bluuebunny/crossref_metadata_2025 huggingface dataset:
Characterization of Strain Distribution and Annealing Response in Deformed Silicon Crystals
Authors: Weissmann S. , Saka T.
Published: March 2019

The strain distribution associated with incipient microplasticity and its response to subsequent annealing were studied in smooth and notched silicon crystals. The characterization of plastic and elastic residual strains was carried out by X-ray topography based on PendellBsung Fringe (PF) patterns and was supplemented by X-ray doublecrystal diffractometry and specimen scanning with automatic Bragg angle control (ABAC). It was shown that the sites at or near the surface were preferred sites where, upon mechanical deformation, dislocation sources became activated. Microplastic zones thus formed constrained long-range, residual, elastic strains.
Some Problems in X-ray Stress Measurements
Authors: Cullity B. D.
Published: March 2019

Some kinds of plastic deformation leave a residual pseudo-macrostress in the material. The existence of this stress in certain specimens introduces errors into the standard x-ray measurement of residual macrostress, namely, in specimens that have been stretched, compressed, bent, rolled, or drawn.

No error is involved in x-ray measurements on peened, ground, or machined surfaces, or in specimens where the source of the stress is remote from the surface examined.

The x-ray and magnetic evidence for pseudo-macrostress is reviewed.
X-ray Diffraction Studies of Shocked Lunar Analogs
Authors: Hanss R. E. , Montague B. R. , Galindo C. P.
Published: March 2019

X-ray diffractometer studies of single-crystal quartz and orthoclase reveal the peak shock pressure experienced by the samples. This procedure may facilitate tapid, quantitative interpretation of the peak shock pressures experienced by materials occurring in lunar or terrestrial impact structures. Shocked specimens were obtained from the NASA 20 mm flat-plate accelerator at Johnson Space Center, Houston. Orthoclase single crystals were shocked normal to the (001) plane at pressure intervals between 0 and 297 kb. The amplitude of the 27.6° two-theta (002) maximum decreases as a function of increasing shock pressure. Quartz single crystals were shocked normal to the (0001) plane at pressure intervals between 0 and 310 kb. Examination of the peak amplitude/ half-width ratios for the 26.6° two-theta (101) and the 20.8° twotheta (100) reveals a general correlation of these ratios with shock pressure. This method seems appropriate for the calibration of shock pressures experienced by crystalline materials.
A Method of Determining the Elastic Properties of Alloys in Selected Crystallographic Directions for X-ray Diffraction Residual Stress Measurement
Authors: Prevey Paul S.
Published: March 2019

A technique and apparatus are described for obtaining the elastic constant E/(1 + v) in selected crystaliographic directions for the purpose of calibrating x-ray diffraction residual stress measurement methods. The preparation of a simple rectangular beam specimen with two active electrical resistance strain gages applied to the test surface is described. Samples are clamped in a diffractometer fixture designed to minimize displacement errors, and loaded in four-point bending to several stress levels below the proportional limit. A method is described for calculating E/(l + v) and an estimate of the experimental error.

Values of E/(l + v) obtained for several alloy-(hkl) combinations are presented. The results indicate that several alloys of current commercial interest exhibit significant elastic anisotropy.
A Modified Diffractometer for X-ray Stress Measurements
Authors: Macherauch E. , Wolfstieg U.
Published: March 2019

Usually, the classical Bragg-Brentano diffractometer arrangement is used for X-ray strain measurements. For measurements in different ψ-directions, the specimen is rotated clockwise or counter-clockwise around the diffractometer axis using a separate driving system (ω-diffractometer).During the measurements, primary and reflected X-ray beams are placed in the same plane as the normal of the specimen and the normals of the measured ﹛h,k,l﹜ -planes. However, the Bragg- Brentano principle also can he applied to strain measurements in different ψ-directions with a number of advantages if the specimen is rotated around an axis lying parallel to the diffractometer plane (ψ- diffractometer) (1). The principle, construction and characteristics of the ψ-diffractometer are described and compared with those of the ω-diffractometer.
X-ray Residual Stress Measurements Using Parallel Beam Optics
Authors: Chrenko Richard M.
Published: March 2019

X-ray residual stress measurements have been made with a commercial portable X-ray diffraction apparatus that uses parallel beam optics and that was specifically designed for residual stress measurements. This machine differs from X-ray diffraction units using the usual parafocusing geometry in several respects, most notably reduced sample placement errors and larger sample sizes that can be accommodated. Two special modes of operation are available and will be discussed. These are the ability to use the side inclining method for stress analysis and the ability to use an oscillating ψ motion, the latter mode being useful for examining large grain size materials.
Proton-Induced X-ray Emission Analysis of Human Autopsy Tissues
Authors: Lear R. D. , Van Rinsvelt H. A. , Adams W. S.
Published: March 2019

