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Title: Rapid sample delivery for megahertz serial crystallography at X-ray FELs

Abstract

Liquid microjets are a common means of delivering protein crystals to the focus of X-ray free-electron lasers (FELs) for serial femtosecond crystallography measurements. The high X-ray intensity in the focus initiates an explosion of the microjet and sample. With the advent of X-ray FELs with megahertz rates, the typical velocities of these jets must be increased significantly in order to replenish the damaged material in time for the subsequent measurement with the next X-ray pulse. Here in this paper, this work reports the results of a megahertz serial diffraction experiment at the FLASH FEL facility using 4.3 nm radiation. The operation of gas-dynamic nozzles that produce liquid microjets with velocities greater than 80 m s-1was demonstrated. Furthermore, this article provides optical images of X-ray-induced explosions together with Bragg diffraction from protein microcrystals exposed to trains of X-ray pulses repeating at rates of up to 4.5 MHz. Finally, the results indicate the feasibility for megahertz serial crystallography measurements with hard X-rays and give guidance for the design of such experiments.

Authors:
ORCiD logo [1];  [2];  [3];  [3];  [4];  [3];  [5];  [6];  [7];  [3];  [8];  [8];  [9];  [3];  [7];  [10];  [2];  [5];  [3];  [8] more »;  [3];  [3];  [11];  [12];  [3];  [13];  [14];  [13];  [13];  [7];  [15];  [9];  [16];  [1];  [17];  [6];  [8];  [1] « less
+ Show Author Affiliations
  1. Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; Univ. of Hamburg (Germany). Dept. of Physics; Univ. of Hamburg (Germany). Hamburg Center for Ultrafast Imaging
  2. Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; Univ. of Hamburg (Germany). Hamburg Center for Ultrafast Imaging
  3. Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science
  4. Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; Hamburg Univ. of Technology, Hamburg (Germany)
  5. Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; Univ. of Hamburg (Germany). Dept. of Physics
  6. Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Photon Science
  7. European X-ray Free-Electron Laser (XFEL), Hamburg (Germany)
  8. Arizona State Univ., Tempe, AZ (United States)
  9. Univ. de Sevilla, Sevilla (Spain). Dept. of Aerospace Engineering and Fluid Mechanics
  10. Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science; Max Planck Inst. of Biochemistry, Martinsried (Germany). Dept. of Cellular and Molecular Biophysics
  11. SLAC National Accelerator Lab., Menlo Park, CA (United States)
  12. Rutgers University Newark, Newark, NJ (United States). Dept. of Physics; SLAC National Accelerator Lab., Menlo Park, CA (United States). Photon Ultrafast Laser Science and Engineering Inst. (PULSE)
  13. Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany)
  14. Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science, and Photon Science
  15. Arizona State Univ., Mesa, AZ (United States). Biodesign Inst., School of Life Sciences
  16. Arizona State Univ., Tempe, AZ (United States). Biodesign Inst., School of Life Sciences
  17. Australian National Univ., Canberra, ACT (Australia). Research School of Physical Sciences and Engineering, Laser Physics Centre
Publication Date:
Research Org.:
SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States)
Sponsoring Org.:
USDOE; European Union (EU); Australian Research Council (ARC); German Research Foundation (DFG)
OSTI Identifier:
1475541
Grant/Contract Number:  
AC02-76SF00515; DPI2016-78887; ERC-614507-Kupper
Resource Type:
Accepted Manuscript
Journal Name:
IUCrJ
Additional Journal Information:
Journal Volume: 5; Journal Issue: 5; Journal ID: ISSN 2052-2525
Publisher:
International Union of Crystallography
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; X-ray free-electron lasers; FELs; X-ray FEL pulse trains; megahertz repetition rates

