Preparation of activated carbon has been attempted using CO2 as the activating agent from Jatropha hull, one of the popular feed stocks for biodiesel manufacture. The response surface methodology technique is utilized to optimize the process conditions. The influences of the three major parameters, activation temperature, activation time, and CO2 flow rate on the properties of activated carbon, are investigated using analysis of variance to identify the significant parameters. The optimum conditions for preparation of activated carbon has been identified to be an activation temperature of 950 degrees C, activation time of 40 min, and CO2 flow rate of 500 ml/min, an iodine number of 1,008 mg/g, and a yield of 18% were obtained, respectively. The BET surface area evaluated using nitrogen adsorption isotherm for the optimal sample corresponds to a 1,207 m(2)/g, with the pore volume of 0.86 cc/g. The activated carbon is heteroporous with the micropore volume contributing to 58%.