The 3.8 MeV proton beam from the University of Florida Van de Graaff accelerator has been used to perform trace element analysis of approximately 1200 samples (mostly from autopsies) of human tissues by proton-induced X-ray emission analysis (PIXE). Fifteen different organs and a variety of diseases have been studied. Preliminary data are presented indicating the variations of various elements in human kidney as a function of age. Analysis of samples from infants also indicate essential and non-essential elements in human kidney. On the average twelve trace elements (with atomic number equal to or larger than nineteen) are observed in each organ. Quantitative measurements have been made on several elements including K, Ca, Mn, Fe, Cu, Zn, Pb, Br, Rb, Sr, Cd, and Ba.
Determination of Sulfur, Ash, and trace Element Content of Coal, Coke, and Fly Using Multielement Tube-Excied X-ray Fluorescence Analsis
Authors: Cooper J. A. , Wheeler B. D. , Wolfe G. J. , Bartell D. M. , Schlafke D. B.
Published: March 2019

A procedure using tube excited energy dispersive x-ray fluorescence analysis with interelement corrections has been developed for multielement analysis of major and trace elements and ash content of coal, coke, and fly ash. The procedure uses pressed pellets and an exponential correction for interelement effects. The average deviations ranged from about 0.0003% for V at an average concentration of about .003% to 0.1% for S at an average concentration of 4%. About 25 elements were measured and 100 second minimum detectable concentrations ranged from about one part per million for elements near arsenic to about one tenth of one percent for sodium.
“Loss on Ignition” in Fused Glass Buttons
Authors: LeHouillier R. , Turmel S. , Claisse P.
Published: March 2019

When a sample is fused with a flux to produce a glass button for X-ray fluorescence analysis, some of the constituents are lost by decomposition (H2O, CO2) or by evaporation (Br, Cl, S) . Therefore the glass button is smaller than if no “Loss on Ignition” had occurred, and the X-ray intensities appear stronger. It is shown that “L.O.I.” can be handled as a regular element and that corrections can be made by means of influence coefficients. Since “L.O.I.” cannot be measured by X-ray fluorescence, one should normally know the “L.O.I.” to make the appropriate corrections, but under certain conditions, X-ray intensities yield both composition and “L.O.I.” as shown by Tertian and as confirmed by our experiments.
Low Energy Mass Absorption Coefficients from Proton Induced X-ray Spectroscopy
Authors: Lurio A. , Reuter W. , Keller J.
Published: March 2019

We describe a new and reliable experimental technique for the measurement of mass absorption coefficients in the 0.1 to 1 keV energy range. In this technique, the absorbing film is supported directly on a substrate which under proton bombardment will generate the x-rays whose absorption will be measured. Results are given for thirteen different metals at the C Kα (277 eV) line.
Processing of Energy Dispersive X-ray Spectra
Authors: Russ J. C.
Published: March 2019

Much attention has been given to the treatment of energy-dispersive X-ray spectra. Descriptions of mathematical approaches (and their implementation in computer programs) have dealt with the major areas of separating peaks from background and from each other. There has been an unspoken but widely accepted underlying assumption that the more complex the approach, and the more general it seems to be, the bette r. This assumption appeals to the mathematicians and programmers but should be sharply challenged by users , whose focus is more properly the analytical results that can be obtained in spec ific circumstances.
Counting Rate Performance of Pulsed - Tube Systems
Authors: Sandborg A. O. , Russ J. C.
Published: March 2019

Energy - dispersive x-ray fluorescence systems are characterized by limited count rate capability, which is an important practical limitation on their application. This arises from two factors: 1) The amplifier time constant is many times greater than needed in wavelength-dispersive systems, in order to permit accurate measurement of pulse height, and reducing the time constant degrades system resolution; 2) x-ray pulses from ail the major and minor elements, as welt as scattered background and/or peaks from the incident radiation, must all be processed, reducing further the effective count rate for a single element of interest. Hence there has been a strong desire to find ways to increase the count rate capability of energy-dispersive systems.
Precision and Reproducibility of Lattice Parameters from Guinier Powder Patterns: Follow-Up and Assessment
Authors: Brown A. , Foris C.M.
Published: March 2019

Lattice parameters, obtained by least-squares refinement of data from calibrated Guinier powder patterns, are compared in an effort to establish procedures for obtaining reproducible 2θ values with Guiniertype focusing camera techniques. The calibration procedure is discussed and a method of calculation to reduce loss of precision is proposed. Effects of particle size and crushing are also discussed as well as some sources of error such as use of only selected calibrant lines, film background, and mutual interference of powder lines.
Scrip-Fortan IV Software for Quantitative XRD
Authors: Wong Edward R. , Yeko John , Engler Philip , Gerron Richard A.
Published: March 2019

X-ray diffraction is ideal for quantitative crystalline phase determination in solid mixtures. Each phase of the mixture will produce its characteristic lines independent of other phases that may or may not be present when diffracting an X-ray beam and will be “proportional” to the amount of the phase present.
The Measurement of Thermally Induced Structural Changes by High Temperature (900°C) Guinier X-Ray Powder Diffraction Techniques
Authors: Fawcett T. G. , Moore Kirchhoff P. , Newman R. A.
Published: March 2019

A new method for the collection and analysis of high temperature Guinier x-ray data has been devised at The Dow Chemical Co. This technique can be used to monitor various types of structural transformation and thermal expansions up to 900°C. The thermal expansions of α-Al2O3 and two TiO2 structures, anatase and rutile, have been characterized for their use as high temperature internal standards.
Comparison of X-Ray Powder Diffraction Techniques
Authors: Das Gupta K.
Published: March 2019

