Geochemical applications of synchrotron x-ray microspectroscopy

1994 ◽  
Vol 52 ◽  
pp. 54-55
Author(s):  
M. L. Rivers ◽  
S. R. Sutton ◽  
S. Bajt ◽  
J. S. Delaney
Keyword(s):  
Oxidation State ◽  
Incident Beam ◽  
Geochemical Evolution ◽  
Wheat Roots ◽  
X Ray ◽  
The Earth ◽  
Synchrotron Light ◽  
Contaminated Waste ◽  
X Ray Absorption ◽  
Mantle Oxidation State

The synchrotron x-ray fluorescence microprobe at bending magnet beamline X-26A at the National Synchrotron Light Source has been used for a number of years for geochemical trace element microanalysis using collimated white radiation. More recently an incident beam monochromator and 8:1 focusing mirror have been added. These optics permit the formation of a small (30-100 micron) intense beam of monochromatic radiation suitable for use in x-ray absorption spectroscopy, including both near edge (XANES) and extended fine structure (EXAFS) techniques. This system has been used to study a number of problems in the earth and environmental sciences, including: oxidation state of uranium in contaminated waste sites; oxidation state of Cr in olivine inclusions in diamonds from the Earth's mantle; oxidation state of Mn in wheat roots infected with the take-all disease. We report here some recent results obtained on studies of the oxidation state of Fe in cosmochemical systems.Oxygen fugacity is one of the most important parameters in determining the cosmochemical and geochemical evolution of a system.

SUT-NANOTEC-SLRI beamline for X-ray absorption spectroscopy

2017 ◽  
Vol 24 (3) ◽  
pp. 707-716 ◽  
Author(s):  
Wantana Klysubun ◽  
Pinit Kidkhunthod ◽  
Pongjakr Tarawarakarn ◽  
Panidtha Sombunchoo ◽  
Chanapa Kongmark ◽  
...  
Keyword(s):  
Absorption Spectroscopy ◽  
Incident Beam ◽  
Intermediate Energy ◽  
Photon Flux ◽  
Joint Research ◽  
X Ray ◽  
University Of Technology ◽  
Synchrotron Light ◽  
X Ray Absorption ◽  
Exafs Spectra

The SUT-NANOTEC-SLRI beamline was constructed in 2012 as the flagship of the SUT-NANOTEC-SLRI Joint Research Facility for Synchrotron Utilization, co-established by Suranaree University of Technology (SUT), National Nanotechnology Center (NANOTEC) and Synchrotron Light Research Institute (SLRI). It is an intermediate-energy X-ray absorption spectroscopy (XAS) beamline at SLRI. The beamline delivers an unfocused monochromatic X-ray beam of tunable photon energy (1.25–10 keV). The maximum normal incident beam size is 13 mm (width) × 1 mm (height) with a photon flux of 3 × 108to 2 × 1010 photons s−1(100 mA)−1varying across photon energies. Details of the beamline and XAS instrumentation are described. To demonstrate the beamline performance,K-edge XANES spectra of MgO, Al2O3, S8, FeS, FeSO4, Cu, Cu2O and CuO, and EXAFS spectra of Cu and CuO are presented.

scholarly journals Environmental Applications of Xanes: Speciation of Tc In Cement After Chemical Treatment and Se After Bacterial Uptake

1994 ◽  
Vol 344 ◽  
Author(s):  
D. K. Shuh ◽  
N. Kaltsoyannis ◽  
J. J. Bucher ◽  
N. M. Edelstein ◽  
S. B. Clark ◽  
...  
Keyword(s):  
Oxidation State ◽  
Chemical Shifts ◽  
National Synchrotron Light Source ◽  
X Ray ◽  
Bacterial Uptake ◽  
Synchrotron Light ◽  
The Common ◽  
Radiation Laboratory ◽  
X Ray Absorption ◽  
Cement Formulation

