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A versatile liquid-jet/sessile droplet system for operando studies of reactions in liquid dispersions and solutions by X-ray absorption spectroscopy

DOI: 10.1039/C8RE00207J DOI Help

Authors: S.-y. Chang (University of Leeds; Diamond Light Source) , T. A. Kathyola (University of Leeds) , E. A. Willneff (University of Leeds) , C.. J. Willis (Infineum UK Ltd) , P. Wilson (Infineum UK Ltd.) , P. J. Dowding (University of Leeds; Infineum UK Ltd) , G. Cibin (Diamond Light Source) , A. B. Kroner (Diamond Light Source) , E. J. Shotton (Diamond Light Source) , S. L. M. Schroeder (University of Leeds; Diamond Light Source)
Co-authored by industrial partner: Yes

Type: Journal Paper
Journal: Reaction Chemistry & Engineering , VOL 4 , PAGES 679 - 687

State: Published (Approved)
Published: March 2019
Diamond Proposal Number(s): 15850 , 14673

Open Access Open Access

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.

Subject Areas: Chemistry


Instruments: B18-Core EXAFS

Documents:
dnnfj45456.pdf