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| - XANES Spectroelectrochemistry: A New Methodfor Determining Formal Potentials
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| Abstract
| - Proof-of-concept experiments are presented outlining theuse of X-ray absorption near-edge structure (XANES) inthe determination of formal potentials. Two redox couplesof Np in 1 M perchloric acid are used for the demonstration. XANES data obtained as a function of appliedpotential are used to quantitatively determine the relativeconcentrations of Np(VI)/Np(V) and Np(IV)/Np(III). Bulkelectrolysis is done in the X-ray beam with the solutionmaintained under electrochemical control. Relative concentrations are extracted from the data using a principalcomponent (factor) analysis. The formal potentials of thetwo redox couples determined using this method agreewith those previously published. The results establish insitu XANES spectroelectrochemistry as a viable methodfor determining formal potentials. Examples, taken fromenvironmental or heteropolyanion chemistry, are discussedfor which this methodology will provide information currently unavailable from other established techniques.
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