To prepare carbon molecular sieves (CMSs), methane was pyrolyzed in an attempt to deposit fine carbon particles on the micropore mouths of the carbon substrates being heated; the carbon substrates included grain-based activated carbons and commercial activated carbons. To explore the effects of heat treatment alone, blank experiments were conducted by heating the samples in N-2. The resultant products were characterized by N-2-adsorption at 77 K. Methane failed to deposit carbon at 800 degrees C. The porosity of activated carbons, however, was substantially influenced by heat treatment alone. The surface areas and micropore volumes of the activated carbons from grain sorghum decreased by 39.32% and 36.84%, respectively, upon heat treatment alone; this is attributable to the destruction of pore structure by sintering. In contrast, the corresponding values of the commercial activated carbons increased by 59.86% and 62.16%, respectively, upon heat treatment alone; this can be attributable to the development of microporosity. (c) 2005 Elsevier Ltd. All rights reserved.