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Electrochemical Platforms and Methods for the Deposition, Stripping, and Detection of Transition and F-block Elements
註釋Preconcentration of f-elements on electrode surfaces from flowing samples can lead to fast and sensitive spectroscopic detection. In this work, a new in-line electrochemical analytical platform was developed to study the electrochemical deposition and stripping of transition and lanthanide metal ions, including new ways to perform those operations under flowing conditions for enhanced preconcentration. Metal ions were injected, deposited, stripped, and analyzed in a single platform, leveraging an electrochemical quartz crystal microbalance for mass detection, and inductively coupled optical emission spectroscopy for elemental detection. This system minimizes sample size and manipulation and handles multiple experiments without disassembly. The platform was demonstrated using a new pulsed electrodeposition with redox replacement technique for precious metal recovery. An expanded version of this platform, which includes two independent flow injection circuits instead of just one, was used to study the electroprecipitation of lanthanum and neodymium and revealed that preconcentration is enhanced by migration when supporting electrolyte is not added. Moreover, transitions in the electric potential at constant current are proposed as indicators of a high pH layer at the electrode surface that enables precipitation. Additionally, a new microfluidic chip with removable electrodes was developed for voltammetric detection, with a new design of removable microelectrodes. A finite element numerical model that predicts the limiting current on the microchannel electrode of this chip was developed, incorporating non-idealities in the channel and electrode geometry that were previously not considered in the literature.