A method of element separation has been worked out with the use of substoichiometric exchange reactions in combination with extraction chromatography. The principle of the method consists in the successive displacement of elements with lower extraction constants from their complexes by a substoichiometric amount of an aqueous solution of a competitive metal with a higher extraction constant. As stationary phase a chloroform solution of zinc diethyldithiocarbamate was used in the column, and a porous polytetrafluoroethylene (Ftoroplast PF-4) was employed as an inert supporting material. The method was used for the radioactivation determination of zinc, copper, cadmium, silver, mercury, managanese, cobalt and iron traces in yttrium, molybdenum, zirconium, niobium and beryllium. When samples weighing 0.1–1 g are irradiated for 20 hrs with a neutron flux of 1.2·1013 n·cm−2·sec−1, the determination sensitivity is 10−4−10−8%.