Serial small- and wide-angle X-ray scattering with laboratory sources

Mark A Levenstein; Karen Robertson; Thomas D Turner; Liam Hunter; Cate O'Brien; Cedrick O'Shaughnessy; Alexander N Kulak; Pierre Le Magueres; Jakub Wojciechowski; Oleksandr O Mykhaylyk; Nikil Kapur; Fiona C Meldrum

doi:10.1107/S2052252522007631

Serial small- and wide-angle X-ray scattering with laboratory sources

IUCrJ. 2022 Aug 13;9(Pt 5):538-543. doi: 10.1107/S2052252522007631. eCollection 2022 Sep 1.

Affiliations

¹ Université Paris-Saclay, CEA, CNRS, NIMBE, 91191 Gif-sur-Yvette, France.
² Department of Chemical and Environmental Engineering, University of Nottingham, University Park, Nottingham NG7 2RD, United Kingdom.
³ School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, United Kingdom.
⁴ Soft Matter Analytical Laboratory, Department of Chemistry, The University of Sheffield, Brook Hill, Sheffield S3 7HF, United Kingdom.
⁵ Rigaku Americas Corporation, 9009 New Tails Drive, The Woodlands, TX 77381, USA.
⁶ Rigaku Europe SE, Hugenottenallee 167, Neu-Isenburg 63263, Germany.
⁷ School of Mechanical Engineering, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, United Kingdom.

Abstract

Recent advances in X-ray instrumentation and sample injection systems have enabled serial crystallography of protein nanocrystals and the rapid structural analysis of dynamic processes. However, this progress has been restricted to large-scale X-ray free-electron laser (XFEL) and synchrotron facilities, which are often oversubscribed and have long waiting times. Here, we explore the potential of state-of-the-art laboratory X-ray systems to perform comparable analyses when coupled to micro- and millifluidic sample environments. Our results demonstrate that commercial small- and wide-angle X-ray scattering (SAXS/WAXS) instruments and X-ray diffractometers are ready to access samples and timescales (≳5 ms) relevant to many processes in materials science including the preparation of pharmaceuticals, nanoparticles and functional crystalline materials. Tests of different X-ray instruments highlighted the importance of the optical configuration and revealed that serial WAXS/XRD analysis of the investigated samples was only possible with the higher flux of a microfocus setup. We expect that these results will also stimulate similar developments for structural biology.

Keywords: crystallization; microfluidics; rapid structural analysis; serial SAXS; serial WAXS.

Grants and funding

The authors acknowledge the Engineering and Physical Sciences Research Council UK (EPSRC) for funding a Strategic Equipment Grant for Flow-Xl (grant No. EP/T006331/1 supporting KR, NK, FCM and TT) and a Programme Grant which funds the Crystallization in the Real World Consortium (grant No. EP/R018820/1 supporting CO’S and FCM). This project also received funding from the European Research Council (ERC) under the project DYNAMIN, (grant No. 788968). OOM thanks the EPSRC for the capital equipment grant to purchase the Xeuss 2.0 SAXS/WAXS Laboratory Beamline (grant No. EP/M028437/1).