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We report the synthesis of NiFe2O4 nanoparticles by the complexation EDTA‐citrate method under acidic (pH = 3) and basic (pH = 9) conditions. The structural, optical, vibrational, magnetic, and electrochemical properties were studied. The samples have crystallite sizes of 21 nm (pH 3) and 73 nm (pH 9), with rounded particles and layered structures. The 57Fe Mössbauer spectra at 12 K showed that both...