In this paper, nanospinels NiMnxFe2-xO4 (x = 0.05, 0.1, 0.3, 0.5, 0.7, and 1) were prepared by sol-gel method in the presence of nitrate-metal-ethylene glycol (EG) polymerized complex. The nanospinels were characterized using thermogravimetry analysis (TGA), X-ray powder diffraction (XRD), Fourier infrared spectroscopy (FTIR), and transmission electron microscope (TEM). The adsorption of an azo dye, reactive blue 5 (RB5), from water was determined using the prepared nanospinels. The effect of operational parameters such as the initial dye concentration, the concentration of nanospinels, temperature, and pH on the degradation of dye was investigated. The adsorption process follows second-order kinetics and Arrhenius behavior. Two common models, the Langmuir and Freundlich isotherms were used to investigate the interaction of dye and nanospinels. The isotherm evaluations revealed that the Freundlich model provides better fit to the experimental data than that of the Langmuir model. The photocatalytic degradation of RB5 at pH 1 under UV irradiation was examined. The results showed that the degradation of RB5 dye follows merely an adsorption process. (C) 2011 Elsevier B.V. All rights reserved.