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制备了多壁碳纳米管(MWCNT)修饰碳糊电极,并研究了锆-钙-茜素红(ARS)异多核络合物在该电极上的阳极吸附伏安行为.该方法用于锆的测定具有较高的灵敏度和较好的选择性.在极谱分析仪上采用二阶导数线性扫描伏安法进行分析,在0.128mol·L-1氨基乙酸和0.048mol·L-1邻苯二甲酸氢钾缓冲液(pH4.0)中,在200mV富集60~120s,从200~1200mV以200mV.s-1的速率线性扫描,络合物吸附在修饰电极表面,于840mV(vs.SCE)处产生一灵敏的溶出峰,为络合物中配体茜素红的氧化所产生.络合物的峰电流与锆的浓度在6.0×10-12~6.0×10-11mol·L-1(富集时间120s),6.0×10-11~2.0×10-9mol·L-1(富集时间90s)和2.0×10-9~1.0×10-7mol·L-1(富集时间60s)范围内分三段呈良好的线性关系,检出限(S/N=3)为2.0×10-12mol·L-1(富集时间180s).方法用于岩矿样品中痕量锆的测定,结果满意.
The multiwalled carbon nanotubes (MWCNT) modified carbon paste electrode was prepared and the anodic adsorption voltammetry of zirconium-calcium-alizarin red (ARS) heteronuclear complex on the electrode was investigated. The method was applied to the determination of zirconium Determination with high sensitivity and better selectivity in the polarographic analyzer using second-order derivative linear sweep voltammetry analysis, 0.128mol · L-1 amino acid and 0.048mol · L-1 o-benzene two (PH4.0), and was enriched for 60-120 s at 200 mV and linearly scanned at a rate of 200 mV.s-1 from 200-1200 mV. The complex was adsorbed on the surface of the modified electrode and the membrane was incubated at 840 mV (vs.SCE ) Produced a sensitive dissolution peak, which was produced by the oxidation of the alizarin red complex in the complex.The peak current of the complex and the concentration of zirconium were between 6.0 × 10-12 ~ 6.0 × 10-11 mol·L-1 (Enrichment time 120s), 6.0 × 10-11 ~ 2.0 × 10-9mol·L-1 (enrichment time 90s) and 2.0 × 10-9 ~ 1.0 × 10-7mol·L-1 (enrichment time 60s) The detection limit (S / N = 3) was 2.0 × 10-12 mol·L-1 (enrichment time was 180s). The method was applied to the determination of trace zirconium in rock samples Satisfactory results.