Gaseous detectors for energy dispersive X-ray fluorescence analysis

Science.gov (United States)

Veloso, J. F. C. A.; Silva, A. L. M.

2018-01-01

The energy resolution capability of gaseous detectors is being used in the last years to perform studies on the detection of characteristic X-ray lines emitted by elements when excited by external radiation sources. One of the most successful techniques is the Energy Dispersive X-ray Fluorescence (EDXRF) analysis. Recent developments in the new generation of micropatterned gaseous detectors (MPGDs), triggered the possibility not only of recording the photon energy, but also of providing position information, extending their application to EDXRF imaging. The relevant features and strategies to be applied in gaseous detectors in order to better fit the requirements for EDXRF imaging will be reviewed and discussed, and some application examples will be presented.

Wavelength dispersive X-ray absorption fine structure imaging by parametric X-ray radiation

International Nuclear Information System (INIS)

Inagaki, Manabu; Sakai, Takeshi; Sato, Isamu; Hayakawa, Yasushi; Nogami, Kyoko; Tanaka, Toshinari; Hayakawa, Ken; Nakao, Keisuke

2008-01-01

The parametric X-ray radiation (PXR) generator system at Laboratory for Electron Beam Research and Application (LEBRA) in Nihon University is a monochromatic and coherent X-ray source with horizontal wavelength dispersion. The energy definition of the X-rays, which depends on the horizontal size of the incident electron beam on the generator target crystal, has been investigated experimentally by measuring the X-ray absorption near edge structure (XANES) spectra on Cu and CuO associated with conventional X-ray absorption imaging technique. The result demonstrated the controllability of the spectrum resolution of XANES by adjusting of the horizontal electron beam size on the target crystal. The XANES spectra were obtained with energy resolution of several eV at the narrowest case, which is in qualitative agreement with the energy definition of the PXR X-rays evaluated from geometrical consideration. The result also suggested that the wavelength dispersive X-ray absorption fine structure measurement associated with imaging technique is one of the promising applications of PXR. (author)

Single atom identification by energy dispersive x-ray spectroscopy

International Nuclear Information System (INIS)

Lovejoy, T. C.; Dellby, N.; Krivanek, O. L.; Ramasse, Q. M.; Falke, M.; Kaeppel, A.; Terborg, R.; Zan, R.

2012-01-01

Using aberration-corrected scanning transmission electron microscope and energy dispersive x-ray spectroscopy, single, isolated impurity atoms of silicon and platinum in monolayer and multilayer graphene are identified. Simultaneously acquired electron energy loss spectra confirm the elemental identification. Contamination difficulties are overcome by employing near-UHV sample conditions. Signal intensities agree within a factor of two with standardless estimates.

Energy-dispersive X-ray microanalysis of elements' content and ...

African Journals Online (AJOL)

This study was designed to investigate elements' content and anti-microbial effects of two Malaysian plants, Pereskia bleo and Goniothalamus umbrosus. Elements' analysis was carried out using Energy Dispersive X-ray Microanalysis combined with Variable Pressure Scanning Electron Microscope (EDX, VPSEM).

In-situ and operando characterization of batteries with energy-dispersive synchrotron x-ray diffraction

Science.gov (United States)

Paxton, William Arthur

Batteries play a pivotal role in the low-carbon society that is required to thwart the effects of climate change. Alternative low-carbon energy sources, such as wind and solar, are often intermittent and unreliable. Batteries are able capture their energy and deliver it later when it is needed. The implementation of battery systems in grid-level and transportation sectors is essential for efficient use of alternative energy sources. Scientists and engineers need better tools to analyze and measure the performance characteristics of batteries. One of the main hindrances in the progress of battery research is that the constituent electrode materials are inaccessible once an electrochemical cell is constructed. This leaves the researcher with a limited number of available feedback mechanisms to assess the cell's performance, e.g., current, voltage, and impedance. These data are limited in their ability to reveal the more-localized smaller-scale structural mechanisms on which the batteries' performance is so dependent. Energy-dispersive x-ray diffraction (EDXRD) is one of the few techniques that can internally probe a sealed battery. By analyzing the structural behavior of battery electrodes, one is able to gain insight to the physical properties on which the battery's performance is dependent. In this dissertation, EDXRD with ultrahigh energy synchrotron radiation is used to probe the electrodes of manufactured primary and secondary lithium batteries under in-situ and operando conditions. The technique is then applied to solve specific challenges facing lithium ion batteries. Diffraction spectra are collected from within a battery at 40 micrometer resolution. Peak-fitting is used to quantitatively estimate the abundance of lithiated and non-lithiated phases. Through mapping the distribution of phases within, structural changes are linked to the battery's galvanic response. A three-dimensional spatial analysis of lithium iron phosphate batteries suggests that evolution

A low cost multi-purpose experimental arrangement for variants in energy dispersive X-ray fluorescence analysis

International Nuclear Information System (INIS)

Nascimento Filho, V.F.; Silva, R.M.C.; Moraes, L.M.B.; Parreira, P.S.; Appoloni, R.C.; Silva, R.M.C.

2005-01-01

Based in an X-ray tower with four exits (two line and two point beams) experimental conditions were arranged to carry out variants in energy dispersive X-ray fluorescence analysis: (1) the conventional one (EDXRF), with excitation/detection of thin and thick samples, under vacuum and air atmosphere, (2) the X-ray energy dispersive micro- fluorescence analysis(μ-EDXRF), with 2D mapping, using a quartz capillar, (3) the total reflection X-ray fluorescence (TXRF), under He and air atmosphere, and (4) secondary target/polarized X-ray fluorescence (P-EDXRF). It was possible to use a Cu, Mo or W target on the X-ray tube, with or without filter (V, Fe, Ni and Zr), and Si(Li) or Si-PIN semicondutor detectors coupled to a multichannel analyzer. In addition, it was possible to use the point beam to carry out experiments on (5) X-ray radiography and (6) X-ray absorption, and the line beam on (7) X-ray diffractometry studies.

Analysis of kiwi fruit (Accented deliciosa) by energy dispersive X-ray fluorescence spectra

International Nuclear Information System (INIS)

Oliveira, Ana Claudia S.; Oliveira, Marcia L. de; Silva, Lucia C.A.S.; Arthur, Valter; Almeida, Eduardo

2011-01-01

The search for a healthy life has led consumers to eat fruits and vegetables in place of manufactured products, however, the demand for minimally processed products has evolved rapidly. The kiwi has at least eight nutrients beneficial to health: calcium, magnesium, manganese, phosphorus, iron, potassium, sodium and has also high vitamin C, which has wide acceptance in consumer markets. Energy dispersive spectroscopy X-ray (EDX) is the analytical technique used for elemental analysis or chemical characterization of a sample. It is a variant of fluorescence spectroscopy X-ray based on the sample through an investigation of interactions between electromagnetic radiation and matter, analyzing X-rays emitted by matter in response to being struck by charged particles. The aim of this study were to determine potassium, calcium, iron and bromine (K, Ca, Fe and Br, respectively) present in kiwifruit using the technique of fluorescence X-ray energy dispersive (EDXRF). Kiwifruit were peeled, washed and cut into slices and freeze-dried. After drying the sample was held digestion and subsequent reading of the same equipment in the X-ray fluorescence energy dispersive (EDXRF). The results indicated that the contents of potassium, calcium, iron and bromine are present in kiwifruit as expected when compared to Brazilian Table of Food Composition. (author)

Final Report on Developing Microstructure-Property Correlation in Reactor Materials using in situ High-Energy X-rays

Energy Technology Data Exchange (ETDEWEB)

Li, Meimei [Argonne National Lab. (ANL), Argonne, IL (United States); Almer, Jonathan D. [Argonne National Lab. (ANL), Argonne, IL (United States); Yang, Yong [Univ. of Florida, Gainesville, FL (United States); Tan, Lizhen [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

2016-01-01

This report provides a summary of research activities on understanding microstructure – property correlation in reactor materials using in situ high-energy X-rays. The report is a Level 2 deliverable in FY16 (M2CA-13-IL-AN_-0403-0111), under the Work Package CA-13-IL-AN_- 0403-01, “Microstructure-Property Correlation in Reactor Materials using in situ High Energy Xrays”, as part of the DOE-NE NEET Program. The objective of this project is to demonstrate the application of in situ high energy X-ray measurements of nuclear reactor materials under thermal-mechanical loading, to understand their microstructure-property relationships. The gained knowledge is expected to enable accurate predictions of mechanical performance of these materials subjected to extreme environments, and to further facilitate development of advanced reactor materials. The report provides detailed description of the in situ X-ray Radiated Materials (iRadMat) apparatus designed to interface with a servo-hydraulic load frame at beamline 1-ID at the Advanced Photon Source. This new capability allows in situ studies of radioactive specimens subject to thermal-mechanical loading using a suite of high-energy X-ray scattering and imaging techniques. We conducted several case studies using the iRadMat to obtain a better understanding of deformation and fracture mechanisms of irradiated materials. In situ X-ray measurements on neutron-irradiated pure metal and model alloy and several representative reactor materials, e.g. pure Fe, Fe-9Cr model alloy, 316 SS, HT-UPS, and duplex cast austenitic stainless steels (CASS) CF-8 were performed under tensile loading at temperatures of 20-400°C in vacuum. A combination of wide-angle X-ray scattering (WAXS), small-angle X-ray scattering (SAXS), and imaging techniques were utilized to interrogate microstructure at different length scales in real time while the specimen was subject to thermal-mechanical loading. In addition, in situ X-ray studies were

Material specific X-ray imaging using an energy-dispersive pixel detector

Energy Technology Data Exchange (ETDEWEB)

Egan, Christopher K., E-mail: christopher.egan@manchester.ac.uk [School of Materials, University of Manchester, Manchester M13 9PL (United Kingdom); Wilson, Matthew D.; Veale, Matthew C.; Seller, Paul [STFC Rutherford Appleton Laboratory, Harwell, Didcot, Oxfordshire OX11 0QX (United Kingdom); Jacques, Simon D.M.; Cernik, Robert J. [School of Materials, University of Manchester, Manchester M13 9PL (United Kingdom)

2014-04-01

By imaging the X-ray spectral properties or ‘colours’ we have shown how material specific imaging can be performed. Using a pixelated energy-dispersive X-ray detector we record the absorbed and emitted hard X-radiation and measure the energy (colour) and intensity of the photons. Using this technology, we are not only able to obtain attenuation contrast but also to image chemical (elemental) variations inside objects, potentially opening up a very wide range of applications from materials science to medical diagnostics.

Spectral and raw quasi in-situ energy dispersive X-ray data captured via a TEM analysis of an ODS austenitic stainless steel sample under 1 MeV Kr2+ high temperature irradiation.

Science.gov (United States)

Brooks, Adam J; Yao, Zhongwen

2017-10-01

The data presented in this article is related to the research experiment, titled: ' Quasi in-situ energy dispersive X-ray spectroscopy observation of matrix and solute interactions on Y-Ti-O oxide particles in an austenitic stainless steel under 1 MeV Kr 2+ high temperature irradiation' (Brooks et al., 2017) [1]. Quasi in-situ analysis during 1 MeV Kr 2+ 520 °C irradiation allowed the same microstructural area to be observed using a transmission electron microscope (TEM), on an oxide dispersion strengthened (ODS) austenitic stainless steel sample. The data presented contains two sets of energy dispersive X-ray spectroscopy (EDX) data collected before and after irradiation to 1.5 displacements-per-atom (~1.25×10 -3  dpa/s with 7.5×10 14  ions cm -2 ). The vendor software used to process and output the data is the Bruker Esprit v1.9 suite. The data includes the spectral (counts vs. keV energy) of the quasi in-situ scanned region (512×512 pixels at 56k magnification), along with the EDX scanning parameters. The.raw files from the Bruker Esprit v1.9 output are additionally included along with the.rpl data information files. Furthermore included are the two quasi in-situ HAADF images for visual comparison of the regions before and after irradiation. This in-situ experiment is deemed ' quasi' due to the thin foil irradiation taking place at an external TEM facility. We present this data for critical and/or extended analysis from the scientific community, with applications applying to: experimental data correlation, confirmation of results, and as computer based modeling inputs.

In situ multi-element analyses by energy-dispersive X-ray fluorescence on varnishes of historical violins

Energy Technology Data Exchange (ETDEWEB)

Echard, Jean-Philippe [Laboratoire de recherche et de restauration, Musee de la musique, Cite de la musique, 221, avenue Jean-Jaures, 75019 Paris (France)]. E-mail: jpechard@cite-musique.fr

2004-10-08

Varnishes of Italian violins and other historical stringed instruments have been analyzed by energy-dispersive X-ray fluorescence (EDXRF). The instruments whose varnishes were to be analyzed were chosen from the collection kept in Musee de la Musique in Paris. Direct analyses were performed on instrument varnishes, without any sampling and non-destructively, showing inorganic elements such as lead, mercury and iron that could be related to siccatives or pigments. Analytical results and their comparison with old formulae or traditional recipes of violin varnishes, as with the few previous analytical results, will be discussed.

In situ multi-element analyses by energy-dispersive X-ray fluorescence on varnishes of historical violins

International Nuclear Information System (INIS)

Echard, Jean-Philippe

2004-01-01

Varnishes of Italian violins and other historical stringed instruments have been analyzed by energy-dispersive X-ray fluorescence (EDXRF). The instruments whose varnishes were to be analyzed were chosen from the collection kept in Musee de la Musique in Paris. Direct analyses were performed on instrument varnishes, without any sampling and non-destructively, showing inorganic elements such as lead, mercury and iron that could be related to siccatives or pigments. Analytical results and their comparison with old formulae or traditional recipes of violin varnishes, as with the few previous analytical results, will be discussed

Energy-dispersive X-ray reflectivity and GID for real-time growth studies of pentacene thin films

International Nuclear Information System (INIS)

Kowarik, S.; Gerlach, A.; Leitenberger, W.; Hu, J.; Witte, G.; Woell, C.; Pietsch, U.; Schreiber, F.

2007-01-01

We use energy-dispersive X-ray reflectivity and grazing incidence diffraction (GID) to follow the growth of the crystalline organic semiconductor pentacene on silicon oxide in-situ and in real-time. The technique allows for monitoring Bragg reflections and measuring X-ray growth oscillations with a time resolution of 1 min in a wide q-range in reciprocal space extending over 0.25-0.80 A -1 , i.e. sampling a large number of Fourier components simultaneously. A quantitative analysis of growth oscillations at several q-points yields the evolution of the surface roughness, showing a marked transition from layer-by-layer growth to strong roughening after four monolayers of pentacene have been deposited

Photon Counting Energy Dispersive Detector Arrays for X-ray Imaging.

Science.gov (United States)

Iwanczyk, Jan S; Nygård, Einar; Meirav, Oded; Arenson, Jerry; Barber, William C; Hartsough, Neal E; Malakhov, Nail; Wessel, Jan C

2009-01-01

The development of an innovative detector technology for photon-counting in X-ray imaging is reported. This new generation of detectors, based on pixellated cadmium telluride (CdTe) and cadmium zinc telluride (CZT) detector arrays electrically connected to application specific integrated circuits (ASICs) for readout, will produce fast and highly efficient photon-counting and energy-dispersive X-ray imaging. There are a number of applications that can greatly benefit from these novel imagers including mammography, planar radiography, and computed tomography (CT). Systems based on this new detector technology can provide compositional analysis of tissue through spectroscopic X-ray imaging, significantly improve overall image quality, and may significantly reduce X-ray dose to the patient. A very high X-ray flux is utilized in many of these applications. For example, CT scanners can produce ~100 Mphotons/mm(2)/s in the unattenuated beam. High flux is required in order to collect sufficient photon statistics in the measurement of the transmitted flux (attenuated beam) during the very short time frame of a CT scan. This high count rate combined with a need for high detection efficiency requires the development of detector structures that can provide a response signal much faster than the transit time of carriers over the whole detector thickness. We have developed CdTe and CZT detector array structures which are 3 mm thick with 16×16 pixels and a 1 mm pixel pitch. These structures, in the two different implementations presented here, utilize either a small pixel effect or a drift phenomenon. An energy resolution of 4.75% at 122 keV has been obtained with a 30 ns peaking time using discrete electronics and a (57)Co source. An output rate of 6×10(6) counts per second per individual pixel has been obtained with our ASIC readout electronics and a clinical CT X-ray tube. Additionally, the first clinical CT images, taken with several of our prototype photon-counting and

Energy-dispersive X-ray fluorescence – A tool for interdisciplinary ...

Indian Academy of Sciences (India)

Keywords. Energy-dispersive X-ray fluorescence; trace elements; oral cancer; biomonitoring; air pollution. Abstract. Trace elements have been at the focus of attention for decades with considerable emphasis on their role in biology and biomedical sciences, environmental sciences, geology, archaeology and material ...

In situ multi-element analyses by energy-dispersive X-ray fluorescence on varnishes of historical violins

Science.gov (United States)

Echard, Jean-Philippe

2004-10-01

Varnishes of Italian violins and other historical stringed instruments have been analyzed by energy-dispersive X-ray fluorescence (EDXRF). The instruments whose varnishes were to be analyzed were chosen from the collection kept in Musée de la Musique in Paris. Direct analyses were performed on instrument varnishes, without any sampling and non-destructively, showing inorganic elements such as lead, mercury and iron that could be related to siccatives or pigments. Analytical results and their comparison with old formulae or traditional recipes of violin varnishes, as with the few previous analytical results, will be discussed.

A new X-ray pinhole camera for energy dispersive X-ray fluorescence imaging with high-energy and high-spatial resolution

Energy Technology Data Exchange (ETDEWEB)

Romano, F.P., E-mail: romanop@lns.infn.it [IBAM, CNR, Via Biblioteca 4, 95124 Catania (Italy); INFN-LNS, Via S. Sofia 62, 95123 Catania (Italy); Altana, C. [INFN-LNS, Via S. Sofia 62, 95123 Catania (Italy); Dipartimento di Fisica e Astronomia, Università di Catania, Via S. Sofia 64, 95123 Catania (Italy); Cosentino, L.; Celona, L.; Gammino, S.; Mascali, D. [INFN-LNS, Via S. Sofia 62, 95123 Catania (Italy); Pappalardo, L. [IBAM, CNR, Via Biblioteca 4, 95124 Catania (Italy); INFN-LNS, Via S. Sofia 62, 95123 Catania (Italy); Rizzo, F. [INFN-LNS, Via S. Sofia 62, 95123 Catania (Italy); Dipartimento di Fisica e Astronomia, Università di Catania, Via S. Sofia 64, 95123 Catania (Italy)

2013-08-01

A new X-ray pinhole camera for the Energy Dispersive X-ray Fluorescence (ED-XRF) imaging of materials with high-energy and high-spatial resolution, was designed and developed. It consists of a back-illuminated and deep depleted CCD detector (composed of 1024 × 1024 pixels with a lateral size of 13 μm) coupled to a 70 μm laser-drilled pinhole-collimator, positioned between the sample under analysis and the CCD. The X-ray pinhole camera works in a coaxial geometry allowing a wide range of magnification values. The characteristic X-ray fluorescence is induced on the samples by irradiation with an external X-ray tube working at a maximum power of 100 W (50 kV and 2 mA operating conditions). The spectroscopic capabilities of the X-ray pinhole camera were accurately investigated. Energy response and energy calibration of the CCD detector were determined by irradiating pure target-materials emitting characteristic X-rays in the energy working-domain of the system (between 3 keV and 30 keV). Measurements were performed by using a multi-frame acquisition in single-photon counting. The characteristic X-ray spectra were obtained by an automated processing of the acquired images. The energy resolution measured at the Fe–Kα line is 157 eV. The use of the X-ray pinhole camera for the 2D resolved elemental analysis was investigated by using reference-patterns of different materials and geometries. The possibility of the elemental mapping of samples up to an area of 3 × 3 cm{sup 2} was demonstrated. Finally, the spatial resolution of the pinhole camera was measured by analyzing the profile function of a sharp-edge. The spatial resolution determined at the magnification values of 3.2 × and 0.8 × (used as testing values) is about 90 μm and 190 μm respectively. - Highlights: • We developed an X-ray pinhole camera for the 2D X-ray fluorescence imaging. • X-ray spectra are obtained by a multi-frame acquisition in single photon mode. • The energy resolution in the X-ray

Application of energy dispersive x-ray techniques for water analysis

International Nuclear Information System (INIS)

Funtua, I. I.

2000-07-01

Energy dispersive x-ray fluorescence (EDXRF) is a class of emission spectroscopic techniques that depends upon the emission of characteristic x-rays following excitation of the atomic electron energy levels by tube or isotopic source x-rays. The technique has found wide range of applications that include determination of chemical elements of water and water pollutants. Three EDXRF systems, the isotopic source, secondary target and total reflection (TXRF) are available at the Centre for Energy research and Training. These systems have been applied for the analysis of sediments, suspensions, ground water, river and rainwater. The isotopic source is based on 55 Fe, 109 Cd and 241 Am excitations while the secondary target and the total reflection are utilizing a Mo x-ray tube. Sample preparation requirements for water analysis range from physical and chemical pre-concentration steps to direct analysis and elements from Al to U can be determined with these systems. The EDXRF techniques, TXRF in particular with its multielement capability, low detection limit and possibility of direct analysis for water have competitive edge over the traditional methods of atomic absorption and flame photometry

Determination of plutonium in nitric acid solutions using energy dispersive L X-ray fluorescence with a low power X-ray generator

Energy Technology Data Exchange (ETDEWEB)

Py, J. [Laboratoire Chrono-Environnement, UMR CNRS 6249, Université de Franche-Comté, 16 route de Gray, F-25030 Besançon (France); Commissariat à l’Énergie Atomique, Centre de Valduc, F-21120 Is-sur-Tille (France); Groetz, J.-E., E-mail: jegroetz@univ-fcomte.fr [Laboratoire Chrono-Environnement, UMR CNRS 6249, Université de Franche-Comté, 16 route de Gray, F-25030 Besançon (France); Hubinois, J.-C.; Cardona, D. [Commissariat à l’Énergie Atomique, Centre de Valduc, F-21120 Is-sur-Tille (France)

2015-04-21

This work presents the development of an in-line energy dispersive L X-ray fluorescence spectrometer set-up, with a low power X-ray generator and a secondary target, for the determination of plutonium concentration in nitric acid solutions. The intensity of the L X-rays from the internal conversion and gamma rays emitted by the daughter nuclei from plutonium is minimized and corrected, in order to eliminate the interferences with the L X-ray fluorescence spectrum. The matrix effects are then corrected by the Compton peak method. A calibration plot for plutonium solutions within the range 0.1–20 g L{sup −1} is given.

Energy-dispersive X-ray diffraction beamline at Indus-2 synchrotron ...

Indian Academy of Sciences (India)

An energy-dispersive X-ray diffraction beamline has been designed, developed and commissioned at BL-11 bending magnet port of the Indian synchrotron source, Indus-2. The performance of this beamline has been benchmarked by measuring diffraction patterns from various elemental metals and standard inorganic ...

Micro energy dispersive X-ray fluorescence analysis of polychrome lead-glazed Portuguese faiences

International Nuclear Information System (INIS)

Guilherme, A.; Pessanha, S.; Carvalho, M.L.; Santos, J.M.F. dos; Coroado, J.

2010-01-01

Several glazed ceramic pieces, originally produced in Coimbra (Portugal), were submitted to elemental analysis, having as premise the pigment manufacture production recognition. Although having been produced in Coimbra, their location changed as time passed due to historical reasons. A recent exhibition in Coimbra brought together a great number of these pieces and in situ micro Energy Dispersive X-ray Fluorescence (μ-EDXRF) analyses were performed in order to achieve some chemical and physical data on the manufacture of faiences in Coimbra. A non-commercial μ-EDXRF equipment for in situ analysis was employed in this work, carrying some important improvements when compared to the conventional ones, namely, analyzing spot sizes of about 100 μm diameter. The combination of a capillary X-ray lens with a new generation of low power microfocus X-ray tube and a drift chamber detector enabled a portable unit for micro-XRF with a few tens of μm lateral resolution. The advantages in using a portable system emphasized with polycapillary optics enabled to distinguish proximal different pigmented areas, as well as the glaze itself. These first scientific results on the pigment analysis of the collection of faiences seem to point to a unique production center with own techniques and raw materials. This conclusion arose with identification of the blue pigments having in its constitution Mn, Fe Co and As and the yellows as a result of the combination between Pb and Sb. A statistical treatment was used to reveal groups of similarities on the pigments elemental profile.

Energy-dispersive X-ray fluorescence analysis of cerium in ferrosilicon

International Nuclear Information System (INIS)

Marbec, E.R.

1987-01-01

The cerium was determined in ferrosilicon samples by energy-dispersive X-ray fluorescence techniques (XRF) techniques, with a secondary target of gadolinium. The methods employed were: comparison and linear regression with reference materials with cerium concentration between 0.4 and 1.0%. The samples were prepared in the form of pellets and the analytical results are reported as an average of five determinations with a confidence limits at 95% probability. (Author) [es

Influence of experimental conditions on atom column visibility in energy dispersive X-ray spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Dycus, J.H.; Xu, W.; Sang, X. [Department of Materials Science and Engineering, North Carolina State University, 911 Partners Way Engineering Building 1, Raleigh, NC 27606 (United States); D' Alfonso, A.J. [School of Physics, University of Melbourne, Parkville, Victoria 3010 (Australia); Chen, Z. [School of Physics and Astronomy, Monash University, Clayton, Victoria 3800 (Australia); Weyland, M. [Monash Centre for Electron Microscopy, Monash University, Clayton, Victoria 3800 (Australia); Department of Materials Science and Engineering, Monash University, Clayton, Victoria 3800 (Australia); Allen, L.J. [School of Physics, University of Melbourne, Parkville, Victoria 3010 (Australia); Findlay, S.D. [School of Physics and Astronomy, Monash University, Clayton, Victoria 3800 (Australia); LeBeau, J.M., E-mail: jmlebeau@ncsu.edu [Department of Materials Science and Engineering, North Carolina State University, 911 Partners Way Engineering Building 1, Raleigh, NC 27606 (United States)

2016-12-15

Here we report the influence of key experimental parameters on atomically resolved energy dispersive X-ray spectroscopy (EDX). In particular, we examine the role of the probe forming convergence semi-angle, sample thickness, lattice spacing, and dwell/collection time. We show that an optimum specimen-dependent probe forming convergence angle exists to maximize the signal-to-noise ratio of the atomically resolved signal in EDX mapping. Furthermore, we highlight that it can be important to select an appropriate dwell time to efficiently process the X-ray signal. These practical considerations provide insight for experimental parameters in atomic resolution energy dispersive X-ray analysis. - Highlights: • Impacts of microscope operating conditions on EDX signal and atom column contrast are demonstrated. • Influence of sample thickness and lattice spacing is shown. • Conditions for obtaining optimal signal and contrast for different sample types are discussed. • Effects of dwell time during EDX acquisition are discussed.

Comparison between energy dispersive X-ray fluorescence and other nuclear analytical techniques in mineral exploration and mining

International Nuclear Information System (INIS)

Clayton, C.G.; Packer, T.W.; Wormald, M.R.

1979-01-01

At the present time there is an increasing awareness of the value and need for in-situ analytical methods throughout the general area of mineral exploration and mining. Of the alternative techniques, the measurement of natural gamma radiation is well established for uranium exploration and it is now being developed for sea-bed and lake-bed surveying. Energy dispersive X-ray fluorescence equipment is becoming more generally accepted, especially for mine control. Neutron techniques, for so long used routinely in oil well logging, are now being developed for a wide range of applications in all aspects of exploration and mining. It is believed that these techniques will result in major applications in the future. The present paper compares the principal characteristics of energy dispersive X-ray fluorescence and neutron techniques in particular, with special emphasis being given to those factors which affect the accuracy of analytical content; such as elemental resolution, matrix effects, material heterogeneity and neutron transport. A generalised comparison between the techniques is difficult to achieve because of the different nature of radiation interactions, but a range of applications is described and these show the complementary nature of the methods and point to the areas for more active development in the future. (author)

In situ x-ray reflectivity and grazing incidence x-ray diffraction study of L 1{sub 0} ordering in {sup 57}Fe/Pt multilayers

Energy Technology Data Exchange (ETDEWEB)

Raghavendra Reddy, V; Gupta, Ajay; Gome, Anil [UGC-DAE Consortium for Scientific Research, University Campus, Khandwa Road, Indore-452 017 (India); Leitenberger, Wolfram [Institute of Physics, University of Potsdam, 14469 Potsdam (Germany); Pietsch, U [Physics Department, University of Siegen, D-57068 Siegen (Germany)], E-mail: vrreddy@csr.ernet.in, E-mail: varimalla@yahoo.com

2009-05-06

In situ high temperature x-ray reflectivity and grazing incidence x-ray diffraction measurements in the energy dispersive mode are used to study the ordered face-centered tetragonal (fct) L 1{sub 0} phase formation in [Fe(19 A)/Pt(25 A)]{sub x 10} multilayers prepared by ion beam sputtering. With the in situ x-ray measurements it is observed that (i) the multilayer structure first transforms to a disordered FePt and subsequently to an ordered fct L 1{sub 0} phase, (ii) the ordered fct L 1{sub 0} FePt peaks start to appear at 320 deg. C annealing, (iii) the activation energy of the interdiffusion is 0.8 eV and (iv) ordered fct FePt grains have preferential out-of-plane texture. The magneto-optical Kerr effect and conversion electron Moessbauer spectroscopies are used to study the magnetic properties of the as-deposited and 400 deg. C annealed multilayers. The magnetic data for the 400 {sup 0}C annealed sample indicate that the magnetization is at an angle of {approx}50 deg. from the plane of the film.

Energy dispersion of x-ray continua in the energy range 9kev to 19kev refraction on Si wafers

International Nuclear Information System (INIS)

Ebel, H.; Streli, C.; Pepponi, G.; Wobrauschek, P.

2000-01-01

Total reflection of x-rays in matter at given grazing incidence angle is characterized by the occurrence of an energy cut-off. Photons with energies greater than the cut-off energy penetrate into matter and are refracted according to a transition from the optically more dense to the optically less dense medium. Since the refractive index depends on photon energy, an energy dispersion of continuous x-radiation is observed. The present investigation is dedicated to the energy dispersion of continuous x-radiation (Mo, 45 kV) by Si wafers. Theory and experimental results are in excellent agreement. (author)

Analysis of siliceous geologic materials by energy-dispersive X-ray fluorescence

International Nuclear Information System (INIS)

Roca, M.; Bayon, A.

1987-01-01

The determination of the elements Al, Si, K, Ca, Ti, Cr, Mn and Fe in siliceous geologic samples by energy-dispersive X-ray fluorescence is investigated using the most adequate excitation conditions: direct excitation mode (rhodium anode X-ray tube) for the former two elements, and the secondary targets titanium for K and Ca, and germanium for Ti, Cr, Mn and Fe. For the correction of matrix effects the use of ratio methods has been tested. Procedure files have been defined allowing the automatic simultaneous acquisition and processing of spectra. (author)

Is scanning electron microscopy/energy dispersive X-ray spectrometry (SEM/EDS) quantitative?

Science.gov (United States)

Newbury, Dale E; Ritchie, Nicholas W M

2013-01-01

Scanning electron microscopy/energy dispersive X-ray spectrometry (SEM/EDS) is a widely applied elemental microanalysis method capable of identifying and quantifying all elements in the periodic table except H, He, and Li. By following the "k-ratio" (unknown/standard) measurement protocol development for electron-excited wavelength dispersive spectrometry (WDS), SEM/EDS can achieve accuracy and precision equivalent to WDS and at substantially lower electron dose, even when severe X-ray peak overlaps occur, provided sufficient counts are recorded. Achieving this level of performance is now much more practical with the advent of the high-throughput silicon drift detector energy dispersive X-ray spectrometer (SDD-EDS). However, three measurement issues continue to diminish the impact of SEM/EDS: (1) In the qualitative analysis (i.e., element identification) that must precede quantitative analysis, at least some current and many legacy software systems are vulnerable to occasional misidentification of major constituent peaks, with the frequency of misidentifications rising significantly for minor and trace constituents. (2) The use of standardless analysis, which is subject to much broader systematic errors, leads to quantitative results that, while useful, do not have sufficient accuracy to solve critical problems, e.g. determining the formula of a compound. (3) EDS spectrometers have such a large volume of acceptance that apparently credible spectra can be obtained from specimens with complex topography that introduce uncontrolled geometric factors that modify X-ray generation and propagation, resulting in very large systematic errors, often a factor of ten or more. © Wiley Periodicals, Inc.

Application of energy dispersive X-ray spectrometers with semiconductor detectors in radiometric analyses

International Nuclear Information System (INIS)

Jugelt, P.; Schieckel, M.

1983-01-01

Problems and possibilities of applying semiconductor detector spectrometers in radiometric analyses are described. A summary of the state of the art and tendencies of device engineering and spectra evaluation is given. Liquid-nitrogen cooled Li-drifted Si-detectors and high-purity Ge-detectors are compared. Semiconductor detectors working at room temperature are under development. In this connection CdTe and HgI 2 semiconductor detectors are compared. The use of small efficient computers in the spectrometer systems stimulates the development of algorithms for spectra analyses and for determining the concentration. Fields of application of energy dispersive X-ray spectrometers are X-ray diffraction and X-ray macroanalysis in investigating the structure of extensive surface regions

Analysis of metals in organic compounds by energy dispersive X-ray fluorescence analysis

International Nuclear Information System (INIS)

Anjos, Marcelino J.; Lopes, Ricardo T.; Jesus, Edgar F.O. de

2000-01-01

Using energy dispersive X-ray fluorescence analysis with an X-ray tube filtered with Ti. It was possible to determine the concentration of the elements at ppm level of several elements: K, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn As, Rb, Sr, Y, Zr, and Pb in two types of organic compound enough used in the agriculture: organic compound of urban garbage (Fertilurb) and aviary bed (birds manure). The experimental setup is composed of: x-ray tube (Oxford, 30 kV, 50 μA and W anode), an ORTEC Si-Li detector, with an energy resolution of about 180 eV at 5.9 keV and an ORTEC multichannel-analyser. The X-ray beam is quasi- monochromatic by using Ti filter. The samples were prepared in pellet form with superficial density in the range of 100 mg/cm 2 . The fundamental parameter method was used in order to verify the elemental concentration. The radiation transmission method was going used to the radiation absorption effects correction in the samples. (author)

Automatic energy dispersive x-ray fluorescence analysing apparatus

International Nuclear Information System (INIS)

Russ, J.C.; Carey, R.; Chopra, V.K.

1983-01-01

The invention discloses a number of improvements for an energy dispersive X-ray analysis system having computer supervised data collection, display and processing. The systems with which the improved circuitry and methods may be used include a dual interlocking bus structure so that the analyzer and computer functions communicate directly with each other and the user has immediate keyboard control of both. Such a system normally includes a system base control, a control console and a display console. The portions of the system which have been improved include a new type of ratemeter which gives a voltage output proportional to the intensity of the energy window or windows under consideration, an output which is an absolute digital representation of the intensity count rate, circuitry for input multiplexing and multiple output voltage buffering of the ratemeter to accomodate multiple single channel signals, and a new dead time correction to enable meaningful single channel intensity data to be handled by the system. An extension of the ratemeter is also disclosed for use in conjunction with X-ray mapping, enabling enhancements to be made on mapping SCA data

Energy dispersive X-ray diffraction at high pressure in CHESS

International Nuclear Information System (INIS)

Ruoff, A.L.; Baublitz, M.A. Jr.

1981-01-01

Energy dispersive X-ray techniques were used with a diamond anvil cell in the Cornell High Energy Synchrotron Source (CHESS). It was shown that quantitative relative intensity measurement could be made when the pressure was hydrostatic and the crystals were relatively defect free. The crystal structures of the high pressure polymorphs of Ge, GaAs, GaP, and AlSb were studied. Ge exhibits the β-tetragonal structure as found by Jamieson; however, the transition pressure is 80 +- 5 kbars. GaAs exhibits an orthorhombic structure above 172 +- 7 kbars, GaP the β-Sn structure above 215 +- 8 kbars, and AlSb an orthorhombic structure above 77 +- 5 kbars. (Auth.)

In situ x-ray diffraction studies of three-dimensional C60 polymers

International Nuclear Information System (INIS)

Wood, R A; Lewis, M H; Bennington, S M; Cain, M G; Kitamura, N; Fukumi, A K

2002-01-01

In situ investigations into the P/T field of C 60 fullerene were performed using energy-dispersive x-ray diffraction techniques. Isobars were obtained at 11 and 9 GPa accompanied by isotherms at 750 and 800 K with pressure reaching 13 GPa. The P/T history and pressure isotropy were investigated with the aim of optimizing conditions for 3D polymer formation. Confirmation of the formation of 3D polymers was performed in situ; however, the reclaimed sample did not exhibit the expected high hardness value, due to depolymerization on pressure release. Isotropy in the pressure field promoted formation and retention of the face-centred-cubic structure

First experience with energy dispersive X-ray analysis (EDXA) in lung fibrosis

International Nuclear Information System (INIS)

Liebetrau, G.; Wiesner, B.; Strausz, J.; Zglinicki, T. von

1987-01-01

Biopsies from 68 patients suffering from interstitial lung disease were examined with regard to minerals using energy dispersive X-ray analysis. In 31 patients a higher portion of minerals or elements were found as pigments. The interpretation of these findings is difficult. If there is a occupational exposure and a reaction of the lung parenchyma the findings could be of clinical value. (author)

Practical applications of energy dispersive X-ray microanalysis in diagnostic oral pathology

International Nuclear Information System (INIS)

Daley, T.D.; Gibson, D.

1990-01-01

Energy dispersive X-ray microanalysis is a powerful tool that can reveal the presence and relative quantities of elements in minute particles in biologic materials. Although this technique has been used in some aspects of dental research, it has rarely been applied to diagnostic oral pathology. The purpose of this paper is to inform practicing dentists and oral specialists about the diagnostic potential of this procedure by presenting three case reports. The first case involved the identification of flakes of a metallic material claimed by a 14-year-old girl to appear periodically between her mandibular molars. In the second case, a periodontist was spared a lawsuit when a freely mobile mass in the antrum of his patient was found to be a calcium-phosphorus compound not related to the periodontal packing that had been used. The third case involved the differential diagnosis of amalgam tattoo and graphite tattoo in a pigmented lesion of the hard palate mucosa. The results of the analyses were significant and indicate a role for this technique in the assessment of selected cases. Potential for wider use of energy dispersive X-ray microanalysis in diagnostic oral pathology exists as research progresses

Measurement of grain size of polycrystalline materials with confocal energy dispersive micro-X-ray diffraction technology based on polycapillary X-ray optics

Energy Technology Data Exchange (ETDEWEB)

Sun, Weiyuan; Liu, Zhiguo [The Key Laboratory of Beam Technology and Materials Modification of the Ministry of Education, Beijing Normal University, Beijing 100875 (China); College of Nuclear Science and Technology, Beijing Normal University, Beijing 100875 (China); Beijing Radiation Center, Beijing 100875 (China); Sun, Tianxi, E-mail: stx@bnu.edu.cn [The Key Laboratory of Beam Technology and Materials Modification of the Ministry of Education, Beijing Normal University, Beijing 100875 (China); College of Nuclear Science and Technology, Beijing Normal University, Beijing 100875 (China); Beijing Radiation Center, Beijing 100875 (China); Peng, Song [The Key Laboratory of Beam Technology and Materials Modification of the Ministry of Education, Beijing Normal University, Beijing 100875 (China); College of Nuclear Science and Technology, Beijing Normal University, Beijing 100875 (China); Beijing Radiation Center, Beijing 100875 (China); Ma, Yongzhong [Center for Disease Control and Prevention of Beijing, Beijing 100013 (China); Li, Fangzuo; Sun, Xuepeng; Ding, Xunliang [The Key Laboratory of Beam Technology and Materials Modification of the Ministry of Education, Beijing Normal University, Beijing 100875 (China); College of Nuclear Science and Technology, Beijing Normal University, Beijing 100875 (China); Beijing Radiation Center, Beijing 100875 (China)

2014-11-11

The confocal energy dispersive micro-X-ray diffraction (EDMXRD) based on polycapillary X-ray optics was used to determine the grain size of polycrystalline materials. The grain size of a metallographic specimen of nickel base alloy was measured by using the confocal EDMXRD. The experimental results demonstrated that the confocal EDMXRD had potential applications in measuring large grain size.

New software to model energy dispersive X-ray diffraction in polycrystalline materials

Energy Technology Data Exchange (ETDEWEB)

Ghammraoui, B., E-mail: bahaa.ghammraoui@cea.fr [CEA-Leti, MINATEC Campus, 17 rue des Martyrs, F 38054 Grenoble, Cedex 9 (France); Tabary, J. [CEA-Leti, MINATEC Campus, 17 rue des Martyrs, F 38054 Grenoble, Cedex 9 (France); Pouget, S. [CEA-INAC Sciences de la matieres, 17 rue des Martyrs, F 38054 Grenoble, Cedex 9 (France); Paulus, C.; Moulin, V.; Verger, L. [CEA-Leti, MINATEC Campus, 17 rue des Martyrs, F 38054 Grenoble, Cedex 9 (France); Duvauchelle, Ph. [CNDRI-Insa Lyon, Universite de Lyon, F-69621, Villeurbanne Cedex (France)

2012-02-01

Detection of illicit materials, such as explosives or drugs, within mixed samples is a major issue, both for general security and as part of forensic analyses. In this paper, we describe a new code simulating energy dispersive X-ray diffraction patterns in polycrystalline materials. This program, SinFullscat, models diffraction of any object in any diffractometer system taking all physical phenomena, including amorphous background, into account. Many system parameters can be tuned: geometry, collimators (slit and cylindrical), sample properties, X-ray source and detector energy resolution. Good agreement between simulations and experimental data was obtained. Simulations using explosive materials indicated that parameters such as the diffraction angle or the energy resolution of the detector have a significant impact on the diffraction signature of the material inspected. This software will be a convenient tool to test many diffractometer configurations, providing information on the one that best restores the spectral diffraction signature of the materials of interest.

Application of a portable equipment EDXRF (energy dispersive X-ray fluorescence) in the monitoring of the restoration work of murals paints in the Church of Paroquia Imaculada Conceicao (Sao Paulo, SP)

International Nuclear Information System (INIS)

Appoloni, Carlos Roberto; Parreira, Paulo Sergio; Rizzo, Marcia

2006-01-01

This paper presents the application of the portable EDXRF (energy dispersive X-ray fluorescence) of the Laboratorio de Fisica Nuclear Aplicada of the Universidade Estadual de Londrina in the analysis in situ of pigments in wall paintings, as well as in monitoring restoration processes

Clinical applications of scanning electron microscopy and energy dispersive X-ray analysis in dermatology--an up-date

International Nuclear Information System (INIS)

Forslind, B.

1988-01-01

Dermatological papers comprising scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) analysis data published 1983 through 1986 in international journals are reviewed, as an update to our 1984 paper on Clinical applications of scanning electron microscopy and X-ray microanalysis in dermatology. The present paper not only deals with a review of recent publications in this area but also presents the application of microincineration to hair and cryosectioned freeze-dried skin specimens. Examples of the increased contrast obtained in hair cross sections are presented and a discussion on the feasibility of microincineration at analysis of hair and skin cross sections is given. Particle probe analysis (EDX: energy dispersive X-ray analysis and PMP: proton microprobe analysis) as applied to hair and skin samples are presented with stress put on the proton probe analysis. The complementarity of EDX and PMP is demonstrated and future applications are suggested. 75 references

Energy-dispersive X-ray fluorescence spectrometry of industrial paint samples

International Nuclear Information System (INIS)

Christensen, L.H.; Drabaek, I.

1986-01-01

An energy-dispersive X-ray fluorescence method for the direct, simultaneous determination of major and minor elements in coatings is described. The method relies on the back-scatter/fundamental parameter concept and provides a general solution to matrix problems. The method has been implemented and verified on spectrometers based both on tube excitation and radioisotope excitation. Results demonstrating some performance characteristics are presented. Sample inhomogeneity problems that impede quantification of low-Z elements in some types of paint are discussed. (Auth.)

