The Liquid Jet Endstation for Hard X-ray Scattering and Spectroscopy at the Linac Coherent Light Source

Antolini, Cali; Alfaro, Victor Sosa; Reinhard, Marco; Chatterjee, Gourab; Ribson, Ryan; Sokaras, Dimosthenis; Gee, Leland; Sato, Takahiro; Kramer, Patrick L.; Raj, Sumana Laxmi; Hayes, Brandon; Schleissner, Pamela; Garcia-Esparza, Angel T.; Lim, Jinkyu; Babicz, Jr., Jeffrey Babicz; Follmer, Alec H.; Nelson, Silke; Chollet, Matthieu; Alonso-Mori, Roberto; van Driel, Tim B.

doi:10.3390/molecules29102323

The Liquid Jet Endstation for Hard X-ray Scattering and Spectroscopy at the Linac Coherent Light Source

Journal Article · Wed May 15 00:00:00 EDT 2024 · Molecules

DOI:https://doi.org/10.3390/molecules29102323· OSTI ID:2349466

^[1]; ^[2]; ^[2]; ^[2]; Ribson, Ryan ^[2]; ^[2]; ^[2]; Sato, Takahiro ^[2]; ^[2]; ^[2]; Hayes, Brandon ^[2]; Schleissner, Pamela ^[2]; ^[2]; ^[3]; Babicz, Jr., Jeffrey Babicz ^[2]; ^[4]; Nelson, Silke ^[2]; Chollet, Matthieu ^[2]; ^[2]; ^[2]

SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States); SLAC National Laboratory
SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States)
SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States); The Catholic University of Korea, Bucheon (Korea, Republic of)
Univ. of California, Irvine, CA (United States)

The ability to study chemical dynamics on ultrafast timescales has greatly advanced with the introduction of X-ray free electron lasers (XFELs) providing short pulses of intense X-rays tailored to probe atomic structure and electronic configuration. Fully exploiting the full potential of XFELs requires specialized experimental endstations along with the development of techniques and methods to successfully carry out experiments. The liquid jet endstation (LJE) at the Linac Coherent Light Source (LCLS) has been developed to study photochemistry and biochemistry in solution systems using a combination of X-ray solution scattering (XSS), X-ray absorption spectroscopy (XAS), and X-ray emission spectroscopy (XES). The pump–probe setup utilizes an optical laser to excite the sample, which is subsequently probed by a hard X-ray pulse to resolve structural and electronic dynamics at their intrinsic femtosecond timescales. The LJE ensures reliable sample delivery to the X-ray interaction point via various liquid jets, enabling rapid replenishment of thin samples with millimolar concentrations and low sample volumes at the 120 Hz repetition rate of the LCLS beam. This paper provides a detailed description of the LJE design and of the techniques it enables, with an emphasis on the diagnostics required for real-time monitoring of the liquid jet and on the spatiotemporal overlap methods used to optimize the signal. Additionally, various scientific examples are discussed, highlighting the versatility of the LJE.

View Accepted Manuscript (DOE)

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

Sponsoring Organization:: National Institutes of Health (NIH); USDOE Office of Science (SC), Basic Energy Sciences (BES). Scientific User Facilities (SUF)

Grant/Contract Number:: AC02-76SF00515

OSTI ID:: 2349466

Journal Information:: Molecules, Journal Name: Molecules Journal Issue: 10 Vol. 29; ISSN 1420-3049

Publisher:: MDPICopyright Statement

Country of Publication:: United States

Language:: English

References (65)

