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Instruments / Technical Area	Publication Details	Published	Actions
I20-EDE-Energy Dispersive EXAFS (EDE)	Tracking minority species in redox reactions: a quantitative combined XAS and modulation excitation study Armando Ibraliu , Xiaolei Fan , Luke Keenan , Tathiana Kokumai , Matteo Aramini , Veronica Celorrio , Adam Greer , Daniel Bowron , Christopher Hardacre , Sofia Diaz Moreno Angewandte Chemie International Edition DOI: 10.1002/anie.202401888 Diamond Proposal Number(s): [28203] Show Abstract ▼ Abstract: Understanding nature of intermediates/active species in reactions is a major challenge in chemistry. This is because spectator species typically dominate the experimentally derived data and consequently active phase contributions are masked. Transient methods offer a means to bypass this difficulty. In particular, modulation excitation with phase-sensitive detection (ME-PSD) provides a mechanism to distinguish between spectator and reacting species. Herein, modulation excitation (ME) time-resolved (energy dispersive) X-ray absorption spectroscopy, assisted by phase sensitive detection (PSD) analysis, has been applied to the study of a liquid phase process; in this case the classic ferrocyanide/ferricyanide redox couple. Periodic switches of the electrical potential (anodic/cathodic) enabled the use of the ME approach. Structural changes at fractions as low as 2% of the total number of electroactive species were detected within the X-ray beam probe volume containing ~30 pmol of Fe(II)/Fe(III).	Aug 2024
B07-C-Versatile Soft X-ray beamline: Ambient Pressure XPS and NEXAFS	Near-ambient pressure XPS and NEXAFS study of a superbasic ionic liquid with CO2 Jordan Cole , Zoe Henderson , Andrew G. Thomas , Claudia L. Compeán-González , Adam Greer , Christopher Hardacre , Federica Venturini , Wilson Quevedo Garzon , Pilar Ferrer , David C. Grinter , Georg Held , Karen L. Syres The Journal Of Physical Chemistry C DOI: 10.1021/acs.jpcc.1c05738 Diamond Proposal Number(s): [20532] Show Abstract ▼ Abstract: In situ photoemission and near-edge X-ray absorption fine structure (NEXAFS) techniques have been used to study the interaction of CO2 with an ionic liquid thin film. A thin film of the superbasic ionic liquid (SBIL) trihexyltetradecylphosphonium benzimidazolide ([P66614][benzim]) was prepared on a rutile TiO2 (110) surface and exposed to CO2 at near-ambient pressures. NEXAFS measurements combined with density functional theory calculations indicate a realignment of [benzim]− anions from 27° from the surface normal to 54° upon exposure to CO2. Angle-resolved X-ray photoelectron spectroscopy (AR-XPS) shows evidence of irreversible CO2 absorption in thin films of [P66614][benzim] and a greater concentration of CO2-reacted anions in the deeper layers. These results give a new perspective on CO2 uptake in ionic liquids and fundamental interactions at the liquid–gas interface. Understanding this interfacial behavior is important for developing ILs for gas capture applications and may influence the performance of other IL-based technologies.	Oct 2021

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