scholarly journals High-pressure small-angle X-ray scattering cell for biological solutions and soft materials

2021 ◽  
Vol 54 (1) ◽  
Author(s):  
Durgesh K. Rai ◽  
Richard E. Gillilan ◽  
Qingqiu Huang ◽  
Robert Miller ◽  
Edmund Ting ◽  
...  
Keyword(s):  
High Pressure ◽  
Small Angle ◽  
High Pressures ◽  
Protein Denaturation ◽  
Soft Materials ◽  
High Energy ◽  
Synchrotron Source ◽  
X Ray ◽  
X Ray Scattering ◽  
Ray Scattering

Pressure is a fundamental thermodynamic parameter controlling the behavior of biological macromolecules. Pressure affects protein denaturation, kinetic parameters of enzymes, ligand binding, membrane permeability, ion transduction, expression of genetic information, viral infectivity, protein association and aggregation, and chemical processes. In many cases pressure alters the molecular shape. Small-angle X-ray scattering (SAXS) is a primary method to determine the shape and size of macromolecules. However, relatively few SAXS cells described in the literature are suitable for use at high pressures and with biological materials. Described here is a novel high-pressure SAXS sample cell that is suitable for general facility use by prioritization of ease of sample loading, temperature control, mechanical stability and X-ray background minimization. Cell operation at 14 keV is described, providing a q range of 0.01 < q < 0.7 Å−1, pressures of 0–400 MPa and an achievable temperature range of 0–80°C. The high-pressure SAXS cell has recently been commissioned on the ID7A beamline at the Cornell High Energy Synchrotron Source and is available to users on a peer-reviewed proposal basis.

scholarly journals High-throughput biological small-angle X-ray scattering with a robotically loaded capillary cell

2012 ◽  
Vol 45 (2) ◽  
pp. 213-223 ◽  
Author(s):  
S. S. Nielsen ◽  
M. Møller ◽  
R. E. Gillilan
Keyword(s):  
Data Processing ◽  
Small Angle ◽  
High Energy ◽  
Flow Cell ◽  
Creeping Flow ◽  
Synchrotron Source ◽  
X Ray ◽  
X Ray Scattering ◽  
Wide Range ◽  
Ray Scattering

With the rise in popularity of biological small-angle X-ray scattering (BioSAXS) measurements, synchrotron beamlines are confronted with an ever-increasing number of samples from a wide range of solution conditions. To meet these demands, an increasing number of beamlines worldwide have begun to provide automated liquid-handling systems for sample loading. This article presents an automated sample-loading system for BioSAXS beamlines, which combines single-channel disposable-tip pipetting with a vacuum-enclosed temperature-controlled capillary flow cell. The design incorporates an easily changeable capillary to reduce the incidence of X-ray window fouling and cross contamination. Both the robot-control and the data-processing systems are written in Python. The data-processing code,RAW, has been enhanced with several new features to form a user-friendly BioSAXS pipeline for the robot. The flow cell also supports efficient manual loading and sample recovery. An effective rinse protocol for the sample cell is developed and tested. Fluid dynamics within the sample capillary reveals a vortex ring pattern of circulation that redistributes radiation-damaged material. Radiation damage is most severe in the boundary layer near the capillary surface. At typical flow speeds, capillaries below 2 mm in diameter are beginning to enter the Stokes (creeping flow) regime in which mixing due to oscillation is limited. Analysis within this regime shows that single-pass exposure and multiple-pass exposure of a sample plug are functionally the same with regard to exposed volume when plug motion reversal is slow. The robot was tested on three different beamlines at the Cornell High-Energy Synchrotron Source, with a variety of detectors and beam characteristics, and it has been used successfully in several published studies as well as in two introductory short courses on basic BioSAXS methods.

Small-angle X-ray scattering at high energies

1990 ◽  
Vol 23 (5) ◽  
pp. 401-405 ◽  
Author(s):  
D. P. Siddons ◽  
C. Riekel ◽  
J. B. Hastings
Keyword(s):  
High Pressure ◽  
Phase Separation ◽  
Small Angle ◽  
High Energy ◽  
Perfect Crystal ◽  
Resolution Function ◽  
X Ray ◽  
High Energies ◽  
X Ray Scattering ◽  
Ray Scattering

Initial tests are described of a high-resolution small-angle X-ray scattering apparatus adapted for operation at high photon energies. The energy chosen was 50 keV, and was limited by the available source. All orders of scattering out to the seventh were observed from a sample of 0.9 μm diameter latex spheres in a 4 h experiment. Phase separation in a binary Al–Li alloy was studied by the observation of spherical Al3Li precipitates. This demonstrates that the use of perfect-crystal collimators and analyzers yields a resolution function which does not depend on photon energy. New sources of high-energy photons will make such an apparatus invaluable for the study of highly absorbing samples, or samples in difficult environments such as ovens or high-pressure cells.

scholarly journals Focusing capillary optics for use in solution small-angle X-ray scattering

2007 ◽  
Vol 40 (1) ◽  
pp. 193-195 ◽  
Author(s):  
Jessica S. Lamb ◽  
Sterling Cornaby ◽  
Kurt Andresen ◽  
Lisa Kwok ◽  
Hye Yoon Park ◽  
...  
Keyword(s):  
Small Angle ◽  
Small Volume ◽  
Spot Size ◽  
High Energy ◽  
Synchrotron Source ◽  
X Ray ◽  
X Ray Scattering ◽  
Capillary Optics ◽  
Microfluidic Mixers ◽  
Ray Scattering

Measurements of the global conformation of macromolecules can be carried out using small-angle X-ray scattering (SAXS). Glass focusing capillaries, manufactured at the Cornell High Energy Synchrotron Source (CHESS), have been successfully employed for SAXS measurements on the heme protein cytochromec. These capillaries provide high X-ray flux into a spot size of tens of micrometres, permitting short exposures of small-volume samples. Such a capability is ideal for use in conjunction with microfluidic mixers, where time resolution may be determined by beam size and sample volumes are kept small to facilitate mixing and conserve material.

