X-Ray Spectrometry - Current Research Articles

Current research articles: X-ray Spectrometry

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X-Ray Spectrometry - published by Wiley

X-Ray Spectrometry is devoted to the rapid publication of papers dealing with the theory and application of x-ray spectrometry using electron, x-ray photon, proton, gamma and gamma-x sources. Covering advances in techniques, methods and equipment, this established journal provides the ideal platform for the discussion of more sophisticated X-ray analytical methods.

Current articles of the journal:

Parametric X-ray radiation as a novel source for X-ray imaging

A novel X-ray source based on parametric X-ray radiation (PXR) has been put into practical use at the Laboratory for Electron Beam Research and Application (LEBRA), Nihon University, Japan. The PXR beam has been generated from a Si single crystal irradiated by a 100-MeV electron beam from a linac at the LEBRA. In this study, phase-contrast imaging experiments using a diffraction-enhanced imaging (DEI) method have been carried out by using the parametric X-rays at an energy of 17.5?keV. The successful images obtained by the DEI method have shown detailed inner structures of soft biological tissues more clearly as compared with those by conventional absorption radiography. Given the significant properties of the LEBRA PXR source, i.e., compact system, large X-ray beam irradiation field of approximately 80?mm in diameter and quasi-monochromaticity, the result suggests a possible construction of a compact linac-driven PXR-DEI device and application to medical diagnoses. Copyright © 2012 John Wiley & Sons, Ltd.

Posted on 15 May 2012 | 4:20 am

A total reflection X-ray fluorescence method for the determination of chlorine at trace levels in nuclear materials without sample dissolution

A total reflection X-ray fluorescence (TXRF) method for the determination of chlorine at trace levels in nuclear fuel samples is described. Chlorine present in trace concentrations in nuclear fuel materials such as U3O8, (U,Pu)C, PuO2 and Pu-alloys was first separated from the solid matrix by pyrohydrolysis as HCl and was collected in 5?mM NaOH solution. This solution was analyzed for chlorine by TXRF spectrometry using Cl K? analytical line excited by W L?. Cobalt was used as internal standard. The precision for such chlorine determination was found to be within 27% (n?=?4) when the analysis was carried out in air atmosphere. This could be improved to 8% by making TXRF measurement in flowing helium atmosphere. The results obtained from TXRF determinations were also compared with those obtained from ion chromatography (IC) and were in good agreement. The collection of distillate during pyrohydrolysis in NaOH helped in counterchecking loss of chlorine during TXRF sample preparation. The average deviation of TXRF-determined values in helium-purged TXRF measurements with IC determined values (as chloride) was 15% at a chlorine concentration level in the range of 1–70?µg/mL. Copyright © 2012 John Wiley & Sons, Ltd.

Posted on 14 May 2012 | 7:50 pm

Refractive X-ray shape memory polymer 3D lenses with axial symmetry

Parabolic 3D refractive lenses from shape memory polymers were manufactured and tested using monochromatic X-rays of 10?keV. Four lenses in two sets with focal distances of about 6 and 4?m were used. The lens optical properties in terms of resolution, efficiency and gain were measured. The radiation stability test was performed. Copyright © 2012 John Wiley & Sons, Ltd.

Posted on 14 May 2012 | 7:49 pm

Loose-powder technique for X-ray fluorescence analysis of ancient pottery using a small (100?mg) powdered sample

A molded-loose-powder technique using a small powdered sample (100?mg) was developed for the X-ray fluorescence analysis of 22 components (Na2O, MgO, Al2O3, SiO2, P2O5, K2O, CaO, TiO2, MnO, Fe2O3, V, Cr, Ni, Cu, Zn, Rb, Sr, Y, Zr, Nb, Ba, and Pb) in ancient pottery. This loose powder specimen was prepared by pressing the small powdered sample into a sample holder, formed from a stainless steel disk (48-mm diameter?×?0.8-mm height) with a hole (11-mm diameter), by hand. Calibration standards were prepared by homogenizing chemical reagents containing these 22 analytes using the concentration ranges of 166 ancient potteries and three clay materials from Japan. The calibration curves of these benchmark mixtures exhibited a good linearity (correlation coefficient, r?=?0.990–1.000), accuracy, and reproducibility compared with those of other synthesized specimens and three reference standards. The lower limits of detection were less than tens of mg?kg?1 (e.g., 94?mg?kg?1 for Na2O, 11?mg?kg?1 for P2O5, 1.1?mg?kg?1 for Rb, and 0.9?mg?kg?1 for Y). Using the present method, we determined 22 components in two prehistoric potteries from Japan. The advantage of this method is that only a small amount of sample is required, which can be prepared easily and rapidly and reused for other analyses. Copyright © 2012 John Wiley & Sons, Ltd.

