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作 者:邓培红[1] 费俊杰[2] 张军[1] 黎拒难[2]
机构地区:[1]衡阳师范学院化学与材料科学系,湖南衡阳421008 [2]湘潭大学化学学院,湖南湘潭411105
出 处:《冶金分析》2009年第2期14-18,共5页Metallurgical Analysis
基 金:衡阳师范学院科学基金青年项目(07A19);教育部科学技术研究基金项目(206104);湘潭大学跨学科交叉研究基金项目(05IND08)
摘 要:制备了多壁碳纳米管修饰碳糊电极并研究了钪-钙-茜素红异多核络合物在该电极上的吸附伏安行为,提出了采用二阶导数线性扫描伏安法测定痕量钪的新方法。在0.08mol/L氨基乙酸-0.04mol/L邻苯二甲酸氢钾缓冲溶液(pH3.6)中,在0mV富集90S后,从0~1000mV以200mV/s的速率线性扫描,络合物吸附在修饰电极表面,于-544mV(vs.SCE)处产生一灵敏的溶出峰,为络合物中配体茜素红的还原所产生。二阶导数峰高与钪的浓度在6.0×10^-12~4.0×10^-7mol/L范围内分3段呈良好的线性关系,检出限(S/N=3)为4.0×10^-12mol/L(富集时间180s)。方法用于岩矿样品中痕量钪的测定,测定结果同ICP-AES法的测定结果相一致。A novel method was described for the determination of ultra trace amounts of scandium by second derivation linear sweep voltammetry. A multi-walled carbon nanotubes modified carbon paste electrode is prepared and the adsorptive voltammetric behavior of scandium-calcium-alizarin red S (ABS)hetero-polynuclear complex has been studied in detail at the modified electrode. It was found that in a buffer solution of 0. 08 mol/L glycine - 0.04 mol/L potassium biphthalate at pH 3.6, the complex could be adsorbed on the surface of the electrode after accumulating at 0 mV for 90 s, yielding one sensitive stripping peak which results from the reduction of ABS in the complex at about -544 mV (vs. SCE) when scanning linearly from 0 mV to -1 000 mV at a scan rate of 200 mV/s. The second derivative peak height is proportional to the concentration of Sc(Ⅲ) in the range of 6.0×10^-12 --4.0 ×10^-7 mol/L and the detection limit(S/N=3) was 4.0×10^-12 mol/L(accumulation time for 180 s). The procedure was applied to the determination of trace amounts of scandium in ore samples, and the results were consistent with those obtained by ICP-AES.
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