Why some migration conditions forplastics are not appropriate for

other FCMs.

Peter OldringRepresenting 18 associations directly or

indirectly involved in FCMsFIP Network

25th May 2016 Parma

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Extract from Executive Summary (p9) EuropeanParliament report on 1935/2004 (May 2016)

‘As a general trend, stakeholders who are in favour offurther EU level harmonisation recommend that EUspecific measures should establish a single standardfor analytical (testing) methods, such as compositiondetermination, migration testing, risk assessment, but alsospecific methods for compliance enforcement, thusensuring that the relevant FCM is tested by companies andcompetent authorities across the EU with one and thesame method. Furthermore, the EU single standard foranalytical (testing) methods should be specific for eachFCM, thus reflecting its unique properties and avoidingsituations where non-harmonised FCMs are tested withmethods developed for harmonised FCMs, which could leadto misleading and debatable test results’

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DISCLAIMER

As chair of the 18 associations representing non-plastics, I will try and represent them.

The initiative started with CEPE, EMPAC andalmost immediately CES silicones joined.

Other associations have joined since then.

However, I have to understand and work withanalytical data, in order to make decisions aboutand determine the safety of my company’sproducts.

The work is embryonic, associations are stilljoining and the final format will certainly bedifferent to that initially envisaged.

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Associations participating in Initiative

ACE Beverage cartons – paper, plastics and aluminium flexible APEAL Steel for rigid metal packaging CEFIC-FCA Substance suppliers CELIEGE Cork CEPE Coatings for rigid metal packaging CEPI Paper and paper board CES Silicones Europe: Silicone elastomers for household articles EAA Aluminium EEA Porcelain enamel and porcelain enamelled articles EMPAC Rigid metal packaging ETRMA Rubbers EuPIA Printing inks EWF Waxes FEC Non-stick treatments and coatings, materials and articles FEFCO Carton board FEICA Adhesives FPE Flexible packaging (non-plastic and multi-material) GAE Glass articles, hollow, domestic and flat glass

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The Issue - 1

In the Plastics Regulation (10/2011) andsupporting documentation, (i.e. MigrationGuidelines), some of the simulants, times andtemperatures are inappropriate for some non-plastic FCMs (Food Contact Materials).

Why non-plastics rather than non-harmonised?

Migration conditions for plastics are not used forsome harmonised FCMs, such as ceramics orregenerated cellulose.

However in the absence of harmonisedregulations the conditions used in the PlasticsRegulation are often applied to non-plastics.

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The Issue - 2

National Regulations for non-plastic FCMs aretending to adopt the conditions in 10/2011 –example proposed coating regulations forboth Netherlands and Belgium, althoughdifferent in detail.

Obtaining higher or lower levels of migrantsunder inappropriate conditions may result inmis-interpreting the results:

Plastic simulants and or conditions may causephysical damage / changes to the non-plasticFCM which invalidates the result

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The Issue - 3

Even if no change the simulants andconditions for plastics were chosen to modelplastics and their interaction with foodstuffs.Non-plastics may/will interact differentlygiving mis-leading results (higher or lower).

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Example of non-stick-coatings

Non-stick coatings and treatments are unique:

Whilst there are industrial and professionaluses of the food contact articles, the primaryend use applications are intended to be byconsumers

Potential for repeated use at hightemperatures

Potential for food contact temperatures from<0 C to > 250ºC

Incompatibilities between some coatingmaterials and existing simulants

Need for flexibility in selecting test conditions toreflect actual end use conditions

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Industry response - 1

Members of associations, in the non-harmonisedFCM supply chain, have formed a task force topropose testing conditions better adapted to thespecificity of various materials / sectors.

Each sector is assessing the applicability or not ofthe plastics 10/2011 migration testing guidelinesfor their own sector.

In some cases they are applicable, but in othercases they are not

The Task Force are developing their owncompliance guidelines with separate chapters foreach non-harmonized FCM.

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Industry response - 2

Gaps or lack of feasibility of implementations areidentified and expertise collected and shared tooffer technical solutions for improved compliancetesting.

Test proposals are based on technical /scientifically demonstrated justification.

Common introduction available.

The majority of association’s guidelines are/willbe on their web-site. For those that aren’t it willbe necessary to contact their secretariat for them

The guidelines will be based on the followingformat:

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New Guidelines – common format - 1

Introduction

FCM specific chapter containing:

Scope

Uses

Definitions

Material Specific Properties to be consideredwhen testing this class of FCM

Brief outline as to why plastic testingguidelines may be inappropriate

Test Procedures

Evaluation of test results11

New Guidelines – common format - 2

Annexes

Annex 1: Reasons why plastic guidelines arenot suitable for this class of FCM.

Annex 2: References

The amount of detail in each sector’s chapterswill very considerably, e.g. siliconethermoplastics are relatively specific, whereasadhesives cover the majority of adhesives withdifferent issues for different adhesives.

