Österreichisches Forschungsinstitut
für Chemie und Technik
www.ofi.at
CROPACK 2010
Migration Testing
 Overall migration
 SML tests
 Screening methods
DI Michael Pitzl
www.ofi.at
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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www.ofi.at
Locations and Departments
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
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Packaging
(incl. food commodities)
www.ofi.at
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

...
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Migration
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Mech.
Stress
Light
Hygiene
H2 O
Gas
Migration
Scalping
Product
Flavour
Active
Packaging
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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
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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
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Simulants
www.ofi.at

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:
if ethanol content > 10 %:
adaptation to the actual content!
50 % (v/v) Ethanol

Fatty foods:
Rectified olive oil (D)

Dry foods:
none
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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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www.ofi.at
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
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For materials and articles in contact with foodstuff
Main-REG (EC)
Nr. 1935/2004
GMP-REG (EC)
Recycl.-REG (EC)
A&I-REG (EC)
Nr. 2023/2006
Nr. 282/2008
Nr. 450/2009
Specific Directives
Reg. Cellulose
Vinyl chloride
BADGE, BFDGE, NOGE
2007/42/EC
78/142/EEC
VO (EG) Nr. 1895/2005
Analyses of VC
81/432/EEC
Analysis of
VC-content
80/766/EEC
Plastic
2002/72/EC
Ceramik
84/500/EEC
amanded
VO Nr. 975/2009
amanded2005/
31/EC
Rules Migration
List of Simulants
82/711/EEC
85/572/EEC
amended 97/48/EEC
amended 2007/19/EC
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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 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.
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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
TIC: HUND002.D
3.57
140000
5.96
6.21
3.51
130000
120000
4.18
110000
8.90
3.77
100000
90000
80000
11.15
70000
60000
4.87
50000 3.26
4.74
5.15
40000
7.19
7.29
5.06
9.78
12.74
30000
20000
10000
0
3.00
Time-->
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
www.ofi.at
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
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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/dm²
Sample Name / Storage
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PIM – what‘s next?
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
New simulants
e. g. Tenax:
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PIM – what‘s 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
www.ofi.at
DI Michael Pitzl
(ext. 597, E-Mail: michael.pitzl@ofi.at)
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
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