Co marker determination in rumen liquid sample by energy dispersive X-ray fluorescence

Energy Technology Data Exchange (ETDEWEB)

Almeida, Eduardo de; Nascimento Filho, Virgilio F.; Massoni, Paulo R. [Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil). Lab. de Instrumentacao Nuclear (LIN)]. E-mail: edualm@usp.br; Leite, Laudi C.; Lanna, Dante P.D. [Escola Superior de Agricultura ' Luiz de Queiroz' (ESALQ/USP), Piracicaba, SP (Brazil). Dept. de Zootecnia. Lab. de Anatomia e Fisiologia Animal (LAFA)]. E-mail: lcleite@ciagri.usp.br

2007-07-01

The Co element is used in nutritional studies as marker. This paper describes an analytical methodology for Co determination in rumen liquid sample using energy dispersive X-ray spectrometry (EDXRF). 200 {mu}L of the sample were dried at 60 deg C on 6.35 {mu}m Mylar film. Ga was used as internal standard. The excitation was carried out utilizing Mo target X-ray tube (Zr filter) at 30 kV / 20 mA. The acquisition time was 200 s. The accuracy of this methodology was assessed through standard addition method, the recovery obtained was 98.7 % for Co. The detection limit was 0.15 mg / L for this element. (author)

Co marker determination in rumen liquid sample by energy dispersive X-ray fluorescence

International Nuclear Information System (INIS)

Almeida, Eduardo de; Nascimento Filho, Virgilio F.; Massoni, Paulo R.; Leite, Laudi C.; Lanna, Dante P.D.

2007-01-01

The Co element is used in nutritional studies as marker. This paper describes an analytical methodology for Co determination in rumen liquid sample using energy dispersive X-ray spectrometry (EDXRF). 200 μL of the sample were dried at 60 deg C on 6.35 μm Mylar film. Ga was used as internal standard. The excitation was carried out utilizing Mo target X-ray tube (Zr filter) at 30 kV / 20 mA. The acquisition time was 200 s. The accuracy of this methodology was assessed through standard addition method, the recovery obtained was 98.7 % for Co. The detection limit was 0.15 mg / L for this element. (author)

A spectrometer for X-ray energy-dispersive diffraction using synchrotron radiation

International Nuclear Information System (INIS)

Buras, B.; Gerward, L.; Staun Olsen, J.; Steenstrup, S.

1981-10-01

The paper describes a white-beam X-ray energy dispersive diffractometer using the synchroton radiation from the DORIS ESR. The following features of the instrument are discussed: Horizontal or vertical scattering plane, collimators, sample environment, remote control of gonimeter, data acquisition, energy-sensitive detectors using small-area and large-area detector crystals, modes of operation, powder and single crystal diffraction. An example is given from a high-pressure study of YbH 2 using a diamond anvil cell. (orig./HP)

The Oxford-Diamond In Situ Cell for studying chemical reactions using time-resolved X-ray diffraction

Science.gov (United States)

Moorhouse, Saul J.; Vranješ, Nenad; Jupe, Andrew; Drakopoulos, Michael; O'Hare, Dermot

2012-08-01

A versatile, infrared-heated, chemical reaction cell has been assembled and commissioned for the in situ study of a range of chemical syntheses using time-resolved energy-dispersive X-ray diffraction (EDXRD) on Beamline I12 at the Diamond Light Source. Specialized reactor configurations have been constructed to enable in situ EDXRD investigation of samples under non-ambient conditions. Chemical reactions can be studied using a range of sample vessels such as alumina crucibles, steel hydrothermal autoclaves, and glassy carbon tubes, at temperatures up to 1200 °C.

X-ray analysis and mapping by wavelength dispersive X-ray spectroscopy in an electron microscope

International Nuclear Information System (INIS)

Tanaka, Miyoko; Takeguchi, Masaki; Furuya, Kazuo

2008-01-01

A compact and easy-to-use wavelength dispersive X-ray spectrometer using a multi-capillary X-ray lens attached to a scanning (transmission) electron microscope has been tested for thin-film analysis. B-K spectra from thin-film boron compounds (B 4 C, h-BN, and B 2 O 3 ) samples showed prominent peak shifts and detailed structural differences. Mapping images of a thin W/Si double-layer sample resolved each element clearly. Additionally, a thin SiO 2 film grown on a Si substrate was imaged with O-K X-rays. Energy and spatial resolution of the system is also discussed

Perspectives of in situ/operando resonant inelastic X-ray scattering in catalytic energy materials science

Energy Technology Data Exchange (ETDEWEB)

Liu, Yi-Sheng; Glans, Per-Anders [Advanced Light Source, Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Chuang, Cheng-Hao [Advanced Light Source, Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Department of Physics, Tamkang University, Tamsui 250, Taiwan, ROC (China); Kapilashrami, Mukes [Center for Engineering Concepts Development, Department of Mechanical Engineering, University of Maryland, College Park, MD 20742 (United States); Advanced Light Source, Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Guo, Jinghua, E-mail: jguo@lbl.gov [Advanced Light Source, Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Department of Chemistry and Biochemistry, University of California, Santa Cruz, CA 95064 (United States)

2015-04-15

Highlights: • In-situ/operando soft X-ray RXES and RIXS offer unique perspectives in the energy material science. - Abstract: Growing environmental concerns have renewed the interest for light induced catalytic reactions to synthesize cleaner chemical fuels from syngas. This, however, requires a sound understanding for the dynamics taking place at molecular level as a result of light – matter interaction. We present herein the principles of soft X-ray resonant emission spectroscopy (RXES) and resonant inelastic scattering (RIXS) and the importance of these spectroscopic techniques in materials science in light of their unique ability to emanate characteristic fingerprints on the geometric structure, chemical bonding charge and spin states in addition to chemical sensitivity. The addition of in situ/operando RXES and RIXS capability offers new opportunities to project important material properties and functionalities under conditions nearly identical to the operational modes.

Perspectives of in situ/operando resonant inelastic X-ray scattering in catalytic energy materials science

International Nuclear Information System (INIS)

Liu, Yi-Sheng; Glans, Per-Anders; Chuang, Cheng-Hao; Kapilashrami, Mukes; Guo, Jinghua

2015-01-01

Highlights: • In-situ/operando soft X-ray RXES and RIXS offer unique perspectives in the energy material science. - Abstract: Growing environmental concerns have renewed the interest for light induced catalytic reactions to synthesize cleaner chemical fuels from syngas. This, however, requires a sound understanding for the dynamics taking place at molecular level as a result of light – matter interaction. We present herein the principles of soft X-ray resonant emission spectroscopy (RXES) and resonant inelastic scattering (RIXS) and the importance of these spectroscopic techniques in materials science in light of their unique ability to emanate characteristic fingerprints on the geometric structure, chemical bonding charge and spin states in addition to chemical sensitivity. The addition of in situ/operando RXES and RIXS capability offers new opportunities to project important material properties and functionalities under conditions nearly identical to the operational modes.

Setup for in situ X-ray diffraction studies of thin film growth by magnetron sputtering

CERN Document Server

Ellmer, K; Weiss, V; Rossner, H

2001-01-01

A novel method is described for the in situ-investigation of nucleation and growth of thin films during magnetron sputtering. Energy dispersive X-ray diffraction with synchrotron light is used for the structural analysis during film growth. An in situ-magnetron sputtering chamber was constructed and installed at a synchrotron radiation beam line with a bending magnet. The white synchrotron light (1-70 keV) passes the sputtering chamber through Kapton windows and hits one of the substrates on a four-fold sample holder. The diffracted beam, observed under a fixed diffraction angle between 3 deg. and 10 deg., is energy analyzed by a high purity Ge-detector. The in situ-EDXRD setup is demonstrated for the growth of tin-doped indium oxide (ITO) films prepared by reactive magnetron sputtering from a metallic target.

A method to test the performance of an energy-dispersive X-ray spectrometer (EDS).

Science.gov (United States)

Hodoroaba, Vasile-Dan; Procop, Mathias

2014-10-01

A test material for routine performance evaluation of energy-dispersive X-ray spectrometers (EDS) is presented. It consists of a synthetic, thick coating of C, Al, Mn, Cu, and Zr, in an elemental composition that provides interference-free characteristic X-ray lines of similar intensities at 10 kV scanning electron microscope voltage. The EDS energy resolution at the C-K, Mn-Lα, Cu-Lα, Al-K, Zr-Lα, and Mn-Kα lines, the calibration state of the energy scale, and the Mn-Lα/Mn-Kα intensity ratio as a measure for the low-energy detection efficiency are calculated by a dedicated software package from the 10 kV spectrum. Measurements at various input count rates and processor shaping times enable an estimation of the operation conditions for which the X-ray spectrum is not yet corrupted by pile-up events. Representative examples of EDS systems characterized with the test material and the related software are presented and discussed.

Challenges for energy dispersive X-ray absorption spectroscopy at the ESRF: microsecond time resolution and Mega-bar pressures

International Nuclear Information System (INIS)

Aquilanti, G.

2002-01-01

This Thesis concerns the development of two different applications of energy-dispersive X-ray absorption spectroscopy at the ESRF: time-resolved studies pushed to the microsecond time resolution and high-pressure studies at the limit of the Mega-bar pressures. The work has been developed in two distinct parts, and the underlying theme has been the exploitation of the capabilities of an X-ray absorption spectrometer in dispersive geometry on a third generation synchrotron source. For time-resolved studies, the study of the triplet excited state following a laser excitation of Pt 2 (P 2 O 5 H 2 ) 4 4- has been chosen to push the technique to the microsecond time resolution. In the high-pressure part, the suitability of the energy dispersive X-ray absorption spectrometer for high-pressure studies using diamond anvils cell is stressed. Some technical developments carried out on beamline ID24 are discussed. Finally, the most extensive scientific part concerns a combined X-ray absorption and diffraction study of InAs under pressure. (author)

Energy Dispersive Spectrometry and Quantitative Analysis Short Course. Introduction to X-ray Energy Dispersive Spectrometry and Quantitative Analysis

Science.gov (United States)

Carpenter, Paul; Curreri, Peter A. (Technical Monitor)

2002-01-01

This course will cover practical applications of the energy-dispersive spectrometer (EDS) to x-ray microanalysis. Topics covered will include detector technology, advances in pulse processing, resolution and performance monitoring, detector modeling, peak deconvolution and fitting, qualitative and quantitative analysis, compositional mapping, and standards. An emphasis will be placed on use of the EDS for quantitative analysis, with discussion of typical problems encountered in the analysis of a wide range of materials and sample geometries.

Energy dispersive X-ray fluorescence determination of cadmium in uranium matrix using Cd Kα line excited by continuum

International Nuclear Information System (INIS)

Dhara, Sangita; Misra, N.L.; Aggarwal, S.K.; Venugopal, V.

2010-01-01

An energy dispersive X-ray fluorescence method for determination of cadmium (Cd) in uranium (U) matrix using continuum source of excitation was developed. Calibration and sample solutions of cadmium, with and without uranium were prepared by mixing different volumes of standard solutions of cadmium and uranyl nitrate, both prepared in suprapure nitric acid. The concentration of Cd in calibration solutions and samples was in the range of 6 to 90 μg/mL whereas the concentration of Cd with respect to U ranged from 90 to 700 μg/g of U. From the calibration solutions and samples containing uranium, the major matrix uranium was selectively extracted using 30% tri-n-butyl phosphate in dodecane. Fixed volumes (1.5 mL) of aqueous phases thus obtained were taken directly in specially designed in-house fabricated leak proof Perspex sample cells for the energy dispersive X-ray fluorescence measurements and calibration plots were made by plotting Cd Kα intensity against respective Cd concentration. For the calibration solutions not having uranium, the energy dispersive X-ray fluorescence spectra were measured without any extraction and Cd calibration plots were made accordingly. The results obtained showed a precision of 2% (1σ) and the results deviated from the expected values by < 4% on average.

Characterization of the Carancas-Puno meteorite by energy dispersive X-ray fluorescence, X-ray diffractometry and transmission Moessbauer spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Ceron Loayza, Maria L., E-mail: malucelo@hotmail.com; Bravo Cabrejos, Jorge A. [Universidad Nacional Mayor de San Marcos, Laboratorio de Analisis de Suelos, Facultad de Ciencias Fisicas (Peru)

2011-11-15

We report the results of the study of a meteorite that impacted an inhabited zone on 15 September 2007 in the neighborhood of the town of Carancas, Puno Region, about 1,300 km south of Lima. The analysis carried out by energy dispersive X-ray fluorescence, X-ray diffractometry and transmission Moessbauer spectroscopy (at room temperature and at 4.2 K), reveal the presence in the meteorite sample of magnetic sites assigned to taenite (Fe,Ni) and troilite (Fe,S) phases, and of two paramagnetic doublets assigned to Fe{sup 2 + }, one associated with olivine and the other to pyroxene. In accord with these results, this meteorite is classified as a type IV chondrite meteorite.

Optimization of a spectrometry for energy-dispersive x-ray fluorescence analysis by x-ray tube in combination with secondary target for multielements determination of sediment samples

International Nuclear Information System (INIS)

Zaidi Embong; Husin Wagiran

1997-01-01

The design of an energy-dispersive X-ray fluorescence spectrometer equipped with a conventional X-ray tube and secondary target is described. The spectrometer system constructed in our laboratory consists of a semiconductor detector system, irradiation chamber and X-ray tube. Primary source from X-ray tube was used to produced secondary X-ray from selenium, molybdenum and cadmium targets. The fluorescence X-ray from the sample was detected using Si(Li) detector with resolution of 0. 175 keV (Mn-K(x). The spectrometer was used for determination of multi-elements with atomic number between 20 to 44 in river sediment samples. The X-ray spectrum, from the samples were analysed using computer software which was developed based on Marquardt method. Optimal conditions and detection limits are determined experimentally by variation of excitation parameters for each combination of secondary target and tube voltage

A new device for energy-dispersive x-ray fluorescence

Science.gov (United States)

Swoboda, Walter; Kanngiesser, Birgit; Beckhoff, Burkhard; Begemann, Klaus; Neuhaus, Hermann; Scheer, Jens

1991-12-01

A new measuring chamber for energy-dispersive x-ray fluorescence is presented, which allows excitation of the sample by three (commonly applied) modes: secondary target excitation, Barkla scattering, and Bragg reflection. In spite of the short distances required to obtain high intensities, the transmission of the radiator through the bulk matter of the chamber wall and the collimators could be kept negligibly small. In the case of Bragg reflection, the adjustment of all degrees of freedom of the crystal is performed independently and reproducibly under vacuum conditions. The device allows the choice of excitation mode optimized for the respective analytical problem. An experimental test using an environmental specimen shows the detection limits obtainable.

Photon induced x-ray fluorescence analysis using energy dispersive detector and dichotomous sampler

International Nuclear Information System (INIS)

Jaklevic, J.M.; Loo, B.W.; Goulding, F.S.

1976-01-01

Operating experience in using the photon-excited energy-dispersive x-ray fluorescence analysis system has demonstrated the applicability of this technique to large-scale air-sampling networks. This experience has shown that it is possible to perform automatic sampling and analysis of aerosol particulates at a sensitivity and accuracy more than adequate for most air pollution studies

Analysis of trace elements in medicinal plants with energy dispersive X-ray fluorescence

International Nuclear Information System (INIS)

Ekinci, N.; Polat, R.; Budak, G.; Ekinci, R.

2004-01-01

Mankind still depend on traditional herbal medicine for the treatment of various diseases and ailments. Elemental composition and concentration of medicinal plants have been investigated by energy dispersive X-ray fluorescence. The elements present in medicinal plants are P, Cl, K, Ca, S, Al, Ti, V, Rb, Sr, Zr, Nb, Mo, In, Sn, I and Ce. The physical basis of the used analytical method, the experimental set up and the procedure of sample preparation are presented. (author)

Energy-Dispersive X-Ray Fluorescence Spectrometry: A Long Overdue Addition to the Chemistry Curriculum

Science.gov (United States)

Palmer, Peter T.

2011-01-01

Portable Energy-Dispersive X-Ray Fluorescence (XRF) analyzers have undergone significant improvements over the past decade. Salient advantages of XRF for elemental analysis include minimal sample preparation, multielement analysis capabilities, detection limits in the low parts per million (ppm) range, and analysis times on the order of 1 min.…

Automated energy-dispersive x-ray determination of trace elements in stream sediments

International Nuclear Information System (INIS)

Hansel, J.M.; Martell, C.J.

1977-01-01

Nickel, copper, tungsten, lead, bismuth, niobium, silver, cadmium, and tin are determined in stream sediments using a computer-controlled energy-dispersive x-ray fluorescence system. The system consists of an automatic 20-position sample changer, a silicon lithium-drifted detector, a pulsed molybdenum transmission-target x-ray tube, a multichannel analyzer, and a minicomputer. Samples are analyzed as minus 325-mesh powders. A computer program positions the samples, unfolds overlapping peaks, determines peak intensities for each element, and calculates the ratio of the intensity of each peak to that of the molybdenum Kα Compton peak. Concentrations of each element are then calculated using equations obtained by analyzing prepared standards. Detection limits range from 5 ppM for silver, cadmium, lead, and bismuth to 20 ppM for niobium. The relative standard is 10 percent or less at the 100-ppM level and 20 percent at the 20-ppM level. Samples can be analyzed at the rate of sixty per day

Cr and Yb markers determination in animal feces by energy dispersive X-ray fluorescence

International Nuclear Information System (INIS)

Almeida, Eduardo de; Senicato, Luis A; Nascimento Filho, Virgilio F.; Gomide, Catarina A.

2007-01-01

Chromium and Ytterbium elements are utilized in animal nutritional studies as markers. This paper describes an analytical method for Cr and Yb determination in solid buffalo feces sample using standard addition method and energy dispersive X-ray spectrometry (EDXRF) technique. One gram dried sample was pressed manually in an XRF sample cup with Mylar film (6.3 μm thickness) in the bottom. The experimental conditions were: Mo target X-ray tube with Zr filter, operated at 25 kV/10 mA, and 500 s of acquisition time. The limits of detection for Cr and Yb were 16.6 and 11.4 mg/kg, respectively. This methodology has showed appropriated for simultaneous Cr and Yb determination as marker in animal feces. (author)

Cr and Yb markers determination in animal feces by energy dispersive X-ray fluorescence

Energy Technology Data Exchange (ETDEWEB)

Almeida, Eduardo de; Senicato, Luis A; Nascimento Filho, Virgilio F. [Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil). Lab. de Instrumentacao Nuclear (LIN)]. E-mail: edualm@usp.br; Gomide, Catarina A. [Universidade de Sao Paulo (USP), Pirassununga, SP (Brazil). Faculdade de Zootecnia e Engenharia de Alimentos (FZEA). Dept. de Zootecnia]. E-mail: cbgomide@usp.br

2007-07-01

Chromium and Ytterbium elements are utilized in animal nutritional studies as markers. This paper describes an analytical method for Cr and Yb determination in solid buffalo feces sample using standard addition method and energy dispersive X-ray spectrometry (EDXRF) technique. One gram dried sample was pressed manually in an XRF sample cup with Mylar film (6.3 {mu}m thickness) in the bottom. The experimental conditions were: Mo target X-ray tube with Zr filter, operated at 25 kV/10 mA, and 500 s of acquisition time. The limits of detection for Cr and Yb were 16.6 and 11.4 mg/kg, respectively. This methodology has showed appropriated for simultaneous Cr and Yb determination as marker in animal feces. (author)

A rotational and axial motion system load frame insert for in situ high energy x-ray studies

Energy Technology Data Exchange (ETDEWEB)

Shade, Paul A., E-mail: paul.shade.1@us.af.mil; Schuren, Jay C.; Turner, Todd J. [Materials and Manufacturing Directorate, Air Force Research Laboratory, Wright-Patterson AFB, Ohio 45433 (United States); Blank, Basil [PulseRay, Beaver Dams, New York 14812 (United States); Kenesei, Peter; Goetze, Kurt; Lienert, Ulrich; Almer, Jonathan [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Suter, Robert M. [Carnegie Mellon University, Pittsburgh, Pennsylvania 15213 (United States); Bernier, Joel V.; Li, Shiu Fai [Engineering Directorate, Lawrence Livermore National Laboratory, Livermore, California 94550 (United States); Lind, Jonathan [Carnegie Mellon University, Pittsburgh, Pennsylvania 15213 (United States); Engineering Directorate, Lawrence Livermore National Laboratory, Livermore, California 94550 (United States)

2015-09-15

High energy x-ray characterization methods hold great potential for gaining insight into the behavior of materials and providing comparison datasets for the validation and development of mesoscale modeling tools. A suite of techniques have been developed by the x-ray community for characterizing the 3D structure and micromechanical state of polycrystalline materials; however, combining these techniques with in situ mechanical testing under well characterized and controlled boundary conditions has been challenging due to experimental design requirements, which demand new high-precision hardware as well as access to high-energy x-ray beamlines. We describe the design and performance of a load frame insert with a rotational and axial motion system that has been developed to meet these requirements. An example dataset from a deforming titanium alloy demonstrates the new capability.

Energy dispersive detector for white beam synchrotron x-ray fluorescence imaging

Energy Technology Data Exchange (ETDEWEB)

Wilson, Matthew D., E-mail: Matt.Wilson@stfc.ac.uk; Seller, Paul; Veale, Matthew C. [Science and Technology Facilities Council, Rutherford Appleton Laboratory, Harwell Campus,UK (United Kingdom); Connolley, Thomas [Diamond Light Source, I12 Beamline, Harwell Campus, Didcot, Oxfordshire (United Kingdom); Dolbnya, Igor P.; Malandain, Andrew; Sawhney, Kawal [Diamond Light Source, B16 Beamline, Harwell Campus, Didcot, Oxfordshire (United Kingdom); Grant, Patrick S.; Liotti, Enzo; Lui, Andrew [Department of Materials, University of Oxford Parks Road, Oxford (United Kingdom)

2016-07-27

A novel, “single-shot” fluorescence imaging technique has been demonstrated on the B16 beamline at the Diamond Light Source synchrotron using the HEXITEC energy dispersive imaging detector. A custom made furnace with 200µm thick metal alloy samples was positioned in a white X-ray beam with a hole made in the furnace walls to allow the transmitted beam to be imaged with a conventional X-ray imaging camera consisting of a 500 µm thick single crystal LYSO scintillator, mirror and lens coupled to an AVT Manta G125B CCD sensor. The samples were positioned 45° to the incident beam to enable simultaneous transmission and fluorescence imaging. The HEXITEC detector was positioned at 90° to the sample with a 50 µm pinhole 13 cm from the sample and the detector positioned 2.3m from pinhole. The geometric magnification provided a field of view of 1.1×1.1mm{sup 2} with one of the 80×80 pixels imaging an area equivalent to 13µm{sup 2}. Al-Cu alloys doped with Zr, Ag and Mo were imaged in transmission and fluorescence mode. The fluorescence images showed that the dopant metals could be simultaneously imaged with sufficient counts on all 80x80 pixels within 60 s, with the X-ray flux limiting the fluorescence imaging rate. This technique demonstrated that it is possible to simultaneously image and identify multiple elements on a spatial resolution scale ~10µm or higher without the time consuming need to scan monochromatic energies or raster scan a focused beam of X-rays. Moving to high flux beamlines and using an array of detectors could improve the imaging speed of the technique with element specific imaging estimated to be on a 1 s timescale.

Energy dispersive detector for white beam synchrotron x-ray fluorescence imaging

International Nuclear Information System (INIS)

Wilson, Matthew D.; Seller, Paul; Veale, Matthew C.; Connolley, Thomas; Dolbnya, Igor P.; Malandain, Andrew; Sawhney, Kawal; Grant, Patrick S.; Liotti, Enzo; Lui, Andrew

2016-01-01

A novel, “single-shot” fluorescence imaging technique has been demonstrated on the B16 beamline at the Diamond Light Source synchrotron using the HEXITEC energy dispersive imaging detector. A custom made furnace with 200µm thick metal alloy samples was positioned in a white X-ray beam with a hole made in the furnace walls to allow the transmitted beam to be imaged with a conventional X-ray imaging camera consisting of a 500 µm thick single crystal LYSO scintillator, mirror and lens coupled to an AVT Manta G125B CCD sensor. The samples were positioned 45° to the incident beam to enable simultaneous transmission and fluorescence imaging. The HEXITEC detector was positioned at 90° to the sample with a 50 µm pinhole 13 cm from the sample and the detector positioned 2.3m from pinhole. The geometric magnification provided a field of view of 1.1×1.1mm"2 with one of the 80×80 pixels imaging an area equivalent to 13µm"2. Al-Cu alloys doped with Zr, Ag and Mo were imaged in transmission and fluorescence mode. The fluorescence images showed that the dopant metals could be simultaneously imaged with sufficient counts on all 80x80 pixels within 60 s, with the X-ray flux limiting the fluorescence imaging rate. This technique demonstrated that it is possible to simultaneously image and identify multiple elements on a spatial resolution scale ~10µm or higher without the time consuming need to scan monochromatic energies or raster scan a focused beam of X-rays. Moving to high flux beamlines and using an array of detectors could improve the imaging speed of the technique with element specific imaging estimated to be on a 1 s timescale.

X-ray chemical analyzer for field applications

International Nuclear Information System (INIS)

Gamba, O.O.M.

1977-01-01

A self-supporting portable field multichannel x-ray chemical analyzer system is claimed. It comprises a lightweight, flexibly connected, remotely locatable, radioisotope-excited sensing probe utilizing a cryogenically-cooled solid state semi-conductor crystal detector for fast in situ non-destructive, qualitative and quantitative analysis of elements in solid, powder, liquid or slurried form, utilizing an x-ray energy dispersive spectrometry technique

Low energy x-ray spectrometer

International Nuclear Information System (INIS)

Woodruff, W.R.

1981-01-01

A subkilovolt spectrometer has been produced to permit high-energy-resolution, time-dependent x-ray intensity measurements. The diffracting element is a curved mica (d = 9.95A) crystal. To preclude higher order (n > 1) diffractions, a carbon x-ray mirror that reflects only photons with energies less than approx. 1.1 keV is utilized ahead of the diffracting element. The nominal energy range of interest is 800 to 900 eV. The diffracted photons are detected by a gold-surface photoelectric diode designed to have a very good frequency response, and whose current is recorded on an oscilloscope. A thin, aluminium light barrier is placed between the diffracting crystal and the photoelectric diode detector to keep any uv generated on or scattered by the crystal from illuminating the detector. High spectral energy resolution is provided by many photocathodes between 8- and 50-eV wide placed serially along the diffracted x-ray beam at the detector position. The spectrometer was calibrated for energy and energy dispersion using the Ni Lα 1 2 lines produced in the LLNL IONAC accelerator and in third order using a molybdenum target x-ray tube. For the latter calibration the carbon mirror was replaced by one surfaced with rhodium to raise the cut-off energy to about 3 keV. The carbon mirror reflection dependence on energy was measured using one of our Henke x-ray sources. The curved mica crystal diffraction efficiency was measured on our Low-Energy x-ray (LEX) machine. The spectrometer performs well although some changes in the way the x-ray mirror is held are desirable. 16 figures

A wavelet-based Gaussian method for energy dispersive X-ray fluorescence spectrum

Directory of Open Access Journals (Sweden)

Pan Liu

2017-05-01

Full Text Available This paper presents a wavelet-based Gaussian method (WGM for the peak intensity estimation of energy dispersive X-ray fluorescence (EDXRF. The relationship between the parameters of Gaussian curve and the wavelet coefficients of Gaussian peak point is firstly established based on the Mexican hat wavelet. It is found that the Gaussian parameters can be accurately calculated by any two wavelet coefficients at the peak point which has to be known. This fact leads to a local Gaussian estimation method for spectral peaks, which estimates the Gaussian parameters based on the detail wavelet coefficients of Gaussian peak point. The proposed method is tested via simulated and measured spectra from an energy X-ray spectrometer, and compared with some existing methods. The results prove that the proposed method can directly estimate the peak intensity of EDXRF free from the background information, and also effectively distinguish overlap peaks in EDXRF spectrum.

A laser heating facility for energy-dispersive X-ray absorption spectroscopy

DEFF Research Database (Denmark)

Kantor, Innokenty; Marini, C.; Mathon, O.

2018-01-01

A double-sided laser heating setup for diamond anvil cells installed on the ID24 beamline of the ESRF is presented here. The setup geometry is specially adopted for the needs of energy-dispersive X-ray absorption spectroscopic (XAS) studies of materials under extreme pressure and temperature...... conditions. We illustrate the performance of the facility with a study on metallic nickel at 60 GPa. The XAS data provide the temperature of the melting onset and quantitative information on the structural parameters of the first coordination shell in the hot solid up to melting....

ENDIX. A computer program to simulate energy dispersive X-ray and synchrotron powder diffraction diagrams

International Nuclear Information System (INIS)

Hovestreydt, E.; Karlsruhe Univ.; Parthe, E.; Benedict, U.

1987-01-01

A Fortran 77 computer program is described which allows the simulation of energy dispersive X-ray and synchrotron powder diffraction diagrams. The input consists of structural data (space group, unit cell dimensions, atomic positional and displacement parameters) and information on the experimental conditions (chosen Bragg angle, type of X-ray tube and applied voltage or operating power of synchrotron radiation source). The output consists of the normalized intensities of the diffraction lines, listed by increasing energy (in keV), and of an optional intensity-energy plot. The intensities are calculated with due consideration of the wave-length dependence of both the anomalous dispersion and the absorption coefficients. For a better agreement between observed and calculated spectra provision is made to optionally superimpose, on the calculated diffraction line spectrum, all additional lines such as fluorescence and emission lines and escape peaks. The different effects which have been considered in the simulation are discussed in some detail. A sample calculation of the energy dispersive powder diffraction pattern of UPt 3 (Ni 3 Sn structure type) is given. Warning: the user of ENDIX should be aware that for a successful application it is necessary to adapt the program to correspond to the actual experimental conditions. Even then, due to the only approximately known values of certain functions, the agreement between observed and calculated intensities will not be as good as for angle dispersive diffraction methods

Characterization of breast tissue using energy-dispersive X-ray diffraction computed tomography

International Nuclear Information System (INIS)

Pani, S.; Cook, E.J.; Horrocks, J.A.; Jones, J.L.; Speller, R.D.

2010-01-01

A method for sample characterization using energy-dispersive X-ray diffraction computed tomography (EDXRDCT) is presented. The procedures for extracting diffraction patterns from the data and the corrections applied are discussed. The procedures were applied to the characterization of breast tissue samples, 6 mm in diameter. Comparison with histological sections of the samples confirmed the possibility of grouping the patterns into five families, corresponding to adipose tissue, fibrosis, poorly differentiated cancer, well differentiated cancer and benign tumour.

The description of compton lines in energy-dispersive x-ray Fluorescence

International Nuclear Information System (INIS)

Van Gysel, Mon; Van Espen, P.J.M.

2001-01-01

Energy-Dispersive X-Ray Fluorescence (ED-XRF) is a non-destructive technique for the element analysis in a concentration range ppm - % making use of X rays up to 100 keV. Generally, two photon matter interactions occur, respectively absorption and scattering. The absorption of incident photons gives raise to characteristic lines. Scattering gives an incoherent and a coherent line. A Gaussian peak model is adequate to describe the characteristic and coherent scattered lines. Incoherent lines appear as non-Gaussian, broadened peaks. The profile of a Compton peak is complex. It depends on the geometry and the composition of the sample. Especially, when analyzing a low Z matrix; dominant scattering and multiple scattering may cause large interferences. The absence of an appropriate fitting model makes the Compton profile seen as a limiting factor in the evaluation of spectra. An accurate description of incoherent lines should improve quantitative analysis. Therefore, a suitable fitting model, making use of the expertise of non-linear least squares procedures and Monte-Carlo calculations was systematically investigated. The proposed model, containing a modified Gaussian, is tested on experimental data recorded with a HPGe detector

Instrumental aspects of tube-excited energy-dispersive X-ray fluorescence analysis

International Nuclear Information System (INIS)

Adams, F.; Nullens, H.; Espen, P. van

1983-01-01

Energy-dispersive X-ray fluorescence spectrometry is an attractive and widely used method for sensitive multi-element analysis. The method suffers from the extreme density of spectral components in a rather limited energy range which implies the need for computer based spectrum analysis. The method of iterative least squares analysis is the most powerful tool for this. It requires a systematic and accurate description of the spectral features. Other important necessities for accurate analysis are the calibration of the spectrometer and the correction for matrix absorption effects in the sample; they can be calculated from available physical constants. Ours and similar procedures prove that semi-automatic analyses are possible with an accuracy of the order of 5%. (author)

Analysis of agricultural soils by using energy dispersive X-ray fluorescence

International Nuclear Information System (INIS)

Anjos, Marcelino Jose dos

2000-03-01

In this work, we describe an Energy Dispersive x-ray Fluorescence System with a x-ray tube excitation for trace analysis of environmental samples (soil). The system was used to analyze the contamination of metals in treated soils with doses of 10, 20 and 30 ton/ha of compound organic of urban garbage of the type Fertilurb and 10 ton/ha of aviary bed (manure of birds). Samples of roots and foliages of plant radishes cultivated in these soils were also analyzed. The soil samples were collected in five different depths of 0,5, 5-10, 10-20, 20-40 and 40-60 cm. The experimental set-up is composed by an OXFORD X-ray (30 kV, 50 μA and W anode), an ORTEC Si-Li detector, with an energy resolution of about 180 eV at 5.9 keV and an ORTEC multichannel-analyser. The X-ray spectrum tube is quasi-monochromatic by using of Ti filter. Samples were prepared in pellet form with superficial density in the range of 100 mg/cm 2 . The fundamental parameter method was used in order to verify the elemental concentration. It was possible to determine the concentrations of thirteen elements: K, Ca, Ti, Mn, Fe, Cu, Zn, Br, Rb, Sr, Y, Zr and Pb in the treated soils with compounds organic. The results indicate that the values found for K, Ca, Rb, Sr, Zr and Pb are significantly above the upper confidence limits for the control soil (α = 0.05). There is a real different between these elements compared to their relationship in the control soils, (α=0,05). There is a real difference between these elements compared to their relationship in the control soils, confirming the influence of the organic compounds in the soil. (author)

Analysis of Precious Stones Deposited in Various Rock Samples of Mogok Region by energy dispersive X-ray Fluorescence Spectrometry

International Nuclear Information System (INIS)

Kyi Kyi San; Soe Lwin; Win Win Thar; Sein Htoon

2004-06-01

The analysis of precious stones deposited in various rock samples of Mogok region were investigated by the energy dispersive x-ray fluorescence technique. The x-ray machine with Rh target was used to excite the characteristic x-ray from the sample. X-rays emitted from the sample were measured by a high resolution, cooled Si (Li) detector. The calibration was made by the measurement of minerals which composed in each kind of precious stones. The kind of precious stone deposited in the rocks sample was determined by the measurement of minerals from the rock samples compared with those obtained from each kind of precious stones

In situ electrochemical high-energy X-ray diffraction using a capillary working electrode cell geometry

Energy Technology Data Exchange (ETDEWEB)

Young, Matthias J.; Bedford, Nicholas M.; Jiang, Naisheng; Lin, Deqing; Dai, Liming

2017-05-26

The ability to generate new electrochemically active materials for energy generation and storage with improved properties will likely be derived from an understanding of atomic-scale structure/function relationships during electrochemical events. Here, the design and implementation of a new capillary electrochemical cell designed specifically forin situhigh-energy X-ray diffraction measurements is described. By increasing the amount of electrochemically active material in the X-ray path while implementing low-Zcell materials with anisotropic scattering profiles, an order of magnitude enhancement in diffracted X-ray signal over traditional cell geometries for multiple electrochemically active materials is demonstrated. This signal improvement is crucial for high-energy X-ray diffraction measurements and subsequent Fourier transformation into atomic pair distribution functions for atomic-scale structural analysis. As an example, clear structural changes in LiCoO₂under reductive and oxidative conditions using the capillary cell are demonstrated, which agree with prior studies. Accurate modeling of the LiCoO₂diffraction data using reverse Monte Carlo simulations further verifies accurate background subtraction and strong signal from the electrochemically active material, enabled by the capillary working electrode geometry.

Precision and accuracy of multi-element analysis of aerosols using energy-dispersive x-ray fluorescence

International Nuclear Information System (INIS)

Adams, F.; Van Espen, P.

1976-01-01

Measurements have been carried out for the determination of the inherent errors of energy-dispersive X-ray fluorescence and for the evaluation of its precision and accuracy. The accuracy of the method is confirmed by independent determinations on the same samples using other analytical methods

Determination of the structure factors of a LiF powder sample by the energy dispersive x-ray diffraction

International Nuclear Information System (INIS)

Uno, R.; Ahtee, A.; Paakkari, T.

1977-01-01

The structure factors of a LiF powder sample were determined by energy dispersive x-ray diffraction in the range 9 to 25 keV, with the use of a Si(Li) solid state detector, following the method applied on GaP. Since the absorption coefficient of LiF is small at high energy, a fraction of the incident x-rays penetrates through the sample and does not contribute to the diffraction. This effect was taken into account in the determination of the structure factors. Then the structure factors generally agree, within the limit of 5 % error, with those obtained by the usual angle dispersive method, if the penetrated part of the incident beam is less than 40 %. (author)

Energy dispersive X-ray diffraction as a means to identify illicit materials: A preliminary optimisation study

Energy Technology Data Exchange (ETDEWEB)

Cook, Emily [Department of Medical Physics and Bioengineering, UCL, London WC1E 6BT (United Kingdom)]. E-mail: ecook@medphys.ucl.ac.uk; Fong, Ruby [Clinical Physics Department, St Bartholomew' s Hospital, London EC1A 7BE (United Kingdom); Horrocks, Julie [Clinical Physics Department, St Bartholomew' s Hospital, London EC1A 7BE (United Kingdom); Wilkinson, David [HOSDB, Woodcock Hill, Sandridge, Herts. AL4 9HQ (United Kingdom); Speller, Robert [Department of Medical Physics and Bioengineering, UCL, London WC1E 6BT (United Kingdom)

2007-08-15

Energy dispersive X-ray diffraction is proposed as a suitable non-destructive method to rapidly identify illicit drugs in parcels. A preliminary data set of 7 illicit drug samples and a possible cutting agent has been collected with a range of count times using a tungsten target X-ray source, a high resolution HpGe detector and a variable geometry diffraction cell. These results have been used to calibrate and train multivariate analysis software to predict the drug content in previously unseen spectra.

Energy dispersive X-ray diffraction as a means to identify illicit materials: A preliminary optimisation study

International Nuclear Information System (INIS)

Cook, Emily; Fong, Ruby; Horrocks, Julie; Wilkinson, David; Speller, Robert

2007-01-01

Energy dispersive X-ray diffraction is proposed as a suitable non-destructive method to rapidly identify illicit drugs in parcels. A preliminary data set of 7 illicit drug samples and a possible cutting agent has been collected with a range of count times using a tungsten target X-ray source, a high resolution HpGe detector and a variable geometry diffraction cell. These results have been used to calibrate and train multivariate analysis software to predict the drug content in previously unseen spectra

Scanning electron microscope/energy dispersive x ray analysis of impact residues in LDEF tray clamps

Science.gov (United States)

Bernhard, Ronald P.; Durin, Christian; Zolensky, Michael E.

1993-01-01

Detailed optical scanning of tray clamps is being conducted in the Facility for the Optical Inspection of Large Surfaces at JSC to locate and document impacts as small as 40 microns in diameter. Residues from selected impacts are then being characterized by Scanning Electron Microscopy/Energy Dispersive X-ray Analysis at CNES. Results from this analysis will be the initial step to classifying projectile residues into specific sources.

Radioisotope induced energy dispersive X-ray fluorescence - a diagnostic tool in clinical science

International Nuclear Information System (INIS)

Joseph, Daisy

2010-01-01

Full text: Energy dispersive X-ray fluorescence (EDXRF) - an ideal technique for detecting trace elements in drugs have been used for analyzing drugs marked as Zn supplements (Jasad Bhasm) used for growth in children and Ayurvedic medicines containing toxic elements such as Arsenic (As) and Mercury (Hg). Folklore medicines obtained as plants extracts from Manipur plants were also analyzed for their composition. Zn supplements (Jasad Bhasm) manufactured by various manufacturers were analyzed for their trace elements besides Zn and were compared with laboratory preparations. Similarly the Ayurvedic medicines from different companies were analyzed for their metal composition. All samples in powder form were pelletized and analyzed using an X-ray spectrometer consisting of a Cd 109 radioisotope source, Si (Li) detector of resolution 170 eV at 5.9 KeV Mn X-ray, preamplifier, amplifier and a PC based multichannel analyzer. Varying amounts of trace elements were detected in Jasad Bhasm and interesting results (As and Hg) were seen in the Ayurvedic medicines in addition to other trace elements such as K,Ca,Fe,Cu and Zn. In Manipur plant extracts Sr was predominantly seen in most samples. Their levels of toxicity and significance to human health and diseases will be discussed in the remaining sections of the paper

Capillary based Li-air batteries for in situ synchrotron X-ray powder diffraction studies

DEFF Research Database (Denmark)

Storm, Mie Møller; Johnsen, Rune E.; Younesi, Reza

2015-01-01

For Li-air batteries to reach their full potential as energy storage system, a complete understanding of the conditions and reactions in the battery during operation is needed. To follow the reactions in situ a capillary-based Li-O2 battery has been developed for synchrotron-based in situ X......-ray powder diffraction (XRPD). In this article, we present the results for the analysis of 1st and 2nd deep discharge and charge for a cathode being cycled between 2 and 4.6 V. The crystalline precipitation of Li2O2 only is observed in the capillary battery. However, there are indications of side reactions...... of constant exposure of X-ray radiation to the electrolyte and cathode during charge of the battery was also investigated. X-ray exposure during charge leads to changes in the development of the intensity and the FWHM of the Li2O2 diffraction peaks. The X-ray diffraction results are supported by ex situ X...

A Next-Generation Hard X-Ray Nanoprobe Beamline for In Situ Studies of Energy Materials and Devices

Science.gov (United States)

Maser, Jörg; Lai, Barry; Buonassisi, Tonio; Cai, Zhonghou; Chen, Si; Finney, Lydia; Gleber, Sophie-Charlotte; Jacobsen, Chris; Preissner, Curt; Roehrig, Chris; Rose, Volker; Shu, Deming; Vine, David; Vogt, Stefan

2014-01-01

The Advanced Photon Source is developing a suite of new X-ray beamlines to study materials and devices across many length scales and under real conditions. One of the flagship beamlines of the APS upgrade is the In Situ Nanoprobe (ISN) beamline, which will provide in situ and operando characterization of advanced energy materials and devices under varying temperatures, gas ambients, and applied fields, at previously unavailable spatial resolution and throughput. Examples of materials systems include inorganic and organic photovoltaic systems, advanced battery systems, fuel cell components, nanoelectronic devices, advanced building materials and other scientifically and technologically relevant systems. To characterize these systems at very high spatial resolution and trace sensitivity, the ISN will use both nanofocusing mirrors and diffractive optics to achieve spots sizes as small as 20 nm. Nanofocusing mirrors in Kirkpatrick-Baez geometry will provide several orders of magnitude increase in photon flux at a spatial resolution of 50 nm. Diffractive optics such as zone plates and/or multilayer Laue lenses will provide a highest spatial resolution of 20 nm. Coherent diffraction methods will be used to study even small specimen features with sub-10 nm relevant length scale. A high-throughput data acquisition system will be employed to significantly increase operations efficiency and usability of the instrument. The ISN will provide full spectroscopy capabilities to study the chemical state of most materials in the periodic table, and enable X-ray fluorescence tomography. In situ electrical characterization will enable operando studies of energy and electronic devices such as photovoltaic systems and batteries. We describe the optical concept for the ISN beamline, the technical design, and the approach for enabling a broad variety of in situ studies. We furthermore discuss the application of hard X-ray microscopy to study defects in multi-crystalline solar cells, one

Dispersive X-ray fluorescence applications in energy in environmental problems diagnostic

International Nuclear Information System (INIS)

Odino, R.; Souto, B.; Roca, S.; Campomar, W.

1994-01-01

X-ray fluorescence energy was used to detect the grade of contamination due to a Portland cement factory. X-ray fluorescence was used to determine the incidence of a Portland cement plant in the quality of air in its surroundings. Many contaminants (Cu, Pb, Ni, Br) do not come from the Portland cement industry but other industries in the zone

TX 2000: total reflection and 45o energy dispersive x-ray fluorescence spectrometer

International Nuclear Information System (INIS)

Pasti, F.; Torboli, A.; Valdes, M.

2000-01-01

This equipment, developed by Ital Structures, combines two kinds of energy dispersive X-ray fluorescence techniques, the first using total reflection geometry and the second conventional 45 o geometry. The equipment is completely controlled by a PC and to reach the condition of total reflection is very easy because it is enough to load the file with the right position for the corresponding energy. In this apparatus we used an x-ray tube with an alloy anode of Mo/W with a long fine focus at 2200 W. To monochromatize the x-ray beam while choosing, for example, the Mo K alpha or W L alpha or a piece of white spectrum of 33 keV, we use a highly reflective multilayer made of Si/W with 2d = 45.5 A o . The detector used in the equipment is a lithium drifted silicon detector (Si(Li)) with an excellent energy resolution of 135 eV at 5.9 keV and 1000 cps. We developed two programs written in Windows 95, 98 and NT for a 32 bit microprocessor. The first one is called TYACQ32 and has the following functions: first, complete control of the hardware, second automatic alignment of the TX 2000 spectrometer and third acquisition of spectra. The second program is EDXRF32. This is a program to accomplish spectrum and quantitative analysis for TXRF and EDXRF 45 o degrees analysis. (author)

A Rotational and Axial Motion System Load Frame Insert for In Situ High Energy X-Ray Studies (Postprint)

Science.gov (United States)

2015-09-08

Paul A. Shade, Jay C. Schuren, and Todd J. Turner AFRL/RX Basil Blank PulseRay Peter Kenesei, Kurt Goetze, Ulrich Lienert, and Jonathan Almer...AFRL/RX 2) Basil Blank – PulseRay (continued on page 2) 5d. PROJECT NUMBER 4349 5e. TASK NUMBER 0001 5f...2015) A rotational and axial motion system load frame insert for in situ high energy x-ray studies Paul A. Shade,1,a) Basil Blank,2 Jay C. Schuren,1,b

Single-shot full strain tensor determination with microbeam X-ray Laue diffraction and a two-dimensional energy-dispersive detector.

