Polymer Troubleshooting and QC with FTIR: Techniques and Applications

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

2. 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? Polymer troubleshooting and QC with FTIR

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

4. Analytical Services (70 FTE) Additive analysis In process analysis Elemental analysis Microscopy Thermal analysis Mathematics & statistics Optical Spectroscopy Nuclear Magnetic Resonance Molecular characterisation Chromatogr. & mass spectrom. Engineering plastics, functional groups & titrimetry Polymer troubleshooting and QC with FTIR

5. Optical spectroscopy (6 FTE) - Raman spectroscopy - UV-VIS spectroscopy - Colorimetry - FT IR spectroscopy Polymer troubleshooting and QC with FTIR

6. 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 Polymer troubleshooting and QC with FTIR

7. 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 Polymer troubleshooting and QC with FTIR

8. Polymer troubleshooting and QC with FTIR C2/C3 ratio in EP(D)M according to ASTM D3900

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

10. Polymer troubleshooting and QC with FTIR 1. FTIR identification Unknown sample organic inorganic FTIR NMR Microscopy PyGC XRF Microscopy

11. Examples of FTIR spectra of inorganics talc chalk Polymer troubleshooting and QC with FTIR

12. 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 Polymer troubleshooting and QC with FTIR

13. Example of complaint: SBR gel in EPDM compound Polymer troubleshooting and QC with FTIR

14. Polymer troubleshooting and QC with FTIR FTIR spectrum of cellulose

15. Polymer troubleshooting and QC with FTIR FTIR spectrum of polypropylene

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

17. Polymer troubleshooting and QC with FTIR 4. (FTIR) Research for third parties

18. 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) Polymer troubleshooting and QC with FTIR

19. 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 Polymer troubleshooting and QC with FTIR

20. www.dsm-solutions.com 31(0)46 4760404 “Analysis is our passion”