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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
7.29
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: michael.pitzl@ofi.at)
Contacts
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