Iron ore tailing—a waste material of mineral beneficiation plants, is used as a source of iron for synthesizing magnetite powder. Iron ore tailings containing 15.98% Fe 2 O 3 , 83.36% SiO 2 and 0.44% Al 2 O 3 have been subjected to HCl digestion on a hot plate to extract the entire amount of Fe 2 O 3 as FeCl 3 . A portion of extracted FeCl 3 solution has been used to convert it to FeCl 2 via metallic iron formation by using NaBH 4 as a reducing reagent. Then, the left out FeCl 3 solution and derived FeCl 2 solutions (from FeCl 3 ) are mixed in an appropriate molar ratio (2:1) for synthesizing magnetite powder by the addition of alkali solution. The magnetite powder samples have been characterized by means of powder XRD, SEM, vibrating sample magnetometer and laser particle size analyzer. XRD study confirms the formation of magnetite phase. The magnetite particles synthesized in different ways show varying degrees of magnetization behavior which is attributed to the change in their particle size induced by the use of different precipitating reagents.