AbstractXANES (X-ray Absorption Near Edge Spectroscopy) has been employed to evaluate the efficacy of a process designed to encapsulate and reduce TcO4-in cement matrices, thereby immobilizing Tc. The oxidation state of Se following bioremediation of Se by bacteria has also been determined by XANES. The XANES measurements were performed at the Stanford Synchrotron Radiation Laboratory (SSRL) and the National Synchrotron Light Source (NSLS) at the respective K edges of Tc (21.0 keV) and Se (12.7 keV). Comparison of the XANES spectra of Tc in untreated cement to Tc in slag treated cement and to the chemical shifts of reference materials, shows that the oxidation state of Tc is the same in both cements. Thus, the addition of a reducing agent to the cement formulation does not significantly reduce the TcO4-. The common soil bacterium,Bacillus subtilis, is known to incorporate Se on or within the cell wall when exposed to a Se(IV) solution. The Se XANES spectra ofB. subtilis, as well as bacillus isolated from selenium rich soil, show that the organisms reduce selenite to the red allotrope of elemental Se.

scholarly journals Changes of Pd Oxidation State in Pd/Al2O3 Catalysts Using Modulated Excitation DRIFTS

Catalysts ◽  
2021 ◽  
Vol 11 (1) ◽  
pp. 116
Author(s):  
Gian Luca Chiarello ◽  
Ye Lu ◽  
Miren Agote-Arán ◽  
Riccardo Pellegrini ◽  
Davide Ferri
Keyword(s):  
Particle Size ◽  
Fourier Transform ◽  
Infrared Spectroscopy ◽  
Oxidation State ◽  
Diffuse Reflectance ◽  
X Ray ◽  
Spectral Changes ◽  
Diffuse Reflectance Infrared ◽  
X Ray Absorption ◽  
Reversible Reduction

Infrared spectroscopy is typically not used to establish the oxidation state of metal-based catalysts. In this work, we show that the baseline of spectra collected in diffuse reflectance mode of a series of Pd/Al2O3 samples of increasing Pd content varies significantly and reversibly under alternate pulses of CO or H2 and O2. Moreover, these baseline changes are proportional to the Pd content in Pd/Al2O3 samples exhibiting comparable Pd particle size. Similar measurements by X-ray absorption spectroscopy on a different 2 wt.% Pd/Al2O3 confirm that the baseline changes reflect the reversible reduction-oxidation of Pd. Hence, we demonstrate that changes in oxidation state of metal-based catalysts can be determined using diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) and that this behavior is part of the spectral changes that are returned by experiments under operando conditions.

scholarly journals Magnetic spectroscopy of nanoparticulate greigite, Fe3S4

2017 ◽  
Vol 81 (4) ◽  
pp. 857-872 ◽  
Author(s):  
Richard A. D. Pattrick ◽  
Victoria S. Coker ◽  
Masood Akhtar ◽  
M. Azad Malik ◽  
Edward Lewis ◽  
...  
Keyword(s):  
Absorption Spectra ◽  
Oxidation State ◽  
Magnetic Circular Dichroism ◽  
Covalent Character ◽  
X Ray ◽  
Positive Feature ◽  
A Site ◽  
Intermediate Oxidation ◽  
X Ray Absorption ◽  
Ferrite Spinel

AbstractSynthesis of Ni and Zn substituted nano-greigite, Fe3S4, is achieved from single source diethyldithiocarbamato precursor compounds, producing particles typically 50–100 nm in diameter with plate-like pseudohexagonal morphologies. Up to 12 wt.% Ni is incorporated into the greigite structure, and there is evidence that Zn is also incorporated but Co is not substituted into the lattice. The FeL3X-ray absorption spectra for these materials have a narrow single peak at 707.7 eV and the resulting main X-ray magnetic circular dichroism (XMCD) has the same sign at 708.75 eV. All XMCD spectra also have a broad positive feature at 711 eV, a characteristic of covalent mixing. The greigite XMCD spectra contrast with the three clearly defined XMCD site specific peaks found in the ferrite spinel, magnetite. The FeL2,3X-ray absorption spectra and XMCD spectra of the greigite reflect and reveal the high conductivity of greigite and the very strong covalency of the Fe–S bonding. The electron hopping between Fe3+and Fe2+on octahedral sites results in an intermediate oxidation state of the Fe in the Ohsite of Fe2.5+producing an effective formula of [Fe3+↑]A-site[2Fe2.5+↓]B-siteS42–]. The NiL2,3X-ray absorption spectra and XMCD reveal substitution on the Ohsite with a strongly covalent character and an oxidation state <Ni1.5+in a representative formula [Fe3+↑]A[[(2 – x)Fe2.5+↓][Nix1.5+]]BS42–.

