This study is concerned with the comparative examination of the reduction of 4-nitroso-N,N-dimethylaniline upon graphite, Cu, Cu(Hg), TiO2/ Ti Sn and Pb electrodes using cyclic voltammetry (CV). There was only one irreversible reduction peak observed for each electrode except for graphite, which gave two peaks in the cathodic and one peak in the anodic region. The rate constant of the chemical reaction was found to be 0.930 s(-1). There was no reduction peak observed with Pb electrode. This was also the case for Sn electrode at scan rates higher than 10 mVs(-1). The titanium dioxide coated titanium electrode is found to behave as an effective heterogeneous redox electron carrier and 4-NDMA can he reduced catalytically on the surface of the electrode. The best electrode for the reduction of 4-NDMA was Sn followed by TiO2/ Ti and Cu(Hg).