The Ni1–xAx Fe2O4 (A=Co, Mg; x=0, 0.5) spinal ferrite were compact in chemical “sol-gel” process. The structure and magnetic properties of the samples were done by XRD and VSM. The heat treatment for the samples was performed at 700°C for 2 hours. The crystalline size of NiFe2O4, Ni0.5Co0.5 Fe2O4 and Ni0.5Mg0.5 Fe2O4 were 34.7 nm, 26.8 nm and 29.8 nm, respectively and magnetic measurements showed that the saturation magnetization of these materials were 48.1 emu/g, 34.4 emu/g and 20.36 emu/g, respectively. The values of coercivity (Hc ) of the NiFe2O4, Ni0.5Mg0.5 Fe2O4 and Ni0.5Mg0.5 Fe2O4 are 182 Oe, 460 Oe and 85Oe.