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Nickel ferrite nanoparticles with chemical formula NiFe2O4 were prepared by standard sol-gel auto ignition technique. Citric acid was used as chelating agent and mixed with solution of nickel nitrate and ferric nitrate in 3:1 proportion to balance the oxidizer to reducer ratio. The obtained particles were sintered at 550°C for 4h to remove the water content, impurity and to obtain better crystallinity. The phase purity and structural formation was confirmed through the analysis of X-ray diffraction technique. The results of X-ray diffraction analysis show the single phase cubic spinel nanocrystalline structure. The particles size calculated from FWHM of the strongest peak (311) is 22 nm in the nanometer dimension. The lattice constant, X-ray density and other structural parameters calculated from XRD data are in good agreement with the literature values. The magnetic measurements were taken at room temperature using hysteresis loop technique. Using M-H plot, the different magnetic parameters such as saturation magnetization, coercivity, remanence magnetization and magneton number were deduced.