bluuebunny/crossref_metadata_2025_split huggingface dataset:
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.
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

AbstractFundamental 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.
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

AbstractThe 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.
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

AbstractThis 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.
Niobium Concentration Measurement in Steel Samples with TXRF
Authors: Hegedüs F. , Winkler P. 
Published: March 2019

In nuclear power plants the fast neutron fluence on the pressure vessel (PV) inner wall is measured by the scraping sampling method (1). As the inner plating of the pressure vessel contains 0.5 - 0.6 % of niobium, 93mNb (tt/2 = 16a) isomer is produced by the reaction 93Nb (n, n’). The activity of 93mNb is related to the fast neutron fluence.Scraping samples (few hundred of mg) were taken from the PV inner wall. The niobium was chemically extracted from steel by using a HAP column. This extraction was needed to reduce matrix effects and to avoid interferences of other activities with 93mNb
Mass Absorption Coefficient Determination Using Compton Scattered Tube Radiation: Applications, Limitations and Pitfalls
Authors: Willis J. P. 
Published: March 2019

Trace element determination by X-ray fluorescence spectrometry is subject, like almost all instrumental analytical techniques, to systematic errors, also known as matrix effects. This paper deals with the determination of mass absorption coefficients (MACs), using Compton peak intensities, for the correction of matrix effects arising only from elemental absorption in the sample.When absorption effects are significant the relationship between net analyte peak intensity and concentration will no longer be constant, and corrections will be necessary for accurate analyses.
Quantification of Carbamazepine in Tablets by Powder X-ray Diffractometry
Authors: Suryanarayanan R. 
Published: March 2019

AbstractA powder x-ray diffraction technique has been developed for the quantification of carbamazepine in tablets. The other tablet ingredients were microcrystalline cellulose, starch, stearic acid and silicon dioxide. The tablets were ground in a ball mill and the powder mixed with lithium fluoride (20% w/w) which was the internal standard. Five lines of carbamazepine with d-spacings of 3.38, 3.34, 3.28, 3.26 and 3.23 Å and the 2.01 Å line of lithium fluoride were used for the quantitative analysis. A plot of the intensity ratio (sum of the intensities of the lines of carbamazepine/intensity of die lithium fluoride line) as a function of the weight fraction of carbamazepine in the tablets resulted in a straight line. Using this standard curve, the carbamazepine content in “unknown” tablets was determined and ranged between 98.6 and 101.6% of the actual drug content. The coefficient of variation in the determinations ranged between 0.28 and 2.1%.
Determination of Lattice Parameter and Strain of ϒ' Phases in Nickel-Base Superalloys by Synchrotron Radiation Parallel Beam Diffractometry
Authors: Ohno Katsumi , Ohsumi Kazumasa , Harada Hiroshi , Yamagata Toshihiro , Tamazaki Michio 
Published: March 2019

AbstractThe lattice parameters and strain of ϒ'-phase particles in Nickel-base superalloys, which are duplex type alloys designed for turbine blades and widely called “Ni-base single crystal superalloys”; they are accurately determined by Synchrotron Radiation parallel-beam diffractometry. The superalloys have ϒ' precipitates, an ordered FCC structure based on Ni3Al, in a γ-matrix having disordered FCC structure.In addition, the preparation method of stress-free ϒ'-phase particles, with no composition change in the preparation process, was newly developed to measure the coherency strain of ϒ'-particles due to lattice misfit. The prepared ϒ'-phase particles are similar in composition and form to ϒ'-phase particles in the γ-matrices. The method for determining of the lattice misfit between the γ and γ’ particles was previously reported.
Interdependence of X-Ray Diffraction and X-Ray Fluorescence Data
Authors: Jenkins Ron 
Published: March 2019

