The method of ytterbium(III) trace concentration in the presence of 2-thenoyltrifluoroacetone (TTA) and polyethyleneglycol (PEG) in ammonium chloride is described. The adsorption was performed at the HMDE at À 1.0 V using linear scan voltammetry and square-wave voltammetry. The relationship between properties of the SW response of the mixed ligand complex and parameters of a charge transfer were analyzed using theoretical data of SW redox processes.