Application of carbon molecular sieve (CMS) for gas separation has been found much attention recently. In this work, CMS was prepared from locally available palm shell through carbonization, steam activation and carbon vapour deposition (CVD) technique. After carbonization step, the char produced was subjected to steam activation at various activation times. The activated carbon obtained at 53.2% burn-off, which contain the highest amount of micropore volume was further used in CVD step by using benzene vapour at various deposition conditions. The performance of CMSs produced was examined by assessing the adsorption kinetics of O 2 , N 2 , CO 2 and CH 4 gases. All CMS samples showed a small N 2 and CH 4 uptake compared to the O 2 and CO 2 . The suitable conditions for CVD were found at 800°C, 30 min and 30 vol% benzene of deposition temperature, time and benzene concentration, respectively. At this point the O 2 /N 2 and CO 2 /CH 4 uptake ratios arrived 7.1 and 16.0, respectively.