A Secondary-Source, Energy-Dispersive X-Ray Spectrometer and its Application to Quantitative Analytical Chemistry

1973 ◽  
Vol 17 ◽  
pp. 571-583
Author(s):  
R. P. Larsen ◽  
J. O. Karttunen
Keyword(s):  
Background Radiation ◽  
Energy Dispersive ◽  
Excitation Source ◽  
Secondary Source ◽  
X Rays ◽  
X Ray ◽  
Secondary Sources ◽  
The Individual ◽  
Detection Instrument

AbstractAn energy-dispersive X-ray spectrometer that (1) uses as the primary excitation source the power supply and tungsten X-ray tube from a conventional crystal spectrometer (General Electric XRD-6) and (2) uses as the secondary excitation source elemental metal foils that are readily interchangeable has been built and operated. The use of an X-ray tube with a high-voltage capability, 75 kilovolts max, enables the determination of elements with atomic numbers as high as 66 (terbium) to be based on the K series of X-rays; the highpower capability, 3.7 kilowatts max, enables a particularly intense beam of X-rays to be generated by the secondary source and hence, provides a particularly high detection capability for trace elements in a sample. An instrument that uses interchangeable secondary sources to irradiate the samples has several advantages over those instruments in which excitation is accomplished by direct irradiation with an X-ray tube: (1) the background radiation in the energy range where the X-rays of interest are measured is several orders of magnitude lower and is very uniform and (2) the energy of the excitation radiation can be closely matched to the absorption edges of the elements of interest in the sample.In the application of the instrument, particular emphasis has been placed on the development of tectmiques that will enable an energy-dispersive X-ray spectrometer to be used as the detection instrument for quantitative elemental analysis. Methods for the determination of the individual rare earths, plutonium and uranium at the microgram level with an accuracy of ± 1% are outlined and for the determination of plutonium and uranium at the milligram level with an accuracy of ± 0.1% are proposed.

Current developments in cosmic X-ray astronomy

1969 ◽  
Vol 313 (1514) ◽  
pp. 367-380 ◽  
Keyword(s):  
Background Radiation ◽  
X Rays ◽  
Launch Vehicles ◽  
Experimental Performance ◽  
X Ray ◽  
Wide Range ◽  
Diffuse Background ◽  
Wide Energy ◽  
The Individual

The purpose of this paper is to review the current developments in the observation of 0.2 to 100 keV X-rays originating outside the solar system. Discussion will be limited to experiments which are presently being developed and are likely to be flown within the next three years or so. Throughout this period experimental limits will continue to be set primarily by the available launch vehicles. Small rockets, and for energies above 20 keV, steerable balloons will continue to be the principal means of observation of cosmic X-rays, though with increasing use being made throughout the period of attitude controlled rockets (see, for example, Hazell, Cope & Walker 1968). In 1970 or 1971, the first satellite payloads specifically designed for cosmic X-ray studies should be launched, bringing a notable advance in sensitivity and resolution of the observations. There have been several excellent review articles published recently describing the different techniques useful in X-ray studies (e.g. Giacconiet et al . 1968; Aitken 1968) and therefore it is the present intention to review the current situation from the viewpoint of the observational aims of cosmic X-ray astronomy. For illustration of the kind of data to be expected in the period under review, reference will be made to a wide range of specific payloads. Performance figures quoted have been estimated by the author where not provided by the individual experimenter and and attempt has been made to achieve overall consistency in the criteria for judging experimental performance. The current observational aims of X-ray astronomy may be summarized as follows: (1) The detection of new sources, obtaining approximate positions and intensities. (2) Determination of accurate source positions, to facilitate identification studies. (3) Measurement of the size of a source and, if extended, also its structure. (4) Measurement of the detailed spectrum over a wide energy band for both discrete sources and the diffuse background radiation. (5) Study of source variability. (6) Measurement of polarization of the X-radiation.

