Simple and Intelligent Electrochemical Detection of Ammonia over Cuprous Oxide Thin Film Electrode

Surfaces Pub Date : 2023-11-06 DOI:10.3390/surfaces6040029
Samia A. Kosa, Amna N. Khan, Basma Al-Johani, L. A. Taib, M. Aslam, Wafa A. Bawazir, A. Hameed, M. Tahir Soomro
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Abstract

To realize simple and intelligent electrochemical ammonia (NH3) detection in water, highly dense colloidal copper nanoparticles (CuNPs) were prepared and subsequently deposited onto a glassy carbon electrode (GCE). The CuNPs/GCE was then placed in an oven at 60 °C to intelligently transform CuNPs into cuprous oxide (Cu2O) thin film. The colloidal CuNPs were characterized by ultraviolet-visible (UV-Vis) spectroscopy, whereas the fabricated Cu2O/GCE was subjected to Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and electrochemical impedance spectroscopy (EIS). The XRD of Cu2O/GCE showed the crystalline nature of the thermally converted Cu2O thin film, whereas XPS demonstrated that the thin film formed on the surface of GCE was primarily composed of Cu2O. The SEM images of Cu2O/GCE revealed Cu2O crystals with hexapod morphology. The EIS study exhibited substantially higher charger transfer activity of Cu2O/GCE compared to bare GCE. The drop coating of ammonia (NH3) solution onto Cu2O/GCE enabled the fabricated electrode to be utilized as an electrochemical sensor for NH3 detection in water. The cyclic voltammetric (CV) behavior of NH3/Cu2O/GCE was investigated in 0.1 M pH 7 phosphate buffer, which led to the formation of a copper-ammonia complex and revealed the nobility of the fabricated electrode. The square wave voltammetric (SWV) response was linear over the 10 µM and 1000 µM ranges with a detection limit of 6.23 µM and good reproducibility. The NH3/Cu2O/GCE displayed high selectivity for the detection of NH3 in the presence of various coexisting cations and anions in 0.1 M pH 7 phosphate buffer. The recovery of NH3 in the drinking water sample varied from 98.2% to 99.1%.
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氧化亚铜薄膜电极上氨的简易智能电化学检测
为了实现水中氨(NH3)的简单智能电化学检测,制备了高密度胶体铜纳米粒子(CuNPs),并将其沉积在玻碳电极(GCE)上。然后将CuNPs/GCE置于60℃的烤箱中,将CuNPs智能地转化为氧化亚铜(Cu2O)薄膜。采用紫外-可见(UV-Vis)光谱对胶体Cu2O/GCE进行了表征,采用傅里叶变换红外光谱(FTIR)、x射线衍射(XRD)、x射线光电子能谱(XPS)、扫描电镜(SEM)和电化学阻抗谱(EIS)对制备的Cu2O/GCE进行了表征。Cu2O/GCE的XRD表征了热转化Cu2O薄膜的结晶性质,而XPS表征了GCE表面形成的薄膜主要由Cu2O组成。Cu2O/GCE的SEM图像显示Cu2O晶体具有六足体形态。EIS研究显示,与纯GCE相比,Cu2O/GCE的充电器转移活性明显更高。氨(NH3)溶液滴涂在Cu2O/GCE上,使制备的电极可作为水中NH3检测的电化学传感器。研究了NH3/Cu2O/GCE在0.1 M pH 7磷酸盐缓冲液中的循环伏安(CV)行为,发现铜-氨络合物的形成,揭示了所制备电极的高级性。方波伏安(SWV)响应在10µM和1000µM范围内呈线性,检出限为6.23µM,重现性好。在0.1 M pH 7的磷酸盐缓冲液中,NH3/Cu2O/GCE对不同阳离子和阴离子共存的NH3具有较高的选择性。饮用水样品中NH3的回收率为98.2% ~ 99.1%。
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