimum requirements of ISO 4788.
4.3 Reagents
1
4.3.1 Iso-octane, (2,2,4-trimethyl pentane), a volume fraction of 98,5 % purity or greater, CAS No. 540-84-1 )
4.3.2 Ethanol [a volume fraction of 95 % in aqueous solution], a volume fraction of 96 % purity or greater,
WARNING Both iso-octane and ethanol are volatile flammable solvents. Take care to ensure that the test
specimens are well stoppered, closed and covered to prevent solvent volatilising into the interior of the oven,
incubator or refrigerator and generating an explosive mixture. Care should be taken at all times when handling
these solvents to prevent contact with sources of ignition
1
) The source of this is the Chemical Abstracts published by the American Chemical Society
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4.4 Preparation of test specimens
4.4.1 General
It is essential that test specimens are clean and free from surface contamination (many polymeric coatings can
readily attract dust due to static charges). Before preparing test specimens, remove any surface contamination
from the sample by gently wiping it with a lint free cloth, or by brushing with a soft brush. Under no circumstances
wash the sample with water or solvent. If it is specified in the instructions for use of the article that it should be
washed or cleaned before use see 8.1 of ENV 1186-1: 1994. Minimize handling of the samples and where
necessary, wear cotton gloves.
To ensure that test pieces are well separated and that the surfaces are freely exposed to the extractant during the
period of the test, insert a piece of fine stainless steel gauze between the cut test pieces.
4.4.2 Number of test specimens
Three replicate test specimens are required.
4.4.3 Cutting and preparation of specimen
Lay the sample on the cutting slab (4.2.1) and cut the test specimens of 1 dm² (see 8.3 of ENV 1186-1:1994), using
the 100 mm x 100 mm template (4.2.4). Check, using the rule (4.2.5), that the dimensions of the specimen are
within the specified tolerance (1mm). Fold the test specimens into a fan-like shape or cut into strips approximately
2 cm wide and 5 cm long. Place in the extraction containers (4.2.7).
4.5 Procedure
4.5.1 Exposure to solvent
Take three extraction containers or jars (4.2.7), measure by measuring cylinder (4.2.12) 50 ml of the solvent into
each of these jars and immerse the test specimens in the solvent. Ensure that the test specimens are totally
immersed in the solvent. If the evaporation method is to be used (4.5.2.2) measure into a further two jars by
measuring cylinder the same amount of solvent, plus 10 ml ± 2 ml, to provide blanks. If the distillation method
(4.5.2.3) is to be used measure into those further two jars by measuring cylinder the same amount of solvent in
contact with the test specimens to provide blanks. Stopper the jars. Mark the jars for identification. Mark the liquid
level on the outside of each jar with a suitable marker.
The extraction conditions are to be selected from table 1 (clause 3.1) according to the nature of the polymeric
coating of the samples, or according to clauses 4, 5 and 6 of ENV 1186-1: 1994.
Place the five jars in the thermostatically controlled oven or incubator (4.2.8), set at the test temperature and
observe the temperature, leave the jars for the set test period after the air bath of the thermostatically controlled
oven or incubator has reached the set temperature and taking the permitted time and temperature tolerances into
account, see annex B of ENV 1186-1: 1994. Take the jars from the oven or incubator and allow them to cool down
to room temperature. Check the level of solvent in each. If this has fallen to more than 5 mm below the mark, or
has exposed any part of the test pieces, repeat the test using fresh samples. If the level of solvent in a jar is less
than 5 mm below the mark, remove the test specimen from the jar, and allow the solvent adhering to the test
specimen and support to drain back into the tube. Recover at least 90 % of the original volume of solvent or repeat
the test.
WARNING Both iso-octane and ethanol are volatile flammable solvents. Take care to avoid any loss of solvent
into the interior of the thermostatted device. Place the jars, if possible, in a drip container serving as a possible
solvent reservoir in case of leakage. Do not allow the temperature to exceed 60 °C.
