In this study the V2O5/Nb2O5 catalysts were prepared using grafting and impregnation techniques. Both the V2O5/Nb2O5 prepared catalysts and the adsorption of pyridine on V2O5/Nb2O5 have been studied with FTIR spectroscopy. For grafted catalysts it was shown that a uniform dispersion of vanadium on the support was achieved. However, in the case of impregnated V2O5/Nb2O5 catalysts it was seen that the support was covered by the bulk phase of V2O5. Pyridine was used as a selective probe molecule to characterize both qualitative and quantitative aspects of surface acidity.