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Sample records for energy-dispersive x-ray diffraction

  1. 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

  2. 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.

  3. 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.

  4. 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 ...

  5. 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.

  6. 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.

  7. 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

  8. 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)

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. 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

  15. 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.)

  16. 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

  17. 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)

  18. 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.)

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

    Indian Academy of Sciences (India)

    structure of materials under various thermodynamics conditions, viz. temperature .... design to incorporate KB mirror system when it becomes available. .... peak analysis of diffraction peaks show that diffraction resolution is also ∼2% which is.

  20. The internal strain parameter of gallium arsenide measured by energy-dispersive X-ray diffraction

    International Nuclear Information System (INIS)

    Cousins, C.S.G.; Sheldon, B.J.; Webster, G.E.; Gerward, L.; Selsmark, B.; Staun Olsen, J.

    1989-01-01

    The internal strain parameter of GaAs has been measured by observing the stress-dependence of the integrated intensity of the weak 006 reflection, with the compressive stress along the [1anti 10] axis. An energy-dispersive technique was employed so that the reflection could be obtained at a photon energy close to the minimum in the structure factor, thereby approaching closely the strictly-forbidden condition that applies at any energy in the diamond structure. A value anti A=-0.138±0.005, equivalent to a bond-bending parameter ζ=0.55=0.02, has been found. This is in good agreement with recent theoretical calculations and indirect determinations related to the bandstructure of GaAs. (orig.)

  1. Operation manual for EDXRDDA - a software package for Bragg peak analysis of energy dispersive powder X-ray diffraction data

    International Nuclear Information System (INIS)

    Jayaswal, Balhans; Vijaykumar, V.; Momin, S.N.; Sikka, S.K.

    1992-01-01

    EDXRDDA is a software package for analysis of raw data for energy dispersive x-ray diffraction from powder samples. It resolves the spectra into individual peaks by a constrained non-linear least squares method (Hughes and Sexton, 1988). The profile function adopted is the Gaussian/Lorentzian product with the mixing ratio refinable in the program. The program is implemented on an IBM PC and is highly interactive with extensive plotting facilities. This report is a user's guide for running the program. In the first step after inputting the spectra, the full spectra is plotted on the screen. The user then chooses a portion of this for peak resolution. The initial guess for the peak intensity, peak position are input with the help of a cursor or a mouse. Upto twenty peaks can be fitted at a time in an interval of 500 channels. For overlapping peaks, various constraints can be applied. Bragg peaks and fluorescence peaks with different half widths can be handled simultaneously. The program on execution produces a look up table which contains the refined values of the peak position, half width, peak intensity, integrated intensity, and their error estimates of each peak. The program is very general and can also be used for curve fitting of data from many other experiments. (author). 2 refs., 7 figs., 2 appendices

  2. 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.

  3. 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

  4. In situ characterization of ancient plaster and pigments on tomb walls in Egypt using energy dispersive X-ray diffraction and fluorescence

    International Nuclear Information System (INIS)

    Uda, M.

    2004-01-01

    A portable type of energy dispersive X-ray diffraction and fluorescence (ED-XRDF) spectrometer was developed, whose operation mode is completely different from that of an X-ray diffractometer commercially available. The former is operated in energy dispersive mode but the latter in angle dispersive mode. The performance of the ED-XRDF spectrometer was tested in the field, i.e. in the tomb of Amenhotep III, built in 1364 B.C. or earlier in Egypt. The crystal structure and chemical composition of ancient plaster and pigments were successfully determined in the field using the spectrometer. The same areas investigated by the ED-XRDF spectrometer were also examined with an optical microscope. The plaster is found to be composed of anhydrite, calcite and quartz. White and yellow pigments were identified as huntite and orpiment, respectively. Egyptian blue and goethite were found in the green colored parts

  5. New medical imaging systems exploiting the energy dispersive X-ray diffraction with spectrometric CdZnTe based detector

    International Nuclear Information System (INIS)

    Barbes, Damien

    2016-01-01

    This thesis studies the interest of measuring the coherent scattering of X-rays for breast diagnosis imaging. Nowadays, most of X-ray-based medical imaging techniques use the information of X-rays attenuation through the tissues. It is the case for mammography, the most common breast imaging modality. The recent emergence of energy resolved detectors (based on semiconductors in particular) allows to consider using another phenomenon: the coherent X-ray scattering. Measurement of diffracted spectra can provide new information related to the molecular structure of the examined tissues, in order to improve their characterization and therefore improve the final diagnosis. Two modalities are considered: the breast cancer detection in vivo, following a suspicious mammography result, or biopsy analysis. The coherent scattering measurement system developed during this thesis work uses energy-resolved CdZnTe-based detectors, these detectors combining performances (energy resolution, sensitivity, spatial resolution, and compactness) promising for clinical application. This system is also based on the detector pixelation, which allows to provide an imaging modality capable of characterizing analyzed materials or tissues in one direction without any translation or rotation. A complete study of the measurement system is proposed in this thesis, structured in three main parts: modeling and simulation of the system, development of the processing of the data measured by the detector in order to image and characterize the analyzed sample and finally, designing of a new and more complex experimental setup based on a whole detector and multi-slit collimation system. An experimental validation is proposed for each of these three parts. (author) [fr

  6. A correlative approach to segmenting phases and ferrite morphologies in transformation-induced plasticity steel using electron back-scattering diffraction and energy dispersive X-ray spectroscopy.

    Science.gov (United States)

    Gazder, Azdiar A; Al-Harbi, Fayez; Spanke, Hendrik Th; Mitchell, David R G; Pereloma, Elena V

    2014-12-01

    Using a combination of electron back-scattering diffraction and energy dispersive X-ray spectroscopy data, a segmentation procedure was developed to comprehensively distinguish austenite, martensite, polygonal ferrite, ferrite in granular bainite and bainitic ferrite laths in a thermo-mechanically processed low-Si, high-Al transformation-induced plasticity steel. The efficacy of the ferrite morphologies segmentation procedure was verified by transmission electron microscopy. The variation in carbon content between the ferrite in granular bainite and bainitic ferrite laths was explained on the basis of carbon partitioning during their growth. Copyright © 2014 Elsevier B.V. All rights reserved.

  7. In-situ studies of the recrystallization process of CuInS2 thin films by energy dispersive X-ray diffraction

    International Nuclear Information System (INIS)

    Thomas, D.; Mainz, R.; Rodriguez-Alvarez, H.; Marsen, B.; Abou-Ras, D.; Klaus, M.; Genzel, Ch.; Schock, H.-W.

    2011-01-01

    Recrystallization processes during the sulfurization of CuInS 2 (CIS) thin films have been studied in-situ using energy dispersive X-ray diffraction (EDXRD) with synchrotron radiation. In order to observe the recrystallization isolated from other reactions occurring during film growth, Cu-poor, small grained CIS layers covered with CuS on top were heated in a vacuum chamber equipped with windows for synchrotron radiation in order to analyze the grain growth mechanism within the CIS layer. In-situ monitoring of the grain size based on diffraction line profile analysis of the CIS-112 reflection was utilized to interrupt the recrystallization process at different points. Ex-situ studies by electron backscatter diffraction (EBSD) and energy dispersive X-ray spectroscopy (EDX) performed on samples of intermediate recrystallization states reveal that during the heat treatment Cu and In interdiffuse inside the layer indicating the importance of the mobility of these two elements during CuInS 2 grain growth.

  8. 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.

  9. On the authenticity of eight Reales 1730 Mexican silver coins by X-ray diffraction and by energy dispersion spectroscopy techniques

    International Nuclear Information System (INIS)

    Rojas-Rodriguez, I.; Herrera, A.; Vazquez-Lopez, C.; Apolo, R.; Gonzalez-Hernandez, J.; Hernandez-Landaverde, M.A.; Rodriguez, M.E.

    2004-01-01

    Ancient silver Mexican coins made during the years 1730-1734, were analyzed non-destructively by energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), and by optical microscopy. Nine coins of denomination eight Reales were studied. These coins belong to the numismatic private collection in Mexico. Six elements (copper, aluminum, magnesium, silicon, chromium and silver) were determined quantitatively. The coins reveal a uniform Ag concentration. Some of the items are covered with patina. A strong positive correlation between Al and Cu content and also a strong negative correlation between S and Ag were determined. The weight of the coins varied between 26.1344 and 26.9913 g, which is a good indicator of the authenticity of the items. The purpose of this work is to investigate by precise means if some of the coins were falsified or if really all of them are authentic

  10. Fundamentals of energy dispersive X-ray analysis

    CERN Document Server

    Russ, John C; Kiessling, R; Charles, J

    1984-01-01

    Fundamentals of Energy Dispersive X-ray Analysis provides an introduction to the fundamental principles of dispersive X-ray analysis. It presents descriptions, equations, and graphs to enable the users of these techniques to develop an intuitive and conceptual image of the physical processes involved in the generation and detection of X-rays. The book begins with a discussion of X-ray detection and measurement, which is accomplished by one of two types of X-ray spectrometer: energy dispersive or wavelength dispersive. The emphasis is on energy dispersive spectrometers, given their rather wid

  11. Quantitative energy-dispersive electron probe X-ray microanalysis ...

    Indian Academy of Sciences (India)

    Abstract. An energy-dispersive electron probe X-ray microanalysis (ED-EPMA) technique us- ing an energy-dispersive X-ray detector with an ultra-thin window, designated as low-Z particle. EPMA, has been developed. The low-Z particle EPMA allows the quantitative determination of concentrations of low-Z elements such ...

  12. Tomography with energy dispersive diffraction

    Science.gov (United States)

    Stock, S. R.; Okasinski, J. S.; Woods, R.; Baldwin, J.; Madden, T.; Quaranta, O.; Rumaiz, A.; Kuczewski, T.; Mead, J.; Krings, T.; Siddons, P.; Miceli, A.; Almer, J. D.

    2017-09-01

    X-ray diffraction can be used as the signal for tomographic reconstruction and provides a cross-sectional map of the crystallographic phases and related quantities. Diffraction tomography has been developed over the last decade using monochromatic x-radiation and an area detector. This paper reports tomographic reconstruction with polychromatic radiation and an energy sensitive detector array. The energy dispersive diffraction (EDD) geometry, the instrumentation and the reconstruction process are described and related to the expected resolution. Results of EDD tomography are presented for two samples containing hydroxyapatite (hAp). The first is a 3D-printed sample with an elliptical crosssection and contains synthetic hAp. The second is a human second metacarpal bone from the Roman-era cemetery at Ancaster, UK and contains bio-hAp which may have been altered by diagenesis. Reconstructions with different diffraction peaks are compared. Prospects for future EDD tomography are also discussed.

  13. A correlative approach to segmenting phases and ferrite morphologies in transformation-induced plasticity steel using electron back-scattering diffraction and energy dispersive X-ray spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Gazder, Azdiar A., E-mail: azdiar@uow.edu.au [Electron Microscopy Centre, University of Wollongong, New South Wales 2500 (Australia); Al-Harbi, Fayez; Spanke, Hendrik Th. [School of Mechanical, Materials and Mechatronic Engineering, University of Wollongong, New South Wales 2522 (Australia); Mitchell, David R.G. [Electron Microscopy Centre, University of Wollongong, New South Wales 2500 (Australia); Pereloma, Elena V. [Electron Microscopy Centre, University of Wollongong, New South Wales 2500 (Australia); School of Mechanical, Materials and Mechatronic Engineering, University of Wollongong, New South Wales 2522 (Australia)

    2014-12-15

    Using a combination of electron back-scattering diffraction and energy dispersive X-ray spectroscopy data, a segmentation procedure was developed to comprehensively distinguish austenite, martensite, polygonal ferrite, ferrite in granular bainite and bainitic ferrite laths in a thermo-mechanically processed low-Si, high-Al transformation-induced plasticity steel. The efficacy of the ferrite morphologies segmentation procedure was verified by transmission electron microscopy. The variation in carbon content between the ferrite in granular bainite and bainitic ferrite laths was explained on the basis of carbon partitioning during their growth. - Highlights: • Multi-condition segmentation of austenite, martensite, polygonal ferrite and ferrite in bainite. • Ferrites in granular bainite and bainitic ferrite segmented by variation in relative carbon counts. • Carbon partitioning during growth explains variation in carbon content of ferrites in bainites. • Developed EBSD image processing tools can be applied to the microstructures of a variety of alloys. • EBSD-based segmentation procedure verified by correlative TEM results.

  14. Energy dispersive X-Ray fluorescence spectrometric study of ...

    African Journals Online (AJOL)

    Energy dispersive X-Ray fluorescence spectrometric study of compositional differences in trace elements in dried Moringa oleifera leaves grown in two different agro-ecological locations in Ebonyi State, Nigeria.

  15. X-Ray diffraction and scanning electron microscopy-energy dispersive spectroscopic analysis of ceramõmetal interface at different firing temperatures

    Directory of Open Access Journals (Sweden)

    Monika Saini

    2010-01-01

    Full Text Available Objective: Porcelain chipping from porcelain fused to metal restoration has been Achilles heel till date. There has been advent of newer ceramics in past but but none of them has been a panacea for Porcelain fracture. An optimal firing is thus essential for the clinical success of the porcelain-fused to metal restoration. The aim of the present study was to evaluate ceramo-metal interface at different firing temperature using XRD and SEM-EDS analysis. Clinical implication of the study was to predict the optimal firing temperature at which porcelain should be fused with metal in order to possibly prevent the occasional failure of the porcelain fused to metal restorations. Materials and Methods: To meet the above-mentioned goal, porcelain was fused to metal at different firing temperatures (930-990°C in vacuum. The microstructural observations of interface between porcelain and metal were evaluated using X-ray diffraction and scanning electron microscopy with energy dispersive spectroscopy. Results: Based on the experimental investigation of the interaction zone of porcelain fused to metal samples, it was observed that as the firing temperature was increased, the pores became less in number as well as the size of the pores decreased at the porcelain/metal interface upto 975°C but increased in size at 990°C. The least number of pores with least diameter were found in samples fired at 975°C. Several oxides like Cr 2 O 3 , NiO, and Al 2 O 3 and intermetallic compounds (CrSi 2 , AlNi 3 were also formed in the interaction zone. Conclusions : It is suggested that the presence of pores may trigger the crack propagation along the interface, causing the failure of the porcelain fused to metal restoration during masticatory action.

  16. Silicon supported lipid-DNA thin film structures at varying temperature studied by energy dispersive X-ray diffraction and neutron reflectivity.

    Science.gov (United States)

    Domenici, F; Castellano, C; Dell'Unto, F; Albinati, A; Congiu, A

    2011-11-01

    Non-viral gene transfection by means of lipid-based nanosystems, such as solid supported lipid assemblies, is often limited due to their lack of stability and the consequent loss of efficiency. Therefore not only a detailed thermo-lyotropic study of these DNA-lipid complexes is necessary to understand their interaction mechanisms, but it can also be considered as a first step in conceiving and developing new transfection biosystems. The aim of our study is a structural characterization of 1,2-dioleoyl-sn-glycero-3-phosphatidylcholine (DOPC)-dimethyl-dioctadecyl-ammonium bromide (DDAB)-DNA complex at varying temperature using the energy dispersive X-ray diffraction (EDXD) and neutron reflectivity (NR) techniques. We have shown the formation of a novel thermo-lyotropic structure of DOPC/DDAB thin film self-organized in multi-lamellar planes on (100)-oriented silicon support by spin coating, thus enlightening its ability to include DNA strands. Our NR measurements indicate that the DOPC/DDAB/DNA complex forms temperature-dependent structures. At 65°C and relative humidity of 100% DNA fragments are buried between single lamellar leaflets constituting the hydrocarbon core of the lipid bilayers. This finding supports the consistency of the hydrophobic interaction model, which implies that the coupling between lipid tails and hypo-hydrated DNA single strands could be the driving force of DNA-lipid complexation. Upon cooling to 25°C, EDXD analysis points out that full-hydrated DOPC-DDAB-DNA can switch in a different metastable complex supposed to be driven by lipid heads-DNA electrostatic interaction. Thermotropic response analysis also clarifies that DOPC has a pivotal role in promoting the formation of our observed thermophylic silicon supported lipids-DNA assembly. Copyright © 2011 Elsevier B.V. All rights reserved.

  17. Quantitative analysis with energy dispersive X-ray fluorescence analyser

    International Nuclear Information System (INIS)

    Kataria, S.K.; Kapoor, S.S.; Lal, M.; Rao, B.V.N.

    1977-01-01

    Quantitative analysis of samples using radioisotope excited energy dispersive x-ray fluorescence system is described. The complete set-up is built around a locally made Si(Li) detector x-ray spectrometer with an energy resolution of 220 eV at 5.94 KeV. The photopeaks observed in the x-ray fluorescence spectra are fitted with a Gaussian function and the intensities of the characteristic x-ray lines are extracted, which in turn are used for calculating the elemental concentrations. The results for a few typical cases are presented. (author)

  18. X-ray diffraction

    International Nuclear Information System (INIS)

    Einstein, J.R.; Wei, C.H.

    1982-01-01

    We have been interested in structural elucidation by x-ray diffraction of compounds of biological interest. Understanding exactly how atoms are arranged in three-dimensional arrays as molecules can help explain the relationship between structure and functions. The species investigated may vary in size and shape; our recent studies included such diverse substances as antischistosomal drugs, a complex of cadmium with nucleic acid base, nitrate salts of adenine, and proteins

  19. Material-specific imaging system using energy-dispersive X-ray diffraction and spatially resolved CdZnTe detectors with potential application in breast imaging

    Energy Technology Data Exchange (ETDEWEB)

    Barbes, Damien, E-mail: damien.barbes@cea.fr [Univ. Grenoble Alpes, F-38000 Grenoble (France); CEA, LETI, MINATEC Campus, F-38054 Grenoble (France); Tabary, Joachim, E-mail: joachim.tabary@cea.fr [Univ. Grenoble Alpes, F-38000 Grenoble (France); CEA, LETI, MINATEC Campus, F-38054 Grenoble (France); Paulus, Caroline, E-mail: caroline.paulus@cea.fr [Univ. Grenoble Alpes, F-38000 Grenoble (France); CEA, LETI, MINATEC Campus, F-38054 Grenoble (France); Hazemann, Jean-Louis, E-mail: jean-louis.hazemann@neel.cnrs.fr [Univ.Grenoble Alpes, Inst NEEL, F-38042 Grenoble (France); CNRS, Inst NEEL, F-38042 Grenoble (France); Verger, Loïck, E-mail: loick.verger@cea.fr [Univ. Grenoble Alpes, F-38000 Grenoble (France); CEA, LETI, MINATEC Campus, F-38054 Grenoble (France)

    2017-03-11

    This paper presents a coherent X-ray-scattering imaging technique using a multipixel energy-dispersive system. Without any translation, the technique produces specific 1D image from data recorded by a single CdZnTe detector pixel using subpixelation techniques. The method is described in detail, illustrated by a simulation and then experimentally validated. As the main considered application of our study is breast imaging, this validation involves 2D imaging of a phantom made of plastics mimicking breast tissues. The results obtained show that our system can specifically image the phantom using a single detector pixel. For the moment, in vivo breast imaging applications remain difficult, as the dose delivered by the system is too high, but some adjustments are considered for further work.

