Innovation in nanoscience depends fully on the ability to synthesize nanomaterials as well as to assemble them efficiently into complex architectures. The discovery of graphene and graphene polymer nanocomposites is playing a key role in modern nanoscience and nanotechnology. Graphene oxide (GO), is a derivative of graphene obtained by the use of strong oxidizing agents to obtain graphene oxide, a nonconductive hydrophilic carbon material. Synthesis of graphene oxide was performed using the Hummers method. Graphene oxide was integrated into the polysulfone (PSF) matrix to form polysulfone/graphene oxide nanocomposite. Polysulfone casting suspension was prepared by dissolving polysulfone in N,N-dimethyl acetamide. The polymer composites consisted of homogeneously blended polysulfone and graphene oxide casting solutions and drop coated onto boron-doped diamond electrodes (BDD). Interfacial electrochemical dynamics were characterised using cyclic voltammetry (CV), square wave voltammetry (SWV), and electrochemical impedance spectroscopy (EIS). Scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FTIR) and Raman spectroscopy were used to study the morphology and structure of the prepared materials. Modifying with polysulfone blocks electron transfer in the redox reaction of K3Fe(CN)6. PSF /GO enhances electron transfer even when compared to bare BDD. The diffusion coefficient and sensitivity for PSF-GO/BDD electrode was calculated to be 2.660 x10-4 cm2 s-1 and 6.7587 x10-6 mV s-1 / A.