The thermal behavior of ammonium molybdates, i.e. (NH 4 ) 6 Mo 7 O 24 •4H 2 O (1) and (NH 4 ) 2 MoO 4 (2), was studied in inert (N 2 ) and oxidizing (air) atmospheres by TG/DTA-MS, XRD, FTIR and SEM. The thermal decomposition sequence of 2 had similarities to 1; however, there were significant differences as well. When both of them were annealed, NH 3 and H 2 O were released parallel, and in air the asevolved NH 3 was burnt partially into NO and N 2 O. In both atmospheres, while 1 decomposed in four steps, the thermal decomposition of 2 involved 5 steps. In the case of 1, the intermediate products were Most decomposition steps were endothermic, except for the last step around 400 °C, where crystallization from the residual amorphous phase had an exothermic heat effect. In addition, the combustion of NH 3 also changed the DTA curve into exothermic in some cases. The morphology of the final products was characterized by 1-5 m sheet-like particles, except for annealing 2 in N 2 , when 0.5-1 m thick and 5-10 m long needle-shaped particles were detected.