摘要
本文利用溶液法,设计合成了5-溴水杨醛席夫碱及其镍配合物,通过紫外光谱、红外光谱、热分析技术对目标产物的结构进行了表征和确认。将溴代水杨醛席夫碱镍(Ⅱ)配合物作为电活性物质,制备了配合物修饰碳糊电极,详细考察了电活性物质的种类及用量、石墨用量、石蜡用量对电极的循环伏安行为的影响,确定了修饰碳糊电极的最佳制备条件为电活性物质0.050g、石墨0.30g、石蜡0.18g。以循环伏安图中氧化峰电位和峰电流变化值为指标,与空白修饰电极比较,考察了修饰电极对甲醛的电催化氧化性能,并计算得出甲醛在反应过程的阴极传递系数a=0.510;塔菲尔斜率b=0.115;扩散系数D=1.66×10^-6cm^2/s。甲醛浓度在0.001~0.01mol/L范围内,氧化峰峰电流变化值与其浓度呈线性关系,表明可用修饰碳糊电极对甲醛进行定量分析。
5-Bromosalicylaldehyde schiff base and its nickel complex were synthesized, and characterized with UV-Vis spectroscopy, IR spectroscopy and thermogravimetry analysis (TGA). The electrochemical behaviors of the carbon paste electrode modified with the nickel complex were studied. The best condition for the fabrication of modified carbon paste electrode was optimized to be 0. 050 g of nickel complex, 0.30 g of graphite and 0. 18 g of solid paraffin. The electrochemical catalytic oxidation of formaldehyde was observed on the modified electrode. The electron transfer coefficient of such oxidation process was determined to be 0. 51, and the diffusion coefficient of formaldehyde to be 1. 66 × 10 ^-6 cm^2/s. The oxidation peak current was linear to the concentration of formaldehyde in the range from 0. 001 mol/L to 0.01 mol/L, which indicated that the modified carbon paste electrode could be used for the quantitative analysis of formaldehyde.
出处
《分析科学学报》
CAS
CSCD
2008年第4期421-424,共4页
Journal of Analytical Science
基金
广西科学基金项目(桂科基0731015)