scholarly journals Size and structure of hexanuclear plutonium oxo-hydroxo clusters in aqueous solution from synchrotron analysis

2022 ◽  
Vol 29 (1) ◽  
Author(s):  
Thomas Dumas ◽  
Matthieu Virot ◽  
Denis Menut ◽  
Christelle Tamain ◽  
Cyril Micheau ◽  
...  
Keyword(s):  
Signal To Noise Ratio ◽  
Water Soluble ◽  
Saxs Data ◽  
X Ray ◽  
X Ray Scattering ◽  
Good Signal ◽  
Constrained Conditions ◽  
Future Work ◽  
X Ray Absorption ◽  
Sample Dispersion

The size and shape of a water-soluble hexanuclear plutonium cluster were probed by combining synchrotron small-angle X-ray scattering (SAXS) and extended X-ray absorption fine structure (EXAFS). A specific setup coupling both techniques and dedicated to radioactive samples on the MARS beamline endstation at Synchrotron SOLEIL is described. The plutonium hexanuclear cores are well stabilized by the 1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetic acid ligands and this allows a good evaluation of the setup to probe the very small plutonium core. The results show that, in spite of the constrained conditions required to avoid any risk of sample dispersion, the flux and the sample environment are optimized to obtain a very good signal-to-noise ratio, allowing the detection of small plutonium aggregates in an aqueous phase. The structure of the well defined hexanuclear cluster has been confirmed by EXAFS measurements in solution and correlated with SAXS data processing and modelling. An iterative comparison of classical fit models (Guinier or sphere form factor) with the experimental results allowed a better interpretation of the SAXS signal that will be relevant for future work under environmentally relevant conditions.

Silicon photodiode detector for small-angle X-ray scattering

1990 ◽  
Vol 23 (5) ◽  
pp. 430-432 ◽  
Author(s):  
P. R. Jemian ◽  
G. G. Long
Keyword(s):  
Small Angle ◽  
Signal To Noise Ratio ◽  
Scintillation Counter ◽  
Detector Response ◽  
Silicon Photodiode ◽  
Double Crystal ◽  
Saxs Data ◽  
X Ray ◽  
X Ray Scattering ◽  
Ray Scattering

A photodiode X-ray detector was built to measure small-angle X-ray scattering (SAXS) at a synchrotron-radiation source in conjunction with a double-crystal diffractometer SAXS camera at photon energies between 5 and 11 keV. The photodiode detector response in this energy range is linear at photon counting rates up to 1012 photons s−1 and thus it was not necessary to attenuate the monochromatic X-ray beam with calibrated foils. SAXS data taken with a scintillation counter and the photodiode detector are compared, demonstrating marked improvement in counting statistics, rate of data acquisition and signal-to-noise ratio.

Time-resolved XAFS measurement using quick-scanning techniques at BSRF

2017 ◽  
Vol 24 (3) ◽  
pp. 674-678 ◽  
Author(s):  
Shengqi Chu ◽  
Lirong Zheng ◽  
Pengfei An ◽  
Hui Gong ◽  
Tiandou Hu ◽  
...  
Keyword(s):  
Signal To Noise Ratio ◽  
High Energy ◽  
High Energy Resolution ◽  
Double Crystal ◽  
Time Resolved ◽  
Edge Structure ◽  
X Ray ◽  
Double Crystal Monochromator ◽  
Good Signal ◽  
X Ray Absorption

A new quick-scanning X-ray absorption fine-structure (QXAFS) system has been established on beamline 1W1B at the Beijing Synchrotron Radiation Facility. As an independent device, the QXAFS system can be employed by other beamlines equipped with a double-crystal monochromator to carry out quick energy scans and data acquisition. Both continuous-scan and trapezoidal-scan modes are available in this system to satisfy the time scale from subsecond (in the X-ray absorption near-edge structure region) to 1 min. Here, the trapezoidal-scan method is presented as being complementary to the continuous-scan method, in order to maintain high energy resolution and good signal-to-noise ratio. The system is demonstrated to be very reliable and has been combined with in situ cells to carry out time-resolved XAFS studies.

