Thermal analysis of polystyrene, poly(p-methylstyrene) and poly(alpha-
methylstyrene) has been carried out using evolved-gas analysis by infr
ared and mass spectrometry, and direct-pyrolysis analysis by mass spec
trometric techniques. Evolved-gas analysis, both by infrared and mass
spectrometry, reveals features due mainly to the corresponding monomer
s or stable, volatile, and low relative molecular mass degradation pro
ducts. In direct-pyrolysis mass spectrometry, however, primary decompo
sition products and heavier fragments such as dimers and trimers can a
lso be detected. The ion-temperature profiles of the corresponding mon
omer ions reveal information about the thermal stability of the polyme
rs.