Current versions of the J.C.P.D.S. Powder Diffraction File Include some 26,000 standard patterns and this number is Increasing at the rate of around 1500 patterns per year. Although the actual number of patterns still represents a relatively small fraction of the total number of phases possible, it does include the majority of well known phases. A variety of search/match schemes have been designed under the auspices of the Joint Committee on Powder Diffraction Standards and these include data retrieval methods based both on hand and computer searching.Since the majority of analytical problems involve multiphase materials, one of the greatest problems in qualitative identification is the “unscrambling” of the various phase patterns to allow matches to be made with standard patterns of pure materials.
Analysis of Agglomerate and Slag by Energy Dispersive X-Ray Fluorescence
Authors: Ratyński W. , Cieślak E. , Karwowski H. , Parus J. , Tys J. , Dworak B. 
Published: March 2019

A rapid analytical procedure for simultaneous determination of Ca, Mn and Fe in agglomerate and slag has been developed.A 100 mCi annular source of 238Pu has been used for excitation and Si(Li) detection system with ADC coupled with minicomputer for data acquisition and processing. A modified Heinrich-Rasberry procedure has been applied for analytical results evaluation. The measurement of each sample consumes about 100 s and the data processing time is 20 s approximately. The peaks were integrated in a fixed number of channels and linear background was subtracted. Seven standard samples both of slag and agglomerate have been used for system calibration.
Spectrochemistry in the Iron Foundry: X-Ray Fluorescence vs. Optical Emission
Authors: Gast Richard 
Published: March 2019

The casting of iron is largely a chemical process: that is, the chemistry of molten iron greatly influences the properties of finished castings. Other parameters - casting design, mold integrity, inoculation practice, pouring temperature, and shakeout procedure - are also vital to consistent production. But if the chemistry is wrong, the probability of defective castings is high. For this reason, control of chemical composition has long been a major objective of foundrymen.To be useful for either process control or quality assurance checking, analytical work must be reliable and accurate. Data should also be available in a minimal period of time to make possible the on-line adjustments necessary to achieve proper chemistry, and thus the desired properties, in the final castings.
Evaluation of Pulse Pileup Rejection
Authors: Russ John C. , Sandborg Alan O. 
Published: March 2019

Comparisons of energy- and wavelength-dispersive spectrometry inevitably focus on the count rate limitations of the ED electronics. In some cases the use of amplifiers without pulse pileup rejection, or worse, misadjusted pileup rejection circuits, has led to erroneous results and assumptions regarding maximum tolerable count rates which are far too low.Proper evaluation of pileup rejection must consider both the count rate and energy dependence of the circuits. For example, using a typical ED spectrometer (EDAX, 154 eV, 10 mm2, 6 μsec amplifier time constant) we can first measure the total amplifier throughput curve as shown in Figure 1. This curve is only slightly dependent on photon energy, at least over the range from about 1-10 keV which usually contains the major part of the X rays, and shows a maximum stored count rate of slightly over 3000 cps for an input count rate of slightly less than 10,000 cps. Changing the amplifier shaping time constant will change the scale of the curve, but not its general shape.
Frequency Shift of L-Valence Band Spectra of Niobium and Tin in Nb3Sn Compound
Authors: Wald S. S. , Cheng S. K. 
Published: March 2019

Soft X-ray L-emission spectra of tin in second order diffraction and of niobium in first order have been studied in pure elements, in oxides, and in intermetallic Nb3Sn compound.The study was done by a newly designed soft X-ray vacuum spectrograph. The curved crystal spectrograph is of the Johann type mounting. The radius of curvature of the bent crystal was 50.8 cm. The essential parts of the instrument are (i) an interchangeable bent crystal holder so that the spectrograph can cover a wide range of energy spectra by using crystals of different d-spacings to obtain highest resolution for the particular wavelength range; (ii) an adjustable Hartmann slit to control the effective width of the bent crystal; (iii) a half-shadow device to take two spectra onto the same film in the lower and upper half of the film; (iv) a sharp edge metal fixed to the Rowland circle to obtain a fiducial mark on the film; (v) a water-cooled rotatable Cu anode target; and (vi) a filament with both translational and rotational freedom to ensure optimum beam focusing.
Stress-Depth Profiles in Magnetron Sputtered Mo Films Using Grazing Incidence X-Ray Diffraction (GIXD)
Authors: Ballard B. L. , Predecki P. K. , Braski D. N. 
Published: March 2019

