The magnetic NiFe2O4 nanoparticles have been synthesized and used as adsorbents for removal of an azo dye, Eriochrome black-T (EBT) from aqueous solution. The NiFe2O4 nanoparticles were characterized by scanning electron microscope (SEM), Transmission electron microscope (TEM), X-ray diffraction (XRD) and Fourier transform infrared spectra (FTIR). The adsorption studies were carried out under various parameters, such as pH, adsorbent dosage, contact time and initial dye concentration. The experimental results show that the percentage of adsorption increases with an increase in the adsorbent dosage. The maximum adsorption occurred at the pH value of 6.0. The equilibrium uptake was increased with an increase in the initial dye concentration in solution. Adsorption kinetic data were properly fitted with the pseudo-second-order kinetic model. The experimental isotherms data were analyzed using Langmuir and Freundlich isotherm equations. The best fit was obtained by the Langmuir model with high correlation coefficients (R2 = 0.9733) with a maximum monolayer adsorption capacity of 47.0 m g/g.