A new reagent, N-(2,6-dimethylphenyl)aminoglyoxime (DAGH(2)) has been synthesized and used for developing a simple and rapid extractive method for the spectrophotometric determination of nickel and copper. This method is based on the selective extraction of nickel and copper complexes from aqueous solution into cyclohexanol-dichloromethane (1:1) and the measurement of their absorptions at 470 nm and 410 nm, respectively. Various factors influencing the sensitivity of this method such as wavelength, pH and stirring time and the effect of some foreign ions and the ranges of applicability of Beer＇s law on the determination of nickel and copper have been investigated. Some properties such as composition, extraction and solubility of the complexes formed between DAGH(2) and metal ions [Ni(II) and Cu(II)] have also been studied.