Science.gov (United States)

Abboud, A; Kirchlechner, C; Keckes, J; Conka Nurdan, T; Send, S; Micha, J S; Ulrich, O; Hartmann, R; Strüder, L; Pietsch, U

2017-06-01

The full strain and stress tensor determination in a triaxially stressed single crystal using X-ray diffraction requires a series of lattice spacing measurements at different crystal orientations. This can be achieved using a tunable X-ray source. This article reports on a novel experimental procedure for single-shot full strain tensor determination using polychromatic synchrotron radiation with an energy range from 5 to 23 keV. Microbeam X-ray Laue diffraction patterns were collected from a copper micro-bending beam along the central axis (centroid of the cross section). Taking advantage of a two-dimensional energy-dispersive X-ray detector (pnCCD), the position and energy of the collected Laue spots were measured for multiple positions on the sample, allowing the measurement of variations in the local microstructure. At the same time, both the deviatoric and hydrostatic components of the elastic strain and stress tensors were calculated.

X-ray emission spectroscopy. X-ray fluorescence

International Nuclear Information System (INIS)

Despujols, J.

1992-01-01

Principles of X-ray emission spectrometry are first recalled, then wave-length dispersive and energy dispersive X-ray fluorescence spectrometer are described. They are essentially designed for qualitative and quantitative analysis of elements (Z>10). Sample preparation, calibration, corrections, interferences, accuracy are reviewed. Examples of use in different industries are given. (71 refs.)

Processing and quantification of x-ray energy dispersive spectra in the Analytical Electron Microscope

International Nuclear Information System (INIS)

Zaluzec, N.J.

1988-08-01

Spectral processing in x-ray energy dispersive spectroscopy deals with the extraction of characteristic signals from experimental data. In this text, the four basic procedures for this methodology are reviewed and their limitations outlined. Quantification, on the other hand, deals with the interpretation of the information obtained from spectral processing. Here the limitations are for the most part instrumental in nature. The prospects of higher voltage operation does not, in theory, present any new problems and may in fact prove to be more desirable assuming that electron damage effects do not preclude analysis. 28 refs., 6 figs

Investigations of the phase transition in V3O5 using energy dispersive X-ray diffraction and synchrotron radiation white beam X-ray topography

International Nuclear Information System (INIS)

Asbrink, S.; Gerward, L.; Staun Olsen, J.

1985-01-01

The reversible first order phase transition in V 3 O 5 at T t =155 0 C has been studied using a specially constructed oven, where the temperature can be kept constant within a few hundredths of a degree for several hours. Energy dispersive diffraction measurements have beem made in a temperature region around the phase transition with the fixed crystal method and the θ/2θ scanning method. White beam X-ray topographs have been obtained from the same crystal in the same temperature region using synchrotron radiation. The integrated intensities of the strong h 0 0 reflections show anomalies that are correlated with the corresponding X-ray topographs. Thus, an unexpected increase of crystal perfection is observed a few hundredths of a degree below T t . The energy dependence of the intensity maximum at T t for strong reflections has been determined and semi-quantitatively explained on the basis of extinction theory. (orig.)

In Situ Ptychography of Heterogeneous Catalysts using Hard X-Rays

DEFF Research Database (Denmark)

Baier, Sina; Damsgaard, Christian Danvad; Scholz, Maria

2016-01-01

A new closed cell is presented for in situ X-ray ptychography which allows studies under gas flow and at elevated temperature. In order to gain complementary information by transmission and scanning electron microscopy, the cell makes use of a Protochips E-chipTM which contains a small, thin...... the same sample holder for ex situ electron microscopy before and after the in situ study underlines the unique possibilities available with this combination of electron microscopy and X-ray microscopy on the same sample....

Analytical Energy Dispersive X-Ray Fluorescence Measurements with a Scanty Amounts of Plant and Soil Materials

Science.gov (United States)

Mittal, R.; Rao, P.; Kaur, P.

2018-01-01

Elemental evaluations in scanty powdered material have been made using energy dispersive X-ray fluorescence (EDXRF) measurements, for which formulations along with specific procedure for sample target preparation have been developed. Fractional amount evaluation involves an itinerary of steps; (i) collection of elemental characteristic X-ray counts in EDXRF spectra recorded with different weights of material, (ii) search for linearity between X-ray counts and material weights, (iii) calculation of elemental fractions from the linear fit, and (iv) again linear fitting of calculated fractions with sample weights and its extrapolation to zero weight. Thus, elemental fractions at zero weight are free from material self absorption effects for incident and emitted photons. The analytical procedure after its verification with known synthetic samples of macro-nutrients, potassium and calcium, was used for wheat plant/ soil samples obtained from a pot experiment.

Comparison of sensitivities and detection limits between direct excitation and secondary excitation modes in energy dispersive x-ray fluorescence analysis

International Nuclear Information System (INIS)

Artz, B.E.; Short, M.A.

1976-01-01

A comparison was made between the direct tube excitation mode and the secondary target excitation mode using a Kevex 0810 energy dispersive x-ray fluorescence system. Relative sensitivities and detection limits were determined with two system configurations. The first configuration used a standard, high power, x-ray fluorescence tube to directly excite the specimen. Several x-ray tubes, including chromium, molybdenum, and tungsten, both filtered and not filtered, were employed. The second configuration consisted of using the x-ray tube to excite a secondary target which in turn excited the specimen. Appropriate targets were compared to the direct excitation results. Relative sensitivities and detection limits were determined for K-series lines for elements from magnesium to barium contained in a low atomic number matrix and in a high atomic number matrix

Application of direct peak analysis to energy dispersive x-ray fluorescence spectra

International Nuclear Information System (INIS)

Nielson, K.K.

1977-07-01

A modified Covell method for direct peak analysis has been applied to energy dispersive x-ray fluorescence spectra. The method is background independent and is well-suited to computerized data reduction. It provides acceptable precision, minimizes errors from instrumental gain shift, and permits peak overlap correction. Peak overlap errors exhibit both positive and negative nodes as a function of peak separation distance, and are corrected using concentration ratios determined from thin, single-element standards. Peak precisions and overlaps are evaluated as a function of window width to aid in width selection. Least-square polynomial smoothing prior to peak analysis significantly improves peak area precisions without significantly affecting their accuracies

In Situ Soft X-ray Spectromicroscopy of Early Tricalcium Silicate Hydration

Directory of Open Access Journals (Sweden)

Sungchul Bae

2016-12-01

Full Text Available The understanding and control of early hydration of tricalcium silicate (C3S is of great importance to cement science and concrete technology. However, traditional characterization methods are incapable of providing morphological and spectroscopic information about in situ hydration at the nanoscale. Using soft X-ray spectromicroscopy, we report the changes in morphology and molecular structure of C3S at an early stage of hydration. In situ C3S hydration in a wet cell, beginning with induction (~1 h and acceleration (~4 h periods of up to ~8 h, was studied and compared with ex situ measurements in the deceleration period after 15 h of curing. Analysis of the near-edge X-ray absorption fine structure showed that the Ca binding energy and energy splitting of C3S changed rapidly in the early age of hydration and exhibited values similar to calcium silicate hydrate (C–S–H. The formation of C–S–H nanoseeds in the C3S solution and the development of a fibrillar C–S–H morphology on the C3S surface were visualized. Following this, silicate polymerization accompanied by C–S–H precipitation produced chemical shifts in the peaks of the main Si K edge and in multiple scattering. However, the silicate polymerization process did not significantly affect the Ca binding energy of C–S–H.

A simple method to improve the quantification accuracy of energy-dispersive X-ray microanalysis

International Nuclear Information System (INIS)

Walther, T

2008-01-01

Energy-dispersive X-ray spectroscopy in a transmission electron microscope is a standard tool for chemical microanalysis and routinely provides qualitative information on the presence of all major elements above Z=5 (boron) in a sample. Spectrum quantification relies on suitable corrections for absorption and fluorescence, in particular for thick samples and soft X-rays. A brief presentation is given of an easy way to improve quantification accuracy by evaluating the intensity ratio of two measurements acquired at different detector take-off angles. As the take-off angle determines the effective sample thickness seen by the detector this method corresponds to taking two measurements from the same position at two different thicknesses, which allows to correct absorption and fluorescence more reliably. An analytical solution for determining the depth of a feature embedded in the specimen foil is also provided.

Diffraction anomalous fine structure using X-ray anomalous dispersion

International Nuclear Information System (INIS)

Soejima, Yuji; Kuwajima, Shuichiro

1998-01-01

A use of X-ray anomalous dispersion effects for structure investigation has recently been developed by using synchrotron radiation. One of the interesting method is the observation of anomalous fine structure which arise on diffraction intensity in energy region of incident X-ray at and higher than absorption edge. The phenomenon is so called Diffraction Anomalous Fine Structure (DAFS). DAFS originates in the same physical process an that of EXAFS: namely photoelectric effect at the corresponding atom and the interaction of photoelectron waves between the atom and neighboring atoms. In contrast with EXAFS, the method is available for only the crystalline materials, but shows effective advantages of the structure investigations by a use of diffraction: one is the site selectivity and the other is space selectivity. In the present study, demonstrations of a use of X-ray anomalous dispersion effect for the superstructure determination will be given for the case of PbZrO 3 , then recent trial investigations of DAFS in particular on the superlattice reflections will be introduced. In addition, we discuss about Forbidden Reflection near Edge Diffraction (FRED) which is more recently investigated as a new method of the structure analysis. (author)

The determination of Fe, Mn and Ca in sintered iron and blast-furnace slag by X-ray fluorescent analyses of energy and wave dispersion-comparison of results

International Nuclear Information System (INIS)

Dworak, B.; Gajek, Sz.

1980-01-01

The results of sintered iron and of blast-furnace slag examination obtained by X-ray fluorescent analyses of energy and of wave dispersion are compared. They show that the methods are comparable for such elements as Ca and Fe, whereas for Mn (in sinter) the X-ray fluorescent analysis of wave dispersion is less precise. (author)

Composition measurement in substitutionally disordered materials by atomic resolution energy dispersive X-ray spectroscopy in scanning transmission electron microscopy.

Science.gov (United States)

Chen, Z; Taplin, D J; Weyland, M; Allen, L J; Findlay, S D

2017-05-01

The increasing use of energy dispersive X-ray spectroscopy in atomic resolution scanning transmission electron microscopy invites the question of whether its success in precision composition determination at lower magnifications can be replicated in the atomic resolution regime. In this paper, we explore, through simulation, the prospects for composition measurement via the model system of Al x Ga 1-x As, discussing the approximations used in the modelling, the variability in the signal due to changes in configuration at constant composition, and the ability to distinguish between different compositions. Results are presented in such a way that the number of X-ray counts, and thus the expected variation due to counting statistics, can be gauged for a range of operating conditions. Copyright © 2016 Elsevier B.V. All rights reserved.

Development of analytical software for semi-quantitative analysis of x-ray spectrum acquired from energy-dispersive spectrometer

International Nuclear Information System (INIS)

Karim, A.; Rana, M.A.; Qamar, R.; Latif, A; Ahmad, M.; Farooq, M.A.; Ahmad, Z.

2003-12-01

Software package for elemental analysis for X-ray spectrum obtained from Energy Dispersive Spectrometer (EDS) attached with Scanning Electron Microscope (SEM) has been developed: A Personal Computer Analyzer card PCA-800 is used to acquire data from the EDS. This spectrum is obtained in binary format, which is transformed into ASCII format using PCAII card software. The program is modular in construction and coded using Microsoft's QUICKBASIC compiler linker. Energy line library containing all lines of elements is created for analysis of acquired characteristic X-ray spectrum. Two techniques of peak identification are provided. Statistical tools are employed for smoothing of a curve and for computing area under the curve. Elemental concentration is calculated in weight % and in atomic. (author)

In situ X-ray probing reveals fingerprints of surface platinum oxide.

Science.gov (United States)

Friebel, Daniel; Miller, Daniel J; O'Grady, Christopher P; Anniyev, Toyli; Bargar, John; Bergmann, Uwe; Ogasawara, Hirohito; Wikfeldt, Kjartan Thor; Pettersson, Lars G M; Nilsson, Anders

2011-01-07

In situ X-ray absorption spectroscopy (XAS) at the Pt L(3) edge is a useful probe for Pt-O interactions at polymer electrolyte membrane fuel cell (PEMFC) cathodes. We show that XAS using the high energy resolution fluorescence detection (HERFD) mode, applied to a well-defined monolayer Pt/Rh(111) sample where the bulk penetrating hard X-rays probe only surface Pt atoms, provides a unique sensitivity to structure and chemical bonding at the Pt-electrolyte interface. Ab initio multiple-scattering calculations using the FEFF code and complementary extended X-ray absorption fine structure (EXAFS) results indicate that the commonly observed large increase of the white-line at high electrochemical potentials on PEMFC cathodes originates from platinum oxide formation, whereas previously proposed chemisorbed oxygen-containing species merely give rise to subtle spectral changes.

Dispersive x-ray synchrotron studies of Pt-C multilayers

International Nuclear Information System (INIS)

Smither, R.K.; Rodricks, B.; Lamelas, F.; Medjahed, D.; Dos Passos, W.; Clarke, R.; Ziegler, E.; Fontaine, A.

1989-02-01

We demonstrate the simultaneous acquisition of high-resolution x-ray absorption spectra and scattering data, using a combination of energy-dispersive optics and a two-dimensional CCD detector. Results are presented on the optical constants of Pt and on the reflectivity of a platinum-carbon multilayer at the L/sub III/ absorption edge of Pt. 12 refs., 5 figs

Energy dispersive X-ray fluorescence analysis of ancient coins: The case of Greek silver drachmae from the Emporion site in Spain

International Nuclear Information System (INIS)

Pitarch, A.; Queralt, I.

2010-01-01

Greek colonizers arrived at the Iberian Peninsula at the beginning of the sixth century B.C. and founded a small colony known as Emporion in north-east Spain. By the fifth century B.C., this colony became a small polis with a well-organized administrative structure. In this context, the necessity of coinage was a fact and the first coins were minted. Some of these coins were characterized by using energy dispersive X-ray fluorescence equipment. The analytical study focused on the elemental characterization of the coins minted from the fourth century to the first century B.C. and their compositional evolution during this period. The investigation has pointed out a very high fineness of the alloys throughout the time, with an average silver content around 98.32%, and the feasibility of energy dispersive X-ray fluorescence as a screening tool for the characterization of the alloys.

In situ x-ray fluorescence and californium-252 neutron activation analysis for marine and terrestrial mineral exploration

International Nuclear Information System (INIS)

Wogman, N.A.

1976-12-01

Instrumentation has been designed for in situ analysis of marine and terrestrial minerals using the techniques of x-ray fluorescence and neutron activation analysis. The energy-dispersive x-ray fluorescence analyzer allows more than 20 elements to be quantitatively measured at the 10 ppM level in water depths to 300 m. The analyzer consists of a solid cryogen-cooled Si(Li) detector, a 50 mCi 109 Cd or 57 Co excitation source, and an analyzer-computer system for data storage and manipulation. The neutron activation analysis, which is designed to measure up to 30 elements at parts per hundred to ppM levels, utilizes the man-made element 252 Cf as its neutron activation source. The resulting radioelements which emit characteristic gamma radiation are then analyzed in situ during 2- to 200-s counting intervals with Ge(Li) or NaI(T1) detector systems. An extension of this latter technique, which uses a 252 Cf- 235 U fueled subcritical multiplier, is also being studied. The subcritical facility allows the neutrons from the 252 Cf source to be multiplied, thus providing greater neutron flux. Details of these in situ analysis systems, actual in situ spectra, and recorded data are discussed with respect to the detection of minerals at their varying concentration levels. The system response of each illustrates its usefulness for various rapid environmental mineral exploration studies. These techniques can be utilized on terrestrial surfaces and marine or fresh water sediments. 5 figures, 2 tables

Calibration of energy dispersive x-ray spectrometers for analysis of thin environmental samples

International Nuclear Information System (INIS)

Giauque, R.D.; Garrett, R.B.; Goda, L.Y.

1976-01-01

Four separate techniques for calibrating energy dispersive x-ray spectrometers are described. They include the use of (1) individual evaporated elemental thin-film standards, (2) nebulized multielement standard solution deposits to determine relative elemental sensitivity factors, (3) a semi-empirical approach to calculate relative elemental sensitivity factors, and (4) thick pure element disks. The first three techniques are applicable for a broad range of elements. The utilization of nebulized multielement standard solution deposits, along with an evaporated single element thin-film standard for absolute system calibration, is the most accurate method of the calibration techniques described

Characterization of Roman glass tesserae from the Coriglia excavation site (Italy) via energy-dispersive X-ray fluorescence spectrometry and Raman spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Donais, Mary Kate; Sparks, Andrew; Redente, Monica [Saint Anselm College, Department of Chemistry, Manchester, NH (United States); Pevenage, Jolien van; Moens, Luc; Vincze, Laszlo [Ghent University, Department of Analytical Chemistry, Ghent (Belgium); George, David B. [Saint Anselm College, Department of Classics, Manchester, NH (United States); Vandenabeele, Peter [Ghent University, Department of Archaeology, Ghent (Belgium)

2016-12-15

The combined use of handheld energy-dispersive X-ray fluorescence spectrometry, Raman spectroscopy, and micro-energy-dispersive X-ray fluorescence spectrometry permitted the characterization of Roman glass tesserae excavation from the Coriglia (Italy) archeological site. Analyses of ten different glass colors were conducted as spot analyses on intact samples and as both spot analyses and line scans on select cross-sectioned samples. The elemental and molecular information gained from these spectral measurements allowed for the qualitative chemical characterization of the bulk glass, decolorants, opacifiers, and coloring agents. The use of an antimony opacifier in many of the samples supports the late Imperial phasing as determined through numismatic, fresco, ceramics, and architectural evidence. And dealinization of the exterior glass layers caused by the burial environment was confirmed. (orig.)

The design and fabrication of power splitter used in the timescale system of soft X-ray energy dispersive spectrometer in ICF experiment

International Nuclear Information System (INIS)

Zhang Huige; China Academy of Engineering Physics, Mianyang; Bai Lixin; Yu Ruizhen; Yang Cunbang; Su Cunxiao

2006-01-01

An improved eight power splitter is designed and fabricated newly, which is crucial in the time-scale system of soft X-ray energy dispersive spectrometer. The spectrometer is used in ICF laser facility to measure the evolution of soft X-ray spectrum, whose duration is only several nanoseconds. The synchronization and high bandwidth of signals produced by power splitter are tested, which shows the power splitter could meet the strict requirements of the experiments. The discussion of further improvement of power splitter are also presented. (authors)

X-Ray Source Heights in a Solar Flare: Thick-Target Versus Thermal Conduction Front Heating

Science.gov (United States)

Reep, J. W.; Bradshaw, S. J.; Holman, G. D.

2016-01-01

Observations of solar flares with RHESSI have shown X-ray sources traveling along flaring loops, from the corona down to the chromosphere and back up. The 2002 November 28 C1.1 flare, first observed with RHESSI by Sui et al. and quantitatively analyzed by O'Flannagain et al., very clearly shows this behavior. By employing numerical experiments, we use these observations of X-ray source height motions as a constraint to distinguish between heating due to a non-thermal electron beam and in situ energy deposition in the corona. We find that both heating scenarios can reproduce the observed light curves, but our results favor non-thermal heating. In situ heating is inconsistent with the observed X-ray source morphology and always gives a height dispersion with photon energy opposite to what is observed.

Ship-Borne Geochemical Investigations of Deep-Sea Manganese-Nodule Deposits in the Pacific Using a Radioisotope Energy-Dispersive X-Ray System

DEFF Research Database (Denmark)

Friedrich, G.H.W.; Kunzendorf, Helmar; Plüger, W.L.

1974-01-01

A radioisotope energy-dispersive X-ray (EDX) system has been used on board the German research vessel “Valdivia” during an exploration expedition in the northern equatorial Pacific in 1973. The instrumentation used consisted of an X-ray detection system incorporating a 30 mm2 effective-area Si (Li......) detector with a measured energy resolution of 195 eV for Mn Kα X-rays, standard nuclear electronics, a 1024-channel analyser and a data read-out unit. The X-ray spectra in the manganese-nodule samples were excited by a 30-mCi 238Pu source. The six elements Mn, Fe, Co, Ni, Cu and Zn were analysed on board....... Precision values for the analyses were less than 3% for Mn, Fe, Ni, Cu and Zn and about 5% for Co. A total amount of 350 analyses was carried out during a one-month cruise. Average contents of 190 analysed whole manganese-nodule samples from all the sampling sites of the covered area were 23.3% Mn, 6.7% Fe...

Fast GPU-based spot extraction for energy-dispersive X-ray Laue diffraction

International Nuclear Information System (INIS)

Alghabi, F.; Schipper, U.; Kolb, A.; Send, S.; Abboud, A.; Pashniak, N.; Pietsch, U.

2014-01-01

This paper describes a novel method for fast online analysis of X-ray Laue spots taken by means of an energy-dispersive X-ray 2D detector. Current pnCCD detectors typically operate at some 100 Hz (up to a maximum of 400 Hz) and have a resolution of 384 × 384 pixels, future devices head for even higher pixel counts and frame rates. The proposed online data analysis is based on a computer utilizing multiple Graphics Processing Units (GPUs), which allow for fast and parallel data processing. Our multi-GPU based algorithm is compliant with the rules of stream-based data processing, for which GPUs are optimized. The paper's main contribution is therefore an alternative algorithm for the determination of spot positions and energies over the full sequence of pnCCD data frames. Furthermore, an improved background suppression algorithm is presented.The resulting system is able to process data at the maximum acquisition rate of 400 Hz. We present a detailed analysis of the spot positions and energies deduced from a prior (single-core) CPU-based and the novel GPU-based data processing, showing that the parallel computed results using the GPU implementation are at least of the same quality as prior CPU-based results. Furthermore, the GPU-based algorithm is able to speed up the data processing by a factor of 7 (in comparison to single-core CPU-based algorithm) which effectively makes the detector system more suitable for online data processing

Dendrochemical patterns of calcium, zinc, and potassium related to internal factors detected by energy dispersive X-ray fluorescence (EDXRF)

Science.gov (United States)

Kevin T. Smith; Jean Christophe Balouet; Walter C. Shortle; Michel Chalot; François Beaujard; Hakan Grudd; Don A. Vroblesky; Joel G. Burken

2014-01-01

Energy dispersive X-ray fluorescence (EDXRF) provides highly sensitive and precise spatial resolution of cation content in individual annual growth rings in trees. The sensitivity and precision have prompted successful applications to forensic dendrochemistry and the timing of environmental releases of contaminants. These applications have highlighted the need to...

Fundamental parameters method for quantitative energy dispersive x-ray fluorescence analysis

International Nuclear Information System (INIS)

Demirel, H.; Zararsiz, A.

1986-01-01

In this study, the requirement of the standart material in photon excited energy distributed X-ray fluorescence analysis has been removed. The interaction of X-rays with matter has been taken into account. A computer program has been developed by using the fundamental parameters of X-ray fluorescence technique and the spectral intensity 'K' of pure elements at saturation thickness has been obtained. For experimental purpose a convenient source-target-detector geometry has been designed. In order to excite the samples,Cd-109 radioisotope source has been used. The peak intensities has been obtained in a vacum chamber by counting the emitted X-rays. The calculation of concentration has been performed for double mixed samples correcting the effects of absorption and enchancement factors. The results were in conformity with their certificate values. (author)

Study of soil aggregate breakdown dynamics under low dispersive ultrasonic energies with sedimentation and X-ray attenuation

Science.gov (United States)

Schomakers, Jasmin; Zehetner, Franz; Mentler, Axel; Ottner, Franz; Mayer, Herwig

2015-10-01

It has been increasingly recognized that soil organic matter stabilization is strongly controlled by physical binding within soil aggregates. It is therefore essential to measure soil aggregate stability reliably over a wide range of disruptive energies and different aggregate sizes. To this end, we tested highaccuracy ultrasonic dispersion in combination with subsequent sedimentation and X-ray attenuation. Three arable topsoils (notillage) from Central Europe were subjected to ultrasound at four different specific energy levels: 0.5, 6.7, 100 and 500 J cm-3, and the resulting suspensions were analyzed for aggregate size distribution by wet sieving (2 000-63 μm) and sedimentation/X-ray attenuation (63-2 μm). The combination of wet sieving and sedimentation technique allowed for a continuous analysis, at high resolution, of soil aggregate breakdown dynamics after defined energy inputs. Our results show that aggregate size distribution strongly varied with sonication energy input and soil type. The strongest effects were observed in the range of low specific energies (aggregate stability and release of soil organic matter upon aggregate breakdown.

Study of soil aggregate breakdown dynamics under low dispersive ultrasonic energies with sedimentation and X-ray attenuation**

Science.gov (United States)

Schomakers, Jasmin; Zehetner, Franz; Mentler, Axel; Ottner, Franz; Mayer, Herwig

2016-01-01

It has been increasingly recognized that soil organic matter stabilization is strongly controlled by physical binding within soil aggregates. It is therefore essential to measure soil aggregate stability reliably over a wide range of disruptive energies and different aggregate sizes. To this end, we tested high-accuracy ultrasonic dispersion in combination with subsequent sedimentation and X-ray attenuation. Three arable topsoils (notillage) from Central Europe were subjected to ultrasound at four different specific energy levels: 0.5, 6.7, 100 and 500 J cm−3, and the resulting suspensions were analyzed for aggregate size distribution by wet sieving (2 000-63 μm) and sedimentation/X-ray attenuation (63-2 μm). The combination of wet sieving and sedimentation technique allowed for a continuous analysis, at high resolution, of soil aggregate breakdown dynamics after defined energy inputs. Our results show that aggregate size distribution strongly varied with sonication energy input and soil type. The strongest effects were observed in the range of low specific energies (aggregate stability and release of soil organic matter upon aggregate breakdown. PMID:27099408

Aluminum-containing dense deposits of the glomerular basement membrane: identification by energy dispersive X-ray analysis

International Nuclear Information System (INIS)

Smith, D.M. Jr.; Pitcock, J.A.; Murphy, W.M.

1982-01-01

Heavy metals, including gold, mercury, lead, bismuth, and cadmium, have the potential to cause renal disease. With the development of X-ray microanalysis, these heavy metals can now be identified in tissue deposits. This report describes a case of renal failure, probably related to dysproteinemia, in which granular, electron-opaque dense deposits were present in the glomerular basement membranes. Energy dispersive X-ray analysis demonstrated that these dense deposits contained aluminum. An analysis of this patient's history in relation to the current knowledge of aluminum metabolism suggests that the aluminum deposition occurred secondary to previous glomerular injury. This case emphasizes the need to utilize heavy metal identification technology whenever granular, electron-opaque dense deposits are identified and represents, to our knowledge, the first study to document aluminum deposits within the glomerular basement membrane of humans

Quantitative analysis without standards using local peak-to-background ratios with the energy dispersive X-ray microanalyzer EDR-184

International Nuclear Information System (INIS)

Eggert, F.; Heckel, J.

1986-01-01

The method realized in program QMA-184 of the energy dispersive X-Ray-Microanalyzer EDR-184 for quantitative spectra analyzing of bulk materials by using local peak-to-background ratios is described in detail. The authors demonstrate efficiency and limitations of the used method by discussion of experimental results. (author)

Determination of 40K radioactivity in the soil using energy dispersive X ray fluorescence spectrometer

International Nuclear Information System (INIS)

Lu Weiwei; Song Fuxiang; Zeng Liping; Lu Hongning

2012-01-01

The 40 K radioactive of' the pressed powder sample was determined by Epsilon 5 high-energy polarized energy dispersive X ray fluorescence (EDXRF) spectrometer. The correlation coefficient of the standard curve method was 0.9910, the precision was 2.98% and the relative deviation of the measurement standard samples was up to 6.40%, which showed that the precision and accuracy of the method were also good. Simultaneous measurement of seven soil samples using this method and γ-spectrometer were carried, the results of two analytical methods were compared using a paired t-test by SPSS program, which showed that there was no significant difference in the two sets of data, P>0.05. It indicated that EDXRF could be a potential simple method for analyzing 40 K radioactive in soil samples. (authors)

In Situ X-ray Diffraction Studies of Cathode Materials in Lithium Batteries

International Nuclear Information System (INIS)

Yang, X. Q.; Sun, X.; McBreen, J.; Mukerjee, S.; Gao, Yuan; Yakovleva, M. V.; Xing, X. K.; Daroux, M. L.

1998-01-01

There is an increasing interest in lithiated transition metal oxides because of their use as cathodes in lithium batteries. LiCoO 2 , LiNiO 2 and LiMn 2 O 4 are the three most widely used and studied materials, At present, although it is relative expensive and toxic, LiCoO 2 is the material of choice in commercial lithium ion batteries because of its ease of manufacture, better thermal stability and cycle life. However, the potential use of lithium ion batteries with larger capacity for power tools and electric vehicles in the future will demand new cathode materials with higher energy density, lower cost and better thermal stability. LiNiO 2 is isostructural with LiCoO 2 . It offers lower cost and high energy density than LiCoO 2 . However, it has much poorer thermal stability than LiCoO 2 , in the charged (delithiated) state. Co, Al, and other elements have been used to partially replace Ni in LiNiO 2 system in order to increase the thermal stability. LiMn 2 O 4 has the highest thermal stability and lowest cost and toxicity. However, the low energy density and poor cycle life at elevated temperature are the major obstacles for this material. In order to develop safer, cheaper, and better performance cathode materials, the in-depth understanding of the relationships between the thermal stability and structure, performance and structure are very important. The performance here includes energy density and cycle life of the cathode materials. X-ray diffraction (XRD) is one of the most powerful tools to study these relationships. The pioneer ex situ XRD work on cathode materials for lithium batteries was done by Ohzuku. His XRD studies on LiMn 2 O 4 , LiCoO 2 , LiNiO 2 , LiNi 0.5 Co 0.5 O 2 , and LiAl x Ni 1-x O 2 cathodes at different states of charge have provided important guidelines for the development of these new materials. However, the kinetic nature of the battery system definitely requires an in situ XRD technique to study the detail structural changes of the

Elementary analysis by means of the x fluorescence and energy dispersion

International Nuclear Information System (INIS)

Jbeli, H.

1988-10-01

Three actualisation reports are shown, in the three first chapters, concerning the following subjects: x fluorescence principle, energy dispersive X ray spectroscopy and excitation spectrum characteristics. The matrice effects, the energy equivalence concept, and the correction methods of the interelement effects, related to a calibration curve, are discussed. For the last ones, it is shown that they are supplied to rough values. Quantitative analysis results are shown. A new possibility has been added to those of data processing program usually applied in quantitative analysis. In the second method applied in quantitative analysis, standard samples are used. In both methods an error appreciation analysis is carried out. It is shown that energy dispersive X fluorescence analysis can be applied to thin layers composition and thickness characterization [fr

Insight into the structure of Pd/ZrO2 during the total oxidation of methane using combined in situ XRD, X.-ray absorption and Raman spectroscopy

DEFF Research Database (Denmark)

Grunwaldt, Jan-Dierk; van Vegten, Niels; Baiker, Alfons

2009-01-01

The structure of palladium during the total combustion of methane has been studied by a combination of the complementary in situ techniques X-ray absorption spectroscopy, Raman spectroscopy and X-ray diffraction. The study demonstrates that finely dispersed and oxidized palladium is most active f...

Thermoelectrically cooled semiconductor detectors for non-destructive analysis of works of art by means of energy dispersive X-ray fluorescence

CERN Document Server

Cesareo, R; Castellano, A

1999-01-01

Thermoelectrically cooled semiconductor detectors, such as Si-PIN, Si-drift, Cd sub 1 sub - sub x Zn sub x Te and HgI sub 2 , coupled to miniaturized low-power X-ray tubes, are well suited in portable systems for energy-dispersive X-ray fluorescence (EDXRF), analysis of archaeological samples. The Si-PIN detector is characterized by a thickness of about 300 mu m, an area of about 2x3 mm sup 2 , an energy resolution of about 200-250 eV at 5.9 keV and an entrance window of 25-75 mu m. The Si-drift detector has approximately the same area and thickness, but an energy resolution of 155 eV at 5.9 keV. The efficiency of these detectors is around 100% from 4 to 10 keV, and then decreases versus energy, reaching approx 9% at 30 keV. Coupled to a miniaturized 10 kV, 0.1 mA, Ca-anode or to a miniaturized 30 kV, 0.1 mA, W-anode X-ray tubes, portable systems can be constructed, which are able to analyse K-lines of elements up to about silver, and L-lines of heavy elements. The Cd sub 1 sub - sub x Zn sub x Te detector ha...

Illicit drug detection using energy dispersive x-ray diffraction

Science.gov (United States)

Cook, E. J.; Griffiths, J. A.; Koutalonis, M.; Gent, C.; Pani, S.; Horrocks, J. A.; George, L.; Hardwick, S.; Speller, R.

2009-05-01

Illicit drugs are imported into countries in myriad ways, including via the postal system and courier services. An automated system is required to detect drugs in parcels for which X-ray diffraction is a suitable technique as it is non-destructive, material specific and uses X-rays of sufficiently high energy to penetrate parcels containing a range of attenuating materials. A database has been constructed containing the measured powder diffraction profiles of several thousand materials likely to be found in parcels. These include drugs, cutting agents, packaging and other innocuous materials. A software model has been developed using these data to predict the diffraction profiles which would be obtained by X-ray diffraction systems with a range of suggested detector (high purity germanium, CZT and scintillation), source and collimation options. The aim of the model was to identify the most promising system geometries, which was done with the aid of multivariate analysis (MVA). The most promising systems were constructed and tested. The diffraction profiles of a range of materials have been measured and used to both validate the model and to identify the presence of drugs in sample packages.

Threat detection of liquid explosives and precursors from their x-ray scattering pattern using energy dispersive detector technology

DEFF Research Database (Denmark)

Kehres, Jan; Olsen, Ulrik Lund; Lyksborg, Mark

2017-01-01

Energy dispersive X-ray diffraction (EDXRD) can be applied for identification of liquid threats in luggage scanning in security applications. To define the instrumental design, the framework for data reduction and analysis and test the performance of the threat detection in various scenarios....... Initial testing of the threat detection algorithms with this data set indicate the feasibility of detection levels of > 95 % true positive with

Quantitative analysis of the sediments from the Solimoes/Amazonas river flood plain using energy dispersive x-ray fluorescence technique

International Nuclear Information System (INIS)

Carneiro, Ana E.V.

1995-01-01

A methodology for quantitative analysis of geological, biological and environmental samples with a high fraction of light elements (atomic number less than 13), using energy dispersive X-ray fluorescence technique with radioisotopic excitation, is proposed. The proposed procedure is based on the method of Fundamental Parameters for analytical elements (≥->13 evaluation, and coherent and incoherent scattered radiation for the quantitation of the light fraction of the matrix. In the order to obtain the characteristic X-ray of the elements in the Mn to Zr range a Cd-109 annular radioactive source (1,70 GBq) was used, and for Al to CR, Fe-55 (o,74 GBq). For the X-ray detection a Si (Li) detector coupled to a multichannel emulation card was employed. The characteristic X-ray net intensity as well as the coherent and incoherent scattered intensities were obtained by using the AXL software for spectrum analysis. (author). 89 refs., 37 figs., 32 tabs

Studies of x-ray localization and thickness dependence in atomic-scale elemental mapping by STEM energy-dispersive x-ray spectroscopy using single-frame scanning method.

Science.gov (United States)

Lu, Ping; Moya, Jaime M; Yuan, Renliang; Zuo, Jian Min

2018-03-01

The delocalization of x-ray signals limits the spatial resolution in atomic-scale elemental mapping by scanning transmission electron microscopy (STEM) using energy-dispersive x-ray spectroscopy (EDS). In this study, using a SrTiO 3 [001] single crystal, we show that the x-ray localization to atomic columns is strongly dependent on crystal thickness, and a thin crystal is critical for improving the spatial resolution in atomic-scale EDS mapping. A single-frame scanning technique is used in this study instead of the multiple-frame technique to avoid peak broadening due to tracking error. The strong thickness dependence is realized by measuring the full width at half maxima (FWHM) as well as the peak-to-valley (P/V) ratio of the EDS profiles for Ti K and Sr K + L, obtained at several crystal thicknesses. A FWHM of about 0.16 nm and a P/V ratio of greater than 7.0 are obtained for Ti K for a crystal thickness of less than 20 nm. With increasing crystal thickness, the FWHM and P/V ratio increases and decreases, respectively, indicating the advantage of using a thin crystal for high-resolution EDS mapping. Published by Elsevier B.V.

Calcium detection in secretion granules of avian oviduct by scanning electron microscopy (SEM) and energy-dispersive X-ray microanalysis (EDX)

International Nuclear Information System (INIS)

Makita, T.; Hatsuoka, M.; Sugi, Y.

1983-01-01

Secretion granules in the shell gland, isthmus, and albumin-secreting region of the hen oviduct were analyzed with WET-scanning electron microscopy (SEM) and EDX, a combination of wide-angle backscattered electron detector (BED) and energy-dispersive X-ray microanalyzer (EDX). Glutaraldehyde-fixed but unhydrated, unstained, and uncoated samples were analyzed; Ca was localized in all secretion granules in all three sections of the hen oviduct studied

Energy dispersive soft X-ray fluorescence analysis by radioisotopic α-particle excitation

International Nuclear Information System (INIS)

Robertson, R.

1977-01-01

A Si(Li) X-ray detector system and 210 Po α-particle excitation source are combined to form a spectrometer for low energy X-rays. Its response in terms of Ksub(α) X-ray rate is shown for thick targets of elements from fluorine to copper. Potential applications of the equipment to useful quantitative elemental analysis of geological, biological and organic materials are explored. The results of analyses for oxygen and silicon in rocks and potassium in vegetation samples are included. A semi-empirical method of correcting for absorption and enhancement effects is employed. This is based upon X-ray production and photon absorption cross-sections taken from the literature and upon a minimal number of experimentally derived coefficients. (Auth.)

Application of a portable equipment EDXRF (energy dispersive X-ray fluorescence) in the monitoring of the restoration work of murals paints in the Church of Paroquia Imaculada Conceicao (Sao Paulo, SP); Aplicacao de um equipamento portatil de EDXRF (fluorescencia de raios X por dispersao em energia) no acompanhamento dos trabalhos de restauro de pinturas murais na igreja da Paroquia Imaculada Conceicao (Sao Paulo, SP)

Energy Technology Data Exchange (ETDEWEB)

Appoloni, Carlos Roberto; Parreira, Paulo Sergio, E-mail: appoloni@uel.b, E-mail: parreira@uel.b [Universidade Estadual de Londrina (UEL), PR (Brazil); Rizzo, Marcia [MRizzo Restauracoes - Laboratorio de Conservacao e Restauracao de Bens Culturais Ltda., Sao Paulo, SP (Brazil)

2006-07-01

This paper presents the application of the portable EDXRF (energy dispersive X-ray fluorescence) of the Laboratorio de Fisica Nuclear Aplicada of the Universidade Estadual de Londrina in the analysis in situ of pigments in wall paintings, as well as in monitoring restoration processes

Structure investigation of metal ions clustering in dehydrated gel using x-ray anomalous dispersion effect

CERN Document Server

Soejima, Y; Sugiyama, M; Annaka, M; Nakamura, A; Hiramatsu, N; Hara, K

2003-01-01

The structure of copper ion clusters in dehydrated N-isopropylacrylamide/sodium acrylate (NIPA/SA) gel has been studied by means of small angle X-ray scattering (SAXS) method. In order to distinguish the intensity scattered by Cu ions, the X-ray anomalous dispersion effect around the Cu K absorption edge has been coupled with SAXS. It is found that the dispersion effect dependent on the incident X-ray energy is remarkable only at the momentum transfer q = 0.031 A sup - sup 1 , where a SAXS peak is observed. The results indicate that copper ions form clusters in the dehydrated gel, and that the mean size of clusters is the same as that of SA clusters produced by microphase separation. It is therefore naturally presumed that copper ions are adsorbed into the SA molecules. On the basis of the presumption, a mechanism is proposed for microphase-separation and clustering of Cu ions.

Application of radionuclide sources for excitation in energy-dispersive X-ray fluorescence analysis

International Nuclear Information System (INIS)

Hoffmann, P.

1986-01-01

X-ray fluorescence (XRF) analysis is in broad application in many fields of science where elemental determinations are necessary. Solid and liquid samples are analyzed by this method. Solids are introduced in thin or thick samples as melted glass, pellets, powders or as original specimen. The excitation of X-ray spectra can be performed by specific and polychromic radiation of X-ray tubes, by protons, deuterons, α-particles, heavy ions and synchrotron radiation from accelerators and by α-particles, X- and γ-rays and by bremsstrahlung generated by β - -particles from radionuclide sources. The radionuclides are devided into groups with respect to their decay mode and the energy of the emitted radiation. The broad application of radionuclides in XRF excitation is shown in examples as semi-quantitative analysis of glasses, as quantitative analysis of coarse ceramics and as quantitative determination of heavy elements (mainly actinides) in solutions. The advantages and disadvantages of radionuclide excitation in XRF analysis are discussed. (orig.) [de

Non-matrix corrected organic sulfur determination by energy dispersive X-ray spectroscopy for western Kentucky coals and residues

International Nuclear Information System (INIS)

Clark, C.P.; Freeman, G.B.; Hower, J.C.

1984-01-01

A method for non-matrix corrected organic sulfur analysis by energy dispersive X-ray spectroscopy has been developed using petroleum coke standards. Typically, electron beam microanalysis is a rapid, nondestructive analytical technique to quantitatively measure organic sulfur in coal. The results show good correlation to ASTM values for numerous well characterized coals with a wide range in total and pyritic sulfur content. This direct analysis is capable of reducing error commonly associated with the present ASTM method which relies on an indirect measure of organic sulfur by difference. The precision of the organic sulfur values determined in the present study is comparable to that obtained by ZAF matrix corrected microanalysis. The energy dispersive microanalysis is capable of measuring micro as well as bulk organic sulfur levels

The application of a microstrip gas counter to energy-dispersive x-ray fluorescence analysis

International Nuclear Information System (INIS)

Veloso, J.F.C.A.; Santos, J.M.F. dos; Conde, C.A.N.

1996-01-01

Performance characteristics of a microstrip gas counter operated as a x-ray fluorescence spectrometer are reported. Gas amplification as a function of microstrip anode-cathode voltage was measured, and the breakdown threshold voltage was determined in pure xenon. The detector temporal stability and the effect of gas purity were assessed. Energy resolution and linearity, detection efficiency, and uniformity of spatial response in the 2- to 60-keV x-ray energy range were determined from the pulse-height distributions of the fluorescence x-ray spectra induced in a variety of single- and multi-element sample materials. Energy resolution similar to conventional proportional counters was achieved at 6 keV

Nondestructive, energy-dispersive x-ray fluorescence analysis of product-stream concentrations from reprocessed LWR fuels

International Nuclear Information System (INIS)

Camp, D.C.; Ruhter, W.D.; Benjamin, S.

1979-01-01

Energy-dispersive x-ray fluorescence analysis can be used for quantitative on-line monitoring of the product concentrations in single- or dual-element process streams in a reprocessing plant. The 122-keV gamma ray from 57 Co is used to excite the K x-rays of uranium and/or plutonium in nitric acid solution streams. A collimated HPGe detector is used to measure the excited x-ray intensities. Net solution radioactivity may be measured by eclipsing the exciting radiation, or by measuring it simultaneously with a second detector. The technique is nondestructive and noninvasive, and is easily adapted directly to pipes containing the solution of interest. The dynamic range of the technique extends from below 1 to 500 g/l. Measurement times depend on concentration, but better than 1% counting statistics can be obtained in 100 s for 400 g/l concentrations, and in 1000 s for as little as 10 g/l. Calibration accuracies of 0.3% or better over the entire dynamic range can be achieved easily using carefully prepared standards. Computer-based analysis equipment allows concentration changes in flowing streams to be dynamically monitored. Changes in acid normality of the stream will affect the concentration determined, hence it must also be determined by measuring the intensity of a transmitted 57 Co beam. The computer/disk-based pulse-height analysis system allows all necessary calculations to be done on-line. Experimental requirements for an in-plant installation or a test and evaluation are discussed

Analysis of stainless steel samples by energy dispersive X-ray ...

