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1. Megahertz pulse trains enable multi-hit serial femtosecond crystallography experiments at X-ray free electron lasers

Author

Susannah Holmes, Henry J. Kirkwood, Richard Bean, Klaus Giewekemeyer, Andrew V. Martin, Marjan Hadian-Jazi, Max O. Wiedorn, Dominik Oberthür, Hugh Marman, Luigi Adriano, Nasser Al-Qudami, Saša Bajt, Imrich Barák, Sadia Bari, Johan Bielecki, Sandor Brockhauser, Mathew A. Coleman, Francisco Cruz-Mazo, Cyril Danilevski, Katerina Dörner, Alfonso M. Gañán-Calvo, Rita Graceffa, Hans Fanghor, Michael Heymann, Matthias Frank, Alexander Kaukher, Yoonhee Kim, Bostjan Kobe, Juraj Knoška, Torsten Laurus, Romain Letrun, Luis Maia, Marc Messerschmidt, Markus Metz, Thomas Michelat, Grant Mills, Serguei Molodtsov, Diana C. F. Monteiro, Andrew J. Morgan, Astrid Münnich, Gisel E. Peña Murillo, Gianpietro Previtali, Adam Round, Tokushi Sato, Robin Schubert, Joachim Schulz, Megan Shelby, Carolin Seuring, Jonas A. Sellberg, Marcin Sikorski, Alessandro Silenzi, Stephan Stern, Jola Sztuk-Dambietz, Janusz Szuba, Martin Trebbin, Patrick Vagovic, Thomas Ve, Britta Weinhausen, Krzysztof Wrona, Paul Lourdu Xavier, Chen Xu, Oleksandr Yefanov, Keith A. Nugent, Henry N. Chapman, Adrian P. Mancuso, Anton Barty, Brian Abbey, and Connie Darmanin

Subjects
Science
Abstract

Free-electron lasers are capable of high repetition rates and it is assumed that protein crystals often do not survive the first X-ray pulse. Here the authors address these issues with a demonstration of multi-hit serial crystallography in which multiple FEL pulses interact with the sample without destroying it.

Published
2022
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2. Megahertz serial crystallography

Author

Max O. Wiedorn, Dominik Oberthür, Richard Bean, Robin Schubert, Nadine Werner, Brian Abbey, Martin Aepfelbacher, Luigi Adriano, Aschkan Allahgholi, Nasser Al-Qudami, Jakob Andreasson, Steve Aplin, Salah Awel, Kartik Ayyer, Saša Bajt, Imrich Barák, Sadia Bari, Johan Bielecki, Sabine Botha, Djelloul Boukhelef, Wolfgang Brehm, Sandor Brockhauser, Igor Cheviakov, Matthew A. Coleman, Francisco Cruz-Mazo, Cyril Danilevski, Connie Darmanin, R. Bruce Doak, Martin Domaracky, Katerina Dörner, Yang Du, Hans Fangohr, Holger Fleckenstein, Matthias Frank, Petra Fromme, Alfonso M. Gañán-Calvo, Yaroslav Gevorkov, Klaus Giewekemeyer, Helen Mary Ginn, Heinz Graafsma, Rita Graceffa, Dominic Greiffenberg, Lars Gumprecht, Peter Göttlicher, Janos Hajdu, Steffen Hauf, Michael Heymann, Susannah Holmes, Daniel A. Horke, Mark S. Hunter, Siegfried Imlau, Alexander Kaukher, Yoonhee Kim, Alexander Klyuev, Juraj Knoška, Bostjan Kobe, Manuela Kuhn, Christopher Kupitz, Jochen Küpper, Janine Mia Lahey-Rudolph, Torsten Laurus, Karoline Le Cong, Romain Letrun, P. Lourdu Xavier, Luis Maia, Filipe R. N. C. Maia, Valerio Mariani, Marc Messerschmidt, Markus Metz, Davide Mezza, Thomas Michelat, Grant Mills, Diana C. F. Monteiro, Andrew Morgan, Kerstin Mühlig, Anna Munke, Astrid Münnich, Julia Nette, Keith A. Nugent, Theresa Nuguid, Allen M. Orville, Suraj Pandey, Gisel Pena, Pablo Villanueva-Perez, Jennifer Poehlsen, Gianpietro Previtali, Lars Redecke, Winnie Maria Riekehr, Holger Rohde, Adam Round, Tatiana Safenreiter, Iosifina Sarrou, Tokushi Sato, Marius Schmidt, Bernd Schmitt, Robert Schönherr, Joachim Schulz, Jonas A. Sellberg, M. Marvin Seibert, Carolin Seuring, Megan L. Shelby, Robert L. Shoeman, Marcin Sikorski, Alessandro Silenzi, Claudiu A. Stan, Xintian Shi, Stephan Stern, Jola Sztuk-Dambietz, Janusz Szuba, Aleksandra Tolstikova, Martin Trebbin, Ulrich Trunk, Patrik Vagovic, Thomas Ve, Britta Weinhausen, Thomas A. White, Krzysztof Wrona, Chen Xu, Oleksandr Yefanov, Nadia Zatsepin, Jiaguo Zhang, Markus Perbandt, Adrian P. Mancuso, Christian Betzel, Henry Chapman, and Anton Barty

