A novel Schiff base ligand (N, O system) 5-methoxy-2-phenyliminomethylphenol (5-CH3O-PMP) was synthesized. Using the synthesized ligand as a fluorescent reagent, a fluorometric method was developed for the quantitative analysis of Al(III) ion. The quantitative analysis of Al(III) ion was performed by making the complex compound between Al(III) ion and 5-CH3O-PMP in ethanol-water solution (85/15, v/v, pH 6.2). The excitation wavelength (λem) of the complex compound was 397 nm while the emmision wavelength (λem) was 498 nm. The quantitative analysis of Al(III) ion was carried out by estimating the fluorescence intensity. The various calibration curves were used for the quantitative analysis in the range of 0.27~27 ng/mL Al(III) ion concentrations. The detection limit was 0.027 ng/mL. Using the fluorometric method developed in this study, satisfying results were obtained from various samples such as tap water, hot spring water, river water, sea water and waste water, which contained considerable amounts of interfering ions.