The thermogravimatric decomposition of anilinum octamolybdate has been studied under non-isothermal conditions to elucidate the chemical reactions taking place in the first step of decomposition of the anhydrous compound.The decomposition products were analyzed by gas--liquid chromatography, gas chromatography-mass spectrometry (GC/MS), infrared spectroscopy and X-ray powder diffraction.The main decomposition product of aniline turned out to be indole, which is different from the major product in the isothermal decomposition at the same temperature, i.e. N-ethyl-aniline.A dehydrocyclization reaction is suggested as the rate-dependent process. This is probably due to the catalytic effect of the octamolybdate anion.In the study of the isothermal decomposition of anilinium octamolybdate dihydrate [1], the complex degradation of aniline was found to occur between 468 and 493 K.In the present work, we have analyzed in more detail the anilinium cation degradation process in the first decomposition step and the octamolybdate anion break