Citation Formats

Wiedorn, Max O., Awel, Salah, Morgan, Andrew J., Ayyer, Kartik, Gevorkov, Yaroslav, Fleckenstein, Holger, Roth, Nils, Adriano, Luigi, Bean, Richard, Beyerlein, Kenneth R., Chen, Joe, Coe, Jesse, Cruz-Mazo, Francisco, Ekeberg, Tomas, Graceffa, Rita, Heymann, Michael, Horke, Daniel A., Knoška, Juraj, Mariani, Valerio, Nazari, Reza, Oberthür, Dominik, Samanta, Amit K., Sierra, Raymond G., Stan, Claudiu A., Yefanov, Oleksandr, Rompotis, Dimitrios, Correa, Jonathan, Erk, Benjamin, Treusch, Rolf, Schulz, Joachim, Hogue, Brenda G., Gañán-Calvo, Alfonso M., Fromme, Petra, Küpper, Jochen, Rode, Andrei V., Bajt, Saša, Kirian, Richard A., and Chapman, Henry N. Rapid sample delivery for megahertz serial crystallography at X-ray FELs. United States: N. p., 2018. Web. doi:10.1107/s2052252518008369.
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Wiedorn, Max O., Awel, Salah, Morgan, Andrew J., Ayyer, Kartik, Gevorkov, Yaroslav, Fleckenstein, Holger, Roth, Nils, Adriano, Luigi, Bean, Richard, Beyerlein, Kenneth R., Chen, Joe, Coe, Jesse, Cruz-Mazo, Francisco, Ekeberg, Tomas, Graceffa, Rita, Heymann, Michael, Horke, Daniel A., Knoška, Juraj, Mariani, Valerio, Nazari, Reza, Oberthür, Dominik, Samanta, Amit K., Sierra, Raymond G., Stan, Claudiu A., Yefanov, Oleksandr, Rompotis, Dimitrios, Correa, Jonathan, Erk, Benjamin, Treusch, Rolf, Schulz, Joachim, Hogue, Brenda G., Gañán-Calvo, Alfonso M., Fromme, Petra, Küpper, Jochen, Rode, Andrei V., Bajt, Saša, Kirian, Richard A., & Chapman, Henry N. Rapid sample delivery for megahertz serial crystallography at X-ray FELs. United States. https://doi.org/10.1107/s2052252518008369
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Wiedorn, Max O., Awel, Salah, Morgan, Andrew J., Ayyer, Kartik, Gevorkov, Yaroslav, Fleckenstein, Holger, Roth, Nils, Adriano, Luigi, Bean, Richard, Beyerlein, Kenneth R., Chen, Joe, Coe, Jesse, Cruz-Mazo, Francisco, Ekeberg, Tomas, Graceffa, Rita, Heymann, Michael, Horke, Daniel A., Knoška, Juraj, Mariani, Valerio, Nazari, Reza, Oberthür, Dominik, Samanta, Amit K., Sierra, Raymond G., Stan, Claudiu A., Yefanov, Oleksandr, Rompotis, Dimitrios, Correa, Jonathan, Erk, Benjamin, Treusch, Rolf, Schulz, Joachim, Hogue, Brenda G., Gañán-Calvo, Alfonso M., Fromme, Petra, Küpper, Jochen, Rode, Andrei V., Bajt, Saša, Kirian, Richard A., and Chapman, Henry N. Fri . "Rapid sample delivery for megahertz serial crystallography at X-ray FELs". United States. https://doi.org/10.1107/s2052252518008369. https://www.osti.gov/servlets/purl/1475541.
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@article{osti_1475541,
title = {Rapid sample delivery for megahertz serial crystallography at X-ray FELs},
author = {Wiedorn, Max O. and Awel, Salah and Morgan, Andrew J. and Ayyer, Kartik and Gevorkov, Yaroslav and Fleckenstein, Holger and Roth, Nils and Adriano, Luigi and Bean, Richard and Beyerlein, Kenneth R. and Chen, Joe and Coe, Jesse and Cruz-Mazo, Francisco and Ekeberg, Tomas and Graceffa, Rita and Heymann, Michael and Horke, Daniel A. and Knoška, Juraj and Mariani, Valerio and Nazari, Reza and Oberthür, Dominik and Samanta, Amit K. and Sierra, Raymond G. and Stan, Claudiu A. and Yefanov, Oleksandr and Rompotis, Dimitrios and Correa, Jonathan and Erk, Benjamin and Treusch, Rolf and Schulz, Joachim and Hogue, Brenda G. and Gañán-Calvo, Alfonso M. and Fromme, Petra and Küpper, Jochen and Rode, Andrei V. and Bajt, Saša and Kirian, Richard A. and Chapman, Henry N.},
abstractNote = {Liquid microjets are a common means of delivering protein crystals to the focus of X-ray free-electron lasers (FELs) for serial femtosecond crystallography measurements. The high X-ray intensity in the focus initiates an explosion of the microjet and sample. With the advent of X-ray FELs with megahertz rates, the typical velocities of these jets must be increased significantly in order to replenish the damaged material in time for the subsequent measurement with the next X-ray pulse. Here in this paper, this work reports the results of a megahertz serial diffraction experiment at the FLASH FEL facility using 4.3 nm radiation. The operation of gas-dynamic nozzles that produce liquid microjets with velocities greater than 80 m s-1was demonstrated. Furthermore, this article provides optical images of X-ray-induced explosions together with Bragg diffraction from protein microcrystals exposed to trains of X-ray pulses repeating at rates of up to 4.5 MHz. Finally, the results indicate the feasibility for megahertz serial crystallography measurements with hard X-rays and give guidance for the design of such experiments.},
doi = {10.1107/s2052252518008369},
journal = {IUCrJ},
number = 5,
volume = 5,
place = {United States},
year = {Fri Jul 27 00:00:00 EDT 2018},
month = {Fri Jul 27 00:00:00 EDT 2018}
}
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https://doi.org/10.1107/s2052252518008369
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    Works referencing / citing this record:

    Membrane protein megahertz crystallography at the European XFEL
    journal, November 2019

    Ultracompact 3D microfluidics for time-resolved structural biology
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    Rapid mixing of colliding picoliter liquid droplets delivered through-space from piezoelectric-actuated pipettes characterized by time-resolved fluorescence monitoring
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    • Tellkamp, Friedjof; Khajehpour, Mazdak; Robertson, Wesley D.
    • Review of Scientific Instruments, Vol. 90, Issue 5
    • DOI: 10.1063/1.5050270

    On the characterization of a 1 m long, ultra-precise KB-focusing mirror pair for European XFEL by means of slope measuring deflectometry
    journal, February 2019

    • Siewert, F.; Buchheim, J.; Gwalt, G.
    • Review of Scientific Instruments, Vol. 90, Issue 2
    • DOI: 10.1063/1.5065473

    Evaluation of serial crystallographic structure determination within megahertz pulse trains
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    A guide to sample delivery systems for serial crystallography
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    Megahertz serial crystallography
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    • Wiedorn, Max O.; Oberthür, Dominik; Bean, Richard
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    Membrane protein megahertz crystallography at the European XFEL
    text, January 2019

    • Gisriel, Chris; Coe, Jesse; Letrun, Romain
    • Deutsches Elektronen-Synchrotron, DESY, Hamburg
    • DOI: 10.3204/pubdb-2019-03909

    Evaluation of serial crystallographic structure determination within megahertz pulse trains
    text, January 2019

    • Yefanov, Oleksandr; Oberthür, Dominik; Bean, Richard
    • Deutsches Elektronen-Synchrotron, DESY, Hamburg
    • DOI: 10.3204/pubdb-2019-04763

    Ultracompact 3D microfluidics for time-resolved structural biology
    text, January 2020

    • Knoška, Juraj; Adriano, Luigi; Awel, Salah
    • Deutsches Elektronen-Synchrotron, DESY, Hamburg
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    Megahertz serial crystallography
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    Membrane protein megahertz crystallography at the European XFEL
    text, January 2019

    • Gisriel, Christopher; Coe, Jesse; Letrun, Romain
    • Nature Publishing Group UK
    • DOI: 10.15480/882.2506

    Ultracompact 3D microfluidics for time-resolved structural biology
    text, January 2020

    • Knoska, Juraj; Adriano, Luigi; Awel, Salah
    • Deutsches Elektronen-Synchrotron, DESY, Hamburg
    • DOI: 10.3204/pubdb-2020-00623

    Megahertz serial crystallography
    text, January 2018

    • Wiedorn, Max Oliver; Oberthür, Dominik; Bean, Richard
    • Nature Publishing Group UK
    • DOI: 10.15480/882.2175
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