Coupled X-ray Absorption/UV–vis Monitoring of Fast Oxidation Reactions Involving a Nonheme Iron–Oxo Complex

2019 ◽  
Vol 141 (6) ◽  
pp. 2299-2304 ◽  
Author(s):  
Giorgio Capocasa ◽  
Francesco Sessa ◽  
Francesco Tavani ◽  
Manuel Monte ◽  
Giorgio Olivo ◽  
...  
Keyword(s):  
Nonheme Iron ◽  
Oxidation Reactions ◽  
X Ray ◽  
X Ray Absorption

Adsorption and oxidation of SO2 on the surface of TiO2 nanoparticles: the role of terminal hydroxyl and oxygen vacancy–Ti3+ states

2020 ◽  
Vol 22 (18) ◽  
pp. 9943-9953
Author(s):  
Bing Wang ◽  
Xue Li ◽  
Shanshan Liang ◽  
Runxuan Chu ◽  
Dan Zhang ◽  
...  
Keyword(s):  
High Resolution ◽  
Oxygen Vacancy ◽  
Tio2 Nanoparticles ◽  
Photoelectron Spectroscopy ◽  
Flow Chamber ◽  
Oxidation Reactions ◽  
Edge Structure ◽  
X Ray ◽  
X Ray Absorption

The absorption and oxidation reactions of SO2 on TiO2 nanoparticles were investigated by using a flow chamber, synchrotron X-ray absorption near-edge structure and high resolution synchrotron X-ray photoelectron spectroscopy techniques.

X-ray microanalysis of thin specimens in the transmission electron microscope at voltages up to 1000 Kv.

1978 ◽  
Vol 36 (1) ◽  
pp. 540-541
Author(s):  
G. Cliff ◽  
M.J. Nasir ◽  
G.W. Lorimer ◽  
N. Ridley
Keyword(s):  
Electron Microscope ◽  
Transmission Electron Microscope ◽  
Weight Fraction ◽  
Present Series ◽  
Constant Independent ◽  
X Ray ◽  
Transmission Electron ◽  
Series Of Experiments ◽  
Image Position ◽  
X Ray Absorption

In a specimen which is transmission thin to 100 kV electrons - a sample in which X-ray absorption is so insignificant that it can be neglected and where fluorescence effects can generally be ignored (1,2) - a ratio of characteristic X-ray intensities, I1/I2 can be converted into a weight fraction ratio, C1/C2, using the equationwhere k12 is, at a given voltage, a constant independent of composition or thickness, k12 values can be determined experimentally from thin standards (3) or calculated (4,6). Both experimental and calculated k12 values have been obtained for K(11<Z>19),kα(Z>19) and some Lα radiation (3,6) at 100 kV. The object of the present series of experiments was to experimentally determine k12 values at voltages between 200 and 1000 kV and to compare these with calculated values.The experiments were carried out on an AEI-EM7 HVEM fitted with an energy dispersive X-ray detector.

SIGMAL: A Program for Calculating L-Shell lonization Cross-Sections

1981 ◽  
Vol 39 ◽  
pp. 198-199 ◽  
Author(s):  
R.F. Egerton
Keyword(s):  
Cross Sections ◽  
Fortran Program ◽  
Absorption Data ◽  
X Ray ◽  
Atomic Electrons ◽  
Energy Dependent ◽  
Hydrogenic Model ◽  
Electron Energy Loss ◽  
X Ray Absorption ◽  
Shell Ionization

SIGMAL is a short (∼ 100-line) Fortran program designed to rapidly compute cross-sections for L-shell ionization, particularly the partial crosssections required in quantitative electron energy-loss microanalysis. The program is based on a hydrogenic model, the L1 and L23 subshells being represented by scaled Coulombic wave functions, which allows the generalized oscillator strength (GOS) to be expressed analytically. In this basic form, the model predicts too large a cross-section at energies near to the ionization edge (see Fig. 1), due mainly to the fact that the screening effect of the atomic electrons is assumed constant over the L-shell region. This can be remedied by applying an energy-dependent correction to the GOS or to the effective nuclear charge, resulting in much closer agreement with experimental X-ray absorption data and with more sophisticated calculations (see Fig. 1 ).

point-Analysis Using the Extrapolation Method in the Analytical Electron microscope

1990 ◽  
Vol 48 (2) ◽  
pp. 430-431
Author(s):  
Zenji Horita ◽  
Ryuzo Nishimachi ◽  
Takeshi Sano ◽  
Minoru Nemoto
Keyword(s):  
Electron Microscope ◽  
Extrapolation Method ◽  
X Ray ◽  
Absorption Correction ◽  
Point Analysis ◽  
Analytical Electron ◽  
Analytical Electron Microscope ◽  
Data Points ◽  
Identical Composition ◽  
X Ray Absorption

