A very simple, highly sensitive and selective spectrophotometric procedure was developed for the determination of copper(II). It is based on the reaction at pH 4-9 between the synthesized acetophenone-p-chlorophenylthiosemicarbazone (A-p-ClPT) and Cu(II) forming a green complex, Cu(II):A-p-ClPT (1:2), that floats quantitatively with oleic acid (HOL) surfactant. It exhibits a constant and maximum absorbance at 600 nm in both aqueous and surfactant layers. Beer ' s law is obeyed over the concentration range 0.25-6.35 mg l -1 with a detection limit of 0.021 mg l -1 for a standard aqueous solution of Cu(II) with a concentration of 3.82 mg l -1 (calculated on the basis of 3σ) and molar absorptivities of 5.5 × 10 3 and 1.3 × 10 4 mol l -1 cm -1 in aqueous and surfactant layers, respectively. Sandell's sensitivity was calculated to be 0.244 μg cm -2 and the relative standard deviation (n = 9) was 0.19%. The different analytical parameters affecting the flotation and determination processes were examined. The proposed procedure has been successfully applied to the analysis of Cu(II) in natural waters, certified scrap steel samples and vitamin samples. The results obtained agree well with those samples analyzed by atomic absorption spectrometry (AAS). Moreover, the flotation mechanism is suggested based on some physical and chemical studies on the solid complexes isolated from aqueous and surfactant layers.