Following the discovery of powder diffraction by Debye and Scherrer, a major improvement of the intensity of diffraction patterns was attained by introducing focusing cameras. The focusing principle is exploited in the Seemann-Bohlin camera and with improved general background in the Guinier focusing camera. Guinier used a bent crystal to focus Ka lines from the target radiation. Das Gupta, Schnopper and Metzger reported a modification of the Seemann-Bohlin camera by replacing the slit with a target positioned on the focusing circle. This was further improved by using a microfocus target, 30 x 100 micron, positioned accurately on the focusing circle, Fig. 1 (a). The arrangement was very successful for determining thermal expansion coefficients of elements and a few superconducting alloys at different temperature regions.
The Determination of Elastic Constants Using a Combination of X-Ray Stress Techniques
Authors: Goldsmith Charles , Walker George A.
Published: March 2019

The powder diffraction x-ray technique commonly used to measure strain in polycrystalline materials requires a knowledge of the elastic constants in order to convert the strain into a stress value. For many materials, these constants are not always known. Another technique to measure strain is the x-ray lattice curvature (substrate bending) method which requires no knowledge of the film elastic constants. The strain is measured in the substrate and requires only the elastic constants of the substrate to convert the measured strain into stress. Using a combination of the powder diffraction technique and a double crystal lattice curvature technique, the elastic constants of TaSi2and WSi2have been determined for various crystallographic directions.
A Phi-Psi-Diffract (Meter for Residual Stress Measurements
Authors: Wagner C.N.J. , Boldrick M.S. , Perez-Mendez V.
Published: March 2019

A ϕ-ψ diffractometer has been designed and constructed to evaluate residual stresses in polycrystalline samples by x-ray diffraction. It permits rotations of the x-ray diffraction apparatus, consisting of an x-ray tube and a position-sensitive proportional counter, about two axes ϕ and ψ. The ϕ-rotation from 0° to 360° is carried out about the normal to the surface of the stationary sample, whereas the ψ-motion consists of a rotation from -45° to +45° about an axis lying in the sample surface and the diffraction plane, but perpendicular to the diffraction vector. This ϕ-ψ diffractometer permits the application of the ϕ- and ψ-differential and integral methods for the evaluation of the strain tensor and its gradient averaged over the depth of x-ray penetration into the sample. Assuming that isotropic elasticity theory is applicable, the stress tensor can then be evaluated from the measured strain tensor.
X-Ray Fractography on Fatigue Fractured Surface
Authors: Kodama Shotaro , Misawa Hiroshi , Sekita Yuji
Published: March 2019

The technique analysing the cause and mechanism of fracture from the information obtained by X-ray irradiation on the fractured surface is called “X-ray fractography.” As a basic study of X-ray fractography the residual stress on the fatigue fractured surface and some parameters of the fracture mechanics were investigated.
X-Ray Diffraction Study of Shape Memory in Uranium-Niobium Alloys
Authors: Carpenter D. A. , Vandermeer R. A.
Published: March 2019

An x-ray diffraction study of the reversible deformation inodes associated with the shape memory effect has been carried out on a series of uranium-niobium alloys near the monotectoid composition (6.2 wt. % Nb). Diffraction patterns were measured as a function of strain, in situ, while the specimens were under stress as part of an attempt to explain the “easy-flow”, low-strain plateau in the stress-strain curve. The alloys, consisting of highly twinned, metastable α” (monoclinic) and γ° (tetragonal) phases derived from the high-temperature BCC γ phase, produced broad, overlapping diffraction lines difficult to analyze by conventional techniques. One solution to this problem was to use a segmented step-scan technique so as to apportion the scan time to concentrate on the most difficult regions. This paper discusses data obtained from an α” alloy and a dual-phase α” + γ° alloy.
Automated Qualitative X-Ray Fluorescence Elemental Analysis
Authors: Garbauskas Mary F. , Goehner Raymond P.
Published: March 2019

A series of FORTRAN IV programs have been written to aid in qualitative x-ray fluorescence (XRF) analysis. These programs have been implemented on a DEC PDP 11/34 computer with an RSX-11M operating system and access the NIH elemental data base (1). The programs and their application to XRF analysis in our laboratory will be described.
A New Method for Quantitative X-Ray Fluorescence Analysis of Mixtures of Oxides or Other Compounds by Empirical Parameter Methods
Authors: Mantler Michael
Published: March 2019

Two principal mathematical methods are used for quantitative XRFA: fundamental parameter calculations and the evaluation of empirical parameter equations. A comprehensive computer program based upon fundamental parameter equations was introduced in 1976 by D. Laguitton and M. Mantler (LAMA-I) and improved by T. C. Huang in 1979 (LAMA-II). The present paper describes the features of the theoretical background of a computer program using a new type of empirical (alpha*-) parameter equations. It is essentially designed for convenient analysis of compounds including those containing chemical elements, that cannot be directly measured by conventional X-ray spectrometers, such as oxides, nitrides, and others. The program also communicates automatically with LAMA in order to establish theoretical tables of alpha*-coefficients as well as conventional alpha-coefficients.
FPT: An Integrated Fundamental Parameters Program for Broadband EDXRF Analysis without a Set of Similar Standards
Authors: Gedcke D. A. , Byars L. G. , Jacobus N. C.
Published: March 2019

