Nanosize gold particles were prepared by Ar(+) ion implantation of 10-nm thick gold film deposited onto a SiO(2)/Si(100) wafer possessing no catalytic activity in the CO oxidation. Along with size reduction the valence band of the gold particles and the actual size were determined by ultraviolet- and X-ray photoelectron spectroscopy (UPS, XPS) and by transmission electron microscopy (TEM) as well as atomic force microscopy (AFM), respectively. The catalytic activity was determined in the CO oxidation. Energy distribution of the photoelectrons excited from 5d valence band of gold was strongly affected by Ar(+) implantation. This variation was interpreted by the redistribution of the valence band density of states (DOS). The intrinsic catalytic activity of the gold particles increased with decreasing size. When an Au/FeO(x) interface was created by FeO(x) deposition on large gold nanoparticles, a significant increase in the rate of the CO oxidation was observed. These data can be regarded as an experimental verification of the correlation between the catalytic activity and valence band density of states of gold.