摘要
研究了锆(Ⅳ)-邻苯二酚紫(PV)络合物在碳糊电极上的吸附伏安行为。测定锆最佳条件为:0.08mol/L的HNO3为底液,于0.4V富集50s,从0.4至1.4V以100mV/s的速率线性扫描。在0.85V(vs.SCE)的二次导数氧化峰电流与锆的浓度在3.0×10-9~5.0×10-8mol/L(5.6×10-7mol/LPV)和1.0×10-8~1.0×10-7mol/L(5.6×10-6mol/LPV)成线性关系。富集80s,检出限为1.0×10-9mol/L(S/N=3)。该法用于标准岩石样品中锆的测定,不需萃取分离和掩蔽,直接测定,结果满意。铪(Ⅳ)在同样的实验条件下也于0.85V产生一络合吸附峰,灵敏度稍低于锆。
Anewmethod based on the anodic adsorptive voltammetry of the zirconium(Ⅳ)-pyrocatechol vioˉlet(PV)complex on a carbon paste electrode(CPE)for the determination of zirconium was developed.The zirconium(Ⅳ)-PV complex could be adsorbed on the surface of the CPE and produced a peak at0.85V(vs.SCE)when scanning linearly from0.4to1.4V.Optimal analytical conditions were found to be:0.08mol/L HNO 3 at0.4V for a50s accumulation and at100mV/s scan rate.The linear ranges were3.0×10 -9 -5.0×10 -8 mol/L(5.6×10 -7 mol/L PV)and1.0×10 -8 -1.0×10 -7 mol/L(5.6×10 -6 mol/L PV),respectively.The detection limit was1.0×10 -9 mol/L(S/N=3)for a80s accumulation.The proˉposed method was applied successfully to the direct determination of zirconium in standard rock samples withˉout extracting and masking concomitant ions.
出处
《分析测试学报》
CAS
CSCD
北大核心
2005年第3期34-36,40,共4页
Journal of Instrumental Analysis
基金
中国科学院长春应化所电分析化学国家重点实验室基金资助课题(SKLEAC2003-5)
湖南省教育厅基金资助课题(01C113)
关键词
锆
邻苯二酚紫
碳糊电极
阳极吸附伏安法
Zirconium
Pyrocatechol violet
Carbon paste electrode
Anodic adsorptive voltammetry