Stationary electrode voltammetry and chronoamperometry in an alkali metal carbonate-borate melt Public Deposited

http://ir.library.oregonstate.edu/concern/graduate_thesis_or_dissertations/hx11xj024

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  • The electrochemistry of the lithium-potassium-sodium carbonate-borate melt was explored by voltammetry and chrono-amperometry. In support of this, a controlled-potential polarograph and associated hardware was constructed. Several different types of reference electrodes were tried before choosing a porcelain membrane electrode containing a silver wire immersed in a silver sulfate melt. The special porcelain compounded was used also to construct a planar gold disk electrode. The theory of stationary electrode polarography was summarized and denormalized to provide an overall view. A new approach to the theory of the cyclic background current was also advanced. A computer program was written to facilitate data processing. In addition to providing peak potentials, currents, and n-values, the program also resolves overlapping peaks and furnishes plots of both processed and unprocessed data. Rapid-scan voltammetry was employed to explore the electro- chemical behavior of Zn, Co, Fe, Tl, Sb, As, Ni, Sn, Cd, Te, Bi, Cr, Pb, Cu, and U in the carbonate-borate melt. Most substances gave reasonably well-defined peaks with characteristic peak potentials and n-values. Metal deposition was commonly accompanied by adsorption prepeaks indicative of strong adsorption, and there was also evidence of a preceding chemical reaction for several elements, suggesting decomplexation before reduction. Chromium exhibited behavior indicative of a succeeding irreversible chemical reaction. Diffusion coefficients for copper and chromium were determined by chrono-amperometry. For Cu(II) to Cu(O), D = 1.94 ± .37 x 10⁻⁶ cm²/sec, while for Cr(VI) to Cr(III), D = 2.14 ± .42 x 10⁻⁶ cm²/sec.
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