An Investigation into the Pre-Concentration of Trivalent f-elements in Aqueous Solution via Electroanalytical Techniques
Schumacher, Paul Diedrich
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Historically, separation of trivalent f-elements has been a challenging facet of lanthanide and actinide chemistry for many years due to the similarities in their chemical behavior. Classical radiochemical separation techniques, while accurate, are laborious, time consuming and can require large amounts of analyte. With the increasing emphasis on rapid, trace level analysis of f-elements, faster and more sensitive methods of separation and pre-concentration, a typical requirement when working at the trace level are required.Results herein show the development, characterization and optimization of a simple, rapid and robust pre-concentration technique for trivalent f-elements utilizing a thin mercury film on macro and micro electrodes via electroanalytical techniques in aqueous solutions. The technique is quantitative for removal of f-elements from the electrode. Currently, the technique can reproducibly pre-concentrate 5 pg/L of f-elements in five minutes for subsequent analysis on ICP-MS with the flexibility to pre-concentrate for other separation and detection methods in a variety of solutes. Optimization parameters include pH of the solution, rotation rate of the electrode, concentration of mercury, potential application waveforms, and order of deposition. Additionally, the development and characterization of a novel, modified carbon paste electrode incorporating á-hydroxyisobutyric acid for pre-concentration of f-elements in aqueous solution is also presented. This electrode can reproducibly pre-concentrate 5 pg/L of f-elements and has the added benefit of being mercury-free.