  20. X-ray diffraction

    International Nuclear Information System (INIS)

    Vries, J.L. de.

    1976-01-01

    The seventh edition of Philips' Review of literature on X-ray diffraction begins with a list of conference proceedings on the subject, organised by the Philips' organisation at regular intervals in various European countries. This is followed by a list of bulletins. The bibliography is divided according to the equipment (cameras, diffractometers, monochromators) and its applications. The applications are subdivided into sections for high/low temperature and pressure, effects due to the equipment, small angle scattering and a part for stress, texture and phase analyses of metals and quantitative analysis of minerals

  1. X-ray energy-dispersive diffractometry using synchrotron radiation

    International Nuclear Information System (INIS)

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

    1977-03-01

    In contrast to bremsstrahlung from X-ray tubes, synchrotron radiation is very intense, has a smooth spectrum, its polarization is well defined, and at DESY the range of useful photon energies can be extended to about 70 keV and higher. In addition the X-ray beam is very well collimated. Thus synchrotron radiation seems to be an ideal X-ray source for energy-dispersive diffractometry. This note briefly describes the experimental set up at DESY, shows examples of results, and presents the underlying 'philosophy' of the research programme. (Auth.)

  2. Secondary-source energy-dispersive x-ray spectrometer

    International Nuclear Information System (INIS)

    Larsen, R.P.; Tisue, G.T.

    1975-01-01

    A secondary-source energy-dispersive x-ray spectrometer has been built and tested. In this instrument the primary source of x rays is a tungsten-target tube powered by a high-voltage (75 kV), a high-power (3.7 kW) generator from a wavelength spectrometer (G.E. XRD-6). The primary polychromatic x rays irradiate an elemental foil, the secondary source. Its characteristic essentially monochromatic x rays are used to irradiate the sample. Fluorescent x rays from the sample are detected and resolved by a lithium-drifted silicon detector, multichannel-analyzer system. The design of the instrument provides a convenient means for changing the secondary, and hence, the energy of the excitation radiation

  3. Energy Dispersive X-Ray Fluorescence Spectrometric Study of ...

    African Journals Online (AJOL)

    MBI

    2017-06-11

    Jun 11, 2017 ... Compositional Differences in Trace Elements in Dried Moringa oleifera ... Ti, Cu, Mo, Fe, Zn, Ni, Re, Eu and Pb using Energy Dispersive X-ray fluorescence ... Africa, Southeast Asia (Valdez-Solana et al., 2015). ... vegetable in many countries, including Nigeria .... of other elements in environmental samples.

  4. Scanning electron microscopy-energy dispersive X-ray spectrometer ...

    African Journals Online (AJOL)

    The distribution of arsenic (As) and cadmium (Cd) in himematsutake was analyzed using scanning electron microscopy-energy dispersive X-ray spectrometer (SEM-EDX). The atomic percentage of the metals was confirmed by inductively coupled plasma-mass spectrometer (ICP-MS). Results show that the accumulation of ...

  5. Research Note: Energy dispersive x-ray fluorescence analysis ...

    African Journals Online (AJOL)

    Energy Dispersive X-Ray fluorescence (EDXRF) technique for the analysis of geological, biological and environmental samples is described. The technique has been applied in the analysis of 10 (geological, biological, environmental) standard reference materials. The accuracy and precision of the technique were attested ...

  6. 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.

  7. Compact energy dispersive X-ray microdiffractometer for diagnosis of neoplastic tissues

    Science.gov (United States)

    Sosa, C.; Malezan, A.; Poletti, M. E.; Perez, R. D.

    2017-08-01

    An energy dispersive X-ray microdiffractometer with capillary optics has been developed for characterizing breast cancer. The employment of low divergence capillary optics helps to reduce the setup size to a few centimeters, while providing a lateral spatial resolution of 100 μm. The system angular calibration and momentum transfer resolution were assessed by a detailed study of a polycrystalline reference material. The performance of the system was tested by means of the analysis of tissue-equivalent samples previously characterized by conventional X-ray diffraction. In addition, a simplified correction model for an appropriate comparison of the diffraction spectra was developed and validated. Finally, the system was employed to evaluate normal and neoplastic human breast samples, in order to determine their X-ray scatter signatures. The initial results indicate that the use of this compact energy dispersive X-ray microdiffractometer combined with a simplified correction procedure is able to provide additional information to breast cancer diagnosis.

  8. 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.

  9. Energy dispersive X-ray spectroscopy with microcalorimeters

    International Nuclear Information System (INIS)

    Hollerith, C.; Wernicke, D.; Buehler, M.; Feilitzsch, F. von; Huber, M.; Hoehne, J.; Hertrich, T.; Jochum, J.; Phelan, K.; Stark, M.; Simmnacher, B.; Weiland, W.; Westphal, W.

    2004-01-01

    Shrinking feature sizes in semiconductor device production as well as the use of new materials demand innovation in device technology and material analysis. X-ray spectrometers based on superconducting sensor technology are currently closing the gap between fast energy dispersive spectroscopy (EDS) and high-resolution wavelength dispersive spectroscopy (WDS). This work reports on the successful integration of iridium/gold transition edge sensors in the first industrially used microcalorimeter EDS. The POLARIS microcalorimeter system is installed at the failure analysis lab FA5 at Infineon Technologies AG in Neuperlach (Munich) and is used in routine analysis

  10. 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 (0X-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.)

  11. 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

  12. 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

  13. Submicron X-ray diffraction

    International Nuclear Information System (INIS)

    MacDowell, Alastair; Celestre, Richard; Tamura, Nobumichi; Spolenak, Ralph; Valek, Bryan; Brown, Walter; Bravman, John; Padmore, Howard; Batterman, Boris; Patel, Jamshed

    2000-01-01

    At the Advanced Light Source in Berkeley the authors have instrumented a beam line that is devoted exclusively to x-ray micro diffraction problems. By micro diffraction they mean those classes of problems in Physics and Materials Science that require x-ray beam sizes in the sub-micron range. The instrument is for instance, capable of probing a sub-micron size volume inside micron sized aluminum metal grains buried under a silicon dioxide insulating layer. The resulting Laue pattern is collected on a large area CCD detector and automatically indexed to yield the grain orientation and deviatoric (distortional) strain tensor of this sub-micron volume. A four-crystal monochromator is then inserted into the beam, which allows monochromatic light to illuminate the same part of the sample. Measurement of diffracted photon energy allows for the determination of d spacings. The combination of white and monochromatic beam measurements allow for the determination of the total strain/stress tensor (6 components) inside each sub-micron sized illuminated volume of the sample

  14. Conservation of Moroccan manuscript papers aged 150, 200 and 800 years. Analysis by infrared spectroscopy (ATR-FTIR), X-ray diffraction (XRD), and scanning electron microscopy energy dispersive spectrometry (SEM-EDS).

    Science.gov (United States)

    Hajji, Latifa; Boukir, Abdellatif; Assouik, Jamal; Lakhiari, Hamid; Kerbal, Abdelali; Doumenq, Pierre; Mille, Gilbert; De Carvalho, Maria Luisa

    2015-02-05

    The preservation of manuscripts and archive materials is a serious problem for librarians and restorers. Paper manuscript is subjected to numerous degradation factors affecting their conservation state. This research represents an attempt to evaluate the conservation restoration process applied in Moroccan libraries, especially the alkaline treatment for strengthening weakened paper. In this study, we focused on six samples of degraded and restored paper taken from three different Moroccan manuscripts aged 150, 200 and 800 years. In addition, the Japanese paper used in restoration has been characterized. A modern paper was also analyzed as reference. A three-step analytical methodology based on infrared spectroscopy (ATR-FTIR), X-ray diffraction (XRD) and scanning electron microscopy coupled to energy dispersive spectrometry (SEM-EDS) analysis was developed before and after restoration in order to determine the effect of the consolidation treatment on the paper structure. The results obtained by XRD and ATR-FTIR disclosed the presence of barium sulfate (BaSO4) in all restored paper manuscripts. The presence of calcium carbonate (CaCO3) in all considered samples was confirmed by FTIR spectroscopy. The application of de-acidification treatment causes significant changes connected with the increase of intensity mostly in the region 1426 cm(-1), assigned to the asymmetric and symmetric CO stretching mode of calcite, indicating the effectiveness of de-acidification procedure proved by the rise of the alkaline reserve content allowing the long term preservation of paper. Observations performed by SEM magnify the typical paper morphology and the structure of fibbers, highlighting the effect of the restoration process, manifested by the reduction of impurities. Copyright © 2014 Elsevier B.V. All rights reserved.

  15. The use of combined three-dimensional electron backscatter diffraction and energy dispersive X-ray analysis to assess the characteristics of the gamma/gamma-prime microstructure in alloy 720Li™

    International Nuclear Information System (INIS)

    Child, D.J.; West, G.D.; Thomson, R.C.

    2012-01-01

    Multiple three-dimensional reconstructions of a γ/γ′ phase structure in Alloy 720Li have been carried out by employing a serial milling technique with simultaneous electron backscatter diffraction (EBSD) and energy dispersive x-ray (EDX) analysis data collection. Combining EBSD data with EDX is critical in obtaining maps to distinguish between the chemically differing, but crystallographically similar γ and γ′ phases present in the alloy studied. EDX is shown to allow the differentiation of γ and γ′ phases, with EBSD providing increased grain shape accuracy. The combination of data sources also allowed identification of coherent γ/γ′ phase interfaces that would not be identified using solely EBSD or EDX. The study identifies a region of grain banding within the alloy, which provides the basis for a three-dimensional comparison and discussion of γ′ phase size between coarse and fine grain regions, whilst also identifying coherent γ′ phase interfaces, possible only using both EDX and EBSD systems simultaneously. The majority of the γ′ phase lies in the range of 1–10 μm in non-banded regions, with a detectable particle size limit of 500 nm being established. The validity of the reconstruction has been demonstrated using an electron interaction volumes model, and an assessment of the validity of EBSD and EDX data sources is discussed showing γ′ phase connectivity in all dimensions. -- Highlights: ► Use of combined EBSD/EDX for the 3D analysis of gamma prime in a Ni-based alloy. ► Assessment of 3D reconstruction accuracy using CASINO. ► Observation and validation of gamma prime phase connectivity throughout the alloy. ► Identification and characterisation of grain banding in gamma prime. ► Distinction of phase coherency between gamma and gamma prime.

  16. The use of combined three-dimensional electron backscatter diffraction and energy dispersive X-ray analysis to assess the characteristics of the gamma/gamma-prime microstructure in alloy 720Li Trade-Mark-Sign

    Energy Technology Data Exchange (ETDEWEB)

    Child, D.J., E-mail: d.child@lboro.ac.uk [Department of Materials, Loughborough University, Loughborough, Leicestershire, LE11 3TU (United Kingdom); West, G.D., E-mail: g.west@lboro.ac.uk [Department of Materials, Loughborough University, Loughborough, Leicestershire, LE11 3TU (United Kingdom); Thomson, R.C., E-mail: r.c.thomson@lboro.ac.uk [Department of Materials, Loughborough University, Loughborough, Leicestershire, LE11 3TU (United Kingdom)

    2012-03-15

    Multiple three-dimensional reconstructions of a {gamma}/{gamma} Prime phase structure in Alloy 720Li have been carried out by employing a serial milling technique with simultaneous electron backscatter diffraction (EBSD) and energy dispersive x-ray (EDX) analysis data collection. Combining EBSD data with EDX is critical in obtaining maps to distinguish between the chemically differing, but crystallographically similar {gamma} and {gamma} Prime phases present in the alloy studied. EDX is shown to allow the differentiation of {gamma} and {gamma} Prime phases, with EBSD providing increased grain shape accuracy. The combination of data sources also allowed identification of coherent {gamma}/{gamma} Prime phase interfaces that would not be identified using solely EBSD or EDX. The study identifies a region of grain banding within the alloy, which provides the basis for a three-dimensional comparison and discussion of {gamma} Prime phase size between coarse and fine grain regions, whilst also identifying coherent {gamma} Prime phase interfaces, possible only using both EDX and EBSD systems simultaneously. The majority of the {gamma} Prime phase lies in the range of 1-10 {mu}m in non-banded regions, with a detectable particle size limit of 500 nm being established. The validity of the reconstruction has been demonstrated using an electron interaction volumes model, and an assessment of the validity of EBSD and EDX data sources is discussed showing {gamma} Prime phase connectivity in all dimensions. -- Highlights: Black-Right-Pointing-Pointer Use of combined EBSD/EDX for the 3D analysis of gamma prime in a Ni-based alloy. Black-Right-Pointing-Pointer Assessment of 3D reconstruction accuracy using CASINO. Black-Right-Pointing-Pointer Observation and validation of gamma prime phase connectivity throughout the alloy. Black-Right-Pointing-Pointer Identification and characterisation of grain banding in gamma prime. Black-Right-Pointing-Pointer Distinction of phase coherency

  17. Certification of reference materials by energy-dispersive x-ray fluorescence spectrometry?

    DEFF Research Database (Denmark)

    Christensen, Leif Højslet; Heydorn, Kaj

    1985-01-01

    This paper studies the precision and accuracy that can be achieved using energy-dispersive x-ray fluorescence spectrometry for the determination of total sulphur content in BCR 38 Fly Ash issued by the European Community Bureau of Reference.......This paper studies the precision and accuracy that can be achieved using energy-dispersive x-ray fluorescence spectrometry for the determination of total sulphur content in BCR 38 Fly Ash issued by the European Community Bureau of Reference....

  18. Diffractive X-Ray Telescopes

    International Nuclear Information System (INIS)

    Skinner, G.K.; Skinner, G.K

    2010-01-01

    Diffractive X-ray telescopes using zone plates, phase Fresnel lenses, or related optical elements have the potential to provide astronomers with true imaging capability with resolution several orders of magnitude better than available in any other waveband. Lenses that would be relatively easy to fabricate could have an angular resolution of the order of micro arc seconds or even better, that would allow, for example, imaging of the distorted spacetime in the immediate vicinity of the supermassive black holes in the center of active galaxies What then is precluding their immediate adoption Extremely long focal lengths, very limited bandwidth, and difficulty stabilizing the image are the main problems. The history and status of the development of such lenses is reviewed here and the prospects for managing the challenges that they present are discussed atmospheric absorption

  19. 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)

  20. 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

  1. X-ray diffraction studies of NbTe 2 single crystal

    Indian Academy of Sciences (India)

    The composition of the grown crystals was confirmed on the basis of energy dispersive analysis by X-ray (EDAX) and remaining structural characterization was also accomplished by X-ray diffraction (XRD) studies. Lattice parameters, volume and X-ray density have been carried out for the grown crystals. The particle size ...

  2. X-ray topography and multiple diffraction

    International Nuclear Information System (INIS)

    Chang, S.-L.

    1983-01-01

    A short summary on X-ray topography, which is based on the dynamical theory of X-ray diffraction, is made. The applications and properties related to the use of the multiple diffraction technique are analized and discussed. (L.C.) [pt

  3. 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.

  4. 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

  5. A low power x-ray tube for use in energy dispersive x-ray fluorescence analysis

    International Nuclear Information System (INIS)

    Kataria, S.K.; Govil, Rekha; Lal, M.

    1980-01-01

    A low power X-ray tube with thin molybdenum transmission target for use in energy dispersive X-ray fluorescence (ENDXRF) element analysis has been indigenously built, along with its power supply. The X-ray tube has been in operation since August 1979, and it has been operated upto maximum target voltage of 35 KV and tube current upto 200 μA which is more than sufficient for trace element analysis. This X-ray tube has been used alongwith the indigenously built Si(Li) detector X-ray spectrometer with an energy resolution of 200 eV at 5.9 Kev MnKsub(α) X-ray peak for ENDXRF analysis. A simple procedure of calibration has been developed for thin samples based on the cellulose diluted, thin multielement standard pellets. Analytical sensitivities of the order of a few p.p.m. have been obtained with the experimental setup for elements with 20 < = Z < = 38 and 60 < = Z < = 90. A number of X-ray spectra for samples of environmental, biological, agricultural, industrial and metallurgical interest are presented to demonstrate the salient features of the experimental sep up. (auth.)

  6. X-ray fluorescence spectrometers: a comparison of wavelength and energy dispersive instruments

    International Nuclear Information System (INIS)

    Slates, R.V.

    1977-11-01

    Wavelength dispersive and energy dispersive x-ray fluorescence spectrometers are compared. Separate sections are devoted to principles of operation, sample excitation, spectral resolution, and x-ray detection. Tabulated data from the literature are cited in the comparison of accuracy, precision, and detection limits. Spectral interferences and distortions are discussed. Advantages and limitations are listed for simultaneous wavelength dispersive spectrometers, sequential wavelength dispersive spectrometers, and Si(Li) energy dispersive spectrometers. Accuracy, precision, and detection limits are generally superior for wavelength dispersive spectrometers

  7. Energy dispersion X-ray fluorescence techniques in water pollution analysis

    International Nuclear Information System (INIS)

    Holynska, B.

    1980-01-01

    Advantages and limitations of energy dispersion X-ray fluorescence methods for analysis of pollutants in water are discussed. The necessary equipment for X-ray measurement of insoluble and dissolved trace metals in water is described. Different techniques of enrichment of trace metals are presented: ion exchange on selective Chelex-100 exchanger, precipitation with chelating agents DDTC and APDC, and adsorption on activated carbon. Some results obtained using different preconcentration methods for trace metals determination in different waters are presented. (author)

  8. X-ray diffraction 2 - diffraction principles

    International Nuclear Information System (INIS)

    O'Connor, B.

    1999-01-01

    Full text: The computation of powder diffraction intensities is based on the principle that the powder pattern comprises the summation of the intensity contributions from each of the crystallites (or single crystals) in the material. Therefore, it is of value for powder diffractionists to appreciate the form of the expression for calculating single crystal diffraction pattern intensities. This knowledge is especially important for Rietveld analysis practitioners in terms of the (i) mathematics of the method and (ii) retrieving single crystal structure data from the literature. We consider the integrated intensity from a small single crystal being rotated at velocity ω through the Bragg angle θ for reflection (hkl).... I(hkl) = [l o /ω]. [e 4 /m 2 c 4 ]. [λ 3 δV F(hkl) 2 /υ 2 ].[(1+cos 2 2θ)/2sin2θ] where e, m and c are the usual fundamental constants; λ is the x-ray wavelength, δV is the crystallite volume; F(hkl) is the structure factor; υ is the unit cell volume; and (1+cos 2 θ)/2sin2θ] is the Lorentz-polarisation factor for an unpolarised incident beam. The expression does not include a contribution for extinction. The influence of factors λ, δV, F(hkl) and υ on the intensities should be appreciated by powder diffractionists, especially the structure factor, F(hkl), which is responsible for the fingerprint nature of diffraction patterns, such as the rise and fall of intensity from peak to peak. The structure factor expression represents the summation of the scattered waves from each of the j scattering centres (i e atoms) in the unit cell: F(hkl) Σ f j exp[2πi (h.x j +k.y i +l. z i )] T j . Symbol f is the scattering factor (representing the atom-type scattering efficiency); (x, y, z) are the fractional position coordinates of atom j within the unit cell; and T is the thermal vibration factor for the atom given by: T j = 8π 2 2 > sin 2 θ/λ 2 with 2 > being the mean-square vibration amplitude of the atom (assumed to be isotropic). The

  9. Energy dispersive X-ray diffractometry in texture studies

    International Nuclear Information System (INIS)

    Szpunar, J.A.

