Applications of Optical and Electronic Dispersion to X-Ray Absorption-Edge Spectrometry

1959 ◽  
Vol 3 ◽  
pp. 11-39
Author(s):  
Charles G. Dodd

AbstractThe applications of X-ray emission or fluorescent spectrography to chemical analysis have increased spectacularly in recent years, but little attention has been paid to the potentialities of X-ray absorption techniques. Monochromatic X-ray absorption-edge spectrometry, in particular, is most promising. The ultimate sensitivity of absorption-edge spectrometry probably will be less than that of fluorescent analysis, but this disadvantage may be outweighed by the convenience, economy, and absence of matrix effects with the former method. Both methods appear limited in application only to certain elements.A pulse height analyzer coupled with scintillation and proportional counter detection has been found to permit an increase in sensitivity of absorption-edge spectrometry, primarily because controlled window widths may be utilized in determining transmitted X-ray intensities with a sealer. Further work has led to the development of a new rapid, convenient technique known as “differential pulse amplitude distribution (PAD) peak height analysis.” Work carried out during the development of the new method is described.

1964 ◽  
Vol 8 ◽  
pp. 118-133 ◽  
Author(s):  
William Parrish

AbstractEscape peaks occur when the incident X-ray quantum, energy exceeds the absorption edge energy of the detector element and the resulting X-ray fluorescence is lost from the detector. The most common escape peaks result from 1 K-fluorescence in NaI-scintillation counters and Xe K-, Xe L-, and Kr K-fluorescence in proportional counters. The average pulse amplitude of the escape peak is proportional to the difference of the Energies of the incident and fluorescent X-rays. If the intensity of the escape peak is high as in the case of Mo Kα and a kryptoopreportional counter, and the lower level of the pulse height analyzer is raised to reject the escape peak, the quantum counting efficiency may be reduced by a factor of two. When the pulse height analyzer is set for characteristic incident radiation, escape peaks appear in powder patterns at small diffraction angles. These broad low-intensity peaks are often mistakenly identified as resulting from misalignment, scattering, etc. Each powder reflection can produce its own escape peak which occurs at an angle slightly smaller than the absorption edge of the detector element. In a silicon powder pattern the three strongest reflections produce three resolved escape peaks whose peak intensities are about 4% of their corresponding Cu Kα peaks when the X-ray tube is operated at 50 kV. The escape peak intensities decrease with decreasing X-ray tube voltage and disappear when the voltage is lower than the absorption edge energy of the detector element. Absorption edge peaks observed without the upper level of the pulse height analyzer are similar in appearance, intensity, and diffraction angle to the escape peaks. In complex powder patterns the escape peak pattern is unresolved and may produce a number of very broad peaks.


Author(s):  
R. L. Stears

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.


2000 ◽  
Vol 62 (15) ◽  
pp. 9911-9914 ◽  
Author(s):  
G. Dalba ◽  
N. Daldosso ◽  
P. Fornasini ◽  
M. Grimaldi ◽  
R. Grisenti ◽  
...  

2017 ◽  
Vol 88 (5) ◽  
pp. 053501 ◽  
Author(s):  
M. A. Beckwith ◽  
S. Jiang ◽  
A. Schropp ◽  
A. Fernandez-Pañella ◽  
H. G. Rinderknecht ◽  
...  

MRS Advances ◽  
2019 ◽  
Vol 5 (1-2) ◽  
pp. 37-43
Author(s):  
Amber R. Mason ◽  
Stephanie M. Thornber ◽  
Martin C. Stennett ◽  
Laura J. Gardner ◽  
Dirk Lützenkirchen-Hecht ◽  
...  

ABSTRACTA zirconolite glass-ceramic material is a candidate wasteform for immobilisation of chlorine contaminated plutonium residues, in which plutonium and chlorine are partitioned to the zirconolite and aluminosilicate glass phase, respectively. A preliminary investigation of chlorine speciation was undertaken by analysis of Cl K-edge X-ray Absorption Near Edge Spectroscopy (XANES), to understand the incorporation mechanism. Cl was found to be speciated as the Cl- anion within the glass phase, according to the characteristic chemical shift of the X-ray absorption edge. By comparison with Cl K-edge XANES data acquired from reference compounds, the local environment of the Cl- anion is most closely approximated by the mineral marialite, in which Cl is co-ordinate to 4 x Na and/or Ca atoms.


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