The objective of the present paper is to get a better understanding of the electrochemical properties of organoclays, which were prepared via solid-state intercalation of three cationic surfactants, such as dodecyltrimethylammonium, tetradecyltrimethylammonium, and hexadecyltrimethylammonium, as bromide salts, at different loading levels into the interlayers of two natural smectite clays (AH and DI). The electrochemical properties of the prepared organoclays were investigated by cyclic voltammetry. The cyclic voltammetry response of the electrochemical probe, 〖Fe(CN)〗_6^(3-)/〖Fe(CN)〗_6^(4-), shows that the intensities of the anodic and cathodic peaks don’t increase when the working electrode is based on carbon paste modified with the raw clays (AH or DI), whereas the peaks intensities increase significantly when the working electrode consists of carbon paste modified with organoclays. This increase in the intensity of the current indicates an improvement in the surface conductivity of the carbon paste electrode when they are modified with organoclays. When the working Electrode is based on organoclays modified carbon paste, the potential differences (ΔEp) are ranged between 140 and 170 mV, which are lower than those of the unmodified carbon paste electrode (330 mV) and those modified with raw clays (520 mV). This indicates an easy electron transfer process on the surface of the organoclays modified carbon paste electrodes.