X-ray absorption spectroscopy Yano, Junko; Yachandra, Vittal K. Photosynthesis Research, Vol. 102, Issue 2-3 https://doi.org/10.1007/s11120-009-9473-8	journal	August 2009
X-ray absorption spectroscopy of biological photolysis products: kilohertz photolysis and soft X-ray applications Wang, Hongxin; Peng, Gang; Cramer, Stephen P. Journal of Electron Spectroscopy and Related Phenomena, Vol. 143, Issue 1 https://doi.org/10.1016/j.elspec.2004.10.011	journal	April 2005
Primary reactions in the photochemistry of hexahalide complexes of platinum group metals: A minireview Glebov, Evgeni M.; Pozdnyakov, Ivan P.; Plyusnin, Victor F. Journal of Photochemistry and Photobiology C: Photochemistry Reviews, Vol. 24 https://doi.org/10.1016/j.jphotochemrev.2015.05.003	journal	September 2015
Comprehensive Experimental and Computational Spectroscopic Study of Hexacyanoferrate Complexes in Water: From Infrared to X-ray Wavelengths Ross, Matthew; Andersen, Amity; Fox, Zachary W. The Journal of Physical Chemistry B, Vol. 122, Issue 19 https://doi.org/10.1021/acs.jpcb.7b12532	journal	April 2018
Probing the Excited State of Methylcobalamin Using Polarized Time-Resolved X-ray Absorption Spectroscopy Michocki, Lindsay B.; Miller, Nicholas A.; Alonso-Mori, Roberto The Journal of Physical Chemistry B, Vol. 123, Issue 28 https://doi.org/10.1021/acs.jpcb.9b05854	journal	June 2019
Ultrafast XANES Monitors Femtosecond Sequential Structural Evolution in Photoexcited Coenzyme B ₁₂ Miller, Nicholas A.; Michocki, Lindsay B.; Konar, Arkaprabha The Journal of Physical Chemistry B, Vol. 124, Issue 1 https://doi.org/10.1021/acs.jpcb.9b09286	journal	December 2019
Base-Accelerated Degradation of Nanosized Platinum Electrocatalysts Hersbach, Thomas J. P.; Garcia, Amanda C.; Kroll, Thomas ACS Catalysis, Vol. 11, Issue 15 https://doi.org/10.1021/acscatal.1c02468	journal	July 2021
Ultrafast Photophysics of Transition Metal Complexes Chergui, Majed Accounts of Chemical Research, Vol. 48, Issue 3 https://doi.org/10.1021/ar500358q	journal	February 2015
Structural and Functional Aspects of Metal Sites in Biology Holm, Richard H.; Kennepohl, Pierre; Solomon, Edward I. Chemical Reviews, Vol. 96, Issue 7 https://doi.org/10.1021/cr9500390	journal	January 1996
Theoretical x-ray absorption fine structure standards Rehr, J. J.; Mustre de Leon, J.; Zabinsky, S. I. Journal of the American Chemical Society, Vol. 113, Issue 14 https://doi.org/10.1021/ja00014a001	journal	July 1991
Full Quantitative Multiple-Scattering Analysis of X-ray Absorption Spectra: Application to Potassium Hexacyanoferrat(II) and -(III) Complexes Hayakawa, Kuniko; Hatada, Keisuke; D'Angelo, Paola Journal of the American Chemical Society, Vol. 126, Issue 47 https://doi.org/10.1021/ja045561v	journal	December 2004
Watching Excited State Dynamics with Optical and X-ray Probes: The Excited State Dynamics of Aquocobalamin and Hydroxocobalamin Sension, Roseanne J.; McClain, Taylor P.; Lamb, Ryan M. Journal of the American Chemical Society, Vol. 145, Issue 25 https://doi.org/10.1021/jacs.3c04099	journal	June 2023
Detailed Transient Heme Structures of Mb-CO in Solution after CO Dissociation: An X-ray Transient Absorption Spectroscopic Study Stickrath, Andrew B.; Mara, Michael W.; Lockard, Jenny V. The Journal of Physical Chemistry B, Vol. 117, Issue 16 https://doi.org/10.1021/jp3086705	journal	November 2012
Femtosecond X-ray Absorption Spectroscopy at a Hard X-ray Free Electron Laser: Application to Spin Crossover Dynamics Lemke, Henrik T.; Bressler, Christian; Chen, Lin X. The Journal of Physical Chemistry A, Vol. 117, Issue 4 https://doi.org/10.1021/jp312559h	journal	January 2013