Posted on 11 May 2012 | 7:40 am

Discrepancies in atomic shell and fluorescent X-ray energies in the Evaluated Photon Data Library EPDL97

There are significant differences between the atomic orbital energies listed in the evaluated photon data library EPDL97 and values published elsewhere. In particular, comparisons with the values adopted by the National Institute of Standards and Technology (NIST) show discrepancies up to several hundred electron volts. Although the uncertainties in the EPDL97 atomic orbital energies were recognised by the original authors, the library has subsequently been widely adopted as a primary source of photon transport and atomic relaxation data. We compare experimentally measured X-ray fluorescence spectra with fits using the EPDL97 and NIST line energies. Our results strongly favour the NIST energies for K-shell and L-shell fluorescent X-rays and show that the EPDL97 atomic orbital energy values should not be used for applications, such as X-ray fluorescence, where atomic relaxation phenomena are important. Copyright © 2012 John Wiley & Sons, Ltd.

Posted on 8 May 2012 | 4:21 pm

An etched multilayer as a dispersive element in a curved-crystal spectrometer: implementation and performance

Etched multilayers obtained by forming a laminar grating pattern within interferential multilayer mirrors are used in the soft X-ray range to improve the spectral resolution of wavelength dispersive spectrometers equipped with periodic multilayers. We describe the fabrication process of such an etched multilayer dispersive element, its characterization through reflectivity measurement and simulations, and its implementation in a high-resolution Johann-type spectrometer. The specially designed patterning of a Mo/B4C multilayer is found fruitful in the range of the C K emission as the diffraction pattern narrows by a factor 4 with respect to the non-etched structure. This dispersive element with an improved spectral resolution was successfully implemented for electronic structure study with an improved spectral resolution by X-ray emission spectroscopy. As first results, we present the distinction between the chemical states of carbon atoms in various compounds, such as graphite, SiC and B4C, by the different shape of their C K emission band. Copyright © 2012 John Wiley & Sons, Ltd.

Posted on 3 May 2012 | 2:02 pm

The perspective of new multi-layer reference materials for confocal 3D micro X-ray fluorescence spectroscopy

Multi-layered components are commonly used in hi-tech branches of modern industry. This fact generates a need for suitable reference materials for experimental examination of such specimens, and it also induces the development of mathematical procedures for quantification. To reveal experimentally the chemical composition of (multi-)layered specimens in 3D space in a non-destructive way, a confocal 3D micro X-ray fluorescence spectroscopy (3D ?XRF) can be employed. The scope of this paper covers preparation, preliminary experimental examination and quantification of new, multi-layer stack systems as the perspective of reference materials to be used in 3D ?XRF spectroscopy. The prepared stacks consist of nine individual layers based on a low-Z organic matrix loaded alternately with Cu2O and ZnO oxides. The stacks are characterized by the homogeneous areal distribution of inorganic fillers and the constant thickness of distinguishable layers to the extent of millimeters. A Monte Carlo (MC) simulation was used to reconstruct the chemical composition, mass density and thickness of individual layers within the stacks. Results of the simulation accurately reflected the nominal mass shares of fillers and the thickness of layers additionally determined by optical microscopy and 2D ?XRF scanning. The prepared stack systems seem to be suitable materials for the validation of mathematical procedures for the quantification of multi-layer specimens examined by depth-sensitive X-ray techniques. Copyright © 2012 John Wiley & Sons, Ltd.

