Adsorption on carbon molecular sieves (CMS) prepared by coke deposition has become an interesting area of adsorption due to its microporous nature and favorable separation factor on size and shape selectivity basis for many gaseous systems. In the present work CMS was synthesized from coconut shell through three major steps, namely, carbonization, activation, and coke deposition by hydrocarbon cracking. The crushed, washed, and sieved granules of coconut shell (particle size 2-3 mm) were pretreated with sodium silicate solution and oven-dried at 150 degrees C to create the inorganic sites necessary for coke deposition. Carbonization and activation of the dried granules were carried out at 800 degrees C, for 30 min each. The activated char thus produced was subjected to hydrocarbon cracking at 600 degrees C for periods varying from 30 to 180 min. The product samples were characterized in terms of adsorption isotherm, kinetic adsorption curve, surface area, pore volume, pore size distribution, and characteristic energy of adsorption by using O-2, N-2, C2H2, CO2, C3H6, and CH4.