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Excess levels of nitrite ion in drinking water interact with amine functionalized compounds to form carcinogenic nitrosamines, which cause stomach cancer. Thus, it is indispensable to develop a simple protocol to detect nitrite. In this paper, a Cu-metal-organic framework (Cu-MOF) with graphene oxide (GO) composite was synthesized by ultrasonication followed by solvothermal method and then fabricated on a glassy carbon (GC) electrode for the sensitive and selective determination of nitrite contamination. The SEM image of the synthesized Cu-MOF showed colloidosome-like structure with an average size of 8 μm. Interestingly, the Cu-MOF-GO composite synthesized by ultrasonic irradiation followed by solvothermal process produce controlled size of 3 μm colloidosome-like structure. This was attributed to the formation of an exfoliated sheet-like structure of GO by ultrasonication in addition to the obvious influence of GO providing the oxygen functional groups as a nucleation node for size-controlled growth. On the other hand, the composite prepared without ultrasonication exhibited 6.6 μm size agglomerated colloidosome-like structures, indicating the crucial role of ultrasonication for the formation of size-controlled composites. XPS results confirmed the presence of Cu(II) in the as-synthesized Cu-MOF-GO based on the binding energies at 935.5 eV for Cu 2p 3/2 and 955.4 eV for Cu 2p 1/2 . The electrochemical impedance studies in [Fe(CN) 6 ] 3-/4- redox couple at the composite fabricated electrode exhibited more facile electron transfer than that with Cu-MOF and GO modified electrodes, which helped to utilize Cu-MOF-GO for trace level determination of nitrite in environmental effluent samples. The Cu-MOF-GO fabricated electrode offered a superior sensitive platform for nitrite determination than the Cu-MOF and GO modified electrodes demonstrating oxidation at less positive potential with enhanced oxidation current. The present sensor detects nitrite in the concentration range of 1 × 10 -8 to 1 × 10 -4 M with the lowest limit of detection (LOD) of 1.47 nM (S/N = 3). Finally, the present Cu-MOF-GO electrode was successfully exploited for nitrite ion determination in lake and dye contaminated water samples.

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Ultrasonic Assisted Synthesis of Size-Controlled Cu-Metal–Organic Framework Decorated Graphene Oxide Composite: Sustainable Electrocatalyst for the Trace-Level Determination of Nitrite in Environmental Water Samples