In the present article, various nanometric Fe 50 Ni 50 alloys were synthesized by chemical reduction of the corresponding metal ions, with hydrazine in an aqueous solution. Process variables of reaction temperature, pH of the hydrazine solution and concentration of metal ions were varied in order to determine the optimum synthesis conditions regarding quality, productivity and cost. It is found that pH of hydrazine solution, at low concentration of metal ions, is the most crucial variable affecting the reaction rate, average crystallite and particle sizes of the synthesized nanometric Fe 50 Ni 50 alloy, followed by the total concentration of metal ions. Thus, increase of pH of hydrazine solution acts as an efficient stabilizer in reducing the particle size. On the contrary, at high concentration of metal ions, the structural characteristics of the nanometric Fe 50 Ni 50 alloy are almost insensitive to reaction temperature and pH of hydrazine solution, but the reduction rate is remarkably sensitive to reaction temperature. Based on these results, it is decided that a reaction temperature of 80 • C, pH of the hydrazine solution of 12•5 and concentration of metal ions of 0•6 M represent the optimum synthesis conditions. The role of pH of hydrazine solution in reducing the alloy's average particle size as well as efficient stabilizer confirms tremendous effect of synthesis conditions on the alloy structure and therefore, the importance of this study for industrial production of nanometric Fe 50 Ni 50 alloy.