In the present work, we report the results of electrochemical investigation of the redox behavior of a carbositall electrode (CSE) previously activated by using ultrasonic irradiation and cyclic voltammetry techniques. The utility of an activated CSE (ACSE) as sensor for detection of Gua and Ade was first time investigated by incorporating it in a computer-controlled SI-system coupled with adsorptive stripping voltammetry (AdSVA). In light of the results obtained to date, carbositall is a synthetic pyrocarbon material that consists of nanocarbon phase containing large and small monocrystalline inclusions of boron (4–5%). The production process of this material is based on oriented crystallization under pyrolysis of hydrocarbons in the presence of halides of refractory metals [26]. The remarkable properties of carbositall (e.g. high surface-volume ratio, high electrical conductivity, wide potential window in the positive range, chemical inertness and strong mechanical strength) created interest in its electrochemical applications [27].