Coatings cover many areas and associations ascan be seen from the following slide:

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Different Coatings

1. Can – EMPAC / CEPE

2. Heatseal – EuPIA / FEICA / FPE

3. Coldseal - EuPIA / FEICA / FPE

4. Coatings on plastic film

5. Porcelain enamel coating on metal - EEA

6. Non-stick treatments and coatings (PTFE and Sol-Gel based) – FEC

7. Coatings on Paper and board – CEPI / CITPA

8. Heavy duty – CEPE

9. Coatings on metal foil – FPE

10. Polymeric Coatings on glass

11. Passivation coatings on metals – APEAL

12. Others13

Substrates covered by coatings

Coating paper Aluminium

foil

Metal

packaging

Plastic Kitchen

ware

Glass Metal,

plastic,

concrete

Wood Textiles

1 X

2 X X X X

3 X X

4 X

5 X

6 X

7 X

8 X

9 X

10 X

11 X

12 X X X X X X X X X14

FCM cross sector involvement

During meetings, different FCM sectors foundthat other sectors had similar problems withsome simulants, times or temperatures.

In addition many FCMs are multi-material, hencedifferent associations needed to work together.

It has to be recognised that there are not alwayseasy answers to issues raised.

There is still debate as to whether to tackle thesubject substrate by substrate or material bymaterial e.g. baking paper as paper or as fluoro-polymers, silicones etc.

Some examples of the issues and proposedsolutions follow.

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Issues with 3% Acetic Acid

for Overall Migration

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3% Acetic Acid – 1

A general issue common to many FCM sectors isthe use of 3% acetic acid for overall migration(OM).

OM is NOT a measure of safety, but of inertnessof polymeric materials.

Acetic acid corrodes aluminium, either as acoated substrate or foil layer in a multi-layerFCM.

Acetic acid also corrodes coated tin plate.

There is an issue but no solution has yet beenfound, BUT options are being investigated

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• Two quite distinctprocesses are happeningduring the test– True Migration – a physical

transfer of substances fromthe organic lacquer into thefood simulant

– Corrosion – a chemicalreaction between acetic acidand the aluminiumfoil/substrate causing theformation of aluminiumacetate and the release ofaluminium ions into the foodsimulant

3% Acetic Acid - 2

Migrant

Migrant

Migrant

Aluminium

Acetic Acid

La

cq

ue

r

Acetic Acid

Aluminium

La

cq

ue

r

XH+

Al+++

XH+

Al+++

XH+

Al+++

Schematic Illustration

Acetic Acid – 3: Al+++ Release from LacqueredAluminium Foil (Courtesy FPE)

0.0

1.0

2.0

3.0

4.0

5.0

3% AceticAcid

10 d/ 40 ˚C

Yoghurt pH =4.2

30 d/ 5 ˚C

0.5% CitricAcid

10 d/ 40 ˚C

Alu

min

ium

Re

leas

em

g/k

g >> 100 mg/kg dueto corrosion

NOTE: This is Aluminium ionsrelease and not organic materialmigration

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>>100

3% Acetic Acid – 4

High test results can be obtained, becausewhen the simulant is evaporated to drynessand the residue weighed, the residue islargely aluminium acetate salts

This increases the weight of the residue, forexample:

Aluminium molecular weight = 27

Aluminium triacetate molecular weight =204

Hence up to 87% of the measured result isdue to the simulant, not to the aluminium(ions) released.

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3% Acetic Acid – 5

For FPE the overall migration from coatedaluminium foil is a major issue.

Coatings for rigid metal packaging also havea major issue with 3% acetic acid being usedfor overall migration.

The use of citric acid has been proposed, butthis has the drawback that in practice, for theorganic migrants, it is not volatile enough fora gravimetric determination of overallmigration by evaporation.

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3% Acetic Acid – 6

For can coatings based upon 4 differentchemistries – epoxy, acrylic, polyester,organosol – and applied to tin plate substratethe comparing chloroform soluble part to theresults using silver foil, showed that thisapproach was inappropriate.

Using stainless steel panels gave rise toinsurmountable practical problems.

The same exercise is being repeated forcoated (same 4 coating types) aluminiumsubstrate.

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3% Acetic Acid – 7

The conclusion for can coatings, subject toconfirmation from aluminium coated panels isthat the use of 3% acetic acid is inappropriatefor overall migration as found by CEN TC 194many years ago.

This does not mean that it cannot be used forspecific migration.

As overall migration is a measure of inertnessand not safety, the light metal packaging chainrecommend that 3% acetic acid is not used foroverall migration.