The x-ray fluorescence (XRF) method is well known for its capability to perform fast and accurate quantitative analysis for all elements with atomic numbers greater than ten. Energy dispersive x-ray fluorescence (EDXRF) adds to this capability the benefit of quick qualitative analysis, due to its simultaneous sensitivity to all the elements. The method has the potential for rapid and complete chemical analysis of any sample which arrives on the analytical chemist's doorstep. Although the method has been a productive tool for fast and accurate repetitive analysis of similar samples, its applicability to unique unknowns has been rather limited. The limitation arises from the usual need to calibrate the instrument's response with a set of 6 to 12 standards, whose compositions must be similar to the unknown sample. Anyone who has struggled to develop and maintain such a suite of accurately certified standards knows that a great deal of effort and expense is involved. This effort is well justified when the analyst expects to analyze the same type of material frequently over an extended tine period. However, for a unique sample analysis, the task of developing a suite of similar standards simply makes the analysis impractical. What is needed is a method that requires minimal standards, or uses no standards at all.
A Generalized Matrix Correction Approach for Energy-Dispersive X-Ray Fluorescence Analysis of Paint Using Fundamental Parameters and Scattered Silver Kα Peaks
Authors: Christensen Leif Højslet , Drabæk Iver
Published: March 2019

An energy-dispersive x-ray fluorescence method has been developed for the direct determination of major and minor elements in infinitely thick samples of paint. Matrix absorption and enhancement corrections are iteratively calculated from a knowledge of tabulated fundamental parameters and the unknown weight fractions. An estimate of the significant light element fraction of the bulk sample required for the calculation of matrix attenuation is obtained using the scatter peaks of the silver secondary target. Relative elemental calibration constants and calibration factors for the coherent and incoherent peaks are determined experimentally using either thin-film standards or standards of known total composition. For routine analysis only one absolute standard is required. The method has been applied to different types of paint with a relative standard deviation better than 5% provided the counting statistics are not the limiting factor. The accuracy has been tested by comparing own results with those obtained either from the formulation or from, instrumental neutron activation analysis.
Determination of Boron Oxide in Glass by X-Ray Fluorescence Analysis
Authors: Arai T. , Sohmura T. , Tamenori H.
Published: March 2019

In the last few years, at the Denver X-Ray Analytical Conference, the author and co-workers presented two papers which described the principle and applications of carbon analysis by X-ray fluorescence based upon a monochromatization technique consisting of total reflection and filtering. Instead of the wavelength dispersive method based on Bragg reflection, this monochromatization, combining total reflection by a selected mirror and an appropriate filter, offered an alternative approach for the purpose of increasing measured X-ray intensity. The analytical performance of quantitative determination of carbon content in steel, cast iron and coal were reported.
NCSXRF: A General Geometry Monte Carlo Simulation Code for EDXRF Analysis
Authors: He T. , Gardner R. P. , Verghese K.
Published: March 2019

EDXRF analysis is conveniently split into two parts: (1) the determination of X-ray intensities and (2) the determination of elemental amounts from X-ray intensities. For the first, most EDXRF analysis has been done by some method of integrating the essentially Gaussian distribution of observed full energy pulse heights. This might be done, for example, by least-square fitting of Gaussian distributions superimposed on a straight line or a quadratic background. Recently more elaborate shapes of the energy peaks also have been considered (Kennedy, 1990). After the X-ray intensities have been determined, interelement effects between the analyte element and other elements must be corrected for in order to obtain the elemental amounts from X-ray intensities. This correction can be done either by an empirical correction procedure as in the influence coefficient method which requires measurements on a number of standard samples to determine the required coefficients, or by theoretical calculation as in the fundamental parameters method which does not require standard samples.
Decomposition Spectrometric Data of Energy Dispersive X-Ray Fluorescence Analysis (EDXRF)
Authors: Smolniakov V. I. , Koltun I. A.
Published: March 2019

It is well-known that in EDXRF, using high-resolution semiconductor detectors, evaluation of x-ray fluorescence radiation line intensities from multiplex spectrometric information represents definite difficulties, especially in automation of measurement-calculation procedures.

A common spectrum decomposition problem is to get the following parameters: a number of spectral lines and their centroids, intensities from measured experimental data and their errors.

We have developed special software for solving this problem using personal computers and high-level programming language C. It uses profiles of real-form lines of pure chemical elements produced by semiconductor detector spectrometers and these techniques: digital filters with parameters for suppression of background, multiplex structure analysis, and stable linear least-squares fit to get peak intensities. Also it established special criteria for reliability of the results.

