X-Ray Spectrometry

Current research reports and chronological list of recent articles.

The international scientifc journal 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.

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Additional research articles see Current Chemistry Research Articles. Magazines with similar content (spectroscopy):

 - Analytical Chemistry.

 - Journal of Analytical Atomic Spectrometry.

X-Ray Spectrometry - Abstracts

Comparison of standard-based and standardless methods of quantification used in X-ray fluorescence analysis: Application to the exoskeleton of clams

In this work, we aim at achieving the most accurate quantitative determination of the composition of exoskeletons of bivalves from Tagus estuary with Energy Dispersive X-ray Fluorescence. Samples from the shells of clams ranging from the Bronze Ages to the 16th century A.D. belonging to the Museu Arqueológico de Almada, and also from the shells of clams collected recently in the same region, were analyzed for comparison of the trace element composition and detection of heavy metals. The analysis was performed with 2 Energy Dispersive X-ray Fluorescence setups, one with triaxial geometry and another with a conventional geometry and vacuum capabilities. Samples were pressed as pellets, and the spectra collected with both setups were evaluated using standardless fundamental parameter based software's implemented in each setup, and by comparing with standard reference materials of similar matrix. The comparison of the results obtained with different methods lead to the conclusion that the most realistic results were obtained with calibration curves obtained with external standards and correction the fluorescent intensities with the Compton scattering peak. When comparing the obtained concentrations for all the analyzed periods, results showed a decrease of Fe in the 12th Century. Regarding the environmental current state of the Tagus estuary, there were no heavy metals detected above the safety regulations.
Datum: 07.11.2017

Prototype GaAs X-ray detector and preamplifier electronics for a deep seabed mineral XRF spectrometer

Work towards developing a prototype GaAs based X-ray fluorescence spectrometer focusing on the detector-preamplifier system for in situ characterisation of deep seabed minerals is presented. Such an instrument could be useful for marine geology and provide insight into hydrothermal processes. It would also be beneficial for deep sea mining applications. The GaAs photodiode was electrically characterised at 4 °C (ambient seawater temperature) and 33 °C. A system energy resolution (full width at half maximum) at 5.9 keV of 580 eV at 4°C, limited by the dielectric noise, broadening to 680 eV at 33°C, was recorded. The spectral performance of the system was characterised across the energy range 4.95 keV to 21.17 keV, at 33°C, using high-purity X-ray fluorescence calibration samples excited by a Mo target X-ray tube. The charge output from the system was found to be linear with incident photon energy. The energy resolution was found to broaden from 695 eV at 4.95 keV to 735 eV at 21.17 keV, attributed to the increasing Fano noise with energy. The same X-ray tube was used to fluoresce an unprepared manganese nodule (revealing the presence of Mn, Fe, Ni, Cu, Zn, Pb, Sr, and Mo) and a black smoker hydrothermal vent sample (containing Fe, Co, Ni, Cu, Zn, Pb, and Mo). Such a spectrometer may also find use in future space missions to study the hydrothermal vents that are believed to exist in the oceans of Jupiter's moon Europa.
Datum: 03.11.2017

XRF characterization and source apportionment of PM10 samples collected in a coastal city

In the current study, a yearlong measurement campaign was conducted during the year 2012 in a medium sized coastal Greek city, Patras. PM10 samples were collected once every 3 days, and a number of those samples were analyzed by the use of a commercial X-ray fluorescence system, Epsilon 5 by PANalytical, The Netherlands. PMF model was used for source identification. Because the uncertainty of the measurements is used as input in the model, special emphasis was given in its accurate estimation. Seven PM10 emission sources were identified using PMF 5.0 and were, namely, mineral dust (15%), road dust (4.6%), shipping emissions (3.8%), sea salt (11.9%), biomass burning (6.9%), traffic (46.2%), and sulfates (11.6%). The concentration weighted approach was used to investigate if the contributions of the sources identified in the area are affected by long range transportation events. A methodology of estimating the uncertainty of the day to day source contributions is proposed in this study. A comparison between the 24-hr contribution for the mineral dust factor provided by the model and the calculated contributions for the same factor deduced from appropriate equations (chemical reconstruction) can be used for this purpose. The analysis showed that when the concentrations of the elements associated with the mineral dust source are close to their lowest value, the model assigns zero contribution to the mineral dust source. Following this methodology in the current study, 6 points were identified as bad fitting points, a number that represents less than 10% of the total measurements.
Datum: 02.11.2017

