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本文简要介绍了溶出-收集伏安法的基本原理,设计了双管玻碳电极同位镀汞应用于溶出-收集伏安法的流通电解池,并应用于水样和化探样品中痕量锑和铋的测定。初步探讨了支持电解质浓度、扫描速率、电积时间、电积电位、溶液体积流速、镀汞液浓度等对收集峰电流及被测离子间分辨率的影响,拟定了联合测定10~(-8)～10~(-7)g ml~(-1)锑和铋的方法。试验表明,锑铋峰电流与浓度有良好的线性关系。最低可测至0.5ppb锑和铋。常见离子对测定无干扰。20倍量的Cu和As有干扰,测定矿样中采用巯基棉富集并分出锑和铋,有较好的效果。澄清水样可直接测定,方法的相对标准偏差锑在0.7～3.1%,铋在3.0～4.8%,回收率均为92～103%。对化探标准样品的分析,锑铋的相对误差均约为8%。
In this paper, the basic principle of dissolution-collection voltammetry is briefly introduced. The double-tube glassy carbon electrode is designed to be applied to the electrolytic cell for dissolution-collection voltammetry. It is applied to the trace antimony And bismuth determination. The effects of supporting electrolyte concentration, scanning rate, electrowinning time, electrowinning potential, solution volume flow rate and concentration of mercury plating solution on the peak current and the inter-ion resolution were discussed preliminarily. ) ~ 10 ~ (-7) g ml ~ (-1) antimony and bismuth. Experiments show that the peak current of antimony and bismuth has a good linear relationship with the concentration. The lowest measurable to 0.5ppb antimony and bismuth. Common ion pair determination without interference. 20 times the amount of Cu and As interference, determination of sulfide samples using sulfide enrichment and separation of antimony and bismuth, have a good effect. Clarification of water samples can be directly determined, the relative standard deviation of the method antimony in 0.7 to 3.1%, bismuth in 3.0 to 4.8%, the recovery rates were 92 to 103%. The analysis of geochemical standard samples, the relative error of antimony bismuth are about 8%.