Study of the properties of rare-earth elements (REEs) and their alloys and compounds is important from the viewpoints of both practice and theory, because these elements, by virtue of their valuable properties, are widely used in state-of-the-art technologies. Rare-earth elements show considerable promise for metallurgy, machine building, instrument making, the glass industry, and medicine [1]. Rare-earth silicides and germanides are used in the reactor-building industry. The relative thermal stability of REE along with their large activation cross-sections for neutron capture allows them to be used as neutron-absorbing materials for different units. Rare-earth elements enter into the composition of scintillation materials as activators. The characteristics of these materials significantly depend on the concentrations of REEs; therefore, reliable, sensitive, selective, and rapid procedures are required for their quality control. Rare-earth elements are most often determined by atomic emission spectrometry, which allows impurities of individual lanthanides to be determined in the presence of others. Luminescence and spectrophotometry are also often used. These methods are sensitive and selective, but they often require unavailable and specific reagents. Voltammetric methods are competitive with the above methods and, at the same time, possess important advantages, such as the high sensitivity and reproducibility of the results, rapidity, the possibility of the simultaneous determination of several components, and the availability of equipment [2].The reduction of REE(III) ions, especially Eu(III) and Yb(III), has been studied quite well [3]. There is information on the effect of pH and the supporting electrolyte; the kinetics of the Eu(III) Eu(II) and Yb(III) Yb(II) conversions was studied in [4][5][6][7][8][9][10][11][12][13][14][15][16][17][18]. Eu(III) and Yb(III) can be determined at a dropping mercury electrode (d.m.e) in the presence of other REEs [11][12][13][19][20][21][22][23][24][25][26]. The studies of Eu(III) reduction in aqueous-organic and organic media showed that these media were unsuitable for determining europium(III) because of their low conductivities [27][28][29][30].The REE(III) ions are reduced in the potential range from -1.7 to -2.0 V. There is no unified opinion about the nature of their polarographic waves; different assumptions were made in [31-41]. These waves (or peaks) are obtained at the potentials close to the potentials of the supporting electrolyte reduction and, therefore, are poorly selective. REE(III) can be determined by the proposed procedures only after the electrochemical or chemical separation of foreign REE(III) and Al(III), Cd(II), Co(II), Cu(II), Ni(II), Pb(II), Zn(II), and other ions [33,[42][43][44][45][46]. Therefore, voltammetry in conventional supporting electrolytes offers no advantages over other methods and is rarely used.At present, more than 30 organic ligands have been proposed for the voltammetric determination of individual or combined REEs. The selectivit...