A new selective and sensitive spectrofluorimetric method for the determination of trace amounts of nickel in industrial waste water has been developed. This method is based on the quenching of fluorescence of phenanthroline due to the formation of complex Ni (II)-Phen. The exitation and emission wavelengths were found to be 272 and 366 nm, respectively. There was a linear relationship in the range of 10.0-120 ng.mL-1 for Ni. This method is simple and rapid, and has been applied to the determination of nickel in industrial waste water.