scholarly journals Vibrational resonant inelastic X-ray scattering in liquid acetic acid: a ruler for molecular chain lengths

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Viktoriia Savchenko ◽  
Iulia Emilia Brumboiu ◽  
Victor Kimberg ◽  
Michael Odelius ◽  
Pavel Krasnov ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Acetic Acid ◽  
Molecular Chain ◽  
X Ray ◽  
X Ray Scattering ◽  
Localized Excitations ◽  
Vibrational Excitations ◽  
Chain Lengths ◽  
X Ray Absorption ◽  
Ray Scattering

AbstractQuenching of vibrational excitations in resonant inelastic X-ray scattering (RIXS) spectra of liquid acetic acid is observed. At the oxygen core resonance associated with localized excitations at the O–H bond, the spectra lack the typical progression of vibrational excitations observed in RIXS spectra of comparable systems. We interpret this phenomenon as due to strong rehybridization of the unoccupied molecular orbitals as a result of hydrogen bonding, which however cannot be observed in x-ray absorption but only by means of RIXS. This allows us to address the molecular structure of the liquid, and to determine a lower limit for the average molecular chain length.

scholarly journals Crystalline and magnetic structure of Ba2CuO3+δ investigated by x-ray absorption spectroscopy and resonant inelastic x-ray scattering

2020 ◽  
pp. 1353810
Author(s):  
Roberto Fumagalli ◽  
Abhishek Nag ◽  
Stefano Agrestini ◽  
Mirian Garcia-Fernandez ◽  
Andrew C. Walters ◽  
...  
Keyword(s):  
Magnetic Structure ◽  
Absorption Spectroscopy ◽  
X Ray ◽  
X Ray Scattering ◽  
X Ray Absorption ◽  
Ray Scattering

Structural refinement by restrained molecular-dynamics algorithm with small-angle X-ray scattering constraints for a biomolecule

2004 ◽  
Vol 37 (1) ◽  
pp. 103-109 ◽  
Author(s):  
Masaki Kojima ◽  
Alexander A. Timchenko ◽  
Junichi Higo ◽  
Kazuki Ito ◽  
Hiroshi Kihara ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Molecular Dynamics ◽  
Small Angle ◽  
Protein Structures ◽  
Saxs Data ◽  
X Ray ◽  
X Ray Scattering ◽  
Saxs Curve ◽  
Restrained Molecular Dynamics ◽  
Ray Scattering

A new algorithm to refine protein structures in solution from small-angle X-ray scattering (SAXS) data was developed based on restrained molecular dynamics (MD). In the method, the sum of squared differences between calculated and observed SAXS intensities was used as a constraint energy function, and the calculation was started from given atomic coordinates, such as those of the crystal. In order to reduce the contribution of the hydration effect to the deviation from the experimental (objective) curve during the dynamics, and purely as an estimate of the efficiency of the algorithm, the calculation was first performed assuming the SAXS curve corresponding to the crystal structure as the objective curve. Next, the calculation was carried out with `real' experimental data, which yielded a structure that satisfied the experimental SAXS curve well. The SAXS data for ribonuclease T1, a single-chain globular protein, were used for the calculation, along with its crystal structure. The results showed that the present algorithm was very effective in the refinement and adjustment of the initial structure so that it could satisfy the objective SAXS data.

scholarly journals Structure of the manganese complex in photosystem II: insights from X–ray spectroscopy

2002 ◽  
Vol 357 (1426) ◽  
pp. 1347-1358 ◽  
Author(s):  
Vittal K. Yachandra
Keyword(s):  
Fine Structure ◽  
Emission Spectroscopy ◽  
Structural Models ◽  
Oxidation States ◽  
X Ray ◽  
X Ray Scattering ◽  
Raman Process ◽  
Mn Cluster ◽  
X Ray Absorption ◽  
S States

