1. DSM Research Research Analytical Services P. Meijers Polymer troubleshooting and QC with FTIR DSM Research, CT&A - Analytical Services December 2002 Peter Meijers

2. DSM Research Research Analytical Services P. Meijers Polymer troubleshooting and QC with FTIR Topics to be covered today - Where do we analyse? - Why do we analyse? - What do we analyse? - How do we analyse? - For whom do we analyse?

3. DSM Research Research Analytical Services P. Meijers Polymer troubleshooting and QC with FTIR Research Campus Geleen Performance polymers Life Sciences Industrial Chemicals SABIC Petrochemical Europe Center for Technology & Analysis Technology 60 Anal. Services 70 FTE DSM R&D outside Campus Geleen Third parties

4. DSM Research Research Analytical Services P. Meijers Polymer troubleshooting and QC with FTIR Analytical Services (70 FTE) Additive analysisIn process analysis Elemental analysisMicroscopy Thermal analysisMathematics & statistics Optical Spectroscopy Nuclear Magnetic Resonance Molecular characterisationChromatogr. & mass spectrom. Engineering plastics, functional groups & titrimetry

5. DSM Research Research Analytical Services P. Meijers Polymer troubleshooting and QC with FTIR Optical spectroscopy (6 FTE) - Raman spectroscopy - UV-VIS spectroscopy - Colorimetry - FT IR spectroscopy

6. DSM Research Research Analytical Services P. Meijers Polymer troubleshooting and QC with FTIR FT-IR spectroscopy (MID-IR 4000 – 400 cm -1 ): - Transmission - Transmission via microscope - Reflection (ATR crystals: Diamond, Germanium, Silicon) - Multi bounce HATR (Zinc Selenide) - Real-time kinetic analysis

7. DSM Research Research Analytical Services P. Meijers Polymer troubleshooting and QC with FTIR Some examples of Quality Control with FTIR PE:Branching level, type of comonomer C=C unsaturation: end, side, trans MAA-content in PE-MAA PP:C2 and stabilizer content EPDM:C2/C3 ratio (ASTM D3900) and diene content (D6047) Stabilizer content

8. DSM Research Research Analytical Services P. Meijers Polymer troubleshooting and QC with FTIR C2/C3 ratio in EP(D)M according to ASTM D3900

9. DSM Research Research Analytical Services P. Meijers Polymer troubleshooting and QC with FTIR Troubleshooting with FTIR 1. Identification 2. Complaints 3. Competitor analysis 4. Research for third parties

10. DSM Research Research Analytical Services P. Meijers Polymer troubleshooting and QC with FTIR Unknown sample FTIR organicinorganic NMR Microscopy PyGC XRF Microscopy 1. FTIR identification

11. DSM Research Research Analytical Services P. Meijers Polymer troubleshooting and QC with FTIR Examples of FTIR spectra of inorganics talc chalk

12. DSM Research Research Analytical Services P. Meijers Polymer troubleshooting and QC with FTIR 2. FTIR complaints - Blooming - Small contaminations (up to 10 µm) Organic: cellulose, gels, PE wax, SBR, Ca/Zn-stearate, teflon Inorganic: calcium carbonate, calcium oxide, clay, mica, talc

13. DSM Research Research Analytical Services P. Meijers Polymer troubleshooting and QC with FTIR Example of complaint: SBR gel in EPDM compound

14. DSM Research Research Analytical Services P. Meijers Polymer troubleshooting and QC with FTIR FTIR spectrum of cellulose

15. DSM Research Research Analytical Services P. Meijers Polymer troubleshooting and QC with FTIR FTIR spectrum of polypropylene

16. DSM Research Research Analytical Services P. Meijers Polymer troubleshooting and QC with FTIR 3. FTIR competitor analysis Compound composition: - polymer type - filler type (chalk, clay, talc) (via TG: amount of polymer, carbon black, ash rest)

17. DSM Research Research Analytical Services P. Meijers Polymer troubleshooting and QC with FTIR 4. (FTIR) Research for third parties

18. DSM Research Research Analytical Services P. Meijers Polymer troubleshooting and QC with FTIR FTIR = A POWERFUL TOOL - Direct measurement on material - Quick method - Much chemical info - Not destructive - Small amounts of sample needed However: it is NOT absolute (reference method is needed for quantification)

19. DSM Research Research Analytical Services P. Meijers Polymer troubleshooting and QC with FTIR The Analytical service group at Research campus Geleen has: - Broad toolbox - Long history in material science - Strong knowledge position on polymer materials - Proprietary data bases (additives, spectra) - Experienced and skillful people

20. DSM Research Research Analytical Services P. Meijers www.dsm-solutions.com www.dsm-solutions.com 31(0)46 4760404 “Analysis is our passion”