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    拱桥状NiO/碳纸电极的制备及对葡萄糖的电传感性能

    Preparation and Electrical Sensing Performance on Glucose of Arch Bridge-Like NiO/Carbon Paper Electrode

    • 摘要: 采用纳米NiO构建无酶葡萄糖传感器时,纳米NiO易团聚,导致电极的比表面积和电传感性能降低,因此进行了题示研究。采用恒电位法在碳纸(CP)上修饰纳米NiO,分别以所得的NiO/CP电极、铂片电极和甘汞电极作工作电极、辅助电极和参比电极,在0.1 mol·L−1氢氧化钠溶液中采用安培电流-时间(I-t)法定量检测葡萄糖。扫描电子显微镜(SEM)表征结果显示,合成的NiO/CP电极上纳米NiO呈拱桥状,其表面为层状堆砌结构,有利于增加电极的比表面积和表面的活性位点。能量色散光谱(EDS)表征结果显示,电极中含有C、Ni、O元素,结合SEM图说明纳米NiO已成功与CP复合。循环伏安法结果显示,随着葡萄糖浓度的增大,氧化/还原峰电流绝对值不断增大/减小且分别向高/低电位移动,电极对葡萄糖的电催化过程主要受扩散控制。在检测电位0.50 V下,I-t法表征结果显示:电极对葡萄糖的响应时间约为10 s;电流密度绝对值随着葡萄糖浓度的增大呈台阶式上升,电流密度绝对值与葡萄糖浓度在0.000 5~0.71 mmol·L−1,0.71~4.71 mmol·L−1和4.71~12.21 mmol·L−1内呈线性关系,且电极的重现性、重复性和抗干扰能力均较好;方法用于5%(质量分数)葡萄糖注射液的分析,葡萄糖测定值为理论值的96.44%,且经5次重复测定值的相对标准偏差为4.0%。

       

      Abstract: When constructing an enzyme-free glucose sensor using nano NiO, the nano NiO tends to agglomerate, causing the decrease in the specific surface area and electrical sensing performance of the electrode. Therefore, research mentioned by the title was conducted. Nano NiO was modified on carbon paper (CP) using the constant potential method. With the obtained NiO/CP electrode as the working electrode, the platinum plate as the auxiliary electrode, and the calomel electrode as the reference electrode, glucose was quantitatively detected using Ampere current-time (I-t) method in 0.1 mol·L−1 sodium hydroxide solution. As found by results from SEM characterization, the nano NiO on the synthesized NiO/CP electrode had an arch bridge shape and a layered stacking structure on its surface, which was conducive to increasing the specific surface area of the electrode and the active sites on the surface. As found by results from EDS characterization, the electrode contained C, Ni, and O elements, indicating that nano NiO had successfully combined with CP referring to the SEM image. As found by results from the cyclic voltammetry, the current absolute value of the oxidation/reduction peak continuously increased/reduced and moved towards high/low potential with the increase of glucose concentration, respectively, and the electrocatalytic process of the electrode on glucose was mainly controlled by diffusion. As found by results from the I-t method at a detection potential of 0.50 V, the response time of the electrode to glucose was about 10 s. The absolute value of current density increased step by step with the increase of glucose concentration, and linear relationships between the absolute value of current density and glucose concentration were found in the ranges of 0.000 5-0.71 mmol·L−1, 0.71-4.71 mmol·L−1 and 4.71-12.21 mmol·L−1. The electrode had good reproducibility, repeatability, and anti-interference ability. The method was used for the analysis of 5% (mass fraction) glucose injection, and the determined value of glucose was 96.44% of the theoretical value, and RSD was 4.0% after 5 repeated determination.

       

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