Microdetection of Chromium Mixed–Valences using CuNi/Ti Electrode and Linear Sweep Voltammetry

Nirwan Syarif M.Si
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Abstract

An electrode of non-precious metal has the potency to be utilized as a working electrode for voltammetry measurements of Cr3+ and Cr6+.  The analytical performance of the electrode in determining specific metal species qualitatively and quantitatively was studied. The detection data were recorded and analyzed using cyclic voltammetry (CV) and linear sweep voltammetry (LSV), whereas scanning electron microscope (SEM) and X-ray diffraction (XRD) spectroscopy were used to determine the surface morphology and the presence of crystalline in the electrode. Electroanalytical performance was determined by linear sweep voltammetry. The results show that the reduction of Cr6+ to Cr3+ appeared at +0.84 V (vs Ag/AgCl) and the reduction of Cr3+ to Cr2+ at +0.74 V             (vs Ag/Ag).  The optimum conditions for measuring Cr3+ were found at pH 6, deposition time of 30 seconds, and a scan rate of 160 mVs-1. The optimum pH for measuring Cr6+ is 4, deposition time of 60 seconds, and a scan rate of 140 mVs-1. The regression curve for the Cr3+ is linear in concentration 1 – 10 gL-1 with a correlation coefficient of  0.9883 and a detection limit of 2.08 gL-1. While the Cr6+ is linear in the range of 1 – 10 gL-1 with a correlation coefficient of 0.99 and a detection limit of 2.18 gL-1. There is a slight difference in the individual measurement current and the mixture of Cr3+ and Cr6+ but with a good agreement for the oxidation-reduction potential. The measurement data analysis shows the feasibility of the electrode and the measurement system developed.
用CuNi/Ti电极和线性扫描伏安法微量检测混价铬
一种非贵金属电极具有作为工作电极用于Cr3+和Cr6+伏安测量的潜力。研究了该电极对特定金属种类的定性和定量分析性能。利用循环伏安法(CV)和线性扫描伏安法(LSV)记录和分析检测数据,利用扫描电镜(SEM)和x射线衍射(XRD)光谱分析电极的表面形貌和晶体是否存在。电分析性能采用线性扫描伏安法测定。结果表明:Cr6+在+0.84 V(比Ag/AgCl)下还原为Cr3+, Cr3+在+0.74 V(比Ag/Ag)下还原为Cr2+;测定Cr3+的最佳条件为pH为6,沉积时间为30秒,扫描速率为160 mVs-1。测量Cr6+的最佳pH值为4,沉积时间为60秒,扫描速率为140 mVs-1。在浓度1 ~ 10 gL-1范围内,Cr3+的回归曲线呈线性,相关系数为0.9883,检出限为2.08 gL-1。Cr6+在1 ~ 10 gL-1范围内呈线性关系,相关系数为0.99,检出限为2.18 gL-1。单个测量电流与Cr3+和Cr6+的混合物略有不同,但氧化还原电位一致。测量数据分析表明,所研制的电极和测量系统是可行的。
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