The thermal decomposition reactions of a novel nitro-aromatic polymer were investigated. Infrared spectroscopy was used to detect chemical structure changes that occurred in the solid material when it was heated. Mass spectrometry was employed to identify volatile products. The polymer decomposition mechanisms involved reactions between nitro groups and nearby methyl or methylene functionalities and primarily resulted in the formation of nitrogen monoxide gas and hydroxyl and carbonyl groups in the solid residue. (C) 2004 Wiley Periodicals, Inc.