A study on the recovery of nickel from Fe-Ni alloy scrap was conducted using molten magnesium by dissolving only Ni component and then removing Mg using vacuum distillation method. The recovering faction of nickel higher than 99% was achieved at temperatures above 1,073 K and 99.5% of purity level of nickel was successfully obtained under vacuum degree of 10(-5) torr at temperatures above 1,273 K. The purity, phase, and recovery rate of nickel were examined by scanning electron microscopy, elemental analyser, and X-ray diffraction.