Abstract: Under specified conditions, the cross-linked copolymcr beads of styrene-divinyl-bcnzene were pyrolyzed into carbonaceous adsorbent which may be used as stationary phase in gas solid chromatography. The chromatographic separation efficiency of some spherical carbonaceous adsorbents for various gases were studied. It has been proved that the separation power for inert gases, permanent gases and C₁-C₃ light hydrocarbons is excellent.This kind of adsorbent is similar to carbon molecular sieves (CMS) in separating property, but it shows some good advantage over them.