Other simulants give a measure of inertnessand are generally used for compliance testing 23

Issues with Olive Oil

and Silicone Elastomers

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Silicone Elastomers - 1

Silicones are exempted from (EU) N° 10/2011given that elastomers have different physico-chemical properties compared to plastics

Problems for silicone elastomers arise mainlywith compliance testing for baking moulds

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Silicone Elastomers - 2

Olive / vegetable oils contain componentswhich can penetrate into the siliconeelastomer matrix, which results in anoverestimation of migration compared toreal food. The same applies to substitutesiso-octane and 95% ethanol.

Absorbed oil must be removed by soxhletextraction with a non-polar solvent, whichmay in turn cause additional extraction ofcomponents from the silicone, therebyskewing the results further from reality.

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Silicone Elastomers - 3

A proposed solution is to use Tenax whichdoes not penetrate the silicone elastomermatrix.

Tenax was an accepted substitute underDirective 97/48/EC but its use as asubstitute under 10/2011, lacks clarity(according to CES).

Tenax also overestimates migrationcompared to normal bake ware (e.g.muffins, marble cake) but if the reductionfactor of 5 is applied, the results arecomparable to standard bake ware.

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Silicone Elastomers - 4

The most important criteria to determinesuitability of silicone moulds for food contactis the limit for volatile substances (0.5%) asmandatory according to RecommendationXV of the BfR and the French legislation.

In appropriately post-cured materialsmeeting the limit for volatiles <0.5% themajority of migrants consist of cyclicsiloxanes with Mw >1000Da which accordingto present knowledge, are not expected toendanger human health.

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Issues of paper and board

with aqueous simulants

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Paper & Board (P & B) - 1

As a general rule P & B is only used for dry orfrozen foodstuffs.

P & B consists of cellulosic fibres which aremoisture sensitive and porous.

For contact with ‘wet’ foodstuffs at least oneadditional layer is between the P & B and thefoodstuff – e.g. polythene laminate (milkcarton).

Also like liquid foods, P & B liquid simulants(10/2011 types) will be absorbed and noteven recovered in some cases or the surfacemay be damaged or physically disintegrate inothers, due to the porous nature of P&B. 30

Paper & Board -2

Papers for fatty food may be treated withfluorinated chemicals and testing in ethanolicsimulants would result in total extraction.

This is because the chemicals are applied froman alcoholic solution.

Other simulants for fatty foodstuffs need to beused.

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Issues with 50% Ethanol

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50% Ethanol - 1

Some polyester based coatings showdelamination and swell when tested undersevere time/temperature conditions (e.g. 2 h130 °C) with simulant D1 (50 % ethanol).

The same polymeric coatings do not show anyphysical changes when they are in contactwith milk products under equivalentsterilisation conditions.

Overall migration tests and most specificmigration tests cannot be carried out in milkproducts instead of simulants.

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50% Ethanol - 2

Proposal: Compliance of coatings which arenot resistant to 50 % ethanol can bedemonstrated by

- decreasing testing time and/or temperatureto a level where no physical changes of thecoating film occur

or- migration testing with simulant A (10 %

ethanol) and D2 (vegetable oil) rather than50 % ethanol

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Dissemination

Presentations have been made to:

DGSante

Member States

National Reference Laboratories & JRC

Cefic-FCA

FPF Workshop which included NGOs andacademics

Industry PIRA

FIP Network (today)

The objective is to make people aware of thisinitiative ahead of the migration guidelines forplastics being published 35

Migration Guidelines for 10/2011 - 1

Industry requested that the guidelines containa clear statement to the effect that they onlyapply for harmonised (plastic) FCMs and arenot necessarily appropriate for non-harmonised(non-plastic) FCMs.

This is because in the absence of unequivocalstatements, packers & fillers, control labs, testhouses and many in the supply chain wantcompliance with 10/2011 in order to safeguardthemselves.

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Migration Guidelines for 10/2011 - 2

In the guidelines released for consultation,many sectors of industry felt that whilst thereis a statement to this effect it is still unclear tomany outside of the regulatory community.

The non-plastic FCM sectors would like to see astatement along the following lines: ‘Thesetechnical guidelines are written in theframework of the scope of Regulation (EU) No10/2011 (Article 2) and are only applicablefor plastic materials and articles underthis scope.’

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Migration Guidelines for 10/2011 - 3

We need something in place by the time the10/2011 guidelines are published to minimiseany mis-use of the 10/2011 guidelines.

Some associations have put their draftguidelines on their web-sites.

This allows them to be easily updated etc.

The guidelines for non-plastic FCMs will beshared with the commission ( DG Sante andJRC ).

Discussions are also anticipated withthe experts of the Member States and somemembers of the Council of Europe.

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Acknowledgements

Thank you for your attention

All members of this task force for their inputs.

In particular, for this presentation, ChristaBurger, Michelle Callow, John Dixon, BeateGanster, Ulrich Nehring, Catherine Simoneau,Richard Whitaker.

THANK YOU FOR YOUR ATTENTION

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