The polymeric precursor polystyrene sulphonate beads were used to produce activated carbon spheres (ACSs). ACSs were prepared by carbonization of polymeric precursor at 800 degrees C followed by activation of resultant char with steam and carbon dioxide activation processes. The resulting ACSs were characterized for N-2 adsorption, Raman spectrometry, and scanning electron microscope (SEM). The adsorption properties such as, BET surface area (S-BET), pore volume (V-pore), and micropore volume (V-micro) of ACSs produced at different gasification time and temperature with steam and carbon dioxide activation were investigated in this study. It is found that porosity of ACSs produced from steam and carbon dioxide activation increases with increasing activation time. The results exhibited that ACSs produced from above carbon dioxide activation have shown high S-BET and V-pore 1266 m(2)/g and 1.13 cm(3)/g respectively compared to ACSs from steam activation SBET 949 m(2)/g and V-pore 0.98 cm(3)/g, respectively. SEM study revealed that ACSs produced from carbon dioxide activation have exhibited a smooth surface and better microstructure as compared to ACSs from steam activation process. (C) 2009 Wiley Periodicals, Inc. J Appl Polym Sci 115: 2409-2415, 2010