Determination of the Mechanical Response of Thin Films with X-Rays

1993 ◽  
Vol 308 ◽  
Author(s):  
I. C. Noyan ◽  
G. Sheikh
Keyword(s):  
Thin Film ◽  
Thin Films ◽  
Mechanical Response ◽  
Strain Analysis ◽  
Local Strain ◽  
X Rays ◽  
Stress Strain ◽  
X Ray ◽  
The Individual

ABSTRACTThe mechanical response of a specimen incorporating thin films is dictated by a combination of fundamental mechanical parameters such as Young's moduli of the individual layers, and by configurational parameters such as adhesion strength at the interface(s), residual stress distribution and other process dependent factors. In most systems, the overall response will be dominated by the properties of the (much thicker) substrate. Failure within the individual layers, on the other hand, is dependent on the local strain distributions and can not be predicted from the substrate values alone. To better understand the mechanical response of these systems, the strain within the individual layers of the thin film system must be measured and correlated with applied stresses. Phase selectivity of X-ray stress/strain analysis techniques is well suited for this purpose. In this paper, we will review the use of the traditional x-ray stress/strain analysis methods for the determination of the mechanical properties of thin film systems.

scholarly journals Quantitative analysis by energy dispersive X-ray fluorescence by the transmission method applied to geological samples

1994 ◽  
Vol 51 (2) ◽  
pp. 197-206 ◽  
Author(s):  
S.M. Simabuco ◽  
V.F. Nascimento Filho
Keyword(s):  
Atomic Number ◽  
Energy Dispersive ◽  
X Rays ◽  
Geological Samples ◽  
Transmission Method ◽  
Absorption Effect ◽  
X Ray ◽  
Fundamental Parameters ◽  
Absorption Correction

Three certified samples of different matrices (Soil-5, SL-1/IAEA and SARM-4/SABS) were quantitatively analysed by energy dispersive X-ray fluorescence with radioisotopic excitation. The observed errors were about 10-20% for the majority of the elements and less than 10% for Fe and Zn in the Soil-5, Mn in SL-1, and Ti, Fe and Zn in SARM-4 samples. Annular radioactive sources of Fe-55 and Cd-109 were utilized for the excitation of elements while a Si(Li) semiconductor detector coupled to a multichannel emulation card inserted in a microcomputer was used for the detection of the characteristic X-rays. The fundamental parameters method was used for the determination of elemental sensitivities and the irradiator or transmission method for the correction of the absorption effect of characteristic X-rays of elements on the range of atomic number 22 to 42 (Ti to Mo) and excitation with Cd-109. For elements in the range of atomic number 13 to 23 (Al to V) the irradiator method cannot be applied since samples are not transparent for the incident and emergent X-rays. In order to perform the absorption correction for this range of atomic number excited with Fe-55 source, another method was developed based on the experimental value of the absorption coefficients, associated with absorption edges of the elements.

Oxford HEXameter: Laboratory High Energy X-Ray Diffractometer for Bulk Residual Stress Analysis

2006 ◽  
Vol 524-525 ◽  
pp. 743-748 ◽  
Author(s):  
Alexander M. Korsunsky ◽  
Shu Yan Zhang ◽  
Daniele Dini ◽  
Willem J.J. Vorster ◽  
Jian Liu
Keyword(s):  
Accurate Determination ◽  
High Energy ◽  
Energy Dispersive ◽  
Detector Response ◽  
X Rays ◽  
X Ray Diffraction ◽  
X Ray ◽  
New Instrument ◽  
Synchrotron Beamlines

