A gas-liquid chromatographic method has been developed to separate on a small scale (acid samples as small as 2 mg) the enantiomers of 2-methylbutyric acid and to estimate a few per cent of one isomer as a contaminant in the other. Both the alpha-methylbenzyl ester and the alpha-methylbenzyl amide give a satisfactory resolution of the enantiomers. Chromatographic conditions in the order of importance are the final column temperature, the rate of temperature programming and the initial column temperature.