    1983-01-01

    Information about texture is traditionally obtained from the two-dimensional distributions of crystallographic directions in the reference frame of the specimen. The distributions can be measured using the angular dispersive diffractometry. In such measurements the rotation of the specimen brings the crystallographic planes of differently oriented crystals into the diffraction position. The distribution (pole figure) can be measured continuously or alternatively the angular space can be scanned in different directions and with required accuracy. The subject is discussed, with examples. (author)

  10. Two-dimensional x-ray diffraction

    CERN Document Server

    He, Bob B

    2009-01-01

    Written by one of the pioneers of 2D X-Ray Diffraction, this useful guide covers the fundamentals, experimental methods and applications of two-dimensional x-ray diffraction, including geometry convention, x-ray source and optics, two-dimensional detectors, diffraction data interpretation, and configurations for various applications, such as phase identification, texture, stress, microstructure analysis, crystallinity, thin film analysis and combinatorial screening. Experimental examples in materials research, pharmaceuticals, and forensics are also given. This presents a key resource to resea

  11. Quantitative schemes in energy dispersive X-ray fluorescence implemented in AXIL

    International Nuclear Information System (INIS)

    Tchantchane, A.; Benamar, M.A.; Tobbeche, S.

    1995-01-01

    E.D.X.R.F (Energy Dispersive X-ray Fluorescence) has long been used for quantitative analysis of many types of samples including environment samples. the software package AXIL (Analysis of x-ray spectra by iterative least quares) is extensively used for the spectra analysis and the quantification of x-ray spectra. It includes several methods of quantitative schemes for evaluating element concentrations. We present the general theory behind each scheme implemented into the software package. The spectra of the performance of each of these quantitative schemes. We have also investigated their performance relative to the uncertainties in the experimental parameters and sample description

  12. 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.…

  13. 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

  14. 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 ...

  15. 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)

  16. 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).

  17. 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)

  18. 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.

  19. 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)

  20. Diffraction enhanced x-ray imaging

    International Nuclear Information System (INIS)

    Thomlinson, W.; Zhong, Z.; Johnston, R.E.; Sayers, D.

    1997-09-01

    Diffraction enhanced imaging (DEI) is a new x-ray radiographic imaging modality using synchrotron x-rays which produces images of thick absorbing objects that are almost completely free of scatter. They show dramatically improved contrast over standard imaging applied to the same phantoms. The contrast is based not only on attenuation but also the refraction and diffraction properties of the sample. The diffraction component and the apparent absorption component (absorption plus extinction contrast) can each be determined independently. This imaging method may improve the image quality for medical applications such as mammography

  1. 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.

  2. 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)

  3. Energy dispersive x-ray spectrometry by microcalorimetry for the SEM

    CERN Document Server

    Newbury, D; Sae Woo Nam; Hilton, G; Irwin, K; Small, J; Martinis, J

    2002-01-01

    Analytical x-ray spectrometry for electron beam instruments has advanced significantly with the development of the microcalorimeter energy dispersive x-ray spectrometer (mu cal EDS). The mu cal EDS operates by measuring the temperature rise when a single photon is absorbed in a metal target. A cryoelectronic circuit with electrothermal feedback and a superconducting transition edge sensor serves as the thermometer. Spectral resolution approaching 4.5 eV for high energy photons (6000 eV) and 2 eV for low energy photons below 2000 eV has been demonstrated in energy dispersive operation across a photon energy range from 250 eV to 8 keV. Spectra of a variety of materials demonstrate the power of the mu cal EDS to solve practical problems while operating on a scanning electron microscope platform. (author)

  4. 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)

  5. 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.

  6. 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

  7. X-ray filter for x-ray powder diffraction

    Science.gov (United States)

    Sinsheimer, John Jay; Conley, Raymond P.; Bouet, Nathalie C. D.; Dooryhee, Eric; Ghose, Sanjit

    2018-01-23

    Technologies are described for apparatus, methods and systems effective for filtering. The filters may comprise a first plate. The first plate may include an x-ray absorbing material and walls defining first slits. The first slits may include arc shaped openings through the first plate. The walls of the first plate may be configured to absorb at least some of first x-rays when the first x-rays are incident on the x-ray absorbing material, and to output second x-rays. The filters may comprise a second plate spaced from the first plate. The second plate may include the x-ray absorbing material and walls defining second slits. The second slits may include arc shaped openings through the second plate. The walls of the second plate may be configured to absorb at least some of second x-rays and to output third x-rays.

  8. 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

  9. Structural investigation of GaInP nanowires using X-ray diffraction

    DEFF Research Database (Denmark)

    Kriegner, D.; Persson, Johan Mikael; Etzelstorfer, T.

    2013-01-01

    In this work the structure of ternary GaxIn1−xP nanowires is investigated with respect to the chemical composition and homogeneity. The nanowires were grown by metal–organic vapor-phase epitaxy. For the investigation of ensemble fluctuations on several lateral length scales, X-ray diffraction...... gradients along the sample by recording diffraction patterns at different positions. In addition, compositional variations were found also within single nanowires in X-ray energy dispersive spectroscopy measurements....

  10. X-ray diffraction device comprising cooling medium connections provided on the x-ray tube

    NARCIS (Netherlands)

    1996-01-01

    An X-ray diffraction device comprises a water-cooled X-ray tube which exhibits a line focus as well as, after rotation through 90 DEG , a point focus. Contrary to customary X-ray tubes, the cooling water is not supplied via the housing (12) in which the X-ray tube is mounted, but the cooling water

  11. 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)

  12. 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)

  13. 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)

  14. 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)

  15. 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.

  16. 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.

  17. Polarisation resonance in X-ray diffraction

    International Nuclear Information System (INIS)

    Goodman, P.; Paterson, D.; Matheson, S.

    1994-01-01

    The study of crystal structures by means of dynamic X-ray diffraction has placed a challenge to theoreticians to revise the X-ray diffraction theory based on Maxwell's equation. In this paper the feasibility of using 'polarisation resonance' as a tool in the determination of absolute configuration for asymmetric structures is investigated. Two (left- and right-handed), σ + and σ- , circular polarization states for 3-beam conditions are considered. Moreover, extending interaction into the 3 rd. dimension (normal to the beam) opens the possibility of absolute configuration determination of asymmetric structures in 3 dimensions. The computational scheme used is shown in terms of scattering diagrams. 7 refs., 1 tab., 6 figs

  18. 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

  19. 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

  20. 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....

  1. 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

  2. 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.)

  3. Basic of X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Giacovazzo, C [Bari Univ. (Italy). Dip. Geomineralogico

    1996-09-01

    The basic concepts of X-ray diffraction may be more easily understood if it is made preliminary use of a mathematical background. In these pages the authors will first define the delta function and its use for the representation of a lattice. Then the concepts of Fourier transform and convolution are given. At the end of this talk one should realize that a crystal is the convolution of the lattice with a function representing the content of the unit cell.

  4. Basic of X-ray diffraction

    International Nuclear Information System (INIS)

    Giacovazzo, C.

    1996-01-01

    The basic concepts of X-ray diffraction may be more easily understood if it is made preliminary use of a mathematical background. In these pages the authors will first define the delta function and its use for the representation of a lattice. Then the concepts of Fourier transform and convolution are given. At the end of this talk one should realize that a crystal is the convolution of the lattice with a function representing the content of the unit cell

  5. 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

  6. 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)

  7. 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.

  8. Glancing angle synchrotron X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Cernik, R J [Daresbury Lab., Warrington, WA (United States)

    1996-09-01

    This paper describes in basic detail some of the techniques that can be used to study thin films and surfaces. These are all in the X-ray region and cover reflectivity, diffraction form polycrystalline films, textured films and single crystal films. Other effects such as fluorescence and diffuse scattering are mentioned but not discussed in detail. Two examples of the reflectivity from multilayers and the diffraction from iron oxide films are discussed. The advantages of the synchrotron for these studies is stressed and the experimental geometries that can be employed are described i detail. A brief bibliography is provided at the end to accompany this part of the 1996 Frascati school.

  9. X-ray diffraction and chemical bonding

    International Nuclear Information System (INIS)

    Bats, J.W.

    1976-01-01

    Chemical bonds are investigated in sulfamic acid (H 3 N-SO 3 ), sodium sulfonlate dihydrate (H 2 NC 6 H 4 SO 3 Na.2H 2 O), 2,5-dimercaptothiadiazole (HS-C 2 N 2 S-SH), sodium cyanide dihydrate (NaCN.2H 2 O), sodium thiocyanate (NaSCN) and ammonium thiocyanate (NH 4 SCN) by X-ray diffraction, and if necessary completed with neutron diffraction. Crystal structures and electron densities are determined together with bond length and angles. Also the effects of thermal motion are discussed

  10. Glancing angle synchrotron X-ray diffraction

    International Nuclear Information System (INIS)

    Cernik, R.J.

    1996-01-01

    This paper describes in basic detail some of the techniques that can be used to study thin films and surfaces. These are all in the X-ray region and cover reflectivity, diffraction form polycrystalline films, textured films and single crystal films. Other effects such as fluorescence and diffuse scattering are mentioned but not discussed in detail. Two examples of the reflectivity from multilayers and the diffraction from iron oxide films are discussed. The advantages of the synchrotron for these studies is stressed and the experimental geometries that can be employed are described i detail. A brief bibliography is provided at the end to accompany this part of the 1996 Frascati school

  11. 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

  12. 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

  13. 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)

  14. 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

  15. 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.

  16. 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.

  17. 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.

  18. 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.

  19. 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)

  20. 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

  1. 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)

  2. 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

  3. 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)

  4. 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)

  5. 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.

  6. 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.

  7. 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.

  8. 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

  9. 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.

  10. 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

  11. X-ray diffraction imaging of material microstructures

    KAUST Repository

    Varga, Laszlo

    2016-10-20

    Various examples are provided for x-ray imaging of the microstructure of materials. In one example, a system for non-destructive material testing includes an x-ray source configured to generate a beam spot on a test item; a grid detector configured to receive x- rays diffracted from the test object; and a computing device configured to determine a microstructure image based at least in part upon a diffraction pattern of the x-rays diffracted from the test object. In another example, a method for determining a microstructure of a material includes illuminating a beam spot on the material with a beam of incident x-rays; detecting, with a grid detector, x-rays diffracted from the material; and determining, by a computing device, a microstructure image based at least in part upon a diffraction pattern of the x-rays diffracted from the material.

  12. 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.

  13. Diffracted X-ray tracking: new system for single molecular detection with X-rays

    CERN Document Server

    Sasaki, Y C; Adachi, S; Suzuki, Y; Yagi, N

    2001-01-01

    We propose a new X-ray methodology for direct observations of the behaviors of single molecular units in real time and real space. This new system, which we call Diffracted X-ray Tracking (DXT), monitors the Brownian motions of a single molecular unit by observations of X-ray diffracted spots from a nanocrystal, tightly bound to the individual single molecular unit in bio-systems. DXT does not determine any translational movements, but only orientational movements.

  14. Diffracted X-ray tracking: new system for single molecular detection with X-rays

    International Nuclear Information System (INIS)

    Sasaki, Y.C.; Okumura, Y.; Adachi, S.; Suzuki, Y.; Yagi, N.

    2001-01-01

    We propose a new X-ray methodology for direct observations of the behaviors of single molecular units in real time and real space. This new system, which we call Diffracted X-ray Tracking (DXT), monitors the Brownian motions of a single molecular unit by observations of X-ray diffracted spots from a nanocrystal, tightly bound to the individual single molecular unit in bio-systems. DXT does not determine any translational movements, but only orientational movements

  15. 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.

  16. 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.

  17. 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

  18. 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...

  19. 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

  20. 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

  1. 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)

  2. 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)

  3. 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.

  4. 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.

  5. 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

  6. 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

  7. 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.

  8. A high resolution position sensitive X-ray MWPC for small angle X-ray diffraction

    International Nuclear Information System (INIS)

    Bateman, J.E.; Connolly, J.F.; Stephenson, R.; Tappern, G.J.

    1981-02-01

    A small sealed-off delay line readout MWPC X-ray detector has been designed and built for small angle X-ray diffraction applications. Featuring a sensitive area of 100 mm x 25 mm it yields a spatial resolution of 0.13 mm (standard deviation) with a high rate capability and good quantum efficiency for copper K radiation. (author)

  9. 100 years of discovery of X-ray diffraction

    International Nuclear Information System (INIS)

    Zhang Tao

    2012-01-01

    X-ray diffraction was discovered by Max von Laue a hundred years ago. Later, through the work of William H. Bragg and William L. Bragg, an experimental analysis method was developed to solve the structure of molecules at the atomic level. Over the past hundred years, science and technology has been dramatically changed by X-ray diffraction analysis, which has also undergone considerable development. The recent emergence of hard X-ray free electron lasers has provided a new dimension for X-ray diffraction analysis, promising even greater progress in the fields of physics, chemistry and biology. (author)

  10. 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

  11. Characterization of Metalloproteins and Biomaterials by X-ray Absorption Spectroscopy and X-ray Diffraction

    DEFF Research Database (Denmark)

    Frankær, Christian Grundahl

    This thesis presents thework on combining complementary X-rays techniques for studying the structures of proteins and other biomaterials, and consists of three different projects: (i) Characterization of protein powders with X-ray powder diffraction (XRPD). (ii) The combination of X-ray...... crystallography and X-ray absorption spectroscopy (XAS) applied to studying different hexameric insulin conformations. (iii) The structures of polymorphs of strontium ranelate and the distribution of strontium in bone tissue. A procedure for fast identification and verification of protein powders using XRPD...... was correction for disordered bulk-solvent, but also correction for background and optimization of unit cell parameters have to be taken into account. A sample holder was designed for collecting powder diffraction data on a standard laboratory X-ray powder diffractometer. The background was reduced by use...

  12. Depth profiling: RBS versus energy-dispersive X-ray imaging using scanning transmission electron microscopy

    International Nuclear Information System (INIS)

    Markwitz, Andreas

    2000-01-01

    Rutherford backscattering spectrometry (RBS) is known to be one of the techniques ideal for analysis of thin films. Elemental concentrations of matrix components and impurities can be investigated as well as depth profiles of almost each element of the periodic table. Best of all, RBS has both a high sensitivity and a high depth resolution, and is a non-destructive analysis technique that does not require specific sample preparation. Solid-state samples are mounted without preparation inside a high-vacuum analysis chamber. However, depth-related interpretation of elemental depth profiles requires the material density of the specimen and stopping power values to be taken into consideration. In many cases, these parameters can be estimated with sufficient precision. However, the assumed density can be inaccurate for depth scales in the nanometer range. For example, in the case of Ge nanoclusters in 500 nm thick SiO 2 layers, uncertainty is related to the actual position of a very thin Ge nanocluster band. Energy-dispersive X-ray emission (EDX) spectroscopy, using a high-resolution scanning transmission electron microscope (STEM) can assist in removing this uncertainty. By preparing a thin section of the specimen, EDX can be used to identify the position of the Ge nanocluster band very precisely, by correlating the Ge profile with the depth profiles of silicon and oxygen. However, extraction of the concentration profiles from STEM-EDX spectra is in general not straightforward. Therefore, a combination of the two very different analysis techniques is often the best and only successful way to extract high-resolution concentration profiles

  13. Elemental contents in exotic Brazilian tropical fruits evaluated by energy dispersive X-ray fluorescence

    Directory of Open Access Journals (Sweden)

    Oliveira Alessandra Lopes de

    2006-01-01

    Full Text Available The exotic flavor of Brazilian tropical fruits led to increased consumption. Consumers awareness regarding balanced diets, makes necessary determining nutritional composition - vitamins and minerals of the fruits ordinarily consumed. This study contributed to the evaluation of macro (K, Ca and microelements (Mn, Fe, Cu, Zn and Br in eight exotic Brazilian tropical fruits: "abiu" (Lucuma caimito Ruiz & Pav., "jenipapo" (Genipa americana L., "jambo rosa" (rose apple, Eugenia Jambos L., "jambo vermelho" (Syzygium malaccence L., Merr & Perry, "macaúba" (Acrocomia aculeata Jacq. Lood. Ex Mart., "mangaba" (Hancornia speciosa, "pitanga" (Brazilian Cherry, Eugenia uniflora L., and tamarind (Tamarindus indica L., using the Energy Dispersive X-Ray Fluorescence (EDXRF technique. "jambo vermelho" and "macaúba" presented the highest values of K concentrations, 1,558 and 1,725 mg 100 g-1, respectively. On the other hand, Ca concentrations were highest in "macaúba" (680 mg 100 g-1 and "jenipapo" (341 mg 100 g-1. The microelemental concentrations in these eight fruits ranged from: 0.9 to 2.0 mg 100 g-1 for Mn, 3.9 to 11.4 mg 100 g-1 for Fe, 0.5 to 1.0 mg 100 g-1 for Cu, 0.6 to 1.5 mg 100 g-1 for, Zn and 0.3 to 1.3 mg 100 g-1 for Br. The amounts of macro and microelements in the eight fruits analyzed were compared to other tropical fruits and it was found that some of them could be classified as rich sources for these macro and microelements.

  14. 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)

  15. Thin film characterisation by advanced X-ray diffraction techniques

    International Nuclear Information System (INIS)

    Cappuccio, G.; Terranova, M.L.

    1996-09-01

    The Fifth School on X-ray diffraction from polycrystalline materials was devoted to thin film characterization by advanced X-ray diffraction techniques. Twenty contributions are contained in this volume; all twenty are recorded in the INIS Database. X-ray diffraction is known to be a powerful analytical tool for characterizing materials and understanding their structural features. The aim of these articles is to illustrate the fundamental contribution of modern diffraction techniques (grazing incidence, surface analysis, standing waves, etc.) to the characterization of thin and ultra-thin films, which have become important in many advanced technologies

  16. X-ray Microprobe for Fluorescence and Diffraction Analysis

    International Nuclear Information System (INIS)

    Ice, G.E.