Diffraction of penetrating radiation such as neutrons or high energy X-rays provides a powerful non-destructive method for the evaluation of residual stresses in engineering components. In particular, strain scanning using synchrotron energy-dispersive X-ray diffraction has been shown to offer a fast and highly spatially resolving measurement technique. Synchrotron beamlines provide best available instruments in terms of flux and low beam divergence, and hence spatial and measurement resolution and data collection rate. However, despite the rapidly growing number of facilities becoming available in Europe and across the world, access to synchrotron beamlines for routine industrial and research use remains regulated, comparatively slow and expensive. A laboratory high energy X-ray diffractometer for bulk residual strain evaluation (HEXameter) has been developed and built at Oxford University. It uses a twin-detector setup first proposed by one of the authors in the energy dispersive X-ray diffraction mode and allows simultaneous determination of macroscopic and microscopic strains in two mutually orthogonal directions that lie approximately within the plane normal to the incident beam. A careful procedure for detector response calibration is used in order to facilitate accurate determination of lattice parameters by pattern refinement. The results of HEXameter measurements are compared with synchrotron X-ray data for several samples e.g. made from a titanium alloy and a particulate composite with an aluminium alloy matrix. Experimental results are found to be consistent with synchrotron measurements and strain resolution close to 2×10-4 is routinely achieved by the new instrument.

Determination of K shell absorption parameters for some lanthanides using the X-ray attenuation method

2015 ◽  
Vol 93 (12) ◽  
pp. 1532-1540 ◽  
Author(s):  
F. Akman ◽  
R. Durak ◽  
M.R. Kaçal
Keyword(s):  
Cross Section ◽  
Cross Sections ◽  
Experimental Results ◽  
Secondary Source ◽  
X Rays ◽  
Strength Parameters ◽  
X Ray ◽  
Total Attenuation ◽  
First Time

The total attenuation cross section at the K edge, absorption jump ratio, jump factor, Davisson–Kirchner ratio, and oscillator strength parameters for the K shell were determined by measuring the total attenuation cross sections around the K edge for Pr, Nd2O3, and Sm. The measurements were performed in a secondary excitation geometry using the Kα2, Kα1, Kβ1, and Kβ2 X-rays (in the region from 31.817 to 55.293 keV) from different secondary source targets excited by the 59.54 keV γ-photons from an 241Am annular source. It is the first time that the Davisson–Kirchner ratio values have been determined for present samples. The experimental results were compared with the theoretically calculated and other available experimental results.

Energy-Dispersive X-Ray Techniques for Accurate Heavy Element Assay

1986 ◽  
Vol 30 ◽  
pp. 285-292 ◽  
Author(s):  
H. Ottmar ◽  
H. Eberle ◽  
P. Matussek ◽  
I. Michel-Piper
Keyword(s):  
Absorption Edge ◽  
Heavy Element ◽  
Accurate Determination ◽  
Energy Dispersive ◽  
X Rays ◽  
Specific Absorption ◽  
X Ray ◽  
Xrf Analysis ◽  
Analysis Technique

Energy-dispersive X-ray techniques can be employed in two different ways for the accurate determination of element concentrations in specimens: (1) spectrometry of fluoresced characteristic X-rays as widely applied in the various modes of the traditional XRF analysis technique, and (2) spectrometry of the energy-differential transmittance of an X-ray continuum at the element-specific absorption-edge energies.

Photoelectron Spectrometry: A New Approach to X-Ray Analysis

1972 ◽  
Vol 16 ◽  
pp. 74-89 ◽  
Author(s):  
Manfred O. Krause
Keyword(s):  
Energy Range ◽  
Emission Spectra ◽  
Atomic Level ◽  
Energy Dispersive ◽  
New Technique ◽  
X Rays ◽  
Electron Spectrometer ◽  
New Approach ◽  
X Ray

AbstractPhotoelectron spectrometry is shown to be an excellent technique for the analysis of x rays in the ultrasoft and soft x-ray regions. X rays are converted into photoelectrons which are ejected from a suitable atomic level, and the photoelectrons are analyzed with an electron spectrometer. The method is energy dispersive, provides a resolution ranging from 0.1 eV at 20 eV to 1.1 eV at 3 keV, and gives well-defined intensity characteristics throughout the range. The energy range can be extended into the 10 keV decade. Properties of the new technique are discussed, compared with conventional techniques, and exemplified by a series of measurements which include determination of the emission spectra of M x rays of yttrium to rhodium, L x rays of zirconium, and the band structures of molybdenum and holmium.

