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

J Synchrotron Radiat. 2022 Jul 1;29(Pt 4):1014-1019. doi: 10.1107/S1600577522005136. Epub 2022 May 25.

Abstract

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.

Keywords: 3D printing; cyclic olefin copolymer; in situ dialysis; in-house measurements; small-angle X-ray scattering.

MeSH terms

  • Printing, Three-Dimensional*
  • Renal Dialysis*
  • Scattering, Small Angle
  • X-Ray Diffraction
  • X-Rays