Mixed ligand complexes of germanium(IV), gallium(III) and titanium(IV) were produced with stilbazo using surfactants, as well as ion-associates of acid complexes of chlorides of tellurium, antimony and iron with azoderivatives of ethoxyacridine. Optimum conditions were established for the formation of complexes and their physico-chemical and analytical characteristics were determined. According to the researches of the complexes a new method was developed to determine metals in different objects.