scholarly journals Photoreduction and validation of haem–ligand intermediate states in protein crystals byin situsingle-crystal spectroscopy and diffraction

IUCrJ ◽  
2017 ◽  
Vol 4 (3) ◽  
pp. 263-270 ◽  
Author(s):  
Demet Kekilli ◽  
Tadeo Moreno-Chicano ◽  
Amanda K. Chaplin ◽  
Sam Horrell ◽  
Florian S. N. Dworkowski ◽  
...  
Keyword(s):  
Crystal Structures ◽  
Structural Data ◽  
X Rays ◽  
Solvated Electrons ◽  
X Ray ◽  
Redox States ◽  
Density Maps ◽  
Correct Assignment ◽  
Wide Range

Powerful synergies are available from the combination of multiple methods to study proteins in the crystalline form. Spectroscopies which probe the same region of the crystal from which X-ray crystal structures are determined can give insights into redox, ligand and spin states to complement the information gained from the electron-density maps. The correct assignment of crystal structures to the correct protein redox and ligand states is essential to avoid the misinterpretation of structural data. This is a particular concern for haem proteins, which can occupy a wide range of redox states and are exquisitely sensitive to becoming reduced by solvated electrons generated from interactions of X-rays with water molecules in the crystal. Here, single-crystal spectroscopic fingerprinting has been applied to investigate the laser photoreduction of ferric haem in cytochromec′. Furthermore,in situX-ray-driven generation of haem intermediates in crystals of the dye-decolourizing-type peroxidase A (DtpA) fromStreptomyces lividansis described.

scholarly journals Colouring cryo-cooled crystals: online microspectrophotometry

2009 ◽  
Vol 16 (2) ◽  
pp. 163-172 ◽  
Author(s):  
John McGeehan ◽  
Raimond B. G. Ravelli ◽  
James W. Murray ◽  
Robin Leslie Owen ◽  
Florent Cipriani ◽  
...  
Keyword(s):  
High Temporal Resolution ◽  
Electromagnetic Spectrum ◽  
X Rays ◽  
X Ray Diffraction ◽  
High Concentration ◽  
Solvated Electrons ◽  
X Ray ◽  
Redox States ◽  
Wide Range ◽  
Kinetics Of

X-rays can produce a high concentration of radicals within cryo-cooled macromolecular crystals. Some radicals have large extinction coefficients in the visible (VIS) range of the electromagnetic spectrum, and can be observed optically and spectrally. An online microspectrophotometer with high temporal resolution has been constructed that is capable of measuring UV/VIS absorption spectra (200–1100 nm) during X-ray data collection. The typical X-ray-induced blue colour that is characteristic of a wide range of cryo-conditions has been identified as trapped solvated electrons. Disulphide-containing proteins are shown to form disulphide radicals at millimolar concentrations, with absorption maxima around 400 nm. The solvated electrons and the disulphide radicals seem to have a lifetime in the range of seconds up to minutes at 100 K. The temperature dependence of the kinetics of X-ray-induced radical formation is different for the solvated electrons compared with the disulphide radicals. The online microspectrophotometer provides a technique complementary to X-ray diffraction for analysing and characterizing intermediates and redox states of proteins and enzymes.

scholarly journals Development of a novel microfluidic device to study metal geochemistry in situ using X-ray fluorescence microprobe spectroscopy

2021 ◽  
Vol 28 (2) ◽  
pp. 461-471
Author(s):  
Michael A. Chen ◽  
Benjamin D. Kocar
Keyword(s):  
Microfluidic Device ◽  
Microfluidic System ◽  
X Rays ◽  
Thin Glass ◽  
X Ray ◽  
Wide Range ◽  
Etched Silicon ◽  
Materials Used ◽  
Energy Mapping

The study of in situ microscale biogeochemical processes represents a major challenge in the environmental sciences. The combination of microfluidic devices with X-ray fluorescence microprobe spectroscopy may address this need, but typical materials used in these devices attenuate the X-rays needed to analyze key elements of interest, such as Fe or As. In this work, a method is presented for fabricating an etched silicon microfluidic device that is sealed with a 30 µm thin glass window that is sufficiently transparent for X-ray fluorescence microprobe spectroscopy. The capabilities of these devices for X-ray microprobe spectroscopy are demonstrated using an Fe (hydr)oxide solid that is loaded with As and then infused with sulfide, on beamline 4-BM at NSLS-II, resulting in time-variant Fe precipitation reactions and As sorption. Key results include in situ X-ray fluorescence time-series maps of Fe, As and a Br flow tracer, as well as spot XANES at both the Fe K edge and As K edge. Additionally, multiple energy mapping is used to examine the spatial speciation of As over time. The results of this work clearly demonstrate the capabilities of this novel microfluidic system that can be analyzed using X-ray fluorescence microprobe spectroscopy and can be made to study a wide range of complex microscale geochemical systems.

