A novel ferrocene surfactant, N-ferrocenoyl-hexadecamide-O-sulphato-L-serine sodium salt (FS), has been synthesized. Its sulphate head group and chirality make it distinctively different from the ferrocene surfactants reported so far. Its critical micelle concentration (CMC) has been determined using the surface tension method and FS has been extensively electrochemically characterized in aqueous solution. A change in the electrochemical behaviour of FS around its CMC has led to a new method for the determination of the CMC in electrolyte solutions by using cyclic voltammetry. This method has been tested with a positive ferrocene surfactant, dodecyl(ferrocenyl-methyl)dimethylammonium bromide (C12) which has been described earlier. The results obtained for both ferrocene surfactants were found to be in fair agreement with values obtained by surface tension measurements.