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由於近代工业和科学的发展,对於寻找新的微量和超微量元素的分析方法提出了迫切的要求。例如:高純度锗中极微量砷的測定,就是一个困难問題。最初由Laitinen和Kolthoff提出的利用轉动鉑微电极的电流滴定法,由於受到电极面积的限制。测定濃度一般不能低於10~(-5)M,不适宜於痕量元素的测定。我們研究了用大鉑片代替微鉑电极来提高电流滴定灵敏度的可能性,取得了初步結果。在合适的情况下,能测定的最低濃度达到10~(-7)M。本文报告利用大鉑片电极电流滴定法测定痕量砷及锑的方法,从初步实驗結果来看,这个方法可应用於高純度二氧化锗中痕量砷的測定。
Due to the development of modern industry and science, there are urgent requirements for the analysis of new trace and ultra-trace elements. For example: the determination of trace amounts of arsenic in high-purity germanium is a difficult problem. The current titration initially proposed by Laitinen and Kolthoff using a rotating platinum microelectrode is limited by the electrode area. Determination of concentration generally can not be less than 10 ~ (-5) M, not suitable for the determination of trace elements. We studied the possibility of using a large platinum plate instead of a micro platinum electrode to increase the sensitivity of the current titration and achieved preliminary results. Where appropriate, the lowest concentration that can be measured is 10 ~ (-7) M. This paper reports a method for the determination of trace amounts of arsenic and antimony using platinum electrode current titration. From the preliminary experimental results, this method can be applied to the determination of trace amounts of arsenic in high-purity germanium dioxide.