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04 Migrationtesting_Pitzl

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04  Migrationtesting_Pitzl Powered By Docstoc
					             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 %



                                                        2
www.ofi.at
                 Locations and Departments



             Location Arsenal                   Location Brehmstraße
             1030 Vienna, Arsenal Objekt 213,   1110 Vienna, Brehmstraße 14a
             Franz Grill-Straße 5




             Applied Polymer Technology         Packaging
             Varnishes and Adhesives            Medical Products
             Construction                       Eco Technology
             Sports Technology                  Food Analysis
                                                Administration


                                                                               3
                     Packaging
www.ofi.at           (incl. food commodities)


     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
            ...




                                                                             4
                Migration
www.ofi.at



     Mech.
     Stress                 Light       Hygiene


                                                     H2 O

                                                     Gas
             Migration        Product                Flavour


               Scalping                    Active
                                         Packaging


                                                               5
                Potential Migrants
www.ofi.at




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


                                                         6
               Migration
www.ofi.at



  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)
                                                                 7
                 Migration Testing
www.ofi.at




       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

                                                                           8
                      European Standards
www.ofi.at            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




                                                                      9
                 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)
                                               if ethanol content > 10 %:
            milk / milk products:       adaptation to the actual content!

             50 % (v/v) Ethanol
            Fatty foods:
             Rectified olive oil (D)
            Dry foods:
             none


                                                                             10
                Selection of the right Simulant
www.ofi.at


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




                                                  11
                  Standardized Testing Conditions according to
www.ofi.at        European Regulations / Austrian Plastics Regulation



       Migration Testing:
            Unknown contact time, application
             for ambient temperature or lower temperatures:
                                                              Overall migration –
             10 d / 40 °C (all simulants)                      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)




                                                                               12
                Migration Testing
www.ofi.at




        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)




                                                                   13
                 Migration Testing
www.ofi.at




                        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)?


                                                                                     14
www.ofi.at
                        Structure of the actual EU-Laws

 For materials and articles in contact with foodstuff

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

             Specific Directives



                                                                                Plastic            Ceramik
     Reg. Cellulose          Vinyl chloride        BADGE, BFDGE, NOGE         2002/72/EC         84/500/EEC
       2007/42/EC             78/142/EEC          VO (EG) Nr. 1895/2005        amanded          amanded2005/
                                                                            VO Nr. 975/2009        31/EC



                                            Analysis of           Rules Migration      List of Simulants
                 Analyses of VC            VC-content
                                                                    82/711/EEC             85/572/EEC
                  81/432/EEC               80/766/EEC           amended 97/48/EEC    amended 2007/19/EC




                                                                                                               15
                EU-Substances List / Synoptic Document
www.ofi.at




          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).




                                                                        16
                SML / QM
www.ofi.at



        Test Methods: migration test medium + GC, HPLC


        Positive List (excerpt):




                                                         17
              SML – Save Testing Costs
www.ofi.at




     Special Cases:
      100% migration < SML
      Calculation model




                                         18
             Gas Chromatography
www.ofi.at




                                  19
              Chromatographic Separation
www.ofi.at




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




                                                                          20
                  Definitions
www.ofi.at


            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.




                                                                                    21
              Gas Chromatography
www.ofi.at




         Thermodesorber:




                                   22
                        Screening Methods
www.ofi.at




          Migration or directly in food
          Which peaks are explainable, which are not?
         Criticism: Analysis method? Comparability? Undetected
               substances?
   Abundance


                                                         T  : U D 0 .D
                                                          IC H N 0 2
                        3.57                  5.96
                                                6.21
        140000          3.51

        130000

        120000
                               4.18
        110000
                                                                       8.90
                         3.77
        100000

             90000

             80000

             70000                                                                     11.15

             60000                    4.87

             50000 3.26
                                  4.74
                                     5.15               7.19
             40000                                       7.29                 9.78
                                       5.06                                                            12.74
             30000

             20000

             10000

                 0
                 3.00     4.00        5.00    6.00     7.00     8.00   9.00   10.00   11.00    12.00
   Time-->                                                                                                     23
                Special Regulation – Lid Gaskets
www.ofi.at



         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


                                                                   24
                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




                                                                  25
                 How to test „Set off“?
www.ofi.at


     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

                                                                                  26
                  PIM – what‘s next?
www.ofi.at



            New simulants

        e. g. Tenax:




                                       27
               PIM – what‘s next?
www.ofi.at




       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“)




                                                       28
                 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



                                                                              29

				
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