Posted on 20 April 2012 | 7:55 am

Direct observation of fractional change of niobium ionic species in a solution by means of X-ray absorption fine structure spectroscopy

Local coordination of niobium oxalate in oxalic acid solutions was investigated by Nb L3-edge X-ray absorption near edge structure (XANES) spectroscopy that was sensitive to the coordination environment of X-ray absorbing atoms. The Nb L3-edge XANES spectra were measured from solutions of difference pH, and the solution was composed of different molar fractions of NbO(C2O4)2H2O? and NbO(C2O4)33?. The lower energy shift of the spectral peak was observed with the lower pH that was attributed to the greater fraction of NbO(C2O4)2H2O?. The spectral shape was different from those of reference samples representing tetrahedral and octahedral coordination, and the lower symmetry of niobium site was confirmed. The XANES spectra of two ionic species were simulated with the density functional theory calculations, and the mixture of these spectra demonstrated the peak shift caused by the change of solution pH. Copyright © 2012 John Wiley & Sons, Ltd.

Posted on 20 April 2012 | 7:00 am

Determining the elemental composition of Calotropis procera using X-ray Analytical Microscopy

Caloptropis procera (Oshar) is a desert plant that did not receive much attention from the science community. The objective of this study was to investigate the elemental composition of the different parts of the plant using an X-ray analytical microscope, to identify the elements naturally present in the plant and in the future detect the presence of any contaminants absorbed by the plants from the surrounding environment. Stalks, leaves and flowers from three Oshar plants were qualitatively and quantitatively analyzed. Leaves were scanned to establish the elemental spatial distribution within individual leaves. Subsequently, parts of the plants were dried, crushed and pulverized, then analyzed to determine elemental concentrations. The major elements present throughout the plant were Cl, K and Ca with varied concentrations. Other elements (Mg, Si, P, Fe, Sr, Mn and Br) are present in the leaf with various low concentrations of <5%. Major, minor and trace elements present in the various plant parts were determined. The outcome of this study will be used as a pilot for further investigations pertaining to the utilization of the Oshar plant for environmental cleaning purposes. Copyright © 2012 John Wiley & Sons, Ltd.

Posted on 31 March 2012 | 7:07 am

Calculation of X-ray tube spectra by means of photon generation yields and a modified Kramers background for side-window X-ray tubes

Popular X-ray tube models available in the literature, i.e. ‘Pella’, ‘Ebel’, and ‘Finkelshtein and Pavlova’, are systematically evaluated with the focus on the estimation of the associated uncertainties. Also taken in consideration and compared is our recent semi-empirical own approach already employed in our lab. This has been working for the common target elements rhodium, molybdenum and tungsten and was further extended in the present work for the target elements copper, chromium and vanadium. By using a modern scanning electron microscope/energy dispersive spectroscopy (SEM/EDS) system this time, higher performances such as stability of the beam current and especially the better energy resolution of the EDS have enabled the reliable extension of our own X-ray tube spectrum approach into the low-energy range, due to increasing interest. Hence, also the more challenging X-ray lines of copper, chromium and vanadium L-series lying in the energy range below 1–2?keV are included into the model. Such low-energy L-lines or, e.g. M-lines of tungsten, are not treated explicitly by the other existing popular algorithms for the nowadays widely used geometries of side-window tubes, offering a unique virtue to our present, modern approach. With our own model, a measurement uncertainty of the X-ray tube spectra (considering the uncertainties associated with the SEM beam current, the detector acceptance solid angle and efficiency of the spectrometer) within 15% has been estimated. The validation of the approach is demonstrated with metrological measurements with a calibrated SEM/EDS system geometrically configured as a side-window X-ray tube. Copyright © 2012 John Wiley & Sons, Ltd.

Posted on 30 March 2012 | 9:53 am

Contribution of bremsstrahlung of free electrons to formation of the background component for NaK X-ray fluorescence

Bremsstrahlung of free electrons (photo, Auger and Compton electrons) that occur in an irradiated sample is compared with probable components of the radiation background, such as diffuse scattering of the sample radiation by the analyzing crystal, X-ray fluorescence of the analyzing crystal and high orders of Bragg's reflection of the polychromatic primary radiation scattered in the sample under study. The comparison is performed within a range of NaK? line. It is revealed that response functions, represented by experimental intensities of background samples, are in good agreement with calculated summary values of the background intensity. The contributions of bremsstrahlung of free electrons to the formation of the background component of the analytical signal are estimated within the considered range of the X-ray fluorescence spectrum. Copyright © 2012 John Wiley & Sons, Ltd.