Subjects
Science
Abstract

The new European X-Ray Free-Electron Laser (EuXFEL) is the first XFEL that generates X-ray pulses with a megahertz inter-pulse spacing. Here the authors demonstrate that high-quality and damage-free protein structures can be obtained with the currently available 1.1 MHz repetition rate pulses using lysozyme as a test case and furthermore present a β-lactamase structure.

Published
2018
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3. Rapid sample delivery for megahertz serial crystallography at X-ray FELs

Author

Max O. Wiedorn, Salah Awel, Andrew J. Morgan, Kartik Ayyer, Yaroslav Gevorkov, Holger Fleckenstein, Nils Roth, Luigi Adriano, Richard Bean, Kenneth R. Beyerlein, Joe Chen, Jesse Coe, Francisco Cruz-Mazo, Tomas Ekeberg, Rita Graceffa, Michael Heymann, Daniel A. Horke, Juraj Knoška, Valerio Mariani, Reza Nazari, Dominik Oberthür, Amit K. Samanta, Raymond G. Sierra, Claudiu A. Stan, Oleksandr Yefanov, Dimitrios Rompotis, Jonathan Correa, Benjamin Erk, Rolf Treusch, Joachim Schulz, Brenda G. Hogue, Alfonso M. Gañán-Calvo, Petra Fromme, Jochen Küpper, Andrei V. Rode, Saša Bajt, Richard A. Kirian, and Henry N. Chapman

Subjects
X-ray free-electron lasers, FELs, X-ray FEL pulse trains, megahertz repetition rates, Crystallography, QD901-999
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. 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−1 was 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. The results indicate the feasibility for megahertz serial crystallography measurements with hard X-rays and give guidance for the design of such experiments.

Published
2018
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4. The Natural Breakup Length of a Steady Capillary Jet: Application to Serial Femtosecond Crystallography

Author

Alfonso M. Gañán-Calvo, Henry N. Chapman, Michael Heymann, Max O. Wiedorn, Juraj Knoska, Braulio Gañán-Riesco, José M. López-Herrera, Francisco Cruz-Mazo, Miguel A. Herrada, José M. Montanero, and Saša Bajt

Subjects
capillary jets, breakup length, flow focusing, capillary instability, Crystallography, QD901-999
Abstract

One of the most successful ways to introduce samples in Serial Femtosecond Crystallography has been the use of microscopic capillary liquid jets produced by gas flow focusing, whose length-to-diameter ratio and velocity are essential to fulfill the requirements of the high pulse rates of current XFELs. In this work, we demonstrate the validity of a classical scaling law with two universal constants to calculate that length as a function of the liquid properties and operating conditions. These constants are determined by fitting the scaling law to a large set of experimental and numerical measurements, including previously published data. Both the experimental and numerical jet lengths conform remarkably well to the proposed scaling law. We show that, while a capillary jet is a globally unstable system to linear perturbations above a critical length, its actual and shorter long-term average intact length is determined by the nonlinear perturbations coming from the jet breakup itself. Therefore, this length is determined solely by the properties of the liquid, the average velocity of the liquid and the flow rate expelled. This confirms the very early observations from Smith and Moss 1917, Proc R Soc Lond A Math Phys Eng, 93, 373, to McCarthy and Molloy 1974, Chem Eng J, 7, 1, among others, while it contrasts with the classical conception of temporal stability that attributes the natural breakup length to the jet birth conditions in the ejector or small interactions with the environment.