We have used Mn K–edge absorption and Kβ emission spectroscopy to determine the oxidation states of the Mn complex in the various S states. We have started exploring the new technique of resonant inelastic X–ray scattering spectroscopy; this technique can be characterized as a Raman process that uses K–edge energies (1s to 4p, ca . 6550 eV) to obtain L–edge–like spectra (2p to 3d, ca . 650 eV). The relevance of these data to the oxidation states and structure of the Mn complex is presented. We have obtained extended X–ray absorption fine structure data from the S 0 and S 3 states and observed heterogeneity in the Mn–Mn distances leading us to conclude that there may be three rather than two di– μ –oxo–bridged units present per tetranuclear Mn cluster. In addition, we have obtained data using Ca and Sr X–ray spectroscopy that provide evidence for a heteronuclear Mn1Ca cluster. The possibility of three di– μ –oxo–bridged Mn–Mn moieties and the proximity of Ca is incorporated into developing structural models for the Mn cluster. The involvement of bridging and terminal O ligands of Mn in the mechanism of oxygen evolution is discussed in the context of our X–ray spectroscopy results.

scholarly journals Structural Analysis of the Partially Disordered Protein EspK from Mycobacterium tuberculosis

Crystals ◽  
2020 ◽  
Vol 11 (1) ◽  
pp. 18
Author(s):  
Abril Gijsbers ◽  
Nuria Sánchez-Puig ◽  
Ye Gao ◽  
Peter J. Peters ◽  
Raimond B. G. Ravelli ◽  
...  
Keyword(s):  
Host Response ◽  
Limited Proteolysis ◽  
Maximal Dimension ◽  
Globular Domain ◽  
Saxs Data ◽  
X Ray ◽  
Disordered Protein ◽  
X Ray Scattering ◽  
C Terminus ◽  
New Treatments

For centuries, tuberculosis has been a worldwide burden for human health, and gaps in our understanding of its pathogenesis have hampered the development of new treatments. ESX-1 is a complex machinery responsible for the secretion of virulence factors that manipulate the host response. Despite the importance of these secreted proteins for pathogenicity, only a few of them have been structurally and functionally characterised. Here, we describe a structural study of the ESX-secretion associated protein K (EspK), a 74 kDa protein known to be essential for the secretion of other substrates and the cytolytic effects of ESX-1. Small-Angle X-ray Scattering (SAXS) data show that EspK is a long molecule with a maximal dimension of 228 Å. It consists of two independent folded regions at each end of the protein connected by a flexible unstructured region driving the protein to coexist as an ensemble of conformations. Limited proteolysis identified a 26 kDa globular domain at the C-terminus of the protein consisting of a mixture of α-helices and β-strands, as shown by circular dichroism (CD) and SAXS. In contrast, the N-terminal portion is mainly helical with an elongated shape. Sequence conservation suggests that this architecture is preserved amongst the different mycobacteria species, proposing specific roles for the N- and C-terminal domains assisted by the middle flexible linker.

scholarly journals In Situ Investigation of the Early-Stage Growth of Nanoporous Alumina

2018 ◽  
Vol 2018 ◽  
pp. 1-9
Author(s):  
Thérèse Gorisse ◽  
Ludovic Dupré ◽  
Marc Zelsmann ◽  
Alina Vlad ◽  
Alessandro Coati ◽  
...  
Keyword(s):  
Early Stage ◽  
Grazing Incidence ◽  
Alumina Layer ◽  
Nanoporous Alumina ◽  
X Ray ◽  
X Ray Scattering ◽  
In Situ Investigation ◽  
Low X ◽  
X Ray Absorption

We report the successful use of in situ grazing incidence small-angle X-ray scattering to follow the anodization of aluminum. A dedicated electrochemical cell was designed and developed for this purpose with low X-ray absorption, with the possibility to access all azimuthal angles (360°) and to remotely control the temperature of the electrolyte. Three well-known fabrication techniques of nanoporous alumina, i.e., single, double, and pretextured, were investigated. The differences in the evolution of the scattering images are described and explained. From these measurements, we could determine at which moment the pores start growing even for very short anodization times. Furthermore, we could follow the thickness of the alumina layer as a function of the anodization time by monitoring the period of the Kiessig fringes. This work is aimed at helping to understand the different steps taking place during the anodization of aluminum at the very early stages of nanoporous alumina formation.

