Abstract: The possibility of determination the electrochemical behavior of thionalide and thiourea on a platinum disk microanode is shown. The influence of background electrolytes and buffer mixtures on the conditions, course and results was studied. Based on these data methods for the amperometric determination of Pd(II) and Ag(I) using solutions of thioureas(TU) and thionalide (TNL) on a platinum rotating anode by its oxidation current, with a clear titration curve characterized by a clear endpoint were developed.