Abstract
The electrochemical properties of Nb3O2(SO4)6 · 3H2O5− cluster anion in 9 M sulfuric acid were investigated using DC polarography, cyclic voltammetry, spectroelectrochemistry, and constant potential electrolysis. It was found that Nb3O2(SO4)6 · 3H2O5− in 9 M H2SO4 displays a reduction wave at E = −1.30 V vs. Hg/Hg2 SO4 electrode, and a large irreversible oxidation wave at Epa = −0.30 V. Cyclic voltammetry indicates that the reduction wave involves a reversible one-electron process. Controlled potential electrolysis at E = −1.4 V produces a green Nb(3.33) anion, Nb3O2(SO4)6 · 3H2O6− which is stable on the time scale of bulk electrolysis. Electrochemical reoxidation of Nb(3.33) anion Nb3O2(SO4)6 · 3H2O6− at E = −0.75 V consumes 1 mol e/ mol Nb3 cluster and regenerates the red Nb(3.66) Nb3O2(SO4)6 · 3H2O5− anion. Further oxidation at −0.2 V involves an irreversible four electron process to form Nb(V) species.
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© 1990 Springer Science+Business Media New York
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Sayers, W., Batten, T., May, M., Katovic, V. (1990). Electrochemical Studies of Triangular Niobium Cluster, Nb3O2(SO4)6 · 3H2O5−, in Sulfuric Acid. In: Fackler, J.P. (eds) Metal-Metal Bonds and Clusters in Chemistry and Catalysis. Industry-University Cooperative Chemistry Program Symposia. Springer, Boston, MA. https://doi.org/10.1007/978-1-4899-2492-6_31
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DOI: https://doi.org/10.1007/978-1-4899-2492-6_31
Publisher Name: Springer, Boston, MA
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