In attempt to compare the removal efficiency and yield of the activated carbon prepared using the conventional and microwave-assisted heating is the focus of this work. Toward this olive stone (a biomass precursor) is activated using the popular activating agent potassium hydroxide. The process optimization exercise is carried out by using the standard full factorial statistical design of experiments (response surface methodology). The activated carbons prepared under the optimized conditions are compared based on the adsorption capacity and yield. The adsorption capacity was found higher using microwave heating as compared with conventional heating. The microwave heating requires significantly lesser holding time as compared to conventional heating method to produce activated carbon of comparable quality, with higher yield. The BET surface area of carbon using microwave heating is significantly higher than the conventional heating. Although the mesopore surface area of carbon is not vary significantly, the activation time, power, and nitrogen gas consumption are significantly lower than the conventional heating rendering that the activation process via microwave is more economical than that via conventional heating. The adsorption isotherm data fitted the Langmuir isotherm well and the monolayer adsorption capacity was found to be 12.0 and 8.42 mg/g for microwave and thermally heated activated carbon, respectively. Regeneration studies showed that microwave-irradiated and thermally heated olive stone could be used several times by desorption with an HCl reagent. Both carbons can be used for the efficient removal of Ni2+ (>99%) from contaminated wastewater. (c) 2013 American Institute of Chemical Engineers AIChE J, 60: 237-250, 2014