A mail-in and user facility for X-ray absorption near-edge structure: the CEI-XANES laboratory X-ray spectrometer at the University of Washington

Abstract

There are more than 100 beamlines or endstations worldwide that frequently support X-ray absorption fine-structure (XAFS) measurements, thus providing critical enabling capability for research across numerous scientific disciplines. However, the absence of a supporting tier of more readily accessible, lowerperforming options has caused systemic inefficiencies, resulting in high oversubscription and the omission of many scientifically and socially valuable XAFS applications that are incompatible with the synchrotron facility access model. To this end, this work describes the design, performance and uses of the Clean Energy Institute X-ray absorption near-edge structure (CEI-XANES) laboratory spectrometer and its use as both a user-present and mail-in facility. Such new additions to the XAFS infrastructure landscape raise important questions about the most productive interactions between synchrotron radiation and laboratory-based capabilities; this can be discussed in the framework of five categories, only one of which is competitive. The categories include independent operation on independent problems, use dictated by convenience, presynchrotron preparatory use of laboratory capability, post-synchrotron followup use of laboratory capability, and parallel use of both synchrotron radiation and laboratory systems. Ditter et al. The CEI-XANES laboratory X-ray spectrometer 2087 Figure 1Diagram showing the movement of the detector and the SBCA in a fixedsource Rowland circle in the direction of low (red) to high (blue) energy. Note that both the source position and the direction from the source to the optic are fixed due to the stationary source.

Effect of chlorine and chromium on sulfur solubility in low‐activity waste glass

“…Measurements were performed on the Cr Kα emission lines with an easyXES150 spectrometer (easyXAFS, LLC), which expands upon recent improvements in laboratorybased Rowland circle designs. [32][33][34] Here, the configuration included a Ge(4,2,2) spherically bent crystal analyzer with a radius of .5 m (XRSTech, LLC), a Vortex-ME7 SDD detector (Hitachi High-Tech), and a 100 W X-ray tube source with a tungsten anode (Varex Imaging Corporation). Each sample was sealed on either side by a piece of polyimide tape (DuPont).…”

Operando Laboratory‐Based Multi‐Edge X‐Ray Absorption Near‐Edge Spectroscopy of Solid Catalysts

“…Therefore, only the most promising catalysts are chosen to be investigated in depth, excluding broad catalyst screening which is important for drawing more profound conclusions. Additionally, the need to transport air‐sensitive, toxic, or radioactive samples to the synchrotron facility can severely limit flexibility in studying such functional materials [7, 11–15] . These drawbacks can be overcome by performing XAS experiments in the laboratory, if the lower signal‐to‐noise (S/N) ratio, energy resolution, and longer measurement times of a laboratory‐based setup compared to a synchrotron facility are acceptable for the planned experiment(s).…”

“…Additionally, the need to transport air-sensitive, toxic, or radioactive samples to the synchrotron facility can severely limit flexibility in studying such functional materials. [7,[11][12][13][14][15] These drawbacks can be overcome by performing XAS experiments in the laboratory, if the lower signal-to-noise (S/N) ratio, energy resolution, and longer measurement times of a laboratorybased setup compared to a synchrotron facility are acceptable for the planned experiment(s). Under these restrictions, however, laboratory-based XAS offers new opportunities in advanced catalyst characterization and presents an alternative as well as a complement to precious beamtime at synchrotron facilities.…”

HERMES – a GUI-based software tool for pre-processing of X-ray absorption spectroscopy data from laboratory Rowland circle spectrometers

“…The renaissance of laboratory X-ray absorption spectroscopy (XAS) instrumentation is revolutionizing access to, and uptake of, this technique across the physical sciences and engineering, enabling application of this technique without the need for access to a synchrotron light source (Błachucki et al, 2019;Honkanen et al, 2019;Jahrman et al, 2019a;Schlesiger et al, 2015;Malzer et al, 2018;Mortensen et al, 2016;Ne ´meth et al, 2016;Seidler et al, 2014Seidler et al, , 2016Zeeshan et al, 2019). In particular, commercial and user-built instrumentation based on a Rowland circle spectrometer with spherically bent crystal analyzers (SBCAs) used in the Johann configuration, and utilizing an energy-dispersive X-ray (EDX) detector, are gaining adoption, both as laboratory and regional facilities with a role complementary to, and symbiotic with, use of synchrotron radiation sources (Ditter et al, 2019). Already, this spectrometer design has been exploited to address a wide range of problems in nuclear, functional, catalysis and geological materials, including operando studies (Be `s et al, 2018;Bi et al, 2019a,b;Jahrman et al, 2019b;Kuai et al, 2018;Lutz & Fittschen, 2020;Mottram et al, 2020a,b,c;Moya-Cancino et al, 2019;Nolis et al, 2020;Sun et al, 2021;Wittkowski et al, 2021;Zimmermann et al, 2021).…”