Sample holder for small-angle x-ray scattering static and flow cell measurements

Results are presented for anin situsynchrotron-based ultra-small-angle X-ray scattering (USAXS) study of the solution-mediated formation and growth of nanocrystalline ceria (n-CeO2) using a new remote-controlled, isothermal, circulating fluid flow cell. The fluid flow mitigates or reduces X-ray beam-induced damage, air bubbles or particulate flocculation within the bulk solution, but prevents any coarse particulates that do form from settling out from suspension. Combined with the large-scale range accessible in USAXS studies, the flow cell has enabled measurement,in situand in real time, of structural characteristics from 10 Å to a few micrometres in size as a function of the changing physical and chemical conditions. By applying a multi-component model, the nanoparticle formation and growth component has been identified. Control and online monitoring of flow rate, temperature and pH suspension conditions have permitted real-time studies of the formation and growth of the individual n-CeO2particles from homogeneous dilute solution over several hours. Aspects of the nanoparticle nucleation and growth are revealed that have not been observed directly in measurements on this system.

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Construction of the Sample Holder and Small-Angle X-ray Scattering Measurement for Supercritical Water

Japanese Journal of Applied Physics ◽

10.1143/jjap.37.l768 ◽

1998 ◽

Vol 37 (Part 2, No. 7A) ◽

pp. L768-L770 ◽

Cited By ~ 8

Author(s):

Takeshi Morita ◽

Hiroshi Miyagi ◽

Yuji Shimokawa ◽

Hitoshi Matsuo ◽

Keiko Nishikawa

Keyword(s):

Supercritical Water ◽

Small Angle ◽

Sample Holder ◽

X Ray ◽

X Ray Scattering ◽

Scattering Measurement ◽

Ray Scattering

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Volume-variable sample holder for small-angle x-ray scattering measurements of supercritical solutions and its application to the CHF3–CO2 mixture

Review of Scientific Instruments ◽

10.1063/1.1858580 ◽

2005 ◽

Vol 76 (3) ◽

pp. 033902 ◽

Cited By ~ 3

Author(s):

Takeshi Morita ◽

Tomoko Masakawa ◽

Asako Ayusawa Arai ◽

Masato Nakagawa ◽

Keiko Nishikawa

Keyword(s):

Small Angle ◽

Sample Holder ◽

X Ray ◽

X Ray Scattering ◽

Scattering Measurements ◽

Supercritical Solutions ◽

Ray Scattering

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Small-Angle X-ray Scattering Measurements of Ionic Liquids Pressurized with Carbon Dioxide Using Titanium Sample Holder: 1-Butyl-3-methylimidazolium Bis(trifluoromethylsulfonyl) Amide Mixtures up to 22 MPa

Japanese Journal of Applied Physics ◽

10.7567/jjap.51.076703 ◽

2012 ◽

Vol 51 (7R) ◽

pp. 076703 ◽

Cited By ~ 10

Author(s):

Takeshi Morita ◽

Masayoshi Ushio ◽

Kaori Kanoh ◽

Eiichi Tanaka ◽

Keiko Nishikawa

Keyword(s):

Carbon Dioxide ◽

Ionic Liquids ◽

Small Angle ◽

Sample Holder ◽

Titanium Sample ◽

X Ray ◽

X Ray Scattering ◽

Scattering Measurements ◽

Ray Scattering

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

Journal of Applied Crystallography ◽

10.1107/s0021889812000957 ◽

2012 ◽

Vol 45 (2) ◽

pp. 213-223 ◽

Cited By ~ 48

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.

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A Revised O2 Reduction Model in Li-O2 Batteries as Revealed by in Situ Small Angle X-Ray Scattering

10.26434/chemrxiv.11447775.v1 ◽

2019 ◽

Author(s):

Christian Prehal ◽

Aleksej Samojlov ◽

Manfred Nachtnebel ◽

Manfred Kriechbaum ◽

Heinz Amenitsch ◽

...

Keyword(s):

Small Angle ◽

Wide Angle ◽

Reduction Mechanism ◽

Reduction Model ◽

X Ray ◽

X Ray Scattering ◽

O2 Reduction ◽

Ray Scattering

Here we use in situ small and wide angle X-ray scattering to elucidate unexpected mechanistic insights of the O2 reduction mechanism in Li-O2 batteries.

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In situ Time-Resolved Small-Angle X-ray Scattering Reveals the Formation Kinetics of Polyelectrolyte Complex Micelles

10.26434/chemrxiv.9876395.v1 ◽

2019 ◽

Author(s):

Hao Wu ◽

Jeffrey Ting ◽

Siqi Meng ◽

Matthew Tirrell

Keyword(s):

Small Angle ◽

Self Assembly ◽

Electrostatic Interactions ◽

Polyelectrolyte Complex ◽

Time Resolved ◽

X Ray ◽

X Ray Scattering ◽

Kinetics Of ◽

Ray Scattering

We have directly observed the in situ self-assembly kinetics of polyelectrolyte complex (PEC) micelles by synchrotron time-resolved small-angle X-ray scattering, equipped with a stopped-flow device that provides millisecond temporal resolution. This work has elucidated one general kinetic pathway for the process of PEC micelle formation, which provides useful physical insights for increasing our fundamental understanding of complexation and self-assembly dynamics driven by electrostatic interactions that occur on ultrafast timescales.

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