We compared our investigation with software “EDXRF” (ver.1.32) arid spectrum decomposition with Gaussian peaks.
Recent Developments in Surface and Thin Film Analysis using Low - Energy Electron Induced X-Ray Spectrometry (LEEIXS)
Authors: Romand M.J. , Gaillard F. , Charbonnier M.
Published: March 2019

A review is given of the main gas-discharge sources and auxiliary equipments which were used in soft and ultra-soft X-ray emission spectrometry. Special attention is paid to the basic principles and instrumentation of low-energy electron-induced X-ray spectrometry (LEEIXS) whose excitation source is an electron beam generated in a glow-discharge system. Capabilities of LEEIXS in surface and thin film analysis and characterization are illustrated by examples dealing with control and optimization of surface treatment and thin film deposition processes. Sensitivity of the technique down to the submonolayer range and influence of backscattering phenomena are shown.
Multi-Layer XRF Calculations
Authors: Sumini M. , Fernández J.E.
Published: March 2019

An analytical framework for calculation of multiple scattering intensities emitted by a multi-layer sample are obtained with transport theory. The n-th order Flux solution of the Boltzsiann transport equation renders the iterative solution for multi-layers samples of thin or infinite thickness.

The first-order intensity is written for a generic sample with I layers and for the predominating interactions in the X-ray regime: the photoelectric effect, and the Compton and the Rayleigh scattering. As an example, the case of a thin deposit on an infinite thickness substrate is discussed.
Multiple Scattering Contributions of Thin Films in Reflection Geometry
Authors: Fernández J.E. , Sartori R.
Published: March 2019

The multiple scattering contributions to the emitted intensity of a thin homogeneous sample under X-Ray excitation are studied with recourse to the Boltzmann transport theory. The corrective terms to the XRF characteristic line due to a second collision of either the photoelectric effect (secondary XRF), or the Compton, or the Rayleigh scattering, are deduced for reflection geometry. Analytical expressions for the intensities are given that allow their computation for variable incidence and take-off beam directions and source wavelength.
X-Ray Photoelectron and Fluorescence Spectra of Several Zirconium Oxide Compounds
Authors: Haruyama Tatsuya , Sasaki Goh , Fukushima Sei , Kuchitsu Kozo , Koshizaki Naoto
Published: March 2019

Ila group metal - Zr pcrovskitc type compounds (MZrO3, M=Ba. Sr and Ca) and other oxides were studied by XPS to know the effects of M atoms to Zr atoms. And the feasibility of using XPS and high-resolution XRF for the coordination analysis of Zr atoms was examined for some kinds of stabilized zirconia. An almost linear relationship between the energy of Zr 3d peaks and the radii of Ila group metal ions was found, and, a simple model to interpret this relationship has been proposed. However, no relationship between the energy shifts of Zr 3d spectra or Zr Lα1, 2 spectra and the coordination numbers of Zr atoms in the several Zr oxide compounds was found. Thus, the coordination analysis using XPS or high-resolution XRF is not feasible.
Surface and Thin Film Analysis of Metals and Semiconductors using X-Ray Photoelectron Spectroscopy
Authors: Hofmann S.
Published: March 2019

X-ray excited Photoelectron Spectroscopy (XPS) has become an indispensable tool for the study of metals and semiconductors. Due to the small mean free path of the photoelectrons In solids of the order of a few nanometers for energies in the keV range, it is a surface analysis technique. Its capability of quantitative analysis of all elements except hydrogen and helium and their chemical bonding states has recently been combined with small area and imaging analysis to typical spatial resolutions of about 10 μm. After a brief survey of the basic capabilities and limitations of XPS, some illustrative examples in typical metals and semiconductor research areas are presented, such as surface contamination and failure analysis in microelectronics, oxidation and corrosion, segregation at surfaces and interfaces, oxide/metal and oxide/semiconductor interfaces, and thin film analysis using angle resolved XPS and sputter depth profiling. Recent developments emphasize improved data evaluation and quantification schemes as well as instrumental capabilities with respect to both high spatial and energy resolution, and high power excitation sources such as synchrotron radiation.
TXRF with Various Excitation Sources
Authors: Wobrauschek Peter , Kregsamer Peter , Streli Christina , Rieder Robert , Aiginger Hannes
Published: March 2019

Improving the detection limits in TXRF by optimizing the excitation conditions is the goal of this work. The properties of the exciting radiation due to spectral distribution, polarisation, intensity and energy are investigated and compared to find best conditions. Results are given from experiments performed with synchrotron radiation, Bragg polarized monoenergetic x-rays, high energy cut-off reflector in the primary beam path of a high power x-ray tube and several geometries for the sample reflector.
Uranium Concentration Measurement in Water Samples with TXRF
Authors: Hegedus F. , Winkler P.
Published: March 2019

The Total Reflection X-Ray Fluorescence method was used to detect low level (ppb) uranium concentration in water.
X-Ray Microbeam Spectroscopy with the Use of Capillary Optics
Authors: Larsson S. , Engström P.
Published: March 2019

X-ray micro analysis had suffered from the limited intensity of conventional X-ray sources like X-ray tubes etc. However, with the optical technique described in this paper, the so called “X-ray Capillary Optics” (XCO), it is possible to make X-Ray Fluorescence (XRF) analysis in micro-scale, down to a few μm2 still with conventional sources.
A New User Oriented Intelligent XRF Spectrometer System
Authors: Kataoka Y. , Masukawa N. , Toda K.
Published: March 2019

