sterreichisches Forschungsinstitut

fr Chemie und Technik

www.ofi.at

CROPACK 2010

Migration Testing
Overall migration SML tests Screening methods
DI Michael Pitzl

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Organisation and Facts

Private Testing and Research Institute

Legal form: Association / Ltd. ~ 130 employees (status: 12/2009) ~ 7.000 m2 floor space at 2 locations Business Year 2009: Annual turnover: 13,8 Mio. Euro R&D: ~ 26 % Share of export: ~ 24 %

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Locations and Departments

Location Arsenal 1030 Vienna, Arsenal Objekt 213, Franz Grill-Strae 5

Location Brehmstrae 1110 Vienna, Brehmstrae 14a

Applied Polymer Technology Varnishes and Adhesives Construction Sports Technology

Packaging Medical Products Eco Technology Food Analysis Administration 3

Packaging
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(incl. food commodities)

Main Focus:
Certification / Consulting in case of Damage Claims Testing & Quality Assurance Assessment according to the European Food Legislation / LMSVG Clients R&D-Projects Branch-oriented R&D-Projects Branch-oriented Training and Education

...

Migration
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Mech. Stress

Light

Hygiene H 2O Gas

Migration

Product
Active Packaging

Flavour

Scalping

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

Migration
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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)
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Migration Testing
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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
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European Standards
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concerning plastics in contact with foodstuff

CEN TC 194 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

Simulants
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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

if ethanol content > 10 %: adaptation to the actual content!

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Selection of the right Simulant

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List of simulants: Regulation 85/572/EEC Example:

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Standardized Testing Conditions according to European Regulations / Austrian Plastics Regulation

Migration Testing:
Unknown contact time, application for ambient temperature or lower temperatures:

10 d / 40 C (all simulants)

Overall migration bottom sediments

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)

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Migration Testing
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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)

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Migration Testing
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Migration Tests for finished commodities

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)?

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Structure of the actual EU-Laws

For materials and articles in contact with foodstuff

Main-REG (EC) Nr. 1935/2004 Specific Directives GMP-REG (EC) Nr. 2023/2006 Recycl.-REG (EC) Nr. 282/2008 A&I-REG (EC) Nr. 450/2009

Reg. Cellulose 2007/42/EC

Vinyl chloride 78/142/EEC

BADGE, BFDGE, NOGE VO (EG) Nr. 1895/2005

Plastic 2002/72/EC
amanded VO Nr. 975/2009

Ceramik 84/500/EEC
amanded2005/ 31/EC

Analyses of VC 81/432/EEC

Analysis of VC-content 80/766/EEC

Rules Migration
amended 97/48/EEC

List of Simulants
amended 2007/19/EC

82/711/EEC

85/572/EEC

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EU-Substances List / Synoptic Document

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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).

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SML / QM
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Test Methods: migration test medium + GC, HPLC Positive List (excerpt):

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SML Save Testing Costs

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Special Cases:

100% migration < SML

Calculation model

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Gas Chromatography
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Chromatographic Separation
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Separation of substances mixture due to different retention times of each single analyte during the transport through the chromatographic bed

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Definitions
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DECISION LIMIT: Threshold for the presence of an analyte

(yes/no). If a sample possessed the exact content of the dicision limit, the analyte wouldnt 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.

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Gas Chromatography
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Thermodesorber:

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Screening Methods
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Migration or directly in food Which peaks are explainable, which are not?
Criticism: Analysis method? Comparability? Undetected

substances?
Abundance
T IC: H U ND 002.D

3.57 140000 130000 120000 110000 100000 90000 80000 70000 60000 50000 3.26 40000 30000 20000 10000 0 3.00 Time--> 4.87 4.74 5.15 5.06 4.18 3.77 3.51

5.96 6.21

8.90

11.15

7.19 7.29

9.78 12.74

4.00

5.00

6.00

7.00

8.00

9.00

10.00

11.00

12.00

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Special Regulation Lid Gaskets

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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

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Example - ITX
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Isopropylthioxanthone (ITX)

Photointitiator in UV-curing printing inks

Application: outside of food packaging (compound for milk, cacao, juice) Problems: - Set offeffect - Migration !!! Threshold 0,05 mg/kg ITX in food

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How to test Set off?

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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/foil a) roll b) pile - full-surface contact - flexible - 1kg/dm

Sample Name / Storage

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PIM whats next?

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New simulants

e. g. Tenax:

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PIM whats next?

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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)

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Contacts
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DI Michael Pitzl
(ext. 597, E-Mail: michael.pitzl@ofi.at)

sterreichisches Forschungsinstitut fr Chemie und Technik (ofi) Brehmstrae 14A 1110 Vienna +43-(0)1-798 16 01 ext. +43-(0)1-798 16 01 - 480

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