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    双席夫碱铜配合物修饰玻碳电极用于碳酸饮料中苯甲酸的测定

    Determination of Benzoic Acid in Carbonated Beverage with Modified Glassy Carbon Electrode of Bis-Schiff Base Copper Complex

    • 摘要: 利用溶液法制备双席夫碱铜配合物(M),采用电沉积法将制备的M沉积在玻碳电极(GCE)上制备了双席夫碱铜配合物修饰电极(M/GCE),用于测定碳酸饮料中的苯甲酸的含量。元素分析和红外光谱结果显示,试验成功制备了M;电沉积过程循环伏安曲线变化结果显示M已成功沉积在了GCE表面;扫描电镜(SEM)结果显示M/GCE表面已形成了一层聚合物膜。三电极体系选用M/GCE (工作电极)、饱和甘汞电极(参比电极)、铂丝电极(辅助电极);支持电解质采用0.1 mol·L-1 KCl溶液;电化学方法选用循环伏安法(CV),扫描速率为50 mV·s-1。结果表明,苯甲酸在M/GCE上的氧化峰电位和还原峰电位分别位于-0.007,-0.359 V附近,电极反应可逆性良好,受扩散控制。苯甲酸浓度与其对应的氧化峰电流在0.001 0~2.000 0 mmol·L-1内呈线性关系,检出限(3S/N)为0.27 μmol·L-1。将电极在4℃下放置7 d后,苯甲酸氧化峰电流下降了4.8%。以雪碧样品为基质进行了加标回收试验,回收率为97.6%~102%,测定值的相对标准偏差(n=5)为1.2%。

       

      Abstract: Bis-Schiff base copper complex (M) was prepared by solution synthesis method, then M was deposited on the surface of glassy carbon electrode (GCE) by electrodeposition to prepared modified electrode of M (M/GCE). M/GCE was developed for determination of the content of benzoic acid in carbonated beverage. Elemental analysis and infrared spectroscopy showed that M was successfully prepared in the experiment; the curves of cyclic voltammetry (CV) of the electrodeposition process showed that M had been deposited on the GCE surface; scanning electron microscope (SEM) results showed that a polymer film had been formed on the surface of M/GCE. In the CV analysis for determination of the content of the benzoic acid, the three-electrode system was selected with M/GCE as working electrode, saturated calomel electrode as reference electrode, platinum wire electrode as auxiliary electrode and 0.1 mol·L-1 KCl solution as the supporting electrolyte at the scan rate of 50 mV·s-1. It was shown by results that the oxidation peak potential and reduction peak potential of benzoic acid on M/GCE were ca. -0.007, -0.359 V, respectively. The electrode reaction was reversible and controlled by diffusion. Linear relationship between concentrations and their respective oxidation peak current of benzoic acid found was in the range of 0.001 0-2.000 0 mmol·L-1, with detection limit (3S/N) of 0.27 μmol·L-1. After placing the electrode at 4℃ for 7 d, the oxidation peak current of benzoic acid decreased by 4.8%. A sprite sample was used as a matrix to made a spiked recovery test, giving recoveries of 97.6%-102%; and RSD (n=5) of the measured value found was 1.2%.

       

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