Stationary phase based ontris(3,5-dimethylphenylcarbamoyl) cellulose is prepared under various conditions (precipitation, evaporation, sieving), and examined in HPLC columns for enantioseparation of racemic mixtures 1–10. Number of theoretical plates (N) and separation parameters (α and RS) are compared with those obtained with commercially available column based on the same polymeric material (Chiralcel OD, from Daicel Co.). Higher efficiency of the columns prepared by precipitation under specific conditions and followed by sieving of stationary phase, over those prepared by evaporation and (or without) sieving, is demonstrated.