Volatile phenols in matured spirits were determined by gas-liquid chromatography as their 2,4-dinitrophenyl derivatives. Phenol, o-cresol, m-cresol, p-cresol, guaiacol, p-ethylphenol, p-ethylguaiacol, eugenol, and p-(n-propyl)guaiacol, which occurs only in dark rum, were studied at concentrations ranging from 0 to 2 ppm depending on the phenol and the beverage. Scotch, Spanish, and Japanese whiskies, unlike other whiskies examined, contained o-, m-, and p-cresols. Cresols occur in whiskies as a consequence of the raw materials used, in particular peated malt. The level of p-ethylguaiacol is usually somewhat higher in cognac and other brandies than in whiskies. Dark rums differ from the other spirits examined in containing p-(n-propyl)guaiacol, and, typically, higher levels of p-ethylphenol, p-ethylguaiacol, and eugenol. These phenols also occur in higher quantities in some white rums than in whiskies and brandies. Two discriminant functions were obtained by discriminant analysis, which did not, however, allow the spirits to be classified adequately into their respective groups. By using these functions, 82% of the whiskies, 57% of the brandies, and 50% of the rums were correctly grouped.