Archaeometric study of possible Ninevite-5 pottery from upper Tigris region using SEM-EDS, PEDXRF, and OM

This study aims to reveal the production technology of some representative samples of possible Ninevite-5 potsherds which are generally dated between the Early Jezirah I to EJ-II/EJ-III periods (roughly 3000–2500 bc) and accepted as the typical ceramics reflecting the northern Mesopotamian culture in the first half of the 3rd millennium BC. The samples were selected from the archeological excavation area of Kuriki (upper Tigris region, Turkey) and exposed to multiple analytical techniques including scanning electron microscopy with an energy dispersive spectrometer, optical microscopy, and polarized energy dispersive X-ray fluorescence spectrometry. The results showed that all the samples have high amounts of CaO (up to 29.83 wt.%) indicating use of calcareous clay deposits and they have an analogous chemical compositions in terms of both major oxides and trace elements which implied the use of the same raw materials. The vitrification degrees of the samples, examined by back scattered electron images, suggested that the firing temperature of the potsherds did not exceed the range of 800–900°C. It was also revealed that the firing atmosphere was oxidative which would be attributed to use of kiln firing rather than a bonfire or pit firing. Both the chemical and petrographic results suggested that the investigated samples presumably belong to a regional (upper Tigris) production rather than a local one.
Datum: 30.10.2017

Issue Information

No abstract is available for this article.
Datum: 12.10.2017

Role of the mass attenuation coefficient database in standardization of a silicon drift X-ray detector for PIXE analysis

A simple, inexpensive procedure is described for calibrating a silicon drift detector-based PIXE system for the analysis of geological and other “thick-target” materials. It rests on the use of single element, chemical compound, and National Institute for Standards and Technology multielement standards. Much less effort has been focussed on the impact of mass attenuation coefficients on PIXE's analytical accuracy than on ionization cross sections and fluorescence yields. The calibrated system enables us to investigate the effects of inserting different mass attenuation coefficient datasets into the GUPIX database. For the K X-rays of light elements, accuracy is significantly improved by replacing the formerly used XCOM self-attenuation coefficients by the corresponding FFAST values; this effect decreases rapidly with increasing atomic number. Similar improvement was found for L X-rays of medium-Z, but not for high-Z atoms.
Datum: 27.09.2017

Utilization of nondestructive techniques for analysis of the Martian meteorite NWA 6963 and its implications for astrobiology

Martian meteorites are excellent study materials for understanding the present and past of Mars, as they are important historical astrophysical artifacts because they possess information about Martian geological evolution and physical and chemical characteristics. In our case, we analyzed the NWA 6963 Martian meteorite classified as basaltic shergottite because of its chemical structure. A computerized microtomography (μCT) study in the NWA 6963 Martian meteorite provided us with 2D and 3D images that were extremely useful for ascertaining the internal structure of the analyzed sample and gave us the opportunity to find a crumpled material with a very peculiar structural format. In addition, it was possible to observe through the μCT that this encrusted material also has a completely different density of the meteorite. Calcium, strontium, and potassium were detected qualitatively, among others through the technique of X-ray fluorescence.
Datum: 25.09.2017

Size-resolved analysis of fine and ultrafine fractions of indoor particulate matter using energy dispersive X-ray fluorescence and electron microscopy

