1. Österreichisches Forschungsinstitut für Chemie und Technik www.ofi.at CROPACK 2010 Migration Testing Overall migration SML tests Screening methods DI Michael Pitzl

2. www.ofi.at 2  Private Testing and Research Institute  Legal form: Association / Ltd.  ~ 130 employees (status: 12/2009)  ~ 7.000 m 2 floor space at 2 locations  Business Year 2009: Annual turnover: 13,8 Mio. Euro R&D: ~ 26 % Share of export: ~ 24 % Organisation and Facts

3. www.ofi.at 3 Location Arsenal 1030 Vienna, Arsenal Objekt 213, Franz Grill-Straße 5 Applied Polymer Technology Varnishes and Adhesives Construction Sports Technology Location Brehmstraße 1110 Vienna, Brehmstraße 14a Packaging Medical Products Eco Technology Food Analysis Administration Locations and Departments

4. www.ofi.at 4 Main Focus:  Certification / Consulting in case of Damage Claims  Testing & Quality Assurance  Assessment according to the European Food Legislation / LMSVG  Client‘s R&D-Projects  Branch-oriented R&D-Projects  Branch-oriented Training and Education ... Packaging (incl. food commodities)

5. www.ofi.at 5 Migration Scalping Migration Active Packaging H2OH2O Gas Flavour Product Light Mech. Stress Hygiene

6. www.ofi.at 6 Potential Migrants  Glas -Silicates, heavy metals  Plastics -Plasticizers, monomers, antistatics...  Paper -Additives and fillers (chalk etc.)  Metal -Aluminium, tin for acid contents

7. www.ofi.at 7 Migration How can be prevented that an illegitimate amount of contents of the packaging migrates into the product? Choosing the right packaging! Ensured by migration testing -Compliance with overall migration limit (OML) -Specific migration limits (SML) -Maximum legitimate residual content of the substance in the finished food contact material (QMA) !!! Consideration of actual applied conditions (time and temperature combinations)

8. www.ofi.at 8 Migration Testing Test conditions according to 2002/72/EC Basics for migration tests  82/711/EEC – Basic rules for testing migration  93/8/EEC – 1st amendment  97/48/EEC – 2nd amendment List of simulants: 85/572/EEC  2007/19/EEC – 1st amendment VC in PVC: 78/142/EEC (residual content and transfer to foodstuff) VC-analysis: 80/766/EEC, 81/432/EEC Certain epoxy derivatives: REG (EC) Nr. 1895 / 2005 Plasticizers in gaskets in lids: REG (EC) Nr. 372/2007

9. www.ofi.at 9 CEN TC 194 CEN TC 194 ´Utensils in Contact with Food´ ´Utensils in Contact with Food´ SC 1: General chemical methods  Standard EN 1186: Test methods for overall migration  Standard EN or CEN/TS 13130: Standard methods for the specific migration (SML/QM) currently, 28 parts are published within this standard European Standards concerning plastics in contact with foodstuff

10. www.ofi.at 10  Aqueous foods pH > 4,5 Distilled water (A)  Acidic foods pH  4,5 3 % (w/v) Acetic acid (B)  Alcoholic foods: 10 % (v/v) Ethanol (C)  milk / milk products: 50 % (v/v) Ethanol  Fatty foods: Rectified olive oil (D)  Dry foods: none Simulants if ethanol content > 10 %: adaptation to the actual content!

11. www.ofi.at 11 Selection of the right Simulant List of simulants: Regulation 85/572/EEC Example:

12. www.ofi.at 12 Migration Testing:  Unknown contact time, application for ambient temperature or lower temperatures: 10 d / 40 °C (all simulants)  Unknown contact time & unknown application temperature: 4 h / 100 °C bzw. Reflux (simulant A, B, C) 2 h / 175 °C (simulant D)  Hot filling (< 15 min at 70-100 °C): 2 h / 70 °C (all simulants) Standardized Testing Conditions according to European Regulations / Austrian Plastics Regulation Overall migration – bottom sediments

13. www.ofi.at 13 Migration Testing Substitute test for fatty foods  If the use of fatty food simulants is not feasible for technical reasons Substitution: defined test media and conditions, corresponding to the simulant D Iso-Octan Ethanol (95 %) Modified Polyphenylenoxid (Tenax)

14. www.ofi.at 14 Migration Testing  Consideration of the practical usage conditions of the packaging (e. g. for which foodstuff applied?)  Clarification of the usage conditions Selection of the simulant and test conditions (contact time and temperature)  Is overall migration limit complied (OML)?  Compliance with thresholds of the specific migration (SML) residual content in the commidity (QM)? Migration Tests for finished commodities

