Journal
JOURNAL OF SYNCHROTRON RADIATION
Volume 26, Issue -, Pages 1716-1724Publisher
INT UNION CRYSTALLOGRAPHY
DOI: 10.1107/S1600577519007550
Keywords
X-ray free electron lasers; X-ray near-edge spectroscopy; extended X-ray absorption fine structure; X-ray absorption spectroscopy
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Funding
- National Institutes of Health [GM110501, GM126289, GM055302]
- Office of Science, Office of Basic Energy Sciences (OBES), Division of Chemical Sciences, Geosciences and Biosciences of the Department of Energy (DOE) [DE-AC02-05CH11231]
- Energimyndigheten [2016-05183]
- Vetenskapsradet [2016-05183, 2017-00356]
- Ruth L. Kirschstein NationalResearch Service Award [GM116423-02]
- US DOE, Office of Science, OBES [DE-AC02-76SF00515]
- Vinnova [2017-00356] Funding Source: Vinnova
- Swedish Research Council [2016-05183, 2017-00356] Funding Source: Swedish Research Council
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This work has demonstrated that X-ray absorption spectroscopy (XAS), both Mn XANES and EXAFS, of solutions with millimolar concentrations of metal is possible using the femtosecond X-ray pulses from XFELs. Mn XAS data were collected using two different sample delivery methods, a Rayleigh jet and a drop-on-demand setup, with varying concentrations of Mn. Here, a new method for normalization of XAS spectra based on solvent scattering that is compatible with data collection from a highly variable pulsed source is described. The measured XANES and EXAFS spectra of such dilute solution samples are in good agreement with data collected at synchrotron sources using traditional scanning protocols. The procedures described here will enable XFEL-based XAS on dilute biological samples, especially metalloproteins, with low sample consumption. Details of the experimental setup and data analysis methods used in this XANES and EXAFS study are presented. This method will also benefit XAS performed at high-repetition-rate XFELs such as the European XFEL, LCLS-II and LCLS-II-HE.
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