We used a multistage PIXE inertial impactor with nine different aerodynamic diameter ranges (between 16 and 0.06 μm) to sample indoor particulate matter (PM). X-ray fluorescence (XRF) measurements performed at cutoff diameters (CoDs) of 0.25, 0.5, 1, 2, 4, and 8 μm were used to identify elements in various size fractions. Anthropogenic sources were the dominant sources for fine and ultrafine particle sizes. The XRF results show that natural sources also contribute to the fine and ultrafine fractions of pollutants. Scanning electron microscopy and energy-dispersive system analysis were performed on membranes having PM CoDs of 4, 2, 1, 0.5, and 0.25 μm. Elemental mappings show the membranes with PM of CoDs 0.25 and 0.5 μm having S as a dominant element, confirming the results obtained with XRF. Strong correlation among maps of S, N, and O show that ammonium sulfate is the major constituent at these size fractions. Other elements such as Si, Ca, Fe, Al, and Mg show up in smaller amounts at these size fractions but increase for membranes with larger particles. For size fractions larger than 0.5 μm, there is a good correlation between the elemental maps of these elements and oxygen, indicating that these elements exist mostly in oxide forms. The absence of clear N signals and the correlation between the Ca and S maps indicate that S in these size fractions is not due to ammonium sulfate. The presence of Mg, K, Cl, and Na at these CoDs shows that these elements are due to salts originating from sea breeze.
Datum: 22.09.2017

An upgraded external beam PIXE setup for multielemental analysis of atmospheric aerosol samples

The external beam particle-induced X-ray emission (PIXE) setup has been upgraded by introducing a new silicon drift detector with the aim of obtaining better minimum detection limits (MDLs) at the 2 × 1.7 MV Tandetron accelerator of the Beijing Normal University in China. The upgraded external beam PIXE setup is equipped with two silicon drift detectors for PIXE analysis of low and high Z elements. A surface barrier detector for Rutherford backscattering spectrometry monitors beam and helium flow. Two kinds of aerosol filter samples (quartz fiber filters and Teflon filters) were studied. A 200-μm thick Mylar absorber in front of the medium-high energy X-rays detector was adopted, and it got the best MDLs for atmospheric aerosol samples analysis. Multielemental analysis of quartz fiber filter aerosol samples was achieved. For more accurate and better MDLs of low Z elements in PIXE analysis, it is necessary to keep sufficient helium flow behind the thin samples.
Datum: 15.09.2017

Study of gamma/X-ray interaction in Kondo insulators

We have studied the gamma/X-ray interaction parameters such as mass attenuation coefficient, mean free path (λ), half value layer, 10th value layer, energy-absorption buildup factors, and variation of electrical conductivity with the energy of gamma/X-ray between 1 keV and 100 GeV for Kondo insulators such as FeSi, Ce3Bi4Pt3, SmB6, YbB12, CeNiSn, CeRhSb, CeRuSn, and CeFeP. The variation of photon interaction parameters with incident energy of gamma/X-ray is graphically represented. We have also identified the X-ray absorption edges for the Kondo insulators. This identified X-ray absorption edges are useful in the characterizing of Kondo insulators such as FeSi, Ce3Bi4Pt3, SmB6, YbB12, CeNiSn, CeRhSb, CeRuSn, and CeFeP. Hence, these data are also useful in the material science. This type of data for Kondo insulators is not available in literature. Hence, this work is first of its kind, and it is useful in various fields of nuclear physics.
Datum: 15.09.2017

High concentration measurements of U and Pu with nondestructive and standardless K-edge densitometer device

In nuclear activities such as reprocessing plants, safeguard laboratories, or research centers, U and Pu are regularly analyzed. Fast and accurate analytical devices are favored such as K-edge densitometer. This paper presents the results obtained by this device from assay samples with high U and Pu concentrations. Two processing methods without calibration (except energy calibration) are compared and discussed. Despite literature advising against the use of estimated mass attenuation coefficients for near edge energy, this study shows that these values can contribute to very good results for uranium and plutonium concentration estimations, with a bias less than 1%.
Datum: 14.09.2017