Posted on 19 March 2012 | 11:01 am

Analysis of K-absorption extended X-ray absorption fine structure data of some transition metals

A simplified method of analysis of the extended X-ray absorption fine structure (EXAFS) data is presented. The experimental EXAFS data for cobalt, manganese, chromium, iron and zinc have been analyzed to illustrate the procedure. Theoretical EXAFS data have been generated using standard EXAFS equation employing MathCAD programming. The phase shift parameter has been computed from experimental spectra itself, the backscattering amplitude has been taken from the available theoretical tabulations and other parameters have been taken from crystallographic data. The theoretical EXAFS data agree well with the experimental data. Fourier transforms of both the experimental and theoretical data have been computed, and the two Fourier transforms agree well with each other in case of all the metals. The analysis yields bond length of the first coordination shell that agrees well with the crystallographic value in the metals under consideration. Copyright © 2012 John Wiley & Sons, Ltd.

Posted on 19 March 2012 | 10:58 am

On the 40th anniversary of the journal X-Ray Spectrometry

This journal, X-Ray Spectrometry, celebrates its 40th anniversary this year. The state of the publications on X-ray spectral analysis from 1972 onward is considered. The distribution of materials over countries is presented, as published in X-Ray Spectrometry for 40?years, in 5-year time intervals: 1972–1976, 1977–1981, and so on. The participation of Russian scientists contributing to the publications in this journal is discussed. Copyright © 2012 John Wiley & Sons, Ltd.

Posted on 13 March 2012 | 6:53 am

Three-dimensional density measurements of ultra low density materials by X-ray scatter using confocal micro X-ray fluorescence spectroscopy

Targets used in high energy density physics experiments, such as those fielded at the National Ignition Facility, are typically made of multi-component systems that include metals, metal coatings, and very low density materials. These very low density materials with densities as low as ~10?mg/cm3 must have uniform density throughout. Characterizing their density in 3D is a very difficult problem. One technique used is confocal micro X-ray fluorescence. This technique, which uses a polycapillary optic to focus the X-rays from the X-ray source and another on the detector, measures the density of these materials based upon their X-ray scatter. In order to gain a complete picture of their X-ray scatter, the sample is rastered in 3D to generate a complete 3D density map. As proof of technique, the examination of very low density poly(styrene-divinylbenzene) foams, poly(methylpentene) foams, as well as silica aerogels were completed. Results for the polymer foam materials show a linear correlation (R2?=?0.99) between X-ray scatter intensity and bulk density. However, for higher atomic number materials (e.g. aerogels) the amount of X-ray scatter is very dependent upon the depth of data collection as a result of the absorption of the X-rays by the upper portions of the sample. This self-absorption reduces the ability of this technique to quantify the density of the material in full 3D. Self-absorption modeling will be required to compensate. Scans through the aerogel surface indicate an increased density at the surface due processing. Finally, a 3D image of a machined aerogel tube is presented. Copyright © 2012 John Wiley & Sons, Ltd.

Posted on 7 March 2012 | 8:33 pm

Chemical bonds and elemental compositions of BCxNy layers produced by chemical vapor deposition with trimethylamine borane, triethylamine borane, or trimethylborazine

BCxNy films were produced from single-source precursors in a chemical vapor deposition process. The boranes were introduced as precursors at low pressure conditions and at a temperature of 700?°C, whereas the borazine was handled at 400?°C and with a plasma enhancement at an electrical power input of 40?W. Additionally, as inert or reactive gases, H2, He, N2, and NH3, respectively, were used. The films deposited on Si(100) substrates were chemically characterized by X-ray photoelectron spectroscopy and by synchrotron radiation-based total-reflection X-ray fluorescence combined with near-edge X-ray absorption fine structure and quantified elementally by energy-dispersive X-ray spectroscopy. The results are critically compared. With the application of boranes without NH3, compounds with a dominating carbidic character were identified, whereas with the addition of NH3 to the boranes, a nitridic character was prevalent. In case of using borazine for the synthesis, the nitridic character was found at the application of all auxiliary gases. For both groups stoichiometric formulas derived from energy-dispersive X-ray spectroscopy are proposed: B3.5–4C4N2–2.5 for the carbidic region and B3.5C1.5N5 for the nitridic region. Copyright © 2012 John Wiley & Sons, Ltd.

