Journal of Synchrotron Radiation (Jul 2022)

3D-printed SAXS chamber for controlled in situ dialysis and optical characterization

  • Tamara Ehm,
  • Julian Philipp,
  • Martin Barkey,
  • Martina Ober,
  • Achim Theo Brinkop,
  • David Simml,
  • Miriam von Westphalen,
  • Bert Nickel,
  • Roy Beck,
  • Joachim O. Rädler

DOI
https://doi.org/10.1107/S1600577522005136
Journal volume & issue
Vol. 29, no. 4
pp. 1014 – 1019

Abstract

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3D printing changes the scope of how samples can be mounted for small-angle X-ray scattering (SAXS). In this paper a 3D-printed X-ray chamber, which allows for in situ exchange of buffer and in situ optical transmission spectroscopy, is presented. The chamber is made of cyclic olefin copolymers (COC), including COC X-ray windows providing ultra-low SAXS background. The design integrates a membrane insert for in situ dialysis of the 100 µl sample volume against a reservoir, which enables measurements of the same sample under multiple conditions using an in-house X-ray setup equipped with a 17.4 keV molybdenum source. The design's capabilities are demonstrated by measuring reversible structural changes in lipid and polymer systems as a function of salt concentration and pH. In the same chambers optical light transmission spectroscopy was carried out measuring the optical turbidity of the mesophases and local pH values using pH-responsive dyes. Microfluidic exchange and optical spectroscopy combined with in situ X-ray scattering enables vast applications for the study of responsive materials.

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