Published
2021
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5. Evaluation of serial crystallographic structure determination within megahertz pulse trains

Author

Oleksandr Yefanov, Dominik Oberthür, Richard Bean, Max O. Wiedorn, Juraj Knoska, Gisel Pena, Salah Awel, Lars Gumprecht, Martin Domaracky, Iosifina Sarrou, P. Lourdu Xavier, Markus Metz, Saša Bajt, Valerio Mariani, Yaroslav Gevorkov, Thomas A. White, Aleksandra Tolstikova, Pablo Villanueva-Perez, Carolin Seuring, Steve Aplin, Armando D. Estillore, Jochen Küpper, Alexander Klyuev, Manuela Kuhn, Torsten Laurus, Heinz Graafsma, Diana C. F. Monteiro, Martin Trebbin, Filipe R. N. C. Maia, Francisco Cruz-Mazo, Alfonso M. Gañán-Calvo, Michael Heymann, Connie Darmanin, Brian Abbey, Marius Schmidt, Petra Fromme, Klaus Giewekemeyer, Marcin Sikorski, Rita Graceffa, Patrik Vagovic, Thomas Kluyver, Martin Bergemann, Hans Fangohr, Jolanta Sztuk-Dambietz, Steffen Hauf, Natascha Raab, Valerii Bondar, Adrian P. Mancuso, Henry Chapman, and Anton Barty

Subjects
Crystallography, QD901-999
Abstract

The new European X-ray Free-Electron Laser (European XFEL) is the first X-ray free-electron laser capable of delivering intense X-ray pulses with a megahertz interpulse spacing in a wavelength range suitable for atomic resolution structure determination. An outstanding but crucial question is whether the use of a pulse repetition rate nearly four orders of magnitude higher than previously possible results in unwanted structural changes due to either radiation damage or systematic effects on data quality. Here, separate structures from the first and subsequent pulses in the European XFEL pulse train were determined, showing that there is essentially no difference between structures determined from different pulses under currently available operating conditions at the European XFEL.

Published
2019
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6. Aerodynamically stabilized Taylor cone jets

Author

Miguel A. Herrada, Max O. Wiedorn, Henry N. Chapman, Saša Bajt, Alfonso M. Gañán-Calvo, Francisco Cruz-Mazo, Universidad de Sevilla. Departamento de Ingeniería Aeroespacial y Mecánica de Fluidos, and Ministerio de Economía y Competitividad (MINECO). España

Subjects
Physics, Jet (fluid), Capillary action, Flow (psychology), Function (mathematics), Mechanics, 01 natural sciences, 010305 fluids & plasmas, Taylor cone, Acceleration, 0103 physical sciences, ddc:530, Electrohydrodynamics, 010306 general physics, Conservation of mass
Abstract

Physical review / E 100(3), 031101 (2019). doi:10.1103/PhysRevE.100.031101, We introduce a way to stabilize steady micro/nanoliquid jets issuing from Taylor cones together with coflowing gas streams. We study the dripping-jetting transition of this configuration theoretically through a global stability analysis as a function of the governing parameters involved. A balance between the local radial acceleration to the surface tension gradient, the mass conservation, and the energy balance equations enable us to derive two coupled scaling laws that predict both the minimum jet diameter and its maximum velocity. The theoretical prediction provides a single curve that describes not only the numerical computations but also experimental data from the literature for cone jets assisted with gas coflow. Additionally, we performed a set of experiments to verify what parameters influence the jet length. We adopt a very recent model for capillary jet length to our configuration by combining electrohydrodynamic effects with the gas flow through an equivalent liquid pressure. Due to diameters below 1 μm and high speeds attainable in excess of 100 m/s, this concept has the potential to be utilized for structural biology analyses with x-ray free-electron lasers at megahertz repetition rates as well as other applications., Published by APS, Woodbury, NY

Published
2019
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7. Pinch-off of liquid jets at the finite scale of an interface

Author

Francisco Cruz-Mazo and Howard A. Stone

Subjects
Physics::Fluid Dynamics, Fluid Flow and Transfer Processes, Modeling and Simulation, Computational Mechanics
Abstract

We derive self-similar continuum equationsthat govern the rupture of liquid threads at scales within the influence of interfacial dynamical effects. This regime and the obtained power-law solution for the evolution of the minimum neck radius,hmin=0.00107(tb−t)2.34, fill a void in the literature in between the classical inertial-viscous regime and the stochastic formulation and reconcile flow features such as asymptotic slow boundary conditions far away from the singularity and symmetric profiles, respectively. Due to its inherent ties to the production of monosized droplets from jetting, this work can be utilized to approach, for example, the study of electrosprays or flow focusing at these critical scales for aerospace nano-thruster technology or single-biomolecule imaging with x-ray free-electron lasers.

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