Two new nonionic surfactants; 1-sec-butyl-3-dodecanoylthiourea (DTU) and 1-dodecanoyl-3-phenylthiourea (DPTU) were synthesized and characterized by H-1 NMR, C-13 NMR and FTIR and UV-Vis spectroscopy. The detailed electrochemical fate of DTU and DPTU was investigated in a wide pH range of 2-12 by employing three electroanalytical techniques. The voltammetric signatures of the analytes showed a single irreversible anodic peak followed by two reversible peaks of the oxidation product. The irreversible behavior of the oxidation process was witnessed by the unequal components of total current in square wave voltammetry and scan rate based deviation of peak potential. The involvement of protons accompanying the electron transfer processes was ascertained from peak potential versus pH plots. Critical micelle concentration and hydrophilic-lipophilic balance of the synthesized surfactants were determined for the assessment of their cleaning, wetting and emulsifying properties.