Indian Academy of Sciences (India)

Unknown

the total sample mass absorption coefficients for X-ray energies E0, Ej and ... from published literature (McMaster et al 1969; Bam- bynek et al 1972). .... Table 1. Concentrations of CRM samples determined by EDXRF and VES. Concentrations ...

Energy-dispersive X-ray fluorescence analysis of organic-rich soils and sediments

International Nuclear Information System (INIS)

Parekh, P.P.

1981-01-01

A method has been developed for elemental analysis of environmental samples of soils and sediments rich in organic matter by energy-dispersive X-ray fluorescence spectrometry. It consists of three steps (i) determining the apparent concentration of elements by using calibration coefficients based on geochemical standards, (ii) subsequent assay of the total organic matter (TOM) from loss on ignition at 550 deg C, and (iii) evaluating the correct elemental concentration by normalizing for transparency from an empirical relationship. The main feature of the method is the sample analysis prior to ignition, which avoids any loss of trace elements - especially the volatile toxic elements, such as Zn, As, Se, and Pb - during heating. The method was tested on two organic-rich lake sediments (TOM> 30%). Concentrations of five elements (K, Mn, Fe, Zn, and Pb) determined by the present method and by atomic absorption spectrometry agreed within about +-10%. (author)

In Vitro assessment of dentin erosion after immersion in acidic beverages: surface profile analysis and energy-dispersive X-ray fluorescence spectrometry study

OpenAIRE

Caneppele, Taciana Marco Ferraz; Jeronymo, Raffaela Di Iorio; Di Nicoló, Rebeca; Araújo, Maria Amélia Máximo de; Soares, Luís Eduardo Silva

2012-01-01

The aim of this study was to investigate the effects of some acidic drinks on dentin erosion, using methods of surface profile (SP) analysis and energy-dispersive X-ray fluorescence spectrometry (EDXRF). One hundred standardized dentin slabs obtained from bovine incisor roots were used. Dentin slabs measuring 5x5 mm were ground flat, polished and half of each specimen surface was protected with nail polish. For 60 min, the dentin surfaces were immersed in 50 mL of 5 different drinks (Gatorade...

Energy dispersive X-ray fluorescence spectroscopy/Monte Carlo simulation approach for the non-destructive analysis of corrosion patina-bearing alloys in archaeological bronzes: The case of the bowl from the Fareleira 3 site (Vidigueira, South Portugal)

Energy Technology Data Exchange (ETDEWEB)

Bottaini, C. [Hercules Laboratory, University of Évora, Palacio do Vimioso, Largo Marquês de Marialva 8, 7000-809 Évora (Portugal); Mirão, J. [Hercules Laboratory, University of Évora, Palacio do Vimioso, Largo Marquês de Marialva 8, 7000-809 Évora (Portugal); Évora Geophysics Centre, Rua Romão Ramalho 59, 7000 Évora (Portugal); Figuereido, M. [Archaeologist — Monte da Capelinha, Apartado 54, 7005, São Miguel de Machede, Évora (Portugal); Candeias, A. [Hercules Laboratory, University of Évora, Palacio do Vimioso, Largo Marquês de Marialva 8, 7000-809 Évora (Portugal); Évora Chemistry Centre, Rua Romão Ramalho 59, 7000 Évora (Portugal); Brunetti, A. [Department of Political Science and Communication, University of Sassari, Via Piandanna 2, 07100 Sassari (Italy); Schiavon, N., E-mail: schiavon@uevora.pt [Hercules Laboratory, University of Évora, Palacio do Vimioso, Largo Marquês de Marialva 8, 7000-809 Évora (Portugal); Évora Geophysics Centre, Rua Romão Ramalho 59, 7000 Évora (Portugal)

2015-01-01

Energy dispersive X-ray fluorescence (EDXRF) is a well-known technique for non-destructive and in situ analysis of archaeological artifacts both in terms of the qualitative and quantitative elemental composition because of its rapidity and non-destructiveness. In this study EDXRF and realistic Monte Carlo simulation using the X-ray Monte Carlo (XRMC) code package have been combined to characterize a Cu-based bowl from the Iron Age burial from Fareleira 3 (Southern Portugal). The artifact displays a multilayered structure made up of three distinct layers: a) alloy substrate; b) green oxidized corrosion patina; and c) brownish carbonate soil-derived crust. To assess the reliability of Monte Carlo simulation in reproducing the composition of the bulk metal of the objects without recurring to potentially damaging patina's and crust's removal, portable EDXRF analysis was performed on cleaned and patina/crust coated areas of the artifact. Patina has been characterized by micro X-ray Diffractometry (μXRD) and Back-Scattered Scanning Electron Microscopy + Energy Dispersive Spectroscopy (BSEM + EDS). Results indicate that the EDXRF/Monte Carlo protocol is well suited when a two-layered model is considered, whereas in areas where the patina + crust surface coating is too thick, X-rays from the alloy substrate are not able to exit the sample. - Highlights: • EDXRF/Monte Carlo simulation is used to characterize an archeological alloy. • EDXRF analysis was performed on cleaned and patina coated areas of the artifact. • EDXRF/Montes Carlo protocol is well suited when a two-layered model is considered. • When the patina is too thick, X-rays from substrate are unable to exit the sample.

An Energy Dispersive X-ray Spectroscopy Analysis of Elemental Changes of a Persimmon Phytobezoar Dissolved in Coca-Cola.

Science.gov (United States)

Iwamuro, Masaya; Urata, Haruo; Higashi, Reiji; Nakagawa, Masahiro; Ishikawa, Shin; Shiraha, Hidenori; Okada, Hiroyuki

To investigate the mechanism of phytobezoar dissolution by Coca-Cola(®), persimmon phytobezoar pieces removed from a 60-year-old Japanese woman were analyzed by energy dispersive X-ray spectroscopy. The amount of calcium significantly decreased after dissolution treatment using Coca-Cola(®), suggesting a potential contribution of calcium to dissolution mechanisms. Moreover, immersion in Coca-Cola(®) for 120 hours on the exterior surface revealed that Coca-Cola(®) did not permeate persimmon phytobezoars. This is the first study to investigate the mechanisms of persimmon phytobezoar permeability and dissolution induced by Coca-Cola(®).

Spatially resolved quantification of agrochemicals on plant surfaces using energy dispersive X-ray microanalysis.

Science.gov (United States)

Hunsche, Mauricio; Noga, Georg

2009-12-01

In the present study the principle of energy dispersive X-ray microanalysis (EDX), i.e. the detection of elements based on their characteristic X-rays, was used to localise and quantify organic and inorganic pesticides on enzymatically isolated fruit cuticles. Pesticides could be discriminated from the plant surface because of their distinctive elemental composition. Findings confirm the close relation between net intensity (NI) and area covered by the active ingredient (AI area). Using wide and narrow concentration ranges of glyphosate and glufosinate, respectively, results showed that quantification of AI requires the selection of appropriate regression equations while considering NI, peak-to-background (P/B) ratio, and AI area. The use of selected internal standards (ISs) such as Ca(NO(3))(2) improved the accuracy of the quantification slightly but led to the formation of particular, non-typical microstructured deposits. The suitability of SEM-EDX as a general technique to quantify pesticides was evaluated additionally on 14 agrochemicals applied at diluted or regular concentration. Among the pesticides tested, spatial localisation and quantification of AI amount could be done for inorganic copper and sulfur as well for the organic agrochemicals glyphosate, glufosinate, bromoxynil and mancozeb. (c) 2009 Society of Chemical Industry.

Thermoelectrically cooled semiconductor detectors for non-destructive analysis of works of art by means of energy dispersive X-ray fluorescence

International Nuclear Information System (INIS)

Cesareo, Roberto; Ettore Gigante, Giovanni; Castellano, Alfredo

1999-01-01

Thermoelectrically cooled semiconductor detectors, such as Si-PIN, Si-drift, Cd 1-x Zn x Te and HgI 2 , coupled to miniaturized low-power X-ray tubes, are well suited in portable systems for energy-dispersive X-ray fluorescence (EDXRF), analysis of archaeological samples. The Si-PIN detector is characterized by a thickness of about 300 μm, an area of about 2x3 mm 2 , an energy resolution of about 200-250 eV at 5.9 keV and an entrance window of 25-75 μm. The Si-drift detector has approximately the same area and thickness, but an energy resolution of 155 eV at 5.9 keV. The efficiency of these detectors is around 100% from 4 to 10 keV, and then decreases versus energy, reaching ∼9% at 30 keV. Coupled to a miniaturized 10 kV, 0.1 mA, Ca-anode or to a miniaturized 30 kV, 0.1 mA, W-anode X-ray tubes, portable systems can be constructed, which are able to analyse K-lines of elements up to about silver, and L-lines of heavy elements. The Cd 1-x Zn x Te detector has an area of 4 mm 2 and a thickness of 3 mm. It has an energy resolution of about 300 eV at 5.9 keV, and an efficiency of 100% over the whole range of X-rays. Finally the HgI 2 detector has an efficiency of about 100% in the whole range of X-rays, and an energy resolution of about 200 eV at 5.9 keV. Coupled to a small 50-60 kV, 1 mA, W-anode X-ray tube, portable systems can be constructed, for the analysis of practically all elements. These systems were applied to analysis in the field of archaeometry and in all applications for which portable systems are needed or at least useful (for example X-ray transmission measurements, X-ray microtomography and so on). Results of in-field use of these detectors and a comparison among these room temperature detectors in relation to concrete applications are presented. More specifically, concerning EDXRF analysis, ancient gold samples were analysed in Rome, in Mexico City and in Milan, ancient bronzes in Sassari, in Bologna, in Chieti and in Naples, and sulfur (due to

Energy dispersive x-ray fluorescence spectrometric determination of phosphorus, calcium, iron, zinc, and strontium in human bones

International Nuclear Information System (INIS)

Ohta, Akishige; Matsubayashi, Takashi; Itoman, Moritoshi

1981-01-01

Phosphorus, calcium, iron, zinc and strontium in a human bone extracted by surgery were determined by energy dispersive X-ray fluorescence spectrometry. The bone was decomposed with nitric acid, then diluted with water. A specific quantity of the solution was naturally dried on polyethylene film, and subjected to X-ray analysis. For determining the calibration curves in a mixture of phosphorus, calcium, iron, zinc and strontium, for the analysis of phosphorus and calcium, germanium was used as the secondary target and aluminum as the filter; and for the analysis of iron, zinc and strontium, molybdenum and molybdenum-aluminum were used, respectively. Consequently, the calibration curves were able to be obtained with high precision in the ranges from 5 to 500 μg of phosphorus, from 1 to 50 μg of calcium and from 0.1 to 1.0 μg of iron, zinc and strontium. In this way, in 1 mg of the human bone by wet weight, phosphorus, calcium, iron, zinc and strontium were able to be determined. (J.P.N.)

High-energy synchrotron X-ray radiography of shock-compressed materials

Science.gov (United States)

Rutherford, Michael E.; Chapman, David J.; Collinson, Mark A.; Jones, David R.; Music, Jasmina; Stafford, Samuel J. P.; Tear, Gareth R.; White, Thomas G.; Winters, John B. R.; Drakopoulos, Michael; Eakins, Daniel E.

2015-06-01

This presentation will discuss the development and application of a high-energy (50 to 250 keV) synchrotron X-ray imaging method to study shock-compressed, high-Z samples at Beamline I12 at the Diamond Light Source synchrotron (Rutherford-Appleton Laboratory, UK). Shock waves are driven into materials using a portable, single-stage gas gun designed by the Institute of Shock Physics. Following plate impact, material deformation is probed in-situ by white-beam X-ray radiography and complimentary velocimetry diagnostics. The high energies, large beam size (13 x 13 mm), and appreciable sample volumes (~ 1 cm3) viable for study at Beamline I12 compliment existing in-house pulsed X-ray capabilities and studies at the Dynamic Compression Sector. The authors gratefully acknowledge the ongoing support of Imperial College London, EPSRC, STFC and the Diamond Light Source, and AWE Plc.

The dispersion surface of X-rays very near the absorption edge

International Nuclear Information System (INIS)

Fukamachi, T.; Negishi, R.; Kawamura, T.

1995-01-01

To discuss the X-ray dynamical diffraction when the imaginary part of the X-ray polarizability is larger than the real part, the dispersion surface is studied as a function of the ratio between the real and the imaginary parts of the polarizability. The dispersion surface in the Laue case when the real part is zero has a similar form to that in the Bragg case when the imaginary part is zero. The relations between the dispersion surface and the diffracted intensity are studied in some special cases. The abnormal absorption and the abnormal transmission effect are related to the features of the dispersion surface. (orig.)

Electrochemical cell for in situ x-ray diffraction under ultrapure conditions

DEFF Research Database (Denmark)

Koop, T.; Schindler, W.; Kazimirov, A.

1998-01-01

within a few seconds. The oxygen level in the electrolyte is reduced by continuous N(2) flow to less than 0.2% compared to that of a fresh electrolyte. This can be done while rotating the cell by 360 degrees about the surface normal. The electrode potential is accurately measured at the position......An electrochemical cell has been developed for in situ x-ray diffraction from a working electrode under clean conditions equivalent to ultrahigh vacuum conditions of 5 x 10(-10) mbar. The substrate crystals can be prepared ex situ and transferred into the cell under protection of ultrapure water...... of the crystal using a Luggin capillary and a standard reference electrode. We demonstrate the performance of our cell by in situ synchrotron x-ray diffraction measurements on ultrathin Co layers electrodeposited on Cu(001) in an aqueous H(2)SO(4)/CoSO(4) solution. (C) 1998 American Institute of Physics....

In-situ oxidation study of Pd(100) by surface x-ray diffraction

Energy Technology Data Exchange (ETDEWEB)

Kilic, Volkan; Franz, Dirk; Stierle, Andreas [AG Grenzflaechen, Universitaet Siegen (Germany); Martin, Natalia; Lundgren, Edvin [Department of Synchrotron Radiation Research, Lund University (Sweden); Mantilla, Miguel [MPI fuer Metallforschung, Stuttgart (Germany)

2011-07-01

The oxidation of the Pd(100) surface at oxygen pressures in the 10{sup -6} mbar to 10{sup 3} mbar range and temperatures up to 1000 K has been studied in-situ by surface x-ray diffraction (SXRD). The SXRD experiments were performed at the MPI beamline at the Angstrom Quelle Karlsruhe (ANKA). We present the surface and crystal truncation rod (CTR) data from the ({radical}(5) x {radical}(5)) surface layer. We show that the transformation from the surface oxide to PdO bulk oxide can be observed in-situ under specific pressure and temperature conditions. We compare our results with previously proposed structure models based on low energy electron diffraction (LEED) I(V) curves and density functional theory calculations. Finally, we elucidate the question of commensurability of the surface oxide layer with respect to the Pd(100) substrate.

An attempt to reduce radioactivity for energy-dispersive x-ray analysis

International Nuclear Information System (INIS)

Hamada, S.

1992-01-01

The object of this work is to develop a specimen preparation technique which reduces the intensity of radioactivity of a neutron-irradiated materials for microchemical analysis by analytical electron microscope (AEM) with energy dispersive X-ray spectroscopy (EDXS). A composite specimen preparation technique for the AEM was developed using unirradiated materials. The technique reduced the mass of material from a dummy irradiated specimen by more than a factor of 100. A 1-mm diam. disk was punched from a dummy irradiated 3-mm diam. transmission electron microscope (TEM) disk. The 1-mm disk was then pressed into a hole previously punched at the center of a second 3 mm diam. disk creating a composite disk. The composite disk was electropolished using a twin jet Tenupol until the thickness of the center of the composite was about 100 μm. Approximately 100 μm of nickel plating was then deposited on the surface of the thinned composite. Standard electropolishing by Tenupol unit was performed on the nickel-plated composite specimen and the composite specimen was examined by TEM

The application of energy-dispersive x-ray fluorescence spectrometry (EDXRF) to the analysis of cosmetic evidence in Indian nail polishes

International Nuclear Information System (INIS)

Misra, G.; Sawhney, K.J.S.; Lodha, G.S.; Mittal, V.K.; Sahota, H.S.

1992-01-01

The application of energy-dispersive x-ray fluorescence (EDXRF) spectrometry in the quantitative analysis of samples of Indian nail polishes of apparently similar shades from different manufacturers has been examined by evaluating the possibility of detecting spurious material which is marketed under the guise of a popular brand. On the basis of the number of elements detected, and from the ratios of particular elements [Fe/Ti,Fe/Cu,Ti/Cu] the results are very encouraging. (author)

The application of energy-dispersive x-ray fluorescence spectrometry (EDXRF) to the analysis of cosmetic evidence in Indian nail polishes

Energy Technology Data Exchange (ETDEWEB)

Misra, G. (Forensic Science Lab., Chandigarh (India)); Sawhney, K.J.S.; Lodha, G.S. (Nuclear Research Lab., Srinagar (India)); Mittal, V.K.; Sahota, H.S. (Punjabi Univ., Patiala (India). Dept. of Physics)

1992-05-01

The application of energy-dispersive x-ray fluorescence (EDXRF) spectrometry in the quantitative analysis of samples of Indian nail polishes of apparently similar shades from different manufacturers has been examined by evaluating the possibility of detecting spurious material which is marketed under the guise of a popular brand. On the basis of the number of elements detected, and from the ratios of particular elements (Fe/Ti,Fe/Cu,Ti/Cu) the results are very encouraging. (author).

Application of neutron activation techniques and x-ray energy dispersion spectrometry, in analysis of metallic traces adsorbed by chelex-100 resin

International Nuclear Information System (INIS)

Fernandes, Jair C.; Amaral, Angela M.; Magalhaes, Jesus C.; Pereira, Jose S.J.; Silva, Juliana B. da; Auler, Lucia M.L.A.

2000-01-01

In this work, the authors have investigated optimal conditions of adsorption for several ion metallic groups (cations of heavy metals and transition metals, oxyanions metallics and metalloids and cations of rare earths), as traces (ppb), withdrawn and in mixture of groups, by chelex-100 resin. The experiments have been developed by bath techniques in ammonium acetate tamponade solution 40 mM pH 5,52 content 0,5 g of chelex-100 resin. After magnetic agitation for two hours, resins were dried and submitted to X-ray energy dispersion spectrometry, x-ray fluorescence spectrometry and neutron activation analysis. The results have demonstrated that chelex-100 resin adsorb quantitatively transition element groups and rare earth groups in two cases (withdrawn and simultaneously adsorption)

Forensic applications of scanning electron microscopy/energy dispersive X-ray analyser in Hong Kong.

Science.gov (United States)

Wong, Y S

1982-01-01

Scanning Electron Microscopy - Energy Dispersive X-Ray Analysis (SEM/EDX) has been applied in casework for more than a year in the Forensic Division, Government Laboratory of Hong Kong. The types of samples being analysed are summarised and three cases of scientific interest are described. The first case applies SEM/EDX to characterize microscopic gold particles recovered from clothing of suspects involved in goldsmith robberies. Both elemental and morphological results obtained were used as supporting evidence. The second case describes the three types of beaded ends on fibres found in a single cloth sample. These beaded ends are different in shape and surface features and can be used as an additional parameter in fibre identification. The final case shows the application of vacuum evaporation of graphite on a document sample to reveal the area of paper which has been skillfully mechanically erased. Both the image intensity and the composition of the ink are used to differentiate between original and altered characters on the document.

The Characterisation of Settled Dust by Scanning Electron Microscopy and Energy Dispersive X-ray Analysis

International Nuclear Information System (INIS)

Shilton, Vaughan; Giess, Paul; Mitchell, David; Williams, Craig

2002-01-01

Settled dust has been collected inside the main foyers oft hree University buildings in Wolverhampton City Centre,U.K. Two of the three buildings are located in a street canyon used almost exclusively by heavy duty diesel vehicles. The dust was collected on adhesive carbonspectro-tabs to be in a form suitable for analysis by scanning electron microscope and energy dispersive X-ray analysis. Using these analytical techniques, individual particle analysis was undertaken for morphology and chemistry. Seasonal variations and variations due to location were observed in both the morphological measurements and chemical analysis. Many of the differences appear attributable to the influence of road traffic, in particular, the heavy duty diesel vehicles, travelling along the street canyon

Energy-dispersive X-ray fluorescence of discarded tire samples, using a Si-PIN detector

International Nuclear Information System (INIS)

Lopes, Fabio; Appoloni, C.R.; Melquiades, Fabio L.

2007-01-01

The determination of zinc concentration in samples of discarded tires is of great environmental interest because the process for manufacturing tyres uses S for rubber vulcanization, and ZnO is the reaction catalyst. Discarded tyres are being used in asphalt paving, in the burning process of thermoelectric and cement industries and also for controlling erosion in agricultural areas. Analysis of tyre samples usually requires chemical digestion which is slow and expensive. Aiming to eliminate those limitations, this work uses energy-dispersive X-ray fluorescence (EDXRF) with a portable equipment, once it is a simultaneous multi-element analytical technique, requiring minimal sample preparation. Five samples of discarded tyres have been ground and analysed in the form of pastilles, using a mini X-ray tube (Ag target, MO filter, 25 kV/20 μA) for 200 s, and a Si-PIN semiconductor detector coupled to a multichannel analyser. Zinc concentrations in the range of 40.6 to 44.2 μg g -1 have been obtained, representing 0.4% of the tire composition, which is below the maximum value (2%) recommended by the European Tyre Recycling Association. Concentrations between 0.15 and 0.52 μg g -1 were obtained for Fe

In situ grazing incidence small-angle X-ray scattering investigation of polystyrene nanoparticle spray deposition onto silicon.

Science.gov (United States)

Herzog, Gerd; Benecke, Gunthard; Buffet, Adeline; Heidmann, Berit; Perlich, Jan; Risch, Johannes F H; Santoro, Gonzalo; Schwartzkopf, Matthias; Yu, Shun; Wurth, Wilfried; Roth, Stephan V

2013-09-10

We investigated the spray deposition and subsequent self-assembly during drying of a polystyrene nanoparticle dispersion with in situ grazing incidence small-angle X-ray scattering at high time resolution. During the fast deposition of the dispersion and the subsequent evaporation of the solvent, different transient stages of nanoparticle assembly can be identified. In the first stage, the solvent starts to evaporate without ordering of the nanoparticles. During the second stage, large-scale structures imposed by the breakup of the liquid film are observable. In this stage, the solvent evaporates further and nanoparticle ordering starts. In the late third drying stage, the nanoparticles self-assemble into the final layer structure.

Speckle-based portable device for in-situ metrology of x-ray mirrors at Diamond Light Source

Science.gov (United States)

Wang, Hongchang; Kashyap, Yogesh; Zhou, Tunhe; Sawhney, Kawal

2017-09-01

For modern synchrotron light sources, the push toward diffraction-limited and coherence-preserved beams demands accurate metrology on X-ray optics. Moreover, it is important to perform in-situ characterization and optimization of X-ray mirrors since their ultimate performance is critically dependent on the working conditions. Therefore, it is highly desirable to develop a portable metrology device, which can be easily implemented on a range of beamlines for in-situ metrology. An X-ray speckle-based portable device for in-situ metrology of synchrotron X-ray mirrors has been developed at Diamond Light Source. Ultra-high angular sensitivity is achieved by scanning the speckle generator in the X-ray beam. In addition to the compact setup and ease of implementation, a user-friendly graphical user interface has been developed to ensure that characterization and alignment of X-ray mirrors is simple and fast. The functionality and feasibility of this device is presented with representative examples.

Rigorous quantitative elemental microanalysis by scanning electron microscopy/energy dispersive x-ray spectrometry (SEM/EDS) with spectrum processing by NIST DTSA-II

Science.gov (United States)

Newbury, Dale E.; Ritchie, Nicholas W. M.

2014-09-01

Quantitative electron-excited x-ray microanalysis by scanning electron microscopy/silicon drift detector energy dispersive x-ray spectrometry (SEM/SDD-EDS) is capable of achieving high accuracy and high precision equivalent to that of the high spectral resolution wavelength dispersive x-ray spectrometer even when severe peak interference occurs. The throughput of the SDD-EDS enables high count spectra to be measured that are stable in calibration and resolution (peak shape) across the full deadtime range. With this high spectral stability, multiple linear least squares peak fitting is successful for separating overlapping peaks and spectral background. Careful specimen preparation is necessary to remove topography on unknowns and standards. The standards-based matrix correction procedure embedded in the NIST DTSA-II software engine returns quantitative results supported by a complete error budget, including estimates of the uncertainties from measurement statistics and from the physical basis of the matrix corrections. NIST DTSA-II is available free for Java-platforms at: http://www.cstl.nist.gov/div837/837.02/epq/dtsa2/index.html).

A new method for polychromatic X-ray μLaue diffraction on a Cu pillar using an energy-dispersive pn-junction charge-coupled device

Energy Technology Data Exchange (ETDEWEB)

Abboud, A.; Send, S.; Pashniak, N.; Pietsch, U. [Department of Physics, University of Siegen, Siegen 57072 (Germany); Kirchlechner, C. [Max-Planck-Institut für Eisenforschung GmbH, Düsseldorf 40237 (Germany); Montanuniversität Leoben, Leoben 8700 (Austria); Micha, J. S.; Ulrich, O. [CEA-Grenoble/DRFMC/SprAM, 17 rue des Martyrs, Grenoble Cedex 9, F-38054 (France); Strüder, L. [PNSensor GmbH, Munich 80803 (Germany); Keckes, J. [Montanuniversität Leoben, Leoben 8700 (Austria); Material Center Leoben Forschungs GmbH, Leoben 8700 (Austria)

2014-11-15

μLaue diffraction with a polychromatic X-ray beam can be used to measure strain fields and crystal orientations of micro crystals. The hydrostatic strain tensor can be obtained once the energy profile of the reflections is measured. However, this remains a challenge both on the time scale and reproducibility of the beam position on the sample. In this review, we present a new approach to obtain the spatial and energy profiles of Laue spots by using a pn-junction charge-coupled device, an energy-dispersive area detector providing 3D resolution of incident X-rays. The morphology and energetic structure of various Bragg peaks from a single crystalline Cu micro-cantilever used as a test system were simultaneously acquired. The method facilitates the determination of the Laue spots’ energy spectra without filtering the white X-ray beam. The synchrotron experiment was performed at the BM32 beamline of ESRF using polychromatic X-rays in the energy range between 5 and 25 keV and a beam size of 0.5 μm × 0.5 μm. The feasibility test on the well known system demonstrates the capabilities of the approach and introduces the “3D detector method” as a promising tool for material investigations to separate bending and strain for technical materials.

Energy dispersive X-ray analysis in the electron microscope

CERN Document Server

Bell, DC

2003-01-01

This book provides an in-depth description of x-ray microanalysis in the electron microscope. It is sufficiently detailed to ensure that novices will understand the nuances of high-quality EDX analysis. Includes information about hardware design as well as the physics of x-ray generation, absorption and detection, and most post-detection data processing. Details on electron optics and electron probe formation allow the novice to make sensible adjustments to the electron microscope in order to set up a system which optimises analysis. It also helps the reader determine which microanalytical me

Preliminary results on air pollution inside an iron metallurgical plant, using rotating streaker sampler and energy dispersive X-ray microfluorescence

International Nuclear Information System (INIS)

Nascimento Filho, V.F.; Silva, R.M.C.; Perez, C.A.

2005-01-01

Our aim was to study the chemical concentration of some metals in suspended particulate matter inside an-iron metallurgical plant. Using a rotating streaker air-particulate sampler with 8 and 0.45 microns pore diameter filter, it was possible to collect coarse and fine particulates during a week, with one hour step. After this, each strip of the filter was analyzed by energy dispersive x-ray microfluorescence (μ-EDXRF), using in the excitation a collimated x-ray line beam from a Mo target tube (30 kV, 20 mA, Zr filter) with a quartz capillary (120 mm long, 10 mm entrance diameter and 20 microns inner diameter at exit). The detection was carried out using a Si(Li) semiconductor detector coupled to a multichannel analyzer, and the X-ray spectra were fitted with the AXIL software. The profiles of several elements are shown and the results are discussed.

Energy Dispersive X-Ray Fluorescent Analysis of Soil in the Vicinity of Industrial Areas and Heavy Metal Pollution Assessment

Science.gov (United States)

Singh, V.; Joshi, G. C.; Bisht, D.

2017-05-01

The soil of two agricultural sites near an industrial area was investigated for heavy metal pollution using energy dispersive X-ray fluorescence (EDXRF). The concentration values for 17 elements were determined in the soil samples including eight heavy metal elements, i.e., Fe, Ni, As, Pb, Mn, Cr, Cu, and Zn. The soil near a pulp and paper mill was found to be highly polluted by the heavy metals. The concentration data obtained by EDXRF were further examined by calculating the pollution index and Nemerow integrated pollution index.

Diagnostic Spectrometers for High Energy Density X-Ray Sources

International Nuclear Information System (INIS)

Hudson, L. T.; Henins, A.; Seely, J. F.; Holland, G. E.

2007-01-01

A new generation of advanced laser, accelerator, and plasma confinement devices are emerging that are producing extreme states of light and matter that are unprecedented for laboratory study. Examples of such sources that will produce laboratory x-ray emissions with unprecedented characteristics include megajoule-class and ultrafast, ultraintense petawatt laser-produced plasmas; tabletop high-harmonic-generation x-ray sources; high-brightness zeta-pinch and magnetically confined plasma sources; and coherent x-ray free electron lasers and compact inverse-Compton x-ray sources. Characterizing the spectra, time structure, and intensity of x rays emitted by these and other novel sources is critical to assessing system performance and progress as well as pursuing the new and unpredictable physical interactions of interest to basic and applied high-energy-density (HED) science. As these technologies mature, increased emphasis will need to be placed on advanced diagnostic instrumentation and metrology, standard reference data, absolute calibrations and traceability of results.We are actively designing, fabricating, and fielding wavelength-calibrated x-ray spectrometers that have been employed to register spectra from a variety of exotic x-ray sources (electron beam ion trap, electron cyclotron resonance ion source, terawatt pulsed-power-driven accelerator, laser-produced plasmas). These instruments employ a variety of curved-crystal optics, detector technologies, and data acquisition strategies. In anticipation of the trends mentioned above, this paper will focus primarily on optical designs that can accommodate the high background signals produced in HED experiments while also registering their high-energy spectral emissions. In particular, we review the results of recent laboratory testing that explores off-Rowland circle imaging in an effort to reclaim the instrumental resolving power that is increasingly elusive at higher energies when using wavelength-dispersive

Determination of heavy metals at traces level in leached samples by energy dispersive x-ray fluorescence technique

International Nuclear Information System (INIS)

Simabuco, Silvana M.; Nascimento Filho, Virgilio F. do; Inacio, Graziela R.; Navarro, Angela N.

1996-01-01

In landfill solid residues are disposed in the soil. When made based on technical criteria and specifically operation patterns a safe confinement is warranted according to environmental and public health protection. However, when the disposal is made by a random and unsuitable way serious problems can be caused as groundwater and superficial water contamination through leach action, indicating the usefulness of monitoring landfills. In this way energy dispersive X-ray fluorescence analysis with radioisotopic excitation was applied to evaluate the concentrations of heavy metals at trace levels in leached samples from the Americana City Landfill with pre-concentration of the elements by a non-specific precipitating agent, called ammonium pyrrolidine dithiocarbamate (APDC). (author)

A flexible gas flow reaction cell for in situ x-ray absorption spectroscopy studies

Energy Technology Data Exchange (ETDEWEB)

Kroner, Anna B., E-mail: anna.kroner@diamond.ac.uk; Gilbert, Martin; Duller, Graham; Cahill, Leo; Leicester, Peter; Woolliscroft, Richard; Shotton, Elizabeth J. [Diamond Light Source Ltd., Diamond House, Harwell Science and Innovation Campus, Chilton, Oxfordshire, OX110DE (United Kingdom); Mohammed, Khaled M. H. [UK Catalysis Hub, Research Complex at Harwell, Rutherford Appleton Laboratory, Chilton, Oxfordshire, OX110FA (United Kingdom); School of Chemistry, University of Southampton, Southampton, SO17 1BJ (United Kingdom)

2016-07-27

A capillary-based sample environment with hot air blower and integrated gas system was developed at Diamond to conduct X-ray absorption spectroscopy (XAS) studies of materials under time-resolved, in situ conditions. The use of a hot air blower, operating in the temperature range of 298-1173 K, allows introduction of other techniques e.g. X-ray diffraction (XRD), Raman spectroscopy for combined techniques studies. The flexibility to use either quartz or Kapton capillaries allows users to perform XAS measurement at energies as low as 5600 eV. To demonstrate performance, time-resolved, in situ XAS results of Rh catalysts during the process of activation (Rh K-edge, Ce L{sub 3}-edge and Cr K-edge) and the study of mixed oxide membrane (La{sub 0.6}Sr{sub 0.4}Co{sub 0.2}Fe{sub 0.8}O{sub 3−δ}) under various partial oxygen pressure conditions are described.

Determination of the Effective Detector Area of an Energy-Dispersive X-Ray Spectrometer at the Scanning Electron Microscope Using Experimental and Theoretical X-Ray Emission Yields.

Science.gov (United States)

Procop, Mathias; Hodoroaba, Vasile-Dan; Terborg, Ralf; Berger, Dirk

2016-12-01

A method is proposed to determine the effective detector area for energy-dispersive X-ray spectrometers (EDS). Nowadays, detectors are available for a wide range of nominal areas ranging from 10 up to 150 mm2. However, it remains in most cases unknown whether this nominal area coincides with the "net active sensor area" that should be given according to the related standard ISO 15632, or with any other area of the detector device. Moreover, the specific geometry of EDS installation may further reduce a given detector area. The proposed method can be applied to most scanning electron microscope/EDS configurations. The basic idea consists in a comparison of the measured count rate with the count rate resulting from known X-ray yields of copper, titanium, or silicon. The method was successfully tested on three detectors with known effective area and applied further to seven spectrometers from different manufacturers. In most cases the method gave an effective area smaller than the area given in the detector description.

Scanning electron microscopy and X-ray energy dispersive spectroscopy - useful tools in the analysis of pharmaceutical products

Science.gov (United States)

Sarecka-Hujar, Beata; Balwierz, Radoslaw; Ostrozka-Cieslik, Aneta; Dyja, Renata; Lukowiec, Dariusz; Jankowski, Andrzej

2017-11-01

The quality of the drug, its purity and identification of degradation products provide the highest quality of pharmaceutical products. The energy dispersive spectroscopy (EDS) method analyses the percentage of each element form as well as their distribution, and morphological characteristics of the drug form. We analysed the usefulness of EDS method in testing orally disintegrating tablets (ODT) with trimetazidine hydrochloride with high resolution scanning electron microscopy (SEM, SUPRA25 Carl Zeiss company) with spectrophotometer equipped with an X-ray energy dispersion (EDAX Company). The samples of the analysed tablets were imaged after applying conductive layers of gold on their surface. In the EDS analysis the compositions of each sample of the obtained tablets were observed to be virtually identical. The differences in the content of carbon and oxygen came from differences in the composition of particular tablets. The presence of gold in the composition resulted from the sputtering the surface of tablets with gold during the analysis. Knowing the composition of the tablet, SEM-EDS method helps to locate and identify the impurities and degradation products of the compounds, leading to a better understanding of the mechanisms of their formation.

High temperature monitoring of silicon carbide ceramics by confocal energy dispersive X-ray fluorescence spectrometry

Energy Technology Data Exchange (ETDEWEB)

Li, Fangzuo; Liu, Zhiguo; Sun, Tianxi, E-mail: stx@bnu.edu.cn

2016-04-15

Highlights: • X-ray scattering was used for monitoring oxidation situation of SiC ceramics. • A calibration curve was obtained. • The confocal X-ray scattering technology was based on polycapillary X-ray optics. • The variations of contents of components of SiC ceramics were obtained. - Abstract: In the present work, we presented an alternative method for monitoring of the oxidation situation of silicon carbide (SiC) ceramics at various high temperatures in air by measuring the Compton-to-Rayleigh intensity ratios (I{sub Co}/I{sub Ra}) and effective atomic numbers (Z{sub eff}) of SiC ceramics with the confocal energy dispersive X-ray fluorescence (EDXRF) spectrometer. A calibration curve of the relationship between I{sub Co}/I{sub Ra} and Z{sub eff} was established by using a set of 8 SiC calibration samples. The sensitivity of this approach is so high that it can be easily distinguished samples of Z{sub eff} differing from each other by only 0.01. The linear relationship between the variation of Z{sub eff} and the variations of contents of C, Si and O of SiC ceramics were found, and the corresponding calculation model of the relationship between the ΔZ and the ΔC{sub C}, ΔC{sub Si}, and ΔC{sub O} were established. The variation of contents of components of the tested SiC ceramics after oxidation at high temperature was quantitatively calculated based on the model. It was shown that the results of contents of carbon, silicon and oxygen obtained by this method were in good agreement with the results obtained by XPS, giving values of relative deviation less than 1%. It was concluded that the practicality of this proposed method for monitoring of the oxidation situation of SiC ceramics at high temperatures was acceptable.

Effect of Cl2- and HBr-based inductively coupled plasma etching on InP surface composition analyzed using in situ x-ray photoelectron spectroscopy

International Nuclear Information System (INIS)

Bouchoule, S.; Vallier, L.; Patriarche, G.; Chevolleau, T.; Cardinaud, C.

2012-01-01

A Cl 2 -HBr-O 2 /Ar inductively coupled plasma (ICP) etching process has been adapted for the processing of InP-based heterostructures in a 300-mm diameter CMOS etching tool. Smooth and anisotropic InP etching is obtained at moderate etch rate (∼600 nm/min). Ex situ x-ray energy dispersive analysis of the etched sidewalls shows that the etching anisotropy is obtained through a SiO x passivation mechanism. The stoichiometry of the etched surface is analyzed in situ using angle-resolved x-ray photoelectron spectroscopy. It is observed that Cl 2 -based ICP etching results in a significantly P-rich surface. The phosphorous layer identified on the top surface is estimated to be ∼1-1.3-nm thick. On the other hand InP etching in HBr/Ar plasma results in a more stoichiometric surface. In contrast to the etched sidewalls, the etched surface is free from oxides with negligible traces of silicon. Exposure to ambient air of the samples submitted to Cl 2 -based chemistry results in the complete oxidation of the P-rich top layer. It is concluded that a post-etch treatment or a pure HBr plasma step may be necessary after Cl 2 -based ICP etching for the recovery of the InP material.

Quality in the chemical analysis of biological matrices by fluorescence X-ray by energy dispersive

International Nuclear Information System (INIS)

Sousa, Evely E. de; Paiva, Jose Daniel S. de; Franca, Elvis J. de; Almeida, Macio E.S.; Cantinha, Rebeca S.; Hazin, Clovis A.

2013-01-01

The aim of this study was to obtain multielement analytical curves of high analytical rigor to the analysis of biological matrices by the technique of fluorescence x-ray energy dispersive - EDXRF. Calibration curves were constructed from the reference materials IAEA 140, IAEA 155, IAEA V8, V10 to the International Atomic Energy Agency - IAEA, and SRM1515, SRM 1547, SRM 1570a, SRM 1573a, SEM 1567a, to the National Institute of Standards and Technology - NIST. After energy calibration, all samples were subjected to vacuum to the analyzes by 100 seconds for each group of chemical elements. The voltages used were respectively 15 keV for chemical elements with less than atomic number 22 and 50 keV for the others. After the construction of the curves, the analytical quality was assessed by the analysis of a portion-test of the reference material SRM 2976, also produced by NIST. Based on the number of certified reference materials used for construction of calibration curves in this work, quality analytical protocol was originated with considerable reliability for quantification of chemical elements in biological samples by EDXR

In situ synchrotron X-ray diffraction study on epitaxial-growth dynamics of III–V semiconductors

Science.gov (United States)

Takahasi, Masamitu

2018-05-01

The application of in situ synchrotron X-ray diffraction (XRD) to the molecular-beam epitaxial (MBE) growth of III–V semiconductors is overviewed along with backgrounds of the diffraction theory and instrumentation. X-rays are sensitive not only to the surface of growing films but also to buried interfacial structures because of their large penetration depth. Moreover, a spatial coherence length up to µm order makes X-rays widely applicable to the characterization of low-dimensional structures, such as quantum dots and wires. In situ XRD studies during growth were performed using an X-ray diffractometer, which was combined with an MBE chamber. X-ray reciprocal space mapping at a speed matching a typical growth rate was achieved using intense X-rays available from a synchrotron light source and an area detector. The importance of measuring the three-dimensional distribution of XRD intensity in a reciprocal space map is demonstrated for the MBE growth of two-, one-, and zero-dimensional structures. A large amount of information about the growth process of two-dimensional InGaAs/GaAs(001) epitaxial films has been provided by three-dimensional X-ray reciprocal mappings, including the anisotropic strain relaxation, the compositional inhomogeneity, and the evolution of surface and interfacial roughness. For one-dimensional GaAs nanowires grown in a Au-catalyzed vapor-liquid–solid mode, the relationship between the diameter of the nanowires and the formation of polytypes has been suggested on the basis of in situ XRD measurements. In situ three-dimensional X-ray reciprocal space mapping is also shown to be useful for determining the lateral and vertical sizes of self-assembled InAs/GaAs(001) quantum dots as well as their internal strain distributions during growth.

Pre-Columbian alloys from the royal tombs of Sipan; energy dispersive X-ray fluorescence analysis with a portable equipment

International Nuclear Information System (INIS)

Cesareo, R.; Calza, C.; Dos Anjos, M.; Lopes, R.T.; Bustamante, A.; Fabian S, J.; Alva, W.; Chero Z, L.

2010-01-01

On the north coast of present-day Peru flourished approximately between 50 and 700 AD, the Moche civilization. It was an advanced culture and the Moche were sophisticated metalsmiths, so that they are considered as the finest producers of jewels and artefacts of the region. The Moche metalworking ability was impressively demonstrated by the objects discovered by Walter Alva and coworkers in 1987, in the excavations of the 'Tumbas Reales de Sipan'. About 50 metal objects from these excavations, now at the namesake Museum, in Lambayeque, north of Peru, were analyzed with a portable equipment using energy-dispersive X-ray fluorescence. This portable equipment is mainly composed of a small size X-ray tube and a thermoelectrically cooled X-ray detector. Standard samples of gold and silver alloys were employed for quantitative analysis. It was determined that the analyzed artefacts from the 'Tumbas Reales de Sipan' are mainly composed of gold, silver and copper alloys, of gilded copper and of tumbaga, the last being a poor gold alloy enriched at the surface by depletion gilding, i.e. removing copper from the surface.

In Situ X-ray Diffraction Studies of (De)lithiation Mechanism in Silicon Nanowire Anodes

KAUST Repository

Misra, Sumohan; Liu, Nian; Nelson, Johanna; Hong, Seung Sae; Cui, Yi; Toney, Michael F.

2012-01-01

-Si product has been observed. In this work, we use an X-ray transparent battery cell to perform in situ synchrotron X-ray diffraction on SiNWs in real time during electrochemical cycling. At deep lithiation voltages the known metastable Li 15Si 4 phase forms

Fast Atomic-Scale Elemental Mapping of Crystalline Materials by STEM Energy-Dispersive X-Ray Spectroscopy Achieved with Thin Specimens.

Science.gov (United States)

Lu, Ping; Yuan, Renliang; Zuo, Jian Min

2017-02-01

Elemental mapping at the atomic-scale by scanning transmission electron microscopy (STEM) using energy-dispersive X-ray spectroscopy (EDS) provides a powerful real-space approach to chemical characterization of crystal structures. However, applications of this powerful technique have been limited by inefficient X-ray emission and collection, which require long acquisition times. Recently, using a lattice-vector translation method, we have shown that rapid atomic-scale elemental mapping using STEM-EDS can be achieved. This method provides atomic-scale elemental maps averaged over crystal areas of ~few 10 nm2 with the acquisition time of ~2 s or less. Here we report the details of this method, and, in particular, investigate the experimental conditions necessary for achieving it. It shows, that in addition to usual conditions required for atomic-scale imaging, a thin specimen is essential for the technique to be successful. Phenomenological modeling shows that the localization of X-ray signals to atomic columns is a key reason. The effect of specimen thickness on the signal delocalization is studied by multislice image simulations. The results show that the X-ray localization can be achieved by choosing a thin specimen, and the thickness of less than about 22 nm is preferred for SrTiO3 in [001] projection for 200 keV electrons.

