高分子分析用熱分解装置の開発と応用に関する研究

概要

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A new Curie-point pyrolyzer with a revised maintenance oven for pyrolysis gas chromatography (Py-GC) and a new autosampler, model Auto 330 for Curie-point Py-GC (CpPy-GC) were developed to analyze high molecular weight pyrolyzates. Data using the Auto 330 showed better reproducibility than that observed with the old type autosampler. A new injection system, called a Bio-Probe, was developed to analyze thermally labile samples using a CpPy-GC without thermal degradation or reaction in the pyrolyzer. A Curie-point direct injection probe for mass spectrometry was applied to the discrimination between a copolymer and a blended polymer containing the same monomer ratio as the copolymer. Addition of 0.5% triethylamine to chloroform as the mobile phase to depress the molecular interaction between the sample and the column packing resulted in improved reproducibility in size exclusion chromatography (SEC) of polar condensation polymers. Simultaneous hydrothermal decomposition-derivatization (SHD) of inert condensation polymers with tetramethylammonium hydroxide in alkaline solutions or with an acidic medium of hydrochloric acid (35 wt%)/methanol/acetic anhydride under near-critical pressures and temperatures was investigated by Curie-point heating GC/MS. The derivatives from condensation polymers using SHD provided simple chromatograms, greater structural information and good reproducibility.
社団法人日本分析化学会の論文
1995-09-05