A technique for the analysis of trace amounts of volatile products from polymer degradations

A technique for the qualitative and quantitative analysis of trace amounts (0, 1 mg) of liquid nitrogen-condensable volatiles produced during polymer degradation is described. Products trapped at liquid nitrogen temperature at 10⁻⁵ torr are slowly distilled into a second trap as a result of the gradual warm-up of the first trap. Pressure changes accompanying distillation are detected by a Pirani gauge and are used to characterize individual degradation products following calibration of the system using reference liquids. Quantitative analysis is achieved by fractionation of the products and measurement of the total pressure exerted by each component on complete vaporization in a closed system. Variables influencing the sensitivity of the technique are examined.