Pigments characterization of polychrome vases production at Lipára: New insights by noninvasive spectroscopic methods

One of the most impressive Sicilian pottery production is attributed to the so-called Lipari Painter and his followers, whose vessels—found in the archeological site of Lipari (Aeolian Island, Sicily)—are decorated with characteristic blue, red, and white figures. From the archeological point of view, these artworks keep open many questions concerning dating, production technique, and cultural background. In this context, new data on the manufacture procedures and on the raw materials used for the pigments may contribute to a deeper comprehension of this early Hellenistic vase tradition. The preciousness of the vessels, exhibited at the Archeological Museum of Lipari, imposed the use of in situ nondestructive methods to address new insights on the nature of the colored layers. Thus, analyses by Raman and X-ray fluorescence spectroscopy have been performed with portable instruments on a selection of vessels certainly attributed to Lipari Painter and to some others of his followers. The results of this study testify the use of different pigments: kaolin and gypsum, probably supplied locally, for white layers; Egyptian blue for blue hues; red ochre for brown-reddish hues; and cinnabar for pink and red-purple nuances. The identification of both Egyptian blue and cinnabar opens an interesting discussion about dating and circulation of the raw materials.
Datum: 11.09.2017

A sample carrier for measuring discrete powdered samples with an ITRAX XRF core scanner

The elemental composition of discrete powdered sediment samples can be measured by the energy-dispersive X-ray fluorescence (XRF) system that is installed in XRF core scanners. Because an appropriate sample carrier for powdered samples is currently not available, for example, for the ITRAX XRF core scanner, such a carrier is presented in this technical note. The designed sample carrier can hold 30 sample cups with a volume of 0.88 cm3 each. A maximum of 5 sample carriers, that is, 150 samples, can be measured in one run. The sample cups and carriers are optimized for a measurement procedure with a step size of 5 mm and variable count times up to 100 s per sample. With this setting, data are collected from an area of 100 mm2 in the center of the sample thereby ensuring a good representativeness of the signal because potential sample inhomogeneity is accounted for. Because the described sample carrier system allows rapid element analyses of discrete powdered environmental samples with an XRF core scanner, it may in some cases represent a time- and cost-efficient alternative to conventional XRF analyses.
Datum: 11.09.2017

Determination of effective atomic numbers and mass attenuation coefficients of samples using in-situ energy-dispersive X-ray fluorescence analysis

The matrix effect has a major impact on energy-dispersive X-ray fluorescence analysis (EDXRFA) and is difficult to be evaluated due to that the contents of some low-atomic-number elements cannot be identified by in-situ EDXRFA. Up to today, the fundamental parameter algorithm proposed by Rousseau has been widely applied to correct the matrix effect. Accordingly, determining the matrix and mass attenuation coefficient (μ/ρ) of sample is a key issue for the fundamental parameter algorithm. In present work, the method to deduce μ/ρ by effective atomic number (Zeff) was studied. First, the relationship between Zeff and coherence to Compton scatting ratio (R) of the incident X-ray was determined by standard samples. Then, we deduce Zeff and their μ/ρ. The value of μ/ρ deduced by our method is in good agreement with that calculated by WinXCOM, and the relative change (Δ) is less than 7%. We also deduced Zeff and their μ/ρ of Chinese national standard soil samples employing our method and good agreement with the calculated values were also obtained. We found that the agreement between experimental values of μ/ρ with theoretical values by WinXCOM still exists when the energy of the incident X-ray is greater than 4 keV, and the Δ is less than 10%. The result indicates that our method may be applied directly to in-situ EDXRFA.
Datum: 24.08.2017

Characterization of ashes from greenhouse crops plant biomass residues using X-ray fluorescence analysis and X-ray diffraction

