• Temperton, R.H.; Kawde, A.; Eriksson, A.; Wang, W.; Kokkonen, E.; Jones, R.; Gericke, S.M.; Zhu, S.; Quevedo, W.; Seidel, R.; Schnadt, J.; Shavorskiy, A.; Persson, P.; Uhlig, J.: Dip-and-pull ambient pressure photoelectron spectroscopy as a spectroelectrochemistry tool for probing molecular redox processes. The Journal of Chemical Physics 157 (2022), p. 244701/1-7

10.1063/5.0130222
Open Access Version

Abstract:
Ambient pressure x-ray photoelectron spectroscopy (APXPS) can provide a compelling platform for studying an analyte’s oxidation and reduction reactions in solutions. This paper presents proof-of-principle operando measurements of a model organometallic complex, iron hexacyanide, in an aqueous solution using the dip-and-pull technique. The data demonstrates that the electrochemically active liquid meniscuses on the working electrodes can undergo controlled redox reactions which were observed using APXPS. A detailed discussion of several critical experimental considerations is included as guidance for anyone undertaking comparable experiments.