SIMULTANEOUS HYDROTHERMAL DECOMPOSITION AND METHYLATION - HIGH-RESOLUTION GAS-CHROMATOGRAPHY MASS-SPECTROMETRY FOR POLYMER CHARACTERIZATION

High speed hydrothermal decomposition of some chemically inert condens ation polymers in alkaline solutions under near-critical pressures and temperatures has been investigated by on-line Curie-point heating-hig h resolution GC-MS. The technique also involves simultaneous methylati on with tetramethylammonium hydroxide in a 1 mm i.d. x 20 mm sealed gl ass capillary. The relative standard deviation for the peak intensity (mol %) resulting from ten replicate measurements of poly(butylene ter ephthalate) is approximately 3%. This method requires a small amount o f sample (ca. 0.1 mg) and provides simple chromatograms, greater struc tural information, good reproducibility, and rapid reaction (0.5-15 mi n) without chemical treatment. A brief overview of applications to the characterization of some condensation polymers such as aromatic polye ster, polycarbonate, and aliphatic and aromatic polyamide is also desc ribed.