Absorption correction is often required in quantitative x-ray microanalysis of thin specimens using the analytical electron microscope. For such correction, it is convenient to use the extrapolation method[l] because the thickness, density and mass absorption coefficient are not necessary in the method. The characteristic x-ray intensities measured for the analysis are only requirement for the absorption correction. However, to achieve extrapolation, it is imperative to obtain data points more than two at different thicknesses in the identical composition. Thus, the method encounters difficulty in analyzing a region equivalent to beam size or the specimen with uniform thickness. The purpose of this study is to modify the method so that extrapolation becomes feasible in such limited conditions. Applicability of the new form is examined by using a standard sample and then it is applied to quantification of phases in a Ni-Al-W ternary alloy.The earlier equation for the extrapolation method was formulated based on the facts that the magnitude of x-ray absorption increases with increasing thickness and that the intensity of a characteristic x-ray exhibiting negligible absorption in the specimen is used as a measure of thickness.

EXELFS Studies of Carbon Fibers

1990 ◽  
Vol 48 (2) ◽  
pp. 72-73
Author(s):  
V. Serin ◽  
K. Hssein ◽  
G. Zanchi ◽  
J. Sévely
Keyword(s):  
Carbon Fibers ◽  
Energy Analysis ◽  
Electron Excitation ◽  
Complex Structures ◽  
High Modulus ◽  
Promising Technique ◽  
X Ray ◽  
Fine Structures ◽  
X Ray Absorption

The present developments of electron energy analysis in the microscopes by E.E.L.S. allow an accurate recording of the spectra and of their different complex structures associated with the inner shell electron excitation by the incident electrons (1). Among these structures, the Extended Energy Loss Fine Structures (EXELFS) are of particular interest. They are equivalent to the well known EXAFS oscillations in X-ray absorption spectroscopy. Due to the EELS characteristic, the Fourier analysis of EXELFS oscillations appears as a promising technique for the characterization of composite materials, the major constituents of which are low Z elements. Using EXELFS, we have developed a microstructural study of carbon fibers. This analysis concerns the carbon K edge, which appears in the spectra at 285 eV. The purpose of the paper is to compare the local short range order, determined by this way in the case of Courtauld HTS and P100 ex-polyacrylonitrile carbon fibers, which are high tensile strength (HTS) and high modulus (HM) fibers respectively.

Improving soil remediation through characterization

1995 ◽  
Vol 53 ◽  
pp. 386-387
Author(s):  
E. C. Buck ◽  
N. L. Dietz ◽  
J. K. Bates
Keyword(s):  
Dust Particles ◽  
Radiochemical Analysis ◽  
Solid Product ◽  
Uranium Contamination ◽  
Physical Separation ◽  
X Ray ◽  
Rocky Flats ◽  
Remediation Strategies ◽  
Bearing Materials ◽  
X Ray Absorption

Operations at former weapons processing facilities in the U. S. have resulted in a large volume of radionuclidecontaminated soils and residues. In an effort to improve remediation strategies and meet environmental regulations, radionuclide-bearing particles in contaminant soils from Fernald in Ohio and the Rocky Flats Plant (RFP) in Colorado have been characterized by electron microscopy. The object of these studies was to determine the form of the contaminant radionuclide, so that it properties could be established [1]. Physical separation and radiochemical analysis determined that uranium contamination at Fernald was not present exclusively in any one size/density fraction [2]. The uranium-contamination resulted from aqueous and solid product spills, air-borne dust particles, and from the operation of an incinerator on site. At RFP the contamination was from the incineration of Pu-bearing materials. Further analysis by x-ray absorption spectroscopy indicated that the majority of the uranium was in the 6+ oxidation state [3].