A characterization of ashes obtained by thermal treatments on greenhouse crops plant biomass residues is presented. The chemical analysis, by X-ray fluorescence (wavelength-dispersive X-ray fluorescence), and phase analysis, by X-ray diffraction, of the resultant ashes are reported. Thermal treatments of selected samples of these residues increase the relative amounts of inorganic Mg, Si, P, and S in the ashes, being these amounts as high as increasing temperature. As an opposite effect, Na, Cl, and K contents decrease as increasing temperature by a volatilization process of the chlorides, as confirmed by X-ray diffraction. The crystalline phase analysis of the ashes demonstrates the formation of inorganic constituents of the biomass, including alkaline chlorides and calcium salts (calcite, anhydrite, and apatite). Progressive thermal treatments induce the formation of new silicate phases (akermanite and grossularite) and silica (α-quartz and cristobalite). Furthermore, the particle size of the starting biomass samples does not influence the evolution of the crystalline phases by thermal treatments. In contrast, a previous leaching using water and subsequent heating at 1,000 °C produces the formation of periclase (MgO), lime (CaO), and the silicate gehlenite, without the presence of anhydrite. This study is interesting for future investigations on the residues as a profitable biomass source for energy production and sustainable large-scale management. Some potential applications of the resultant ashes can be proposed.
Datum: 18.08.2017

Synchrotron radiation induced X-ray production cross sections of 66Dy at energies across its Li (i = 1–3) subshell absorption edges

The X-ray production (XRP) cross sections for the 66Dy Lk (k = l, α, η, β2,6,7,15, β1,6, β1,3,4,6, β2,7,15, γ1,5, γ2,3) emission lines have been measured by tuning the incident synchrotron radiation at energies over the range 7.8–9.2 keV and ~10–370 eV above the respective Li (i = 1–3) absorption edges. These measurements aim to check the reliability of the independent particle approximation models used to generate the theoretical data sets of different physical parameters required to calculate the XRP cross sections and also investigate the influence of many body effects on the photoionization process. The measured values have been compared with 4 sets of XRP cross sections calculated using the Dirac–Fock model-based X-ray emission rates, 2 sets of the Li (i = 1–3) subshell photoionization cross sections deduced from the self-consistent Dirac–Hartree–Fock model-based values and the nonrelativistic Hartree–Fock–Slater model-based values, and 2 sets of the fluorescence (ωi) and Coster–Kronig (fij) yields. The present measured Lγ2,3 (originating from decay of the L1 subshell vacancies) XRP cross sections are found to be significantly higher than different sets of theoretical values, whereas a good agreement is generally observed for the various other XRP cross sections and relative intensities.
Datum: 04.08.2017

Mercury in archeological hair samples from Xiongnu burials (Noin-Ula, Mongolia): SR XRF and CXRM analysis

A technique has been developed for determining mercury content in the concentration range of 1–1000 μg/g in hair samples by X-ray fluorescence analysis using synchrotron radiation (synchrotron radiation X-ray fluorescence, Siberian Synchrotron and Terahertz Radiation Center, Budker Institute of Nuclear Physics SB RAS). The mercury content was identified in archeological hair samples from an ancient burial of Xiongnu nobility (Mongolia, mound 22, 1st century BC–1st century AD); the content values were elevated (up to 1100 μg/g) in all the samples (n = 41). An X-ray microanalysis using polycapillary lenses in a confocal scheme (confocal X-ray microscopy station) was developed at the Synchrotron radiation X-ray fluorescence to establish mercury distribution in a cross section of hair shaft with a spatial resolution of 5 μm. The findings of the study make it possible to assume exogenous income of mercury (from the burial environment) to the hair.
Datum: 27.07.2017

The energy dispersive scheme of X-ray fluorescence analysis with a crystal polarizer and polycapillary optics

