Polymer troubleshooting and QC with FTIR DSM Research

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

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? Analytical Services P. Meijers DSM Research

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

Polymer troubleshooting and QC with FTIR 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 Analytical Services P. Meijers DSM Research

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

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

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: C 2 and stabilizer content EPDM: C 2/C 3 ratio (ASTM D 3900) and diene content (D 6047) Stabilizer content Analytical Services P. Meijers DSM Research

Polymer troubleshooting and QC with FTIR C 2/C 3 ratio in EP(D)M according to ASTM D 3900 Analytical Services P. Meijers DSM Research

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

Polymer troubleshooting and QC with FTIR 1. FTIR identification Unknown sample organic NMR Microscopy Py. GC Analytical Services P. Meijers FTIR inorganic XRF Microscopy DSM Research

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

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 Analytical Services P. Meijers DSM Research

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

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

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

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) Analytical Services P. Meijers DSM Research

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

Polymer troubleshooting and QC with 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) Analytical Services P. Meijers DSM Research

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 Analytical Services P. Meijers DSM Research

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