In this work, stem of common reed ash (SCRA) is introduced as a new source of silica in the preparation of
mesoporous materials. Mesoporous silicate MCM-41 nanoparticles were synthesized hydrothermally using sodium silicate
prepared from SCRA as a silica source. The characterization of MCM-41was carried out by X-ray diffraction (XRD),
Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), N2 adsorption/desorption (BET) and
transmission electron microscopy (TEM). SEM shows that MCM-41 nanoparticles are sphere-like with size in the range of
30–50 nm with some degree of agglomeration. TEM image of the synthesized sample shows the open framework structure of
MCM-41. A type IV isotherm can be observed from adsorption/desorption curves, which is the characteristic of mesoporous
materials. The prepared MCM-41 nanoparticles were used as substrate to facilitate the oxidation of methanol through the
modification with an electroactive species. The modification was achieved by impregnation of MCM-41 pores with Ni2+
ions (Ni-doped MCM-41). A modified carbon paste electrode (CPE) was prepared by mixing Ni-doped MCM-41 with
carbon paste (NiMCM-41CPE). Cyclic voltammetry of NiMCM-41CPE shows an increment in current density of methanol
oxidation in comparison with CPE in alkaline solution. Moreover, a decrease in the overpotential of methanol oxidation
occurred on the surface of modified electrode. The effects of some parameters such as scan rate and methanol concentration
are also investigated on the behaviour of NiMCM-41CPE. Also, the heterogeneous electron transfer rate for the catalytic
reaction (k) of methanol is calculated.