Faculty of Natural Sciences

TY - JOUR

T1 - A high-flux automated laboratory small-angle X-ray scattering instrument optimized for solution scattering

AU - Lyngsø, Jeppe

AU - Pedersen, Jan Skov

PY - 2021/2

Y1 - 2021/2

N2 - A commercially available small-angle X-ray scattering (SAXS) NanoSTAR instrument (Bruker AXS) with a liquid-metal-jet source (Excillum) has been optimized for solution scattering and installed at iNANO at Aarhus University. The instrument (named HyperSAXS) employs long high-quality parabolic Montel multilayer optics (Incoatec) and a novel compact scatterless pinhole slit with Ge edges, which was designed and built at Aarhus University. The combination of the powerful source and optimized geometry gives an integrated X-ray intensity close to 109photonss-1 for a standard range of scattering vector moduli q = 0.0098-0.425Å-1, where q = (4πsinθ)/λ and λ is the GaK wavelength of 1.34Å. The high intensity of the instrument makes it possible to measure dilute samples of, for example, protein or surfactant with concentrations of 1mgml-1 in a few minutes. A flow-through cell, built at Aarhus University, in combination with an automated sample handler has been installed on the instrument. The sample handler is based on the commercial Gilson GX-271 injection system (Biolab), which also allows samples to be stored under thermostatted conditions. The sample handler inserts and removes samples, and also cleans and dries the sample cell between measurements. The minimum volume of the flow-through capillary is about 20μl. The high intensity additionally allows time-resolved measurements to be performed with a temporal resolution of seconds. For this purpose a stopped-flow apparatus, (SFM-3000, Bio-Logic) was connected to the flow-through cell by high-performance liquid chromatography tubing. This configuration was chosen as it allows vacuum around the sample cell and thus maintains a low background. The instrument can readily be converted into a low-q setup with a q range of 0.0049-0.34Å-1 and an X-ray intensity of about 5×107photonss-1.

AB - A commercially available small-angle X-ray scattering (SAXS) NanoSTAR instrument (Bruker AXS) with a liquid-metal-jet source (Excillum) has been optimized for solution scattering and installed at iNANO at Aarhus University. The instrument (named HyperSAXS) employs long high-quality parabolic Montel multilayer optics (Incoatec) and a novel compact scatterless pinhole slit with Ge edges, which was designed and built at Aarhus University. The combination of the powerful source and optimized geometry gives an integrated X-ray intensity close to 109photonss-1 for a standard range of scattering vector moduli q = 0.0098-0.425Å-1, where q = (4πsinθ)/λ and λ is the GaK wavelength of 1.34Å. The high intensity of the instrument makes it possible to measure dilute samples of, for example, protein or surfactant with concentrations of 1mgml-1 in a few minutes. A flow-through cell, built at Aarhus University, in combination with an automated sample handler has been installed on the instrument. The sample handler is based on the commercial Gilson GX-271 injection system (Biolab), which also allows samples to be stored under thermostatted conditions. The sample handler inserts and removes samples, and also cleans and dries the sample cell between measurements. The minimum volume of the flow-through capillary is about 20μl. The high intensity additionally allows time-resolved measurements to be performed with a temporal resolution of seconds. For this purpose a stopped-flow apparatus, (SFM-3000, Bio-Logic) was connected to the flow-through cell by high-performance liquid chromatography tubing. This configuration was chosen as it allows vacuum around the sample cell and thus maintains a low background. The instrument can readily be converted into a low-q setup with a q range of 0.0049-0.34Å-1 and an X-ray intensity of about 5×107photonss-1.

KW - X-rays

KW - scattering

KW - small-angle X-ray scattering

KW - SAXS

KW - automation

KW - Protein structure

KW - SOLUTION SCATTERING

KW - Optimisation

KW - beamstop

KW - scatterless slits

KW - two-pinhole collimation

KW - stopped-flow

KW - Time-resolved

KW - solution scattering

KW - timeresolved studies.

KW - protein structure

KW - beamstops

KW - optimization

KW - stopped-flow apparatus

KW - SYSTEM

KW - BLOCK-COPOLYMER MICELLES

KW - WATER

KW - BIOLOGICAL MACROMOLECULES

KW - time-resolved studies

KW - MODULE

KW - PROTEINS

KW - POLY(ETHYLENE OXIDE)

KW - AGGREGATION

KW - BOVINE SERUM-ALBUMIN

U2 - 10.1107/S1600576720016209

DO - 10.1107/S1600576720016209

M3 - Journal article

VL - 54

SP - 295

EP - 305

JO - Journal of Applied Crystallography

JF - Journal of Applied Crystallography

SN - 0021-8898

IS - Part 1

ER -