Microliter volumes are used in electrochemical detection and preconcentration of radionuclides to reduce the dose received by researchers and equipment. Unfortunately, there is a lack of analysis of radionuclides with coupled electrochemical techniques and microliter volume reactors. The goals of this work are (1) to develop a miniaturized micro-electrochemical quartz crystal microbalance (μeQCM) reactor for use in small volume (50–200 μL) electrogravimetric experiments and (2) to use this reactor to characterize the preconcentration of neptunium on carbon electrodes via electroprecipitation. We successfully deposited neptunium in the new μeQCM reactor and verified its operation. We found that preconcentration of neptunium on carbon coated electrodes was possible by chronoamperometry at − 1.6 V Ag/AgCl . The mass shift of the resulting precipitate was indicative of the amount of neptunium on the electrode, although the correlation between the mass increase and activity of the preconcentrated material was not linear. Neptunium precipitate reduced electron transfer to the solution as evidenced by the increase in charge transfer resistance compared to bare electrodes.

中文翻译：

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使用微型电化学石英晶体微天平电化学沉淀镎


微升体积用于放射性核素的电化学检测和预浓缩，以减少研究人员和设备接收的剂量。不幸的是，缺乏利用耦合电化学技术和微升体积反应器对放射性核素进行分析。这项工作的目标是 (1) 开发用于小体积 (50–200 μL) 电重实验的小型化微电化学石英晶体微天平 (μeQCM) 反应器，以及 (2) 使用该反应器来表征镎的预富集通过电沉淀在碳电极上。我们成功地将镎沉积在新型 μeQCM 反应器中并验证了其运行。我们发现，在 − 1.6 V Ag/AgCl 下，可以通过计时电流法将镎预富集在碳涂层电极上。尽管预浓缩材料的质量增加和活性之间的相关性不是线性的，但所得沉淀物的质量转移表明了电极上镎的量。与裸电极相比，电荷转移电阻增加证明了镎沉淀物减少了向溶液的电子转移。