In situ surface/interface x-ray diffractometer for oxide molecular beam epitaxy

Energy Technology Data Exchange (ETDEWEB)

Lee, J. H.; Freeland, J. W.; Hong, Hawoong, E-mail: hhong@aps.anl.gov [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Tung, I. C. [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Department of Materials Science and Engineering, Northwestern University, Evanston, Illinois 60208 (United States); Chang, S.-H.; Bhattacharya, A.; Fong, D. D. [Materials Science Division, Argonne National Laboratory, Argonne, Illinois 60439 (United States)

2016-01-15

In situ studies of oxide molecular beam epitaxy by synchrotron x-ray scattering has been made possible by upgrading an existing UHV/molecular beam epitaxy (MBE) six-circle diffractometer system. For oxide MBE growth, pure ozone delivery to the chamber has been made available, and several new deposition sources have been made available on a new 12 in. CF (ConFlat, a registered trademark of Varian, Inc.) flange. X-ray diffraction has been used as a major probe for film growth and structures for the system. In the original design, electron diffraction was intended for the secondary diagnostics available without the necessity of the x-ray and located at separate positions. Deposition of films was made possible at the two diagnostic positions. And, the aiming of the evaporation sources is fixed to the point between two locations. Ozone can be supplied through two separate nozzles for each location. Also two separate thickness monitors are installed. Additional features of the equipment are also presented together with the data taken during typical oxide film growth to illustrate the depth of information available via in situ x-ray techniques.

In situ surface/interface x-ray diffractometer for oxide molecular beam epitaxy

International Nuclear Information System (INIS)

Lee, J. H.; Freeland, J. W.; Hong, Hawoong; Tung, I. C.; Chang, S.-H.; Bhattacharya, A.; Fong, D. D.

2016-01-01

In situ studies of oxide molecular beam epitaxy by synchrotron x-ray scattering has been made possible by upgrading an existing UHV/molecular beam epitaxy (MBE) six-circle diffractometer system. For oxide MBE growth, pure ozone delivery to the chamber has been made available, and several new deposition sources have been made available on a new 12 in. CF (ConFlat, a registered trademark of Varian, Inc.) flange. X-ray diffraction has been used as a major probe for film growth and structures for the system. In the original design, electron diffraction was intended for the secondary diagnostics available without the necessity of the x-ray and located at separate positions. Deposition of films was made possible at the two diagnostic positions. And, the aiming of the evaporation sources is fixed to the point between two locations. Ozone can be supplied through two separate nozzles for each location. Also two separate thickness monitors are installed. Additional features of the equipment are also presented together with the data taken during typical oxide film growth to illustrate the depth of information available via in situ x-ray techniques

Determination of trace metals in sea waters of the albanian coast by energy-dispersive x-ray fluorescence

International Nuclear Information System (INIS)

Civici, N.

1994-01-01

Preconcentration of trace transition and heavy metal ions by precipitation with APDC has been combined with energy-dispersive X-ray fluorescence for environmental sea water analysis. The preconcentration procedure implies adding of 500 μg Mo ion and 10 ml of 1 % water solution of APDC to a 500 ml water sample at pH 4, filtering off on a Millipore filter and analyzing after drying. Realistic detection limits are at 1 μg * l -1 level and precision varies between 10 - 25% at about 5 μg * l -1 level, depending on the element. Eleven sea water samples, covering Albanian Adriatic and Ionian coast, are analyzed for trace metal ions. (author) 8 refs.; 2 figs.; 5 tabs

Liquid contrabands classification based on energy dispersive X-ray diffraction and hybrid discriminant analysis

International Nuclear Information System (INIS)

YangDai, Tianyi; Zhang, Li

2016-01-01

Energy dispersive X-ray diffraction (EDXRD) combined with hybrid discriminant analysis (HDA) has been utilized for classifying the liquid materials for the first time. The XRD spectra of 37 kinds of liquid contrabands and daily supplies were obtained using an EDXRD test bed facility. The unique spectra of different samples reveal XRD's capability to distinguish liquid contrabands from daily supplies. In order to create a system to detect liquid contrabands, the diffraction spectra were subjected to HDA which is the combination of principal components analysis (PCA) and linear discriminant analysis (LDA). Experiments based on the leave-one-out method demonstrate that HDA is a practical method with higher classification accuracy and lower noise sensitivity than the other methods in this application. The study shows the great capability and potential of the combination of XRD and HDA for liquid contrabands classification.

Liquid contrabands classification based on energy dispersive X-ray diffraction and hybrid discriminant analysis

Energy Technology Data Exchange (ETDEWEB)

YangDai, Tianyi [Department of Engineering Physics, Tsinghua University, Beijing 100084 (China); Key Laboratory of Particle & Radiation Imaging (Tsinghua University), Ministry of Education (China); Zhang, Li, E-mail: zhangli@nuctech.com [Department of Engineering Physics, Tsinghua University, Beijing 100084 (China); Key Laboratory of Particle & Radiation Imaging (Tsinghua University), Ministry of Education (China)

2016-02-01

Energy dispersive X-ray diffraction (EDXRD) combined with hybrid discriminant analysis (HDA) has been utilized for classifying the liquid materials for the first time. The XRD spectra of 37 kinds of liquid contrabands and daily supplies were obtained using an EDXRD test bed facility. The unique spectra of different samples reveal XRD's capability to distinguish liquid contrabands from daily supplies. In order to create a system to detect liquid contrabands, the diffraction spectra were subjected to HDA which is the combination of principal components analysis (PCA) and linear discriminant analysis (LDA). Experiments based on the leave-one-out method demonstrate that HDA is a practical method with higher classification accuracy and lower noise sensitivity than the other methods in this application. The study shows the great capability and potential of the combination of XRD and HDA for liquid contrabands classification.

Liquid contrabands classification based on energy dispersive X-ray diffraction and hybrid discriminant analysis

Science.gov (United States)

YangDai, Tianyi; Zhang, Li

2016-02-01

Energy dispersive X-ray diffraction (EDXRD) combined with hybrid discriminant analysis (HDA) has been utilized for classifying the liquid materials for the first time. The XRD spectra of 37 kinds of liquid contrabands and daily supplies were obtained using an EDXRD test bed facility. The unique spectra of different samples reveal XRD's capability to distinguish liquid contrabands from daily supplies. In order to create a system to detect liquid contrabands, the diffraction spectra were subjected to HDA which is the combination of principal components analysis (PCA) and linear discriminant analysis (LDA). Experiments based on the leave-one-out method demonstrate that HDA is a practical method with higher classification accuracy and lower noise sensitivity than the other methods in this application. The study shows the great capability and potential of the combination of XRD and HDA for liquid contrabands classification.

Use of semiconductors in energy-dispersive X-ray analysis

International Nuclear Information System (INIS)

Schiekel, M.

1983-01-01

The state-of-the-art of the application of semiconductor detectors with high resolution for photon radiation in energy-dispersive spectrometers is reviewed. It is concluded that the use of semiconductor detectors results in an improvement of spectrometers and thus in a wider range of application. Characteristics of the spectrometers, such as energy resolution and efficiency, are discussed and possible applications indicated. (author)

Application of low power X-ray tubes in geology

International Nuclear Information System (INIS)

Massalski, J.M.; Zaraska, W.

1981-01-01

Low power X-ray tubes with transmission anodes for X-ray fluorescence analysis with energy dispersion were elaborated. Paper contains experimental results of application of X-ray tubes in the apparatus for nondestructive measurements of the concentration of some elements in borehole cores. (author)

Single photon energy dispersive x-ray diffraction

International Nuclear Information System (INIS)

Higginbotham, Andrew; Patel, Shamim; Ciricosta, Orlando; Suggit, Matthew J.; Wark, Justin S.; Hawreliak, James A.; Collins, Gilbert W.; Coppari, Federica; Eggert, Jon H.; Tang, Henry

2014-01-01

With the pressure range accessible to laser driven compression experiments on solid material rising rapidly, new challenges in the diagnosis of samples in harsh laser environments are emerging. When driving to TPa pressures (conditions highly relevant to planetary interiors), traditional x-ray diffraction techniques are plagued by increased sources of background and noise, as well as a potential reduction in signal. In this paper we present a new diffraction diagnostic designed to record x-ray diffraction in low signal-to-noise environments. By utilising single photon counting techniques we demonstrate the ability to record diffraction patterns on nanosecond timescales, and subsequently separate, photon-by-photon, signal from background. In doing this, we mitigate many of the issues surrounding the use of high intensity lasers to drive samples to extremes of pressure, allowing for structural information to be obtained in a regime which is currently largely unexplored

Single photon energy dispersive x-ray diffraction

Energy Technology Data Exchange (ETDEWEB)

Higginbotham, Andrew; Patel, Shamim; Ciricosta, Orlando; Suggit, Matthew J.; Wark, Justin S. [Department of Physics, Clarendon Laboratory, University of Oxford, Parks Road, Oxford OX1 3PU (United Kingdom); Hawreliak, James A.; Collins, Gilbert W.; Coppari, Federica; Eggert, Jon H. [Lawrence Livermore National Laboratory, Livermore, California 94551 (United States); Tang, Henry [Department of Earth and Planetary Science, University of California Berkeley, Berkeley, California 94720 (United States)

2014-03-15

With the pressure range accessible to laser driven compression experiments on solid material rising rapidly, new challenges in the diagnosis of samples in harsh laser environments are emerging. When driving to TPa pressures (conditions highly relevant to planetary interiors), traditional x-ray diffraction techniques are plagued by increased sources of background and noise, as well as a potential reduction in signal. In this paper we present a new diffraction diagnostic designed to record x-ray diffraction in low signal-to-noise environments. By utilising single photon counting techniques we demonstrate the ability to record diffraction patterns on nanosecond timescales, and subsequently separate, photon-by-photon, signal from background. In doing this, we mitigate many of the issues surrounding the use of high intensity lasers to drive samples to extremes of pressure, allowing for structural information to be obtained in a regime which is currently largely unexplored.

In situ measurements of X-ray peak profile asymmetry from individual grains

DEFF Research Database (Denmark)

Wejdemann, Christian; Lienert, U.; Pantleon, Wolfgang

2010-01-01

Two copper samples, pre-deformed in tension to 5% plastic strain, are subjected to an in situ tensile deformation of 1% plastic strain while X-ray peak profiles from individual bulk grains are obtained. One sample is oriented with the in situ tensile axis parallel to the pre-deformation axis...

Charged particle induced energy dispersive X-ray analysis

International Nuclear Information System (INIS)

Johansson, S.A.E.

1979-01-01

This review article deals with the X-ray emission induced by heavy, charged particles and the use of this process as an analytical method (PIXE). The physical processes involved, X-ray emission and the various reactions contributing to the background, are described in some detail. The sensitivity is calculated theoretically and the results compared with practical experience. A discussion is given on how the sensitivity can be optimized. The experimental arrangements are described and the various technical problems discussed. The analytical procedure, especially the sample preparation, is described in considerable detail. A number of typical practical applications are discussed. (author)

Electron-probe microanalysis: x-ray spectroscopy

International Nuclear Information System (INIS)

1987-01-01

The main principles on X-ray, energy and wave length dispersive spectroscopy are reviewed. In order to allow the choice of the best operating conditions, the importance of the regulation and control systems is underlined. Emission theory, X-rays nature and its interaction with matter and electrons in the matter is shown. The structure, operating procedures and necessary electronics (single channel - analysis chain) automatic-control system for the threshold-energies discrimination and the energy distribution visualization) associated to the wavelength dispersive spectroscopy are described. The focusing control, resolution, influence of chemical bonds and multilayer-structure monochromators relaled to wavelength dispersive spectroscopy are studied. Concerning the energy-dispersive spectroscopy, the detector, preamplifier, amplifier, analog-digital converter, as well as the utilization and control of the spectrometer are described. Problems and instrumental progress on energy-dispersive spectroscopy related to the electronic-noise control, charge collection and light-elements detection are discussed [fr

X-ray scattering in X-ray fluorescence spectra with X-ray tube excitation - Modelling, experiment, and Monte-Carlo simulation

International Nuclear Information System (INIS)

Hodoroaba, V.-D.; Radtke, M.; Vincze, L.; Rackwitz, V.; Reuter, D.

2010-01-01

X-ray scattering may contribute significantly to the spectral background of X-ray fluorescence (XRF) spectra. Based on metrological measurements carried out with a scanning electron microscope (SEM) having attached a well characterised X-ray source (polychromatic X-ray tube) and a calibrated energy dispersive X-ray spectrometer (EDS) the accuracy of a physical model for X-ray scattering is systematically evaluated for representative samples. The knowledge of the X-ray spectrometer efficiency, but also of the spectrometer response functions makes it possible to define a physical spectral background of XRF spectra. Background subtraction relying on purely mathematical procedures is state-of-the-art. The results produced by the analytical model are at least as reliable as those obtained by Monte-Carlo simulations, even without considering the very challenging contribution of multiple scattering. Special attention has been paid to Compton broadening. Relevant applications of the implementation of the analytical model presented in this paper are the prediction of the limits of detection for particular cases or the determination of the transmission of X-ray polycapillary lenses.

Characterization of sediments laid on Solimoes/Amazonas river flood plains, using energy dispersive X-ray fluorescence technique

International Nuclear Information System (INIS)

Carneiro, Ana E.V.; Nascimento Filho, Virgilio F. do

1997-01-01

This paper proposes sediment analysis with high light elements fraction using dispersive energy X-ray fluorescence technique with radioisotopic excitation, The proposed procedure is based on the Fundamental Parameters for analytical elements (Z ≥ 13) evaluation, and coherent and incoherent scattered radiation for quantification of the light fraction of the matrix (Z < 13). Laid sediments samples on Solimoes/Amazonas river flood plains were analyzed, determining simultaneously the Al, Si, K, Ca, Ti, Fe, Sc, V, Mn, Cu, Zn, Rb, Sr and Zr element concentrations, thus allowing chemical characterization and spatial variability, and some mineralogical and weathering sediments aspects. (author). 15 refs., 11 tabs

Radiation processing with high-energy X-rays

International Nuclear Information System (INIS)

Cleland, Marshall R.; Stichelbaut, Frederic

2009-01-01

The physical, chemical or biological characteristics of selected commercial products and materials can be improved by radiation processing. The ionizing energy can be provided by accelerated electrons with energies between 75 keV and 10 MeV, gamma rays from cobalt-60 with average energies of 1.25 MeV or X-rays with maximum energies up to 7.5 MeV. Electron beams are preferred for thin products, which are processed at high speeds. Gamma rays are used for products that are too thick for treatment with electron beams. High-energy X-rays can also be used for these purposes because their penetration in solid materials is similar to or even slightly greater than that of gamma rays. Previously, the use of X-rays had been inhibited by their slower processing rates and higher costs when compared with gamma rays. Since then, the price of cobalt-60 sources has been increased and the radiation intensity from high-energy, high-power X-ray generators has also increased. For facilities requiring at least 2 MCi of cobalt-60, the capital and operating costs of X-ray facilities with equivalent processing rates can be less than that of gamma-ray irradiators. Several high-energy electron beam facilities have been equipped with removable X-ray targets so that irradiation processes can be done with either type of ionizing energy. A new facility is now being built which will be used exclusively in the X-ray mode to sterilize medical products. Operation of this facility will show that high-energy, high-power X-ray generators are practical alternatives to large gamma-ray sources. (author)

Trace elemental analysis of school chalk using energy dispersive X-ray florescence spectroscopy (ED-XRF)

International Nuclear Information System (INIS)

Maruthi, Y. A.; Das, N. Lakshmana; Ramprasad, S.; Ram, S. S.; Sudarshan, M.

2015-01-01

The present studies focus the quantitative analysis of elements in school chalk to ensure the safety of its use. The elements like Calcium (Ca), Aluminum (Al), Iron (Fe), Silicon (Si) and Chromium (Cr) were analyzed from settled chalk dust samples collected from five classrooms (CD-1) and also from another set of unused chalk samples collected from local market (CD-2) using Energy Dispersive X-Ray florescence(ED-XRF) spectroscopy. Presence of these elements in significant concentrations in school chalk confirmed that, it is an irritant and occupational hazard. It is suggested to use protective equipments like filtered mask for mouth, nose and chalk holders. This study also suggested using the advanced mode of techniques like Digital boards, marker boards and power point presentations to mitigate the occupational hazard for classroom chalk

Trace elemental analysis of school chalk using energy dispersive X-ray florescence spectroscopy (ED-XRF)

Energy Technology Data Exchange (ETDEWEB)

Maruthi, Y. A., E-mail: ymjournal2014@gmail.com [Associate professor, Dept of Environmental Studies, GITAM Institute of Science, GITAM University, Visakhapatnam, A.P (India); Das, N. Lakshmana, E-mail: nldas9@gmail.com [Professor, Dept of Physics, GITAM Institute of Science, GITAM University, Visakhapatnam, A.P (India); Ramprasad, S., E-mail: ramprasadsurakala@gmail.com [Research Scholar, Dept of Environmental science, GITAM Institute of Science, GITAM University, Visakhapatnam, A.P (India); Ram, S. S., E-mail: tracebio@gmail.com [Research Scholar, Dept of Trace element research, UGC-DAE Consortium Centre, Kolkata centre India (India); Sudarshan, M., E-mail: sude@alpha.iuc.res.in [Scientist-F, Dept of Trace element research, UGC-DAE Consortium Centre, Kolkata centre India (India)

2015-08-28

The present studies focus the quantitative analysis of elements in school chalk to ensure the safety of its use. The elements like Calcium (Ca), Aluminum (Al), Iron (Fe), Silicon (Si) and Chromium (Cr) were analyzed from settled chalk dust samples collected from five classrooms (CD-1) and also from another set of unused chalk samples collected from local market (CD-2) using Energy Dispersive X-Ray florescence(ED-XRF) spectroscopy. Presence of these elements in significant concentrations in school chalk confirmed that, it is an irritant and occupational hazard. It is suggested to use protective equipments like filtered mask for mouth, nose and chalk holders. This study also suggested using the advanced mode of techniques like Digital boards, marker boards and power point presentations to mitigate the occupational hazard for classroom chalk.

A critical evaluation of quantitative and qualitative analysis by means of energy-dispersive X-ray measurement in a scanning electron microscope

International Nuclear Information System (INIS)

Blum, F.

1978-12-01

The bombardment of solids in the scanning electron microscope (SEM) by means of energetic electrons results in the generation and emission of various signals that carry information about the characteristics of the target. Those signals which are related to the present context, e.g. the secondary and backscattered electrons as well as the characteristic and continuous X-radiation, are discussed. The brief description of the SEM and the energy dispersive X-ray (EDX) spectrometer is followed by a discussion of various obstacles affecting the reliability of X-ray intensity measurements and data reduction procedures. The observed relative X-ray intensities from pure elements were determined as a function of the atomic number. These functional dependence curves, which were established under standard conditions, served as reliable reference data for the purpose of quantitative corrections. The performance limits of a typical SEM-EDX analytical system were assessed by analysing quantitatively various types of standard reference materials and inhomogeneous samples. A brief discussion of the X-ray source is given in order to estimate whether the recorded X-ray intensities are representative of the electron bombarded areas. This is of importance when microanalyses are performed on inclusions or near phase boundaries. The use of oxide glasses which are suitable to evaluate and interrelative SEM-EDX systems is discussed. The analysis of metal alloys, which developed exaggerated surface topography when sputtered in an ion microprobe mass analyser or glow discharge lamp, is presented as a typical example for the investigation of rough-surface samples [af

Sodium Chloride Diffusion during Muscle Salting Evidenced by Energy-Dispersive X-ray Spectroscopy Imaging.

Science.gov (United States)

Filgueras, Rénata; Peyrin, Frédéric; Vénien, Annie; Hénot, Jean Marc; Astruc, Thierry

2016-01-27

To better understand the relationship between the muscle structure and NaCl transfers in meat, we used energy-dispersive X-ray spectroscopy (EDS) coupled with scanning electron microscopy (SEM) to analyze brined and dry-salted rat muscles. The muscles were freeze-dried to avoid the delocalization of soluble ions that happens in regular dehydration through a graded series of ethanol. Na and Cl maps were superimposed on SEM images to combine the muscle structure and NaCl diffusion. Brining causes rapid diffusion of NaCl through the tissue. Most brine diffuses in a linear front from the muscle surface, but a small proportion enters through the perimysium network. The muscle area penetrated by brine shows heterogeneous patterns of NaCl retention, with some connective tissue islets containing more NaCl than other parts of perimysium. NaCl penetration is considerably slower after dry salting than after brining.

Sample sizing of biological materials analyzed by energy dispersion X-ray fluorescence

International Nuclear Information System (INIS)

Paiva, Jose D.S.; Franca, Elvis J.; Magalhaes, Marcelo R.L.; Almeida, Marcio E.S.; Hazin, Clovis A.

2013-01-01

Analytical portions used in chemical analyses are usually less than 1g. Errors resulting from the sampling are barely evaluated, since this type of study is a time-consuming procedure, with high costs for the chemical analysis of large number of samples. The energy dispersion X-ray fluorescence - EDXRF is a non-destructive and fast analytical technique with the possibility of determining several chemical elements. Therefore, the aim of this study was to provide information on the minimum analytical portion for quantification of chemical elements in biological matrices using EDXRF. Three species were sampled in mangroves from the Pernambuco, Brazil. Tree leaves were washed with distilled water, oven-dried at 60 deg C and milled until 0.5 mm particle size. Ten test-portions of approximately 500 mg for each species were transferred to vials sealed with polypropylene film. The quality of the analytical procedure was evaluated from the reference materials IAEA V10 Hay Powder, SRM 2976 Apple Leaves. After energy calibration, all samples were analyzed under vacuum for 100 seconds for each group of chemical elements. The voltage used was 15 kV and 50 kV for chemical elements of atomic number lower than 22 and the others, respectively. For the best analytical conditions, EDXRF was capable of estimating the sample size uncertainty for further determination of chemical elements in leaves. (author)

Sample sizing of biological materials analyzed by energy dispersion X-ray fluorescence

Energy Technology Data Exchange (ETDEWEB)

Paiva, Jose D.S.; Franca, Elvis J.; Magalhaes, Marcelo R.L.; Almeida, Marcio E.S.; Hazin, Clovis A., E-mail: dan-paiva@hotmail.com, E-mail: ejfranca@cnen.gov.br, E-mail: marcelo_rlm@hotmail.com, E-mail: maensoal@yahoo.com.br, E-mail: chazin@cnen.gov.b [Centro Regional de Ciencias Nucleares do Nordeste (CRCN-NE/CNEN-PE), Recife, PE (Brazil)

2013-07-01

Analytical portions used in chemical analyses are usually less than 1g. Errors resulting from the sampling are barely evaluated, since this type of study is a time-consuming procedure, with high costs for the chemical analysis of large number of samples. The energy dispersion X-ray fluorescence - EDXRF is a non-destructive and fast analytical technique with the possibility of determining several chemical elements. Therefore, the aim of this study was to provide information on the minimum analytical portion for quantification of chemical elements in biological matrices using EDXRF. Three species were sampled in mangroves from the Pernambuco, Brazil. Tree leaves were washed with distilled water, oven-dried at 60 deg C and milled until 0.5 mm particle size. Ten test-portions of approximately 500 mg for each species were transferred to vials sealed with polypropylene film. The quality of the analytical procedure was evaluated from the reference materials IAEA V10 Hay Powder, SRM 2976 Apple Leaves. After energy calibration, all samples were analyzed under vacuum for 100 seconds for each group of chemical elements. The voltage used was 15 kV and 50 kV for chemical elements of atomic number lower than 22 and the others, respectively. For the best analytical conditions, EDXRF was capable of estimating the sample size uncertainty for further determination of chemical elements in leaves. (author)

Pre-Columbian alloys from the royal tombs of Sipan; energy dispersive X-ray fluorescence analysis with a portable equipment

Energy Technology Data Exchange (ETDEWEB)

Cesareo, R. [Dip. di Matematica e Fisica, Universita di Sassari, via Vienna 2, 07100, Sassari (Italy)], E-mail: cesareo@uniss.it; Calza, C.; Dos Anjos, M.; Lopes, R.T. [Nuclear Instrumentation Laboratory, COPPE, Universidade Federal do Rio de Janeiro (Brazil); Bustamante, A.; Fabian S, J. [Universidad Nacional Mayor de San Marcos, Lima (Peru); Alva, W.; Chero Z, L. [Museo ' Tumbas Reales de Sipan' , Lambayeque (Peru)

2010-04-15

On the north coast of present-day Peru flourished approximately between 50 and 700 AD, the Moche civilization. It was an advanced culture and the Moche were sophisticated metalsmiths, so that they are considered as the finest producers of jewels and artefacts of the region. The Moche metalworking ability was impressively demonstrated by the objects discovered by Walter Alva and coworkers in 1987, in the excavations of the 'Tumbas Reales de Sipan'. About 50 metal objects from these excavations, now at the namesake Museum, in Lambayeque, north of Peru, were analyzed with a portable equipment using energy-dispersive X-ray fluorescence. This portable equipment is mainly composed of a small size X-ray tube and a thermoelectrically cooled X-ray detector. Standard samples of gold and silver alloys were employed for quantitative analysis. It was determined that the analyzed artefacts from the 'Tumbas Reales de Sipan' are mainly composed of gold, silver and copper alloys, of gilded copper and of tumbaga, the last being a poor gold alloy enriched at the surface by depletion gilding, i.e. removing copper from the surface.

Dibenzylammonium and sodium dibenzyldithiocarbamates as precipitants for preconcentration of trace elements in water for analysis by energy dispersive X-ray fluorescence

International Nuclear Information System (INIS)

Moore, R.V.

1982-01-01

Precipitation with combined dibenzylammonium dibenzyldithiocarbamate and sodium dibenzyldithiocarbamate at pH 5.0 can be used to separate 22 trace elements from water. Membrane filtration of the precipitate yielded a thin sample, suitable for analysis by energy dispersive X-ray fluorescence spectrometry. Alkalis, alkaline earths, lanthanides, and halides were not precipitated, permitting a clean separation of trace elements from the macro constituents of drinking water and drinking water supplies. Methods are given for preparation of reagents of higher purity than previously described

Some considerations on X-ray fluorescence use in museum measurements - The case of medieval silver coins

International Nuclear Information System (INIS)

Constantinescu, B.; Bugoi, R.; Oberlaender-Tarnoveanu, E.; Parvan, K.

2005-01-01

The purpose of this paper is to give a general layout for the potential applications of Energy-Dispersive X-Ray Fluorescence (ED-XRF) technique for ancient silver coin characterization, using in-situ (in museums) measurements. Examples concerning originality testing, provenance (mines, workshops) identification, counterfeits selection, historical studies (manufacturing technologies, commercial, military and political relationships) are given. Two study cases of medieval coins are described: German brakteaten pfennige and Moldavian groschen. Other analysis methods and their use in the study of medieval coins are illustrated with the example of Particle Induced X-ray Emission (PIXE) technique. (authors)

Handbook of X-Ray Data

CERN Document Server

Zschornack, Günter

2007-01-01

This sourcebook is intended as an X-ray data reference for scientists and engineers working in the field of energy or wavelength dispersive X-ray spectrometry and related fields of basic and applied research, technology, or process and quality controlling. In a concise and informative manner, the most important data connected with the emission of characteristic X-ray lines are tabulated for all elements up to Z = 95 (Americium). This includes X-ray energies, emission rates and widths as well as level characteristics such as binding energies, fluorescence yields, level widths and absorption edges. The tabulated data are characterized and, in most cases, evaluated. Furthermore, all important processes and phenomena connected with the production, emission and detection of characteristic X-rays are discussed. This reference book addresses all researchers and practitioners working with X-ray radiation and fills a gap in the available literature.

A portable X-ray diffraction apparatus for in situ analyses of masters' paintings

Science.gov (United States)

Eveno, Myriam; Duran, Adrian; Castaing, Jacques

2010-09-01

It is rare that the analyses of materials in paintings can be carried out by taking micro-samples. Valuable works of art are best studied in situ by non-invasive techniques. For that purpose, a portable X-ray diffraction and fluorescence apparatus has been designed and constructed at the C2RMF. This apparatus has been used for paintings of Rembrandt, Leonardo da Vinci, Van Gogh, Mantegna, etc. Results are given to illustrate the performance of X-ray diffraction, especially when X-ray fluorescence does not bring sufficient information to conclude.

A portable X-ray diffraction apparatus for in situ analyses of masters' paintings

International Nuclear Information System (INIS)

Eveno, Myriam; Duran, Adrian; Castaing, Jacques

2010-01-01

It is rare that the analyses of materials in paintings can be carried out by taking micro-samples. Valuable works of art are best studied in situ by non-invasive techniques. For that purpose, a portable X-ray diffraction and fluorescence apparatus has been designed and constructed at the C2RMF. This apparatus has been used for paintings of Rembrandt, Leonardo da Vinci, Van Gogh, Mantegna, etc. Results are given to illustrate the performance of X-ray diffraction, especially when X-ray fluorescence does not bring sufficient information to conclude. (orig.)

The (CuGaSe{sub 2}){sub 1-x}(MgSe){sub x} alloy system (0{<=}x{<=}0.5): X-ray diffraction, energy dispersive spectrometry and differential thermal analysis

Energy Technology Data Exchange (ETDEWEB)

Grima Gallardo, P.; Munoz, M.; Ruiz, J. [Centro de Estudios en Semiconductores (C.E.S.), Dpto. Fisica, Fac. Ciencias, La Hechicera, Merida (Venezuela); Delgado, G.E. [Laboratorio de Cristalografia, Dpto. Quimica, Fac. Ciencias, Universidad de Los Andes, Merida 5101 (Venezuela); Briceno, J.M. [Laboratorio de Analisis Quimico y Estructural (LAQUEM), Dpto. Fisica, Fac. Ciencias, La Hechicera, Merida (Venezuela)

2004-07-01

The (CuGaSe{sub 2}){sub 1-x}(MgSe){sub x} alloy system (0<x{<=}0.5) was investigated using X-ray powder diffraction, energy dispersion spectrometry and differential thermal analysis. The solubility of MgSe in CuGaSe{sub 2} was found to be nearly complete for all the compositions studied, although traces of MgSe appear as a secondary phase at x{>=}0.15. All the alloys showed the chalcopyrite structure and the lattice parameters of the unit cell do not follow a linear behavior but showed a soft local maximum at x {proportional_to} 0.15. In the single-phase field, the increasing behavior of the lattice parameters can be reproduced using an extension for quaternary alloys of Jaffe and Zunger's model for chalcopyrites. (copyright 2004 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

Superiority of Low Energy 160 KV X-Rays Compared to High Energy 6 MV X-Rays in Heavy Element Radiosensitization for Cancer Treatment

Science.gov (United States)

Lim, Sara N.; Pradhan, Anil K.; Nahar, Sultana N.; Barth, Rolf F.; Yang, Weilian; Nakkula, Robin J.; Palmer, Alycia; Turro, Claudia

2013-06-01

High energy X-rays in the MeV range are generally employed in conventional radiation therapy from linear accelerators (LINAC) to ensure sufficient penetration depths. However, lower energy X-rays in the keV range may be more effective when coupled with heavy element (high-Z or HZ) radiosensitizers. Numerical simulations of X-ray energy deposition for tumor phantoms sensitized with HZ radiosensitizers were performed using the Monte Carlo code Geant4. The results showed enhancement in energy deposition to radiosensitized phantoms relative to unsensitized phantoms for low energy X-rays in the keV range. In contrast, minimal enhancement was seen using high energy X-rays in the MeV range. Dose enhancement factors (DEFs) were computed and showed radiosensitization only in the low energy range nitrate, was initially used because it was 7x less toxic that an equivalent amount of carboplatin in vitro studies. This would allow us to separate the radiotoxic and the chemotoxic effects of HZ sensitizers. Results from this study showed a 10-fold dose dependent reduction in surviving fractions (SF) of radiosensitized cells treated with low energy 160 kV X-rays compared to those treated with 6 MV X-rays. This is in agreement with our simulations that show an increase in dose deposition in radiosensitized tumors for low energy X-rays. Due to unforeen in vivo toxicity, however, another in vitro study was performed using the commonly used, Pt-based chemotherapeutic drug carboplatin which confirmed earlier results. This lays the ground work for a planned in vivo study using F98 glioma bearing rats. This study demonstrates that while high energy X-rays are commonly used in cancer radiotherapy, low energy keV X-rays might be much more effective with HZ radiosensitization.

The effect of water on the stability of iron oxide and iron carbide nanoparticles in hydrogen and syngas followed by in situ X-ray absorption spectroscopy

NARCIS (Netherlands)

Thuene, P.C.; Moodley - Gengan, P.; Scheijen, F.J.E.; Fredriksson, H.O.A.; Lancee, R.J.; Kropf, J.; Miller, J.T.; Niemantsverdriet, J.W.

2012-01-01

The effect of water on iron-based nanoparticles under hydrogen and syngas was investigated by in situ X-ray absorption spectroscopy. The iron oxide (¿-Fe2O3) nanoparticles, dispersed as a monolayer on flat silica surfaces, were readily converted into metallic iron in dry hydrogen at 350 °C and into

Quantitative atomic resolution elemental mapping via absolute-scale energy dispersive X-ray spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Chen, Z. [School of Physics and Astronomy, Monash University, Clayton, Victoria 3800 (Australia); Weyland, M. [Monash Centre for Electron Microscopy, Monash University, Clayton, Victoria 3800 (Australia); Department of Materials Science and Engineering, Monash University, Clayton, Victoria 3800 (Australia); Sang, X.; Xu, W.; Dycus, J.H.; LeBeau, J.M. [Department of Materials Science and Engineering, North Carolina State University, Raleigh, NC 27695 (United States); D' Alfonso, A.J.; Allen, L.J. [School of Physics, University of Melbourne, Parkville, Victoria 3010 (Australia); Findlay, S.D., E-mail: scott.findlay@monash.edu [School of Physics and Astronomy, Monash University, Clayton, Victoria 3800 (Australia)

2016-09-15

Quantitative agreement on an absolute scale is demonstrated between experiment and simulation for two-dimensional, atomic-resolution elemental mapping via energy dispersive X-ray spectroscopy. This requires all experimental parameters to be carefully characterized. The agreement is good, but some discrepancies remain. The most likely contributing factors are identified and discussed. Previous predictions that increasing the probe forming aperture helps to suppress the channelling enhancement in the average signal are confirmed experimentally. It is emphasized that simple column-by-column analysis requires a choice of sample thickness that compromises between being thick enough to yield a good signal-to-noise ratio while being thin enough that the overwhelming majority of the EDX signal derives from the column on which the probe is placed, despite strong electron scattering effects. - Highlights: • Absolute scale quantification of 2D atomic-resolution EDX maps is demonstrated. • Factors contributing to remaining small quantitative discrepancies are identified. • Experiment confirms large probe-forming apertures suppress channelling enhancement. • The thickness range suitable for reliable column-by-column analysis is discussed.

In-situ X-ray diffraction system using sources and detectors at fixed angular positions

Science.gov (United States)

Gibson, David M [Voorheesville, NY; Gibson, Walter M [Voorheesville, NY; Huang, Huapeng [Latham, NY

2007-06-26

An x-ray diffraction technique for measuring a known characteristic of a sample of a material in an in-situ state. The technique includes using an x-ray source for emitting substantially divergent x-ray radiation--with a collimating optic disposed with respect to the fixed source for producing a substantially parallel beam of x-ray radiation by receiving and redirecting the divergent paths of the divergent x-ray radiation. A first x-ray detector collects radiation diffracted from the sample; wherein the source and detector are fixed, during operation thereof, in position relative to each other and in at least one dimension relative to the sample according to a-priori knowledge about the known characteristic of the sample. A second x-ray detector may be fixed relative to the first x-ray detector according to the a-priori knowledge about the known characteristic of the sample, especially in a phase monitoring embodiment of the present invention.

High Resolution, Non-Dispersive X-Ray Calorimeter Spectrometers on EBITs and Orbiting Observatories

Science.gov (United States)

Porter, Frederick S.

2010-01-01

X-ray spectroscopy is the primary tool for performing atomic physics with Electron beam ion trap (EBITs). X-ray instruments have generally fallen into two general categories, 1) dispersive instruments with very high spectral resolving powers but limited spectral range, limited count rates, and require an entrance slit, generally, for EBITs, defined by the electron beam itself, and 2) non-dispersive solid-state detectors with much lower spectral resolving powers but that have a broad dynamic range, high count rate ability and do not require a slit. Both of these approaches have compromises that limit the type and efficiency of measurements that can be performed. In 1984 NASA initiated a program to produce a non-dispersive instrument with high spectral resolving power for x-ray astrophysics based on the cryogenic x-ray calorimeter. This program produced the XRS non-dispersive spectrometers on the Astro-E, Astro-E2 (Suzaku) orbiting observatories, the SXS instrument on the Astro-H observatory, and the planned XMS instrument on the International X-ray Observatory. Complimenting these spaceflight programs, a permanent high-resolution x-ray calorimeter spectrometer, the XRS/EBIT, was installed on the LLNL EBIT in 2000. This unique instrument was upgraded to a spectral resolving power of 1000 at 6 keV in 2003 and replaced by a nearly autonomous production-class spectrometer, the EBIT Calorimeter Spectrometer (ECS), in 2007. The ECS spectrometer has a simultaneous bandpass from 0.07 to over 100 keV with a spectral resolving power of 1300 at 6 keV with unit quantum efficiency, and 1900 at 60 keV with a quantum efficiency of 30%. X-ray calorimeters are event based, single photon spectrometers with event time tagging to better than 10 us. We are currently developing a follow-on instrument based on a newer generation of x-ray calorimeters with a spectral resolving power of 3000 at 6 keV, and improved timing and measurement cadence. The unique capabilities of the x-ray

Evaluation on the stability of Hg in ABS disk CRM during measurements by wavelength dispersive X-ray fluorescence spectrometry.

Science.gov (United States)

Ohata, Masaki; Kidokoro, Toshihiro; Hioki, Akiharu

2012-01-01

The stability of Hg in an acrylonitrile-butadiene-styrene disk certified reference material (ABS disk CRM, NMIJ CRM 8116-a) during measurements by wavelength dispersion X-ray fluorescence (WD-XRF) analysis was evaluated in this study. The XRF intensities of Hg (L(α)) and Pb (L(α)) as well as the XRF intensity ratios of Hg (L(α))/Pb (L(α)) observed under different X-ray tube current conditions as well as their irradiation time were examined to evaluate the stability of Hg in the ABS disk CRM. The observed XRF intensities and the XRF intensity ratios for up to 32 h of measurements under 80 mA of X-ray tube current condition were constant, even though the surface of the ABS disk CRM was charred by the X-ray irradiation with high current for a long time. Moreover, the measurements on Hg and Pb in the charred disks by an energy dispersive XRF (ED-XRF) spectrometer showed constant XRF intensity ratios of Hg (L(α))/Pb (L(α)). From these results, Hg in the ABS disk CRM was evaluated to be sufficiently stable for XRF analysis.

Scanning electron microscope/energy dispersive x ray analysis of impact residues on LDEF tray clamps

Science.gov (United States)

Bernhard, Ronald P.; Durin, Christian; Zolensky, Michael E.

1992-01-01

To better understand the nature of particulates in low-Earth orbit (LEO), and their effects on spacecraft hardware, we are analyzing residues found in impacts on the Long Duration Exposure Facility (LDEF) tray clamps. LDEF experiment trays were held in place by 6 to 8 chromic-anodized aluminum (6061-T6) clamps that were fastened to the spacecraft frame using three stainless steel hex bolts. Each clamp exposed an area of approximately 58 sq cm (4.8 cm x 12.7 cm x .45 cm, minus the bolt coverage). Some 337 out of 774 LDEF tray clamps were archived at JSC and are available through the Meteoroid & Debris Special Investigation Group (M&D SIG). Optical scanning of clamps, starting with Bay/Row A01 and working toward H25, is being conducted at JSC to locate and document impacts as small as 40 microns. These impacts are then inspected by Scanning Electron Microscopy/Energy Dispersive X-ray Analysis (SEM/EDXA) to select those features which contain appreciable impact residue material. Based upon the composition of projectile remnants, and using criteria developed at JSC, we have made a preliminary discrimination between micrometeoroid and space debris residue-containing impact features. Presently, 13 impacts containing significant amounts of unmelted and semi-melted micrometeoritic residues were forwarded to Centre National d'Etudes Spatiales (CNES) in France. At the CNES facilities, the upgraded impacts were analyzed using a JEOL T330A SEM equipped with a NORAN Instruments, Voyager X-ray Analyzer. All residues were quantitatively characterized by composition (including oxygen and carbon) to help understand interplanetary dust as possibly being derived from comets and asteroids.

Trace and ultratrace determination of heavy metal ions by energy-dispersive X-ray fluorescence spectrometry using graphene as solid sorbent in dispersive micro solid-phase extraction

Energy Technology Data Exchange (ETDEWEB)

Kocot, Karina; Sitko, Rafal, E-mail: rafal.sitko@us.edu.pl

2014-04-01

In this paper, the adsorptive properties of graphene nanosheets were used for simultaneous preconcentration of cobalt, nickel, copper and lead ions from water samples. The developed methodology is based on dispersive micro-solid phase extraction (DMSPE) which is miniaturized and a simplified version of classical solid phase extraction technique. In proposed procedure only 200 μL of suspension containing graphene (0.2 mg), ammonium pyrrolidine dithiocarbamate (APDC) (0.8 mg) and Triton-X-100 (0.1 mg) is rapidly injected to 50 mL of water sample. Then, graphene nanosheets with adsorbed metal-APDC chelates are collected on membrane filter and measured using energy-dispersive X-ray fluorescence (EDXRF) spectrometry. The various parameters including pH, amount of APDC, sample volume, amount of Triton-X-100 and sorption time were optimized in order to obtain the best recoveries. The experiment shows that Co, Ni, Cu and Pb can be simultaneously preconcentrated at pH of 5 with high recoveries (97%, 96%, 99% and 96% for Co, Ni, Cu and Pb, respectively) and very good precision (RSDs within 2.6–3.4%). Due to the excellent enrichment factors ranging from 400 to 2500 the proposed DMSPE–EDXRF procedure offers low detection limits. For optimized measurement conditions (voltage and current of X-ray tube, primary beam filter) the detection limits are even 0.08, 0.07, 0.08 and 0.20 ng mL{sup −1} for Co, Ni, Cu and Pb, respectively. - Highlights: • Excellent detection limits using EDXRF • A new preconcentration procedure combining DMSPE and EDXRF measurement • Graphene as a promising and efficient solid sorbent in DMSPE • Simple, fast, inexpensive and environmental friendly method.

In situ synchrotron X-ray studies during metal-organic chemical vapor deposition of semiconductors

Energy Technology Data Exchange (ETDEWEB)

Thompson, Carol [Northern Illinois Univ., DeKalb, IL (United States); Argonne National Lab., Argonne, IL (United States); Highland, Matthew J.; Perret, Edith; Fuoss, Paul H.; Streiffer, Stephen K.; Stephenson, G. Brian [Argonne National Lab., Argonne, IL (United States); Richard, Marie-Ingrid [Universite Paul Cezanne Aix-Marseille, Marseille (France)

2012-07-01

In-situ, time-resolved techniques provide valuable insight into the complex interplay of surface structural and chemical evolution occurring during materials synthesis and processing of semiconductors. Our approach is to observe the evolution of surface structure and morphology at the atomic scale in real-time during metal organic vapor phase deposition (MOCVD) by using grazing incidence x-ray scattering and X-ray fluorescence, coupled with visible light scattering. Our vertical-flow MOCVD chamber is mounted on a 'z-axis' surface diffractometer designed specifically for these studies of the film growth, surface evolution and the interactions within a controlled growth environment. These techniques combine the ability of X-rays to penetrate a complex environment for measurements during growth and processing, with the sensitivity of surface scattering techniques to atomic and nanoscale structure. In this talk, we outline our program and discuss examples from our in-situ and real-time X-ray diffraction and fluorescence studies of InN, GaN, and InGaN growth on GaN(0001).

Cyclic olefin homopolymer-based microfluidics for protein crystallization and in situ X-ray diffraction

International Nuclear Information System (INIS)

Emamzadah, Soheila; Petty, Tom J.; De Almeida, Victor; Nishimura, Taisuke; Joly, Jacques; Ferrer, Jean-Luc; Halazonetis, Thanos D.

