Results of a study devoted to provide the pure enantiomers of isoflurane and desflurane from racemic mixtures using gas chromatography are presented. For that purpose, a cyclodextrin-based selector described in earlier work was immobilized on porous glass beads. The adsorption isotherms were determined and applied to predict operating parameters which provide the highest possible productivity of the separation. The analysis included evaluation of the performance of larger columns applying simplifying scale-up considerations. Using repetitive batches, the method can provide per day with a laboratory scale column approximately 1 g pure enantiomer. Selected model predictions were validated experimentally.