By the method of radio isotopes (method of depleting) the redistribution of 63Ni was investigated in the surface layer of iron after the Electric-spark alloying by titanium and zirconium in a carbon containing atmosphere and in air. It is proved that the Electric-spark alloying results in diffusive penetration of 63Ni both in the alloyed layer and in material of basis. The depth of isotope’s penetration depends on the nature of an anode material. Alloying by titanium results in penetration of nickel on the depth of 10 μm, that is almost 2 times more than the depth of its penetration if a zirconium anode is used. In particular, a microhardness, microstructure and phase composition of alloyed layers are examined. It is assumed that alloying of iron by zirconium results in the hardness increase. The alloyed layer equals to 10 GPa (at treatment in kerosene) and to 8,6 GPa (at treatment in propane-butane) that exceeds the microhardness values at alloying by titanium.