Gas chromatographic – mass spectrometric analysis of compounds generated upon thermal degradation of some stationary phases in gas chromatography – Part II

Abstract
The applicability of capillary columns for gas chromatography is often limited by stationary phase degradation at elevated temperatures. In order to achieve a better understanding of column thermostability, column bleed products have been analyzed qualitatively by gas chromatography‐mass spectrometry (GC‐MS). Three silicone stationary phases were studied: SE‐52, SE‐54, and OV‐1701. Each of these was immobilized in the columns. The proportion of cyclics containing diphenyl in column bleed from SE‐52 reflected to a large extent the composition of the polymer, while for SE‐54 the proportion of such cyclics was unexpectedly high. The polar moiety of OV‐1701, the cyanopropyl(phenyl)siloxy unit, was found to exert a highly destabilizing effect on the polymer, and the thermal degradation products consisted mainly of cyclosiloxanes containing this unit.