Local Structure, Electronic Behavior, and Electrocatalytic Reactivity of CO-Reduced Platinum–Iron Oxide Nanoparticles Duchesne, Paul N.; Chen, Guangxu; Zheng, Nanfeng The Journal of Physical Chemistry C, Vol. 117, Issue 49 https://doi.org/10.1021/jp4093496	journal	November 2013
X-ray Spectroscopic Study of Solvent Effects on the Ferrous and Ferric Hexacyanide Anions Penfold, T. J.; Reinhard, M.; Rittmann-Frank, M. H. The Journal of Physical Chemistry A, Vol. 118, Issue 40 https://doi.org/10.1021/jp5055588	journal	September 2014
Atomistic characterization of the active-site solvation dynamics of a model photocatalyst van Driel, Tim B.; Kjær, Kasper S.; Hartsock, Robert W. Nature Communications, Vol. 7, Issue 1 https://doi.org/10.1038/ncomms13678	journal	November 2016
Coherent structural trapping through wave packet dispersion during photoinduced spin state switching Lemke, Henrik T.; Kjær, Kasper S.; Hartsock, Robert Nature Communications, Vol. 8, Issue 1 https://doi.org/10.1038/ncomms15342	journal	May 2017
Few-femtosecond time-resolved measurements of X-ray free-electron lasers Behrens, C.; Decker, F. -J.; Ding, Y. Nature Communications, Vol. 5, Issue 1 https://doi.org/10.1038/ncomms4762	journal	April 2014
Achieving few-femtosecond time-sorting at hard X-ray free-electron lasers Harmand, M.; Coffee, R.; Bionta, M. R. Nature Photonics, Vol. 7, Issue 3 https://doi.org/10.1038/nphoton.2013.11	journal	February 2013
Liquid explosions induced by X-ray laser pulses Stan, Claudiu A.; Milathianaki, Despina; Laksmono, Hartawan Nature Physics, Vol. 12, Issue 10 https://doi.org/10.1038/nphys3779	journal	May 2016
Generation and characterization of ultrathin free-flowing liquid sheets Koralek, Jake D.; Kim, Jongjin B.; Brůža, Petr Nature Communications, Vol. 9, Issue 1 https://doi.org/10.1038/s41467-018-03696-w	journal	April 2018
Vibrational wavepacket dynamics in Fe carbene photosensitizer determined with femtosecond X-ray emission and scattering Kunnus, Kristjan; Vacher, Morgane; Harlang, Tobias C. B. Nature Communications, Vol. 11, Issue 1 https://doi.org/10.1038/s41467-020-14468-w	journal	January 2020
Ferricyanide photo-aquation pathway revealed by combined femtosecond Kβ main line and valence-to-core x-ray emission spectroscopy Reinhard, Marco; Gallo, Alessandro; Guo, Meiyuan Nature Communications, Vol. 14, Issue 1 https://doi.org/10.1038/s41467-023-37922-x	journal	May 2023
Charge transfer driven by ultrafast spin transition in a CoFe Prussian blue analogue Cammarata, Marco; Zerdane, Serhane; Balducci, Lodovico Nature Chemistry, Vol. 13, Issue 1 https://doi.org/10.1038/s41557-020-00597-8	journal	December 2020
Direct observation of coherent femtosecond solvent reorganization coupled to intramolecular electron transfer Biasin, Elisa; Fox, Zachary W.; Andersen, Amity Nature Chemistry, Vol. 13, Issue 4 https://doi.org/10.1038/s41557-020-00629-3	journal	February 2021
Influence of pump laser fluence on ultrafast myoglobin structural dynamics Barends, Thomas R. M.; Gorel, Alexander; Bhattacharyya, Swarnendu Nature, Vol. 626, Issue 8000 https://doi.org/10.1038/s41586-024-07032-9	journal	February 2024
Tunable x-ray free electron laser multi-pulses with nanosecond separation Decker, Franz-Josef; Bane, Karl L.; Colocho, William Scientific Reports, Vol. 12, Issue 1 https://doi.org/10.1038/s41598-022-06754-y	journal	February 2022