    2005-01-01

    X-ray diffraction (see unit 1.1) and x-ray excited fluorescence analysis are powerful techniques for the nondestructive measurement of crystal structure and chemical composition. X-ray fluorescence analysis is inherently nondestructive with orders of magnitude lower power deposited for the same detectable limit as with fluorescence excited by charged particle probes (Sparks, 1980). X-ray diffraction analysis is sensitive to crystal structure with orders-of-magnitude greater sensitivity to crystallographic strain than electron probes (Rebonato, et al. 1989). When a small-area x-ray microbeam is used as the probe, chemical composition (Z>14), crystal structure, crystalline texture, and crystalline strain distributions can be determined. These distributions can be studied both at the surface of the sample and deep within the sample (Fig. 1). Current state-of-the-art can achieve an ∼1 mm-D x-ray microprobe and an ∼0.1 mm-D x-ray microprobe has been demonstrated (Bilderback, et al., 1994). Despite their great chemical and crystallographic sensitivities, x-ray microprobe techniques have until recently been restricted by inefficient x-ray focusing optics and weak x-ray sources; x-ray microbeam analysis was largely superseded by electron techniques in the 50's. However, interest in x-ray microprobe techniques has now been revived (Howells, et al., 1983; Ice and Sparks, 1984; Chevallier, et al., 1997; Riekel 1992; Thompson, el al., 1992; and Making and Using... 1997) by the development of efficient x-ray focusing optics and ultra-high intensity synchrotron x-ray sources (Buras and Tazzari, 1984; Shenoy, et al., 1988). These advances have increased the achievable microbeam flux by more than 11 orders of magnitude (Fig. 2) (Ice, 1997); the flux in a tunable 1 mm-D beam on a 'so called' 3rd-generation synchrotron source such as the APS can exceed the flux in a fixed-energy mm2 beam on a conventional source. These advances make x-ray microfluorescence and x-ray

  17. Historical development of synchrotron x-ray diffraction topography

    International Nuclear Information System (INIS)

    Kawado, Seiji

    2011-01-01

    After a short history of X-ray diffraction topography, from the early stage of laboratory X-ray topography to recent synchrotron-radiation applications, is described, the development of science and technology for the synchrotron X-ray topography and its industrial applications are reviewed in more detail. In addition, the recent trend to synchrotron topography research is clarified on the basis of several data obtained from 256 papers which have been published since 2000. (author)

  18. Diffraction peaks in x-ray spectroscopy: Friend or foe?

    International Nuclear Information System (INIS)

    Tissot, R.G.; Goehner, R.P.

    1992-01-01

    Diffraction peaks can occur as unidentifiable peaks in the energy spectrum of an x-ray spectrometric analysis. Recently, there has been increased interest in oriented polycrystalline films and epitaxial films on single crystal substrates for electronic applications. Since these materials diffract x-rays more efficiently than randomly oriented polycrystalline materials, diffraction peaks are being observed more frequently in x-ray fluorescent spectra. In addition, micro x-ray spectrometric analysis utilizes a small, intense, collimated x-ray beam that can yield well defined diffraction peaks. In some cases these diffraction peaks can occur at the same position as elemental peaks. These diffraction peaks, although a possible problem in qualitative and quantitative elemental analysis, can give very useful information about the crystallographic structure and orientation of the material being analyzed. The observed diffraction peaks are dependent on the geometry of the x-ray spectrometer, the degree of collimation and the distribution of wavelengths (energies) originating from the x-ray tube and striking the sample

  19. 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.

  20. Diffractive sub-picosecond manipulation of x-rays

    International Nuclear Information System (INIS)

    Adams, B.

    2004-01-01

    A class of X-ray optical elements for the sub-picosecond manipulation of X-rays is proposed. The design of these elements is based upon a time-dependent dynamical diffraction theory that synthesizes the eikonal theory with the Takagi-Taupin theory. A brief outline of the theory is given

  1. High-resolution X-ray diffraction studies of multilayers

    DEFF Research Database (Denmark)

    Christensen, Finn Erland; Hornstrup, Allan; Schnopper, H. W.

    1988-01-01

    High-resolution X-ray diffraction studies of the perfection of state-of-the-art multilayers are presented. Data were obtained using a triple-axis perfect-crystal X-ray diffractometer. Measurements reveal large-scale figure errors in the substrate. A high-resolution triple-axis set up is required...

  2. Preparation of specimens for analysis by: X-ray diffraction and X-ray fluorescence analysis

    International Nuclear Information System (INIS)

    Banos L, L.

    2004-01-01

    Specimen preparation is one of the most important requirements in the analysis of samples by X-ray Diffraction and X-ray Fluorescence. This statement is especially true for samples containing different types of materials. There are many forms of specimen suitable for X-ray analysis and the type of the sample as received will generally determine the method of pretreatment. It is convenient to refer to the material received for analysis as the sample, and that, which is actually analyzed as the specimen. The powder Diffraction method assumes that the particles in the specimen are ideally random orientation and that there are enough crystallites in the specimen to achieve a representative intensity distribution for these crystallites. X ray Fluorescence is essentially a comparative method of analysis, it is vital that all standards and unknowns be presented to the spectrometer in a reproducible and identical manner. (Author) 3 refs., 6 figs

  3. 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.

  4. 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.

  5. A differential scanning calorimetric and X-ray diffraction

    Indian Academy of Sciences (India)

    X-ray diffraction analysis of the two groups demonstrated predominance of austenitic ... Discrete crystallographic structure and absence of multiple phases showed ... Division of Orthodontics, Indian Army, 10 Corps Dental Unit, C/O 56 APO, ...

  6. Thin film characterisation by advanced X-ray diffraction techniques

    Energy Technology Data Exchange (ETDEWEB)

    Cappuccio, G; Terranova, M L [eds.; INFN, Laboratori Nazionali di Frascati, Rome (Italy)

    1996-09-01

    This report described the papers presented at the 5. School on X-ray diffraction from polycrystalline materials held at Frascati (Rome) in 2-5 October 1996. A separate abstract was prepared for each of the papers.

  7. Synchrotron x-ray diffraction study of liquid surfaces

    DEFF Research Database (Denmark)

    Als-Nielsen, Jens Aage; Pershan, P.S.

    1983-01-01

    A spectrometer for X-ray diffraction and refraction studies of horizontal, free surfaces of liquids is described. As an illustration smetic-A layering at the surface of a liquid crystal is presented.......A spectrometer for X-ray diffraction and refraction studies of horizontal, free surfaces of liquids is described. As an illustration smetic-A layering at the surface of a liquid crystal is presented....

  8. X-ray diffraction identification of clay minerals by microcomputer

    International Nuclear Information System (INIS)

    Rodrigues, S.; Imasava, F.J.

    1988-01-01

    The identification of clay minerals by X-ray powder diffraction are done by searching an unknown pattern with a file of standard X-ray diffraction patterns. For this searching done by hand is necessary a long time. This paper shows a program in ''Basic'' language to be utilized in microcomputers for the math of the unknown pattern, using the high velocity of comparison of the microcomputer. A few minutes are used for the match. (author) [pt

  9. Theory of time-resolved inelastic x-ray diffraction

    DEFF Research Database (Denmark)

    Lorenz, Ulf; Møller, Klaus Braagaard; Henriksen, Niels Engholm

    2010-01-01

    Starting from a general theory of time-resolved x-ray scattering, we derive a convenient expression for the diffraction signal based on a careful analysis of the relevant inelastic scattering processes. We demonstrate that the resulting inelastic limit applies to a wider variety of experimental...... conditions than similar, previously derived formulas, and it directly allows the application of selection rules when interpreting diffraction signals. Furthermore, we present a simple extension to systems simultaneously illuminated by x rays and a laser beam....

  10. CCD-based X-ray detectors for X-ray diffraction studies

    International Nuclear Information System (INIS)

    Ito, K.; Amemiya, Y.

    1999-01-01

    CCD-based X-ray detectors are getting to be used for X-ray diffraction studies especially in the studies where real time (automated) measurements and time-resolved measurements are required. Principles and designs of two typical types of CCD-based detectors are described; one is ths system in which x-ray image intensifiers are coupled to maximize the detective quantum efficiency for time-resolved measurements, and the other is the system in which tapered optical fibers are coupled for the reduction of the image into the CCD, which is optimized for automated measurements for protein crystallography. These CCD-based X-ray detectors have an image distortion and non-uniformity of response to be corrected by software. Correction schemes which we have developed are also described. (author)

  11. 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)

  12. 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.)

  13. 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.

  14. The comparative study of contents of zinc and lead in ore samples of Namtu-Bawdwin Mine by wet analysis, X-ray fluorescence and X-ray diffraction methods

    Energy Technology Data Exchange (ETDEWEB)

    Kyaw-Soe,

    1990-05-01

    Lead-zinc ores taken from Namtu-Bawdwin area had been analyzed by wet processes in the Department of Chemistry, 1984. These ore samples have been analyzed by energy dispersive X-ray fluorescence method in the Department of Physics and X-ray diffraction method is also used to determine elements of lead and zinc compounds in these ore samples in the University`s Research Centre. In brief, we study comparatively the contents of lead and zinc and their compounds using the methods of wet processes, X-ray fluorescence and X-ray diffraction. (author).

  15. 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

  16. 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)

  17. 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

  18. 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.

  19. 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(®).

  20. 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.

  1. 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.

  2. 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.

  3. 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

  4. X-ray photoelectron spectroscopy, high-resolution X-ray diffraction ...

    Indian Academy of Sciences (India)

    the crystalline quality through full-width at half-maximum values. .... angular divergence of ∆α = 12 arc sec. X-rays generated from the monochromator were diffracted from (0 0 6) LiNbO3 atomic planes with the (+, −, −, +, +) geometry. [8].

  5. Spectroscopic imaging, diffraction, and holography with x-ray photoemission

    International Nuclear Information System (INIS)

    1992-02-01

    X-ray probes are capable of determining the spatial structure of an atom in a specific chemical state, over length scales from about a micron all the way down to atomic resolution. Examples of these probes include photoemission microscopy, energy-dependent photoemission diffraction, photoelectron holography, and X-ray absorption microspectroscopy. Although the method of image formation, chemical-state sensitivity, and length scales can be very different, these X-ray techniques share a common goal of combining a capability for structure determination with chemical-state specificity. This workshop will address recent advances in holographic, diffraction, and direct imaging techniques using X-ray photoemission on both theoretical and experimental fronts. A particular emphasis will be on novel structure determinations with atomic resolution using photoelectrons

  6. Spectroscopic imaging, diffraction, and holography with x-ray photoemission

    Energy Technology Data Exchange (ETDEWEB)

    1992-02-01

    X-ray probes are capable of determining the spatial structure of an atom in a specific chemical state, over length scales from about a micron all the way down to atomic resolution. Examples of these probes include photoemission microscopy, energy-dependent photoemission diffraction, photoelectron holography, and X-ray absorption microspectroscopy. Although the method of image formation, chemical-state sensitivity, and length scales can be very different, these X-ray techniques share a common goal of combining a capability for structure determination with chemical-state specificity. This workshop will address recent advances in holographic, diffraction, and direct imaging techniques using X-ray photoemission on both theoretical and experimental fronts. A particular emphasis will be on novel structure determinations with atomic resolution using photoelectrons.

  7. 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

  8. Crystallized solids characterization by X-ray diffraction

    International Nuclear Information System (INIS)

    Broll, N.

    1996-01-01

    This work deals with the crystallized solids characterization by X-ray diffraction. The powders diffraction principle is described. Then are given the different powders diffraction experimental methods. An X-ray diffraction device is essentially constituted of three parts: the X-rays source, the sample and the detector. The source is usually constituted by an X-rays tube whereas the sample can be fixed on a photographic chamber or put on a goniometer. The different photographic chambers which can be used (Debye-Scherrer, Seeman-Bohlin and Guinier) are described. The powders diffractometer the most used is a Bragg-Brentano focusing diffractometer because it allows to obtain very sharp spectral lines and an important diffracted intensity. The detectors which are the mainly used are the scintillation counters. The most important use in powders diffractometry is the identification of the different phases of a sample. The phases identification consists to compare the unknown sample spectrum at those of standard materials indexed until now. Two methods exist at present. They are explained and their limits in the phases search are given. Another use of the X-ray diffraction is the quantitative analysis. It consists to determine the concentrations of each crystal phases of a sample. The principles of these quantitative methods are given. The lattice parameters of a polycrystal material can be determined from its X-ray pattern too with a very high precision. The way to index powders patterns is given. The residual stresses of materials can also be estimated. The principle of this measured method is explained. It is at last possible to study from an X-ray pattern, the material grain orientations during the different steps of preparation and working. (O.M.). 13 refs., 19 figs., 1 tab

  9. X-ray diffraction topography. Stages and tendencies of development

    International Nuclear Information System (INIS)

    Shul'pina, I.L.

    2000-01-01

    The physical foundation of X-ray diffraction topography, its methods, the achievements in image theory, the stages of evolution were described in this review. It was found that modern topography is well along in development associated with the use of third-generation synchrotron radiation and with its adaptation to advance materials and problems of materials science. Some proposals about prospects for X-ray topography progress in the future have been made [ru

  10. X-ray diffraction microtomography using synchrotron radiation

    CERN Document Server

    Barroso, R C; Jesus, E F O; Oliveira, L F

    2001-01-01

    The X-ray diffraction computed tomography technique is based on the interference phenomena of the coherent scatter. For low-momentum transfer, it is most probable that the scattering interaction will be coherent. A selective discrimination of a given element in a scanned specimen can be realized by fixing the Bragg angle which produces an interference peak and then, to carry out the computed tomography in the standard mode. The image reconstructed exalts the presence of this element with respect to other ones in a sample. This work reports the feasibility of a non-destructive synchrotron radiation X-ray diffraction imaging technique. This research was performed at the X-ray Diffraction beam line of the National Synchrotron Light Laboratory (LNLS) in Brazil. The coherent scattering properties of different tissue and bone substitute materials were evaluated. Furthermore, diffraction patterns of some polycrystalline solids were studied due to industrial and environmental human exposure to these metals. The obtai...

  11. Three-dimensional x-ray diffraction detection and visualization

    International Nuclear Information System (INIS)

    Allahkarami, Masoud; Hanan, Jay C

    2014-01-01

    A new method of sensing and analyzing three-dimensional (3D) x-ray diffraction (XRD) cones was introduced. Using a two-dimensional area detector, a sequence of frames was collected while moving the detector away from the sample with small equally spaced steps and keeping all other parameters constant. A 3D dataset was created from the subsequent frames. The 3D x-ray diffraction (XRD 3 ) pattern contains far more information than a one-dimensional profile collected with the conventional diffractometer and 2D x-ray diffraction (XRD 2 ). The present work discusses some fundamentals about XRD 3 , such as the data collection method, 3D visualization, diffraction data interpretation and potential applications of XRD 3 . (paper)

  12. High resolution X-ray diffraction studies on unirradiated

    Indian Academy of Sciences (India)

    High-resolution X-ray diffraction technique, employing a three-crystal monochromator–collimator combination is used to study the irradiation induced defects in flux grown Sr-hexaferrite crystals irradiated with 50 MeV Li3+ ion beams at room temperature with a fluence value of 1 × 1014 ions/cm2. The diffraction curves of the ...

  13. Surface and interface strains studied by x-ray diffraction

    International Nuclear Information System (INIS)

    Akimoto, Koichi; Emoto, Takashi; Ichimiya, Ayahiko

    1998-01-01

    The authors have developed a technique of X-ray diffraction in order to measure strain fields near semiconductor surface and interface. The diffraction geometry is using the extremely asymmetric Bragg-case bulk reflection of a small incident angle to the surface and a large angle exiting from the surface. The incident angle of the X-rays is set near critical angle of total reflection by tuning X-ray energy of synchrotron radiation at the Photon Factory, Japan. For thermally grown-silicon oxide/Si(100) interface, the X-ray intensity of the silicon substrate 311 reflection has been measured. From comparison of the full width at half maxima (FWHM) of X-ray rocking curves of various thickness of silicon oxides, it has been revealed that silicon substrate lattice is highly strained in the thin (less than about 5 nm) silicon oxide/silicon system. In order to know the original silicon surface strain, the authors have also performed the same kind of measurements in the ultra-high vacuum chamber. A clean Si(111) 7x7 surface gives sharper X-ray diffraction peak than that of the native oxide/Si(111) system. From these measurements, it is concluded that the thin silicon oxide film itself gives strong strain fields to the silicon substrates, which may be the reason of the existence of the structural transition layer at the silicon oxide/Si interface

  14. 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 ...

  15. 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.)

  16. Application of energy dispersive X-ray fluorescent technique in the pollution study of water

    Energy Technology Data Exchange (ETDEWEB)

    Htun, Kyi

    1993-03-01

    The abundance of major trace elements in water in the surface well, tube well, lake and river were measured. The technique outlined here is very useful in the study of the pollution of environmental radioactivity. For the above measurements the Si(Li) X-ray detection system was used in conjunction with a personal computer

  17. 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)

  18. Coherent X-ray diffraction studies of mesoscopic materials

    International Nuclear Information System (INIS)

    Shabalin, Anatoly

    2015-12-01

    This thesis is devoted to three separate projects, which can be considered as independent. First, the dynamical scattering effects in the Coherent X-ray Diffractive Imaging (CXDI) method are discussed. Based on the simulation results, a straightforward method for correction for the refraction and absorption artifacts in the Bragg CXDI reconstruction is suggested. The second part summarizes the results of an Coherent X-ray Diffractive Imaging experiment with a single colloidal crystal grain. A remarkable result is that positions of individual particles in the crystal lattice have been resolved in three dimensions. The third project is devoted to X-ray diffraction experimental studies of structural evolution of colloidal crystalline films upon incremental heating. Based on the results of the analysis a model of structural evolution of a colloidal crystal upon heating on nanoscopic and mesoscopic length scales is suggested.

  19. 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)

  20. Data acquisition and processing system of energy dispersive X-ray spectrometer with microprocessor

    International Nuclear Information System (INIS)

    Horkay, G.; Kis-Varga, M.; Lakatos, T.; Molnar, J.; Zsurzs, M.

    1984-01-01

    For quantitative analysis of chemical elements by the method of X-ray spectroscopy a multichannel analyzer on the base of minicomputer with the INTEL 8080 A microprocessor is developed. The data acquisition and data processing systems which comprise a central processor, memory unit, ADC and display are described. Major system subprograms are enumerated. An example of Pb concentration determinating in a bronze specimen is given

  1. X-ray powder diffraction data on miscellaneous lanthanide compounds

    International Nuclear Information System (INIS)

    Ferguson, I.F.; Hughes, T.E.

    1978-08-01

    Recent work on neutron absorbing materials has produced various new X-ray diffraction powder patterns of compounds of the lanthanides. Various inconsistencies in previously published data have been noted, and accurate measurements have been made of the lattice parameters of the rare earth oxides Sm 2 0 3 , Eu 2 0 3 , Gd 2 0 3 which have the monoclinic rare earth type B- structure, as well as Eu0. These data are recorded for reference. The optimum conditions for obtaining X-ray powder diffraction data from europium compounds are also noted. (author)

  2. 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

  3. Molybdenum cell for x-ray diffraction measurements of fluid alkali metals at high temperatures and high pressures

    Science.gov (United States)

    Matsuda, Kazuhiro; Tamura, Kozaburo; Katoh, Masahiro; Inui, Masanori

    2004-03-01

    We have developed a sample cell for x-ray diffraction measurements of fluid alkali metals at high temperatures and high pressures. All parts of the cell are made of molybdenum which is resistant to the chemical corrosion of alkali metals. Single crystalline molybdenum disks electrolytically thinned down to 40 μm were used as the walls of the cell through which x rays pass. The crystal orientation of the disks was controlled in order to reduce the background from the cell. All parts of the cell were assembled and brazed together using a high-temperature Ru-Mo alloy. Energy dispersive x-ray diffraction measurements have been successfully carried out for fluid rubidium up to 1973 K and 16.2 MPa. The obtained S(Q) demonstrates the applicability of the molybdenum cell to x-ray diffraction measurements of fluid alkali metals at high temperatures and high pressures.

  4. 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)

  5. 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.

