Characterization and temperature-programmed studies were performed over Pd/titania catalysts to examine their activity in the reduction of NO with methane. The catalyst was prepared using a wet impregnation technique and Pd-acetate was used as a precursor for palladium. Techniques such as BET surface area measurements, X-ray diffraction, laser Raman spectroscopy, X-ray photoelectron spectroscopy, and scanning electron microscopy were used for the characterization of the catalyst before and after the reaction. Temperature-programmed reduction (TPR) and temperature-programmed desorption (TPD) were also used to probe the surface to understand its adsorption/desorption characteristics and reducing capabilities. The results obtained from these studies together with the reaction investigations have given some important insight into the functionality of this catalyst.