Oil fly ash from power generation plants was activated with 30% NH4OH and used for selective adsorption of carbon dioxide from CO2/N-2 mixture. The treated samples were characterized for their surface area, morphology, crystalline phase, chemical composition and surface functional groups. Energy dispersive X-ray analysis showed an increase in the carbon contents from 45 to 73 wt% as a result of leaching out metal oxides. XRD proved that chemical activation of ash resulted in diminishing of major crystalline phases of zeolite, and other alumino-silicates leaving only quartz and mullite. BET analysis showed an increase in surface area from 59 to 318 m(2)/g after chemical activation and the pore volume increased from 0.0368 to 0.679 cm(3)/g. This increase in pore volume is supported by the results of SEM, where more micropores were opened with well-defined particle sizes and porous structure. The TGA of the treated fly ash showed stability at higher temperature as the weight loss decreased with increasing temperature. For treated ash, the FTIR displayed new peaks of amine functional group. The treated ash was used for the removal of CO2 from CO2/N-2 mixture and the maximum adsorption/capturing capacity was found to be 240 mg/g. This capacity increases with increase in initial gas concentration, inlet flow rate and temperature suggesting the endothermic nature of the interaction between the gas molecules and the surface of the ash. (c) 2012 Elsevier B.V. All rights reserved.