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In Situ Spectroelectrochemistry at Free-Standing Liquid-Liquid Interfaces: UV-vis Spectroscopy, Microfocus X-ray Absorption Spectroscopy and Fluorescence Imaging

DOI: 10.1021/jp312060f DOI Help

Authors: Yvonne Grunder , J. Frederick W. Mosselmans (Diamond Light Source) , Sven L. M. Schroeder (The University of Manchester) , Robert A. W. Dryfe (University of Manchester)
Co-authored by industrial partner: No

Type: Journal Paper
Journal: The Journal Of Physical Chemistry C , VOL 117 (11) , PAGES 5765–5773

State: Published (Approved)
Published: February 2013
Diamond Proposal Number(s): 7405

Abstract: A windowless electrochemical cell for the spectroscopic investigation of the liquid–liquid interface, using a dual droplet configuration, has been designed. The setup permits in situ probing of the bulk solutions and the interfacial region by fiber-optic UV–vis spectroscopy, microfocus X-ray fluorescence (XRF) elemental mapping, and microfocus X-ray absorption near-edge structure (?XANES) spectroscopy. The electrodeposition of Au, induced by ion transfer of the tetrachloroaurate complex from a halogenated solvent (containing a weak reducing agent) to the aqueous phase, has been monitored by a combination of the three techniques. The reaction can be followed in situ by UV–vis spectroscopy by detecting the oxidized form of the reducing agent. Voltammetric evidence suggests the formation of interfacial Au(I) species, whereas ?XANES detect the presence of metallic Au(0).

Subject Areas: Chemistry, Physics

Instruments: I18-Microfocus Spectroscopy