2009-01-01

A cyclic olefin homopolymer-based microfluidics system has been established for protein crystallization and in situ X-ray diffraction. Microfluidics is a promising technology for the rapid identification of protein crystallization conditions. However, most of the existing systems utilize silicone elastomers as the chip material which, despite its many benefits, is highly permeable to water vapour. This limits the time available for protein crystallization to less than a week. Here, the use of a cyclic olefin homopolymer-based microfluidics system for protein crystallization and in situ X-ray diffraction is described. Liquid handling in this system is performed in 2 mm thin transparent cards which contain 500 chambers, each with a volume of 320 nl. Microbatch, vapour-diffusion and free-interface diffusion protocols for protein crystallization were implemented and crystals were obtained of a number of proteins, including chicken lysozyme, bovine trypsin, a human p53 protein containing both the DNA-binding and oligomerization domains bound to DNA and a functionally important domain of Arabidopsis Morpheus’ molecule 1 (MOM1). The latter two polypeptides have not been crystallized previously. For X-ray diffraction analysis, either the cards were opened to allow mounting of the crystals on loops or the crystals were exposed to X-rays in situ. For lysozyme, an entire X-ray diffraction data set at 1.5 Å resolution was collected without removing the crystal from the card. Thus, cyclic olefin homopolymer-based microfluidics systems have the potential to further automate protein crystallization and structural genomics efforts

Bulk substrate porosity verification by applying Monte Carlo modeling and Castaing's formula using energy-dispersive x-rays

Science.gov (United States)

Yung, Lai Chin; Fei, Cheong Choke; Mandeep, Jit Singh; Amin, Nowshad; Lai, Khin Wee

2015-11-01

The leadframe fabrication process normally involves additional thin-metal layer plating on the bulk copper substrate surface for wire bonding purposes. Silver, tin, and copper flakes are commonly adopted as plating materials. It is critical to assess the density of the plated metal layer, and in particular to look for porosity or voids underneath the layer, which may reduce the reliability during high-temperature stress. A fast, reliable inspection technique is needed to assess the porosity or void weakness. To this end, the characteristics of x-rays generated from bulk samples were examined using an energy-dispersive x-ray (EDX) detector to examine the porosity percentage. Monte Carlo modeling was integrated with Castaing's formula to verify the integrity of the experimental data. Samples with different porosity percentages were considered to test the correlation between the intensity of the collected x-ray signal and the material density. To further verify the integrity of the model, conventional cross-sectional samples were also taken to observe the porosity percentage using Image J software measurement. A breakthrough in bulk substrate assessment was achieved by applying EDX for the first time to nonelemental analysis. The experimental data showed that the EDX features were not only useful for elemental analysis, but also applicable to thin-film metal layer thickness measurement and bulk material density determination. A detailed experiment was conducted using EDX to assess the plating metal layer and bulk material porosity.

Application of in situ x-ray diffraction techniques in heterogenous catalytic systems

International Nuclear Information System (INIS)

Sharifah Bee Abd Hamid

2002-01-01

A broad range of techniques is available today for the characterisation of catalysts and the investigation of catalyst reaction mechanisms. However, only a limited number of those are suitable for in situ studies, i.e experiments performed in conditions mimicking or close as possible to real operating conditions. Various commercially and in-house developed in situ X-Ray diffraction (XRD) cells have been used to obtain information on the phase and structure of materials at the initial formation stage, activation methodology, calcination, reduction and carburization. A major advantage of the in situ X-ray cells is that it allows direct observations on the decomposition of precursors leading to various phases in a controlled environment, i.e. controlled temperature and pressure under specified gases. The cells can be operated both at high temperatures and high pressures, equipped with Position Sensitive Detector (PSD), feature which was used to study phase transformation occurring during the activation of various solids. In MoO 3 , XRD results provide detailed information on the hydrogen insertion into its lattice, followed by carburization providing good understanding on the mechanism in the solid transformation leading to the metastable MoC 1 -x phase. For the Bi-SnO x systems, the environmental cell coupled with XRD and PSD allow the design of activation procedure to obtain the active Bi 2 Sn 2 O 7 . The in situ XRD technique reveals crucial information on the initial stage of oxides formations prior to condensation reaction shown in MCM-41 and titania systems. In this presentation, discussions on general achievements and problems relating to the use of in situ XRD techniques as well as of specific examples selected to illustrate the use and potential of in situ XRD are made. It is not intended to be a review of the art but a highlight of the challenges which the catalytic and material scientists face when entering the avenue. (Author)

Quantitative determination on heavy metals in different stages of wine production by Total Reflection X-ray Fluorescence and Energy Dispersive X-ray Fluorescence: Comparison on two vineyards

Energy Technology Data Exchange (ETDEWEB)

Pessanha, Sofia [Centro Fisica Atomica, Departamento de Fisica, Faculdade de Ciencias, Universidade de Lisboa, Av. Prof. Gama Pinto, 2, 1649-003 Lisboa (Portugal); Carvalho, Maria Luisa, E-mail: luisa@cii.fc.ul.p [Centro Fisica Atomica, Departamento de Fisica, Faculdade de Ciencias, Universidade de Lisboa, Av. Prof. Gama Pinto, 2, 1649-003 Lisboa (Portugal); Becker, Maria; Bohlen, Alex von [Institute for analytical Sciences, Bunsen-Kirchhoff-Str. 11, 44139 Dortmund (Germany)

2010-06-15

The purpose of this study is to determine the elemental content, namely heavy metals, of samples of vine-leaves, grapes must and wine. In order to assess the influence of the vineyard age on the elemental content throughout the several stages of wine production, elemental determinations of trace elements were made on products obtained from two vineyards aged 6 and 14 years from Douro region. The elemental content of vine-leaves and grapes was determined by Energy Dispersive X-Ray Fluorescence (EDXRF), while analysis of the must and wine was performed by Total Reflection X-ray Fluorescence (TXRF). Almost all elements present in wine and must samples did not exceed the recommended values found in literature for wine. Bromine was present in the 6 years old wine in a concentration 1 order of magnitude greater than what is usually detected. The Cu content in vine-leaves from the older vineyard was found to be extremely high probably due to excessive use of Cu-based fungicides to control vine downy mildew. Higher Cu content was also detected in grapes although not so pronounced. Concerning the wine a slightly higher level was detected on the older vineyard, even so not exceeding the recommended value.

Quantitative determination on heavy metals in different stages of wine production by Total Reflection X-ray Fluorescence and Energy Dispersive X-ray Fluorescence: Comparison on two vineyards

International Nuclear Information System (INIS)

Pessanha, Sofia; Carvalho, Maria Luisa; Becker, Maria; Bohlen, Alex von

2010-01-01

The purpose of this study is to determine the elemental content, namely heavy metals, of samples of vine-leaves, grapes must and wine. In order to assess the influence of the vineyard age on the elemental content throughout the several stages of wine production, elemental determinations of trace elements were made on products obtained from two vineyards aged 6 and 14 years from Douro region. The elemental content of vine-leaves and grapes was determined by Energy Dispersive X-Ray Fluorescence (EDXRF), while analysis of the must and wine was performed by Total Reflection X-ray Fluorescence (TXRF). Almost all elements present in wine and must samples did not exceed the recommended values found in literature for wine. Bromine was present in the 6 years old wine in a concentration 1 order of magnitude greater than what is usually detected. The Cu content in vine-leaves from the older vineyard was found to be extremely high probably due to excessive use of Cu-based fungicides to control vine downy mildew. Higher Cu content was also detected in grapes although not so pronounced. Concerning the wine a slightly higher level was detected on the older vineyard, even so not exceeding the recommended value.

In situ anodization of aluminum surfaces studied by x-ray reflectivity and electrochemical impedance spectroscopy

International Nuclear Information System (INIS)

Bertram, F.; Evertsson, J.; Messing, M. E.; Mikkelsen, A.; Lundgren, E.; Zhang, F.; Pan, J.; Carlà, F.; Nilsson, J.-O.

2014-01-01

We present results from the anodization of an aluminum single crystal [Al(111)] and an aluminum alloy [Al 6060] studied by in situ x-ray reflectivity, in situ electrochemical impedance spectroscopy and ex situ scanning electron microscopy. For both samples, a linear increase of oxide film thickness with increasing anodization voltage was found. However, the slope is much higher in the single crystal case, and the break-up of the oxide film grown on the alloy occurs at a lower anodization potential than on the single crystal. The reasons for these observations are discussed as are the measured differences observed for x-ray reflectivity and electrochemical impedance spectroscopy.

Application of X-rays and Synchrotron X Rays to Residual Stress Evaluation Near Surfaces

International Nuclear Information System (INIS)

Pyzalla, Anke

1999-01-01

A nondestructive residual stress analysis can be performed using diffraction methods. The easiest accessible radiation is characteristic X radiation that has a penetration depth of ∼10 microm suitable for the determination of the residual stresses in near-surface layers. Special techniques have been developed, e.g., with respect to in situ analyses of the stress state in oxide layers and the residual stress analysis in coarse grained zones of steel welds or annealed Ni-base alloys. Depending on the size of the gauge volume, neutron diffraction can provide information at depths of tens of millimetres of steel and many tens of millimetres of Al. An alternative to the use of the characteristic synchrotron radiation is the use of a high-energy polychromatic beam in an energy dispersive arrangement, which gives access to higher penetration depths at still gauge volumes as small as 100 microm x 100 microm x 1 mm in steel rods of 15-mm diameter. The combination of neutrons with conventional X rays and monochromatic and polychromatic synchrotron radiation allows for a comprehensive investigation of the phase composition, the texture, and the residual stresses

Investigation of multilayered nanocomposites as low energy X-Rays attenuators

Energy Technology Data Exchange (ETDEWEB)

Silva, Liliane; Batista, Adriana S.M.; Nascimento, Jefferson P.; Furtado, Clascídia A.; Faria, Luiz O., E-mail: asfisica@gmail.com, E-mail: adriananuclear@yahoo.com.br, E-mail: farialo@cdtn.br, E-mail: nascimentopatricio@yahoo.com.br, E-mail: clas@cdtn.br [Universidade Federal de Minas Gerais (UFMG), Belo Horizonte, MG (Brazil); Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil)

2017-11-01

The development of radiation attenuating materials has application in radioprotection and conditioning of short-lived waste. Polymeric materials can serve as a matrix for the dispersion of nanomaterials with good attenuation features, resulting in lightweight, conformable, flexible and easy-to-process materials. Thus, some well-known shielding materials could be used in low proportion for the formation of new materials. On the other hand, nanostructured carbon materials, such as graphene oxide (GO) and carbon nanotubes (NTCs), have been reported recently to show enhanced attenuation properties. In this sense, polymeric matrixes provide the necessary flexibility for use in various applications that require molding. For the present work, poly(vinylidene fluoride) [PVDF] homopolymers and its fluorinated copolymers were filled with nanosized metallic and graphene oxides in order to produce nanocomposites with increased low energy X-ray attenuation efficiency. Film samples of PVDF/reduced Graphene Oxide [PVDF/rGO] and Poly(vinylidene fluoride – tryfluorethylene)/Barium Oxide [P(VDF-TrFE)/BaO] were synthesized. In a second step, the samples were then sandwiched between Kapton® layers and exposed to X-rays source (8.5 keV). The samples were characterized with Scanning Electron Microscopy (SEM) and Energy Dispersive Spectroscopy (EDS). The attenuation coefficient was evaluated and compared with the attenuation of the individual constituents. It was observed an increase in the linear attenuation coefficient of the layered materials, justifying further investigation of these nanostructured composites as X-ray or gamma radiation attenuators. (author)

Investigation of multilayered nanocomposites as low energy X-Rays attenuators

International Nuclear Information System (INIS)

Silva, Liliane; Batista, Adriana S.M.; Nascimento, Jefferson P.; Furtado, Clascídia A.; Faria, Luiz O.

2017-01-01

The development of radiation attenuating materials has application in radioprotection and conditioning of short-lived waste. Polymeric materials can serve as a matrix for the dispersion of nanomaterials with good attenuation features, resulting in lightweight, conformable, flexible and easy-to-process materials. Thus, some well-known shielding materials could be used in low proportion for the formation of new materials. On the other hand, nanostructured carbon materials, such as graphene oxide (GO) and carbon nanotubes (NTCs), have been reported recently to show enhanced attenuation properties. In this sense, polymeric matrixes provide the necessary flexibility for use in various applications that require molding. For the present work, poly(vinylidene fluoride) [PVDF] homopolymers and its fluorinated copolymers were filled with nanosized metallic and graphene oxides in order to produce nanocomposites with increased low energy X-ray attenuation efficiency. Film samples of PVDF/reduced Graphene Oxide [PVDF/rGO] and Poly(vinylidene fluoride – tryfluorethylene)/Barium Oxide [P(VDF-TrFE)/BaO] were synthesized. In a second step, the samples were then sandwiched between Kapton® layers and exposed to X-rays source (8.5 keV). The samples were characterized with Scanning Electron Microscopy (SEM) and Energy Dispersive Spectroscopy (EDS). The attenuation coefficient was evaluated and compared with the attenuation of the individual constituents. It was observed an increase in the linear attenuation coefficient of the layered materials, justifying further investigation of these nanostructured composites as X-ray or gamma radiation attenuators. (author)

In-Situ Synchrotron X-ray Study of the Phase and Texture Evolution of Ceria and Superconductor Films Deposited by Chemical Solution Method

DEFF Research Database (Denmark)

Yue, Zhao; Grivel, Jean-Claude; He, Dong

2012-01-01

In situ synchrotron x-ray diffraction is used to study the phase and texture formation of ceria based films and superconductor films deposited by the chemical solution method on technical substrates. Combined analysis using in situ synchrotron x-ray diffraction, thermogravimetry/differential ther......In situ synchrotron x-ray diffraction is used to study the phase and texture formation of ceria based films and superconductor films deposited by the chemical solution method on technical substrates. Combined analysis using in situ synchrotron x-ray diffraction, thermogravimetry...

A new energy dispersive X-ray spectrometer developed in ATOMKI (Debrecen, Hungary)

International Nuclear Information System (INIS)

Bacso, J.; Kalinka, G.; Kovacs, P.; Lakatos, T.

1982-01-01

A new X-ray spectrometer developed in ATOMKI is described. The measuring head contains a p-type Si(Li) detector surrounded by an Al collimator, a charge sensitive preamplifier and a vacuum cryostat. The analog pulse processor uses filters with variable parameters. The characteristic properties of the spectrometer (energy resolution, its dependence on load, stability) are investigated. The background is measured using three different radioactive sources and the results are compared with those of other pulse forming techniques. (D.Gy.)

In situ analysis of elemental depth distributions in thin films by combined evaluation of synchrotron x-ray fluorescence and diffraction

International Nuclear Information System (INIS)

Mainz, R.; Klenk, R.

2011-01-01

In this work we present a method for the in situ analysis of elemental depth distributions in thin films using a combined evaluation of synchrotron x-ray fluorescence and energy-dispersive x-ray diffraction signals. We recorded diffraction and fluorescence signals simultaneously during the reactive annealing of thin films. By means of the observed diffraction signals, the time evolution of phases in the thin films during the annealing processes can be determined. We utilized this phase information to parameterize the depth distributions of the elements in the films. The time-dependent fluorescence signals were then taken to determine the parameters representing the parameterized depth distributions. For this latter step, we numerically calculated the fluorescence intensities for a given set of depth distributions. These calculations handle polychromatic excitation and arbitrary functions of depth distributions and take into account primary and secondary fluorescence. Influences of lateral non-uniformities of the films, as well as the accuracy limits of the method, are investigated. We apply the introduced method to analyze the evolution of elemental depth distributions and to quantify the kinetic parameters during a synthesis process of CuInS 2 thin films via the reactive annealing of Cu-In precursors in a sulfur atmosphere.

In situ investigation of the surface silvering of late Roman coins by combined use of high energy broad-beam and low energy micro-beam X-ray fluorescence techniques

Energy Technology Data Exchange (ETDEWEB)

Romano, F.P., E-mail: romanop@lns.infn.it [IBAM, CNR, Via Biblioteca 4, 95124 Catania (Italy); LNS, INFN, Via S. Sofia 62, 95123 Catania (Italy); Garraffo, S. [ITABC, CNR, Via Salaria km 29.300, 00016 Monterotondo, Roma (Italy); Pappalardo, L. [IBAM, CNR, Via Biblioteca 4, 95124 Catania (Italy); LNS, INFN, Via S. Sofia 62, 95123 Catania (Italy); Rizzo, F. [LNS, INFN, Via S. Sofia 62, 95123 Catania (Italy); Dipartimento di Fisica e Astronomia, Universita di Catania, Via S. Sofia 64, 95123 Catania (Italy)

2012-07-15

The compositional analysis of archeological metals performed with the X-ray Fluorescence technique (XRF) provides information on the ancient technology. One of the most interesting case-study concerns the techniques used by Romans for silvering the surface of coins. Different metallurgical processes have been suggested in previous studies. Recently the investigation has been addressed to the mercury-silvering and to its possible use in the mass-production of coins minted during the late period (after 294 AD). In the present paper the non-destructive investigation of the silvering process used for manufacturing the Roman nummi - the important typology of coin introduced by Diocletian in his monetary reform - is approached by the combined use of the standard X-Ray Fluorescence (XRF) and the low energy micro-X-Ray Fluorescence (LE-{mu}XRF) portable methods. The research was focused on the systematic determination of the mercury presence in a large number of samples and on its correlation with silver in the surface of the coins. 1041 Roman nummi belonging to the Misurata Treasure were analyzed in situ, at the Leptis Magna Museum (Al Khums, Libya). The treasure, composed of about 108 thousand silvered coins, gives the unique opportunity to study the Roman coinage in a wide interval of time (about 40 years in the period 294-333 AD) and in almost all the imperial mints operating in the Roman world. - Highlights: Black-Right-Pointing-Pointer Custom-building of a high energy broad-beam and a low energy micro-beam XRF Black-Right-Pointing-Pointer In situ analysis of the silvering methods in late Roman nummi with plated surfaces Black-Right-Pointing-Pointer The broad-beam XRF was applied for the detection of mercury traces in the coin alloy. Black-Right-Pointing-Pointer The low energy micro-XRF was used to scan the surface patina of the coins. Black-Right-Pointing-Pointer The correlation between mercury and silver at the coin surface was evidenced.

Setup for in situ x-ray diffraction study of swift heavy ion irradiated materials

Science.gov (United States)

Kulriya, P. K.; Singh, F.; Tripathi, A.; Ahuja, R.; Kothari, A.; Dutt, R. N.; Mishra, Y. K.; Kumar, Amit; Avasthi, D. K.

2007-11-01

An in situ x-ray diffraction (XRD) setup is designed and installed in the materials science beam line of the Pelletron accelerator at the Inter-University Accelerator Centre for in situ studies of phase change in swift heavy ion irradiated materials. A high vacuum chamber with suitable windows for incident and diffracted X-rays is integrated with the goniometer and the beamline. Indigenously made liquid nitrogen (LN2) temperature sample cooling unit is installed. The snapshots of growth of particles with fluence of 90MeV Ni ions were recorded using in situ XRD experiment, illustrating the potential of this in situ facility. A thin film of C60 was used to test the sample cooling unit. It shows that the phase of the C60 film transforms from a cubic lattice (at room temperature) to a fcc lattice at around T =255K.

Setup for in situ x-ray diffraction study of swift heavy ion irradiated materials.

Science.gov (United States)

Kulriya, P K; Singh, F; Tripathi, A; Ahuja, R; Kothari, A; Dutt, R N; Mishra, Y K; Kumar, Amit; Avasthi, D K

2007-11-01

An in situ x-ray diffraction (XRD) setup is designed and installed in the materials science beam line of the Pelletron accelerator at the Inter-University Accelerator Centre for in situ studies of phase change in swift heavy ion irradiated materials. A high vacuum chamber with suitable windows for incident and diffracted X-rays is integrated with the goniometer and the beamline. Indigenously made liquid nitrogen (LN2) temperature sample cooling unit is installed. The snapshots of growth of particles with fluence of 90 MeV Ni ions were recorded using in situ XRD experiment, illustrating the potential of this in situ facility. A thin film of C60 was used to test the sample cooling unit. It shows that the phase of the C60 film transforms from a cubic lattice (at room temperature) to a fcc lattice at around T=255 K.

Energy dispersive X-ray microanalysis of zinc and calcium in organelles of insulin-producing cells of the mouse, rat, and a fish

Energy Technology Data Exchange (ETDEWEB)

Falkmer, S; Odselius, R [Lund Univ. (Sweden); Blondel, B; Prentki, M; Wollheim, C B [Geneva Univ. (Switzerland)

1985-01-01

By means of energy dispersive X-ray microanalysis in the scanning-transmission electron microscope, spectra were obtained from quick-frozen, cryo-ultramicrotome-cut, freeze-dried sections of insulin cells from a fish and a mouse. It was shown that both zinc and calcium are present in significant quantities in native islet cell ..beta.. granules. In the ..beta.. granules of the rat RINm5F insuloma cells calcium, but not zinc, seemed to accumulate; the zinc contents in the secretion granules of these neoplastic ..beta.. cells were probably below the detection limit.

The adsorption of methanol and water on SAPO-34: in situ and ex situ X-ray diffraction studies

DEFF Research Database (Denmark)

Wragg, David S.; Johnsen, Rune; Norby, Poul

2010-01-01

The adsorption of methanol on SAPO-34 has been studied using a combination of in situ synchrotron powder X-ray diffraction to follow the process and ex situ high resolution powder diffraction to determine the structure. The unit cell volume of SAPO-34 is found to expand by 0.5% during methanol ad...

Development of an in situ temperature stage for synchrotron X-ray spectromicroscopy

Energy Technology Data Exchange (ETDEWEB)

Chakraborty, R., E-mail: rupak@alum.mit.edu, E-mail: buonassisi@mit.edu; Serdy, J.; Culpepper, M. L.; Buonassisi, T., E-mail: rupak@alum.mit.edu, E-mail: buonassisi@mit.edu [Department of Mechanical Engineering, Massachusetts Institute of Technology, Cambridge, Massachusetts 02139 (United States); West, B.; Stuckelberger, M.; Bertoni, M. I. [School of Electrical, Computer and Energy Engineering, Arizona State University, Tempe, Arizona 85287 (United States); Lai, B.; Maser, J. [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States)

2015-11-15

In situ characterization of micro- and nanoscale defects in polycrystalline thin-film materials is required to elucidate the physics governing defect formation and evolution during photovoltaic device fabrication and operation. X-ray fluorescence spectromicroscopy is particularly well-suited to study defects in compound semiconductors, as it has a large information depth appropriate to study thick and complex materials, is sensitive to trace amounts of atomic species, and provides quantitative elemental information, non-destructively. Current in situ methods using this technique typically require extensive sample preparation. In this work, we design and build an in situ temperature stage to study defect kinetics in thin-film solar cells under actual processing conditions, requiring minimal sample preparation. Careful selection of construction materials also enables controlled non-oxidizing atmospheres inside the sample chamber such as H{sub 2}Se and H{sub 2}S. Temperature ramp rates of up to 300 °C/min are achieved, with a maximum sample temperature of 600 °C. As a case study, we use the stage for synchrotron X-ray fluorescence spectromicroscopy of CuIn{sub x}Ga{sub 1−x}Se{sub 2} (CIGS) thin-films and demonstrate predictable sample thermal drift for temperatures 25–400 °C, allowing features on the order of the resolution of the measurement technique (125 nm) to be tracked while heating. The stage enables previously unattainable in situ studies of nanoscale defect kinetics under industrially relevant processing conditions, allowing a deeper understanding of the relationship between material processing parameters, materials properties, and device performance.

Analysis of agricultural soils by using energy dispersive X-ray fluorescence; Analise de solos agricolas por fluorescencia de raios-X por dispersao de energia

Energy Technology Data Exchange (ETDEWEB)

Anjos, Marcelino Jose dos

2000-03-01

In this work, we describe an Energy Dispersive x-ray Fluorescence System with a x-ray tube excitation for trace analysis of environmental samples (soil). The system was used to analyze the contamination of metals in treated soils with doses of 10, 20 and 30 ton/ha of compound organic of urban garbage of the type Fertilurb and 10 ton/ha of aviary bed (manure of birds). Samples of roots and foliages of plant radishes cultivated in these soils were also analyzed. The soil samples were collected in five different depths of 0,5, 5-10, 10-20, 20-40 and 40-60 cm. The experimental set-up is composed by an OXFORD X-ray (30 kV, 50 {mu}A and W anode), an ORTEC Si-Li detector, with an energy resolution of about 180 eV at 5.9 keV and an ORTEC multichannel-analyser. The X-ray spectrum tube is quasi-monochromatic by using of Ti filter. Samples were prepared in pellet form with superficial density in the range of 100 mg/cm{sup 2}. The fundamental parameter method was used in order to verify the elemental concentration. It was possible to determine the concentrations of thirteen elements: K, Ca, Ti, Mn, Fe, Cu, Zn, Br, Rb, Sr, Y, Zr and Pb in the treated soils with compounds organic. The results indicate that the values found for K, Ca, Rb, Sr, Zr and Pb are significantly above the upper confidence limits for the control soil ({alpha} = 0.05). There is a real different between these elements compared to their relationship in the control soils, ({alpha}=0,05). There is a real difference between these elements compared to their relationship in the control soils, confirming the influence of the organic compounds in the soil. (author)

Using angular dispersion and anomalous transmission to shape ultramonochromatic x rays

Energy Technology Data Exchange (ETDEWEB)

Shvyd' ko, Yuri; Stoupin, Stanislav; Shu, Deming; Khachatryan, Ruben [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States)

2011-11-15

Optical spectrometers, instruments that work with highly monochromatic light, are commonly rated by the spectral bandwidth, which defines the ability to resolve closely spaced spectral components. Another equally important feature is the spectral contrast, the ability to detect faint objects among these components. Here we demonstrate that a combined effect of angular dispersion (AD) and anomalous transmission (AT) of x rays in Bragg reflection from asymmetrically cut crystals can shape spectral distributions of x rays to profiles with high contrast and small bandwidths. The AD and AT x-ray optics is implemented as a five-reflection, three-crystal arrangement featuring a combination of the above-mentioned attributes so desirable for x-ray monochromators and analyzers: a spectral contrast of {approx_equal} 500, a bandwidth of {approx_equal} 0.46 meV, and a remarkably large angular acceptance of {approx_equal} 107 {mu}rad with 9.1 keV x rays. The new optics can become a foundation for the next-generation inelastic x-ray scattering spectrometers for studies of atomic dynamics.

A Soft X-ray Spectrometer using a Highly Dispersive Multilayer Grating

International Nuclear Information System (INIS)

Warwick, Tony; Padmore, Howard; Voronov, Dmitriy; Yashchuk, Valeriy

2010-01-01

There is a need for higher resolution spectrometers as a tool for inelastic x-ray scattering. Currently, resolving power around R = 10,000 is advertised. Measured RIXS spectra are often limited by this instrumental resolution and higher resolution spectrometers using conventional gratings would be prohibitively large. We are engaged in a development program to build blazed multilayer grating structures for diffracting soft x-rays in high order. This leads to spectrometers with dispersion much higher than is possible using metal coated-gratings. The higher dispersion then provides higher resolution and the multilayer gratings are capable of operating away from grazing incidence as required. A spectrometer design is presented with a total length 3.8 m and capable of 10 5 resolving power.

A Soft X-ray Spectrometer using a Highly Dispersive Multilayer Grating

International Nuclear Information System (INIS)

Warwick, Tony; Padmore, Howard; Voronov, Dmitriy; Yashchuk, Valeriy

2010-01-01

There is a need for higher resolution spectrometers as a tool for inelastic x-ray scattering. Currently, resolving power around R = 10,000 is advertised. Measured RIXS spectra are often limited by this instrumental resolution and higher resolution spectrometers using conventional gratings would be prohibitively large. We are engaged in a development program to build blazed multilayer grating structures for diffracting soft x-rays in high order. This leads to spectrometers with dispersion much higher than is possible using metal coated-gratings. The higher dispersion then provides higher resolution and the multilayer gratings are capable of operating away from grazing incidence as required. A spectrometer design is presented with a total length 3.8m and capable of 10 5 resolving power.

Solution spectroelectrochemical cell for in situ X-ray absorption fine structure

International Nuclear Information System (INIS)

Antonio, M.R.; Soderholm, L.

1995-01-01

A purpose-built spectroelectrochemical cell for in situ fluorescence XAFS (X-ray Absorption Fine Structure) measurements of bulk solution species during constant-potential electrolysis is described. The cell performance was demonstrated by the collection of europium L 3 -edge XANES (X-ray Absorption Near Edge Structure) throughout the course of electrolysis of an aqueous solution of EuCl 3 ·6H 2 O in 1 M H 2 SO 4 . The europium L 3 -edge resonances reported here for the Eu III and Eu II ions demonstrate that their 2p 3/2 → 5d electronic transition probabilities are not the same

On-axis microscopes for the inelastic x-ray scattering beamline at NSLS-II

Energy Technology Data Exchange (ETDEWEB)

Gofron, K. J., E-mail: kgofron@bnl.gov; Cai, Y. Q.; Coburn, D. S.; Antonelli, S.; Suvorov, A. [National Synchrotron Light Source II, Brookhaven National Laboratory, Upton, NY 11973 (United States); Flores, J. [Department of Physics and Astronomy, Stony Brook University, NY 11794 (United States)

2016-07-27

A novel on-axis X-ray microscope with 3 µm resolution, 3x magnification, and a working distance of 600 mm for in-situ sample alignment and X-ray beam visualization for the Inelastic X-ray Scattering (IXS) beamline at NSLS-II is presented. The microscope uses reflective optics, which minimizes dispersion, and allows imaging from Ultraviolet (UV) to Infrared (IR) with specifically chosen objective components (coatings, etc.). Additionally, a portable high resolution X-ray microscope for KB mirror alignment and X-ray beam characterization was developed.

Material Discriminated X-Ray CT System by Using New X-Ray Imager with Energy Discriminate Function

Directory of Open Access Journals (Sweden)

Toru Aoki

2008-04-01

Full Text Available Material discriminated X-ray CT system has been constructed by using conventional X-ray tube (white X-ray source and photon-counting X-ray imager as an application with energy band detection. We have already reported material identify X-ray CT using K-shell edge method elsewhere. In this report the principle of material discrimination was adapted the separation of electron-density and atomic number from attenuation coefficient mapping in X-ray CT reconstructed image in two wavelength X-ray CT method using white X-ray source and energy discriminated X-ray imager by using two monochrome X-ray source method. The measurement phantom was prepared as four kinds material rods (Carbon(C, Iron(Fe, Copper(Cu, Titanium(Ti rods of 3mm-diameter inside an aluminum(Al rod of 20mm-diameter. We could observed material discriminated X-ray CT reconstructed image, however, the discrimination properties were not good than two monochrome X-ray CT method. This results was could be explained because X-ray scattering, beam-hardening and so on based on white X-ray source, which could not observe in two monochrome X-ray CT method. However, since our developed CdTe imager can be detect five energy-bands at the same time, we can use multi-band analysis to decrease the least square error margin. We will be able to obtain more high separation in atomic number mapping in X-ray CT reconstructed image by using this system.

Effective Energy Determination Of Radiodiagnostic X-Rays

International Nuclear Information System (INIS)

Sumarni; Mart, Terry

2000-01-01

X-rays have been used for diagnostic radiology to produce image on film that give anatomy information. Effective energy should be known to get benefit exposure. Half value layer (HVL) as shown as monoenergetic x-rays has similar spectra of energy x-rays. It has been done measurement with x-ray machine Tanka at P3KRBIN-Batan for 40 kVp to 119 kVp of potential found of Aluminium HVL are 0.115 cm to 0.385 cm and energy effective between 23.24 keV to 37.5 keV

Development of Compton X-ray spectrometer for high energy resolution single-shot high-flux hard X-ray spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Kojima, Sadaoki, E-mail: kojima-s@ile.osaka-u.ac.jp, E-mail: sfujioka@ile.osaka-u.ac.jp; Ikenouchi, Takahito; Arikawa, Yasunobu; Sakata, Shohei; Zhang, Zhe; Abe, Yuki; Nakai, Mitsuo; Nishimura, Hiroaki; Shiraga, Hiroyuki; Fujioka, Shinsuke, E-mail: kojima-s@ile.osaka-u.ac.jp, E-mail: sfujioka@ile.osaka-u.ac.jp; Azechi, Hiroshi [Institute of Laser Engineering, Osaka University, 2-6 Yamada-oka, Suita, Osaka 565-0871 (Japan); Ozaki, Tetsuo [National Institute for Fusion Science, 322-6 Oroshi, Toki, Gifu 509-5292 (Japan); Miyamoto, Shuji; Yamaguchi, Masashi; Takemoto, Akinori [Laboratory of Advanced Science and Technology for Industry, University of Hyogo, 3-1-2 Kouto, Kamigori-cho, Ako-gun, Hyogo 678-1205 (Japan)

2016-04-15

Hard X-ray spectroscopy is an essential diagnostics used to understand physical processes that take place in high energy density plasmas produced by intense laser-plasma interactions. A bundle of hard X-ray detectors, of which the responses have different energy thresholds, is used as a conventional single-shot spectrometer for high-flux (>10{sup 13} photons/shot) hard X-rays. However, high energy resolution (Δhv/hv < 0.1) is not achievable with a differential energy threshold (DET) X-ray spectrometer because its energy resolution is limited by energy differences between the response thresholds. Experimental demonstration of a Compton X-ray spectrometer has already been performed for obtaining higher energy resolution than that of DET spectrometers. In this paper, we describe design details of the Compton X-ray spectrometer, especially dependence of energy resolution and absolute response on photon-electron converter design and its background reduction scheme, and also its application to the laser-plasma interaction experiment. The developed spectrometer was used for spectroscopy of bremsstrahlung X-rays generated by intense laser-plasma interactions using a 200 μm thickness SiO{sub 2} converter. The X-ray spectrum obtained with the Compton X-ray spectrometer is consistent with that obtained with a DET X-ray spectrometer, furthermore higher certainly of a spectral intensity is obtained with the Compton X-ray spectrometer than that with the DET X-ray spectrometer in the photon energy range above 5 MeV.

Instrument for x-ray absorption spectroscopy with in situ electrical control characterizations

International Nuclear Information System (INIS)

Huang, Chun-Chao; Chang, Shu-Jui; Yang, Chao-Yao; Tseng, Yuan-Chieh; Chou, Hsiung

2013-01-01

We report a synchrotron-based setup capable of performing x-ray absorption spectroscopy and x-ray magnetic circular dichroism with simultaneous electrical control characterizations. The setup can enable research concerning electrical transport, element- and orbital-selective magnetization with an in situ fashion. It is a unique approach to the real-time change of spin-polarized electronic state of a material/device exhibiting magneto-electric responses. The performance of the setup was tested by probing the spin-polarized states of cobalt and oxygen of Zn 1-x Co x O dilute magnetic semiconductor under applied voltages, both at low (∼20 K) and room temperatures, and signal variations upon the change of applied voltage were clearly detected

Debris of potassium–magnesium silicate glass generated by femtosecond laser-induced ablation in air: An analysis by near edge X-ray absorption spectroscopy, micro Raman and energy dispersive X-ray spectroscopy

International Nuclear Information System (INIS)

Grehn, M.; Seuthe, T.; Reinhardt, F.; Höfner, M.; Griga, N.; Eberstein, M.; Bonse, J.

2014-01-01

The redeposited material (debris) resulting from ablation of a potassium–magnesium silicate glass upon scanning femtosecond laser pulse irradiation (130 fs, 800 nm) in air environment is investigated by means of three complementary surface analytical methods. Changes in the electronic band structure of the glass constituent Magnesium (Mg) were identified by X-ray Absorption Near Edge Structure spectroscopy (XANES) using synchrotron radiation. An up-shift of ≈0.8 eV of a specific Magnesium K-edge absorption peak in the spectrum of the redeposited material along with a significant change in its leading edge position was detected. In contrast, the surface left after laser ablation exhibits a downshift of the peak position by ≈0.9 eV. Both observations may be related to a change of the Mg coordinative state of the laser modified/redeposited glass material. The presence of carbon in the debris is revealed by micro Raman spectroscopy (μ-RS) and was confirmed by energy dispersive X-ray spectroscopy (EDX). These observations are attributed to structural changes and chemical reactions taking place during the ablation process.

Evaluation of the composition of filters additional of equipment radiological intraoral by energy dispersive x-ray fluorescence (EDXRF)

International Nuclear Information System (INIS)

Franca, Alana Caroline; Torres, Catarina A.M.P.; Rocha, Ana S.S.; Deniak, Valeriy; Lara, Alessandro L.; Paschuk, Sergei A.; Fernandes, Angela; Westphalen, Fernando Henrique

2013-01-01

The need for high quality standards for radiographic images in order to make a diagnosis assertive, and being the additional filtration required in the intraoral X-ray equipment show the need of evaluating these filters. This study aims to examine the influence of the elemental composition of the filters of X-ray of dental intraoral equipment in the radiographic images quality. The filters analysis were performed by using the energy dispersive X-ray fluorescence method (EDXRF). Ten conventional filters were analysed. In this study, 33 radiographic exposures were performed using films: twenty radiographs in the incisor region and ten in the molar region, three exposures were also made in the same regions with same conditions without using filter. After radiographs development, optical density was measure and all radiographs were submitted to subjective evaluation by dental radiologists. Data obtained were correlated to effects evaluation of the elemental composition of all filters in the quality of the radiographic images. The elements found were: aluminum, cobalt, copper, sulfur, iron, manganese, titanium, zinc, and zirconium. The images obtained were identified in groups: Molars to 0.3 s; Incisors to 0.2 s; Incisors to 0.3 s, and for the group without filters. From the results obtained it was concluded that both unclear radiographs and ideal radiographs were produced by using filters of elementary common. Therefore, conventional filters evaluated were an acceptable option to produce quality images in dental radiology, despite differences in the composition of the alloys. (author)

Evaluation of the composition of filters additional of equipment radiological intraoral by energy dispersive x-ray fluorescence (EDXRF)

Energy Technology Data Exchange (ETDEWEB)

Franca, Alana Caroline; Torres, Catarina A.M.P.; Rocha, Ana S.S.; Deniak, Valeriy; Lara, Alessandro L.; Paschuk, Sergei A., E-mail: alanacarolinef@gmail.com, E-mail: sergei@utfpr.edu.br [Universidade Tecnologica Federal do Parana (CPGEI/UTFPR), Curitiba, PR (Brazil). Programa de Pos-Graduacao em Engenharia Eletrica e Informatica Industrial; Fernandes, Angela; Westphalen, Fernando Henrique, E-mail: angelafernandes@ufpr.br [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Setor de Ciencias da Saude

2013-07-01

The need for high quality standards for radiographic images in order to make a diagnosis assertive, and being the additional filtration required in the intraoral X-ray equipment show the need of evaluating these filters. This study aims to examine the influence of the elemental composition of the filters of X-ray of dental intraoral equipment in the radiographic images quality. The filters analysis were performed by using the energy dispersive X-ray fluorescence method (EDXRF). Ten conventional filters were analysed. In this study, 33 radiographic exposures were performed using films: twenty radiographs in the incisor region and ten in the molar region, three exposures were also made in the same regions with same conditions without using filter. After radiographs development, optical density was measure and all radiographs were submitted to subjective evaluation by dental radiologists. Data obtained were correlated to effects evaluation of the elemental composition of all filters in the quality of the radiographic images. The elements found were: aluminum, cobalt, copper, sulfur, iron, manganese, titanium, zinc, and zirconium. The images obtained were identified in groups: Molars to 0.3 s; Incisors to 0.2 s; Incisors to 0.3 s, and for the group without filters. From the results obtained it was concluded that both unclear radiographs and ideal radiographs were produced by using filters of elementary common. Therefore, conventional filters evaluated were an acceptable option to produce quality images in dental radiology, despite differences in the composition of the alloys. (author)

Determination of multi-element profiles of soil using energy dispersive X-ray fluorescence (EDXRF)

International Nuclear Information System (INIS)

Yu, K.N.; Yeung, Z.L.L.; Lee, L.Y.L.; Stokes, M.J.; Kwok, R.C.W.

2002-01-01

The source profile for soil in Hong Kong is important both for determination of the main air pollutant source in Hong Kong and for assessment of the impact of Asian dust storms on Hong Kong. Soil associated with different rock types have been sampled, and the concentrations of 19 chemical elements, Na, Al, Si, Ti, V, Cr, Mn, Fe, Co, K, Ca, Ni, Cu, Zn, Pb, Rb, Sr, Y and Zr, have been determined using energy dispersive X-ray fluorescence. A profile for the average soil for Hong Kong has been determined by taking average values for the different soil categories. The values for the Hong Kong soil are commensurate with values for rural soil derived by other workers, except that Hong Kong soil has much lower Fe and Ca concentrations. The abundance of Al, Ca and Fe in the average Hong Kong soil are 9.23%, 0.11% and 0.85%. We conclude that Ca provides a good marker element for identifying dust episodes in Hong Kong while Al does not

Two-dimensional in situ metrology of X-ray mirrors using the speckle scanning technique

Energy Technology Data Exchange (ETDEWEB)

Wang, Hongchang, E-mail: hongchang.wang@diamond.ac.uk; Kashyap, Yogesh; Laundy, David; Sawhney, Kawal [Diamond Light Source Ltd, Harwell Science and Innovation Campus, Didcot OX11 0DE (United Kingdom)

2015-06-06

The two-dimensional slope error of an X-ray mirror has been retrieved by employing the speckle scanning technique, which will be valuable at synchrotron radiation facilities and in astronomical telescopes. In situ metrology overcomes many of the limitations of existing metrology techniques and is capable of exceeding the performance of present-day optics. A novel technique for precisely characterizing an X-ray bimorph mirror and deducing its two-dimensional (2D) slope error map is presented. This technique has also been used to perform fast optimization of a bimorph mirror using the derived 2D piezo response functions. The measured focused beam size was significantly reduced after the optimization, and the slope error map was then verified by using geometrical optics to simulate the focused beam profile. This proposed technique is expected to be valuable for in situ metrology of X-ray mirrors at synchrotron radiation facilities and in astronomical telescopes.

Wavelength Dispersive X-ray Fluorescence Spectrometry for the Analysis of Organic Polymer Film

International Nuclear Information System (INIS)

Choi, Yong Suk; Park, Yong Joon; Kim, Jong Yun

2008-01-01

Recently, many studies have been focused on the thin films because there are numerous industrial processes relevant to thin films such as fuel cells, sensors, lubricants, coatings, and so on. Physical and chemical properties of solid surface have been modified by ultra-thin coatings such as Langmuir-Blodgett (LB) method with a variety of types of organic functional materials for the specific purposes in many applications. In addition, the layer-by-layer technique using polyelectrolyte films are now of interest as biosensors, electrochromic and electroluminescent devices, etc. In general, several methods such as X-ray or neutron reflectivity, and quartz crystal microbalance (QCM) have been utilized for the thin film analysis. These optical techniques can measure the film thicknesses up to hundreds of nanometers while X-ray photoelectron spectroscopy is widely used to study a few nanometers thick films. Other methods such as X-ray Photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and atom force microscopy (AFM) have also been used in the film analysis in spite of some disadvantages for each method. X-ray fluorescence (XRF) has long been used as a rapid and simple analytical tool for the analysis of elemental composition of materials. XRF technique is suitable for on-line or in-line real-time monitoring because it is a non-destructive and rapid analysis with good precision and good accuracy at low cost. The aim of this work is to develop a new analytical technique for the quantitative analysis of polymer film on metal substrate. In the present study, Compton peak profile was investigated under different experimental conditions by using wavelength-dispersive XRF (WD-XRF). Compared to energy-dispersive XRF (ED-XRF), WD-XRF is more adequate in an accurate quantitative analysis of thin organic film

Study of trace element correlations with drought tolerance in different sorghum genotypes using Energy Dispersive X-Rays Fluorescence (EDXRF) technique

International Nuclear Information System (INIS)

Abu Assar, A.H.; Joseph, Daisy; Choudhury, R.K.; Saxena, A.; Suprasanna, P.; Bapat, V.A.

2000-01-01

Drought tolerant and susceptible genotypes of sorghum plants were analysed by Energy Dispersive X-Ray Fluorescence (EDXRF) technique to study the correlation of trace elements with drought tolerance capacities for sorghum plants. Samples prepared from mature seeds, young seedlings and old plants were analyzed using 109 Cd radioisotope source and a Si(Li) semiconductor detector of resolution 170 eV for 5.9 keV Mn K α X-ray. The elements such as K, Fe, Cu, Zn, Rb and Sr and Y were seen to be present in varying concentrations in different samples. The trace element profile in the seeds of 11 genotypes and in seedlings (young and old) of four sorghum genotypes that were studied exhibited considerable variation in their concentrations. Some seed genotypes showed the presence of Hg in small amounts. It was observed that in most of the genotypes (seeds), K and Fe concentrations were more in the tolerant genotype as compared to the susceptible type. Concentration of Fe decreased with maturity in the tolerant group while it increased with maturity in the susceptible group. The genotype Arfa Gadamak (AG) showed a distinct abnormality in its young seedling with high level of Zn. (author)

Analysis of ancient masterly pieces of work by means of X-ray fluorescence analysis by dispersion in the energy

International Nuclear Information System (INIS)

Cesareo, R.; Cappio B, C.; Brunetti, A.; Rosales, M.A.; Castellano, A.; Gigante, G.E.; Fiorini, C.

