Thermal decomposition studies on two energetic triazole derivatives, viz N-(2,4-dinitrophenyI)-3-nitro-1,2,4-triazole (1a) and N-(2,4-dinitrophenyl)-3-azido-1.2,4-triazole (1b) have been investigated using simultaneous TG-DTA and TG-GC/MS techniques. Both compounds (1a) & (1b) showed good thermal stability, with exothermic decomposition peaks at 349 degrees C and 217 degrees C, respectively on DTA. Compound (1a) was found thermally more stable, and showed gradual weight loss after 250 degrees C. Kinetic parameters were calculated from the DTA peak temperatures, at different heating rates according to the method of Ozawa and Kissinger and refined for accuracy as per the ASTM E698 standard. Qualitative analysis of gaseous species produced during the decomposition was analysed using mass spectrometry, using the TG-GC/MS techniques. As evident from mass spectrum both compounds showed presence of CO(2), NO(2), NO, HCN, N(2), & H(2)O among the products of decomposition. (c) 2011 Elsevier B.V. All rights reserved.