Chemical and orientational imaging of polymeric samples

1994 ◽  
Vol 52 ◽  
pp. 68-69
Author(s):  
H. Ade ◽  
B. Hsiao ◽  
G. Mitchell ◽  
E. Rightor ◽  
A. P. Smith ◽  
...  
Keyword(s):  
Ethylene Terephthalate ◽  
National Laboratory ◽  
Brookhaven National Laboratory ◽  
Carbonyl Groups ◽  
Aromatic Rings ◽  
Edge Structure ◽  
X Ray ◽  
Scanning Transmission ◽  
Polymeric Samples ◽  
X Ray Absorption

We have used the Scanning Transmission X-ray Microscope at beamline X1A (X1-STXM) at Brookhaven National Laboratory (BNL) to acquire high resolution, chemical and orientation sensitive images of polymeric samples as well as point spectra from 0.1 μm areas. This sensitivity is achieved by exploiting the X-ray Absorption Near Edge Structure (XANES) of the carbon K edge. One of the most illustrative example of the chemical sensitivity achievable is provided by images of a polycarbonate/pol(ethylene terephthalate) (70/30 PC/PET) blend. Contrast reversal at high overall contrast is observed between images acquired at 285.36 and 285.69 eV (Fig. 1). Contrast in these images is achieved by exploring subtle differences between resonances associated with the π bonds (sp hybridization) of the aromatic groups of each polymer. PET has a split peak associated with these aromatic groups, due to the proximity of its carbonyl groups to its aromatic rings, whereas PC has only a single peak.

Quantitative x-ray microanalysis and thickness determination using ζ factor

1996 ◽  
Vol 54 ◽  
pp. 580-581
Author(s):  
M. Watanabe ◽  
Z. Horita ◽  
M. Nemoto
Keyword(s):  
Diffusion Couple ◽  
Extrapolation Method ◽  
Thin Specimen ◽  
Beam Position ◽  
X Ray ◽  
Thickness Determination ◽  
Experimental Limitation ◽  
X Ray Absorption

X-ray absorption in quantitative x-ray microanalysis of thin specimens may be corrected without knowledge of thickness when the extrapolation method or the differential x-ray absorption (DXA) method is used. However, there is an experimental limitation involved in each method. In this study, a method is proposed to overcome such a limitation. The method is developed by introducing the ζ factor and by combining the extrapolation method and DXA method. The method using the ζ factor, which is called the ζ-DXA method in this study, is applied to diffusion-couple experiments in the Ni-Al system.For a thin specimen where incident electrons are fully transparent, the characteristic x-ray intensity generated from a beam position, I, may be represented as I = (NρW/A)Qωaist.

X-Ray absorption edge elemental imaging of B. thuringienis

1989 ◽  
Vol 47 ◽  
pp. 212-213
Author(s):  
R. L. Stears
Keyword(s):  
Absorption Edge ◽  
Elemental Distribution ◽  
X Rays ◽  
Differential Absorption ◽  
Synchrotron Source ◽  
High Brightness ◽  
X Ray ◽  
Elemental Imaging ◽  
Cellular Integrity ◽  
X Ray Absorption

Because of the nature of the bacterial endospore, little work has been done on analyzing their elemental distribution and composition in the intact, living, hydrated state. The majority of the qualitative analysis entailed intensive disruption and processing of the endospores, which effects their cellular integrity and composition.Absorption edge imaging permits elemental analysis of hydrated, unstained specimens at high resolution. By taking advantage of differential absorption of x-ray photons in regions of varying elemental composition, and using a high brightness, tuneable synchrotron source to obtain monochromatic x-rays, contact x-ray micrographs can be made of unfixed, intact endospores that reveal sites of elemental localization. This study presents new data demonstrating the application of x-ray absorption edge imaging to produce elemental information about nitrogen (N) and calcium (Ca) localization using Bacillus thuringiensis as the test specimen.

Extended Core Edge Fine Structure in the E.M.

1980 ◽  
Vol 38 ◽  
pp. 120-121
Author(s):  
R.D. Leapman
Keyword(s):  
Fine Structure ◽  
Electron Scattering ◽  
Inelastic Electron ◽  
High Resolution Imaging ◽  
X Ray ◽  
Analytical Electron ◽  
Analytical Electron Microscope ◽  
Core Electrons ◽  
Resolution Imaging ◽  
X Ray Absorption

Extended X-ray Absorption Fine Structure (EXAFS) analysis makes use of synchrotron radiaion to measure modulations in the absorption coefficient above core edges and hence to obtain information about local atomic environments. EXAFS arises when ejected core electrons are backscattered by surrounding atoms and interfere with the outgoing waves. Recently, interest has also been shown in using inelastic electron scattering1-4. Some advantages of Extended X-ray-edge Energy Loss Fine Structure (EXELFS) are: a) small probes formed by the analytical electron microscope give spectra from μm to nm sized areas, compared with mm diameter areas for the X-ray technique, b) EXELFS can be combined with other techniques such as electron diffraction or high resolution imaging, and c) EXELFS is sensitive to low Z elements with K edges from ˜200 eV to ˜ 3000 eV (B to Cl).

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