X-Ray Free Electron Lasers Bergmann, Uwe; Yachandra, Vittal; Yano, Junko Energy and Environment Series https://doi.org/10.1039/9781782624097	book	August 2017
Introducing a standard method for experimental determination of the solvent response in laser pump, X-ray probe time-resolved wide-angle X-ray scattering experiments on systems in solution Kjær, Kasper Skov; van Driel, Tim B.; Kehres, Jan Phys. Chem. Chem. Phys., Vol. 15, Issue 36 https://doi.org/10.1039/C3CP50751C	journal	January 2013
Solvent control of charge transfer excited state relaxation pathways in [Fe(2,2′-bipyridine)(CN) ₄ ] ²⁻ Kjær, Kasper S.; Kunnus, Kristjan; Harlang, Tobias C. B. Physical Chemistry Chemical Physics, Vol. 20, Issue 6 https://doi.org/10.1039/C7CP07838B	journal	January 2018
Finding intersections between electronic excited state potential energy surfaces with simultaneous ultrafast X-ray scattering and spectroscopy Kjær, Kasper S.; Van Driel, Tim B.; Harlang, Tobias C. B. Chemical Science, Vol. 10, Issue 22 https://doi.org/10.1039/C8SC04023K	journal	January 2019
Resolving structures of transition metal complex reaction intermediates with femtosecond EXAFS Britz, Alexander; Abraham, Baxter; Biasin, Elisa Physical Chemistry Chemical Physics, Vol. 22, Issue 5 https://doi.org/10.1039/C9CP03483H	journal	January 2020
Capturing photochemical and photophysical transformations in iron complexes with ultrafast X-ray spectroscopy and scattering Gaffney, Kelly J. Chemical Science, Vol. 12, Issue 23 https://doi.org/10.1039/D1SC01864G	journal	January 2021
Reaction dynamics studied via femtosecond X-ray liquidography at X-ray free-electron lasers Choi, Eun Hyuk; Lee, Yunbeom; Heo, Jun Chemical Science, Vol. 13, Issue 29 https://doi.org/10.1039/D2SC00502F	journal	January 2022
Initial metal–metal bond breakage detected by fs X-ray scattering in the photolysis of Ru ₃ (CO) ₁₂ in cyclohexane at 400 nm Kong, Q. Y.; Laursen, M. G.; Haldrup, K. Photochemical & Photobiological Sciences, Vol. 18, Issue 2 https://doi.org/10.1039/c8pp00420j	journal	January 2019
A multi-crystal wavelength dispersive x-ray spectrometer Alonso-Mori, Roberto; Kern, Jan; Sokaras, Dimosthenis Review of Scientific Instruments, Vol. 83, Issue 7 https://doi.org/10.1063/1.4737630	journal	July 2012
Photooxidation and photoaquation of iron hexacyanide in aqueous solution: A picosecond X-ray absorption study Reinhard, M.; Penfold, T. J.; Lima, F. A. Structural Dynamics, Vol. 1, Issue 2 https://doi.org/10.1063/1.4871751	journal	March 2014
Spectral encoding method for measuring the relative arrival time between x-ray/optical pulses Bionta, M. R.; Hartmann, N.; Weaver, M. Review of Scientific Instruments, Vol. 85, Issue 8 https://doi.org/10.1063/1.4893657	journal	August 2014
Observing heme doming in myoglobin with femtosecond X-ray absorption spectroscopya) Levantino, M.; Lemke, H. T.; Schirò, G. Structural Dynamics, Vol. 2, Issue 4 https://doi.org/10.1063/1.4921907	journal	May 2015
Performance of ePix10K, a high dynamic range, gain auto-ranging pixel detector for FELs Blaj, G.; Dragone, A.; Kenney, C. J. PROCEEDINGS OF THE 13TH INTERNATIONAL CONFERENCE ON SYNCHROTRON RADIATION INSTRUMENTATION – SRI2018, AIP Conference Proceedings https://doi.org/10.1063/1.5084693	conference	January 2019
Elucidation of the photoaquation reaction mechanism in ferrous hexacyanide using synchrotron x-rays with sub-pulse-duration sensitivity March, Anne Marie; Doumy, Gilles; Andersen, Amity The Journal of Chemical Physics, Vol. 151, Issue 14 https://doi.org/10.1063/1.5117318	journal	October 2019
