Inert gas condensation was used to generate nanocrystalline Ladoped CeO, -=. Non-stoichiometric CeO,-x-based materials were found to be excellent catalysts in recent studies for the selective reduction of SO,. To understand better the stoichiometry-related catalytic properties, the surface chemistry of nanocrystalline La-doped CeO, -= was investigated through in situ oxidatiowreduction thermal treatments. Oxidation in CO, and reduction in H, atmospheres were performed between 30 O C and 600 O C in a reaction chamber connected to an x-ray photoelectron spectrometer analytical chamber. Curve fitting and target factor analysis were used to obtain a semiquantitative measurement of the transformation between + 3 and +4 oxidation states during these reactions. Target factor analysis was found to be a very useful tool for analyzing the contributions corresponding to Ce+3 and Ce".