A green and simple technique for the separation via flotation and spectrophotometric detection of U(VI) in water and real ore samples is presented in this research study in which the heterocyclic azo dye 4-(2pyridyl azo) resorcinol (NaPAR) is used to preconcentrate the uranyl(VI) ions to form a reddish complex in the aqueous solution in the pH range 5.0.-6.0. The oleic acid (HOL) surfactant was used to float the formed 1:1 U(VI):NaPAR complex successfully and completely to the scum layer. The physicochemical characteristics of the proposed analytical technique have been determined. Under optimum parameters, the following physicochemical characteristics were obtained. Beer's law was obeyed up to 300 µg l-1, the correlation coefficient (R2) was calculated to be R2 = 0.9995. According to IUPAC recommendations, the limit of detection (LOD) and limit of quantification (LOQ) are 0.9 and 3.1 µg l-1 (n = 5), respectively. The molar absorptivity (Ɛ) is 0.63X106 l mol-1cm-1 in the scum layer with a preconcentration factor 100 and the RSD (n=5) is 2.5%. Excess amount of the chelating agent NaPAR was used to mask the effects of diverse ions on the flotation efficiency .The proposed procedure was applied to determine U(VI) in water samples as well as in U-Th and granite ore samples. The separation mechanism is explained.