scholarly journals Improvement of SAXS Lab Equipment by Using Scatterless Apertures

2014 ◽  
Vol 70 (a1) ◽  
pp. C1330-C1330
Author(s):  
Joerg Wiesmann ◽  
Andreas Kleine ◽  
Christopher Umland ◽  
André Beerlink ◽  
Juergen Graf ◽  
...  
Keyword(s):  
Signal To Noise Ratio ◽  
Experimental Setup ◽  
High Flux ◽  
Signal To Noise ◽  
Minimum Diameter ◽  
X Ray ◽  
X Ray Scattering ◽  
Wide Range ◽  
Beam Stop ◽  
Synchrotron Beamlines

Parasitic scattering caused by apertures is a well-known problem in X-ray analytics, which forces users and manufacturers to adapt their experimental setup to this unwanted phenomenon. Increased measurement times due to lower photon fluxes, a lower resolution caused by an enlarged beam stop, a larger beam defining pinhole-to-sample distance due to the integration of an antiscatter guard and generally a lower signal-to-noise ratio leads to a loss in data quality. In this presentation we will explain how the lately developed scatterless pinholes called SCATEX overcome the aforementioned problems. SCATEX pinholes are either made of Germanium or of Tantalum and momentarily have a minimum diameter of 30µm. Thus, these novel apertures are applicable to a wide range of different applications and X-ray energies. We will show measurements which were performed either at home-lab small angle X-ray scattering (SAXS) systems such as the NANOSTAR of Bruker AXS or at synchrotron beamlines. At the PTB four-crystal monochromator beamline at BESSY II data was collected for a comparison of conventional pinholes, scatterless Germanium slit systems and SCATEX pinholes. At the Nanofocus Endstation P03 beamline at PETRA III we compared the performance of our SCATEX apertures with conventional Tungsten slit systems under high flux density conditions.

scholarly journals Encapsulation Through The Use Of Emulsified Microemulsions

2021 ◽  
Author(s):  
Ruby R. Rafanan
Keyword(s):  
Controlled Release ◽  
Continuous Phase ◽  
Pharmaceutical Products ◽  
Water Soluble ◽  
Scanning Calorimetry ◽  
Food Grade ◽  
X Ray ◽  
X Ray Scattering ◽  
Food Applications ◽  
Glycerol Monooleate

Emulsified microemulsions (EMEs), first described in detail in 2005 by the group of Garti, consist of a thermodynamically stable water-in-oil microemulsion phase (w1/o) further dispersed within an aqueous continuous phase (w2). These internally-structured w1/o/w2 dispersions are promising controlled release vehicles for water-soluble flavouring compounds, drugs and nutraceuticals. With a stable internal droplet structure, storage stability is improved over non-thermodynamically stable structured emulsions and may exhibit unique controlled release behaviour. Use of food-grade components allows for wider and safer applications in food and pharmaceutical products. In this thesis, a food-grade w1/o microemulsion consisting of glycerol monooleate, tricaprylin and water was dispersed in an aqueous (w2) phase by membrane emulsification and stabilized by a caseinate-pectin complex to produce w1/o/w2 EMEs. The resulting EME showed no signs of phase separation for weeks at room temperature. The microemulsion and EME were characterized by differential scanning calorimetry (DSC), cryo-TEM and small angle x-ray scattering (SAXS) to determine whether the microemulsion’s internal structure was maintained after emulsification. It was shown that EME droplets displayed ordering around the periphery consistent with some loss of microemulsion structure, but maintained the characteristic disordered microemulsion structure at the droplet core. Overall, this research demonstrated the feasibility of developing EME for possible applications in food and non-food applications.

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