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Title: XANES and EXAFS of dilute solutions of transition metals at XFELs

Abstract

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.

Authors:
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Publication Date:
Research Org.:
Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22). Chemical Sciences, Geosciences & Biosciences Division
OSTI Identifier:
1598524
DOE Contract Number:  
AC02-05CH11231
Resource Type:
Journal Article
Journal Name:
Journal of Synchrotron Radiation (Online)
Additional Journal Information:
Journal Volume: 26; Journal Issue: 5; Journal ID: ISSN 1600-5775
Publisher:
International Union of Crystallography
Country of Publication:
United States
Language:
English

Citation Formats

Chatterjee, Ruchira, Weninger, Clemens, Loukianov, Anton, Gul, Sheraz, Fuller, Franklin D., Cheah, Mun Hon, Fransson, Thomas, Pham, Cindy C., Nelson, Silke, Song, Sanghoon, Britz, Alexander, Messinger, Johannes, Bergmann, Uwe, Alonso-Mori, Roberto, Yachandra, Vittal K., Kern, Jan, and Yano, Junko. XANES and EXAFS of dilute solutions of transition metals at XFELs. United States: N. p., 2019. Web. doi:10.1107/s1600577519007550.
Chatterjee, Ruchira, Weninger, Clemens, Loukianov, Anton, Gul, Sheraz, Fuller, Franklin D., Cheah, Mun Hon, Fransson, Thomas, Pham, Cindy C., Nelson, Silke, Song, Sanghoon, Britz, Alexander, Messinger, Johannes, Bergmann, Uwe, Alonso-Mori, Roberto, Yachandra, Vittal K., Kern, Jan, & Yano, Junko. XANES and EXAFS of dilute solutions of transition metals at XFELs. United States. doi:10.1107/s1600577519007550.
Chatterjee, Ruchira, Weninger, Clemens, Loukianov, Anton, Gul, Sheraz, Fuller, Franklin D., Cheah, Mun Hon, Fransson, Thomas, Pham, Cindy C., Nelson, Silke, Song, Sanghoon, Britz, Alexander, Messinger, Johannes, Bergmann, Uwe, Alonso-Mori, Roberto, Yachandra, Vittal K., Kern, Jan, and Yano, Junko. Wed . "XANES and EXAFS of dilute solutions of transition metals at XFELs". United States. doi:10.1107/s1600577519007550.
@article{osti_1598524,
title = {XANES and EXAFS of dilute solutions of transition metals at XFELs},
author = {Chatterjee, Ruchira and Weninger, Clemens and Loukianov, Anton and Gul, Sheraz and Fuller, Franklin D. and Cheah, Mun Hon and Fransson, Thomas and Pham, Cindy C. and Nelson, Silke and Song, Sanghoon and Britz, Alexander and Messinger, Johannes and Bergmann, Uwe and Alonso-Mori, Roberto and Yachandra, Vittal K. and Kern, Jan and Yano, Junko},
abstractNote = {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.},
doi = {10.1107/s1600577519007550},
journal = {Journal of Synchrotron Radiation (Online)},
issn = {1600-5775},
number = 5,
volume = 26,
place = {United States},
year = {2019},
month = {8}
}

Works referenced in this record:

Perspective: Opportunities for ultrafast science at SwissFEL
journal, November 2017

  • Abela, Rafael; Beaud, Paul; van Bokhoven, Jeroen A.
  • Structural Dynamics, Vol. 4, Issue 6
  • DOI: 10.1063/1.4997222

Energy-dispersive X-ray emission spectroscopy using an X-ray free-electron laser in a shot-by-shot mode
journal, November 2012

  • Alonso-Mori, R.; Kern, J.; Gildea, R. J.
  • Proceedings of the National Academy of Sciences, Vol. 109, Issue 47, p. 19103-19107
  • DOI: 10.1073/pnas.1211384109

Photon-in photon-out hard X-ray spectroscopy at the Linac Coherent Light Source
journal, April 2015

  • Alonso-Mori, Roberto; Sokaras, Dimosthenis; Zhu, Diling
  • Journal of Synchrotron Radiation, Vol. 22, Issue 3
  • DOI: 10.1107/S1600577515004488

Demonstration of self-seeding in a hard-X-ray free-electron laser
journal, August 2012


Geometrical fitting of experimental XANES spectra by a full multiple-scattering procedure
journal, June 2001


X-ray detectors at the Linac Coherent Light Source
journal, April 2015

  • Blaj, Gabriel; Caragiulo, Pietro; Carini, Gabriella
  • Journal of Synchrotron Radiation, Vol. 22, Issue 3
  • DOI: 10.1107/S1600577515005317

Femtosecond XANES Study of the Light-Induced Spin Crossover Dynamics in an Iron(II) Complex
journal, January 2009


Recent advances on ultrafast X-ray spectroscopy in the chemical sciences
journal, January 2014

  • Chen, L. X.; Zhang, X.; Shelby, M. L.
  • Chem. Sci., Vol. 5, Issue 11
  • DOI: 10.1039/C4SC01333F

