Abstract. Alpha and beta cyclodextrin (a-and /3-CD) were chemically bonded to porous layer fused silica open tubular columns and used as gas-solid chromatographic (GSC) stationary phases for the separation of Cl to C6 hydrocarbons and a variety of inorganic gases. In general, these cyclodextrin PLOT columns were superior to the analogous packed columns. The capillary columns show similar selectivities with an increase in efficiency and number of theoretical plates over the packed columns. The cyclodextrin stationary phases show good selectivities toward the light hydrocarbons and inorganic gases on capillary columns as short as ten meters. Subambient temperatures allow the baseline resolution of oxygen from nitrogen. These columns have been effectively utilized at temperatures up to 260°C without loss of efficiency or degradation of selectivity.