Österreichisches forschungsinstitut für chemie und technik cropack 2010 migration testing overall...
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Österreichisches Forschungsinstitutfür 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-Straße 5
Applied Polymer TechnologyVarnishes and AdhesivesConstruction Sports Technology
Location Brehmstraße1110 Vienna, Brehmstraße 14a
PackagingMedical 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
Client‘s R&D-Projects
Branch-oriented R&D-Projects
Branch-oriented Training and Education
...
Packaging (incl. food commodities)
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Migration
Scalping
Migration
Active Packagin
g
H2O
Gas
FlavourProduct
LightMech. 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 substance in 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 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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CEN TC 194CEN 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
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Aqueous foods pH > 4,5 Distilled water (A)
Acidic foods pH 4,53 % (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/EEC
Example:
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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 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
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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 of VC-content 80/766/EEC
Ceramik84/500/EEC
amanded2005/31/EC
Plastic2002/72/EC
amanded VO Nr. 975/2009
Rules Migration
82/711/EEC amended 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 of each single analyte during the transport through the chromatographic 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 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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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
5.96 6.21
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 off–effect
- 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 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?
New simulants
e. g. Tenax:
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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“)
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Österreichisches Forschungsinstitutfür Chemie und Technik (ofi)Brehmstraße 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])
Contacts