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4.5.2 Determination of extracted substances
4.5.2.1 Preparation of dishes
Take five dishes (4.2.9), marked for identification, place the dishes in an oven maintained at 105 °C to 110 °C, for a
period of 30 min ± 5 min, to dry. Remove the dishes from the oven, place in a desiccator (4.2.11) and allow to cool
to ambient temperature. Weigh and record the individual masses of each dish. Replace the dishes in the oven and
repeat the cycle of heating, cooling and weighing until individual consecutive masses differ by not more than 0,5
mg. Record their final masses.
4.5.2.2 Evaporation method
For each jar containing the solvent, pour 20 ml to 25 ml into a prepared dish. By means of a steam bath, hot plate
or other form of heating evaporate to a low volume (4.2.10), taking care to avoid loss, in particular, by sputtering or
overheating of the residues.
NOTE 1 The evaporation should be carried out in a fume cupboard.
When most of the solvent has evaporated, pour the remaining solvent from each of the jars into the respective
dishes and continue the evaporation. Wash out each of the tubes which had contained test specimens with two
lots of 5 ml ± 1 ml of fresh solvent and pour these washings into the respective dishes. Continue the evaporation.
NOTE 2 A stream of nitrogen may be used to facilitate evaporation.
When the solvent has almost completely evaporated, place the dish in an oven maintained at 105 °C to 110 °C, for
a period of 30 min ± 5 min, to complete the evaporation and dry the residue. Remove the dishes from the oven,
place in a desiccator (4.2.11) and allow to cool to ambient temperature. Weigh and record the individual masses of
each dish and residue. Replace the dishes in the oven and repeat the cycle of heating, cooling and weighing until
individual consecutive masses differ by not more than 0,5 mg. Determine the mass of the residue by subtracting
the original mass of the dish from the final mass of the dish and residue.
4.5.3 Distillation method
For each jar, transfer the contents to a round bottom flask (250 ml is suitable). Rinse each jar twice, including the
blank jars, with 20 ml ± 2 ml of fresh solvent, add these rinses to the respective flasks. Place the flasks in an
electric heating mantle and connect to a side arm distillation arrangement or use a rotary evaporator. Distil off the
solvent until approximately 15 ml to 25 ml remains in the flask. Transfer the remaining solvents to an evaporating
dish. Rinse the flask with 10 ml ± 1 ml of fresh solvent and add the rinses to the appropriate dishes. Continue the
evaporation of the solvent by means of a steam bath, hot plate or other form of heating, proceeding as in 4.5.2.2.
NOTE The evaporation should be carried out in a fume cupboard.
Continue with clauses 6 and 7.
5 Cell method
5.1 Principle
The total migrateable substances extracted from a sample of the polymeric coating is determined as the mass of
non-volatile residue after evaporation of the solvent following immersion.
One surface of the test specimen of at least 1 dm² (single side considered) is exposed in a cell to the extraction
solvent for set periods of time and at set temperatures and then removed. The extraction solvent is evaporated to
dryness, the mass of the non-volatile residue is determined and expressed as milligrams per square decimetre of
surface area of the test specimen. The measured value is compared to the EC-official overall migration limit and
taking the analytical tolerance of this method (± 1mg/dm²) into account.
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5.2 Apparatus
5.2.1 Cutting slab, clean smooth glass, metal or plastics slab of suitable area to prepare test specimens,
250 mm x 250 mm is suitable.
5.2.2 Tweezers, stainless steel, blunt nosed.
5.2.3 Cutting implement, scalpel, scissors or sharp knife or other suitable device.
5.2.4 Analytical balance capable determining a change in mass of 0,1 mg.
5.2.5 Cell, type B (as shown in Figure C.3 of ENV 1186-1: 1994), either the aluminium (anodized) cells or the
cells with the stainless steel (316 grade) lids and rings, are suitable for the extraction solvents.
