A process is provided for making a modified carbon molecular sieve which is suitable for separating gases having different adsorption rates on the sieve. The process involves modifying a starting sieve support having a majority of micropores with an effective pore size of about 4.5 to 20 angstroms, with a two-step process in which the sieve is contacted with two different concentrations of a volatile carbon-containing organic compound, preferably a hydrocarbon. The concentration of the carbon-containing compound used in the first step is larger than that in the second step, so that the pore openings of the micropores of the support are narrowed successively in two distinct steps without filling the micropores themselves. The invention also discloses an improved carbon molecular sieve and the separation of gases, such as oxygen from nitrogen, by the use of this improved adsorbent.