The concentrations of volatile fatty acids (VFA) in soils are important in studies involving phytotoxicity and fermentation processes. Concentrations of acetic, propionic, and butyric acids as low as 0.21, 0.14, and 0.10 mmol kg‐1soil in water extracts were accurately determined. The extracts were filtered through 45 μm millipore disc filters and injected directly into a gas chromatograph following addition of purified formic acid. The formic acid eliminated ghosting of peaks. The gas chromatograph was equipped with a flame ionization detector and a 60/80 Carbopack C/0.3% Carbowax 20M/0.1% H3PO4packed precolumn (0.15 m) and column (1.83 m). The precolumn was changed after 150 to 200 sample injections when contaminated beyond acceptable limits. There was good separation of VFA with no interfering organic volatiles in extracts of soil containing glucose, cellulose or straw incubated anaerobically for as long as 4 weeks. The advantages of the procedure are relative rapidity and simplicity as well as improved sensitivity in measuring small quantities of volatile fatty acids in soil