A method for determination of the composition of binary mixtures of a metal or radionuclide species by optimized repeated two-phase separations (SORTS) was proposed and theoretically substantiated. Its principle consists in repeated equilibration of two immiscible phases, one being the original liquid or solid matrix with minimal adjustment of its composition and varying the phase ratio (separation stage cut) as the optimized parameter. The batch separation technique may consist in the repeated solvent extraction or aqueous biphasic distribution, or in the replicate equilibration with solvent or leaching solution. Results of SORTS can be presented e.g. by Tukey box diagrams as the characteristic fingerprints of original species composition.