Electrochemical studies of sodium and its salts were carried out in 0.1 M TBAP and in electrolyte-free tetrahydrofuran solutions at room temperature. Working electrodes employed in these studies were platinum and mercury film ultramicroelectrodes, as well as a sodium electrode. The electrochemical reduction of sodium salts in 0.1 M TBAP/THF solutions leads to deposition of sodium on the platinum surface, and at more negative potentials, a stripping wave attributed to formation of the sodium anion is observed; the oxidation wave for the sodium anion is not observed. Possible mechanisms for the removal of the anion by competing processes are discussed. The results obtained from electrochemical studies of sodium electrodes and of sodium salts at a mercury film electrode are presented.