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Development of extended X-ray absorption fine structure spectroelectrochemistry and its application to structural studies of transition-metal ions in aqueous solution

Journal Article · · Anal. Chem.; (United States)
DOI:https://doi.org/10.1021/ac00127a016· OSTI ID:6954007

Extended X-ray absorption fine structure (EXAFS) measurements were performed on solutions of various transition-metal complexes. Electrochemical methods were used to generate and maintain the materials in a chosen oxidation state. A spectroelectrochemical cell was constructed with a reticulated vitreous carbon electrode and followed the basic design of an optically transparent thin-layer electrochemical cell. Cell performance was tested on ferrocyanide with chronoamperometry, chronoabsorptometry, and cyclic voltammetry. X-ray absorption spectra of cobalt(III/II) sepulchrate were examined in a potentiostatic study. Fluorescence EXAFS spectra of Ru(NH/sub 3/)/sub 6//sup 3 +/ were evaluated for sensitivity enhancement as a function of concentration. Cytochrome c spectra have been recorded and gave a Fe(III)-N distance of 1.97 A and a Fe(II)-N distance of 1.99 A.

Research Organization:
Univ. of Cincinnati, OH
OSTI ID:
6954007
Journal Information:
Anal. Chem.; (United States), Journal Name: Anal. Chem.; (United States) Vol. 58:14; ISSN ANCHA
Country of Publication:
United States
Language:
English