A simple procedure for precolumn fluorescence derivatization of low-molecular-weight aliphatic alcohols (C
1-C
4) with 9-fluorenylmethyl chloroformate is presented.The derivatization reaction proceeds in 1:1 (v/v) aqueous-acetonitrile solution at room temperature with asodium phosphate buffer of pH 12.5 as a catalyst. Stablefluorescent derivatives of the alcohols are formed within10 min. The four derivatives are separated by reversed-phase high-performance liquid chromatography and detected by a fluorescence detector at an excitation wavelength of 259 nm and an emission wavelength of 311 nm.The method detection limits are 4, 40, 70, and 30 pmolfor methanol, ethanol, propanol, and butanol, respectively, per 5-
L injection volume. The relative standarddeviations are 3.7% for methanol at 75 pmol and 2.1, 1.5,and 2.2% for ethanol, propanol, and butanol, respectively,at 750 pmol. As a preliminary application, the methodwas used to determine methanol concentration in laboratory air and ethanol content in a commercial alcoholicbeverage.