Posted on 7 March 2012 | 8:21 pm

Energy dispersive X-ray fluorescence analysis of archeological metal artifacts from the Final Bronze Age

Energy dispersive X-ray fluorescence (EDXRF) is widely used in the study of archeological metal artifacts, heritage and art history, where the fragile nature of the objects requires the use of noninvasive techniques such as the EDXRF, which in addition, is fast and very affordable.An EDXRF analysis of copper-based artifacts from Late Bronze Age metal hoards from Central Portugal is presented.The EDXRF measurements were carried out by using an X-ray tube with a Mo anode and a commercial Si-PIN detector. The data acquisition was performed by keeping small distances between the X-ray window, the sample and the detector. Both patinated and polished areas were analyzed: the relative composition of the artifacts was inferred from the fluorescence spectra obtained. Copyright © 2012 John Wiley & Sons, Ltd.

Posted on 7 March 2012 | 8:20 pm

Similarity between blackbody and synchrotron radiation analyzed by Tsallis entropy

It is believed that blackbody and bremsstrahlung are completely different phenomena. However, their spectral shapes are somewhat similar to each other. We demonstrate that synchrotron radiation spectra, which are relativistic magnetic bremsstrahlung, can be approximated by blackbody radiation through Tsallis entropy under the dulite gas approximation at Tsallis non-extensive parameter q?=?1.05. The error of mean square is 4?×?10?6 within the range of 5?×?104?eV without adjusting any parameters. This approximation will be applied to more complex bremsstrahlung such as an X-ray tube. Copyright © 2012 John Wiley & Sons, Ltd.

Posted on 20 February 2012 | 9:05 pm

An accurate determination of the K-shell X-ray fluorescence yield of silicon

A measurement of the K-shell fluorescence yield of silicon is undertaken in which identified sources of systematic errors in previous measurements are reduced or eliminated. This enables a stringent test of the only two sets of theoretical predictions available for atomic numbers less than 18. Our result ?K?=?0.0495?±?0.0015 is very slightly lower than the non-relativistic Hartree-Fock-Slater (HFS) prediction of 0.0514. This stringent test of the HFS predictions helps to refine the fundamental parameter database of the X-ray fluorescence analysis technique, whose importance for light elements is increasing. Our work indicates the need for new theoretical calculations of K-shell fluorescence yields for these elements. Copyright © 2012 John Wiley & Sons, Ltd.

Posted on 9 February 2012 | 4:13 pm

Undersized (12.5?mm diameter) glass beads with minimal amount (11?mg) of geochemical and archeological silicic samples for X-ray fluorescence determination of major oxides

The small glass bead technique was developed to assay precious silicic samples for geochemical and archeological analyses. Undersized (12.5?mm diameter) glass beads were prepared for wavelength dispersive X-ray fluorescence determination of major oxides (Na2O, MgO, Al2O3, SiO2, P2O5, K2O, CaO, TiO2, MnO, and total Fe2O3). Synthetic calibration standards were prepared by compounding chemical reagents (oxides, carbonates, and diphosphate). For reliable calibration, recipe compositions of standard specimens were constructed on the basis of the evenness of plot intervals on a calibration curve. Calibration curves showed good linearity (correlation coefficient: r?>?0.998). Analytical results of major oxides in granitic and basaltic rocks, obsidian, and ancient pottery were obtained with good precision (relative standard deviations were the following: <3% for more than 10.0 mass% of analyte, <5% for 1.0–10.0 mass% of analyte, and <15% for 0.1–1.0 mass% of analyte). Lower limits of detection were roughly a sub-percentage of analyte in an unprepared sample: 0.3 mass% for Na2O, 1.0 mass% for SiO2, 0.01 mass% for MnO, and so on. The present preparation reduced the following analytical scales: (1) amount of sample from 400?mg to 11?mg (97% cutting out), (2) amount of Li2B4O7 as an alkali flux from 4000?mg to 396?mg (90% cutting out), and (3) weight of platinum crucible from 80?g to 12.5?g (84% cutting out). This small-scale preparation might enable us to conduct destructive pretreatment of valuable and limited silicic samples such as archeological ceramics and stone tools, geochemical minerals in rock, and sediments and sand. Copyright © 2012 John Wiley & Sons, Ltd.

