A new modified glassy carbon electrode (GCE) with grafted polymer (GP)/SiO 2 nanoparticles (SiO 2 NPs) were prepared using mechanical attachment method to produce a new sensor in cyclic voltammetric technique. The new working electrode GP/SiO 2 NPs/GCE was characterized by a standard solution of 1 mM K 4 [Fe(CN) 6 ] with 1 M K 2 HPO 4 as an electrolyte to study the redox current peaks of FeII/FeIII ions at different concentrations such as scan rate, pH, determination of diffusion coefficient (D f), reliability and stability of the modified GCE. It was found that the new modified electrode enhanced the redox current peaks of FeII/FeIII from 12 µA to 20 µA and-5 µA to-15 µA for oxidation and reduction peaks in GCE, repectevely. So, the current ratio (Ipa/Ipc) for the new modified electrode was 1, and the potential peak separation (ΔEpa-c) was 100 mV, which indicated good electrochemical properties as an irreversible electrode and heterogeneous reaction. Good reliability and stability of modified GCE was obseved with low detection limit. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) analysis of the nano-deposit was also studied.