The catalytic adsorption of NO on activated carbon materials provides an appropriated alternative for the control of low-concentration emissions of this air pollutant. The surface complexes formed upon NO adsorption at 30 °C were studied by X-ray photoelectron spectroscopy (XPS) and temperature-programmed desorption (TPD). The effects of the addition of O2 and the presence of copper as a catalyst were studied. Copper assisted the oxygen transfer to the carbon matrix. For the Cu-impregnated carbon sample, the presence of O2 favored NO adsorption by increasing the breakthrough time, the adsorption capacity, and the formation of nitrogen and oxygen complexes of higher thermal stabilities, which mainly desorbed as NO and CO2.