Abstract: Chiral 3′-chloro-1-phenylpropanol (CPNL) was prepared by asymmetric catalytic reduction of 3′-chloro-phenylpropanone (CPNN), and gas chromatography was applied to the determination of the product and the unreacted raw material in the reaction liquid. 2-Methyl-phenylpropanol was used as internal standard and the chiral capillary chromatographic column, CP-Chirasil-Dex CB with chemical bonded β-cyclodextrin as stantionary phase was used for separation. Both the separation of CPNN and CPNL and the separation of the enantiomorphs of (R) and (S) CPNL were carried out effectively. Errors due to in-accurate sample introductions were overcome by the use of internal standard. Values of detection limit (3S/N) for CPNN and (S) CPNL were found to be 13.14 mg·L-1 and 18.75 mg·L-1 respectively. Results of recovery tests for the 2 above mentioned compounds found by addition of standards were in the ranges of 99.5%-101.8% and 96.5%-100.4% respectively. Values of RSD′s (n=6) found were 0.39% for CPNN and 0.74% for both the (R)-and (S)-CPNL.