AbstractIntrinsic stresses as a function of σ, the 1/e penetration depth were measured for a smooth, 1μm thick, fine grained, cylindrical post magnetron sputtered molybdenum film deposited on a vycor glass substrate in the dynamic deposition mode. Using grazing incidence diffraction and the Mo (321) reflection, lattice spacing profiles were determined for τ values from 200-4400 Å. The in-plane intrinsic stresses parallel and perpendicular to the post axis were determined employing the ϕ-integral method and assuming elastic isotropy. The results were related to the surface structure and composition profiles via atomic force microscopy (AFM) and auger electron spectroscopy (AES) respectively.
Resolving Common Element Problem by Using Different Lines in Fundamental Parameters Method Multilayer Thin Film Analysis
Authors: Feng Liangyuan 
Published: March 2019

The presence of one or more common elements in different layers often complicates or hampers the analysis of a multilayer thin film system. Some constraints or preconditions are usually required in order to reach a mathematical solution. For example, either the concentration(s) of the common element(s) in, or the thickness(es) of one of the relevant layers must be known.An alternative approach is the use of more than one analyzing line for the element in question. Although this approach has long been proposed, there have been no detailed studies seen in literature. An attraction of using this approach is that it requires no prior knowledge of either the concentration or the thickness. The author has implemented this approach, and studied in detail its feasibility and pitfalls for practical applications.
High Accuracy Analysis of BPSG Thin Films on Silicon Wafers by X-Ray Wafer Analyzer
Authors: Kohno H. , Arai T. , Araki Y. , Wilson R. 
Published: March 2019

The wafer analyzer has been used to fulfil many applications needs in the semiconductor industry. The prominent features of the XRF method for the semiconductor industry are:analysis of many types of films, e.g., oxides, silicides and metallic alloys, and simultaneous analysis of film thickness and compositions.In the past, the analysis results of BPSG (Boron-doped Phospho-Silicate Glass) films, with thicknesses greater than 4000 Å, were reported. With the recent increased demand for larger scale and higher quality semiconductor devices (larger than 64 Mbit), more accurate analysis with high precision has been required.
Evaluation of σ33 From Diffraction Experiments Performed With Synchrotron Radiation in the Ω - and Ψ - Goniometries
Authors: Detempte I. , Ruppersberg H. 
Published: March 2019

AbstractA formalism which was proposed by Ruppersberg (1992) for a self consistent evaluation of stress gradients in the case of strongly varying σ33(T) stresses is applied for studying the variation of the stress components with distance z from the irradiated surface of a ground hardened steel plate.
Thickness Gauging of Organic Films on Large Plastic Body Parts With an Xrf Probe Based on a Roomtemperature Mercuric Iodide Detector
Authors: Buckens Pierre F. , Iwanczyk Jan S. , Wang Yuzhong J. , Marano Richard S. 
Published: March 2019

AbstractThe variability of adhesion promoter (primer) film thickness has been identified at Ford Motor Company as an important factor in maintaining the quality of paint on exterior plastic body parts. XRF offers unique advantages for non-destructive film monitoring. Monitoring of large parts for process control requires a non-contact approach using a small mobile probe. Previous attempts to implement a practical XRF gauging probe have been hampered by the choice of available x-ray detection technologies; proportional counters cannot resolve the layer's fluorescent lines properly and suffer from instability, while Si(Li) or Ge detectors need cooling to low temperatures, which makes their usage impractical for mobile probe.The recent commercial availability of state-of-the-art Mercuric Iodide (HgI2) x-ray detectors led to the development of a lightweight XRF probe that contains an x-ray tube and a HgI2 detector. Thickness measurements of primer films on plastic substrates were characterized, and 15 sec. acquisition yielded precision of 0.225 and 0.525 pm for film thicknesses of 5 and 20 µm respectively. Ti was added to the substrate and Cr to the film as tagging elements. A ratiometric technique, taking into account absorption of the Ti signal in the film, yields excellent linearity and compensates for instrumental errors such as sampleto- probe distance variation and x-ray source fluctuations.
Investigation Of Geometrical Effects in X-Ray Microfluorescence Analysis of Geological Samples
Authors: Lankosz Marek , Pella Peter A. 
Published: March 2019