Digital x-ray mapping of nanometer-size supported bimetallic catalysts

1988 ◽  
Vol 46 ◽  
pp. 530-531
Author(s):  
L. T. Germinario
Keyword(s):  
Background Radiation ◽  
Metal Cluster ◽  
Single Element ◽  
Beam Diameter ◽  
X Rays ◽  
X Ray ◽  
Major Interest ◽  
Induced Changes

Understanding the role of metal cluster composition in determining catalytic selectivity and activity is of major interest in heterogeneous catalysis. The electron microscope is well established as a powerful tool for ultrastructural and compositional characterization of support and catalyst. Because the spatial resolution of x-ray microanalysis is defined by the smallest beam diameter into which the required number of electrons can be focused, the dedicated STEM with FEG is the instrument of choice. The main sources of errors in energy dispersive x-ray analysis (EDS) are: (1) beam-induced changes in specimen composition, (2) specimen drift, (3) instrumental factors which produce background radiation, and (4) basic statistical limitations which result in the detection of a finite number of x-ray photons. Digital beam techniques have been described for supported single-element metal clusters with spatial resolutions of about 10 nm. However, the detection of spurious characteristic x-rays away from catalyst particles produced images requiring several image processing steps.

Preparation And elemental analysis of ancient fibers

1987 ◽  
Vol 45 ◽  
pp. 410-411
Author(s):  
Allen Angel ◽  
Kathryn A. Jakes
Keyword(s):  
Cross Sections ◽  
Physical Structure ◽  
Energy Dispersive ◽  
Archaeological Sites ◽  
X Ray ◽  
Long Term Storage ◽  
Backscattered Electron ◽  
Electron Imaging

Fabrics recovered from archaeological sites often are so badly degraded that fiber identification based on physical morphology is difficult. Although diagenetic changes may be viewed as destructive to factors necessary for the discernment of fiber information, changes occurring during any stage of a fiber's lifetime leave a record within the fiber's chemical and physical structure. These alterations may offer valuable clues to understanding the conditions of the fiber's growth, fiber preparation and fabric processing technology and conditions of burial or long term storage (1).Energy dispersive spectrometry has been reported to be suitable for determination of mordant treatment on historic fibers (2,3) and has been used to characterize metal wrapping of combination yarns (4,5). In this study, a technique is developed which provides fractured cross sections of fibers for x-ray analysis and elemental mapping. In addition, backscattered electron imaging (BSI) and energy dispersive x-ray microanalysis (EDS) are utilized to correlate elements to their distribution in fibers.

Problems in Thin-Film X-ray Quantification

1990 ◽  
Vol 48 (2) ◽  
pp. 458-459
Author(s):  
J N Chapman ◽  
W A P Nicholson
Keyword(s):  
Thin Film ◽  
Specimen Thickness ◽  
X Rays ◽  
Characteristic Peak ◽  
Local Composition ◽  
X Ray ◽  
Measured Ratio ◽  
Path Lengths ◽  
Composition Changes

Energy dispersive x-ray microanalysis (EDX) is widely used for the quantitative determination of local composition in thin film specimens. Extraction of quantitative data is usually accomplished by relating the ratio of the number of atoms of two species A and B in the volume excited by the electron beam (nA/nB) to the corresponding ratio of detected characteristic photons (NA/NB) through the use of a k-factor. This leads to an expression of the form nA/nB = kAB NA/NB where kAB is a measure of the relative efficiency with which x-rays are generated and detected from the two species.Errors in thin film x-ray quantification can arise from uncertainties in both NA/NB and kAB. In addition to the inevitable statistical errors, particularly severe problems arise in accurately determining the former if (i) mass loss occurs during spectrum acquisition so that the composition changes as irradiation proceeds, (ii) the characteristic peak from one of the minority components of interest is overlapped by the much larger peak from a majority component, (iii) the measured ratio varies significantly with specimen thickness as a result of electron channeling, or (iv) varying absorption corrections are required due to photons generated at different points having to traverse different path lengths through specimens of irregular and unknown topography on their way to the detector.

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