A series of vanadium-tin mixed oxide catalysts have been prepared by the solid-state reaction of V2O5 and SnO2 at 1250 degrees C. The fresh and the used catalysts have been characterized by X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). High temperature oxygen chemisorption (HTOC) has been employed to titrate the coordinatively unsaturated vanadia sites. Ammoxidation of mesitylene has been carried out on these catalysts and an optimum composition of vanadium is arrived at. Better yields of tricyanobenzene (TCB) compared to literature values are obtained. A good correlation between the oxygen uptake and the TCB yield extends the applicability of HTOC to the fused oxide system.