An analytical method has been developed for the fluorimetric determination of nanogram amounts of aluminium in solution. The method is based on the reaction of aluminium with B-hydroxyquinoli-ne-5-sulfonic acid in presence of hexadeciltrimethylammonium bromide as a surfactant agent. Synchronous scanned first and second derivative fluorimetry has been employed to increase the sensitivity of the method. The influence of reaction variables as well as instrumental parameters is discussed. The interference of various foreign ions has also been examined and in some cases eliminated or reduced by addition of 1, 10-phenanthroline.