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

被引:18
作者
Gruender, Yvonne [1 ]
Mosselmans, J. Frederick W. [2 ]
Schroeder, Sven L. M. [1 ,3 ]
Dryfe, Robert A. W. [1 ]
机构
[1] Univ Manchester, Sch Chem, Manchester M13 9PL, Lancs, England
[2] Diamond Light Source, Didcot OX11 0DE, Oxon, England
[3] Univ Manchester, Sch Chem Engn & Analyt Sci, Manchester M13 9PL, Lancs, England
基金
英国工程与自然科学研究理事会;
关键词
GOLD NANOPARTICLES; PD NANOPARTICLES; ION TRANSFER; ELECTRODEPOSITION; NUCLEATION; CLUSTERS; FILMS;
D O I
10.1021/jp312060f
中图分类号
O64 [物理化学(理论化学)、化学物理学];
学科分类号
070304 ; 081704 ;
摘要
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 (mu 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 mu XANES detect the presence of metallic Au(0).
引用
收藏
页码:5765 / 5773
页数:9
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