纳米 P 沸石修饰碳糊电极上负载的金铜双金属纳米粒子作为一种高效电催化剂和灵敏传感器用于测定肼。

Gold-copper bimetallic nanoparticles supported on nano P zeolite modified carbon paste electrode as an efficient electrocatalyst and sensitive sensor for determination of hydrazine.

机构信息

Analytical division, Faculty of Chemistry, University of Mazandaran, Postal code 47416-95447, Babolsar, Iran.

Analytical division, Faculty of Chemistry, University of Mazandaran, Postal code 47416-95447, Babolsar, Iran.

出版信息

Biosens Bioelectron. 2018 Jun 1;107:111-117. doi: 10.1016/j.bios.2018.02.016. Epub 2018 Feb 5.

Abstract

In this report, a facile, efficient and low cost electrochemical sensor based on bimetallic Au-Cu nanoparticles supported on P nanozeolite modified carbon paste electrode (Au-Cu/NPZ/CPE) was constructed and its efficiency for determination of hydrazine in trace level was studied. For this purpose, agro waste material, stem sweep ash (SSA) was employed as the starting material (silica source) for the synthesis of nano P zeolite (NPZ). After characterization of the synthesized NPZ by analytical instruments (scanning electronic microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscopy), construction of Au-Cu/NPZ/CPE was performed by three steps procedure involving preparation of nano P zeolite modified carbon paste electrode (NPZ/CPE), introducing Cu ions into nano zeolite structure by ion exchange and electrochemical reduction of Cu ions upon applying constant potential. This procedure is followed by partial replacement of Cu by Au due to galvanic replacement reaction (GRR). The electrochemical properties of hydrazine at the surface of Au-Cu/NPZ/CPE was evaluated using cyclic voltammetry (CV), amperometry, and chronoamperometry methods in 0.1 M phosphate buffer solution (PBS). It was found that the prepared sensor has higher electrocatalytic activity at a relatively lower potential compared to other modified electrodes including Au/NPZ/CPE, Cu/NPZ/CPE, Au-Cu/CPE and etc. Moreover, the proposed electrochemical sensor presented the favorable analytical properties for determination of hydrazine such as low detection limit (0.04 µM), rapid response time (3 s), wide linear range (0.01-150 mM), and high sensitivity (99.53 µA mM) that are related to the synergic effect of bimetallic of Au-Cu, porous structure and enough surface area of NPZ. In addition, capability of Au-Cu/NPZ/CPE sensor was successfully tested in real samples with good accuracy and precision.

摘要

在本报告中,构建了一种基于负载在 P 纳米沸石修饰碳糊电极上的双金属 Au-Cu 纳米粒子的简便、高效和低成本电化学传感器,并研究了其用于痕量肼测定的效率。为此,采用农业废料——秸秆灰(SSA)作为合成纳米 P 沸石(NPZ)的起始材料(硅源)。通过分析仪器(扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X 射线衍射(XRD)和傅里叶变换红外(FT-IR)光谱)对合成的 NPZ 进行表征后,通过三步程序构建 Au-Cu/NPZ/CPE,包括制备纳米 P 沸石修饰碳糊电极(NPZ/CPE)、通过离子交换将 Cu 离子引入纳米沸石结构以及施加恒电位时电化学还原 Cu 离子。随后,由于电置换反应(GRR),部分 Cu 被 Au 取代。在 0.1 M 磷酸盐缓冲溶液(PBS)中,通过循环伏安法(CV)、安培法和计时安培法评估肼在 Au-Cu/NPZ/CPE 表面的电化学性质。结果发现,与其他修饰电极(包括 Au/NPZ/CPE、Cu/NPZ/CPE、Au-Cu/CPE 等)相比,制备的传感器在相对较低的电位下具有更高的电催化活性。此外,所提出的电化学传感器在测定肼方面具有有利的分析特性,例如低检测限(0.04 μM)、快速响应时间(3 s)、宽线性范围(0.01-150 mM)和高灵敏度(99.53 μA mM),这与 Au-Cu 的协同效应、多孔结构和 NPZ 的足够表面积有关。此外,Au-Cu/NPZ/CPE 传感器在实际样品中的测试能力具有良好的准确性和精密度。

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