The present study focuses on the removal of CO by the water-gas shift reaction over the bimetal CeO2 and Ni nanoparticles (NPs) dispersed in the multi-scale web of activated carbon micro/nanofibers (CNFs/ACF). The CNFs were grown on an ACF substrate, using catalytic chemical vapor deposition and acetylene as the carbon source. The Ni NPs had dual roles as the catalyst: (1) for decomposing acetylene and (2) for the oxidation of CO. The CeO2 dispersed in the ACFs provided necessary nascent oxygen for the oxidation. Approximately 80 % conversion of CO was achieved at 400 A degrees C, using 2 % (v/v) CO in nitrogen. The high reaction rate [similar to 0.75 A mu mol CO/g-s] on the prepared material was attributed to the catalytic Ni NPs, oxygen providing CeO2, surface functional groups-containing ACF, and active exposed edges of hexagon in the CNFs. The prepared bimetal containing CNF/ACF web is a potential catalyst for the effective removal of CO without requiring an external supply of O-2 or a promoter. [GRAPHICS] .