  6. 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)

  7. X-Ray Diffraction Project Final Report, Fiscal Year 2006

    International Nuclear Information System (INIS)

    Dane V. Morgan

    2006-01-01

    An x-ray diffraction diagnostic system was developed for determining real-time shock-driven lattice parameter shifts in single crystals at the gas gun at TA-IV at Sandia National Laboratories (SNL). The signal-to-noise ratio and resolution of the system were measured using imaging plates as the detector and by varying the slit width. This report includes tests of the x-ray diffraction system using a phosphor coupled to a charge-coupled device (CCD) camera by a coherent fiber-optic bundle. The system timing delay was measured with a newly installed transistor-transistor logic (TTL) bypass designed to reduce the x-ray delay time. The axial misalignment of the Bragg planes was determined with respect to the optical axis for a set of eight LiF [lithium fluoride] crystals provided by SNL to determine their suitability for gas gun experiments

  8. 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.)

  9. 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

  10. Direct methods for surface X-ray diffraction

    International Nuclear Information System (INIS)

    Saldin, D. K.; Harder, R.; Shneerson, V. L.; Vogler, H.; Moritz, W.

    2000-01-01

    We develop of a direct method for surface X-ray diffraction that exploits the holographic feature of a known reference wave from the substrate. A Bayesian analysis of the optimal inference to be made from an incomplete data set suggests a maximum entropy algorithm that balances agreement with the data and other statistical considerations

  11. X-Ray diffraction Investigation of Electrochemically Deposited Copper

    DEFF Research Database (Denmark)

    Pantleon, Karen; Jensen, Jens Dahl; Somers, Marcel A.J.

    2004-01-01

    by the determination of X-ray diffraction (XRD) pole figures and the calculation of the orientation distribution functions. XRD results are discussed in relation to the morphologies of the electrodeposits as investigated with light optical microscopy and correlated with the process parameters during electrodeposition....

  12. The three dimensional X-ray diffraction technique

    DEFF Research Database (Denmark)

    Juul Jensen, Dorte; Poulsen, Henning Friis

    2012-01-01

    This introductory tutorial describes the so called 3 dimensional X-ray diffraction (3DXRD) technique, which allows bulk non-destructive structural characterizations of crystalline materials. The motivations and history behind the development of this technique are described and its potentials...

  13. Fusion bonding of Si wafers investigated by x ray diffraction

    DEFF Research Database (Denmark)

    Weichel, Steen; Grey, Francois; Rasmussen, Kurt

    2000-01-01

    The interface structure of bonded Si(001) wafers with twist angle 6.5 degrees is studied as a function of annealing temperature. An ordered structure is observed in x-ray diffraction by monitoring a satellite reflection due to the periodic modulation near the interface, which results from...

  14. Quantitative determination of phases by X-ray diffraction

    International Nuclear Information System (INIS)

    Azevedo, A.L.T.

    1979-01-01

    The internal standard method for the quantitative determination of phases by X-ray diffraction is presented. The method is applicable to multi-phase materials which may be treated as powder. A discussion on sample preparation and some examples follow. (Author) [pt

  15. Residual cold-work determination by X-ray diffraction

    International Nuclear Information System (INIS)

    Pireau, A.; Vanderborck, Y.

    1990-01-01

    The determination of the cold-work level of materials for fast breeder reactors can be made by different techniques. The report compares different methods for an application on austenitic stainless steels and demonstrates that the X-ray diffraction procedure is a reliable technique. A round robin test has been performed between three laboratories; the results are presented and discussed

  16. X-ray diffraction study of pure plutonium under pressure

    Energy Technology Data Exchange (ETDEWEB)

    Faure, Ph. [CEA, Valduc, F-21120 Is-sur-Tille (France)], E-mail: philippe.faure@cea.fr; Genestier, C. [CEA, Valduc, F-21120 Is-sur-Tille (France)

    2009-03-15

    Atomic volume and bulk modulus represent basic cohesion properties of a material and are therefore linked to many other physical properties. However, large discrepancies are found in the literature regarding values for the bulk modulus of pure plutonium ({alpha}-phase). New X-ray diffraction measurements of plutonium in diamond anvil cell are presented and the isothermal bulk modulus is extracted.

  17. 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

  18. Chemical analysis of coal by energy dispersive x-ray fluorescence utilizing artificial standards

    International Nuclear Information System (INIS)

    Wheeler, B.D.

    1982-01-01

    Accurate determinations of the elemental composition of coal by classical methods can be quite difficult and are normally very time consuming. X-ray fluorescence utilizing the powder method, however, has the ability of providing accurate and rapid analyses. Unfortunately, well characterized standards, although available, are not plentiful. In addition, the durability of stability of ground and pelletized coal samples is poor resulting in deterioration with time. As a result, artificial coal standards were prepared from certified geological materials by fusing in lithium tetraborate in percentages approximating expected ash contents and compositions in coal. Since the lithium tetraborate comprises about the same percentage of the standard as does the carbon, hydrogen, and oxygen in coal, the ground and pelletized coal sample can be assayed against the fused calibration curves by compensating for the differences in the mass absorption coefficients of the two matrices. 5 figures, 4 tables

  19. Diffraction enhanced X-ray imaging of mammals crystalline lens

    International Nuclear Information System (INIS)

    Antunes, A.; Hoennicke, M.G.; Safatle, A.M.V.; Cusatis, C.; Moraes Barros, P.S.; Morelhao, S.L.

    2005-01-01

    Crystalline lenses are transparent biological materials where the organization of the lens fibers can also be affected by changes at molecular level, and therefore the structure and morphology of the tissue can be correlated to the loss of transparency of the lens. In this work, internal structure of mammal lenses regarding the long-range ordering of the fibers are investigated by diffraction enhanced X-ray imaging (DEI) radiography. Moreover, DEI and absorption X-ray synchrotron radiographs for healthy and cataractous crystalline lenses are compared. Significant differences in healthy and cataractous crystalline lenses are observed

  20. Raman spectroscopy and X-ray diffraction studies on celestite

    International Nuclear Information System (INIS)

    Chen Yenhua; Yu Shucheng; Huang, Eugene; Lee, P.-L.

    2010-01-01

    High-pressure Raman spectroscopy and X-ray diffraction studies of celestite (SrSO 4 ) were carried out in a diamond anvil cell at room temperature. Variation in the Raman vibrational frequency and change of lattice parameters with pressure indicate that a transformation occurs in celestite. This transformation caused an adjustment in the Sr-O polyhedra that affected the stretching-force constant of SO 4 . Moreover, compressibilities along the crystallographic axes decreased in the order a to c to b. From the compression data, the bulk modulus of the celestite was 87 GPa. Both X-ray and Raman data show that the transition in celestite is reversible.

  1. 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)

  2. 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.

  3. 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

  4. 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

  5. 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

  6. 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.

  7. 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.

  8. 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)

  9. 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.

  10. MSL Chemistry and Mineralogy X-Ray Diffraction X-Ray Fluorescence (CheMin) Instrument

    Science.gov (United States)

    Zimmerman, Wayne; Blake, Dave; Harris, William; Morookian, John Michael; Randall, Dave; Reder, Leonard J.; Sarrazin, Phillipe

    2013-01-01

    This paper provides an overview of the Mars Science Laboratory (MSL) Chemistry and Mineralogy Xray Diffraction (XRD), X-ray Fluorescence (XRF) (CheMin) Instrument, an element of the landed Curiosity rover payload, which landed on Mars in August of 2012. The scientific goal of the MSL mission is to explore and quantitatively assess regions in Gale Crater as a potential habitat for life - past or present. The CheMin instrument will receive Martian rock and soil samples from the MSL Sample Acquisition/Sample Processing and Handling (SA/SPaH) system, and process it utilizing X-Ray spectroscopy methods to determine mineral composition. The Chemin instrument will analyze Martian soil and rocks to enable scientists to investigate geophysical processes occurring on Mars. The CheMin science objectives and proposed surface operations are described along with the CheMin hardware with an emphasis on the system engineering challenges associated with developing such a complex instrument.

  11. 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)

  12. Single-pulse x-ray diffraction using polycapillary optics for in situ dynamic diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Maddox, B. R., E-mail: maddox3@llnl.gov; Akin, M. C., E-mail: akin1@llnl.gov; Teruya, A.; Hunt, D.; Hahn, D.; Cradick, J. [Lawrence Livermore National Laboratory, Livermore, California 94550 (United States); Morgan, D. V. [National Security Technologies LLC, Los Alamos, New Mexico 87544 (United States)

    2016-08-15

    Diagnostic use of single-pulse x-ray diffraction (XRD) at pulsed power facilities can be challenging due to factors such as the high flux and brightness requirements for diffraction and the geometric constraints of experimental platforms. By necessity, the x-ray source is usually positioned very close, within a few inches of the sample. On dynamic compression platforms, this puts the x-ray source in the debris field. We coupled x-ray polycapillary optics to a single-shot needle-and-washer x-ray diode source using a laser-based alignment scheme to obtain high-quality x-ray diffraction using a single 16 ns x-ray pulse with the source >1 m from the sample. The system was tested on a Mo sample in reflection geometry using 17 keV x-rays from a Mo anode. We also identified an anode conditioning effect that increased the x-ray intensity by 180%. Quantitative measurements of the x-ray focal spot produced by the polycapillary yielded a total x-ray flux on the sample of 3.3 ± 0.5 × 10{sup 7} molybdenum Kα photons.

  13. Modern X-ray diffraction. X-ray diffractometry for materials scientists, physicists, and chemicists. 2. rev. and enl. ed.

    International Nuclear Information System (INIS)

    Spiess, Lothar; Teichert, Gerd; Schwarzer, Robert; Behnken, Herfried; Genzel, Christoph

    2009-01-01

    This book offers a comprehensive survey over the applications of X-ray diffractions in fields like materials technique, metallurgy, electrotechniques, mechanical engineering, as well as micro- and nanotechniques. The necessary baic knowledges of X-ray diffraction are mediated foundedly and illustratively. Thereby new techniques and evaluation procedures are presented as well as well known methods

  14. Multiple x-ray diffraction simulation and applications

    International Nuclear Information System (INIS)

    Costa, C.A.B.S. da.

    1989-09-01

    A computer program (MULTX) was implemented for simulation X-ray multiple diffraction diagrams in Renninger geometries. The program uses the X-ray multiple diffraction theory for imperfect crystals. The iterative calculation of the intensities is based on the Taylor series general term, and the primary beam power expansion is given as function of the beam x penetration in the crystal surface. This development allows to consider the simultaneous interaction of the beams involved in the multiple diffraction phenomenon. The simulated diagrams are calculated point-to-point and the tests for the Si and GaAs presented good reproduction of the experimental diagrams for different primary reflections. (L.C.J.A.)

  15. 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.

  16. Instrument and method for X-ray diffraction, fluorescence, and crystal texture analysis without sample preparation

    Science.gov (United States)

    Gendreau, Keith (Inventor); Martins, Jose Vanderlei (Inventor); Arzoumanian, Zaven (Inventor)

    2010-01-01

    An X-ray diffraction and X-ray fluorescence instrument for analyzing samples having no sample preparation includes a X-ray source configured to output a collimated X-ray beam comprising a continuum spectrum of X-rays to a predetermined coordinate and a photon-counting X-ray imaging spectrometer disposed to receive X-rays output from an unprepared sample disposed at the predetermined coordinate upon exposure of the unprepared sample to the collimated X-ray beam. The X-ray source and the photon-counting X-ray imaging spectrometer are arranged in a reflection geometry relative to the predetermined coordinate.

  17. Discovery and development of x-ray diffraction

    Science.gov (United States)

    Jeong, Yeuncheol; Yin, Ming; Datta, Timir

    2013-03-01

    In 1912 Max Laue at University of Munich reasoned x-rays to be short wavelength electromagnetic waves and figured interference would occur when scattered off crystals. Arnold Sommerfeld, W. Wien, Ewald and others, raised objections to Laue's idea, but soon Walter Friedrich succeeded in recording x-ray interference patterns off copper sulfate crystals. But the Laue-Ewald's 3-dimensional formula predicted excess spots. Fewer spots were observed. William Lawrence Bragg then 22 year old studying at Cambridge University heard the Munich results from father William Henry Brag, physics professor at Univ of Leeds. Lawrence figured the spots are 2-d interference of x-ray wavelets reflecting off successive atomic planes and derived a simple eponymous equation, the Bragg equation d*sin(theta) = n*lamda. 1913 onward the Braggs dominated the crystallography. Max Laue was awarded the physics Nobel in 1914 and the Braggs shared the same in 1915. Starting with Rontgen's first ever prize in 1901, the importance of x-ray techniques is evident from the four out of a total 16 physics Nobels between 1901-1917. We will outline the historical back ground and importance of x-ray diffraction giving rise to techniques that even in 2013, remain work horses in laboratories all over the globe.

  18. 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.)

  19. 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

  20. Sampling and analytical methodologies for energy dispersive X-ray fluorescence analysis of airborne particulate matter

    International Nuclear Information System (INIS)

    1993-01-01

    The present document represents an attempt to summarize the most important features of the different forms of ED-XFR as applied to the analysis of airborne particulate matter. It is intended to serve as a set of guidelines for use by participants in the IAEA's own programmes, and other scientists, who are not yet fully experienced in the application of ED-XRF to airborne particulate samples, and who wish either to make a start on using this technique or to improve their existing procedures. The methodologies for sampling described in this document are of rather general applicability. Emphasis is also placed on the sources of errors affecting the sampling of airborne particulate matter. The analytical part of the document describes the different forms of ED-XRF and their potential applications. Spectrum evaluation, a key step in X-ray spectrometry, is covered in depth, including discussion on several calibration and peak fitting techniques and computer programs especially designed for this purpose. 148 refs, 25 figs, 13 tabs

  1. Extinction correction in white X-ray and neutron diffraction

    International Nuclear Information System (INIS)

    Tomiyoshi, S.; Yamada, M.; Watanabe, H.

    1980-01-01

    Extinction effects in white-beam X-ray and neutron diffraction are considered. In white-beam diffraction, a small deviation of the wavelength from the Bragg condition Δlambda is a variable which represents the line profile of the diffraction peaks, so that by using the new parameter Δlambda the theory is converted to one in white-beam diffraction. It is shown that for a convex crystal, primary extinction agrees with the results calculated already for monochromatic diffraction. The same relation is shown to hold in secondary extinction. It is concluded that extinction theory derived for monochromatic diffraction is applicable without any modification in white-beam diffraction. (Auth.)

  2. 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

  3. Analysis of SHLW by Energy Dispersive X-Ray Fluorescence (EDXRF) technique

    International Nuclear Information System (INIS)

    Vadivu, Senthil; Seshadreesan, N.P.; Kumar, R.; Venkatasubramani, C.R.

    2012-01-01

    The simulated high level liquid waste (SHLW) sample expected from fuel reprocessing experiments containing uranium and about 20 various other elements were analysed by EDXRF technique. An investigation with respect to Nd estimation, a burn up monitor, in presence of varying concentrations of U was also carried out. The simulated raffinate solution with a mixture of 20 expected elements was used as standard solution. Four samples of varying concentrations were prepared by appropriate dilution from the standard solution. Calibrations were carried out for its various constituent elements. The elements such as Cs, Mo, Sr,Y, Cd, Ba, Ce, U and La were analysed using W-filter whereas the elements such as Nd, Fe and Ni were analysed using Ge secondary target. The results of 4 simulated samples analysed using FDXRF are given. These values for each element are the mean of the three values obtained. The results obtained for different simulated waste are also shown. These solutions are of different compositions and therefore, vary in their matrix effects. Nevertheless, the medium of second simulated waste is in 3.5N HNO 3 where as the calibration is done with 0.1N HNO 3 medium and hence this might be the cause for large deviations observed in some of the results. A trend of the non-interference of the Uranium matrix in the assay of Nd was demonstrated typically at a fixed concentration of 92.3 ppm in uranium matrix of 900 and 6000 ppm. In both the cases, it was observed that the concentration of Nd measured remained same. This is in accordance to the fact that the characteristic X-ray energy peaks of Nd (L-lines) and U (M-lines) are well separated in the spectrum and the contribution of the low energy peak of Uranium to the higher energy peak of Nd is negligible. But the limiting concentration of Uranium may be the one in which a overlapping of its peak occurs

  4. 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)

  5. 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.

  6. Iron speciation of airborne subway particles by the combined use of energy dispersive electron probe X-ray microanalysis and Raman microspectrometry.

    Science.gov (United States)

    Eom, Hyo-Jin; Jung, Hae-Jin; Sobanska, Sophie; Chung, Sang-Gwi; Son, Youn-Suk; Kim, Jo-Chun; Sunwoo, Young; Ro, Chul-Un

    2013-11-05

    Quantitative energy-dispersive electron probe X-ray microanalysis (ED-EPMA), known as low-Z particle EPMA, and Raman microspectrometry (RMS) were applied in combination for an analysis of the iron species in airborne PM10 particles collected in underground subway tunnels. Iron species have been reported to be a major chemical species in underground subway particles generated mainly from mechanical wear and friction processes. In particular, iron-containing particles in subway tunnels are expected to be generated with minimal outdoor influence on the particle composition. Because iron-containing particles have different toxicity and magnetic properties depending on their oxidation states, it is important to determine the iron species of underground subway particles in the context of both indoor public health and control measures. A recently developed analytical methodology, i.e., the combined use of low-Z particle EPMA and RMS, was used to identify the chemical species of the same individual subway particles on a single particle basis, and the bulk iron compositions of airborne subway particles were also analyzed by X-ray diffraction. The majority of airborne subway particles collected in the underground tunnels were found to be magnetite, hematite, and iron metal. All the particles collected in the tunnels of underground subway stations were attracted to permanent magnets due mainly to the almost ubiquitous ferrimagnetic magnetite, indicating that airborne subway particles can be removed using magnets as a control measure.

  7. X-ray diffraction study of directionally grown perylene crystallites

    DEFF Research Database (Denmark)

    Breiby, Dag W.; Lemke, H. T.; Hammershøj, P.

    2008-01-01

    Using grazing incidence X-ray diffraction, perylene crystallites grown on thin highly oriented poly(tetrafluoroethylene) (PTFE) films on silicon substrates have been investigated. All the perylene crystallites are found to orient with the ab plane of the monoclinic unit cell parallel to the subst......Using grazing incidence X-ray diffraction, perylene crystallites grown on thin highly oriented poly(tetrafluoroethylene) (PTFE) films on silicon substrates have been investigated. All the perylene crystallites are found to orient with the ab plane of the monoclinic unit cell parallel...... to the substrate. The scattering data is interpreted as a trimodal texture of oriented perylene crystallites, induced by interactions between the perylene molecules and the oriented PTFE substrate. Three families of biaxial orientations are seen, with the axes (h = 1, 2, or 3) parallel to the PTFE alignment......, all having the ab-plane parallel to the substrate. About 92% of the scattered intensity corresponds to a population with highly parallel to (PTFE)....