Ultrafast Photophysics of Transition Metal Complexes
journal, February 2015

  • Chergui, Majed
  • Accounts of Chemical Research, Vol. 48, Issue 3
  • DOI: 10.1021/ar500358q

The X-ray Pump–Probe instrument at the Linac Coherent Light Source
journal, April 2015

  • Chollet, Matthieu; Alonso-Mori, Roberto; Cammarata, Marco
  • Journal of Synchrotron Radiation, Vol. 22, Issue 3
  • DOI: 10.1107/S1600577515005135

Drop-on-demand sample delivery for studying biocatalysts in action at X-ray free-electron lasers
journal, February 2017

  • Fuller, Franklin D.; Gul, Sheraz; Chatterjee, Ruchira
  • Nature Methods, Vol. 14, Issue 4
  • DOI: 10.1038/nmeth.4195

Megahertz data collection from protein microcrystals at an X-ray free-electron laser
journal, August 2018

  • Grünbein, Marie Luise; Bielecki, Johan; Gorel, Alexander
  • Nature Communications, Vol. 9, Issue 1
  • DOI: 10.1038/s41467-018-05953-4

CSPAD-140k: A versatile detector for LCLS experiments
journal, August 2013

  • Herrmann, Sven; Boutet, Sébastien; Duda, Brian
  • Nuclear Instruments and Methods in Physics Research Section A: Accelerators, Spectrometers, Detectors and Associated Equipment, Vol. 718
  • DOI: 10.1016/j.nima.2013.01.057

Structural characterization of the active form of PerR: insights into the metal-induced activation of PerR and Fur proteins for DNA binding
journal, July 2009


Transient electronic and magnetic structures of nickel heated by ultrafast laser pulses
journal, September 2009


X-ray absorption spectroscopy using a self-seeded soft X-ray free-electron laser
journal, January 2016

  • Kroll, Thomas; Kern, Jan; Kubin, Markus
  • Optics Express, Vol. 24, Issue 20
  • DOI: 10.1364/OE.24.022469

Femtosecond X-ray Absorption Spectroscopy at a Hard X-ray Free Electron Laser: Application to Spin Crossover Dynamics
journal, January 2013

  • Lemke, Henrik T.; Bressler, Christian; Chen, Lin X.
  • The Journal of Physical Chemistry A, Vol. 117, Issue 4
  • DOI: 10.1021/jp312559h

Ultrafast myoglobin structural dynamics observed with an X-ray free-electron laser
journal, April 2015

  • Levantino, Matteo; Schirò, Giorgio; Lemke, Henrik Till
  • Nature Communications, Vol. 6, Issue 1
  • DOI: 10.1038/ncomms7772

Metalloprotein entatic control of ligand-metal bonds quantified by ultrafast x-ray spectroscopy
journal, June 2017


Polarized XANES Monitors Femtosecond Structural Evolution of Photoexcited Vitamin B 12
journal, January 2017

  • Miller, Nicholas A.; Deb, Aniruddha; Alonso-Mori, Roberto
  • Journal of the American Chemical Society, Vol. 139, Issue 5
  • DOI: 10.1021/jacs.6b11295

Experimental Demonstration of a Soft X-Ray Self-Seeded Free-Electron Laser
journal, February 2015


ATHENA , ARTEMIS , HEPHAESTUS : data analysis for X-ray absorption spectroscopy using IFEFFIT
journal, June 2005


Theoretical approaches to x-ray absorption fine structure
journal, July 2000


Ultrafast Excited State Relaxation of a Metalloporphyrin Revealed by Femtosecond X-ray Absorption Spectroscopy
journal, July 2016

  • Shelby, Megan L.; Lestrange, Patrick J.; Jackson, Nicholas E.
  • Journal of the American Chemical Society, Vol. 138, Issue 28
  • DOI: 10.1021/jacs.6b02176

New insight into metalloporphyrin excited state structures and axial ligand binding from X-ray transient absorption spectroscopic studies
journal, October 2014

  • Shelby, Megan L.; Mara, Michael W.; Chen, Lin X.
  • Coordination Chemistry Reviews, Vol. 277-278
  • DOI: 10.1016/j.ccr.2014.05.025

Concentric-flow electrokinetic injector enables serial crystallography of ribosome and photosystem II
journal, November 2015

  • Sierra, Raymond G.; Gati, Cornelius; Laksmono, Hartawan
  • Nature Methods, Vol. 13, Issue 1
  • DOI: 10.1038/nmeth.3667

Nanoflow electrospinning serial femtosecond crystallography
journal, October 2012

  • Sierra, Raymond G.; Laksmono, Hartawan; Kern, Jan
  • Acta Crystallographica Section D Biological Crystallography, Vol. 68, Issue 11, p. 1584-1587
  • DOI: 10.1107/S0907444912038152

Photon Beam Transport and Scientific Instruments at the European XFEL
journal, June 2017

  • Tschentscher, Thomas; Bressler, Christian; Grünert, Jan
  • Applied Sciences, Vol. 7, Issue 6
  • DOI: 10.3390/app7060592

Megahertz serial crystallography
journal, October 2018