2004-01-01

Energy dispersive X-ray fluorescence (EDXRF) analysis has been widely used for the analysis of works of art because it is non-destructive, multi-elemental, simple to utilize, and relatively inexpensive. In the last few years, miniaturized and portable X-ray tubes and high-resolution semiconductor detectors have been developed. This progress allowed the design and construction of portable equipments that can be easily transported all over the world, for use in museums, excavations, etc. In this work, these portable systems will be described and their usefulness demonstrated in the analysis of objects of archaeological value. First, we present the analysis of a lot of gold prehispanic jewels from the Museo del Templo Mayor in Mexico City; in the second place we present the results of analysis of the golden altar of St. Ambrogio in Milan, which is considered one of the most important goldsmith's works ever realized and the gold pigments from the fresco 'The chapel of the Scrovegni' by Giotto. In the third place we give a brief account of Mycenaean and pre-Mycenaean gold objects from the Museum Benaki in Athens. Finally, the results of bulk nuragic copper based ingots from the nuragic village of St. Imbenia are presented. (Author) 19 refs., 5 tabs., 8 figs

Semiconductor detectors in current energy dispersive X-ray spectral analysis

Energy Technology Data Exchange (ETDEWEB)

Betin, J; Zhabin, E; Krampit, I; Smirnov, V

1980-04-01

A review is presented of the properties of semiconductor detectors and of the possibilities stemming therefrom of using the detectors in X-ray spectral analysis in industries, in logging, in ecology and environmental control, in medicine, etc.

Pre-Columbian alloys from the royal tombs of Sipán; energy dispersive X-ray fluorescence analysis with a portable equipment.

Science.gov (United States)

Cesareo, R; Calza, C; Dos Anjos, M; Lopes, R T; Bustamante, A; Fabian S, J; Alva, W; Chero Z, L

2010-01-01

On the north coast of present-day Peru flourished approximately between 50 and 700 AD, the Moche civilization. It was an advanced culture and the Moche were sophisticated metalsmiths, so that they are considered as the finest producers of jewels and artefacts of the region. The Moche metalworking ability was impressively demonstrated by the objects discovered by Walter Alva and coworkers in 1987, in the excavations of the "Tumbas Reales de Sipán". About 50 metal objects from these excavations, now at the namesake Museum, in Lambayeque, north of Peru, were analyzed with a portable equipment using energy-dispersive X-ray fluorescence. This portable equipment is mainly composed of a small size X-ray tube and a thermoelectrically cooled X-ray detector. Standard samples of gold and silver alloys were employed for quantitative analysis. It was determined that the analyzed artefacts from the "Tumbas Reales de Sipán" are mainly composed of gold, silver and copper alloys, of gilded copper and of tumbaga, the last being a poor gold alloy enriched at the surface by depletion gilding, i.e. removing copper from the surface. Copyright 2009 Elsevier Ltd. All rights reserved.

Standard test methods for chemical analysis of ceramic whiteware materials using wavelength dispersive X-Ray fluorescence spectrometry

CERN Document Server

American Society for Testing and Materials. Philadelphia

2004-01-01

1.1 These test methods cover the determination of ten major elements (SiO2, Al2O3, Fe2O3, MgO, CaO, Na2O, K2O, TiO2, P2O5, MnO, and LOI in ceramic whitewares clays and minerals using wavelength dispersive X-ray fluorescence spectrometry (WDXRF). The sample is first ignited, then fused with lithium tetraborate and the resultant glass disc is introduced into a wavelength dispersive X-ray spectrometer. The disc is irradiated with X-rays from an X-ray tube. X-ray photons emitted by the elements in the samples are counted and concentrations determined using previously prepared calibration standards. (1) In addition to 10 major elements, the method provides a gravimetric loss-on-ignition. Note 1—Much of the text of this test method is derived directly from Major element analysis by wavelength dispersive X-ray fluorescence spectrometry, included in Ref (1). 1.2 Interferences, with analysis by WDXRF, may result from mineralogical or other structural effects, line overlaps, and matrix effects. The structure of the...

Sodium lauryl sulfate enhances nickel penetration through guinea-pig skin. Studies with energy dispersive X-ray microanalysis

International Nuclear Information System (INIS)

Lindberg, M.; Sagstroem, S.R.; Roomans, G.M.; Forslind, B.

1989-01-01

The effect of sodium lauryl sulphate (SLS), a common ingredient of detergents, on the penetration of nickel through the stratum corneum in the guinea-pig skin model was studied with energy dispersive X-ray microanalysis (EDX) to evaluate the barrier-damaging properties of this common detergent. The EDX technique allows a simultaneous determination of physiologically important elements, e.g., Na, Mg, P, Cl, K, Ca and S in addition to Ni at each point of measurement in epidermal cell strata. Our results show that SLS reduces the barrier function to Ni-ion penetration of the stratum corneum. In addition we have shown that EDX allows analysis of the influence of different factors involved in nickel penetration through the skin by giving data on the physiological effects on the epidermal cells caused by the applied substances

Semiconductor detectors in current energy dispersive X-ray spectral analysis

International Nuclear Information System (INIS)

Betin, J.; Zhabin, E.; Krampit, I.; Smirnov, V.

1980-01-01

A review is presented of the properties of semiconductor detectors and of the possibilities stemming therefrom of using the detectors in X-ray spectral analysis in industries, in logging, in ecology and environmental control, in medicine, etc. (M.S.)

Studying fatigue damage evolution in uni-directional composites using x-ray computed tomography

DEFF Research Database (Denmark)

Mikkelsen, Lars Pilgaard

, it will be possible to lower the costs of energy for wind energy based electricity. In the present work, a lab-source x-ray computed tomography equipment (Zeiss Xradia 520 Versa) has been used in connection with ex-situ fatigue testing of uni-directional composites in order to identify fibre failure during...... comparable x-ray studies) have been used in order to ensure a representative test volume during the ex-situ fatigue testing. Using the ability of the x-ray computed tomography to zoom into regions of interest, non-destructive, the fatigue damage evolution in a repeating ex-situ fatigue loaded test sample has...... improving the fatigue resistance of non-crimp fabric used in the wind turbine industry can be made....

X-ray spectroscopy and X-ray crystallography of metalloenzymes at XFELs

International Nuclear Information System (INIS)

Yano, Junko

2016-01-01

The ultra-bright femtosecond X-ray pulses provided by X-ray Free Electron Lasers (XFELs) open capabilities for studying the structure and dynamics of a wide variety of biological and inorganic systems beyond what is possible at synchrotron sources. Although the structure and chemistry at the catalytic sites have been studied intensively in both biological and inorganic systems, a full understanding of the atomic-scale chemistry requires new approaches beyond the steady state X-ray crystallography and X-ray spectroscopy at cryogenic temperatures. Following the dynamic changes in the geometric and electronic structure at ambient conditions, while overcoming X-ray damage to the redox active catalytic center, is key for deriving reaction mechanisms. Such studies become possible by using the intense and ultra-short femtosecond X-ray pulses from an XFEL, where sample is probed before it is damaged. We have developed methodology for simultaneously collecting crystallography data and X-ray emission spectra, using an energy dispersive spectrometer at ambient conditions. In addition, we have developed a way to collect metal L-edge data of dilute samples using soft X-rays at XFELs. The advantages and challenges of these methods will be described in this review. (author)

Soft X-ray radiation damage in EM-CCDs used for Resonant Inelastic X-ray Scattering

Science.gov (United States)

Gopinath, D.; Soman, M.; Holland, A.; Keelan, J.; Hall, D.; Holland, K.; Colebrook, D.

2018-02-01

Advancement in synchrotron and free electron laser facilities means that X-ray beams with higher intensity than ever before are being created. The high brilliance of the X-ray beam, as well as the ability to use a range of X-ray energies, means that they can be used in a wide range of applications. One such application is Resonant Inelastic X-ray Scattering (RIXS). RIXS uses the intense and tuneable X-ray beams in order to investigate the electronic structure of materials. The photons are focused onto a sample material and the scattered X-ray beam is diffracted off a high resolution grating to disperse the X-ray energies onto a position sensitive detector. Whilst several factors affect the total system energy resolution, the performance of RIXS experiments can be limited by the spatial resolution of the detector used. Electron-Multiplying CCDs (EM-CCDs) at high gain in combination with centroiding of the photon charge cloud across several detector pixels can lead to sub-pixel spatial resolution of 2-3 μm. X-ray radiation can cause damage to CCDs through ionisation damage resulting in increases in dark current and/or a shift in flat band voltage. Understanding the effect of radiation damage on EM-CCDs is important in order to predict lifetime as well as the change in performance over time. Two CCD-97s were taken to PTB at BESSY II and irradiated with large doses of soft X-rays in order to probe the front and back surfaces of the device. The dark current was shown to decay over time with two different exponential components to it. This paper will discuss the use of EM-CCDs for readout of RIXS spectrometers, and limitations on spatial resolution, together with any limitations on instrument use which may arise from X-ray-induced radiation damage.

Uranium oxidation kinetics monitored by in-situ X-ray diffraction

Energy Technology Data Exchange (ETDEWEB)

Zalkind, S., E-mail: shimonzl@nrcn.org.il; Rafailov, G.; Halevy, I.; Livneh, T.; Rubin, A.; Maimon, H.; Schweke, D.

2017-03-15

The oxidation kinetics of U-0.1 wt%Cr at oxygen pressures of 150 Torr and the temperature range of 90–150 °C was studied by means of in-situ X-ray diffraction (XRD). A “breakaway” in the oxidation kinetics is found at ∼0.25 μm, turning from a parabolic to a linear rate law. At the initial stage of oxidation the growth plane of UO{sub 2}(111) is the prominent one. As the oxide thickens, the growth rate of UO{sub 2}(220) plane increases and both planes grow concurrently. The activation energies obtained for the oxide growth are Q{sub parabolic} = 17.5 kcal/mol and Q{sub linear} = 19 kcal/mol. Enhanced oxidation around uranium carbide (UC) inclusions is clearly observed by scanning electron microscopy (SEM).

Apparatus development for high-pressure X-ray diffraction using synchrotron radiation

International Nuclear Information System (INIS)

Martinez, L.G.; Orlando, M.T.D.; Rossi, J.L.; Passamai Junior, J.L.; Melo, F.C.L.; Ferreira, F.F.

2006-01-01

Some phenomena in the field of condensed matter physics can be studied when the matter is submitted to extreme conditions of pressure, magnetic fields or temperatures. Once submitted to these conditions it is generally necessary to measure the properties of the matter in situ. The existence of a synchrotron light laboratory in Brazil opens up the chance of studying materials in extreme conditions by techniques like X-ray diffraction and absorption. However, when compared to high-energy synchrotrons accelerators, the Brazilian source offers a narrower energy range and lower flux. These facts impose limitation to perform diffraction experiments by energy dispersion and, consequently, the use of pressure cells with denser anvils like diamond. However, for a lower-pressure range, preliminary studies showed the viability of measurements in an angular dispersion configuration. This allows the use of silicon carbide anvils B 4C . In this work it is described the development of a hydrostatic pressure cell suitable for X-rays diffraction measurements in the Brazilian Synchrotron Light Laboratory using materials and technologies developed by the institutions and researchers involved in this project (IPEN, UFES, CTA and LNLS). This development can provide the scientific community with the possibility of performing X-ray diffraction measurements under hydrostatic pressure, initially up to 2 GPa, with possibilities of increasing the maximum pressure to higher values, with or without application of magnetic fields and high or low temperatures. (author)

Excitation methods for energy dispersive analysis

International Nuclear Information System (INIS)

Jaklevic, J.M.

1976-01-01

The rapid development in recent years of energy dispersive x-ray fluorescence analysis has been based primarily on improvements in semiconductor detector x-ray spectrometers. However, the whole analysis system performance is critically dependent on the availability of optimum methods of excitation for the characteristic x rays in specimens. A number of analysis facilities based on various methods of excitation have been developed over the past few years. A discussion is given of the features of various excitation methods including charged particles, monochromatic photons, and broad-energy band photons. The effects of the excitation method on background and sensitivity are discussed from both theoretical and experimental viewpoints. Recent developments such as pulsed excitation and polarized photons are also discussed

Comparison of in situ polymerization and solution-dispersion techniques in the preparation of Polyimide/Montmorillonite (MMT) Nanocomposites.

Science.gov (United States)

Ahmad, Mansor Bin; Gharayebi, Yadollah; Salit, Mohd Sapuan; Hussein, Mohd Zobir; Shameli, Kamyar

2011-01-01

In this paper, Polyimide/Montmorillonite Nanocomposites (PI/MMT NCs), based on aromatic diamine (4-Aminophenyl sulfone) (APS) and aromatic dianhydride (3,3',4,4'-benzophenonetetracarboxylic dianhydride) (BTDA) were prepared using in situ polymerization and solution-dispersion techniques. The prepared PI/MMT NCs films were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). The XRD results showed that at the content of 1.0 wt % Organo Montmorillonite (OMMT) for two techniques and 3.0 wt % OMMT for the in situ polymerization technique, the OMMT was well-intercalated, exfoliated and dispersed into polyimide matrix. The OMMT agglomerated when its amount exceeded 10 wt % and 3.0 wt % for solution-dispersion and in situ polymerization techniques respectively. These results were confirmed by the TEM images of the prepared PI/MMT NCs. The TGA thermograms indicated that thermal stability of prepared PI/MMT NCs were increased with the increase of loading that, the effect is higher for the samples prepared by in situ polymerization technique.

Synchrotron radiation microbeam X-ray fluorescence analysis of zinc concentration in remineralized enamel in situ.

Science.gov (United States)

Matsunaga, Tsunenori; Ishizaki, Hidetaka; Tanabe, Shuji; Hayashi, Yoshihiko

2009-05-01

Remineralization is an indispensable phenomenon during the natural healing process of enamel decay. The incorporation of zinc (Zn) into enamel crystal could accelerate this remineralization. The present study was designed to investigate the concentration and distribution of Zn in remineralized enamel after gum chewing. The experiment was performed at the Photon Factory. Synchrotron radiation was monochromatized and X-rays were focused into a small beam spot. The X-ray fluorescence (XRF) from the sample was detected with a silicon (Si) (lithium (Li)) detector. X-ray beam energy was tuned to detect Zn. The examined samples were small enamel fragments remineralized after chewing calcium phosphate-containing gum in situ. The incorporation of Zn atom into hydroxyapatite (OHAP), the main component of enamel, was measured using Zn K-edge extended X-ray absorption fine structure (EXAFS) with fluorescence mode at the SPring-8. A high concentration of Zn was detected in a superficial area 10-microm deep of the sectioned enamel after gum chewing. This concentration increased over that in the intact enamel. The atomic distance between Zn and O in the enamel was calculated using the EXAFS data. The analyzed atomic distances between Zn and O in two sections were 0.237 and 0.240 nm. The present experiments suggest that Zn is effectively incorporated into remineralized enamel through the physiological processes of mineral deposition in the oral cavity through gum-chewing and that Zn substitution probably occurred at the calcium position in enamel hydroxyapatite.

Two-energy twin image removal in atomic-resolution x-ray holography

International Nuclear Information System (INIS)

Nishino, Y.; Ishikawa, T.; Hayashi, K.; Takahashi, Y.; Matsubara, E.

2002-01-01

We propose a two-energy twin image removal algorithm for atomic-resolution x-ray holography. The validity of the algorithm is shown in a theoretical simulation and in an experiment of internal detector x-ray holography using a ZnSe single crystal. The algorithm, compared to the widely used multiple-energy algorithm, allows efficient measurement of holograms, and is especially important when the available x-ray energies are fixed. It enables twin image free holography using characteristic x rays from laboratory generators and x-ray pulses of free-electron lasers

In situ X-ray diffraction studies on the piezoelectric response of PZT thin films

Energy Technology Data Exchange (ETDEWEB)

Davydok, A., E-mail: davydok@mpie.de [Aix Marseille Université, CNRS, Université de Toulon, IM2NP UMR 7334, 13397 Marseille (France); Max-Planck-Institut für Eisenforschung, Department Structure and Nano-/Micromechanics of Materials, D-40237 Düsseldorf (Germany); Cornelius, T.W. [Aix Marseille Université, CNRS, Université de Toulon, IM2NP UMR 7334, 13397 Marseille (France); Mocuta, C. [SOLEIL Synchrotron, DiffAbs beamline, L' Orme des Merisiers, Saint-Aubin - BP 48, 91192 Gif-sur-Yvette Cedex (France); Lima, E.C. [Universidade Federal do Tocantins, 77500-000 Porto Nacional, TO (Brazil); Araujo, E.B. [Departamento de Fisica e Quimica, Universidade Estadual Paulista, Av. Brasil, 56 Centro, 15385-000 Ilha Solteira, SP (Brazil); Thomas, O. [Aix Marseille Université, CNRS, Université de Toulon, IM2NP UMR 7334, 13397 Marseille (France)

2016-03-31

Piezoelectric properties of randomly oriented self-polarized PbZr{sub 0.50}Ti{sub 0.50}O{sub 3} (PZT) thin films were investigated using in situ synchrotron X-ray diffraction. Possibilities for investigating the piezoelectric effect using micro-sized hard X-ray beams are demonstrated and perspectives for future dynamical measurements on PZT samples with variety of compositions and thicknesses are given. Studies performed on the crystalline [100, 110] directions evidenced piezoelectric anisotropy. The piezoelectric coefficient d{sub 33} was calculated in terms of the lab reference frame (d{sub perp}) and found to be two times larger along the [100] direction than along the [110] direction. The absolute values for the d{sub perp} amount to 120 and 230 pm/V being in good agreement with experimental and theoretical values found in literature for bulk PZT ceramics. - Highlights: • We performed in situ synchrotron X-ray diffraction studies on (PZT) thin films. • We discuss anisotropy of piezo effect in different crystallographic directions. • Perpendicular component Piezo coefficient of thin PZT layer is defined.

Structural and microstructural changes during anion exchange of CoAl layered double hydroxides. An in situ X-ray powder diffraction study

International Nuclear Information System (INIS)

Johnsen, Rune E.; Krumeich, Frank; Norby, Poul

2010-01-01

Anion-exchange processes in cobalt-aluminium layered double hydroxides (LDHs) were studied by in situ synchrotron X-ray powder diffraction (XRPD). The processes investigated were CoAl-CO 3 →CoAl-Cl →CoAl-CO 3 , CoAl-Cl→CoAl-NO 3 and CoAl-CO 3 →CoAl-SO 4 . The XRPD data show that the CoAl-CO 3 →CoAl-Cl process is a two-phase transformation, where the amount of the CoAl-CO 3 phase decreases exponentially while that of the CoAl-Cl phase increases exponentially. Energy-dispersive X-ray spectroscopy (EDXS) studies of a partially chloride-exchanged CoAl-CO 3 LDH sample along with in situ XRPD data suggested that the individual particles in the CoAl-CO 3 sample are generally anion-exchanged with chloride one at a time. In contrast with the CoAl-CO 3 →CoAl-Cl transformation, the XRPD data show that the reverse CoAl-Cl→CoAl-CO 3 process is a one-phase transformation. Rietveld refinements indicate that the occupancy factors of the carbon and oxygen sites of the carbonate group increase, while that of the chloride site decreases. In the CoAl-Cl→CoAl-NO 3 anion-exchange reaction, the XRPD patterns reveal the existence of two intermediate phases in addition to the initial CoAl-Cl and final CoAl-NO 3 phases. The in situ data indicate that one of these intermediates is a mixed nitrate- and chloride-based LDH phase, where the disorder decreases as the nitrate content increases. The XRPD data of the partial CoAl-CO 3 →CoAl-SO 4 anion-exchange reaction show that the process is a two-phase transformation involving a sulfate-containing LDH with a 1H polytype structure. (orig.)

Nanocalorimeter platform for in situ specific heat measurements and x-ray diffraction at low temperature

Science.gov (United States)

Willa, K.; Diao, Z.; Campanini, D.; Welp, U.; Divan, R.; Hudl, M.; Islam, Z.; Kwok, W.-K.; Rydh, A.

2017-12-01

Recent advances in electronics and nanofabrication have enabled membrane-based nanocalorimetry for measurements of the specific heat of microgram-sized samples. We have integrated a nanocalorimeter platform into a 4.5 T split-pair vertical-field magnet to allow for the simultaneous measurement of the specific heat and x-ray scattering in magnetic fields and at temperatures as low as 4 K. This multi-modal approach empowers researchers to directly correlate scattering experiments with insights from thermodynamic properties including structural, electronic, orbital, and magnetic phase transitions. The use of a nanocalorimeter sample platform enables numerous technical advantages: precise measurement and control of the sample temperature, quantification of beam heating effects, fast and precise positioning of the sample in the x-ray beam, and fast acquisition of x-ray scans over a wide temperature range without the need for time-consuming re-centering and re-alignment. Furthermore, on an YBa2Cu3O7-δ crystal and a copper foil, we demonstrate a novel approach to x-ray absorption spectroscopy by monitoring the change in sample temperature as a function of incident photon energy. Finally, we illustrate the new insights that can be gained from in situ structural and thermodynamic measurements by investigating the superheated state occurring at the first-order magneto-elastic phase transition of Fe2P, a material that is of interest for magnetocaloric applications.

Low energy (soft) x rays

International Nuclear Information System (INIS)

Hoshi, Masaharu; Antoku, Shigetoshi; Russell, W.J.; Miller, R.C.; Nakamura, Nori; Mizuno, Masayoshi; Nishio, Shoji.

1987-05-01

Dosimetry of low-energy (soft) X rays produced by the SOFTEX Model CMBW-2 was performed using Nuclear Associates Type 30 - 330 PTW, Exradin Type A2, and Shonka-Wyckoff ionization chambers with a Keithley Model 602 electrometer. Thermoluminescent (BeO chip) dosimeters were used with a Harshaw Detector 2000-A and Picoammeter-B readout system. Beam quality measurements were made using aluminum absorbers; exposure rates were assessed by the current of the X-ray tube and by exposure times. Dose distributions were established, and the average factors for non-uniformity were calculated. The means of obtaining accurate absorbed and exposed doses using these methods are discussed. Survival of V79 cells was assessed by irradiating them with soft X rays, 200 kVp X rays, and 60 Co gamma rays. The relative biological effectiveness (RBE) values for soft X rays with 0, 0.2, 0.7 mm added thicknesses of aluminum were 1.6, which were compared to 60 Co. The RBE of 200 kVp X rays relative to 60 Co was 1.3. Results of this study are available for reference in future RERF studies of cell survival. (author)

Bone age assessment by dual-energy X-ray absorptiometry in children: an alternative for X-ray?

Science.gov (United States)

Heppe, D H M; Taal, H R; Ernst, G D S; Van Den Akker, E L T; Lequin, M M H; Hokken-Koelega, A C S; Geelhoed, J J M; Jaddoe, V W V

2012-02-01

The aim of the study was to validate dual-energy X-ray absorptiometry (DXA) as a method to assess bone age in children. Paired dual-energy X-ray absorptiometry (DXA) scans and X-rays of the left hand were performed in 95 children who attended the paediatric endocrinology outpatient clinic of University Hospital Rotterdam, the Netherlands. We compared bone age assessments by DXA scan with those performed by X-ray. Bone age assessment was performed by two blinded observers according to the reference method of Greulich and Pyle. Intra-observer and interobserver reproducibility were investigated using the intraclass correlation coefficient (ICC), and agreement was tested using Bland and Altman plots. The intra-observer ICCs for both observers were 0.997 and 0.991 for X-ray and 0.993 and 0.987 for DXA assessments. The interobserver ICC was 0.993 and 0.991 for X-ray and DXA assessments, respectively. The mean difference between bone age assessed by X-ray and DXA was 0.11 years. The limits of agreement ranged from -0.82 to 1.05 years, which means that 95% of all differences between the methods were covered by this range. Results of bone age assessment by DXA scan are similar to those obtained by X-ray. The DXA method seems to be an alternative for assessing bone age in a paediatric hospital-based population.

Micro energy-dispersive x-ray fluorescence spectrometry study of dentin coating with nanobiomaterials

Science.gov (United States)

Soares, Luís. Eduardo Silva; Nahorny, Sídnei; Marciano, Fernanda Roberta; Zanin, Hudson; Lobo, Anderson de Oliveira

2015-06-01

New biomaterials such as multi-walled carbon nanotubes oxide/graphene oxide (MWCNTO/GO), nanohydroxyapatite (nHAp) and combination of them together or not to acidulated phosphate fluoride gel (F) have been tested as protective coating before root dentin erosion. Fourteen bovine teeth were cleaned, polished, divided into two parts (n=28) and assigned to seven groups: (Control) - without previous surface treatment; F treatment; nHAp; MWCNTO/GO; F+nHAp; F+MWCNTO/GO and F+MWCNTO/GO/nHAp composites. Each sample had two sites of pre-treatments: acid etched area and an area without treatment. After the biomaterials application, the samples were submitted to six cycles (demineralization: orange juice, 10 min; remineralization: artificial saliva, 1 h). Micro energy-dispersive X-ray fluorescence spectrometry (μ-EDXRF) mapping area analyses were performed after erosive cycling on both sites (n=84). μ-EDXRF mappings showed that artificial saliva and MWCNTO/GO/nHAp/F composite treatments produced lower dentin demineralization than in the other groups. Exposed dentin tubules allowed better interaction of nanobiomaterials than in smear layer covered dentin. Association of fluoride with other biomaterials had a positive influence on acid etched dentin. MWCNTO/GO/nHAp/F composite treatment resulted in levels of demineralization similar to the control group.

Custom AFM for X-ray beamlines: in situ biological investigations under physiological conditions

Energy Technology Data Exchange (ETDEWEB)

Gumí-Audenis, B. [ESRF, The European Synchrotron, Grenoble (France); Institute for Bioengineering of Catalonia (IBEC), Barcelona (Spain); Physical Chemistry Department, Universitat de Barcelona, Barcelona (Spain); Networking Biomedical Research Center on Bioengineering, Biomaterials and Nanomedicine (CIBER-BBN), Madrid (Spain); Carlà, F. [ESRF, The European Synchrotron, Grenoble (France); Vitorino, M. V. [University of Lisboa, Falculty of Science, Biosystems and Integrative Sciences Institute - BIOISI, Lisbon (Portugal); Panzarella, A. [ESRF, The European Synchrotron, Grenoble (France); Porcar, L. [Institut Laue-Langevin, Grenoble (France); Boilot, M. [ORTEC, Marseille (France); Guerber, S. [CEA, LETI Grenoble (France); Bernard, P. [ESRF, The European Synchrotron, Grenoble (France); Rodrigues, M. S. [University of Lisboa, Falculty of Science, Biosystems and Integrative Sciences Institute - BIOISI, Lisbon (Portugal); Sanz, F.; Giannotti, M. I. [Institute for Bioengineering of Catalonia (IBEC), Barcelona (Spain); Physical Chemistry Department, Universitat de Barcelona, Barcelona (Spain); Networking Biomedical Research Center on Bioengineering, Biomaterials and Nanomedicine (CIBER-BBN), Madrid (Spain); Costa, L., E-mail: luca.costa@esrf.fr [ESRF, The European Synchrotron, Grenoble (France)

2015-09-30

The performance of a custom atomic force microscope for grazing-incidence X-ray experiments on hydrated soft and biological samples is presented. A fast atomic force microscope (AFM) has been developed that can be installed as a sample holder for grazing-incidence X-ray experiments at solid/gas or solid/liquid interfaces. It allows a wide range of possible investigations, including soft and biological samples under physiological conditions (hydrated specimens). The structural information obtained using the X-rays is combined with the data gathered with the AFM (morphology and mechanical properties), providing a unique characterization of the specimen and its dynamics in situ during an experiment. In this work, lipid monolayers and bilayers in air or liquid environment have been investigated by means of AFM, both with imaging and force spectroscopy, and X-ray reflectivity. In addition, this combination allows the radiation damage induced by the beam on the sample to be studied, as has been observed on DOPC and DPPC supported lipid bilayers under physiological conditions.

Wave-dispersive x-ray spectrometer for simultaneous acquisition of several characteristic lines based on strongly and accurately shaped Ge crystal

International Nuclear Information System (INIS)

Hayashi, Kouichi; Nakajima, Kazuo; Fujiwara, Kozo; Nishikata, Susumu

2008-01-01

Si and Ge are widely used as analyzing crystals for x-rays. Drastic and accurate shaping of Si or Ge gives significant advance in the x-ray field, although covalently bonded Si or Ge crystals have long been believed to be not deformable to various shapes. Recently, we developed a deformation technique for obtaining strongly and accurately shaped Si or Ge wafers of high crystal quality, and the use of the deformed wafer made it possible to produce fine-focused x-rays. In the present study, we prepared a cylindrical Ge wafer with a radius of curvature of 50 mm, and acquired fluorescent x-rays simultaneously from four elements by combining the cylindrical Ge wafer with a position-sensitive detector. The energy resolution of the x-ray fluorescence spectrum was as good as that obtained using a flat single crystal, and its gain was over 100. The demonstration of the simultaneous acquisition of high-resolution x-ray fluorescence spectra indicated various possibilities of x-ray spectrometry, such as one-shot x-ray spectroscopy and highly efficient wave-dispersive x-ray spectrometers

Evaluation of an in-situ x-ray fluorescence analyzer for inorganic pollutants in sediments and water columns

International Nuclear Information System (INIS)

Wogman, N.A.

1979-09-01

The applicability of an energy dispersive x-ray fluorescence spectrometer for measurement of trace elements in sediments and in water columns from Coast Guard vessels has been investigated. This investigation was conducted in both freshwater and saltwater areas and included Puget Sound, Lake Washington, Lake Union, and the ship canal in the State of Washington. The spectrometer system consisted of a solid cryogen-cooled Si(Li) detector and a 109 Cd excitation source. Sediments and water columns were viewed through a 0.2 mm Be window. This study showed the feasibility of measuring trace elements at concentrations ranging from 20 to about 100 ppM. Measurements of this sensitivity with a 100 mCi 109 Cd source are possible for time intervals as short as 5 minutes. This in-situ measurement capability permits the on-site mapping of pollution and avoids the problem of sediment disturbance which is inherent in the collection of grab samples of the sediment surface. Recommendations for an improved analyzer system included a detector assembly which could be towed, or allow continuous sediment surface analysis thereby recording the average composition of a large area

Performance of a gaseous detector based energy dispersive X-ray fluorescence imaging system: Analysis of human teeth treated with dental amalgam

Science.gov (United States)

Silva, A. L. M.; Figueroa, R.; Jaramillo, A.; Carvalho, M. L.; Veloso, J. F. C. A.

2013-08-01

Energy dispersive X-ray fluorescence (EDXRF) imaging systems are of great interest in many applications of different areas, once they allow us to get images of the spatial elemental distribution in the samples. The detector system used in this study is based on a micro patterned gas detector, named Micro-Hole and Strip Plate. The full field of view system, with an active area of 28 × 28 mm2 presents some important features for EDXRF imaging applications, such as a position resolution below 125 μm, an intrinsic energy resolution of about 14% full width at half maximum for 5.9 keV X-rays, and a counting rate capability of 0.5 MHz. In this work, analysis of human teeth treated by dental amalgam was performed by using the EDXRF imaging system mentioned above. The goal of the analysis is to evaluate the system capabilities in the biomedical field by measuring the drift of the major constituents of a dental amalgam, Zn and Hg, throughout the tooth structures. The elemental distribution pattern of these elements obtained during the analysis suggests diffusion of these elements from the amalgam to teeth tissues.

Treatment of foods with high-energy X rays

International Nuclear Information System (INIS)

Cleland, M.R.; Meissner, J.; Herer, A.S.; Beers, E.W.

2001-01-01

The treatment of foods with ionizing energy in the form of gamma rays, accelerated electrons, and X rays can produce beneficial effects, such as inhibiting the sprouting in potatoes, onions, and garlic, controlling insects in fruits, vegetables, and grains, inhibiting the growth of fungi, pasteurizing fresh meat, poultry, and seafood, and sterilizing spices and food additives. After many years of research, these processes have been approved by regulatory authorities in many countries and commercial applications have been increasing. High-energy X rays are especially useful for treating large packages of food. The most attractive features are product penetration, absorbed dose uniformity, high utilization efficiency and short processing time. The ability to energize the X-ray source only when needed enhances the safety and convenience of this technique. The availability of high-energy, high-power electron accelerators, which can be used as X-ray generators, makes it feasible to process large quantities of food economically. Several industrial accelerator facilities already have X-ray conversion equipment and several more will soon be built with product conveying systems designed to take advantage of the unique characteristics of high-energy X rays. These concepts will be reviewed briefly in this paper

Treatment of foods with high-energy X rays

Science.gov (United States)

Cleland, M. R.; Meissner, J.; Herer, A. S.; Beers, E. W.

2001-07-01

The treatment of foods with ionizing energy in the form of gamma rays, accelerated electrons, and X rays can produce beneficial effects, such as inhibiting the sprouting in potatoes, onions, and garlic, controlling insects in fruits, vegetables, and grains, inhibiting the growth of fungi, pasteurizing fresh meat, poultry, and seafood, and sterilizing spices and food additives. After many years of research, these processes have been approved by regulatory authorities in many countries and commercial applications have been increasing. High-energy X rays are especially useful for treating large packages of food. The most attractive features are product penetration, absorbed dose uniformity, high utilization efficiency and short processing time. The ability to energize the X-ray source only when needed enhances the safety and convenience of this technique. The availability of high-energy, high-power electron accelerators, which can be used as X-ray generators, makes it feasible to process large quantities of food economically. Several industrial accelerator facilities already have X-ray conversion equipment and several more will soon be built with product conveying systems designed to take advantage of the unique characteristics of high-energy X rays. These concepts will be reviewed briefly in this paper.

Resonant inelastic X-ray spectroscopy of atoms and simple molecules: Satellite features and dependence on energy detuning and photon polarization

Energy Technology Data Exchange (ETDEWEB)

Žitnik, M., E-mail: matjaz.zitnik@ijs.si [Jožef Stefan Institute, P.O. Box 3000, SI-1001 Ljubljana (Slovenia); University of Ljubljana, Faculty of Mathematics and Physics, Jadranska 21, SI-1000 Ljubljana (Slovenia); Kavčič, M.; Bohinc, R.; Bučar, K.; Mihelič, A. [Jožef Stefan Institute, P.O. Box 3000, SI-1001 Ljubljana (Slovenia); Cao, W. [Research Centre for Molecular Materials, University of Oulu, P.O. Box 3000, FIN-90014 Oulu (Finland); Guillemin, R.; Journel, L.; Marchenko, T.; Carniato, S.; Kawerk, E. [Sorbonne Universités, UPMC Univ Paris 06, UMR 7614, Laboratoire de Chimie Physique Matière et Rayonnement, F-75005 Paris (France); CNRS, UMR 7614, Laboratoire de Chimie Physique Matière et Rayonnement, F-75005 Paris (France); Piancastelli, M.N. [Sorbonne Universités, UPMC Univ Paris 06, UMR 7614, Laboratoire de Chimie Physique Matière et Rayonnement, F-75005 Paris (France); CNRS, UMR 7614, Laboratoire de Chimie Physique Matière et Rayonnement, F-75005 Paris (France); Department of Physics and Astronomy, Uppsala University, P.O. Box 516, 75120 Uppsala (Sweden); Simon, M. [Sorbonne Universités, UPMC Univ Paris 06, UMR 7614, Laboratoire de Chimie Physique Matière et Rayonnement, F-75005 Paris (France); CNRS, UMR 7614, Laboratoire de Chimie Physique Matière et Rayonnement, F-75005 Paris (France)

2015-10-15

We summarize recent results dealing with high resolution (resonant) X-ray spectroscopy of atomic and molecular targets in the tender X-ray energy region. We comment on advantages, new possibilities and problems related to RIXS spectroscopy with respect to the standard photoabsorption technique, where scanning the probe energy is the only option. In particular, three research areas are covered: X-ray emission mediated by energy dependent photoabsorption to multi-electron excited states, the Cl K core-hole clock studies exemplified by systematic study of chloro(fluoro)-hydrocarbon targets and the polarization dependent X-ray emission studies. Due to its spectral selectivity and simultaneous detection capability, high resolution wavelength dispersive X-ray spectroscopy has the capability to resolve structural and dynamical properties of matter within new instrumentation frontiers.

Resonant inelastic X-ray spectroscopy of atoms and simple molecules: Satellite features and dependence on energy detuning and photon polarization

International Nuclear Information System (INIS)

Žitnik, M.; Kavčič, M.; Bohinc, R.; Bučar, K.; Mihelič, A.; Cao, W.; Guillemin, R.; Journel, L.; Marchenko, T.; Carniato, S.; Kawerk, E.; Piancastelli, M.N.; Simon, M.

2015-01-01

We summarize recent results dealing with high resolution (resonant) X-ray spectroscopy of atomic and molecular targets in the tender X-ray energy region. We comment on advantages, new possibilities and problems related to RIXS spectroscopy with respect to the standard photoabsorption technique, where scanning the probe energy is the only option. In particular, three research areas are covered: X-ray emission mediated by energy dependent photoabsorption to multi-electron excited states, the Cl K core-hole clock studies exemplified by systematic study of chloro(fluoro)-hydrocarbon targets and the polarization dependent X-ray emission studies. Due to its spectral selectivity and simultaneous detection capability, high resolution wavelength dispersive X-ray spectroscopy has the capability to resolve structural and dynamical properties of matter within new instrumentation frontiers.

In situ laser heating and radial synchrotron X-ray diffraction ina diamond anvil cell

Energy Technology Data Exchange (ETDEWEB)

Kunz, Martin; Caldwell, Wendel A.; Miyagi, Lowell; Wenk,Hans-Rudolf

2007-06-29

We report a first combination of diamond anvil cell radialx-ray diffraction with in situ laser heating. The laser-heating setup ofALS beamline 12.2.2 was modified to allow one-sided heating of a samplein a diamond anvil cell with an 80 W yttrium lithium fluoride laser whileprobing the sample with radial x-ray diffraction. The diamond anvil cellis placed with its compressional axis vertical, and perpendicular to thebeam. The laser beam is focused onto the sample from the top while thesample is probed with hard x-rays through an x-ray transparentboron-epoxy gasket. The temperature response of preferred orientation of(Fe,Mg)O is probed as a test experiment. Recrystallization was observedabove 1500 K, accompanied by a decrease in stress.

High Pressure In Situ X-ray Diffraction Study of MnO to 120 GPa and Comparison with Shock Compression Experiment

Science.gov (United States)

Yagi, Takehiko; Kondo, Tadashi; Syono, Yasuhiko

1997-07-01

In order to clarify the nature of the phase transformation in MnO observed at around 90 GPa by shock compression experiment (Syono et al., this symposium), high pressure in situ x-ray experiments were carried out up to 120 GPa. Powdered sample was directly compressed in Mao-Bell type diamond anvil and x-ray experiments were carried out using angle dispersive technique by combining synchrotron radiation and imaging plate detector. Distortion of the B1 structured phase into hexagonal unit cell was observed from 25-40 GPa, which continues to increase up to 90 GPa. At around 90 GPa, discontinuous change of the diffraction was observed. This new phase cannot be explained by a simple B2 structure and the analysis of this phase is in progress. This high pressure phase has metallic appearance, which reverses to transparent MnO on release of pressure.

Novel micro-reactor flow cell for investigation of model catalysts using in situ grazing-incidence X-ray scattering.

Science.gov (United States)

Kehres, Jan; Pedersen, Thomas; Masini, Federico; Andreasen, Jens Wenzel; Nielsen, Martin Meedom; Diaz, Ana; Nielsen, Jane Hvolbæk; Hansen, Ole; Chorkendorff, Ib

2016-03-01

The design, fabrication and performance of a novel and highly sensitive micro-reactor device for performing in situ grazing-incidence X-ray scattering experiments of model catalyst systems is presented. The design of the reaction chamber, etched in silicon on insulator (SIO), permits grazing-incidence small-angle X-ray scattering (GISAXS) in transmission through 10 µm-thick entrance and exit windows by using micro-focused beams. An additional thinning of the Pyrex glass reactor lid allows simultaneous acquisition of the grazing-incidence wide-angle X-ray scattering (GIWAXS). In situ experiments at synchrotron facilities are performed utilizing the micro-reactor and a designed transportable gas feed and analysis system. The feasibility of simultaneous in situ GISAXS/GIWAXS experiments in the novel micro-reactor flow cell was confirmed with CO oxidation over mass-selected Ru nanoparticles.

Beamline electrostatic levitator for in situ high energy x-ray diffraction studies of levitated solids and liquids

Energy Technology Data Exchange (ETDEWEB)

Gangopadhyay, A.K.; Lee, G.W.; Kelto, K.F.; Rogers, J.R.; Goldman, A.I.; Robinson, D.S.; Rathz, T.J.; Hyers, R.W. (WU); (UAB); (NASA); (UMASS, Amherst)

2010-07-19

Determinations of the phase formation sequence, crystal structures and the thermo-physical properties of materials at high temperatures are hampered by contamination from the sample container and environment. Containerless processing techniques, such as electrostatic (ESL), electromagnetic, aerodynamic, and acoustic levitation, are most suitable for these studies. An adaptation of ESL for in situ structural studies of a wide range of materials using high energy (30-130 keV) x rays at a synchrotron source is described here. This beamline ESL (BESL) allows the in situ determination of the atomic structures of equilibrium solid and liquid phases, undercooled liquids and time-resolved studies of solid-solid and liquid-solid phase transformations. The use of area detectors enables the rapid acquisition of complete diffraction patterns over a wide range (0.5-14 {angstrom}{sup -1}) of reciprocal space. The wide temperature range (300-2500 K), containerless processing environment under high vacuum (10{sup -7}-10{sup -8} Torr), and fast data acquisition capability, make BESL particularly well suited for phase stability studies of high temperature solids and liquids. An additional, but important, feature of BESL is the capability for simultaneous measurements of a host of thermo-physical properties including the specific heat, enthalpy of transformation, solidus and liquidus temperatures, density, viscosity, and surface tension, all on the same sample during the structural measurements.

Micro energy-dispersive X-ray fluoresence mapping of enamel and dental materials after chemical erosion.

Science.gov (United States)

Soares, Luís Eduardo Silva; de Oliveira, Rodrigo; Nahórny, Sídnei; Santo, Ana Maria do Espírito; Martin, Airton Abrahão

2012-10-01

Energy-dispersive X-ray fluorescence was employed to test the hypothesis that beverage consumption or mouthwash utilization will change the chemical properties of dental materials and enamel mineral content. Bovine enamel samples (n = 45) each received two cavity preparations (n = 90), each pair filled with one of three dental materials (R: nanofilled composite resin; GIC: glass-ionomer cement; RMGIC: resin-modified GIC). Furthermore, they were treated with three different solutions (S: saliva; E: erosion/Pepsi Twist®; or EM: erosion+mouthwash/Colgate Plax®). It was found that mineral loss in enamel was greater in GICE samples than in RE > RMGICE > RMGICEM > REM > GICEM. An increased percentage of Zr was found in REM indicating organic matrix degradation. Dental materials tested (R, GIC, and RMGIC) were not able to protect adjacent enamel from acid erosion by the soft drink tested. The use of mouthwash promoted protection of enamel after erosion by the soft drink. To avoid chemical dissolution by mouthwashes, protection by resin composites with surface sealants is recommended.

Energy-dispersive X-ray fluorescence analysis of traces of heavy metals (Mn, Fe, Co, Ni, Cu, Zn, Ta, Pb, U) in mineral waters after separation on the cellulose-exchanger Hyphan

International Nuclear Information System (INIS)

Burba, P.; Lieser, K.H.

1979-01-01

Trace elements in mineral water are separated in small columns on the cellulose-exchanger Hyphan, eluted by diluted hydrochloric acid, bound on 100 mg of Hyphan by shaking and determined by energy-dispersive X-ray fluorescence. The following heavy metals can be analysed quantitatively if present in water in concentrations >= 1 ppb: Mn, Fe, Co, Ni, Cu, Zn, Ta, Pb and U. Several commercial mineral waters, a sodium chloride spring and seawater were analyzed for trace elements. The results obtained by X-ray fluorescence and by atomic absorption agree within the limits of error. (orig.) [de

Effective absorption correction for energy dispersive X-ray mapping in a scanning transmission electron microscope: analysing the local indium distribution in rough samples of InGaN alloy layers.

Science.gov (United States)

Wang, X; Chauvat, M-P; Ruterana, P; Walther, T

2017-12-01

We have applied our previous method of self-consistent k*-factors for absorption correction in energy-dispersive X-ray spectroscopy to quantify the indium content in X-ray maps of thick compound InGaN layers. The method allows us to quantify the indium concentration without measuring the sample thickness, density or beam current, and works even if there is a drastic local thickness change due to sample roughness or preferential thinning. The method is shown to select, point-by-point in a two-dimensional spectrum image or map, the k*-factor from the local Ga K/L intensity ratio that is most appropriate for the corresponding sample geometry, demonstrating it is not the sample thickness measured along the electron beam direction but the optical path length the X-rays have to travel through the sample that is relevant for the absorption correction. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.

