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.

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.

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 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

scholarly journals Synthesis and Advanced Characterization of Polymer-Protein Core-Shell Nanoparticles

Catalysts ◽  
2021 ◽  
Vol 11 (6) ◽  
pp. 730
Author(s):  
Erik Sarnello ◽  
Tao Li
Keyword(s):  
Particle Size ◽  
Small Angle ◽  
Core Shell ◽  
Assembly Process ◽  
Shell Nanoparticles ◽  
X Ray ◽  
X Ray Scattering ◽  
Wide Range ◽  
Core Shell Nanoparticles ◽  
Ray Scattering

Enzyme immobilization techniques are widely researched due to their wide range of applications. Polymer–protein core–shell nanoparticles (CSNPs) have emerged as a promising technique for enzyme/protein immobilization via a self-assembly process. Based on the desired application, different sizes and distribution of the polymer–protein CSNPs may be required. This work systematically studies the assembly process of poly(4-vinyl pyridine) and bovine serum albumin CSNPs. Average particle size was controlled by varying the concentrations of each reagent. Particle size and size distributions were monitored by dynamic light scattering, ultra-small-angle X-ray scattering, small-angle X-ray scattering and transmission electron microscopy. Results showed a wide range of CSNPs could be assembled ranging from an average radius as small as 52.3 nm, to particles above 1 µm by adjusting reagent concentrations. In situ X-ray scattering techniques monitored particle assembly as a function of time showing the initial particle growth followed by a decrease in particle size as they reach equilibrium. The results outline a general strategy that can be applied to other CSNP systems to better control particle size and distribution for various applications.

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.

scholarly journals The new NCPSS BL19U2 beamline at the SSRF for small-angle X-ray scattering from biological macromolecules in solution

2016 ◽  
Vol 49 (5) ◽  
pp. 1428-1432 ◽  
Author(s):  
Na Li ◽  
Xiuhong Li ◽  
Yuzhu Wang ◽  
Guangfeng Liu ◽  
Ping Zhou ◽  
...  
Keyword(s):  
Data Processing ◽  
Small Angle ◽  
Dynamic Range ◽  
Silicon Crystal ◽  
High Dynamic Range ◽  
Biological Macromolecules ◽  
Shanghai Synchrotron Radiation Facility ◽  
X Ray ◽  
X Ray Scattering ◽  
Ray Scattering

The beamline BL19U2 is located in the Shanghai Synchrotron Radiation Facility (SSRF) and is its first beamline dedicated to biological material small-angle X-ray scattering (BioSAXS). The electrons come from an undulator which can provide high brilliance for the BL19U2 end stations. A double flat silicon crystal (111) monochromator is used in BL19U2, with a tunable monochromatic photon energy ranging from 7 to 15 keV. To meet the rapidly growing demands of crystallographers, biochemists and structural biologists, the BioSAXS beamline allows manual and automatic sample loading/unloading. A Pilatus 1M detector (Dectris) is employed for data collection, characterized by a high dynamic range and a short readout time. The highly automated data processing pipeline SASFLOW was integrated into BL19U2, with help from the BioSAXS group of the European Molecular Biology Laboratory (EMBL, Hamburg), which provides a user-friendly interface for data processing. The BL19U2 beamline was officially opened to users in March 2015. To date, feedback from users has been positive and the number of experimental proposals at BL19U2 is increasing. A description of the new BioSAXS beamline and the setup characteristics is given, together with examples of data obtained.

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

SGTools: a suite of tools for processing and analyzing large data sets from in situ X-ray scattering experiments

2022 ◽  
Vol 55 (1) ◽  
Author(s):  
Nie Zhao ◽  
Chunming Yang ◽  
Fenggang Bian ◽  
Daoyou Guo ◽  
Xiaoping Ouyang
Keyword(s):  
Data Processing ◽  
Small Angle ◽  
Large Data ◽  
Large Data Sets ◽  
Data Sets ◽  
X Ray ◽  
Intensity Mapping ◽  
X Ray Scattering ◽  
Ray Scattering

In situ synchrotron small-angle X-ray scattering (SAXS) is a powerful tool for studying dynamic processes during material preparation and application. The processing and analysis of large data sets generated from in situ X-ray scattering experiments are often tedious and time consuming. However, data processing software for in situ experiments is relatively rare, especially for grazing-incidence small-angle X-ray scattering (GISAXS). This article presents an open-source software suite (SGTools) to perform data processing and analysis for SAXS and GISAXS experiments. The processing modules in this software include (i) raw data calibration and background correction; (ii) data reduction by multiple methods; (iii) animation generation and intensity mapping for in situ X-ray scattering experiments; and (iv) further data analysis for the sample with an order degree and interface correlation. This article provides the main features and framework of SGTools. The workflow of the software is also elucidated to allow users to develop new features. Three examples are demonstrated to illustrate the use of SGTools for dealing with SAXS and GISAXS data. Finally, the limitations and future features of the software are also discussed.

scholarly journals X-ray Metrology for the SemiconductorIndustry Tutorial

2019 ◽  
Vol 124 ◽  
Author(s):  
Daniel F. Sunday ◽  
Wen-li Wu ◽  
Scott Barton ◽  
R. Joseph Kline
Keyword(s):  
Data Processing ◽  
Small Angle ◽  
Semiconductor Industry ◽  
Critical Dimension ◽  
Next Generation ◽  
Dimensional Metrology ◽  
X Ray ◽  
X Ray Scattering ◽  
Short Course ◽  
Ray Scattering

The semiconductor industry is in need of new, in-line dimensional metrology methods with higherspatial resolution for characterizing their next generation nanodevices. The purpose of this short course is to train the semiconductor industry on the NIST-developed critical dimension small angle X-ray scattering (CDSAXS) method. The topics will include both data processing and instrumentation. The short course will also provide an opportunity for discussion of the requirements for CDSAXS and the necessary improvements in X-ray source technology. Expected audience include semiconductor manufacturers, equipment manufacturers, and component manufacturers. The presentations were made at “X-ray Metrology for the Semiconductor Industry” short course at the National Institute of Standards and Technology on Aug. 25, 2016.

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