AbstractGeometrical effects occur when primary x-rays irradiate a mineral inclusion which lies close to the boundary between it and a surrounding mineral having a different chemical composition. An investigation of one of these near-edge effects was performed in the case when x-ray microfluorescence is applied for analysis. Analytical mathematical expressions were developed to correct for this effect and were tested exper imentally.
A New Method for Fast XRPD Using a Position Sensitive Detector
Authors: Göbel Herbert E. 
Published: March 2019

The scanning speed of powder diffractometers can be increased by about two orders of magnitude by replacing the normal detection system (receiving slit/scintillation counter) by a linear position sensitive detector (PSD) which collects diffracted x-rays of a larger part of the diffractometer measuring arc simultaneously. The velocity increase is proportional to the section of the arc 29 in which the diffracted x-rays are detected. With respect to the Bragg-Brentano focussing geometry, a range of several degrees (typically 5°) can be tolerated without affecting the resolution remarkably. Diffractograms over extended angular regions of 2θ are received by slewing the PSD continuously along the arc while the diffracted x-rays are accumulated with their accurate 2θ angle address on a digital base.The method has been named the continuous position sensitive detection technique (CPSD). With this technique, diffraction patterns with similar quality (resolution, linearity, peak/background ratio) as conventional, scintillation counter recorded diagrams can be received at slewing rates of several hundred degrees per minute. Additionally, the CPSD technique augments the number of crystallites contributing to the diffraction intensity by the same amount, thus producing much better crystallite statistics for quantitative measurements.
Some Studies of Chlorinated Poly(Vinyl Chloride) Using X-Ray Photoelectron Spectroscopy
Authors: Gianelos James , Grulke Eric A. 
Published: March 2019

Chlorinated poly(vinyl chloride) (CPVC) is similar in many ways to its thermoplastic parent poly(vinyl chloride) (PVC), Chlorination imparts superior high temperature properties, which make CPVC preferable for many and varied applications.Our primary purpose in studying CPVC with x-ray photoelectron spectroscopy (XPS) was to see whether we could gain insight into how chlorine substitutes into the PVC molecule. We also hoped we would obtain insights into the chlorination reaction itself, and how variations would affect the final product.
A Combined Derivative Method for Peak Search Analysis
Authors: Huang T. C. , Parrish W. 
Published: March 2019

AbstractA comprehensive study of derivative methods for the peak search analysis of X-ray diffraction data was made to determine the relative merits of the methods. The peak positions were best determined by the cubic first derivative method which had an intrinsic error ≤ 0.001°, and random error ∼ ± 0.003 ° to 0.02 ° depending on the counting statistical noise. The quadratic/cubic second derivative method had the highest resolution with a separation limit ≥ 1/2w (w = full width at half maximum). An effective algorithm combining the cubic first derivative and the quadratic/cubic second derivative methods was developed for high precision and resolution. The method uses a full screen menu for parameter selection, and the entire peak search analysis including peak identification and position determination, and graphic and numeric display of results at the color terminal is completed in a few seconds using a time sharing mode on an IBM 3083 central processing unit. The combined derivative method should be also applicable to other spectra such as gamma-rays, X-ray fluorescence, optical, infrared, ESCA, Mossbauer, etc.