The interphase distribution of the 0,01 mol/l zirconium(IV) in water — HCl –naphthalene-2-sulfonic acid (NSA) — 0.1 mol/l solution of diantipyrylhepthane in dichloroethane and water — HCl — NSA — diantipyrylmethane (DAM) (or diantipyrylheptane (DAH) systems has been studied studied. Compared to the conventional system on the bases of organic solvent stratifying extraction systems provide a higher degree of extraction. Besides there are no toxic components and volatiles in their composition. Depending on the concentration of HCl DAH in contrast to DAM is capable of educe zirconium (IV) complexes through various extraction mechanisms. It has been shown there is a possibility to use water — DAM — NSA — 0,5 mol/l HCl system for quantitative extraction of zirconium (IV) from solutions with subsequent photometric detection with bromopyrogallol red. The spectrophotometric properties of the resulting pH 1,8 mixed-ligand complex have been studied (ε585 2,7 · 10–3). Beer’s law is feasible in zirconium concentration range from 1 to 28 μg/ml.