In Situ Synchrotron Radiation Research in Materials Science

MRS Bulletin ◽  
1999 ◽  
Vol 24 (1) ◽  
pp. 13-20 ◽  
Author(s):  
Pedro A. Montano ◽  
Hiroyuki Oyanagi
Keyword(s):  
Synchrotron Radiation ◽  
Materials Science ◽  
X Rays ◽  
X Ray ◽  
Curved Trajectories ◽  
Wide Range ◽  
Materials Research ◽  
Novel Processing ◽  
Characterization Of Materials

X-rays have found a wide range of applications in chemistry, physics, and materials engineering since their discovery in 1895 by W. Roentgen. The materials science community uses x-ray-based techniques extensively for characterization of materials. In the 1970s a new tunable source of x-rays from the radiation produced by synchrotron accelerators emerged. Synchrotron radiation (SR) is an intense and forward-focused beam of radiation that is emitted when the path of an electron traveling at almost the speed of light is bent by a magnetic field. Figure 1 illustrates the evolution of radiation intensity provided by various x-ray sources. In situ SR techniques provide real-time observation of atomic arrangements with high spatial sensitivity and precision, which are important features not only in fundamental materials research, but also in the development of novel processing techniques and in the search for new exotic materials. A major advantage of SR is that it covers a wide range of wavelengths continuously from infrared to gamma rays. This feature is attractive since a wealth of detailed information on the electronic and structural properties of materials can be obtained by optimizing the wavelength of the radiation.Since the establishment of “first generation” facilities in the early 1970s, the x-ray emittance from synchrotron storage rings, where electrons traveling at almost relativistic speed s are constrained by magnetic fields to follow curved trajectories, has shown dramatic improvements. See Table I for an extensive list of SR facilities presentiy in use throughout the world.

In Situ Testing and X Rays Radiation Effects of Pt/Bi3.15Nd0.85Ti3O12/Pt Ferroelectric Capacitors

2013 ◽  
Vol 712-715 ◽  
pp. 293-297
Author(s):  
Li Li
Keyword(s):  
Radiation Effects ◽  
Hysteresis Loops ◽  
Electrical Performance ◽  
Hysteresis Curve ◽  
X Rays ◽  
Shanghai Synchrotron Radiation Facility ◽  
X Ray ◽  
In The Beginning ◽  
Ferroelectric Capacitors

Pt/Bi3.15Nd0.85Ti3O12(BNT)/Pt ferroelectric capacitors were monitored using in situ X-ray irradiation with 10 keV at BL14B1 beamline (Shanghai Synchrotron Radiation Facility). BL14B1 combined with a ferroelectric analyzer enabled measurements in situ of electrical performance. The hysteresis curve (PE) of distortion depended on the polarization during irradiation, but the diffracted intensities of the (117) peak did not change in the beginning. ThePEcurve had a negligible change from 2.09×109Gy to 4.45×109Gy. Finally, bothPrandPr+very rapidly increased, but the intensities of (117) decreased. The hysteresis loops were remarkably deformed at the maximum total dose of 4.87×109Gy.

Applications of High-Resolution Powder X-Ray Diffraction

2007 ◽  
Vol 130 ◽  
pp. 7-14 ◽  
Author(s):  
Andrew N. Fitch
Keyword(s):  
High Resolution ◽  
Synchrotron Radiation ◽  
Powder Diffraction ◽  
X Rays ◽  
X Ray Diffraction ◽  
Crystalline Materials ◽  
X Ray ◽  
Structural Characterisation ◽  
Pdf Analysis

The highly-collimated, intense X-rays produced by a synchrotron radiation source can be harnessed to build high-resolution powder diffraction instruments with a wide variety of applications. The general advantages of using synchrotron radiation for powder diffraction are discussed and illustrated with reference to the structural characterisation of crystalline materials, atomic PDF analysis, in-situ and high-throughput studies where the structure is evolving between successive scans, and the measurement of residual strain in engineering components.

scholarly journals The XXL Survey

2018 ◽  
Vol 620 ◽  
pp. A18 ◽  
Author(s):  
C. H. A. Logan ◽  
B. J. Maughan ◽  
M. N. Bremer ◽  
P. Giles ◽  
M. Birkinshaw ◽  
...  
Keyword(s):  
Angular Resolution ◽  
False Positive Rate ◽  
High Sensitivity ◽  
Point Sources ◽  
Selection Function ◽  
X Rays ◽  
Cluster Emission ◽  
X Ray ◽  
Wide Range ◽  
Function Modelling

