Dip-and-pull ambient pressure photoelectron spectroscopy as spectroelecrochemistry tool for probing molecular redox processes

Ambient pressure X-ray photoelectron spectroscopy (APXPS) can provide a compelling platform for studying an analyte's oxidation and reduction reactions in a solution. 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 meniscus on the working electrode 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.