Excited state charge distribution and bond expansion of ferrous complexes observed with femtosecond valence-to-core x-ray emission spectroscopy Ledbetter, Kathryn; Reinhard, Marco E.; Kunnus, Kristjan The Journal of Chemical Physics, Vol. 152, Issue 7 https://doi.org/10.1063/1.5139441	journal	February 2020
Tracking structural solvent reorganization and recombination dynamics following e⁻ photoabstraction from aqueous I⁻ with femtosecond x-ray spectroscopy and scattering Vester, Peter; Kubicek, Katharina; Alonso-Mori, Roberto The Journal of Chemical Physics, Vol. 157, Issue 22 https://doi.org/10.1063/5.0107224	journal	December 2022
Ultrafast X-Ray Scattering Measurements of Coherent Structural Dynamics on the Ground-State Potential Energy Surface of a Diplatinum Molecule Haldrup, Kristoffer; Levi, Gianluca; Biasin, Elisa Physical Review Letters, Vol. 122, Issue 6 https://doi.org/10.1103/PhysRevLett.122.063001	journal	February 2019
Observation of Seeded Mn K β Stimulated X-Ray Emission Using Two-Color X-Ray Free-Electron Laser Pulses Kroll, Thomas; Weninger, Clemens; Fuller, Franklin D. Physical Review Letters, Vol. 125, Issue 3 https://doi.org/10.1103/PhysRevLett.125.037404	journal	July 2020
Optically Induced Anisotropy in Time-Resolved Scattering: Imaging Molecular-Scale Structure and Dynamics in Disordered Media with Experiment and Theory Montoya-Castillo, Andrés; Chen, Michael S.; Raj, Sumana L. Physical Review Letters, Vol. 129, Issue 5 https://doi.org/10.1103/PhysRevLett.129.056001	journal	July 2022
Quantitative Analysis of X-Ray Absorption Near Edge Structure Data by a Full Multiple Scattering Procedure: The Fe-CO Geometry in Photolyzed Carbonmonoxy-Myoglobin Single Crystal Longa, S. Della; Arcovito, A.; Girasole, M. Physical Review Letters, Vol. 87, Issue 15 https://doi.org/10.1103/PhysRevLett.87.155501	journal	September 2001
Linac Coherent Light Source: The first five years Bostedt, Christoph; Boutet, Sébastien; Fritz, David M. Reviews of Modern Physics, Vol. 88, Issue 1 https://doi.org/10.1103/RevModPhys.88.015007	journal	March 2016
Design and performance of an ultra-high-vacuum-compatible artificial channel-cut monochromator Narayanan, Suresh; Sandy, Alec; Shu, Deming Journal of Synchrotron Radiation, Vol. 15, Issue 1 https://doi.org/10.1107/S090904950705340X	journal	December 2007
The X-ray Correlation Spectroscopy instrument at the Linac Coherent Light Source Alonso-Mori, Roberto; Caronna, Chiara; Chollet, Matthieu Journal of Synchrotron Radiation, Vol. 22, Issue 3 https://doi.org/10.1107/S1600577515004397	journal	April 2015
The X-ray Pump–Probe instrument at the Linac Coherent Light Source Chollet, Matthieu; Alonso-Mori, Roberto; Cammarata, Marco Journal of Synchrotron Radiation, Vol. 22, Issue 3 https://doi.org/10.1107/S1600577515005135	journal	April 2015
Anisotropy enhanced X-ray scattering from solvated transition metal complexes Biasin, Elisa; van Driel, Tim B.; Levi, Gianluca Journal of Synchrotron Radiation, Vol. 25, Issue 2 https://doi.org/10.1107/S1600577517016964	journal	February 2018
The Macromolecular Femtosecond Crystallography Instrument at the Linac Coherent Light Source Sierra, Raymond G.; Batyuk, Alexander; Sun, Zhibin Journal of Synchrotron Radiation, Vol. 26, Issue 2 https://doi.org/10.1107/S1600577519001577	journal	February 2019
Pump–probe experimental methodology at the Linac Coherent Light Source Glownia, James M.; Gumerlock, Karl; Lemke, Henrik T. Journal of Synchrotron Radiation, Vol. 26, Issue 3 https://doi.org/10.1107/S160057751900225X	journal	April 2019