The semi-quantitative analysis, which is called ‘Standardless Analysis’, plays a major role in X-ray fluorescent analysis, especially in the field of research and development. The main feature of the semi-quantitative analysis is the fact that the composition of a sample can be obtained directly from a qualitative scan without any prior knowledge of the sample.
Problems in the Use of Multilayers for Soft X-Ray Spectroscopy and Analysis: A Comparison of Theoretically and Experimentally Determined Refraction Effects
Authors: Martins E. , Urch D.S.
Published: March 2019

Refraction effects cause the effective 2d spacing of multilayers to vary so that the simple Bragg equation is not applicable when such devices are used for soft X-ray spectroscopy. This paper describes how the refraction term can be determined experimentally. These results compare well with dispersion and absorption terms calculated from atomic scattering factors.
A Method for In-Situ Calibration of Semiconductor Detectors
Authors: Wernisch J. , August H.J. , Lindner-Schbnthaler A.
Published: March 2019

A method of semiconductor detector calibration by variation of the incidence angle of the x-radiation is discussed.
Analytical X-Ray Analysis Techniques: A Panorama of Some of the Applications in Latin America
Authors: Vazquez C. , de Leyt D.V. , LaBrecque J. J.
Published: March 2019

In general Latin America countries function differently in respect to the rest of the world because of their geographic allocations, economic and social situations. The areas of science and technologies are not excluded from this general rule. Thus, the following question arises : How has the area of analytical x-ray analysis techniques developed in Latin America in respect to the developed countries?
Measurements of Low Concentration Components in Iron Ores using Fusion Method
Authors: Yamada K. , Kohno H. , Arai T.
Published: March 2019

The problem of background radiation in X-ray fluorescence trace element analysis of fused-glass iron ore samples is addressed. A first-order model of coherent and Comptcn scattering with primary absorption is presented and used to correct measurements. Overlap coefficients for elements in iron ores are presented. The importance of these corrections is demonstrated. The accuracy achieved with X-ray measurements after background corrections compares well with the accuracy of chemical analysis.
The Local Structure of Chromium(III) in the Mixed Glycerol Aqueous Solution
Authors: Watanabe T. , Taniguchi K. , Ninomiya T. , Ikeda S.
Published: March 2019

Chromium glycerate solutions are exposed to X-ray absorption fine structure analysis to clarify the local structure around the chromium atom by the use of a laboratory XAFS system. The chromium solution is stabilized by addition of water soluble polyvinyl alcohol so that after excess water, the solution is a kind of homogenized “sol” without any apparent charge to the solution state. The new technique has been developed, because chromium is an element which has relatively small X-Ray absorption.

The comformations of two novel chromium glycerate compounds, which are prepared under both NH4OH and NaOH basic conditions, are examined with XANES and EXAFS techniques. From these experiments, it is suggested that these two chromium glycerates may have Cr-O-Cr bridge bonds consisting of chromium dimer complexes in common.
X-Ray Optics for Scanning Fluorescence Microscopy and Other Applications
Authors: Ryon Richard W. , Warburton William K.
Published: March 2019

Scanning x-ray fluorescence microscopy is analogous to scanning electron microscopy. Maps of the distribution of chemical elements are produced by scanning the specimen with a very small x-ray beam while collecting the XRF spectrum. Our goal is to perform such scanning microscopy with resolution in the range of <1 to 10 μm, using standard laboratory x-ray tubes. In order to increase the radiation flux on the specimen, we are investigating mirror optics in the Kirkpatrick-Baez (K-B) configuration, K-B optics uses two curved mirrors mounted orthogonally along the optical axis. The first mirror provides vertical focus, the second mirror provides horizontal focus. We have used two types of mirrors: synthetic multilayers and crystals. Multilayer mirrors are used with lower energy radiation such as Cu Kμ. At higher energies such as Ag Kct, silicon wafers are used in order to increase the incidence angles and thereby the photon collection efficiency. In order to increase the surface area of multilayers which reflects x-rays at the Bragg angle, we have designed mirrors with the spacing between layers graded along the optic axis in order to compensate for the changing angle of incidence. Likewise, to achieve a large reflecting surface with silicon, the wafers are placed on a specially designed lever arm which is bent into a log spiral by applying force at one end. In this way, the same diffracting angle is maintained over the entire surface of the wafer, providing a large solid angle for photon collection.
Software Development for X-Ray Microbeam Spectroscopy
Authors: Rindby A. , Voglis P. , Nilsson G. , Stocklassa B.
Published: March 2019

Software has been developed for performing image reconstruction of analytical results from an X-ray microbeam spectrometer. The software system has been developed on a conventional IBM-AT compatible computer and runs under WINDOW 3,0 system. The interactive part is developed as a complete “window-style” program where the operator controls the sample movement, the MCA and the micrograph image from the microscope.