Posted on 9 February 2012 | 4:13 pm

Measurement of proton beam fluence by PIXE analysis of residual gas

Knowledge of beam fluence has a crucial role in quantitative particle-induced X-ray emission analysis. In some situations, a direct measurement of the beam charge on the target is either impossible or impractical. In such cases, indirect determination of the beam fluence can utilise the characteristic X-ray of argon or other gases, which was being kept at a stable low partial pressure in the vicinity of the analysed sample. As the X-ray signal of argon depends on the total charge, it can be used to quantify the charge. This paper describes the experimental design, the hardware and software modules that we created, the validation of the method, the application of the method during elemental analyses of fragile philatelic samples with overprints, and the lessons learned. Copyright © 2012 John Wiley & Sons, Ltd.

Posted on 9 February 2012 | 4:11 pm

Role of polarization Bremsstrahlung in the formation of thick target Bremsstrahlung spectra in the energy range of 5–10?keV

Role of polarization Bremsstrahlung in the formation of total Bremsstrahlung (BS) spectra in thick targets of Al, Ti, Sn and Pb, produced by complete absorption of 90Sr beta particles having an energy range of 0–546?keV, are studied in the photon energy region of 5 to 10?keV. The theoretical BS spectral photon distributions, obtained from Elwert corrected (nonrelativistic) Bethe–Heitler theory, a modified Elwert factor (relativistic) Bethe–Heitler theory that describe ordinary Bremsstrahlung (OB) and a modified Elwert factor (relativistic) Bethe–Heitler theory for BS spectra that includes the polarization Bremsstrahlung (PB) into OB in stripped atom approximation, were compared with the experimentally measured BS spectral photon distributions. It has been observed that the experimental results are in agreement with the modified Elwert factor (relativistic) Bethe–Heitler theory at photon energy from 5 to 10?keV. It has been also observed that the contribution of PB into OB decreases with increase in end-point energy of beta emitter and the energy of the emitted photon. Further, it has been found that the contribution of PB into OB increases with increase in atomic number of the target atom. This indicates the importance of PB in the formation of BS produced by continuous beta particle. Copyright © 2012 John Wiley & Sons, Ltd.

Posted on 25 January 2012 | 10:46 am

Chemical analysis of very small-sized samples by wavelength-dispersive X-ray fluorescence

The chemical characterisation of very small-sized samples is often of major interest in forensic analysis, studies of artworks, particulate matter on filters, raw materials impurities, and so on, although it generally poses considerable problems owing to the difficulty of obtaining precise and accurate results. This study was undertaken to develop a set of methods for the chemical characterisation of very small-sized samples by wavelength-dispersive X-ray fluorescence.To conduct the study, sample preparation (as beads and pellets) and measurement conditions were optimised to reach the necessary detection and quantification limits and to obtain the appropriate measurement uncertainty for characterising the types of materials involved. The measurements were validated by using reference materials.Three test methods were developed. In two methods, the samples were prepared in the form of beads (one method being for geological materials and the other for the analysis of nongeological materials such as particulate matter on filters, glasses, frits, and ceramic glazes and pigments). In the third method, the samples were prepared in the form of pellets for the analysis of volatile elements in geological materials. In the three methods, detection limits, quantification limits and measurement uncertainties were obtained similar to those found when a bead or pellet is prepared by the usual methods from 0.5?g sample. However, in this study, sample size was between 30 and 40 times smaller in the case of beads and 100 times smaller in the case of pellets, thus broadening the range of possible wavelength-dispersive X-ray fluorescence applications in the chemical characterisation of materials. Copyright © 2012 John Wiley & Sons, Ltd.

