Investigations of the electrochemical behavior of Cu(II), Pb(II), and Cd(II) ,V(v) ions in the presence of the organic reagents. An original method for evaluation of the stability constant of the adsorpted species,has been proposed. Using the adsorptive accumulation on the electrode, a number of original methods for determination of the heavy metal in different systems have been developed. The 4-phenylthiosemicarbazide has been proposed for determination of the cadmium in river waters, the thiosemicarbaziddiacetic acid and 8-quinolinaldehyde thiosemicarbazide – for copper determination in the river waters, apple and tomato juices, 8-quinolinaldehyde semicarbazone - for determination of the lead in wheat flour and petrol. The metrological parameters of the proposed methods have been evaluated using standard additions, AAS spectrometry, and reference materials.