  8. Elasticity of Tantalum to 105 Gpa using a stress and angle-resolved x-ray diffraction

    International Nuclear Information System (INIS)

    Cynn, H; Yoo, C S

    1999-01-01

    Determining the mechanical properties such as elastic constants of metals at Mbar pressures has been a difficult task in experiment. Following the development of anisotropic elastic theory by Singh et al.[l], Mao et a1.[2] have recently developed a novel experimental technique to determine the elastic constants of Fe by using the stress and energy-dispersive x-ray diffraction (SEX). In this paper, we present an improved complementary technique, stress and angle-resolved x-ray diffraction (SAX), which we have applied to determine the elastic constants of tantalum to 105 GPa. The extrapolation of the tantalum elastic data shows an excellent agreement with the low-pressure ultrasonic data[3]. We also discuss the improvement of this SAX method over the previous SEX.[elastic constant, anisotropic elastic theory, angle-dispersive synchrotron x-ray diffraction, mechanical properties

  9. X-ray diffraction and measurement of residual stresses

    International Nuclear Information System (INIS)

    Maeder, G.; Lebrun, J.L.; Corcaud, L.

    1977-01-01

    X-ray diffraction technique is a non destructive method for measuring the residual stresses in mechanical parts. This method, called sin 2 PSI method is investigated. It is applied to the measurement of elastic constants in different directions of crystals of Zr alloy (Zircaloy 4) and Ti alloy (TA6V). Stresses in TA6V sheets welded by TIG and electron beam processes are also studied [fr

  10. 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.

  11. X-ray diffraction from single GaAs nanowires

    Energy Technology Data Exchange (ETDEWEB)

    Biermanns, Andreas

    2012-11-12

    In recent years, developments in X-ray focussing optics have allowed to produce highly intense, coherent X-ray beams with spot sizes in the range of 100 nm and below. Together with the development of new experimental stations, X-ray diffraction techniques can now be applied to study single nanometer-sized objects. In the present work, X-ray diffraction is applied to study different aspects of the epitaxial growth of GaAs nanowires. Besides conventional diffraction methods, which employ X-ray beams with dimensions of several tens of {mu}m, special emphasis lies on the use of nanodiffraction methods which allow to study single nanowires in their as-grown state without further preparation. In particular, coherent X-ray diffraction is applied to measure simultaneously the 3-dimensional shape and lattice parameters of GaAs nanowires grown by metal-organic vapor phase epitaxy. It is observed that due to a high density of zinc-blende rotational twins within the nanowires, their lattice parameter deviates systematically from the bulk zinc-blende phase. In a second step, the initial stage in the growth of GaAs nanowires on Si (1 1 1) surfaces is studied. This nanowires, obtained by Ga-assisted growth in molecular beam epitaxy, grow predominantly in the cubic zinc-blende structure, but contain inclusions of the hexagonal wurtzite phase close to their bottom interface. Using nanodiffraction methods, the position of the different structural units along the growth axis is determined. Because the GaAs lattice is 4% larger than silicon, these nanowires release their lattice mismatch by the inclusion of dislocations at the interface. Whereas NWs with diameters below 50 nm are free of strain, a rough interface structure in nanowires with diameters above 100 nm prevents a complete plastic relaxation, leading to a residual strain at the interface that decays elastically along the growth direction. Finally, measurements on GaAs-core/InAs-shell nanowire heterostructures are presented

  12. miniPixD : a compact sample analysis system which combines X-ray imaging and diffraction

    International Nuclear Information System (INIS)

    Moss, Robert; Crews, Chiaki; Speller, Robert; Wilson, Matthew

    2017-01-01

    This paper introduces miniPixD : a new, compact system that utilises transmission X-ray imaging and X-ray diffraction (XRD) to locate and identify materials of interest within an otherwise opaque volume. The system and the embodied techniques have utility in security screening, medical diagnostics, non-destructive testing (NDT) and quality assurance (QA). This paper outlines the design of the system including discussion on the choice of components and presents some data from relevant samples which are compared to other energy dispersive and angular dispersive XRD techniques.

  13. X-ray diffraction at Bragg angles around π/2

    International Nuclear Information System (INIS)

    Mayolo, C.M.G. de.

    1991-01-01

    X-ray diffraction at Bragg angles around π/2 is studied from the theoretical and experimental points of view. The proposed corrections to the dynamical theory in the θ β ≅ π/2 cases, has been reviewed showing the equivalence between two formalisms leading to a corrected expression for the dependence of the angular parameter y with the angle of incidence. An expression for y valid in the conventional and θ β ≅ π/2 cases has been obtained. A general expression for Bragg law and for energy resolution after a Bragg diffraction was also deduced. (author)

  14. Nano structured materials studied by coherent X-ray diffraction

    International Nuclear Information System (INIS)

    Gulden, Johannes

    2013-03-01

    Structure determination with X-rays in crystallography is a rapidly evolving field. Crystallographic methods for structure determination are based on the assumptions about the crystallinity of the sample. It is vital to understand the structure of possible defects in the crystal, because they can influence the structure determination. All conventional methods to characterize defects require a modelling through simulated data. No direct methods exist to image the core of defects in crystals. Here a new method is proposed, which will enable to visualize the individual scatterers around and at defects in crystals. The method is based on coherent X-ray scattering. X-rays are perfectly suited since they can penetrate thick samples and buried structures can be investigated Recent developments increased the coherent flux of X-Ray sources such as synchrotrons by orders of magnitude. As a result, the use of the coherent properties of X-rays is emerging as a new aspect of X-ray science. New upcoming and operating X-ray laser sources will accelerate this trend. One new method which has the capacity to recover structural information from the coherently scattered photons is Coherent X-ray Diffraction Imaging (CXDI). The main focus of this thesis is the investigation of the structure and the dynamics of colloidal crystals. Colloidal crystals can be used as a model for atomic crystals in order to understand the growth and defect structure. Despite the large interest in these structures, many details are still unknown.Therefore, it is vital to develop new approaches to measure the core of defects in colloidal crystals. After an introduction into the basics of the field of coherent X-ray scattering, this thesis introduces a novel method, Small Angle Bragg Coherent Diffractive Imaging, (SAB-CDI). This new measurement technique which besides the relevance to colloidal crystals can be applied to a large variety of nano structured materials. To verify the experimental possibilities the

  15. Nano structured materials studied by coherent X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Gulden, Johannes

    2013-03-15

    Structure determination with X-rays in crystallography is a rapidly evolving field. Crystallographic methods for structure determination are based on the assumptions about the crystallinity of the sample. It is vital to understand the structure of possible defects in the crystal, because they can influence the structure determination. All conventional methods to characterize defects require a modelling through simulated data. No direct methods exist to image the core of defects in crystals. Here a new method is proposed, which will enable to visualize the individual scatterers around and at defects in crystals. The method is based on coherent X-ray scattering. X-rays are perfectly suited since they can penetrate thick samples and buried structures can be investigated Recent developments increased the coherent flux of X-Ray sources such as synchrotrons by orders of magnitude. As a result, the use of the coherent properties of X-rays is emerging as a new aspect of X-ray science. New upcoming and operating X-ray laser sources will accelerate this trend. One new method which has the capacity to recover structural information from the coherently scattered photons is Coherent X-ray Diffraction Imaging (CXDI). The main focus of this thesis is the investigation of the structure and the dynamics of colloidal crystals. Colloidal crystals can be used as a model for atomic crystals in order to understand the growth and defect structure. Despite the large interest in these structures, many details are still unknown.Therefore, it is vital to develop new approaches to measure the core of defects in colloidal crystals. After an introduction into the basics of the field of coherent X-ray scattering, this thesis introduces a novel method, Small Angle Bragg Coherent Diffractive Imaging, (SAB-CDI). This new measurement technique which besides the relevance to colloidal crystals can be applied to a large variety of nano structured materials. To verify the experimental possibilities the

  16. Design and fabrication of micro X-ray diffraction system

    Energy Technology Data Exchange (ETDEWEB)

    Park, Yang Soon; Han, Sun Ho; Kim, Jong Goo; Jee, Kwang Yong

    2006-10-15

    It has been observed that microstructure changes occur at the pellet periphery(rim) of the fuel at very high burn-up. Despite its narrow range (below some hundreds microns in depth), this peripheral region(rim) determines the behaviour of nuclear fuel. To determine lattice parameter with XRD at intervals as small as 30-50 {mu} m in radial direction of irradiated fuel samples, a micro X-ray diffraction system was designed and fabricated. This report describes the micro X-ray diffraction system consisted of an X-ray microbeam alignment system and a sample micro translation system, its characterization, and its performance test through the analysis for the micro region of some specimens. This system will be set in a radiation shielded glove box, and then used for analysis of lattice parameter change and the phase change at intervals as small as 30-50 {mu} m in radial direction of the rim of an irradiated fuel sample and a fuel cladding.

  17. Design and fabrication of micro X-ray diffraction system

    International Nuclear Information System (INIS)

    Park, Yang Soon; Han, Sun Ho; Kim, Jong Goo; Jee, Kwang Yong

    2006-10-01

    It has been observed that microstructure changes occur at the pellet periphery(rim) of the fuel at very high burn-up. Despite its narrow range (below some hundreds microns in depth), this peripheral region(rim) determines the behaviour of nuclear fuel. To determine lattice parameter with XRD at intervals as small as 30-50 μ m in radial direction of irradiated fuel samples, a micro X-ray diffraction system was designed and fabricated. This report describes the micro X-ray diffraction system consisted of an X-ray microbeam alignment system and a sample micro translation system, its characterization, and its performance test through the analysis for the micro region of some specimens. This system will be set in a radiation shielded glove box, and then used for analysis of lattice parameter change and the phase change at intervals as small as 30-50 μ m in radial direction of the rim of an irradiated fuel sample and a fuel cladding

  18. 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)

  19. Serial femtosecond X-ray diffraction of enveloped virus microcrystals

    Directory of Open Access Journals (Sweden)

    Robert M. Lawrence

    2015-07-01

    Full Text Available Serial femtosecond crystallography (SFX using X-ray free-electron lasers has produced high-resolution, room temperature, time-resolved protein structures. We report preliminary SFX of Sindbis virus, an enveloped icosahedral RNA virus with ∼700 Å diameter. Microcrystals delivered in viscous agarose medium diffracted to ∼40 Å resolution. Small-angle diffuse X-ray scattering overlaid Bragg peaks and analysis suggests this results from molecular transforms of individual particles. Viral proteins undergo structural changes during entry and infection, which could, in principle, be studied with SFX. This is an important step toward determining room temperature structures from virus microcrystals that may enable time-resolved studies of enveloped viruses.

  20. Diffraction enhanced kinetic depth X-ray imaging

    Science.gov (United States)

    Dicken, A.

    An increasing number of fields would benefit from a single analytical probe that can characterise bulk objects that vary in morphology and/or material composition. These fields include security screening, medicine and material science. In this study the X-ray region is shown to be an effective probe for the characterisation of materials. The most prominent analytical techniques that utilise X-radiation are reviewed. The study then focuses on methods of amalgamating the three dimensional power of kinetic depth X-ray (KDFX) imaging with the materials discrimination of angular dispersive X-ray diffraction (ADXRD), thus providing KDEX with a much needed material specific counterpart. A knowledge of the sample position is essential for the correct interpretation of diffraction signatures. Two different sensor geometries (i.e. circumferential and linear) that are able to collect end interpret multiple unknown material diffraction patterns and attribute them to their respective loci within an inspection volume are investigated. The circumferential and linear detector geometries are hypothesised, simulated and then tested in an experimental setting with the later demonstrating a greater ability at discerning between mixed diffraction patterns produced by differing materials. Factors known to confound the linear diffraction method such as sample thickness and radiation energy have been explored and quantified with a possible means of mitigation being identified (i.e. via increasing the sample to detector distance). A series of diffraction patterns (following the linear diffraction approach) were obtained from a single phantom object that was simultaneously interrogated via KDEX imaging. Areas containing diffraction signatures matched from a threat library have been highlighted in the KDEX imagery via colour encoding and match index is inferred by intensity. This union is the first example of its kind and is called diffraction enhanced KDEX imagery. Finally an additional

  1. X-ray diffraction imaging of biological cells

    CERN Document Server

    Nakasako, Masayoshi

    2018-01-01

    In this book, the author describes the development of the experimental diffraction setup and structural analysis of non-crystalline particles from material science and biology. Recent advances in X-ray free electron laser (XFEL)-coherent X-ray diffraction imaging (CXDI) experiments allow for the structural analysis of non-crystalline particles to a resolution of 7 nm, and to a resolution of 20 nm for biological materials. Now XFEL-CXDI marks the dawn of a new era in structural analys of non-crystalline particles with dimensions larger than 100 nm, which was quite impossible in the 20th century. To conduct CXDI experiments in both synchrotron and XFEL facilities, the author has developed apparatuses, named KOTOBUKI-1 and TAKASAGO-6 for cryogenic diffraction experiments on frozen-hydrated non-crystalline particles at around 66 K. At the synchrotron facility, cryogenic diffraction experiments dramatically reduce radiation damage of specimen particles and allow tomography CXDI experiments. In addition, in XFEL ex...

  2. X-ray diffraction without sample preparation: Proof-of-principle experiments

    International Nuclear Information System (INIS)

    Hansford, Graeme M.

    2013-01-01

    The properties of a novel X-ray diffraction (XRD) technique having very low sensitivity to the sample morphology were previously elucidated through theoretical considerations and model simulations (Hansford, 2011). This technique opens up the possibility of mineralogical analysis by XRD without sample preparation. Here, the results of proof-of-principle experimental tests are presented. Two sets of experiments were performed using a vacuum chamber equipped with an X-ray tube source, sample holder and charge-coupled detector. Firstly, a pressed-powder pellet of α-quartz was placed in three different positions relative to the X-ray source and detector. The changes in position represent gross sample movements which would be inconceivable in conventional XRD analysis. The resulting back-reflection energy-dispersive spectra show a very high degree of correspondence other than an overall intensity factor dependent on the distance between the sample and detector. Secondly, the back-reflection spectrum of an unprepared limestone hand specimen, having mm-scale surface morphology, was compared to the spectrum of a calcite pressed-powder pellet. The correspondence of the diffraction peaks in the spectra demonstrate that the limestone is comprised dominantly of calcite. In both cases, the claims of the earlier paper are fully supported by the results of these experimental tests. -- Highlights: • Proof-of-principle tests of a novel X-ray diffraction (XRD) method were conducted. • Very low sensitivity to sample position and orientation was demonstrated. • Insensitivity to sample morphology is inferred. • A simple analysis of an unprepared limestone hand specimen was performed. • This technique enables mineralogical analysis by XRD without sample preparation

  3. Optimization of an X-ray diffraction imaging system for medical and security applications

    International Nuclear Information System (INIS)

    Marticke, Fanny

    2016-01-01

    X-ray diffraction imaging is a powerful noninvasive technique to identify or characterize different materials. Compared to traditional techniques using X-ray transmission, it allows to extract more material characteristic information, such as the Bragg peak positions for crystalline materials as well as the molecular form factor for amorphous materials. The potential of this technique has been recognized by many researchers and numerous applications such as luggage inspection, nondestructive testing, drug detection and biological tissue characterization have been proposed. The method of energy dispersive X-ray diffraction (EDXRD) is particularly suited for this type of applications as it allows the use of a conventional X-ray tube, the acquisition of the whole spectrum at the same time and parallelized architectures to inspect an entire object in a reasonable time. The purpose of the present work is to optimize the whole material characterization chain. Optimization comprises two aspects: optimization of the acquisition system and of data processing. The last one concerns especially the correction of diffraction pattern degraded by acquisition process. Reconstruction methods are proposed and validated on simulated and experimental spectra. System optimization is realized using figures of merit such as detective quantum efficiency (DQE), contrast to noise ratio (CNR) and receiver operating characteristic (ROC) curves.The first chosen application is XRD based breast imaging which aims to distinguish cancerous tissues from healthy tissues. Two non-multiplexed collimation configurations combining EDXRD and ADXRD are proposed after optimization procedure. A simulation study of the whole system and a breast phantom was realized to determine the required dose to detect a 4 mm carcinoma nodule. The second application concerns detection of illicit materials during security check. The possible benefit of a multiplexed collimation system was examined. (author) [fr

  4. 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.

  5. In vivo energy dispersive X-ray fluorescence for measuring the content of essential and toxic trace elements in teeth

    International Nuclear Information System (INIS)

    Zaichick, V.; Ovchjarenko, N.; Zaichick, S.

    1999-01-01

    The calibration and application of a facility, based on energy dispersive X-ray fluorescent analysis (EDXRF) using 109 Cd as an excitation source, for in vivo and in vitro estimation of Ca, Pb, Sr and Zn in tooth enamel is described. During the in vivo measurements, the device ensures tissue protection of face and mouth cavity from radiation, and only a small part of tooth surface under study is irradiated. To calibrate the facility, the contents of Ca, Sr and Zn were analyzed simultaneously in the enamel of 50 teeth by EDXRF and instrumental neutron activation analysis (INAA). Standards prepared from powdered tooth enamel with additions of chemically pure lead compounds were used to calibrate for lead graduation. Enamel calcium is suggested as an internal standard during in vivo EDXRF of teeth. The content of enamel Sr, Zn and Pb was determined by EDXRF in 35 permanent intact teeth of teenagers and adults. It was shown that lead concentration didn't exceed 3 μg/g for all the teeth

  6. Standard test method for analysis of uranium and thorium in soils by energy dispersive X-Ray fluorescence spectroscopy

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2011-01-01

    1.1 This test method covers the energy dispersive X-ray fluorescence (EDXRF) spectrochemical analysis of trace levels of uranium and thorium in soils. Any sample matrix that differs from the general ground soil composition used for calibration (that is, fertilizer or a sample of mostly rock) would have to be calibrated separately to determine the effect of the different matrix composition. 1.2 The analysis is performed after an initial drying and grinding of the sample, and the results are reported on a dry basis. The sample preparation technique used incorporates into the sample any rocks and organic material present in the soil. This test method of sample preparation differs from other techniques that involve tumbling and sieving the sample. 1.3 Linear calibration is performed over a concentration range from 20 to 1000 μg per gram for uranium and thorium. 1.4 The values stated in SI units are to be regarded as the standard. The inch-pound units in parentheses are for information only. 1.5 This standard...

  7. Characterization of wood dust from furniture by scanning electron microscopy and energy-dispersive x-ray analysis.

    Science.gov (United States)

    Gómez Yepes, Milena Elizabeth; Cremades, Lázaro V

    2011-01-01

    Study characterized and analyzed form factor, elementary composition and particle size of wood dust, in order to understand its harmful health effects on carpenters in Quindío (Colombia). Once particle characteristics (size distributions, aerodynamic equivalent diameter (D(α)), elemental composition and shape factors) were analyzed, particles were then characterized via scanning electron microscopy (SEM) in conjunction with energy dispersive X-ray analysis (EDXRA). SEM analysis of particulate matter showed: 1) cone-shaped particle ranged from 2.09 to 48.79 µm D(α); 2) rectangular prism-shaped particle from 2.47 to 72.9 µm D(α); 3) cylindrically-shaped particle from 2.5 to 48.79 µm D(α); and 4) spherically-shaped particle from 2.61 to 51.93 µm D(α). EDXRA reveals presence of chemical elements from paints and varnishes such as Ca, K, Na and Cr. SEM/EDXRA contributes in a significant manner to the morphological characterization of wood dust. It is obvious that the type of particles sampled is a complex function of shapes and sizes of particles. Thus, it is important to investigate the influence of particles characteristics, morphology, shapes and D(α) that may affect the health of carpenters in Quindío.