Mirror to measure small angle x-ray scattering signal in high energy density experiments

2020 ◽  
Vol 91 (12) ◽  
pp. 123501
Author(s):  
M. Šmíd ◽  
C. Baehtz ◽  
A. Pelka ◽  
A. Laso García ◽  
S. Göde ◽  
...  
Keyword(s):  
Energy Density ◽  
Small Angle ◽  
High Energy ◽  
High Energy Density ◽  
X Ray ◽  
X Ray Scattering ◽  
Scattering Signal ◽  
Ray Scattering

A multi-length-scale USAXS/SAXS facility: 10–50 keV small-angle X-ray scattering instrument

2013 ◽  
Vol 46 (5) ◽  
pp. 1508-1512 ◽  
Author(s):  
Byron Freelon ◽  
Kamlesh Suthar ◽  
Jan Ilavsky
Keyword(s):  
Small Angle ◽  
Soft Matter ◽  
High Energy ◽  
X Rays ◽  
X Ray ◽  
X Ray Scattering ◽  
Wide Range ◽  
And Performance ◽  
New Facility ◽  
Ray Scattering

Coupling small-angle X-ray scattering (SAXS) and ultra-small-angle X-ray scattering (USAXS) provides a powerful system of techniques for determining the structural organization of nanostructured materials that exhibit a wide range of characteristic length scales. A new facility that combines high-energy (HE) SAXS and USAXS has been developed at the Advanced Photon Source (APS). The application of X-rays across a range of energies, from 10 to 50 keV, offers opportunities to probe structural behavior at the nano- and microscale. An X-ray setup that can characterize both soft matter or hard matter and high-Zsamples in the solid or solution forms is described. Recent upgrades to the Sector 15ID beamline allow an extension of the X-ray energy range and improved beam intensity. The function and performance of the dedicated USAXS/HE-SAXS ChemMatCARS-APS facility is described.

Influence of high energy electron irradiation on the network structure of gelatin hydrogels as investigated by small-angle X-ray scattering (SAXS)

2017 ◽  
Vol 19 (19) ◽  
pp. 12064-12074 ◽  
Author(s):  
Emilia I. Wisotzki ◽  
Paolo Tempesti ◽  
Emiliano Fratini ◽  
Stefan G. Mayr
Keyword(s):  
Electron Irradiation ◽  
Network Structure ◽  
Small Angle ◽  
High Energy ◽  
Energy Electron ◽  
High Energy Electron ◽  
X Ray ◽  
X Ray Scattering ◽  
Structural Differences ◽  
Ray Scattering

Small-angle X-ray scattering revealed ranging structural differences in physically entangled and irradiation-crosslinked gelatin hydrogels.

Probing evaporation induced assembly across a drying colloidal droplet using in situ small-angle X-ray scattering at the synchrotron source

Soft Matter ◽  
2014 ◽  
Vol 10 (10) ◽  
pp. 1621 ◽  
Author(s):  
D. Sen ◽  
J. Bahadur ◽  
S. Mazumder ◽  
G. Santoro ◽  
S. Yu ◽  
...  
Keyword(s):  
Small Angle ◽  
Synchrotron Source ◽  
X Ray ◽  
X Ray Scattering ◽  
Ray Scattering

scholarly journals Determination of nanostructure of liposomes containing two model drugs by X-ray scattering from a synchrotron source

2013 ◽  
Vol 20 (5) ◽  
pp. 721-728 ◽  
Author(s):  
Alexandr Nasedkin ◽  
Jan Davidsson ◽  
Mont Kumpugdee-Vollrath
Keyword(s):  
Experimental Data ◽  
Small Angle ◽  
Structural Parameters ◽  
Water Layer ◽  
Synchrotron Source ◽  
X Ray ◽  
X Ray Scattering ◽  
Extract Information ◽  
Ray Scattering

Small-angle X-ray scattering has been employed to study how the introduction of paracetamol and acetylsalicylic acid into a liposome bilayer system affects the system's nanostructure. An X-ray scattering model, developed for multilamellar liposome systems [Pabstet al.(2000),Phys. Rev. E,62, 4000–4009], has been used to fit the experimental data and to extract information on how structural parameters, such as the number and thickness of the bilayers of the liposomes, thickness of the water layer in between the bilayers, size and volume of the head and tail groups, are affected by the drugs and their concentration. Even though the experimental data reveal a complicated picture of the drug–bilayer interaction, they clearly show a correlation between nanostructure, drug and concentration in some aspects. The localization of the drugs in the bilayers is discussed.

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