制备了Bi(Ⅲ)修饰铂电极,用循环伏安法表征了Bi(Ⅲ)在电极上的吸附特性,探讨了电极的响应机理.通过优化实验条件,建立了一种测定Bi(Ⅲ)的示波双电位滴定法.在0.1 moL/L的硝酸溶液中(pH=1.0).用制备的修饰铂电极作为双指示电极,以EDTA标准溶液滴定Bi(Ⅲ),利用示波器屏幕上荧光点的显著最大位移指示滴定终点.Bi(Ⅲ)在1.19×10(-1)～1.44×10(-2)moL/L时,回收率为99.8%～100.1%,检出限(S,N=3)为1.0×10(-4)mol/L.该修饰电极具有良好的稳定性和重现性,在含有1.0×10(-2)moL/L Bi(Ⅲ)的溶液中,连续7次测定,所得终点电位值均在100 mV左右,其相对标准偏差(RSD)为0.04%.应用该方法测定含铋样品,RSD值(n=7)小于0.25%,回收率为99.5%～100.5%,测定结果与指示剂法测定值相符.
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