15. www.ofi.at 15 Structure of the actual EU-Laws For materials and articles in contact with foodstuff Main-REG (EC) Nr. 1935/2004 Specific Directives BADGE, BFDGE, NOGE VO (EG) Nr. 1895/2005 Vinyl chloride 78/142/EEC Reg. Cellulose 2007/42/EC Analyses of VC 81/432/EEC Analysis of VC-content 80/766/EEC Ceramik 84/500/EEC amanded2005/ 31/EC Plastic 2002/72/EC amanded VO Nr. 975/2009 Rules Migration 82/711/EEC amended 97/48/EEC List of Simulants 85/572/EEC amended 2007/19/EC GMP-REG (EC) Nr. 2023/2006 Recycl.-REG (EC) Nr. 282/2008 A&I-REG (EC) Nr. 450/2009

16. www.ofi.at 16 EU-Substances List / Synoptic Document  EU-Substances List -Based on: 2002/72/EG incl. supplements -Containing an authorised positive list of monomers and an incomplete list of additives  For certain substances thresholds are available which are expressed -either as maximum quantity in material or article (QM) -or as specific migration limit in food (SML).

17. www.ofi.at 17 SML / QM Test Methods: migration test medium + GC, HPLC Positive List (excerpt):

18. www.ofi.at 18 SML – Save Testing Costs Special Cases:  100% migration < SML  Calculation model

19. www.ofi.at 19 Gas Chromatography

20. www.ofi.at 20 Chromatographic Separation Separation of substances mixture due to different retention times of each single analyte during the transport through the chromatographic bed

21. www.ofi.at 21 Definitions  DECISION LIMIT : Threshold for the presence of an analyte (yes/no). If a sample possessed the exact content of the dicision limit, the analyte wouldn‘t be detected in 50 % of the measurements despite the presence of the analyte („false negative“).  DETECTION LIMIT : minimal concentration of an analyte, which is detected with a high likeliness (e. g. 95 %). The detection limit is usually twice the amount of the decision limit.  DETERMINATION LIMIT: lowest concentration of an analyte, which can be quantitatively detected with a determined accuracy. Quantitative analyse results are only declared above the determination limit. The determination limit equals approximately the triple amount of the decision limit.

22. www.ofi.at 22 Thermodesorber: Gas Chromatography

23. www.ofi.at 23 Screening Methods  Migration or directly in food  Which peaks are explainable, which are not? Criticism : Analysis method? Comparability? Undetected substances?

24. www.ofi.at 24 Special Regulation – Lid Gaskets Regulation 372/2007/EG  laying down transitional migration limits for plasticizers in gaskets in lids intended to come into contact with food SML for:  fatty food: 300mg/kg*  all others: 60 mg/kg*  baby / infant food: 30 mg/kg* (restriction for ESBO) * of food or food simulant

25. www.ofi.at 25 Example - ITX Isopropylthioxanthone (ITX)  Photointitiator in UV-curing printing inks  Application: outside of food packaging (compound for milk, cacao, juice)  Problems: -Set off–effect -Migration !!! Threshold 0,05 mg/kg ITX in food

26. www.ofi.at 26 How to test „Set off“? IVLV „cluster commodities“ Working group of German-speaking testing laboratories eurofins, Fresenius, GALAB, GfU, innoform, ISEGA, MUVA, Nehring, ofi, SQTS Agreement on common test conditions: Time / Temperature - at customer - at laboratory: a) guideline value 10 days at 40 °C b) alternatively according to actual application Pressure - three-dimensional - pile (according to customer) - flat/foila) roll b) pile - full-surface contact - flexible - 1kg/dm² Sample Name / Storage

27. www.ofi.at 27 PIM – what‘s next?  New simulants e. g. Tenax:

28. www.ofi.at 28 PIM – what‘s next?  Priority: 1. Specific migration 2. Overall migration  Overall migration: Test conditions OM1-9  Regulations for repeated contacts  Multi-layer materials and articles  Test at 10 d 60 °C for storage times > 30 d  Substitute simulants („scientific evidence“)

29. www.ofi.at 29 Österreichisches Forschungsinstitut für Chemie und Technik (ofi) Brehmstraße 14A 1110 Vienna  +43-(0)1-798 16 01 – ext.  +43-(0)1-798 16 01 - 480 DI Michael Pitzl (ext. 597, E-Mail: michael.pitzl@ofi.at) Contacts