Abstract
The thermal volatilization analysis (TVA) and subambient thermal volatilization analysis (SATVA) techniques are described. In addition to rate profiling of the volatile product flux of thermal degradation under high-vacuum conditions through measurement of pressure in the vacuum line as a function of sample temperature, the TVA technique is shown to afford a convenient method for an isolation, on the basis of volatility under high-vacuum conditions, of product fractions of thermal degradation for subsequent spectroscopic analysis. The capacity and flexibility of TVA as a platform for these analyses are illustrated in a case study format by degrading poly(bisphenol A, 2-hydroxy propylether). The overall degradation process is quantified, and most significant pathways of thermolysis are identified through subsequent spectroscopic analysis of products of decomposition. The design and construction of a modified vacuum-tight long-path gas IR cell, as an interface allowing for the application of Fourier transform infrared spectroscopy (FT-IR) for the on-line analysis of volatile products of polymer degradation, is detailed. Proof of concept and application of this new analytical technique, subsequently referred to as TVA/FT-IR, is illustrated through the examination of appropriate aspects of the thermal degradation of polymethyl methacrylate polymers.
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