A description of the spectrometer and the software system is given. Applications of the technique in analysing documents are presented.
Scanning X-Ray Analytical Microscope using X-Ray Guide Tube
Authors: Shimomura Shuichi , Nakazawa Hiromoto
Published: March 2019

A scanning X-ray analytical microscope was constructed using X-ray guide tube(XGT). XGT is a glass capillary which guides and focuses x-rays by total external reflection at the inner wall. The nature of X-ray beam passed through XGT is varied depending on the form of XGT. The cylindrical and conical types were used for the present setup. A small area (10μm × 10μm) of the sample was irradiated by the X-ray microbeam formed by XGT. Fluorescent and diffracted X-rays from the small area were detected by SSD. By scanning the sample in the plane normal to the X-ray microbeam, the intensity distributions of such secondary x-rays were measured and used as picture elements for constructing x-ray mapping images. The sample was a thin-section of an old chinaware. The images suggest a wide application of this instrument.
XRF and Other Surface Analysis Techniques
Authors: Russ John C.
Published: March 2019

Most users of X-Ray Fluorescence analysis (XRF) are accustomed to thinking of it as a bulk analysis method, and certainty in many cases it does report the representative average composition of the sample. But whereas the trace analysis of lead in gasoline may extend to a depth of several cm., that for a light element in a moderately absorbing matrix may take place only within a few micrometers of the surface, placing severe demands on the specimen preparation method to produce a surface layer representative of the bulk material. XRF is rarely used specifically to analyze surfaces, except for some coating thickness measurements. Nevertheless, many of the same laboratories that rely heavily on XRF are called upon to perform surface analysis for various purposes, and therefore this invited survey paper witt seek to present an overview of some of the major techniques which are available.
Monte Carlo Simulations of XRF Intensities in Samples Containing a Dispersed Phase
Authors: Vrebos B. A. R. , Helsen J. A.
Published: March 2019

For the analysis of solid samples, such as alloys, by means of XRF, one normally assumes that either the samples are completely homogeneous, or that heterogeneity effects can be neglected or cancelled out. The authors have studied this effect by means of Monte Carlo Simulations. Two particular geometries have been studied. For the first simulations the sample consisted of alternating lamellae of different composition, perpendicular to the irradiated surface. Later, the more realistic distribution of a spherical dispersed phase in a matrix was simulated.
K-Edge X-ray Fluorescence Analysis for Actinide and Heavy Elements Solution Concentration Measurements
Authors: Camp David C.
Published: March 2019

There are currently no plans for the commercial reprocessing of nuclear fuel in the U.S. This is not the case in Japan, England, France, Germany, or the USSR. The U.S. does, however, include the reprocessing of spent nuclear fuel as a part of its defense programs. The Office of Safeguards and Security of DOE's Defense Programs has funded the development and optimization of numerous nondestructive analysis techniques including K-edge x-ray fluorescence analysis. This paper reviews some of the implementation efforts resulting from R&D supported by that office.

In 1979, the concept of using K-edge x-ray fluorescence analysis (K XRFA) for the analysis of actinide solution concentrations was first presented. K XRFA using small radioactive Co-57 sources has been shown to be a practical way to measure actinide solution concentrations in offline, at-line, or on-line configurations. The experimental methodology is elegant and the hardware is simple.
Evaluation of the New Generation of Dual-Anode X-ray Tubes
Authors: Kikkert J. N. , de Koning J. J.
Published: March 2019

Traditionally users of x-ray spectrometers have been forced to optimize their instrument for light element analysis and heavy element analysis through the choice of either a light or heavy element anode. The advent of the rhodium tube brought some relief to this situation, but some compromise was still required. The recent addition of the scandium side-window tube to the range has provided twice the excitation efficiency of the chromium tube, whilst providing an equivalent heavy element performance.

In the past there have been attempts to produce x-ray tubes combining the properties of both light and heavy element tubes. An example of this is the dual-target tube which has two preferentially excited targets (anodes) of different materials constructed side-by-side.
Wavelength Dispersing Devices for Soft and Ultrasoft X-ray Spectrometers
Authors: Arai Tomoya , Shoji Takashi , Ryon Richard W.
Published: March 2019

Spectrographic analysis of light elements by soft and ultrasoft fluorescent x-rays has become a useful technique for many applications of elemental analysis, using single crystals, soap multilayers and a combination of total reflection and filtering.

Instead of the wavelength dispersive method based on Bragg reflection which provides high resolution combined with low reflecting intensity, monochromatization combining total reflection by a selected mirror and an appropriate filter offered an alternative approach in order to increase measurable intensity with reasonable spectral resolution.

Recently, the use of synthetic multilayers, which are prepared by sputter/evaporation techniques, has been introduced for the detection of soft and ultrasoft x-rays. Studies on the use of these new wavelength dispersing devices have been conducted and it has been found that the reflectivity of these devices is very high compared with single crystals and soap multilayers and that their resolving power is fairly good.
Analysis of River Sediments from the Tigre River (Venezuela) by Radioisotope Excited X-ray Fluorescence*
Authors: LaBrecque J. J. , Schorin H. , Rosales P. A.
Published: March 2019

The chemical and mineral analyses of river and stream sediments are often employed for geochemical exploration. Their contents are considered to be representative of part or all of the catchment area. In environmental science the analysis of sediments provides information concerning the hydrochemical and ecological interactions of the water and their changes with time. Local and/or time dependent contamination of water bodies can also be determined by analysis of their sediments.

