Low-dimensional metal nanoparticles (MNPs) intercalated with three-dimensional multiwalled carbon nanotube (MWCNT) materials may be combined to produce new nanocomposites for enhancing their chemical, structural, and morphological features. These composites have interesting physical and chemical characteristics that can be used in electrochemical sensing systems that work significantly well. This research presents a new method for detecting nitrite using an electrochemical sensor that utilizes a flat-electrode made of GCE fabricated by nanocomposite of MWCNTs intercalated with yttrium oxide (Y2O3) and iron oxide (Fe2O3) as Y/Fe-MWCNT at higher temperature. FT-IR, UV–vis., SEM, powder XRD, EDS, BET, and TEM were significantly used to characterize in detail the nanocomposite after its preparation by the solid-state chemical approach. Using CV, LSV, and EIS techniques, the electrochemical attributes of both the bare and Y/Fe-MWCNT fabricated electrodes (with the help of 5 % Nafion as conducting coating binder) were investigated. In addition, the linear relationship between nitrite concentration and peak current of LSV was seen between 1.0 and 1.6 M, with a lower limit of detection (LOD) of 0.027 M. When compared to modified electrodes with nitrite, the electrocatalytic behavior of the nanocomposite electrode is enhanced significantly. At applied potential window of −0.1 to +1.8 V, the Y/Fe-MWCNT sensor shows good selectivity even when there are a lot of interfering chemicals and metal ions. In addition, different PBS electrolyte solutions with pH values ranging from 6.5 to 8 were used to study the prepared sensor. The standard addition method was employed to detect the unidentified nitrite concentration in various real samples including sea water, industrial wastewater, and well water. It introduced a new route for the development of noble sensor probe with nanocomposite materials by electrochemical approach for the safety of environmental and health care field in a broad scale.
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