In meso in situ serial X-ray crystallography of soluble and membrane proteins

International Nuclear Information System (INIS)

Huang, Chia-Ying; Olieric, Vincent; Ma, Pikyee; Panepucci, Ezequiel; Diederichs, Kay; Wang, Meitian; Caffrey, Martin

2015-01-01

A method for performing high-throughput in situ serial X-ray crystallography with soluble and membrane proteins in the lipid cubic phase is described. It works with microgram quantities of protein and lipid (and ligand when present) and is compatible with the most demanding sulfur SAD phasing. The lipid cubic phase (LCP) continues to grow in popularity as a medium in which to generate crystals of membrane (and soluble) proteins for high-resolution X-ray crystallographic structure determination. To date, the PDB includes 227 records attributed to the LCP or in meso method. Among the listings are some of the highest profile membrane proteins, including the β 2 -adrenoreceptor–G s protein complex that figured in the award of the 2012 Nobel Prize in Chemistry to Lefkowitz and Kobilka. The most successful in meso protocol to date uses glass sandwich crystallization plates. Despite their many advantages, glass plates are challenging to harvest crystals from. However, performing in situ X-ray diffraction measurements with these plates is not practical. Here, an alternative approach is described that provides many of the advantages of glass plates and is compatible with high-throughput in situ measurements. The novel in meso in situ serial crystallography (IMISX) method introduced here has been demonstrated with AlgE and PepT (alginate and peptide transporters, respectively) as model integral membrane proteins and with lysozyme as a test soluble protein. Structures were solved by molecular replacement and by experimental phasing using bromine SAD and native sulfur SAD methods to resolutions ranging from 1.8 to 2.8 Å using single-digit microgram quantities of protein. That sulfur SAD phasing worked is testament to the exceptional quality of the IMISX diffraction data. The IMISX method is compatible with readily available, inexpensive materials and equipment, is simple to implement and is compatible with high-throughput in situ serial data collection at macromolecular

Simple procedure for nutrient analysis of coffee plant with energy dispersive X-ray fluorescence spectrometry (EDXRF)

Energy Technology Data Exchange (ETDEWEB)

Tezotto, Tiago; Favarin, Jose Laercio; Neto, Ana Paula; Azevedo, Ricardo Antunes, E-mail: tiago.tezotto@usp.br [Escola Superior de Agricultura Luiz de Queiroz (ESALQ/USP), Piracicaba, SP (Brazil); Gratao, Priscila Lupino [Universidade Estadual Paulista Julio de Mesquita Filho (UNESP/ FCAV), Jaboticabal, SP (Brazil). Dept. de Biologia Aplicada a Agropecuaria; Mazzafera, Paulo [Universidade Estadual de Campinas (UNICAMP/IB), SP (Brazil). Dept. Biologia Vegetal

2013-07-15

Nutrient analysis is used to estimate nutrient content of crop plants to manage fertilizer application for sustained crop production. Direct solid analysis of agricultural and environmental samples by energy dispersive X-ray fluorescence spectrometry (EDXRF) was chosen as alternative technique to evaluate the simultaneous multielemental quantification of the most important essential elements in coffee (Coffea arabica L.) plants. Inductively coupled plasma atomic emission spectrometry and certified reference materials made from leaves were used to calibrate and check the trueness of EDXRF method for the determination of the concentration of several nutrients in coffee leaves and branches. Fluorescence spectrometry proved to be advantageous and presented low cost as loose powder samples could be used. Samples collected from a field experiment where coffee plants were treated with excess of Ni and Zn were used to verify the practical application of the method. Good relationships were achieved between certified values and data obtained by EDXRF, with recoveries ranging from 82 to 117 %.(author)

In situ X-ray powder diffraction, synthesis, and magnetic properties of InVO 3

Science.gov (United States)

Lundgren, Rylan J.; Cranswick, Lachlan M. D.; Bieringer, Mario

2006-12-01

We report the first synthesis and high-temperature in situ X-ray diffraction study of InVO 3. Polycrystalline InVO 3 has been prepared via reduction of InVO 4 using a carbon monoxide/carbon dioxide buffer gas. InVO 3 crystallizes in the bixbyite structure in space group Ia-3 (206) with a=9.80636(31) Å with In 3+/V 3+ disorder on the (8 b) and (24 d) cation sites. In situ powder X-ray diffraction experiments and thermal gravimetric analysis in a CO/CO 2 buffer gas revealed the existence of the metastable phase InVO 3. Bulk samples with 98.5(2)% purity were prepared using low-temperature reduction methods. The preparative methods limited the crystallinity of this new phase to approximately 225(50) Å. Magnetic susceptibility and neutron diffraction experiments suggest a spin-glass ground state for InVO 3.

ON NEUTRAL ABSORPTION AND SPECTRAL EVOLUTION IN X-RAY BINARIES

International Nuclear Information System (INIS)

Miller, J. M.; Cackett, E. M.; Reis, R. C.

2009-01-01

Current X-ray observatories make it possible to follow the evolution of transient and variable X-ray binaries across a broad range in luminosity and source behavior. In such studies, it can be unclear whether evolution in the low-energy portion of the spectrum should be attributed to evolution in the source, or instead to evolution in neutral photoelectric absorption. Dispersive spectrometers make it possible to address this problem. We have analyzed a small but diverse set of X-ray binaries observed with the Chandra High Energy Transmission Grating Spectrometer across a range in luminosity and different spectral states. The column density in individual photoelectric absorption edges remains constant with luminosity, both within and across source spectral states. This finding suggests that absorption in the interstellar medium strongly dominates the neutral column density observed in spectra of X-ray binaries. Consequently, evolution in the low-energy spectrum of X-ray binaries should properly be attributed to evolution in the source spectrum. We discuss our results in the context of X-ray binary spectroscopy with current and future X-ray missions.

The color of X-rays: Spectral X-ray computed tomography using energy sensitive pixel detectors

NARCIS (Netherlands)

Schioppa, E.J.

2014-01-01

Energy sensitive X-ray imaging detectors are produced by connecting a semiconductor sensor to a spectroscopic pixel readout chip. In this thesis, the applicability of such detectors to X-ray Computed Tomography (CT) is studied. A prototype Medipix based silicon detector is calibrated using X-ray

In situ flash x-ray high-speed computed tomography for the quantitative analysis of highly dynamic processes

Science.gov (United States)

Moser, Stefan; Nau, Siegfried; Salk, Manfred; Thoma, Klaus

2014-02-01

The in situ investigation of dynamic events, ranging from car crash to ballistics, often is key to the understanding of dynamic material behavior. In many cases the important processes and interactions happen on the scale of milli- to microseconds at speeds of 1000 m s-1 or more. Often, 3D information is necessary to fully capture and analyze all relevant effects. High-speed 3D-visualization techniques are thus required for the in situ analysis. 3D-capable optical high-speed methods often are impaired by luminous effects and dust, while flash x-ray based methods usually deliver only 2D data. In this paper, a novel 3D-capable flash x-ray based method, in situ flash x-ray high-speed computed tomography is presented. The method is capable of producing 3D reconstructions of high-speed processes based on an undersampled dataset consisting of only a few (typically 3 to 6) x-ray projections. The major challenges are identified, discussed and the chosen solution outlined. The application is illustrated with an exemplary application of a 1000 m s-1 high-speed impact event on the scale of microseconds. A quantitative analysis of the in situ measurement of the material fragments with a 3D reconstruction with 1 mm voxel size is presented and the results are discussed. The results show that the HSCT method allows gaining valuable visual and quantitative mechanical information for the understanding and interpretation of high-speed events.

An energy-dispersive X-ray monochromator for measurements in the soft X-ray spectra: design, construction and first measurements. Ein energiedispersiver Roentgenmonochromator mit der Moeglichkeit von Messungen im weichen Roentgenbereich: Entwurf, Aufbau und erste Messungen

Energy Technology Data Exchange (ETDEWEB)

Steil, S.

1993-12-01

An Energy-Dispersive X-ray Monochromator (EDM) for time-resolved X-ray absorption spectroscopy was built in the Synchrotron radiation laboratory at the 3.5 GeV ELectron Stretcher and Accelerator (ELSA). Bragg angles up to 70 and a specially designed vacuum system allow measurements down to an energy of 2.149 keV (P K-edge) with a Si(111)-crystal. Compared to a standard double crystal monochromator and for an EXAFS spectrum at the Cu K-edge at 8.979 keV for concentrated samples, the EDM boosts time resolution by 3 orders of magnitude. The time resolution increases by a factor of 50 for a XANES spectrum at the S K-edge at 2.472 keV for a rubber sample with 4% sulfur. The energy resolution of the EDM is limited by the Darwin width [Omega] of the Bragg crystal. The harmonics in the 'monochromatized' beam, which increase to lower energies, could be nearly eliminated by using a quartz mirror. The spherical aberration of the focus was described theoretically for a cylindrically bent crystal and compared with measurements. In a first time-resolved measurement at the S K-edge, which comprehended about 120 spectra taken in 40 minutes, the thermal ageing of a rubber sample was investigated to demonstrate the performance of the monochromator. (orig.)

Energy dispersive X-ray fluorescence analysis with Bragg polarized Mo radiation. Energiedispersive Roentgenfluoreszenzanalyse mit Bragg-polarisierter Mo Strahlung

Energy Technology Data Exchange (ETDEWEB)

Gloeckl, H

1983-01-01

The aim of introducing energy dispersive analysis into X-ray fluorescence analysis is to suppress background from the Bremsstrahlung spectrum and the characteristic radiation without an undue reduction of the signal. The variant under consideration uses linearly polarization radiation obtained after a Bragg reflection,under delta = 90/sup 0/. In an introductory part, Bragg reflection, fluorescence and strong radiation are considered quantitatively with respect to counting statistics and detection limits. In the experimental part two combinations are describe, of a Ta crystal with a Cr tube and of a Mo crystal with a Mo tube. Details of adjustment, sample preparation and calibration and detection limits are given. The pros and cons of the Ta/Cr and the Mo/Mo are contrasted and proposals for further improvements are given.

Probing Stress States in Silicon Nanowires During Electrochemical Lithiation Using In Situ Synchrotron X-Ray Microdiffraction

Directory of Open Access Journals (Sweden)

Imran Ali

2018-04-01

Full Text Available Silicon is considered as a promising anode material for the next-generation lithium-ion battery (LIB due to its high capacity at nanoscale. However, silicon expands up to 300% during lithiation, which induces high stresses and leads to fractures. To design silicon nanostructures that could minimize fracture, it is important to understand and characterize stress states in the silicon nanostructures during lithiation. Synchrotron X-ray microdiffraction has proven to be effective in revealing insights of mechanical stress and other mechanics considerations in small-scale crystalline structures used in many important technological applications, such as microelectronics, nanotechnology, and energy systems. In the present study, an in situ synchrotron X-ray microdiffraction experiment was conducted to elucidate the mechanical stress states during the first electrochemical cycle of lithiation in single-crystalline silicon nanowires (SiNWs in an LIB test cell. Morphological changes in the SiNWs at different levels of lithiation were also studied using scanning electron microscope (SEM. It was found from SEM observation that lithiation commenced predominantly at the top surface of SiNWs followed by further progression toward the bottom of the SiNWs gradually. The hydrostatic stress of the crystalline core of the SiNWs at different levels of electrochemical lithiation was determined using the in situ synchrotron X-ray microdiffraction technique. We found that the crystalline core of the SiNWs became highly compressive (up to -325.5 MPa once lithiation started. This finding helps unravel insights about mechanical stress states in the SiNWs during the electrochemical lithiation, which could potentially pave the path toward the fracture-free design of silicon nanostructure anode materials in the next-generation LIB.

Thermal expansion behavior study of Co nanowire array with in situ x-ray diffraction and x-ray absorption fine structure techniques

Science.gov (United States)

Mo, Guang; Cai, Quan; Jiang, Longsheng; Wang, Wei; Zhang, Kunhao; Cheng, Weidong; Xing, Xueqing; Chen, Zhongjun; Wu, Zhonghua

2008-10-01

In situ x-ray diffraction and x-ray absorption fine structure techniques were used to study the structural change of ordered Co nanowire array with temperature. The results show that the Co nanowires are polycrystalline with hexagonal close packed structure without phase change up until 700 °C. A nonlinear thermal expansion behavior has been found and can be well described by a quadratic equation with the first-order thermal expansion coefficient of 4.3×10-6/°C and the second-order thermal expansion coefficient of 5.9×10-9/°C. The mechanism of this nonlinear thermal expansion behavior is discussed.

Capacity of X-ray fluorescence analysis

International Nuclear Information System (INIS)

Wobrauschek, P.; Kregsamer, P.

1997-01-01

X-Ray fluorescence analysis (XRF) is a powerful analytical tool for the qualitative and quantitative determination of chemical elements in a sample. Two different detection principles are accepted widely: wavelength dispersive and energy dispersive. Various sources for XRF are discussed: X-ray tubes, accelerators for particle induced XRF, radioactive isotopes, and the use of synchrotron radiation. Applications include environmental, technical, medical, fine art, and forensic studies. Due to the demands of research and application special techniques like total reflection XRF (TXRF) were developed with ultimately achievable detection limits in the femtogram region. The elements detectable by XRF range from Be to U. (author)

Dendrochemical patterns of calcium, zinc, and potassium related to internal factors detected by energy dispersive X-ray fluorescence (EDXRF)

Science.gov (United States)

Smith, Kevin T.; Balouet, Jean Christophe; Shortle, Walter C.; Chalot, Michel; Beaujard, François; Grudd, Håkan; Vroblesky, Don A.; Burkem, Joel G.

2014-01-01

Energy dispersive X-ray fluorescence (EDXRF) provides highly sensitive and precise spatial resolution of cation content in individual annual growth rings in trees. The sensitivity and precision have prompted successful applications to forensic dendrochemistry and the timing of environmental releases of contaminants. These applications have highlighted the need to distinguish dendrochemical effects of internal processes from environmental contamination. Calcium, potassium, and zinc are three marker cations that illustrate the influence of these processes. We found changes in cation chemistry in tree rings potentially due to biomineralization, development of cracks or checks, heartwood/sapwood differentiation, intra-annual processes, and compartmentalization of infection. Distinguishing internal from external processes that affect dendrochemistry will enhance the value of EDXRF for both physiological and forensic investigations.

In situ X-ray studies of film cathodes for solid oxide fuel cells

International Nuclear Information System (INIS)

Fuoss, Paul; Chang, Kee-Chul; You, Hoydoo

2013-01-01

Highlights: •Synchrotron X-rays are used to study in operando the structural and chemical changes of LSM and LSCF film cathodes during half-cell operations. •A-site and B-site cations actively segregate or desegregate on the changes of temperature, pO 2 , and electrochemical potential. •Chemical lattice expansions show that oxygen-cathode interface is the primary source of rate-limiting processes. •The surface and subsurface of the LSM and LSCF films have different oxidation-states due to vacancy concentration changes. •Liquid-phase infiltration and coarsening processes of cathode materials into porous YSZ electrolyte backbone were monitored by USAXS. -- Abstract: Synchrotron-based X-ray techniques have been used to study in situ the structural and chemical changes of film cathodes during half-cell operations. The X-ray techniques used include X-ray reflectivity (XR), total-reflection X-ray fluorescence (TXRF), high-resolution diffraction (HRD), ultra-small angle X-ray scattering (USAXS). The epitaxial thin film model cathodes for XR, TXRF, and HRD measurements are made by pulse laser deposition and porous film cathodes for USAX measurements are made by screen printing technique. The experimental results reviewed here include A-site and B-site segregations, lattice expansion, oxidation-state changes during cell operations and liquid-phase infiltration and coarsening of cathode to electrolyte backbone

Reduction of variable-truncation artifacts from beam occlusion during in situ x-ray tomography

DEFF Research Database (Denmark)

Borg, Leise; Jørgensen, Jakob Sauer; Frikel, Jürgen

2017-01-01

Many in situ x-ray tomography studies require experimental rigs which may partially occlude the beam and cause parts of the projection data to be missing. In a study of fluid flow in porous chalk using a percolation cell with four metal bars drastic streak artifacts arise in the filtered...... and artifact-reduction methods are designed in context of FBP reconstruction motivated by computational efficiency practical for large, real synchrotron data. While a specific variable-truncation case is considered, the proposed methods can be applied to general data cut-offs arising in different in situ x-ray...... backprojection (FBP) reconstruction at certain orientations. Projections with non-trivial variable truncation caused by the metal bars are the source of these variable-truncation artifacts. To understand the artifacts a mathematical model of variable-truncation data as a function of metal bar radius and distance...

Estimation of the effective energy for the diagnostic X-ray

International Nuclear Information System (INIS)

Ogama, Noboru; Fujimoto, Nobuhisa; Nishitani, Motohiro; Yamada, Katsuhiko

2001-01-01

Because X-ray exposure doses to patients during X-ray diagnoses have been increasing with recent advances in medical technology, it is important that optimum control of the radiation dose be maintained during diagnoses. For an evaluation of an exposure dose, the effective energy of the X-ray must be determined, but this is difficult to accomplish during the diagnosis. Here we propose a new method to estimate the effective energy of an X-ray. The magnitude of energy released from an X-ray generator (2 peaks, 12 peaks, inverter, and constant potential) depends on various parameters, including tube voltage, tube current, tube voltage waveform, and total filtration of the X-ray tube. Therefore the measurement of an X-ray's effective energy was conducted by the half-value layer measurement method, which changes the values of these parameters. The data obtained by this method were analyzed to clarify the relationships between X-ray effective energy and the respective parameters. It was thus demonstrated that these relationships could be expressed by a simple linear approximation formula. For the calculation of X-ray effective energy by use of this approximation formula, errors were found to be within a range of -2.11% to 10.4%. Therefore, this method is considered usable for an accurate estimation of an X-ray's effective energy without the need for its direct determination during diagnosis. (author)

In-situ reactive of x-ray optics by glow discharge

International Nuclear Information System (INIS)

Johnson, E.D.; Garrett, R.F.

1987-01-01

We have developed a method of in-situ reactive glow discharge cleaning of x-ray optical surfaces which is capable of complete removal of carbon contamination. Our work is the first to successfully clean an entire optical system in-situ and characterize its performance at short wavelengths (as low as 10 /angstrom/). The apparatus required is quite simple and can easily be fitted to most existing UHV (ultra high vacuum) mirror boxes of monochromators. The advantages of this technique over previously available methods include dramatic improvements in instrument performance and reductions in down time since the whole process typically takes a few days. This paper will briefly describe our results and detail the experimental considerations for application of the technique on different monochromator geometries. Possible improvements and extensions of the technique are also discussed

The Study of the Oxide Coating Effect on Bone-Implant Interface Formation by Means of Electron Microscopy Method with Energy Dispersive X-ray Analysis

International Nuclear Information System (INIS)

Gudakova, A.A.; Danilchenko, S.N.; Sukhodub, L.F.; Luk'yanchenko, V.V.; Zykova, A.V.; Safonov, V.I.

2006-01-01

The experimental results of the measurement of the tissue constituent elements distribution, as well as impurity elements in the tissues around a Ti-implant with protective TiO 2 oxide coating are presented. Study of morphology, qualitative and quantitative analysis were carried out by means of scanning electron microscopy method with energy dispersive X-ray analysis. The results show weak migration of Ti into the bone tissue near the interface and protective role of the oxide coatings

Hohlraums energy balance and x-ray drive

International Nuclear Information System (INIS)

Kilkenny, J.D.

1994-01-01

For many years there has been an active ICF program in the US concentrating on x-ray drive. X-ray drive is produced by focusing laser beams into a high Z hohlraum. Conceptually, the radiation field comes close to thermodynamic equilibrium, that is it becomes isotropic and Planckian. These properties lead to the benefits of x-ray drive--it is relatively easy to obtain drive symmetry on a capsule with no small scalelengths drive perturbations. Other advantages of x-ray drive is the higher mass ablation rate, leading to lower growth rates for hydrodynamic instabilities. X-ray drive has disadvantages, principally the loss of energy to the walls of the hohlraum. This report is divided into the following sections: (1) review of blackbody radiation; (2) laser absorption and conversion to x-rays; (3) x-ray absorption coefficient in matter and Rosseland mean free path; (4) Marshak waves in high Z material; (5) x-ray albedo; and (6) power balance and hohlraum temperature

In-situ measurement of the strain relaxation of GaN nanograins during X-ray irradiation

International Nuclear Information System (INIS)

Choe, Hyeokmin; Lee, Sanghwa; Sohn, Yuri; Kim, Chinkyo

2008-01-01

GaN nanograins were grown on a c-plane sapphire substrate and their strain relaxation due to X-ray irradiation was investigated in-situ by utilizing synchrotron xray scattering. The GaN nanograins were constantly exposed to the synchrotron X-ray and θ-2θ scans through the (002) Bragg peak of GaN were repeatedly carried out during the irradiation. The Bragg peak of the compressively strained GaN nanograins gradually shifted toward higher angle, which implies that the GaN nanograins in compressive strain experienced strain relaxation during X-ray irradiation. (copyright 2008 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

Synthesis of nanostructured iron oxides dispersed in carbon materials and in situ XRD study of the changes caused by thermal treatment

Science.gov (United States)

Gonçalves, Gustavo R.; Schettino, Miguel A.; Morigaki, Milton K.; Nunes, Evaristo; Cunha, Alfredo G.; Emmerich, Francisco G.; Passamani, Edson C.; Baggio-Saitovitch, Elisa; Freitas, Jair C. C.

2015-07-01

Carbon-based magnetic nanocomposites are of large interest for applications in catalysis, magnetic separation, water cleaning, and magnetic resonance imaging, among others. This work describes the synthesis of nanocomposites consisting of iron oxides dispersed into a char (obtained from the carbonization at 700 °C of a lignocellulosic precursor) and the study of the thermal transformations occurring in these materials as a consequence of heat treatments. The materials were prepared by impregnation of the char with iron nitrate in the presence of ammonium hydroxide in aqueous suspension. X-ray diffraction experiments performed using synchrotron radiation and Mössbauer spectroscopy showed that the as-prepared material was composed of amorphous Fe3+ oxides. Scanning electron microscopy images combined with energy-dispersive X-ray spectrometry indicated a homogeneous dispersion of iron oxides and of silica particles (naturally present in the lignocellulosic precursor) throughout the char. X-ray diffractograms recorded in situ during the heat treatment of the as-prepared material showed the presence of small hematite crystallites (average size 22 nm) starting from ca. 300 °C. Further heating caused a progressive growth of the hematite crystallites up to ca. 500 °C, when the conversion to magnetite (Fe3O4) started to take place. At higher temperatures, wüstite (Fe1-xO) was detected as an intermediate phase and austenitic iron (γ-Fe) became the dominant phase at temperatures from 900 °C. A steep weight loss was observed in the TG curve accompanying this last reduction stage; upon cooling, γ-Fe was converted into α-Fe (ferrite), which was the dominant phase at room temperature in this heat-treated sample.

Grain rotation and lattice deformation during photoinduced chemical reactions revealed by in situ X-ray nanodiffraction.

Science.gov (United States)

Huang, Zhifeng; Bartels, Matthias; Xu, Rui; Osterhoff, Markus; Kalbfleisch, Sebastian; Sprung, Michael; Suzuki, Akihiro; Takahashi, Yukio; Blanton, Thomas N; Salditt, Tim; Miao, Jianwei

2015-07-01

In situ X-ray diffraction (XRD) and transmission electron microscopy (TEM) have been used to investigate many physical science phenomena, ranging from phase transitions, chemical reactions and crystal growth to grain boundary dynamics. A major limitation of in situ XRD and TEM is a compromise that has to be made between spatial and temporal resolution. Here, we report the development of in situ X-ray nanodiffraction to measure high-resolution diffraction patterns from single grains with up to 5 ms temporal resolution. We observed, for the first time, grain rotation and lattice deformation in chemical reactions induced by X-ray photons: Br(-) + hv → Br + e(-) and e(-) + Ag(+) → Ag(0). The grain rotation and lattice deformation associated with the chemical reactions were quantified to be as fast as 3.25 rad s(-1) and as large as 0.5 Å, respectively. The ability to measure high-resolution diffraction patterns from individual grains with a temporal resolution of several milliseconds is expected to find broad applications in materials science, physics, chemistry and nanoscience.

Correlation between X-ray and high energy gamma-ray emission form Cygnus X-3

International Nuclear Information System (INIS)

Weekes, T.C.; Danaher, S.; Fegan, D.J.; Porter, N.A.

1981-01-01

In May-June 1980, the 4.8 hour modulated X-ray flux from Cygnus X-3 underwent a significant change in the shape of the light curve; this change correlates with the peak in the high-energy (E > 2 x 10 12 eV) gamma ray emission at the same epoch. (orig.)

Chromosome translocations in chinese medical X-ray workers analyzed by fluorescence in situ hybridization

International Nuclear Information System (INIS)

Sun Yuanming; Li Jin; Wang Qin; Tang Weisheng; Wang Zhiquan

2002-01-01

Objective: To study long-term radiation effect in occupational workers exposed to low dose X-rays using the method of fluorescence in situ hybridization (FISH). Method: Chromosome translocations of 25 medical X-ray workers were analyzed by FISH with chromosome No. 4 and No. 7 probes according to PAINT (The Protocol for Aberration Identification and Nomenclature Terminology) system. Results: The frequency of genome translocation in X-ray workers was (13.14 ± 1.23)/1000 cells. The rate of complete and incomplete translocation was 1:1.7. According to the calendar year of entry before/after the year of 1965 as the border, the data showed that the incomplete translocation of the after 1965 group was obviously higher than those of the controls (P < 0.01 and P < 0.05, respectively). Conclusion: The chromosome translocation in early Chinese medical X-ray workers is mainly the incomplete one, the frequency of translocation does not dependent on chromosomal DNA content, and incomplete and complete ones increase along with prolongation of working years in their position

Energy weighted x-ray dark-field imaging.

Science.gov (United States)

Pelzer, Georg; Zang, Andrea; Anton, Gisela; Bayer, Florian; Horn, Florian; Kraus, Manuel; Rieger, Jens; Ritter, Andre; Wandner, Johannes; Weber, Thomas; Fauler, Alex; Fiederle, Michael; Wong, Winnie S; Campbell, Michael; Meiser, Jan; Meyer, Pascal; Mohr, Jürgen; Michel, Thilo

2014-10-06

The dark-field image obtained in grating-based x-ray phase-contrast imaging can provide information about the objects' microstructures on a scale smaller than the pixel size even with low geometric magnification. In this publication we demonstrate that the dark-field image quality can be enhanced with an energy-resolving pixel detector. Energy-resolved x-ray dark-field images were acquired with a 16-energy-channel photon-counting pixel detector with a 1 mm thick CdTe sensor in a Talbot-Lau x-ray interferometer. A method for contrast-noise-ratio (CNR) enhancement is proposed and validated experimentally. In measurements, a CNR improvement by a factor of 1.14 was obtained. This is equivalent to a possible radiation dose reduction of 23%.

Novel micro-reactor flow cell for investigation of model catalysts using in situ grazing-incidence X-ray scattering

DEFF Research Database (Denmark)

Kehres, Jan; Pedersen, Thomas; Masini, Federico

2016-01-01

at synchrotron facilities are performed utilizing the micro-reactor and a designed transportable gas feed and analysis system. The feasibility of simultaneous in situ GISAXS/GIWAXS experiments in the novel micro-reactor flow cell was confirmed with CO oxidation over mass-selected Ru nanoparticles.......The design, fabrication and performance of a novel and highly sensitive micro-reactor device for performing in situ grazing-incidence X-ray scattering experiments of model catalyst systems is presented. The design of the reaction chamber, etched in silicon on insulator (SIO), permits grazing......-incidence small-angle X-ray scattering (GISAXS) in transmission through 10 µm-thick entrance and exit windows by using micro-focused beams. An additional thinning of the Pyrex glass reactor lid allows simultaneous acquisition of the grazing-incidence wide-angle X-ray scattering (GIWAXS). In situ experiments...

Novel micro-reactor flow cell for investigation of model catalysts using in situ grazing-incidence X-ray scattering

Science.gov (United States)

Kehres, Jan; Pedersen, Thomas; Masini, Federico; Andreasen, Jens Wenzel; Nielsen, Martin Meedom; Diaz, Ana; Nielsen, Jane Hvolbæk; Hansen, Ole

2016-01-01

The design, fabrication and performance of a novel and highly sensitive micro-reactor device for performing in situ grazing-incidence X-ray scattering experiments of model catalyst systems is presented. The design of the reaction chamber, etched in silicon on insulator (SIO), permits grazing-incidence small-angle X-ray scattering (GISAXS) in transmission through 10 µm-thick entrance and exit windows by using micro-focused beams. An additional thinning of the Pyrex glass reactor lid allows simultaneous acquisition of the grazing-incidence wide-angle X-ray scattering (GIWAXS). In situ experiments at synchrotron facilities are performed utilizing the micro-reactor and a designed transportable gas feed and analysis system. The feasibility of simultaneous in situ GISAXS/GIWAXS experiments in the novel micro-reactor flow cell was confirmed with CO oxidation over mass-selected Ru nanoparticles. PMID:26917133

Simulation and evaluation of the absorption edge subtraction technique in energy-resolved X-ray radiography applied to the cultural heritage studies

International Nuclear Information System (INIS)

Leyva Pernia, Diana; Cabal Rodriguez, Ana E.; Pinnera Hernandez, Ibrahin; Leyva Fabelo, Antonio; Abreu Alfonso, Yamiel; Espen, Piet Van

2011-01-01

In this work the mathematical simulation of photon transport in the matter was used to evaluate the potentials of a new energy-resolved X-ray radiography system. The system is intended for investigations of cultural heritage object, mainly painting. The radiographic system uses polychromatic radiation from an X-ray tube and measures the spectrum transmitted through the object with an energy-dispersive X-ray detector on a pixel-by-pixel basis. Manipulation of the data-set obtained allows constructing images with enhanced contrast for certain elements. Here the use of the absorption edge subtraction technique was emphasized. The simulated results were in good agreement with the experimental data.(author)

Analysis of selected elements in tobacco by wavelength dispersive X-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Martin, J.M.

1988-01-01

A rapid method for the determination of 16 elements in tobacco by wavelength dispersive X-ray fluorescence spectrometry has been developed. The method is accurate and precise, and requires only 9 min per sample for quantitation. Sample preparation consists of placing a portion of dried, ground tobacco in a sample cup, and pressing at 25 tons pressure to make a compressed pellet. This pellet is then automatically analyzed by X-ray fluorescence for 16 elements. The results are stored on a computer disk for future recall and report generation. The elements are: Al, Br, Ca, Cl, Cu, Fe, K, Mg, Mn, Na, P, S, Si, Sr, Ti and Zn

A comparative transmission electron microscopy, energy dispersive x-ray spectroscopy and spatially resolved micropillar compression study of the yttria partially stabilised zirconia - porcelain interface in dental prosthesis

Energy Technology Data Exchange (ETDEWEB)

Lunt, Alexander J.G., E-mail: alexander.lunt@chch.ox.ac.uk [Department of Engineering Science, University of Oxford, Parks Road, Oxford, Oxfordshire OX1 3PJ (United Kingdom); Mohanty, Gaurav, E-mail: gaurav.mohanty@empa.ch [EMPA Materials Science & Technology, Feuerwerkerstrasse 39, CH-3602 Thun (Switzerland); Ying, Siqi, E-mail: siqi.ying@eng.ox.ac.uk [Department of Engineering Science, University of Oxford, Parks Road, Oxford, Oxfordshire OX1 3PJ (United Kingdom); Dluhoš, Jiří, E-mail: jiri.dluhos@tescan.cz [TESCAN Brno, s.r.o., Libušina tř. 1, 623 00 Brno-Kohoutovice (Czech Republic); Sui, Tan, E-mail: tan.sui@eng.ox.ac.uk [Department of Engineering Science, University of Oxford, Parks Road, Oxford, Oxfordshire OX1 3PJ (United Kingdom); Neo, Tee K., E-mail: neophyte@singnet.com.sg [Specialist Dental Group, Mount Elizabeth Orchard, 3 Mount Elizabeth, #08-03/08-08/08-10, 228510 (Singapore); Michler, Johann, E-mail: johann.michler@empa.ch [EMPA Materials Science & Technology, Feuerwerkerstrasse 39, CH-3602 Thun (Switzerland); Korsunsky, Alexander M., E-mail: alexander.korsunsky@eng.ox.ac.uk [Department of Engineering Science, University of Oxford, Parks Road, Oxford, Oxfordshire OX1 3PJ (United Kingdom)

2015-12-01

Recent studies into the origins of failure of yttria partially stabilised zirconia–porcelain veneered prosthesis have revealed the importance of micro-to-nano scale characterisation of this interface zone. Current understanding suggests that the heat treatment, residual stresses and varying microstructure at this location may contribute to near-interface porcelain chipping. In this study the chemical, microstructural and mechanical property variation across the interfacial zone has been characterised at two differing length scales and using three independent techniques; energy dispersive X-ray spectroscopy, transmission electron microscopy and micropillar compression. Energy dispersive X-ray spectroscopy mapping of the near-interface region revealed, for the first time, that the diffusional lengths of twelve principal elements are limited to within 2–6 μm of the interface. This study also revealed that 0.2–2 μm diameter zirconia grains had become detached from the bulk and were embedded in the near-interface porcelain. Transmission electron microscopy analysis demonstrated the presence of nanoscale spherical features, indicative of tensile creep induced voiding, within the first 0.4–1.5 μm from the interface. Within zirconia, variations in grain size and atomistic structure were also observed within the 3 μm closest to the interface. Micropillar compression was performed over a 100 μm range on either side of the interface at the spatial resolution of 5 μm. This revealed an increase in zirconia and porcelain loading modulus at close proximities (< 5 μm) to the interface and a decrease in zirconia modulus at distances between 6 and 41 μm from this location. The combination of the three experimental techniques has revealed intricate details of the microstructural, chemical and consequently mechanical heterogeneities in the YPSZ–porcelain interface, and demonstrated that the length scales typically associated with this behaviour are approximately ± 5

Elemental profiling of laser cladded multilayer coatings by laser induced breakdown spectroscopy and energy dispersive X-ray spectroscopy

Science.gov (United States)

Lednev, V. N.; Sdvizhenskii, P. A.; Filippov, M. N.; Grishin, M. Ya.; Filichkina, V. A.; Stavertiy, A. Ya.; Tretyakov, R. S.; Bunkin, A. F.; Pershin, S. M.

2017-09-01

Multilayer tungsten carbide wear resistant coatings were analyzed by laser induced breakdown spectroscopy (LIBS) and energy dispersive X-ray (EDX) spectroscopy. Coaxial laser cladding technique was utilized to produce tungsten carbide coating deposited on low alloy steel substrate with additional inconel 625 interlayer. EDX and LIBS techniques were used for elemental profiling of major components (Ni, W, C, Fe, etc.) in the coating. A good correlation between EDX and LIBS data was observed while LIBS provided additional information on light element distribution (carbon). A non-uniform distribution of tungsten carbide grains along coating depth was detected by both LIBS and EDX. In contrast, horizontal elemental profiling showed a uniform tungsten carbide particles distribution. Depth elemental profiling by layer-by-layer LIBS analysis was demonstrated to be an effective method for studying tungsten carbide grains distribution in wear resistant coating without any sample preparation.

Structural study on Ni nanowires in an anodic alumina membrane by using in situ heating extended x-ray absorption fine structure and x-ray diffraction techniques

International Nuclear Information System (INIS)

Cai Quan; Chen Xing; Chen Zhongjun; Wang Wei; Mo Guang; Wu Zhonghua; Zhang Junxi; Zhang Lide; Pan Wei

2008-01-01

Polycrystalline Ni nanowires have been prepared by electrochemical deposition in an anodic alumina membrane template with a nanopore size of about 60 nm. In situ heating extended x-ray absorption fine structure and x-ray diffraction techniques are used to probe the atomic structures. The nanowires are identified as being mixtures of nanocrystallites and amorphous phase. The nanocrystallites have the same thermal expansion coefficient, of 1.7 x 10 -5 K -1 , as Ni bulk; however, the amorphous phase has a much larger thermal expansion coefficient of 3.5 x 10 -5 K -1 . Details of the Ni nanowire structures are discussed in this paper

The color of X-rays Spectral X-ray computed tomography using energy sensitive pixel detectors

CERN Document Server

Schioppa, Enrico Junior

Energy sensitive X-ray imaging detectors are produced by connecting a semiconductor sensor to a spectroscopic pixel readout chip. In this thesis, the applicability of such detectors to X-ray Computed Tomography (CT) is studied. A prototype Medipix based silicon detector is calibrated using X-ray fluorescence. The charge transport properties of the sensor are characterized using a high energy beam of charged particles at the Super Proton Synchrotron (SPS) at the European Center for Nuclear Research (CERN). Monochromatic X-rays at the European Synchrotron Radiation Facility (ESRF) are used to determined the energy response function. These data are used to implement a physics-based CT projection operator that accounts for the transmission of the source spectrum through the sample and detector effects. Based on this projection operator, an iterative spectral CT reconstruction algorithm is developed by extending an Ordered Subset Expectation Maximization (OSEM) method. Subsequently, a maximum likelihood based algo...

European X-ray spectroscopy and polarimetry payload for Spacelab

Energy Technology Data Exchange (ETDEWEB)

Andresen, R D; Whitcomb, G [European Space Research and Technology Centre, Noordwijk (Netherlands); Brinkman, A C [Space Research Laboratory, Utrecht, The Netherlands; Beuermann, K [Max-Planck-Institut fuer Physik und Astrophysik, Garching/Muenchen (Germany, F.R.). Inst. fuer Extraterrestrische Physik; Culhane, J L [University Coll., London (UK). Mullard Space Science Lab.; Griffiths, R [Leicester Univ. (UK); Manno, V [ESA Headquarters, Paris, France; Rocchia, R [CEA Centre d' Etudes Nucleaires de Saclay, 91 - Gif-sur-Yvette (France)

1976-08-01

A group of instruments for X-ray spectroscopy and polarimetry studies of a number of cosmic X-ray sources is being designed for possible use on Spacelab. Large area Bragg spectrometers and polarimeters for photon energies above 2 keV are described. For the energy range below 2 keV, both dispersive and non-dispersive spectrometers are employed at the common focus of a nested array of paraboloids. Following a brief outline of the scientific background to the mission, the properties of the individual instruments are discussed.

Application of the nuclear x-ray fluorescence method to prospecting for gold in-situ

International Nuclear Information System (INIS)

Zhang, Y.; Xie, T.; Zhou, S.; Ge, L.

1989-01-01

Arsenic and chalcophile elements are often associated with gold, and can be considered indicator elements when prospecting for gold deposits. The nuclear geophysics X-ray fluorescence method can be used to search for hidden gold deposits by measuring fluorescence intensities of the indicator elements in situ. The method can speed geologic investigation and reduce exploration cost. Three types of portable radioisotope X-ray fluorescence analyzers, designed and manufactured by Chengdu College of Geology and Chongqing Geological Instrument Factory, are briefly introduced. These analyzers are widely used in different stages of geologic investigation for gold in China. In the two case histories presented five anomalous zones of X-ray fluorescence intensity related to gold mineralization are located and one hidden gold deposit is discovered with gold content of 23 g/t

DCARR: a spectrograph for measuring low-energy x rays

International Nuclear Information System (INIS)

Anon.

1978-01-01

DCARR, the Differential Critical Angle Reflection Refraction detector system, is described. This detector was designed to measure low-energy x rays, 500 to 5000 eV, with a high degree of resolution, 250 eV. DCARR was developed because these low-energy measurements are of interest in the diagnostics of x-radiation in nuclear tests and available equipment could not make measurements at this low an energy in field tests. DCARR is a versatile piece of equipment that can also be used as a laboratory tool, such as in measuring the low-energy x rays emitted by lasers and various x-ray machines

Industry-relevant magnetron sputtering and cathodic arc ultra-high vacuum deposition system for in situ x-ray diffraction studies of thin film growth using high energy synchrotron radiation.

Science.gov (United States)

Schroeder, J L; Thomson, W; Howard, B; Schell, N; Näslund, L-Å; Rogström, L; Johansson-Jõesaar, M P; Ghafoor, N; Odén, M; Nothnagel, E; Shepard, A; Greer, J; Birch, J

2015-09-01

We present an industry-relevant, large-scale, ultra-high vacuum (UHV) magnetron sputtering and cathodic arc deposition system purposefully designed for time-resolved in situ thin film deposition/annealing studies using high-energy (>50 keV), high photon flux (>10(12) ph/s) synchrotron radiation. The high photon flux, combined with a fast-acquisition-time (film formation processes. The high-energy synchrotron-radiation based x-rays result in small scattering angles (industry-relevant processes. We openly encourage the materials research community to contact us for collaborative opportunities using this unique and versatile scientific instrument.

A standards-based method for compositional analysis by energy dispersive X-ray spectrometry using multivariate statistical analysis: application to multicomponent alloys.

Science.gov (United States)

Rathi, Monika; Ahrenkiel, S P; Carapella, J J; Wanlass, M W

2013-02-01

Given an unknown multicomponent alloy, and a set of standard compounds or alloys of known composition, can one improve upon popular standards-based methods for energy dispersive X-ray (EDX) spectrometry to quantify the elemental composition of the unknown specimen? A method is presented here for determining elemental composition of alloys using transmission electron microscopy-based EDX with appropriate standards. The method begins with a discrete set of related reference standards of known composition, applies multivariate statistical analysis to those spectra, and evaluates the compositions with a linear matrix algebra method to relate the spectra to elemental composition. By using associated standards, only limited assumptions about the physical origins of the EDX spectra are needed. Spectral absorption corrections can be performed by providing an estimate of the foil thickness of one or more reference standards. The technique was applied to III-V multicomponent alloy thin films: composition and foil thickness were determined for various III-V alloys. The results were then validated by comparing with X-ray diffraction and photoluminescence analysis, demonstrating accuracy of approximately 1% in atomic fraction.

Energy-angle correlation correction algorithm for monochromatic computed tomography based on Thomson scattering X-ray source

Science.gov (United States)

Chi, Zhijun; Du, Yingchao; Huang, Wenhui; Tang, Chuanxiang

2017-12-01

The necessity for compact and relatively low cost x-ray sources with monochromaticity, continuous tunability of x-ray energy, high spatial coherence, straightforward polarization control, and high brightness has led to the rapid development of Thomson scattering x-ray sources. To meet the requirement of in-situ monochromatic computed tomography (CT) for large-scale and/or high-attenuation materials based on this type of x-ray source, there is an increasing demand for effective algorithms to correct the energy-angle correlation. In this paper, we take advantage of the parametrization of the x-ray attenuation coefficient to resolve this problem. The linear attenuation coefficient of a material can be decomposed into a linear combination of the energy-dependent photoelectric and Compton cross-sections in the keV energy regime without K-edge discontinuities, and the line integrals of the decomposition coefficients of the above two parts can be determined by performing two spectrally different measurements. After that, the line integral of the linear attenuation coefficient of an imaging object at a certain interested energy can be derived through the above parametrization formula, and monochromatic CT can be reconstructed at this energy using traditional reconstruction methods, e.g., filtered back projection or algebraic reconstruction technique. Not only can monochromatic CT be realized, but also the distributions of the effective atomic number and electron density of the imaging object can be retrieved at the expense of dual-energy CT scan. Simulation results validate our proposal and will be shown in this paper. Our results will further expand the scope of application for Thomson scattering x-ray sources.

Advantages of intermediate X-ray energies in Zernike phase contrast X-ray microscopy.

Science.gov (United States)

Wang, Zhili; Gao, Kun; Chen, Jian; Hong, Youli; Ge, Xin; Wang, Dajiang; Pan, Zhiyun; Zhu, Peiping; Yun, Wenbing; Jacobsen, Chris; Wu, Ziyu

2013-01-01

Understanding the hierarchical organizations of molecules and organelles within the interior of large eukaryotic cells is a challenge of fundamental interest in cell biology. Light microscopy is a powerful tool for observations of the dynamics of live cells, its resolution attainable is limited and insufficient. While electron microscopy can produce images with astonishing resolution and clarity of ultra-thin (3D images of cryo-preserved cells. The relatively low X-ray energy (3D imaging (e.g., ~1 μm DoF for 20 nm resolution). An X-ray microscope operating at intermediate energy around 2.5 keV using Zernike phase contrast can overcome the above limitations and reduces radiation dose to the specimen. Using a hydrated model cell with an average chemical composition reported in literature, we calculated the image contrast and the radiation dose for absorption and Zernike phase contrast, respectively. The results show that an X-ray microscope operating at ~2.5 keV using Zernike phase contrast offers substantial advantages in terms of specimen size, radiation dose and depth-of-focus. Copyright © 2012 Elsevier Inc. All rights reserved.