Isolation of phenols from Eucalyptus wood pyrolysis tar was carried out with the objective of recovering valuable pure phenols, such as phenol, cresols, guaiacol, 4-methylguaiacol, catechol and syringol. The approach included a primary conversion of the raw wood tar into a lighter oil. Phenolic compounds were further separated from the oil by liquid-liquid extraction using alkali and organic solvents. GC/MS analysis of acetyl-derivatized phenolic compounds was used to evaluate the separation method. The primary conversion allowed the isolation of a lighter oil containing the desirable compounds without causing major chemical changes in the distilled oil. Liquid-liquid extraction by alkali and organic solvents essentially yielded a phenolic fraction. Removal of phenols was more efficient under highly alkaline conditions. An evaluation of the analytical procedure for the determination of phenols was also undertaken.