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Instruments / Technical Area	Publication Details	Published
B18-Core EXAFS	A versatile liquid-jet/sessile droplet system for operando studies of reactions in liquid dispersions and solutions by X-ray absorption spectroscopy S.-y. Chang , T. A. Kathyola , E. A. Willneff , C.. J. Willis , P. Wilson , P. J. Dowding , G. Cibin , A. B. Kroner , E. J. Shotton , S. L. M. Schroeder Reaction Chemistry & Engineering 4, 679 - 687 DOI: 10.1039/C8RE00207J Diamond Proposal Number(s): [15850, 14673] Open Access Show Abstract ▼ Abstract: Herein, we designed a versatile cell for operando X-ray absorption spectroscopy (XAS) monitoring of chemical and physical transformations in liquid solutions and dispersions by fluorescence-yield detection. The cell operates under atmospheric pressure, and the composition of the gas phase can be varied, allowing monitoring of gas–liquid reactions. Samples can be examined as a flowing liquid-jet or as a sessile droplet. Both liquid-jet and droplet operations of the cell were demonstrated at the Ca K-edge through time-resolved studies of CaCO3 formation from CO2 and solid Ca(OH)2 in an aqueous suspension. The liquid-jet reaction was performed at 28 °C, and the droplet reaction was performed at ambient temperature, but both configurations had the scope to be modified for operations at higher temperatures. The liquid-jet volumes were recycled, permitting the use of the cell in a continuous sampling loop for process studies in larger reactor vessels. The jet supply tube was interchangeable, permitting adjustment of the jet size through the tubing bore size. Larger bore sizes minimized the pressure drop at the nozzle and thereby the risk of blockage of the liquid supply by the suspended particulates or growth of solid deposits. Sessile droplet operation enabled studies with minimal sample volumes and mechanical disturbances under controlled environmental conditions. The cell is portable and modular and is based on readily available standard vacuum equipment parts. Furthermore, the operation under a He atmosphere allows measurements above 4 keV, covering part of the tender X-ray range, and it is also applicable to the hard X-ray range.	Mar 2019
	Time-resolved, in situ DRIFTS/EDE/MS studies on alumina supported Rh catalysts: effects of ceriation on the Rh catalysts in the process of CO oxidation Anna B. Kroner , Mark A. Newton , Moniek Tromp , Andrea E. Russell , Andrew J. Dent , John Evans Catalysis, Structure & Reactivity 3, 13 - 23 DOI: 10.1080/2055074X.2016.1266762 Open Access Show Abstract ▼ Abstract: The effect of ceria doping by oxide surface modification and controlled metal surface modification (CSM) on the structure-function properties of Rh/γ-Al2O3 catalysts in the process of CO oxidation were studied by a combined array of Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS)/Energy Dispersive X-ray Absorption Fine Structure/Mass Spectrometry techniques applied simultaneously under time-resolved, in situ conditions in the temperature range of 298–573 K. The addition of each promoter element by CSM exhibits multiple effects on the catalysts structure. The DRIFTS/XAS studies indicate that CeOx facilitate the protection of Rh particles against extensive oxidation in atmospheres of air, O2 and CO, without reducing the coverage of oxidisable adsorbed CO.	Feb 2017
B18-Core EXAFS	A flexible gas flow reaction cell for in situ x-ray absorption spectroscopy studies Anna B. Kroner , Khaled M. H. Mohammed , Martin Gilbert , Graham Duller , Leo Cahill , Peter Leicester , Richard Woolliscroft , Elizabeth J. Shotton AIP Conference Proceedings Synchrotron Radiation Instrumentation 2015 DOI: 10.1063/1.4952837 Diamond Proposal Number(s): [7546, 7638] Open Access Show Abstract ▼ Abstract: A capillary-based sample environment with hot air blower and integrated gas system was developed at Diamond to conduct X-ray absorption spectroscopy (XAS) studies of materials under time-resolved, in situ conditions. The use of a hot air blower, operating in the temperature range of 298-1173 K, allows introduction of other techniques e.g. X-ray diffraction (XRD), Raman spectroscopy for combined techniques studies. The flexibility to use either quartz or Kapton capillaries allows users to perform XAS measurement at energies as low as 5600 eV. To demonstrate performance, time-resolved, in situ XAS results of Rh catalysts during the process of activation (Rh K-edge, Ce L3-edge and Cr K-edge) and the study of mixed oxide membrane (La 0.6 Sr 0.4 Co 0.2 Fe 0.8 O 3-G) under various partial oxygen pressure conditions are described.	Jul 2016

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