5.2.6 Glass tubes, ground neck, and stoppers, for retaining the food simulant.
5.2.7 Pipettes, complying with the minimum requirements of ISO 648, 50 ml and 100 ml.
5.2.8 Thermostatically controlled oven or incubator capable of maintaining the test temperature and meeting
temperature tolerance values within those specified for the test temperature, see annex B of ENV 1186-1: 1994.
WARNING The interior/sample space of the oven or incubator should not have any exposed heating elements, to
minimize safety hazards arising from any loss of flammable test media during the test period.
5.2.9 Dishes, stainless steel, nickel, platinum, platinum alloy, gold 50 mm to 90 mm diameter and maximum
weight 100 g, for evaporation of solvents and weighing of residues. Glass, glass ceramic, ceramic or aluminium
dishes may be used provided that the surface characteristics are such that the weights of the dishes after
evaporation of any specified solvent followed by conditioning in the desiccator used achieves a constancy of
0,5 mg.
5.2.10 Steam bath, hot plate, distillation apparatus or rotary evaporator.
5.2.11 Desiccator with anhydrous calcium chloride or self indicating silica gel.
5.2.12 Measuring cylinder, of a capacity of 50 ml, complying with the minimum requirements of ISO 4788.
5.3 Reagents
1
5.3.1 Iso-octane, (2,2,4-trimethyl pentane), a volume fraction of 98,5 % purity or greater, CAS No. 540-84-1 )
5.3.2 Ethanol, a volume fraction of 96 % purity or greater, a volume fraction of 95 % in aqueous solution.
WARNING Both iso-octane and ethanol are volatile flammable solvents. Take care to ensure that the test
specimens are well stoppered, closed and covered to prevent solvent volatilising into the interior of the oven,
incubator or refrigerator and generating an explosive mixture. Care should be taken at all times when handling
these solvents to prevent contact with sources of ignition.
1
) The source of this is the Chemical Abstracts published by the American Chemical Society
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SIST-TS CEN/TS 14234:2003
CEN/TS 14234:2002 (E)
5.4 Preparation of test specimens
5.4.1 General
It is essential that test specimens are clean and free from surface contamination (many polymeric coatings can
readily attract dust due to static charges). Before preparing test specimens, remove any surface contamination
from the sample by gently wiping it with a lint free cloth, or by brushing with a soft brush. Under no circumstances
wash the sample with water or solvent. If it is specified in the instructions for use of the article that it should be
washed or cleaned before use see 8.1 of ENV 1186-1: 1994. Minimize handling of the samples and where
necessary, wear cotton gloves.
5.4.2 Number of test specimens
Three replicate test specimen are required.
5.4.3 Cutting test specimens
Lay the sample on the cutting slab (5.2.1) with the surface to be in contact with the food simulant uppermost. Take
the ring from the cell (5.2.5) and place on the surface of the sample. Cut out the test specimen by cutting round the
outer edge of the ring, using the cutting implement (5.2.3).
5.5 Procedure
5.5.1 Exposure to solvent
Take three cells (5.2.5), mark these for identification purposes. Dismantle and place on the base of each cell one
test specimens. Reassemble the cells, ensuring that the clamping screw wheel is well tightened down.
Measure by measuring cylinder an appropriate amount of the solvent into each cell through the filler hole and
replace the filler plug. The ratio between the area in square decimetres exposed to the amount of food simulant in
millilitres should be a maximum 1/50. If the evaporation method is to be used (5.5.2.2) measure into two tubes
(5.2.6) by measuring cylinder the same amount of solvent, plus 10 ml ± 2 ml, to provide blanks. If the distillation
method (5.5.2.3) is to be used measure into those two tubes by measuring cylinder the same amount of solvent in
contact with the test specimens to provide blanks. Stopper the tubes. Mark the tubes for identification. Mark the
liquid level on the outside of each tube with a suitable marker.
The extraction conditions are to be selected from table 1 (3.1) according to the nature of the polymeric coating of
the samples, or according
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