The ammonium salt of 12-molybdophosphoric acid has been prepared by the solid-state interaction of the ammonium salts of molybdenum and phosphorus. The catalysts obtained by pretreatment of the precursor at various temperatures, have been characterized by nitrogen adsorption, X-ray diffraction (XRD), Fourier-transformed infrared (FTIR) spectroscopy and temperature-programmed decomposition (TPD) of the catalysts. Ammoxidation of 2-methylpyrazine has been carried out on these catalysts. The amount of ammonium salt present in the catalyst has been correlated with the activity and selectivity of the catalysts.