A simple gas chromatographic (GC) procedure has been developed to estimate the individual alkylated phenols used as antioxidants to improve the shelf life of fuels and lubricants. Preparative gas chromatography was applied for separation and collection in sufficient quantity of the isomers of tertiary butyl, octyl and dodecyl phenols prepared by catalytic alkylation of phenol with isobutylene or its oligomers. The separated fractions were characterised by Infra-red spectrometry (IR) and paper chromatography. Out of several GC columns studied, a high resolution capillary column of 100% Methyl, Silicone gum (SE-30) as stationary phase gave best results. Data generated on various pac and capillary columns are in good agreement.