Combining binary metal nanoparticles (MNPs) with two-dimensional materials can create innovative nanocomposites with unique physical and chemical properties, which are particularly useful for developing efficient electro-chemical sensing systems. This study presents a unique approach for detecting and validating the hazardous substance 4-Methoxyphenol (4-MP) electrochemical approach with conjugated nanocomposite (NC). This approach utilizes an electrochemical sensor constructed on a glassy carbon electrode (GCE), modified with hybrid composite material including graphene oxide (GO) conjugated binary yttrium oxide (Y2O3) and cobalt oxide (Co3O4) as GO@Co3O4/Y2O3 NCs. After preparing the NCs using the solid-state chemical method, various techniques were used to characterize the materials by using various techniques including Scanning Electron Microscopy (SEM), Energy-Dispersive X-ray Spectroscopy (EDS), Fourier-Transform Infrared Spectroscopy (FTIR), X-ray Diffraction (XRD), Ultraviolet–Visible Spectroscopy (UV/Vis), Brunauer–Emmett–Teller Surface Area Analysis (BET), and Transmission Electron Microscopy (TEM). Cyclic voltammetry (CV), linear sweep voltammetry (LSV), and impedance spectroscopy (EIS) were used to examine the electrochemical characterization and sensing application of the fabricated electrodes. Under standard laboratory circumstances, we used LSV to measure the 4-MP detection limit, which linear dynamic range (LDR) from 0.67 to 2.08 M. Based on the calibration curve’s slope, the sensor’s sensitivity was found to be 2.9 µAµM−1cm−2. It was calculated the limit of quantification (LOQ) of 0.19 M and a lower limit of detection (LOD) of 0.057 M. Compared to other modified electrodes for 4-MP detection, the composite electrode demonstrated superior electrocatalytic performance. The GO@Co3O4/Y2O3 NCs sensor demonstrates excellent selectivity, even among several interfering substances and metal ions. For optimization, different phosphate buffered saline (PBS) solutions with pH values ranging from 5.7 to 8.0 were used to evaluate the sensor activity. The sensor’s effectiveness in detecting unknown 4-MP concentrations was tested in various real-samples, including seawater, industrial wastewater, tap water, and well water, using a standard addition method. This study introduces a new approach for developing an electrochemical sensor aimed at monitoring environmental chemicals. The sensor incorporates cobalt nanoparticles on carbon materials to introduce the inorganic-carbon composite materials for the safety in environmental and healthcare applications on a large scale.
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