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Ehm, Tamara; Philipp, Julian; Barkey, Martin; Ober, Martina; Brinkop, Achim Theo; Simml, David; Westphalen, Miriam von; Nickel, Bert; Beck, Roy und Rädler, Joachim O. (2022): 3D-printed SAXS chamber for controlled in situ dialysis and optical characterization. In: Journal of Synchrotron Radiation, Bd. 29: S. 1014-1019 [PDF, 837kB]

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 ml 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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