X-ray photoelectron spectroscopy and time-of-flight secondary ion mass spectrometry were employed to study surface composition and electronic properties of Au/TiO2 catalysts produced by co-precipitation and deposition-precipitation techniques. As shown, the surface characteristics of the catalysts were dependent on the preparation route and pre-treatment conditions and exhibited correlation with catalytic performance of the samples. In the catalyst prepared by deposition - precipitation in a sodium-free environment and calcined at a moderate temperature, which demonstrated the highest and stable activity in CO oxidation at room temperature, a maximum fraction of reduced <$E roman Ti sup 3+> species and the largest level of surface hydroxylation were observed. Deterioration of catalytic properties of the samples prepared and pre-treated under different conditions is discussed in view of the alterations in the surface composition.

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