In this work, we have first performed qualitative elemental scans by both energy dispersive (radioisotope excited) and conventional wavelength dispersive X-ray fluorescence of the different grain size fractions.
The Use of Rapid Quantitative X-ray Fluorescence Analysis in Paper Manufacturing and Construction Materials Industry
Authors: Kocman Vladimir , Foley Linda , Woodger Stanley C.
Published: March 2019

A modern analytical laboratory of a large corporation manufacturing paper, construction materials and chemicals must be sufficiently diversified in methodology to provide accurate results in the shortest possible time. Among other techniques the implementation of an automated “menu” driven wavelength dispersive spectrometer allowed for the setting-up of a variety of quantitative X-ray fluorescence methods.
Fundamental Parameters vs. Multiple Regression Calculations for the Determination of Europium in Oxide Catalyst Supports by XRF
Authors: Kenny Eva M. , Brittain Harry G.
Published: March 2019

Fundamental parameters calculations are used for the analysis of europium in the concentration range of 0.1 WT% to 30.0 WT% in the oxidic catalyst supports alumina, calcia, magnesia lanthania, and thoria. The precision and accuracy of this method is dependent on how the sample matrix is defined in the fundamental parameters program and the number and concentration of the standards used. Results comparable to the multiple regression method are obtained when the matrix stoichiometry is defined as Eu2O3 and the catalyst oxide (i.e. Al2O3 etc). It is also necessary to use standards which bracket the europium concentration in the samples. When these conditions are met, the results are comparable to those obtained from a ten point multiple regression calibration curve but with a considerable saving of standard preparation time. The precision is better than ±2% relative. The % relative difference between the fundamental parameters and multiple regression results is also 2%. Data is presented which illustrates the effect of defining the sample stoichiometry in the XRF11 computer program.
TSX-PLUS Multi-Tasking Upgrade for the Nicolet L-11 Powder Diffraction System
Authors: Fitzpatrick J. , Queen David L.
Published: March 2019

In August of 1982, a single-user, dual-translator, automated powder diffraction system was purchased by the Denver Research Institute for use on project work in the Chemical and Materials Sciences Division. Within a short period of time, the system had already become saturated with users. Scheduling conflicts arose around the need for one user to be reducing data while another was acquiring or the need of a user to begin a data collection run on one goniometer after another had already been started. In view of these problems, an answer was sought in the form of hardware and software changes which would allow many users access to the system simultaneously, either for the purpose of data collection, data reduction or program development. A low-cost, minimum impact solution was eventually found which we feel, has significantly increased the utility of the basic L-11 system without sacrificing either flexibility or speed.
Low Thermal Expansion of Alkali Zirconium Phosphates Using a Microcomputer Automated Diffractometer
Authors: Lenain G. E. , McKinstry H. A. , Limaye S. Y.
Published: March 2019

The thermal expansion of ceraptic materials has become a property of interest to more people recently since the desirability of a thermally stable space platform was recognized. The interest in low thermal expansion materials in the past has been driven mildly by the recognition that low thermal expansion will foster good thermal shock resistance. The tradition of the ceramics industry for nearly one hundred years has been that zircon and cordierite were the low expanding materials. Fused silica has long been recognized for its low expansion. But when in 1947 Hummel (1957, I960) found ultra-low-expanding bodies in the lithium aluminum silicates with spodumene and later β-eucryptite structures, a new kind of phenomena had been introduced. Roy (1949), Roy, Roy and Osborn (1950) and Roy and Osborn (1959) provided much of the crystal chemical and phase diagram background on this family.
Total-Reflection X-ray Fluorescence of Thin Layers on and in Solids
Authors: De Boer D. K. G. , van den Hoogenhof W. W.
Published: March 2019

The angular dependence of Total-reflection X-Ray Fluorescence intensities can behave in various ways. The variety is discussed by examining the x-ray intensity distribution in the material under investigation. It is shown that for thin layers on solids, interference fringes are present due to x-ray standing waves. This phenomenon is exploited to determine the depth distribution of elements in layered specimens.
Trace Element Analysis of Solutions at the PPB Level
Authors: Meltzer Carl , King Bi-Shia
Published: March 2019

We have developed a technique to determine the dissolved solid components of water and other liquids by Energy- Dispersive X-Ray Fluorescence (EDXRF) spectrometry. The liquid samples are presented to the spectrometer as small dried spots of the residue remaining after evaporation of the liquid. The dried residues are mounted on thin plastic films cemented to 35 mm plastic slide mounts. Elements from sodium through uranium are detected with detection limits less than one nanogram in favorable cases. Precision of the measurement is better than 2 % relative in favorable cases for secondary-target excitation, and is typically 5 to 10 % for direct excitation given the geometry of the instrument. Detection limits are as low as a part per billion relative to the original liquid for solutions whose total dissolved solid content is 1000 part per million or less.
Current and Future Energy Dispersive EXAFS Detector Systems
Authors: Derbyshire G. E. , Helsby W. I. , Dent A. J. , Wright S. A. , Farrow R. C. , Greaves G. N. , Morrell C. , Baker G. J.
Published: March 2019

This paper presents a review of the current status of photodiode array systems adapted for Energy Dispersive EXAFS (EDE) using a synchrotron radiation source. The performance of a conventional Reticon PDA is compared with that of a hybrid CCD. The specification of a new detector system for EDE is discussed in the light of experience gained with current linear detectors.