Oxygen K-edge X-ray absorption spectra of liquids with minimization of window contamination

Vogt, Linda I.; Cotelesage, Julien H.; Titus, Charles J.; Sharifi, Samin; Butterfield, Albert E.; Hillman, Peter; Pickering, Ingrid J.; George, Graham N.; George, Simon J.

doi:10.1107/s1600577521009942

Title: Oxygen K-edge X-ray absorption spectra of liquids with minimization of window contamination

Journal Article · 18 October 2021 · Journal of Synchrotron Radiation (Online)

DOI: https://doi.org/10.1107/s1600577521009942 · OSTI ID:1872786

^[1]; Cotelesage, Julien H. ^[1];

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^[3]; Hillman, Peter ^[3];

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Univ. of Saskatchewan, Saskatoon, SK (Canada)
Stanford Univ., CA (United States)
Chevron Energy Technology Company, Richmond, CA (United States)
Simon Scientific, Berkeley, CA (United States)

We report oxygen K-edge X-ray absorption spectroscopy is used routinely to study a range of solid materials. However, liquid samples are studied less frequently at the oxygen K-edge due to the combined challenges of high-vacuum conditions and oxygen contamination of window materials. A modular sample holder design with a twist-seal sample containment system that provides a simple method to encapsulate liquid samples under high-vacuum conditions is presented. This work shows that pure silicon nitride windows have lower oxygen contamination than both diamond- and silicon-rich nitride windows, that the levels of oxygen contamination are related to the age of the windows, and provides a protocol for minimizing the background oxygen contamination. Acid-washed 100 nm-thick silicon nitride windows were found to give good quality oxygen K-edge data on dilute liquid samples.

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Research Organization:: SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES); Chevron Energy Technology Company; Natural Sciences and Engineering Research Council of Canada (NSERC)

Grant/Contract Number:: AC02-76SF00515; RGPIN-2016-05810; RGPIN-2019-05351

OSTI ID:: 1872786

Journal Information:: Journal of Synchrotron Radiation (Online), Vol. 28, Issue 6; ISSN 1600-5775

Publisher:: International Union of CrystallographyCopyright Statement

Country of Publication:: United States

Language:: English

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