Ultra trace amounts of uranyl ions was extracted using a reliable, simple and selective solidified floating organic drop microextraction (SFODME) method and determined by UV-Vis spectrophotometry. Di-2-ethylhexylphosphoric acid (HDEHP) was applied as complexing ligand during the microextraction process and Arsenazo III (AIII) was used as the chromogenic reagent through spectrophotometric determination. The effects of the important experimental parameters on UO 2 -AIII complex formation and color development were studied. Other important experimental parameters affected microextraction recovery, such as; type and volume of extracting organic solvent, acid concentration of sample solution, ligand concentration, stirring rate, extraction time and temperature, and salt addition effect were also evaluated and optimized. Under the optimized conditions a linear response was obtained over the range of 0.8-75 ng mL -1 for uranyl ions. The interfering effect of some foreign ions on extraction and determination of uranyl ions were also investigated. Limit of detection, relative standard deviation and enrichment factor of the proposed SFODME-UV method were obtained as 0.1 ng mL -1 , 3.7% and 125 for uranyl ions, respectively. The proposed method was applied successfully for the extraction and determination of uranyl ions in natural water samples. Good agreement was observed between the results of proposed SFODME method and those reported by official standard method.