04 Migrationtesting_Pitzl

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sterreichisches Forschungsinstitutfr Chemie und Technik

www.ofi.at

CROPACK 2010

Migration Testing Overall migration SML tests Screening methods

DI Michael Pitzl


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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 %

Organisation and Facts


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Location Arsenal1030 Vienna, Arsenal Objekt 213,Franz Grill-Strae 5

Applied Polymer Technology

Varnishes and Adhesives

Construction

Sports Technology

Location Brehmstrae1110 Vienna, Brehmstrae 14a

Packaging

Medical Products

Eco Technology

Food Analysis

Administration

Locations and Departments


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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

...

Packaging(incl. food commodities)


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Migration

Scalping

Migration

ActivePackaging

H2O

Gas

FlavourProduct

Light

Mech.

Stress Hygiene


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Potential Migrants

Glas

- Silicates, heavy metals

Plastics

- Plasticizers, monomers, antistatics ...

Paper

- Additives and fillers (chalk etc.)

Metal

- Aluminium, tin for acid contents


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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 substancein the finished food contact material (QMA)

!!! Consideration of actual applied conditions

(time and temperature combinations)


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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 ofsimulants: 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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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

European Standardsconcerning plastics in contact with foodstuff


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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

Simulants

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


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Selection of the right Simulant

List of simulants:

Regulation 85/572/EECExample:


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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


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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)


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Migration Testing

Consideration of the practical usage conditions of the packaging (e. g. for whichfoodstuff 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


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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

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 ofVC-content80/766/EEC

Ceramik84/500/EEC

amanded2005/31/EC

Plastic

2002/72/EC

amandedVO Nr. 975/2009

Rules Migration

82/711/EECamended 97/48/EEC

List of Simulants

85/572/EECamended 2007/19/EC

GMP-REG (EC)

Nr. 2023/2006

Recycl.-REG (EC)

Nr. 282/2008

A&I-REG (EC)

Nr. 450/2009


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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).


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SML / QM

Test Methods: migration test medium + GC, HPLC

Positive List (excerpt):


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SML Save Testing Costs

Special Cases:

100% migration < SML

Calculation model


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Gas Chromatography


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Chromatographic Separation

Separation of substances mixture due to different retention times ofeach single analyte during the transport through thechromatographic bed


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Definitions

DECISION LIMIT: Threshold for the presence of an analyte

(yes/no). If a sample possessed the exact content of the dicisionlimit, 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 isdetected 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 thetriple amount of the decision limit.


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Thermodesorber:

Gas Chromatography


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Screening Methods

Migration or directly in food

Which peaks are explainable, which are not?

Criticism: Analysis method? Comparability? Undetected

substances?

3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.000

10000

20000

30000

40000

50000

60000

70000

80000

90000

100000

110000

120000

130000

140000

Time-->

Abundance

TIC: HUND002.D

3.26

3.51

3.57

3.77

4.18

4.74

4.87

5.06

5.15

5.966.21

7.19

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8.90

9.78

11.15

12.74


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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


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Example - ITX

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?

IVLV cluster commodities

Working group of German-speaking testing laboratorieseurofins, Fresenius, GALAB, GfU, innoform, ISEGA, MUVA, Nehring, of i, 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) rollb) pile- full-surface contact- flexible - 1kg/dm

Sample Name / Storage


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PIMwhats next?

New simulants

e. g. Tenax:


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PIMwhats next?

Priority:1. Specific migration

2. Overall migration

Overall migration:

Test conditions OM1-9 Regulations forrepeated contacts

Multi-layermaterials and articles

Test at 10 d 60 C for storage times > 30 d

Substitute simulants(scientific evidence)


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sterreichisches Forschungsinstitutfr Chemie und Technik (ofi)

Brehmstrae 14A1110 Vienna

+43-(0)1-798 16 01 ext.

+43-(0)1-798 16 01 - 480

DI Michael Pitzl(ext. 597, E-Mail: [email protected])

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04 Migrationtesting_Pitzl