A kinetic investigation of the ammoxidation of 3-picoline to 3-cyanopyrdine has been studied over V2O5/ZRO(2) Catalyst in a differential flow reactor in the temperature range 573-683 K. The partial pressures of 3-picoline, oxygen and ammonia were varied and rates were measured for the formation of 3-cyanopyridine. Kinetics studies reveal that the mechanism of the reaction is of the "Redox" type. The rate equation deduced, assuming a study state involving a three stage oxidation-reduction process, represented the data most satisfactorily for conversion of 3-picoline to nicotinonitrile. Catalysts have been characterized using IR, XRD, ESR, Surface area and ammonia desorption methods with a view to understanding the structure and nature of bonding over the surface of the catalyst. A tentative mechanism of the process has been suggested.