The ePix10k 2-megapixel hard X-ray detector at LCLS van Driel, Tim Brandt; Nelson, Silke; Armenta, Rebecca Journal of Synchrotron Radiation, Vol. 27, Issue 3 https://doi.org/10.1107/S1600577520004257	journal	April 2020
The Cornell-SLAC pixel array detector at LCLS Hart, P.; Boutet, S.; Carini, G. 2012 IEEE Nuclear Science Symposium and Medical Imaging Conference (2012 NSS/MIC), 2012 IEEE Nuclear Science Symposium and Medical Imaging Conference Record (NSS/MIC) https://doi.org/10.1109/NSSMIC.2012.6551166	conference	October 2012
Studies of the ePix100 low-noise x-ray camera at SLAC Carini, G. A.; Alonso-Mori, R.; Blaj, G. 2014 IEEE Nuclear Science Symposium and Medical Imaging Conference (NSS/MIC) https://doi.org/10.1109/NSSMIC.2014.7431079	conference	November 2014
Time-Resolved X-ray Absorption Spectroscopy of Carbon Monoxide-Myoglobin Recombination After Laser Photolysis Mills, D. M.; Lewis, A.; Harootunian, A. Science, Vol. 223, Issue 4638 https://doi.org/10.1126/science.223.4638.811	journal	February 1984
Metalloprotein entatic control of ligand-metal bonds quantified by ultrafast x-ray spectroscopy Mara, Michael W.; Hadt, Ryan G.; Reinhard, Marco Eli Science, Vol. 356, Issue 6344 https://doi.org/10.1126/science.aam6203	journal	June 2017
Spectral encoding of x-ray/optical relative delay Bionta, Mina R.; Lemke, H. T.; Cryan, J. P. Optics Express, Vol. 19, Issue 22 https://doi.org/10.1364/OE.19.021855	journal	January 2011
Megahertz x-ray microscopy at x-ray free-electron laser and synchrotron sources Vagovič, Patrik; Sato, Tokushi; Mikeš, Ladislav Optica, Vol. 6, Issue 9 https://doi.org/10.1364/OPTICA.6.001106	journal	January 2019
Light-Induced Relaxation of Photolyzed Carbonmonoxy Myoglobin: A Temperature-Dependent X-Ray Absorption Near-Edge Structure (XANES) Study Arcovito, A.; Lamb, D. C.; Nienhaus, G. U. Biophysical Journal, Vol. 88, Issue 4 https://doi.org/10.1529/biophysj.104.054973	journal	April 2005
Microfluidic liquid sheets as large-area targets for high repetition XFELs Hoffman, David J.; Van Driel, Tim B.; Kroll, Thomas Frontiers in Molecular Biosciences, Vol. 9 https://doi.org/10.3389/fmolb.2022.1048932	journal	December 2022
Ultrafast X-ray Photochemistry at European XFEL: Capabilities of the Femtosecond X-ray Experiments (FXE) Instrument Khakhulin, Dmitry; Otte, Florian; Biednov, Mykola Applied Sciences, Vol. 10, Issue 3 https://doi.org/10.3390/app10030995	journal	February 2020

Similar Records

The DREAM Endstation at the Linac Coherent Light Source

Journal Article · Tue Oct 18 20:00:00 EDT 2022 · Applied Sciences · OSTI ID:1894259

A Flat Analyzer Polycapillary Spectrometer for X-ray Absorption Spectroscopy of Dilute Transition Metals at X-ray-Free Electron Lasers

Journal Article · Sat Dec 13 19:00:00 EST 2025 · Photon Science · OSTI ID:3024710

XANES and EXAFS of dilute solutions of transition metals at XFELs

Journal Article · Wed Aug 07 00:00:00 EDT 2019 · Journal of Synchrotron Radiation (Online) · OSTI ID:1598524

Related Subjects

EXAFS
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
47 OTHER INSTRUMENTATION
74 ATOMIC AND MOLECULAR PHYSICS
X-ray absorption spectroscopy
X-ray diffraction
X-ray emission spectroscopy
X-ray scattering
XANES
XFEL
biochemistry
photochemistry
time-resolved X-ray studies

The Liquid Jet Endstation for Hard X-ray Scattering and Spectroscopy at the Linac Coherent Light Source

Citation Formats

References (65)

Similar Records

Related Subjects