Volatile acids were separated from food samples by a steam distillation according to AOAC methods, neutralized, and evaporated to dryness. The acids were then liberated with an equivalent amount of 0.5N dichloroacetic acid in acetone. Three microliters of the acetone solution containing from 0.1 to 1.0 mg of each acid per ml was injected directly into the column of the gas chromatograph. Experimental conditions were: Six-foot glass column; support, Anakrom 110/120 mesh; substrate, 10.5% ethyleneglycol adipate and 1.75% phosphoric acid; column temperature, 100°C; Sr90 detector temperature, 170°C; vaporizer temperature, 200°C; detector voltage, 1400 volts; argon flow rate, 50 ml per minute. Peak heights and responses relative to methyl enanthate (heptanoate) as an internal standard were used to calculate concentrations of the individual acids. Recoveries from known mixtures were 95—105% for lower concentrations of the acids and 97—101% for higher concentrations. Results of analyses of frozen whole eggs and of frozen fish fillets agreed with results by AOAC methods.