SynopsisPolyester thermosets have been prepared from maleic anhydride, phthalic anhydride, dibromoneopentyl glycol, and styrene, and their thermal degradation has been studied. Thermogravimetry has shown that degradation in air occurs in three main stages. For the 10% bromine polyester, the weight losses corresponded to 16.376, 69.7%, and 13.9% of the original polymer weight-the temperatures of the DTG peak maxima being 217OC, 345OC, and 530°C, respectively. Infrared analysis of the residues showed that above 25OOC there was a gradual reduction in the absorbance of all peaks with increasing temperature, indicating the degradation of all parts of the 3-dimensional polymer structure was occurring in a simultaneous manner. Degradation of the dibromoneopentyl glycol polyesters a t 53OOC in air proved to be a very complex process since a mixture of organic products was produced which gave rise to well over 100 peaks in the capillary column chromatograms. Under the conditions used, the low temperature degradation products proved to be rich in phthalic anhydride with no benzaldehyde being detected. The yields of benzene, toluene, styrene, and naphthalene increased with increase in temperature.