XAS spectroelectrochemistry: Reliable measurement of X-ray absorption spectra from redox manipulated solutions at room temperature

Abstract

The design and operation of a low-volume spectroelectrochemical cell for X-ray absorption spectroscopy (XAS) of solutions at room temperature is described. Fluorescence XAS measurements are obtained from samples contained in the void space of a 50?μL reticulated vitreous carbon (sponge) working electrode. Both rapid electrosynthesis and control of the effects of photoreduction are achieved by control over the flow properties of the solution through the working electrode, where a good balance between the rate of consumption of sample and the minimization of decomposition was obtained by pulsing the flow of the solution by 1-2?μL with duty cycle of ?3?s while maintaining a small net flow rate ..