The efficiency of the polarization scheme based on polycapillary optics and a diamond crystal polarizer was demonstrated. The scheme provides suppression of the background of scattered radiation in measuring X-ray fluorescence spectra. A quasi-parallel X-ray beam with an angular divergence of 4.2 mrad was formed by a microfocus source with a copper anode and polycapillary half-lens. Simultaneous polarization and monochromatization of radiation was obtained with a crystal of natural diamond, which was set at the diffraction reflection (113). The degree of polarization of CuKα1 spectral line and the maximum radiation flux were respectively equal to 99.86% and 5 · 106 photon/s. In the direction orthogonal to the plane of diffraction, the maximum attenuation of the background was up to 19 dB.
Datum: 12.07.2017

Novel sample treatment procedures for the determination of phosphorus in Cu-based alloys using X-ray fluorescence spectrometry to solve the microstructural effect issue

The accurate analysis of hard CuP and CuPAg-type solders using X-ray fluorescence spectrometry is a difficult task. Surface milling, the most common sample preparation method for calibration materials, results in poor accuracy for the phosphorus analysis, as evidenced by the unacceptable values of the root mean square error. Meanwhile, the analysis of real samples provides incorrect results, and microstructural effects are the main source of error. Thus, this effect was negated by considering the information depth of the phosphorus Kα line and the microstructure size of the alloys. Phosphorus was measured using a thin layer of the sample (a thickness of several micrometers). As a result, the analyzed layer was a poor representative of the sample. Two different approaches for solving the microstructural effect issue were proposed. In the first method, the alloy was remelted under controlled conditions to obtain fine-grain samples, which successfully limited the microstructural effects. The second solution used specially prepared thin layer samples, and the sample dissolution eliminated the microstructural effect. Using the developed sample treatment methods resulted in an improvement in the accuracy of the phosphorus calibration curves. This allowed for the correct determination of phosphorus and other alloying elements in the Cu-based alloys with low uncertainties.
Datum: 12.07.2017

PIXE-based detection of elemental accumulation during direct organogenesis in Blepharispermum subsessile DC.: An endangered medicinal plant of Odisha, India

Particle-induced X-ray emission was used to investigate mineral accumulation during different developmental stages of direct organogenesis from cotyledon explants of Blepharispermum subsessile beginning from shoot bud initiation and formation to in vitro regenerated roots. Mineral uptake and accumulation appeared selective and varied between different stages of shoot bud initiation and formation (Stage 1), proliferation of leafy shoots (Stage 2), and in vitro regenerated roots (Stage 3). The concentrations of 2 macro elements, K and Ca, were found in higher quantity during proliferation of shoot buds to leafy shoots stage suggesting their role in cell division, bud formation, and multiplication of the plant. Most of the micronutrients such as Mn, Fe, Ni, Cu, and Zn were found to be accumulated in higher quantities in in vitro regenerated roots, as they provide the plant with a larger surface area and hence a greater potential for mineral uptake. The results of particle-induced X-ray emission test suggest that the information on the accumulation of elements during developmental stages in vitro could be useful for formulating a media for the induction of high-frequency regeneration of in this important endangered medicinal plant species for its ex situ conservation.
Datum: 10.07.2017

Optimization of L-shell X-ray fluorescence detection of lead in bone phantoms using synchrotron radiation

Closely related toxicity and retention mechanisms of lead (Pb) in the human body involve the bone tissues where Pb can accumulate and reside on a time scale ranging from years to tens of years. In vivo measurements of bone Pb can, therefore, play an important role in a comprehensive health risk assessment of Pb exposure. In vivo L-shell X-ray fluorescence (LXRF) measurement of bone Pb was first demonstrated over 4 decades ago. Implementation of the method, however, encountered challenges associated with low sensitivity and calibration procedure. In this study, the LXRF measurement was optimized by varying the incident photon energy and the excitation-detection geometry. The Canadian Light Source synchrotron radiation was used to compare 2 different excitation-detection geometries of 90° and 135° using 3 different X-ray photon energies: 15.8, 16.6, and 17.5 keV. These energies optimized excitation of the L3 subshell of Pb and simulated the most intense K-shell emissions of zirconium, niobium, and molybdenum, respectively. Five rectangular plaster-of-Paris bone phantoms with Pb concentrations of 0, 7, 17, 26, and 34 μg/g, and one rectangular 3.1-mm-thick resin phantom mimicked the X-ray attenuation properties of human bone and soft tissue, respectively. Optimal LXRF detection was obtained by the 15.8-keV energy and the 90° and 135° geometries for the bare bone and the bone and soft tissue phantoms, respectively.
Datum: 29.06.2017

