X-ray photoelectron spectroscopy (XPS) has been applied to the study pertaining to preparation and characterization of catalysts used in propylene polymerization. The analysis has indicated support/donor interaction in active support (adduct) and active support/TiCl4 interaction during catalyst preparation process. A systematic study has been made to identify suitable adduct from a set of three adducts for catalyst synthesis. Precise binding energy of Titanium species on catalyst surface has been measured and its dispersion on support has been evaluated to correlate catalyst performance with the surface spectroscopic parameters.