Context. The XMM-XXL survey has used observations from the XMM-Newton observatory to detect clusters of galaxies over a wide range in mass and redshift. The moderate PSF (FWHM ~ 6″ on-axis) of XMM-Newton means that point sources within or projected onto a cluster may not be separated from the cluster emission, leading to enhanced luminosities and affecting the selection function of the cluster survey. Aims. We present the results of short Chandra observations of 21 galaxy clusters and cluster candidates at redshifts z > 1 detected in the XMM-XXL survey in X-rays or selected in the optical and infra-red. Methods. With the superior angular resolution of Chandra, we investigate whether there are any point sources within the cluster region that were not detected by the XMM-XXL analysis pipeline, and whether any point sources were misclassified as distant clusters. Results. Of the 14 X-ray selected clusters, 9 are free from significant point source contamination, either having no previously unresolved sources detected by Chandra or with less than about 10% of the reported XXL cluster flux being resolved into point sources. Of the other five sources, one is significantly contaminated by previously unresolved AGN, and four appear to be AGN misclassified as clusters. All but one of these cases are in the subset of less secure X-ray selected cluster detections and the false positive rate is consistent with that expected from the XXL selection function modelling. We also considered a further seven optically selected cluster candidates associated with faint XXL sources that were not classed as clusters. Of these, three were shown to be AGN by Chandra, one is a cluster whose XXL survey flux was highly contaminated by unresolved AGN, while three appear to be uncontaminated clusters. By decontaminating and vetting these distant clusters, we provide a pure sample of clusters at redshift z > 1 for deeper follow-up observations, and demonstrate the utility of using Chandra snapshots to test for AGN in surveys with high sensitivity but poor angular resolution.

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 In situ damage assessment using synchrotron X-rays in materials loaded by a Hopkinson bar

2014 ◽  
Vol 372 (2015) ◽  
pp. 20130191 ◽  
Author(s):  
Weinong W. Chen ◽  
Matthew C. Hudspeth ◽  
Ben Claus ◽  
Niranjan D. Parab ◽  
John T. Black ◽  
...  
Keyword(s):  
High Speed ◽  
Particle Interaction ◽  
Tensile Failure ◽  
High Rate ◽  
X Rays ◽  
Contrast Imaging ◽  
X Ray ◽  
Damage Initiation ◽  
Dynamic Experiments

Split Hopkinson or Kolsky bars are common high-rate characterization tools for dynamic mechanical behaviour of materials. Stress–strain responses averaged over specimen volume are obtained as a function of strain rate. Specimen deformation histories can be monitored by high-speed imaging on the surface. It has not been possible to track the damage initiation and evolution during the dynamic deformation inside specimens except for a few transparent materials. In this study, we integrated Hopkinson compression/tension bars with high-speed X-ray imaging capabilities. The damage history in a dynamically deforming specimen was monitored in situ using synchrotron radiation via X-ray phase contrast imaging. The effectiveness of the novel union between these two powerful techniques, which opens a new angle for data acquisition in dynamic experiments, is demonstrated by a series of dynamic experiments on a variety of material systems, including particle interaction in granular materials, glass impact cracking, single crystal silicon tensile failure and ligament–bone junction damage.

scholarly journals X-Ray Fluorescence Analysis of a Gold Ibex and other Artifacts from Akrotiri

2019 ◽  
Vol 11 ◽  
Author(s):  
A. G. Karydas ◽  
T. Pantazis ◽  
C. Doumas ◽  
A. Vlachopoulos ◽  
P. Nomikos ◽  
...  
Keyword(s):  
Bulk Composition ◽  
Fluorescence Analysis ◽  
Wall Painting ◽  
Inorganic Elements ◽  
X Ray ◽  
Wide Range ◽  
Soldering Technology ◽  
Excavation Area

In-situ X-ray fluorescence analysis (XRF) of ancient artifacts from the excavation area was performed using a novel X-ray instrumentation, composed of a portable silicon PIN thermoelectrically cooled X-ray detector, a miniature X-ray source, and portable data acquisition devices. The main objective of the analyses in Akrotiri was to explore the potential of the technique to provide answers to a wide range of archaeometric questions regarding the bulk composition of metal alloys, especially of gold, the characterization of corrosion products in bronze artifacts, identification of inorganic elements which are fingerprints of the minerals used in wall-painting pigments, and of the painting materials and techniques used for the decoration of clay vase surfaces. Among the analysed artifacts are a unique gold ibex, a bronze dagger and blade, various pigments from the wall paintings of room 3 in Xeste 3, decoration pigments from rosettes of faience, a bichrome jug, and other clay vases. The results of the in-situ XRF survey, primarily those of the bulk composition and soldering technology of the gold ibex, are discussed and compared with literature.

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