Improved Rayleigh to Compton scattering ratio curves for mass attenuation coefficients determination for X-ray fluorescence analysis

Nondestructive assays are essentials for certain types of sample materials, and, among those, the X-ray fluorescence technique enables the determinations of stable elements, and there is an increasing effort on the development of equipment to suit the various needs. Nevertheless, a great difficulty on the analysis of unknown materials' composition is to account for self-absorption of the fluorescence photons that must be considered in the elemental concentration calculation. The correlation between the Rayleigh to Compton scattering ratio to the mass attenuation coefficient has proved to follow a single polynomial function for the first 20 elements of the periodical table with a correlation factor higher than of 0.998 for the sixth order function. The Rayleigh to Compton scattering ratios for pure elements and the 22.16 keV photons, the main energy from an X-ray tube with silver anode, were determined with the MCNP6 Monte Carlo computer code. Two scattering angles were considered. Reference samples were measured, and the calculated results were compared to the literature values of the mass attenuation coefficient for some known samples and showed to be within 20% for de 90° scattering angle. Only Lucite was slightly above 20%. Curve fit coefficients are also presented for the 7.11- and 17.40-keV photon energies.
Datum: 22.06.2017

Quantitative speciation of manganese oxide mixtures by RIXS/RRS spectroscopy

Resonant inelastic X-ray scattering, also named X-ray resonant Raman scattering, was recently used to discriminate local chemical environments. By means of this novel technique, the speciation of samples could be attained in a variety of samples and experimental conditions. Until now, this discrimination methodology had been applied only to pure compounds, being the speciation possible by two different mathematical treatments. Nevertheless, the effectiveness/sensitivity of this technique has not been tested yet in samples containing mixtures of oxides of the same element. In this work, the first results of quantitative speciation of mixtures of manganese compounds, using resonant inelastic X-ray scattering/X-ray resonant Raman scattering spectroscopy, are presented. The results show that it is possible to discriminate and quantify oxide mixtures of the same element in slightly different proportions, allowing a quantitative speciation of compound mixtures in a variety of experimental conditions, presenting also several advantages over conventional spectroscopic techniques. Copyright © 2017 John Wiley & Sons, Ltd.
Datum: 13.06.2017

Evaluation of metal release from battery and electronic components in soil using SR-TXRF and EDXRF

Potentially toxic elements may be leached contaminating the soil, surface, and ground water due to the improper disposal of batteries and electronic devices. The objective of this study was to evaluate metal release from batteries and electronic components deposited in specific receptacles filled with soil in which acid rain was simulated. The leachate solution and the soil were analyzed by synchrotron radiation total reflection x-ray fluorescence and benchtop energy dispersive x-ray fluorescence, respectively. Results indicate that batteries released K, Mn, Fe, Cu, Zn, and Pb and electronic component released Ti, Mn, Fe, Cu, Zn, and Pb. For batteries' leachate test samples, higher amounts of Fe, Cu, Mn, Zn, and Pb have been released compared with electronic component ones under same the experimental conditions. The Fe, Cu, and Pb concentrations in battery leachate test samples were above their National Environment Council maximum permitted values (MPV) and in the electronic waste leachate ones, only the Pb concentrations was above MPV. For soil sample containing batteries K, Mn and Zn presented higher concentrations, mainly at the 10-cm topsoil, ranging from 0.16 to 0.50, 0.27 to 8.67, and 0.03 to 1.26, in % (% w/w), respectively. The Zn–C battery soil samples present similar behavior to the alkaline ones. The impact due to the Pb release was higher in the soil test samples with electronic components, in which their concentrations ranged from 51 to 394 mg/kg, above its MPV up to 28-cm soil layer. The X-ray fluorescence techniques employed were suitable for water and soil environmental evaluation.
Datum: 07.06.2017

