The first use of bis(acetylacetone)propylenediimine, H2(pnAA2) for the determination of copper and nickel by flow injection analysis - spectrophoto metry has been studied. The proposed methods are simple, rapid and accurate and have been applied to the determination of copper and nickel in copper - based alloys and industrial waste water. The procedures gave satisfactory results. Two methods have been developed for the determination of copper. Firstly, copper can be determined spectrophotometrically at 355 nm, based on the reaction of copper(II) and bis(acetylacetone)propylenediimine in aqueous phase using flow injection system. The carrier stream was deionized water and the reagent streams were acetate buffer (pH5) and 0.5% (w/v) bis (acetylacetone) propylenediimine solution. The calibration graph was linear up to 120 ppm copper,based on injection volume of 500 . The relative standard deviation (n=10) was 4.16% for 20 ppm copper. The sampling rate was 36 h-1. Secondly, copper can be determined spectrometrically at 355 nm after extraction of the Copper(II)bis(acetylacetone)propylene diiminate chelate into chloroform. The carrier stream was deionized water and the reagent streams were acetate buffer (pH5) and 0.5% (w/v) bis (acetylacetone)propylenediimine solution. The calibration graph was linear up to 120 ppm copper, based on injection volumes of 250 . The relative standard deviation (n = 10) was 4.52% for 20 ppm copper. The sampling rate was 18 h-1. It has been found that the flow injection - extraction method gave an improved sensitivity. The method for the determination of nickel by flow injection analysis - spectrophotometry at 360 nm was developed, based on the reaction of nickel(II) and bis(acetylacetone)propylenediimine in aqueous phase. The carrier stream was deionized water and the reagent streams were phosphates buffer (pH7) and 2.0% (w/v) bis(acetylacetone)propylene diimine solution. The reaction stream was heated to 60 C and then cooled to room temperature prior to absorbance measurement. The calibration graph was linear up to 100 ppm nickel, based on injection volume of 500 . The relative standard deviation (n = 10) was 4.06% for 20 ppm nickel. The sampling rate was 30 h-1.