scholarly journals Probing the variability in oxidation states of magnetite nanoparticles by single-particle spectroscopy

2018 ◽  
Vol 6 (4) ◽  
pp. 875-882 ◽  
Author(s):  
A. Fraile Rodríguez ◽  
C. Moya ◽  
M. Escoda-Torroella ◽  
A. Romero ◽  
A. Labarta ◽  
...  
Keyword(s):  
Oxidation State ◽  
Absorption Spectroscopy ◽  
Magnetite Nanoparticles ◽  
Single Particle ◽  
Cation Distribution ◽  
Oxidation States ◽  
Magnetic Response ◽  
X Ray ◽  
Single Particle Spectroscopy ◽  
X Ray Absorption

Single-particle X-ray absorption spectroscopy reveals that the oxidation state and cation distribution of individual magnetite nanoparticles may be largely heterogeneous even when the macroscopic structural and magnetic response of the ensembles is uniform.

Insights into sulfur poisoning and regeneration of Cu-SSZ-13 catalysts: In situ Cu and S K-edge XAS studies

2021 ◽  
Author(s):  
Vitaly Mesilov ◽  
Sandra Dahlin ◽  
Susanna Liljegren Bergman ◽  
Peter Sams Hammershøi ◽  
Shibo Xi ◽  
...  
Keyword(s):  
Selective Catalytic Reduction ◽  
Oxidation State ◽  
Absorption Spectroscopy ◽  
Catalytic Reduction ◽  
Sulfur Poisoning ◽  
X Ray ◽  
Scr Catalysts ◽  
X Ray Absorption

In situ Cu and S K-edge X-ray absorption spectroscopy (XAS) was used for the investigation of sulfur-poisoned and regenerated Cu-SSZ-13 selective catalytic reduction (SCR) catalysts. Sulfur in the oxidation state...

scholarly journals Changes in u(VI) SPeciation Upon Sorption onto Montmorillonite from Aqueous and Organic Solutions

1991 ◽  
Vol 257 ◽  
Author(s):  
Catherine Chisholm-Brause ◽  
Steven D. Conradson ◽  
P. Gary Eller ◽  
David E. Morris
Keyword(s):  
Oxidation State ◽  
Aqueous Systems ◽  
X Ray ◽  
Ph Values ◽  
Uranium Oxidation ◽  
Organic Solutions ◽  
X Ray Absorption ◽  
Hydrolysis Of ◽  
Uranium Species ◽  
Lines Of Evidence

ABSTRACTThe speciation of UO22+ and UO22+/ TBP mixtures has been investigated in solution and intercalated with the reference smectite clay SAz-1 using x-ray absorption, Raman, andluminescence spectroscopies. Neither aquated UO22+ nor its TBP complex undergoes any detectable changes in uranium oxidation state on intercalation. Further, at the pH values employed in this work, there is no evidence for hydrolysis of the uranium species to generate dimeric or higher order uranium oligomers. However, we do find indications that the structures of the solution complexes are altered on intercalation, particularly for the UO22+TBP system and for more dilute UO22+/aqueous systems. In addition, several lines of evidence suggest that, at the loading levels used in this study, the uranyl species is interacting with two or more spectroscopically distinguishable sites on SAz-1.

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