  8. Diamond-anvil cell for radial x-ray diffraction

    International Nuclear Information System (INIS)

    Chesnut, G N; Schiferl, D; Streetman, B D; Anderson, W W

    2006-01-01

    We have designed a new diamond-anvil cell capable of radial x-ray diffraction to pressures of a few hundred GPa. The diffraction geometry allows access to multiple angles of Ψ, which is the angle between each reciprocal lattice vector g(hkl) and the compression axis of the cell. At the 'magic angle', Ψ∼54.7 0 , the effects of deviatoric stresses on the interplanar spacings, d(hkl), are significantly reduced. Because the systematic errors, which are different for each d(hkl), are significantly reduced, the crystal structures and the derived equations of state can be determined reliably. At other values of Ψ, the effects of deviatoric stresses on the diffraction pattern could eventually be used to determine elastic constants

  9. X-ray diffraction measurements in KCl shocked along [100

    International Nuclear Information System (INIS)

    D'Almeida, T.; Gupta, Y.M.

    2000-01-01

    Real time x-ray diffraction measurements were used to examine the polymorphic phase transformation in KCl shocked along the [100] direction. Shock wave continuum data, obtained previously by Hayes, were used to design the experiments and to predict diffraction from KCl shocked to different peak stresses. Here, we present the results obtained below the transition stress: between 1.4 and 2 GPa. Diffraction data obtained were quantitatively related to macroscopic compression. Interplanar spacing measurements revealed isotropic compression of the unit cell in contrast to previously reported results. Above the transition stress, descriptions of the atomic arrangement with respect to shock propagation (not available in the literature) are required for setting up the detection system. Hence, continuum results in combination with various crystallographic considerations were utilized to obtain data above the transition stress

  10. X-ray diffraction of multilayers and superlattices

    International Nuclear Information System (INIS)

    Bartels, W.J.; Hornstra, J.; Lobeek, D.J.W.

    1986-01-01

    Recursion formulae for calculating the reflected amplitude ratio of multilayers and superlattices have been derived from the Takagi-Taupin differential equations, which describe the dynamical diffraction of X-rays in deformed crystals. Calculated rocking curves of complicated layered structures, such as non-ideal superlattices on perfect crystals, are shown to be in good agreement with observed diffraction profiles. The kinematical theory can save computing time only in the case of an ideal superlattice, for which a geometric series can be used, but the reflections must be below 10% so that multiple reflections can be neglected. For a perfect crystal of arbitrary thickness the absorption at the center of the dynamical reflection is found to be proportional to the square root of the reflectivity. Sputter-deposited periodic multilayers of tungsten and carbon can be considered as an artificial crystal, for which dynamical X-ray diffraction calculations give results very similar to those of a macroscopic optical description in terms of the complex index of refraction and Fresnel reflection coefficients. (orig.)

  11. Modern trends in x-ray powder diffraction

    International Nuclear Information System (INIS)

    Goebel, H.E.; Snyder, R.L.

    1985-01-01

    The revival of interest in X-ray powder diffraction, being quoted as a metamorphosis from the 'ugly duckling' to a 'beautiful swan', can be attributed to a number of modern developments in instrumentation and evaluation software. They result in faster data collection, improved accuracy and resolution, and better detectability of minor phases. The ease of data evaluation on small computers coupled direct to the instrument allows convenient execution of previously tedious and time-consuming off-line tasks like qualitative and quantitative analysis, characterization of microcrystalline properties, indexing, and lattice-constant refinements, as well as structure refinements or even exploration of new crystal structures. Powder diffraction has also progressed from an isolated analytical laboratory method to an in situ technique for analysing solid-state reactions or for the on-stream control of industrial processes. The paper surveys these developments and their real and potential applications, and tries to emphasize new trends that are regarded as important steps for the further progress of X-ray powder diffraction

  12. X-ray diffraction analysis device with electronic photon counter

    International Nuclear Information System (INIS)

    Fillit, R.Y.; Bruyas, H.; Patay, F.

    1985-01-01

    The means provided to control the movements around the three axes are composed of step-by-step motors related to exits control logic which is connected to the calculation and monitored by a clock. The clock monitors also the calculator so as that the calculator controls, together with the programmable clock and control logic, the coordination of the whole rotation movements, along the three rotation axes, their velocity, their duration and the acquisition of the measured intensities of the diffracted X-ray beam [fr

  13. Automation of a Guinier camera for X-ray diffraction

    International Nuclear Information System (INIS)

    Duijn, J.H.

    1988-01-01

    The automation of a Guinier X-ray diffraction camera is discussed. The photographic plate in the conventional setup has been replaced by a curved proportional counter (CPC) which has an electronic readout system. As a result the recording time has been reduced from a few hours to a few minutes. The construction and optimum dimensions of the CPC are discussed and the most essential parts of the readout electronics are highlighted. A linewidth of 200 μm FWHM and an accuracy of 30 μm are achieved. 45 refs.; 53 figs.; 4 tabs

  14. Accidental exposure with X-ray diffraction equipment

    International Nuclear Information System (INIS)

    Montanez, O.; Blanco, D.

    1991-01-01

    The shutter on one of the windows of an X-ray diffraction apparatus was accidentally left open, exposing the worker to the radiation. The worker was wearing a dosimeter film, which was processed immediately to evaluate the potential risk. It was determined that the exposure rate was 350 Roentgen/minute on the skin surface, with corrections being made for the worker's thin clothing. It was concluded that in spite of the worker receiving a relative high dose, it did not reach the threshold value for producing deterministic effects such as cataracts, erythema, and skin damage

  15. New methods of X-ray diffraction spectrometry. II

    International Nuclear Information System (INIS)

    Soerum, H.; Bremer, J.

    1980-01-01

    The construction principles for a flexible X-ray spectrometer can be equipped either with a single curved crystal or with two curved crystals are described. A few of the theoretical 4+32 possible working modes are selected for a closer investigation and examples of recorded spectra are given. It is shown in the general single-crystal case that for a wavelength close to a cut-off energy the narrow diffraction cone has an elliptic section, as predicted by the theory. The spectrometer is discussed in terms of intensity, resolution and dispersive power. A comparison with other types of spectrometer is made. (Auth.)

  16. Powder X-ray diffraction study af alkali alanates

    DEFF Research Database (Denmark)

    Cao, Thao; Mosegaard Arnbjerg, Lene; Jensen, Torben René

    Powder X-ray diffraction study of alkali alanates Thao Cao, Lene Arnbjerg, Torben R. Jensen. Center for Materials Crystallography (CMC), Center for Energy Materials (CEM), iNANO and Department of Chemistry, Aarhus University, DK-8000, Denmark. Abstract: To meet the energy demand in the future...... for mobile applications, new materials with high gravimetric and volumetric storage capacity of hydrogen have to be developed. Alkali alanates are promising for hydrogen storage materials. Sodium alanate stores hydrogen reversibly at moderate conditions when catalysed with, e.g. titanium, whereas potassium...

  17. Synchrotron X-ray diffraction using triple-axis spectrometry

    International Nuclear Information System (INIS)

    Als-Nielsen, J.

    1980-12-01

    High resolution X-ray diffraction studies of (i) monolayers of the noble gases Kr and Ar physiosorbed on graphite (ii) smectic A fluctuations in the nematic and the smectic A phases of liquid crystals are described. The apparatus used is a triple axis spectrometer situated at the storage ring DORIS at Hasylab, DESY, Hamburg. A monochromatic, well collimated beam is extracted from the synchrotron radiation spectrum by Bragg reflection from perfect Si or Ge crystals. The direction of the beam scattered from the sample is determined by Bragg reflection from a perfect Si or Ge crystal. High intensities even with resolution extending beyond the wavelength of visible light can be obtained. (Auth.)

  18. X-ray diffraction analysis of InAs nanowires

    International Nuclear Information System (INIS)

    Davydok, Anton

    2013-01-01

    Semiconductor nanowires have attracted great interest as building blocks for future electronic and optoelectronic devices. The variability of the growth process opens the opportunity to control and combine the various properties tailoring for specific application. It was shown that the electrical and optical characteristics of the nanowires are strongly connected with their structure. Despite intensive research in this field, the growth process is still not fully understood. In particular, extensive real structure investigations are required. Most of the reports dedicated on the structural researches are based on the results of scanning electron microscopy (SEM) or transmission electron microscopy (TEM). SEM provides an image of the surface with nanostructures and is mainly used to describe the morphology of the sample, but it does not bring information about the internal structure, phase composition and defect structure. At the same time, the internal structure can be examined by TEM down to atomic scale. TEM image of good quality are very expensive due to the efforts in sample preparation and in localisation of a single object. All these aspects make the statistical structural analysis difficult. In the present work, X-ray diffraction analysis has been applied for structural investigation of InAs nanowires grown by different techniques. Using various X-ray diffraction geometries, the nanowire systems were investigated in terms of the lattice parameters, phase composition, strains and displacement fields and stacking defects. In particular, realizing grazing incidence diffraction and controlling the penetration depth of X-ray beam, we characterized sample series grown by Au-assisted metal organic phase epitaxy on GaAs [111]B substrate with different growth time. According to the results of SEM and X-ray investigations, a model of the growth process has been proposed. A more detailed analysis was performed on InAs nanowires grown by molecular beam epitaxy (MBE) on

  19. 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

  20. 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

  1. X-ray Diffraction Study of Arsenopyrite at High Pressure

    Energy Technology Data Exchange (ETDEWEB)

    D Fan; M Ma; W Zhou; S Wei; Z Chen; H Xie

    2011-12-31

    The high-pressure X-ray diffraction study of a natural arsenopyrite was investigated up to 28.2 GPa using in situ angle-dispersive X-ray diffraction and a diamond anvil cell at National Synchrotron Light Source, Brookhaven National Laboratory. The 16:3:1 methanol-ethanol-water mixture was used as a pressure-transmitting medium. Pressures were measured using the ruby-fluorescence method. No phase change has been observed up to 28.2 GPa. The isothermal equation of state (EOS) was determined. The values of K{sub 0}, and K'{sub 0} refined with a third-order Birch-Murnaghan EOS are K{sub 0} = 123(9) GPa, and K'{sub 0} = 5.2(8). Furthermore, we confirm that the linear compressibilities ({beta}) along a, b and c directions of arsenopyrite is elastically isotropic ({beta}{sub a} = 6.82 x 10{sup -4}, {beta}{sub b} = 6.17 x 10{sup -4} and {beta}{sub c} = 6.57 x 10{sup -4} GPa{sup -1}).

  2. Characterization of Brazilian asphalt using X-ray diffraction

    International Nuclear Information System (INIS)

    Cardoso, Edson R.; Pinto, Nivia G.V.; Almeida, Ana P.G.; Braz, Delson; Lopes, Ricardo T.; Barroso, Regina C.; Motta, Laura M.G.

    2007-01-01

    Asphalt is a sticky, black and highly viscous liquid or semi-solid that is presented in most crude petroleum and in some natural deposits. The X ray diffraction can give valuable information over the characteristics of a material. Thus, the X-ray diffraction (XRD) method was employed to investigate parameters that characterize and differentiate asphalt groups (Boscan, CAP20, CAP40, CAP50/60, CAP50/70 and CAP85/100). The scattering measurements were carried out in θ-2θ reflection geometry using a powder diffractometer Shimadzu XRD-6000 at the Nuclear Instrumentation Laboratory, Brazil. Scans were typically done from 8 deg to 28 deg every 0.05. The parameters analyzed were: FWHM, peak area, peak center, peak height, left half width and right half width. Thus, in this study, scattering profiles from different asphalt groups were carefully measured in order to establish characteristic signatures of these materials. The results indicate that by using three parameters (peak centroid, peak area and peak intensity) it is possible to characterize and differentiate the asphalt. (author)

  3. Quantitative analysis of minerals by X-ray diffraction

    International Nuclear Information System (INIS)

    Pietroluongo, L.R.V.; Veiga, M.M. da

    1982-01-01

    Considerations about the X-ray diffraction technique for quantitative analyses are made; some experiments carried out at CETEM - Centro de Tecnologia Mineral (Rio de Janeiro, Brazil) with synthetic samples and real samples of diatomites (from northeastern region of Brazil) are described. Quartz quantification has been a problem for analytical chemists and is of great importance to the industries which use this raw material. Comments are made about the main factors influencing the intensity of diffracted X-rays, such as: the crystallinity of the mineral phase; the granulometry, the preferential orientation; sample preparation and pressing, the chemical composition of standards and experimental analytical conditions. Several analytical methods used are described: direct measurement of the height or area of a peak resulting from a particular reflection and comparison with a pre-calibrated curve; method of sequential addition of the mineral of interest in the sample and extrapolation of results for ZERO addition; methods of external and internal standards. (C.L.B.) [pt

  4. Energy dispersive X-ray fluorescence spectrometry for the direct multi-element analysis of dried blood spots

    Science.gov (United States)

    Marguí, E.; Queralt, I.; García-Ruiz, E.; García-González, E.; Rello, L.; Resano, M.

    2018-01-01

    Home-based collection protocols for clinical specimens are actively pursued as a means of improving life quality of patients. In this sense, dried blood spots (DBS) are proposed as a non-invasive and even self-administered alternative to sampling whole venous blood. This contribution explores the potential of energy dispersive X-ray fluorescence spectrometry for the simultaneous and direct determination of some major (S, Cl, K, Na), minor (P, Fe) and trace (Ca, Cu, Zn) elements in blood, after its deposition onto clinical filter papers, thus giving rise to DBS. For quantification purposes the best strategy was to use matrix-matched blood samples of known analyte concentrations. The accuracy and precision of the method were evaluated by analysis of a blood reference material (Seronorm™ trace elements whole blood L3). Quantitative results were obtained for the determination of P, S, Cl, K and Fe, and limits of detection for these elements were adequate, taking into account their typical concentrations in real blood samples. Determination of Na, Ca, Cu and Zn was hampered by the occurrence of high sample support (Na, Ca) and instrumental blanks (Cu, Zn). Therefore, the quantitative determination of these elements at the levels expected in blood samples was not feasible. The methodology developed was applied to the analysis of several blood samples and the results obtained were compared with those reported by standard techniques. Overall, the performance of the method developed is promising and it could be used to determine the aforementioned elements in blood samples in a simple, fast and economic way. Furthermore, its non-destructive nature enables further analyses by means of complementary techniques to be carried out.

  5. Energy dispersive X-ray spectrometry study of the protective effects of fluoride varnish and gel on enamel erosion.

    Science.gov (United States)

    De Carvalho Filho, Antonio Carlos Belfort; Sanches, Roberto Pizarro; Martin, Airton Abrahão; Do Espírito Santo, Ana Maria; Soares, Luís Eduardo Silva

    2011-09-01

    Dental erosion is a risk factor for dental health, introduced by today's lifestyle. Topical fluoride applications in the form of varnishes and gel may lead to deposition of fluoride on enamel. This in vitro study aimed to evaluate the effect of two fluoride varnishes and one fluoride gel on the dissolution of bovine enamel by acids. Enamel samples (72) were divided (n = 8): artificial saliva (control-G1), Pepsi Twist® (G2), orange juice (G3), Duraphat® + Pepsi Twist® (G4), Duraphat® + orange juice (G5), Duofluorid® + Pepsi Twist® (G6), Duofluorid® + orange juice (G7), fluoride gel + Pepsi Twist® (G8), and fluoride gel + orange juice (G9). Fluoride gel was applied for 4 min and the varnishes were applied and removed after 6 h. The samples were submitted to six cycles (demineralization: Pepsi Twist® or orange juice, 10 min; remineralization: saliva, 1 h). Samples were analyzed by energy-dispersive X-ray fluorescence (144 line-scanning). The amount of Ca and P decreased significantly in the samples of G2 and G3, and the Ca/P ratio decreased in G3. Mineral gain (Ca) was greater in G9 samples than in G4 > G3 > G5 > G1, and (P) greater in G7 samples than in G9 > G4-6 > G2-3. The protective effect of Duofluorid® was significantly lower than fluoride gel against orange juice. The fluoride varnishes can interfere positively with the dissolution of dental enamel in the presence of acidic beverages. Fluoride gel showed the best protection level to extrinsic erosion with low costs. Copyright © 2010 Wiley-Liss, Inc.

  6. Quantification of rutile in anatase by X-ray diffraction

    International Nuclear Information System (INIS)

    Chavez R, A.

    2001-01-01

    Nowadays the discovering of new and better materials required in all areas of the industry has been lead to the human being to introduce him to this small and great world. The crystalline materials, have properties markedly directional. When it is necessary to realize a quantitative analysis to these materials the task is not easy. The main objective of this work is the research of a real problem, its solution and perfecting of a technique involving the theoretical and experimental principles which allow the quantification of crystalline phases. The chapter 1 treats about the study of crystalline state during the last century, by means of the X-ray diffraction technique. The chapter 2 studies the nature and production of X-rays, the chapter 3 expounds the principles of the diffraction technique which to carry out when it is satisfied the Bragg law studying the powder diffraction method and its applications. In the chapter 4 it is explained how the intensities of the beams diffracted are determined by the atoms positions inside of the elemental cell of the crystal. The properties of the crystalline samples of anatase and rutile are described in the chapter 5. The results of this last analysis are the information which will be processed by means of the auxiliary software: Diffrac AT, Axum and Peakfit as well as the TAFOR and CUANTI software describing this part with more detail in the chapters 6 and 7 where it is mentioned step by step the function of each software until to reach the quantification of crystalline phases, objective of this work. Finally, in the chapter 8 there are a results analysis and conclusions. The contribution of this work is for those learned institutions of limited resources which can tackle in this way the characterization of materials. (Author)

  7. A new theory for X-ray diffraction.

    Science.gov (United States)

    Fewster, Paul F

    2014-05-01

    This article proposes a new theory of X-ray scattering that has particular relevance to powder diffraction. The underlying concept of this theory is that the scattering from a crystal or crystallite is distributed throughout space: this leads to the effect that enhanced scatter can be observed at the `Bragg position' even if the `Bragg condition' is not satisfied. The scatter from a single crystal or crystallite, in any fixed orientation, has the fascinating property of contributing simultaneously to many `Bragg positions'. It also explains why diffraction peaks are obtained from samples with very few crystallites, which cannot be explained with the conventional theory. The intensity ratios for an Si powder sample are predicted with greater accuracy and the temperature factors are more realistic. Another consequence is that this new theory predicts a reliability in the intensity measurements which agrees much more closely with experimental observations compared to conventional theory that is based on `Bragg-type' scatter. The role of dynamical effects (extinction etc.) is discussed and how they are suppressed with diffuse scattering. An alternative explanation for the Lorentz factor is presented that is more general and based on the capture volume in diffraction space. This theory, when applied to the scattering from powders, will evaluate the full scattering profile, including peak widths and the `background'. The theory should provide an increased understanding of the reliability of powder diffraction measurements, and may also have wider implications for the analysis of powder diffraction data, by increasing the accuracy of intensities predicted from structural models.