Confocal macro X-ray fluorescence spectrometer on commercial 3D printer

Novel confocal X-ray fluorescence (XRF) spectrometer was designed and constructed for 3D analysis of elementary composition in the surface layer of spatially extended objects having unlimited chemical composition and geometrical shape. The main elements of the XRF device were mounted on a moving frame of a commercial 3D printer. The XRF unit consists of a silicon drift detector and a low-power transmission-type X-ray tube. Both the excitation and secondary X-ray beams were formed and regulated by simple collimator systems in order to create a macro confocal measuring setup. The spatial accuracy of the mechanical stages of the 3D printer achieved was less than 5 μm at 100-μm step-size. The diameter of the focal spot of the confocal measuring arrangement was between 1.5 and 2.0 mm. The alignment of the excitation and secondary X-ray beams and the selection of the measuring spot on the sample surface were ensured by two laser beams and a digital microscope for visualization of the irradiated spot. The elements of the optical system together with the XRF spectrometer were mounted on the horizontal arm of the 3D printer, which mechanical design is capable of synchronized moving the full spectroscopic device within vertical directions. Analytical capability and the 3D spatial resolution of the confocal spectrometer were determined. Copyright © 2017 John Wiley & Sons, Ltd.
Datum: 31.05.2017

Synchrotron XANES and ED-XRF analyses of fine-paste ware from 13th to 14th century maritime Southeast Asia

The combination of energy dispersive X-ray fluorescence (ED-XRF) and synchrotron X-ray absorption near-edge structure (XANES) provides the detailed composition of fine-paste ware (FPW) kendis, dated back to 13th–14th century maritime Southeast Asia. Sources of clay and production sites were classified according to Al2O3, SiO2, α-Fe2O3 and γ-Fe2O3 as well as trace elements. The similarities based on these components provided another evidence of a trade route between Kota Cina in North Sumatra of Indonesia and Kok Moh on Satingphra Peninsula, a well-known production area in present-day Thailand. In additions, the uniquely large contribution of α-Fe2O3 in XANES spectra suggests that Nakhon Si Thammarat province of Thailand could also be one of FPW production areas in maritime Southeast Asia. Copyright © 2017 John Wiley & Sons, Ltd.
Datum: 17.05.2017

A device for X-Ray elemental mapping using annular radioisotope source

An energy-dispersive system is described for elemental mapping by X-ray fluorescence spectrometry. The present study describes the design of an X-ray fluorescence spectrometer and presents its performance in elemental mapping applications. The spectrometer is based on a new ring-shaped collimator with a pinhole in the center of it and a ring-shaped Am-241 isotope mounted in the collimator as a source for excitation of X-ray fluorescence. The photons were detected by high-resolution Si (Li) detector coupled to a multi-channel analyser and cooled by liquid nitrogen. In this study, we used two samples; one of them was made from pure elemental powders, and the second one was a piece of a stone and three types of maps were plotted. In the maps type one, the areas of the elements were shown with a single color. These maps only show the location of the elements in the sample. In the maps type two, the area of each element was shown with different colors because of the count (intensity) related to the area. In the third type of the maps for each element, depending on the elements' position on the sample, the counts were plotted in three dimensions. The areas with higher intensity have greater height, and areas with lower intensity have lower altitude. These two last types of maps provide information about the homogeneity or heterogeneity of the elemental distribution in the samples. The spectrometer can perform non-destructive analyses of samples and objects in the air. Copyright © 2017 John Wiley & Sons, Ltd.
Datum: 16.05.2017

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