SummaryIn this study, the separation of polar compounds in solvating gas chromatography (SGC) was investigated. Capillary columns (250 gm i.d.) packed with deactivated siliceous particles, including SE-54 encapsulated silica particles, diol-bonded silica particles, and polyethylenimine (PEI) coated particles, and nonsiliceous particles of styrene-divinylbenzene were used. Polar compounds that were used as test solutes included ketones, aldehydes, esters, nitro-containing compounds, alcohols, phenols, fatty acids, and amines. It was found that capillary columns packed with SE-54 encapsulated particles were suitable for the separation of medium polar compounds, columns packed with diol bonded silica particles could be used for separation of strongly polar compounds such as fatty acids, and columns packed with PEI coated silica particles were suitable for the separation of basic compounds such as alkylamines under SGC conditions. Columns containing the polymeric particles could be used for the separation of medium polar compounds and weak bases, however, low column efficiency was observed. SGC was found to provide better separation of polar compounds than high pressure gas chromatography (HPGC). A sample of a peppermint oil was separated within 8 min under SGC conditions.