Posted on 25 January 2012 | 10:45 am

Determination of Pb, Zr, Ti, Sr, Cr, Nb and La in lead zirconate titanate ceramics by particle-induced X-ray emission

A particle-induced X-ray emission (PIXE) technique has been used in the determination of the principal components Pb, Zr and Ti and the substituting elements Sr, Cr, Nb and La in lead zirconate titanate ceramics. In general, precision of analysis was concentration dependent from each element under study. For Pb, precision varied between 0.13% and 0.16%, at higher concentration of 59.32–64.5%. It was around 6–9% for Sr, Cr and Nb at concentrations of 1% or lower. Particular attention was devoted to the estimation of the analysis trueness. With this purpose, three methods were applied: (1) comparison of PIXE and inductively coupled plasma optical emission spectrometry concentrations, (2) recovery study and (3) comparison with a laboratory standard. Trueness of analysis was around 100?±?10% for the evaluated elements Pb, Zr, Ti, Sr and Cr. The expected stoichiometry and elemental composition homogeneity of a wide group of produced ceramics were confirmed by the PIXE technique. Copyright © 2012 John Wiley & Sons, Ltd.

Posted on 25 January 2012 | 10:32 am

Determination of Pb, As, Cd and trace elements in polluted soils near a lead–zinc mine using polarized X-ray fluorescence spectrometry and the characteristics of the elemental distribution in the area

Polarization energy dispersive X-ray fluorescence spectrometry was used in the determination of Pb, As and Cd, as well as Cr, Cu, Zn, Ni and other minor and trace elements in the soil samples taken from a polluted area by lead mine exploitation. Two difficulties have to be overcome. One is strong overlap of Pb L? over As K? and another is lack of suitable certified reference materials. The different excitation conditions and analytical lines were tried to reduce the impact of overlap of Pb L? over As K?. When KBr was used as the second target, compared with Zr, the proportion from Pb L? was reduced about six times. Even so, however, the overlap was not reduced enough to be ignored. The inductively coupled plasma atomic emission spectrometry and mass spectrometry methods were used to analyze parts of soil samples and provide data for compensating lack of reference materials. By this method, the analytical concentration range of Pb, As and Cd were significantly extended. The analytical range of Pb, As and Cd were 1.4?µg/g~4.2%, 0.6?µg/g~9.3% and 0.5?µg/g~1500?µg/g, respectively. The high concentrations of Pb, As and Cd were found in the samples in the vicinity of the Pb-Zn mine. The concentrations of Pb, As, Cd, Zn and Cu were higher than the Class III in the Chinese environmental quality standard for soils. The highest concentrations of Pb, As, Cd and Zn in the soil samples were 14?960, 2726, 65 and 9439?µg/g, respectively. Copyright © 2012 John Wiley & Sons, Ltd.

Posted on 23 January 2012 | 12:36 pm

Nondestructive method for the calculation of bulk material composition by X-ray fluorescence, using surface analysis on corroded bronze objects

The formation of patina on the surface of archeological bronze objects is a complex phenomenon, being influenced by various parameters induced by the environment and the alloy composition. Over several years, many attempts have been made to analyze the bulk composition of the alloys by nondestructive surface measurements. In this paper, we propose an analytical approach to evaluate the composition of bronze alloys using neural network analysis and X-ray fluorescence spectrometry. Copyright © 2012 John Wiley & Sons, Ltd.

Posted on 23 January 2012 | 12:34 pm

A critical analysis of the experimental L-shell Coster–Kronig and fluorescence yields data

A critical analysis of the methods used to determine the L-shell Coster–Kronig and fluorescence yield data are given. The collected data sets have a large scatter, indicating methodological issues. The K?-L coincidence technique and the synchrotron ionization methods are analyzed in detail, and it is demonstrated that both methods have unrecognized systematic errors. It is emphasized that the synchrotron measurements clearly show deviations from the exclusively used exponential form of the energy dependence of the photoionization cross-section. Thus, the far-range extrapolation introduces an error, which magnitude is difficult to assess. Comment on the use of polarization-sensitive devices to detect polarized X-ray is offered. New strategies are recommended for the measurement of these parameters. Copyright © 2012 John Wiley & Sons, Ltd.

Posted on 23 January 2012 | 12:34 pm

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