  8. High-pressure X-ray diffraction study of bulk- and nanocrystalline GaN

    DEFF Research Database (Denmark)

    Jorgensen, J.E.; Jakobsen, J.M.; Jiang, Jianzhong

    2003-01-01

    Bulk- and nanocrystalline GaN have been studied by high-pressure energy-dispersive X-ray diffraction. Pressure-induced structural phase transitions from the wurtzite to the NaCl phase were observed in both materials. The transition pressure was found to be 40 GPa for the bulk-crystalline GaN, while...... the wurtzite phase was retained up to 60 GPa in the case of nanocrystalline GaN. The bulk moduli for the wurtzite phases were determined to be 187 ( 7) and 319 ( 10) GPa for the bulk- and nanocrystalline phases, respectively, while the respective NaCl phases were found to have very similar bulk moduli [ 208...

  9. 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)

  10. Intensity of diffracted X-rays from biomolecules with radiation damage caused by strong X-ray pulses

    International Nuclear Information System (INIS)

    Kai, Takeshi; Tokuhisa, Atsushi; Moribayashi, Kengo; Fukuda, Yuji; Kono, Hidetoshi; Go, Nobuhiro

    2014-01-01

    In order to realize the coherent X-ray diffractive imaging of single biomolecules, the diffraction intensities, per effective pixel of a single biomolecule with radiation damage, caused by irradiation using a strong coherent X-ray pulse, were examined. A parameter survey was carried out for various experimental conditions, using a developed simulation program that considers the effect of electric field ionization, which was slightly reported on in previous studies. The two simple relationships among the parameters were identified as follows: (1) the diffraction intensity of a biomolecule slightly increases with the incident X-ray energy; and that (2) the diffraction intensity is approximately proportional to the target radius, when the radius is longer than 400 Å, since the upper limit of the incident intensity for damage to the biomolecules marginally changes with respect to the target radius. (author)

  11. Variable-metric diffraction crystals for x-ray optics

    International Nuclear Information System (INIS)

    Smither, R.K.; Fernandez, P.B.

    1992-01-01

    A variable-metric (VM) crystal is one in which the spacing between the crystalline planes changes with position in the crystal. This variation can be either parallel to the crystalline planes or perpendicular to the crystalline planes of interest and can be produced by either introducing a thermal gradient in the crystal or by growing a crystal made of two or more elements and changing the relative percentages of the two elements as the crystal is grown. A series of experiments were performed in the laboratory to demonstrate the principle of the variable-metric crystal and its potential use in synchrotron beam lines. One of the most useful applications of the VM crystal is to increase the number of photons per unit bandwidth in a diffracted beam without losing any of the overall intensity. In a normal synchrotron beam line that uses a two-crystal monochromator, the bandwidth of the diffracted photon beam is determined by the vertical opening angle of the beam which is typically 0.10--0.30 mrad or 20--60 arcsec. When the VM crystal approach is applied, the bandwidth of the beam can be made as narrow as the rocking curve of the diffracting crystal, which is typically 0.005--0.050 mrad or 1--10 arcsec. Thus a very large increase of photons per unit bandwidth (or per unit energy) can be achieved through the use of VM crystals. When the VM principle is used with bent crystals, new kinds of x-ray optical elements can be generated that can focus and defocus x-ray beams much like simple lenses where the focal length of the lens can be changed to match its application. Thus both large magnifications and large demagnifications can be achieved as well as parallel beams with narrow bandwidths

  12. X-Ray Diffraction and Fluorescence Instrument for Mineralogical Analysis at the Lunar Surface, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — We propose to develop LUNA, a compact and lightweight X-Ray Diffraction (XRD) / X-Ray Fluorescence (XRF) instrument for mineralogical analysis of regolith, rock...

  13. X-Ray Diffraction and Fluorescence Instrument for Mineralogical Analysis at the Lunar Surface, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — We propose to develop a compact and lightweight X-Ray Diffraction (XRD) / X-Ray Fluorescence (XRF) instrument for analysis of mineralogical composition of regolith,...

  14. 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.)

  15. 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.

  16. Acemetacin cocrystal structures by powder X-ray diffraction

    Science.gov (United States)

    Bolla, Geetha

    2017-01-01

    Cocrystals of acemetacin drug (ACM) with nicotinamide (NAM), p-aminobenzoic acid (PABA), valerolactam (VLM) and 2-pyridone (2HP) were prepared by melt crystallization and their X-ray crystal structures determined by high-resolution powder X-ray diffraction. The powerful technique of structure determination from powder data (SDPD) provided details of molecular packing and hydrogen bonding in pharmaceutical cocrystals of acemetacin. ACM–NAM occurs in anhydrate and hydrate forms, whereas the other structures crystallized in a single crystalline form. The carboxylic acid group of ACM forms theacid–amide dimer three-point synthon R 3 2(9)R 2 2(8)R 3 2(9) with three different syn amides (VLM, 2HP and caprolactam). The conformations of the ACM molecule observed in the crystal structures differ mainly in the mutual orientation of chlorobenzene fragment and the neighboring methyl group, being anti (type I) or syn (type II). ACM hydrate, ACM—NAM, ACM–NAM-hydrate and the piperazine salt of ACM exhibit the type I conformation, whereas ACM polymorphs and other cocrystals adopt the ACM type II conformation. Hydrogen-bond interactions in all the crystal structures were quantified by calculating their molecular electrostatic potential (MEP) surfaces. Hirshfeld surface analysis of the cocrystal surfaces shows that about 50% of the contribution is due to a combination of strong and weak O⋯H, N⋯H, Cl⋯H and C⋯H interactions. The physicochemical properties of these cocrystals are under study. PMID:28512568

  17. Acemetacin cocrystal structures by powder X-ray diffraction

    Directory of Open Access Journals (Sweden)

    Geetha Bolla

    2017-05-01

    Full Text Available Cocrystals of acemetacin drug (ACM with nicotinamide (NAM, p-aminobenzoic acid (PABA, valerolactam (VLM and 2-pyridone (2HP were prepared by melt crystallization and their X-ray crystal structures determined by high-resolution powder X-ray diffraction. The powerful technique of structure determination from powder data (SDPD provided details of molecular packing and hydrogen bonding in pharmaceutical cocrystals of acemetacin. ACM–NAM occurs in anhydrate and hydrate forms, whereas the other structures crystallized in a single crystalline form. The carboxylic acid group of ACM forms theacid–amide dimer three-point synthon R32(9R22(8R32(9 with three different syn amides (VLM, 2HP and caprolactam. The conformations of the ACM molecule observed in the crystal structures differ mainly in the mutual orientation of chlorobenzene fragment and the neighboring methyl group, being anti (type I or syn (type II. ACM hydrate, ACM—NAM, ACM–NAM-hydrate and the piperazine salt of ACM exhibit the type I conformation, whereas ACM polymorphs and other cocrystals adopt the ACM type II conformation. Hydrogen-bond interactions in all the crystal structures were quantified by calculating their molecular electrostatic potential (MEP surfaces. Hirshfeld surface analysis of the cocrystal surfaces shows that about 50% of the contribution is due to a combination of strong and weak O...H, N...H, Cl...H and C...H interactions. The physicochemical properties of these cocrystals are under study.

  18. [Diffraction gratings used in x-ray spectroscopy]: Final report

    International Nuclear Information System (INIS)

    Smith, H.I.

    1988-01-01

    This subcontract was initiated in order to facilitate the development at MIT of technologies for fabricating the very fine diffraction grating required in x-ray spectroscopy at Lawrence Livermore Laboratory (LLL). These gratings are generally gold transmission gratings with spatial periods of 200 nm or less. The major focus of our efforts was to develop a means of fabricating gratings of 100 nm period. We explored two approaches: e-beam fabrication of x-ray lithography masks, and achromatic holographic lithography. This work was pursued by Erik Anderson as a major component of his Ph.D. thesis. Erik was successful in both the e-beam and holographic approaches. However, the e-beam method proved to be highly impractical: exposure times of about 115 days would be required to cover an area of 1 cm 2 . The achromatic holography, on the other hand, should be capable of exposing areas well in excess of 1 cm 2 in times under 1 hour. Moreover, 100 nm-period gratings produced by achromatic holography are coherent over their entire area whereas gratings produced by e-beam lithography are coherent only over areas /approximately/100 μm. The remainder of this report consists of portions excerpted from Erik Anderson's thesis. These contain all the details of our work on 100 nm period gratings. 26 refs., 17 figs

  19. Biological imaging by soft X-ray diffraction microscopy

    Science.gov (United States)

    Shapiro, David

    We have developed a microscope for soft x-ray diffraction imaging of dry or frozen hydrated biological specimens. This lensless imaging system does not suffer from the resolution or specimen thickness limitations that other short wavelength microscopes experience. The microscope, currently situated at beamline 9.0.1 of the Advanced Light Source, can collect diffraction data to 12 nm resolution with 750 eV photons and 17 nm resolution with 520 eV photons. The specimen can be rotated with a precision goniometer through an angle of 160 degrees allowing for the collection of nearly complete three-dimensional diffraction data. The microscope is fully computer controlled through a graphical user interface and a scripting language automates the collection of both two-dimensional and three-dimensional data. Diffraction data from a freeze-dried dwarf yeast cell, Saccharomyces cerevisiae carrying the CLN3-1 mutation, was collected to 12 run resolution from 8 specimen orientations spanning a total rotation of 8 degrees. The diffraction data was phased using the difference map algorithm and the reconstructions provide real space images of the cell to 30 nm resolution from each of the orientations. The agreement of the different reconstructions provides confidence in the recovered, and previously unknown, structure and indicates the three dimensionality of the cell. This work represents the first imaging of the natural complex refractive contrast from a whole unstained cell by the diffraction microscopy method and has achieved a resolution superior to lens based x-ray tomographic reconstructions of similar specimens. Studies of the effects of exposure to large radiation doses were also carried out. It was determined that the freeze-dried cell suffers from an initial collapse, which is followed by a uniform, but slow, shrinkage. This structural damage to the cell is not accompanied by a diminished ability to see small features in the specimen. Preliminary measurements on frozen

  20. 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

  1. 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)

  2. 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

  3. 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).

  4. X-ray diffraction patterns of thermally-reduced graphenes

    International Nuclear Information System (INIS)

    Ju, Hae-Mi; Choi, Sung-Ho; Huh, Seung-Hun

    2010-01-01

    Thermally-reduced graphenes (GPs) from graphene oxides (GOs) in the range of 200 - 800 .deg. C have been investigated by using X-ray diffraction (XRD). The temperature-dependent evolutions of the (002) peaks show that exfoliation of GO sheets occurs, along with wrinkling, at ∼200 .deg. C and that high-quality GPs are produced at ∼ 600 .deg. C (GP 600 ). These phenomena are explained by the vaporization of intercalated water molecules and the effective removal of the oxide groups of GO by thermal annealing, respectively. GP 600 exhibited a clean and sharp (002) peak corresponding to an interlayer distance of 3.392 A, which is close to that of conventional graphene (∼3.4 A). The structure of GP 600 is further discussed.

  5. Powder X-ray diffraction laboratory, Reston, Virginia

    Science.gov (United States)

    Piatak, Nadine M.; Dulong, Frank T.; Jackson, John C.; Folger, Helen W.

    2014-01-01

    The powder x-ray diffraction (XRD) laboratory is managed jointly by the Eastern Mineral and Environmental Resources and Eastern Energy Resources Science Centers. Laboratory scientists collaborate on a wide variety of research problems involving other U.S. Geological Survey (USGS) science centers and government agencies, universities, and industry. Capabilities include identification and quantification of crystalline and amorphous phases, and crystallographic and atomic structure analysis for a wide variety of sample media. Customized laboratory procedures and analyses commonly are used to characterize non-routine samples including, but not limited to, organic and inorganic components in petroleum source rocks, ore and mine waste, clay minerals, and glassy phases. Procedures can be adapted to meet a variety of research objectives.

  6. Simulating X-ray diffraction of textured films

    DEFF Research Database (Denmark)

    Breiby, Dag W.; Bunk, Oliver; Andreasen, Jens Wenzel

    2008-01-01

    Computationally efficient simulations of grazing-incidence X-ray diffraction (GIXD) are discussed, with particular attention given to textured thin polycrystalline films on supporting substrates. A computer program has been developed for simulating scattering from thin films exhibiting varying...... degrees of preferred orientation. One emphasized common case is that of a 'fibre' symmetry axis perpendicular to the sample plane, resulting from crystallites having one well defined crystal facet towards the substrate, but no preferred inplane orientation. Peak splitting caused by additional scattering......, the mathematically simplest possible descriptions are sought whenever feasible. The practical use of the program is demonstrated for a selected thin-film example, perylene, which is of relevance for organic electronics....

  7. X-ray diffraction study of choline chloride's β form

    International Nuclear Information System (INIS)

    Petrouleas, V.; Lemmon, R.M.; Christensen, A.

    1978-01-01

    The organic salt choline chloride exists in two crystalline polymorphs. One (the α form) is extraordinarily sensitive to ionizing radiation, the other (the β form) is not. The present report describes an x-ray diffraction study of the β form. The structure has been found to be highly disordered face centered cubic. A reasonable least-square refinement of the intensity data has been achieved in the centrosymmetric space group Fm3 or Fm3m by use of a molecular model with restrained bond lengths. The results show that in the β form the electronic density due to the choline cation is closely spaced around the N, so that hydrogen bonding to the chloride is unlikely. Comparison with infrared and NMR data indicates that the disordering is dynamic and can be ascribed to rotations of the choline ion around crystallographic symmetry axes. Possible connections of these results with the radiation stability of the β form are discussed

  8. Precise rotational alignment of x-ray transmission diffraction gratings

    International Nuclear Information System (INIS)

    Hill, S.L.

    1988-01-01

    Gold transmission diffraction gratings used for x-ray spectroscopy must sometimes be rotationally aligned to the axis of a diagnostic instrument to within sub-milliradian accuracy. We have fabricated transmission diffraction gratings with high line-densities (grating period of 200 and 300 nm) using uv holographic and x-ray lithography. Since the submicron features of the gratings are not optically visible, precision alignment is time consuming and difficult to verify in situ. We have developed a technique to write an optically visible alignment pattern onto these gratings using a scanning electron microscope (SEM). At high magnification (15000 X) several submicron lines of the grating are observable in the SEM, making it possible to write an alignment pattern parallel to the grating lines in an electron-beam-sensitive coating that overlays the grating. We create an alignment pattern by following a 1-cm-long grating line using the SEM's joystick-controlled translation stage. By following the same grating line we are assured the traveled direction of the SEM electron beam is parallel to the grating to better than 10 μradian. The electron-beam-exposed line-width can be large (5 to 15 μm wide) depending on the SEM magnification, and is therefore optically visible. The exposed pattern is eventually made a permanent feature of the grating by ion beam etching or gold electroplating. The pattern can be used to accurately align the grating to the axis of a diagnostic instrument. More importantly, the alignment of the grating can be quickly verified in situ

  9. Phosphor Scanner For Imaging X-Ray Diffraction

    Science.gov (United States)

    Carter, Daniel C.; Hecht, Diana L.; Witherow, William K.

    1992-01-01

    Improved optoelectronic scanning apparatus generates digitized image of x-ray image recorded in phosphor. Scanning fiber-optic probe supplies laser light stimulating luminescence in areas of phosphor exposed to x rays. Luminescence passes through probe and fiber to integrating sphere and photomultiplier. Sensitivity and resolution exceed previously available scanners. Intended for use in x-ray crystallography, medical radiography, and molecular biology.

  10. X-ray diffraction and X-ray standing-wave study of the lead stearate film structure

    Energy Technology Data Exchange (ETDEWEB)

    Blagov, A. E.; Dyakova, Yu. A.; Kovalchuk, M. V.; Kohn, V. G.; Marchenkova, M. A.; Pisarevskiy, Yu. V.; Prosekov, P. A., E-mail: prosekov@crys.ras.ru [Russian Academy of Sciences, Shubnikov Institute of Crystallography (Russian Federation)

    2016-05-15

    A new approach to the study of the structural quality of crystals is proposed. It is based on the use of X-ray standing-wave method without measuring secondary processes and considers the multiwave interaction of diffraction reflections corresponding to different harmonics of the same crystallographic reflection. A theory of multiwave X-ray diffraction is developed to calculate the rocking curves in the X-ray diffraction scheme under consideration for a long-period quasi-one-dimensional crystal. This phase-sensitive method is used to study the structure of a multilayer lead stearate film on a silicon substrate. Some specific structural features are revealed for the surface layer of the thin film, which are most likely due to the tilt of the upper layer molecules with respect to the external normal to the film surface.

  11. 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.

  12. Nanostructured diffractive optical devices for soft X-ray microscopes

    CERN Document Server

    Hambach, D; Schneider, G

    2001-01-01

    The new transmission X-ray microscope (TXM) installed at the BESSY II electron storage ring uses an off-axis transmission zone plate (OTZ) as diffractive and focusing element of the condenser-monochromator setup. A high resolution micro-zone plate (MZP) forms a magnified image on a CCD-detector. Both, the OTZ with an active area of up to 24 mm sup 2 and the MZP with zone widths as small as 25 nm are generated by a process including electron beam lithography (EBL), dry etching and subsequent electroplating of nickel on top of silicon membrane substrates with about 100-150 nm thickness. The combination of a larger zone width and the usage of nickel zone structures allows to increase the diffraction efficiency of the condenser element at least by a factor of 3 compared to the earlier used KZP7 condenser zone plate in the TXM at BESSY I. Groove diffraction efficiencies of 21.6% and 14.7% were measured for MZP objectives with 40 and 25 nm outermost zone width, respectively.

  13. Fundamentals of powder x-ray diffraction practice

    International Nuclear Information System (INIS)

    Raftery, T.

    2002-01-01

    Full text: The goal of powder Xray diffraction is to gain information about a specimen or sample. Key aspects of this goal are 1. the sample selection, preparation and presentation; 2. the data collection process and conditions; 3. the interaction between these and the interpretation of the data. The 'ideal' powder (or polycrystalline) xray diffraction sample is fine grained, randomly orientated, homogenous and representative. There exists standard sample selection and preparation techniques for powders - sometimes however, the required information must be gained by alternate sample selection and preparation techniques. While there are few variables in the data collection process, there are some significant ones such as matching diffractometer resolution and intensity to the data collection goal whether that is phase identity, quantitative analysis or structure refinement, etc. There are also options of optical arrangement (Bragg-Brintano versus parallel beam versus Debye-Scherrer). One important aspect of the collection process is the assessment of the data quality. Powder xray diffraction has many applications from the straight-forward confirmation of phase identity and purity to structural analysis. Some of these applications will be considered and the interaction between the goal of the application and aspects of sample selection. Copyright (2002) Australian X-ray Analytical Association Inc

  14. Diagnosis of electrocution: The application of scanning electron microscope and energy-dispersive X-ray spectroscopy in five cases.

    Science.gov (United States)

    Visonà, S D; Chen, Y; Bernardi, P; Andrello, L; Osculati, A

    2018-03-01

    Deaths from electricity, generally, do not have specific findings at the autopsy. The diagnosis is commonly based on the circumstances of the death and the morphologic findings, above all the current mark. Yet, the skin injury due to an electrocution and other kinds of thermal injuries often cannot be differentiated with certainty. Therefore, there is a great interest in finding specific markers of electrocution. The search for the metallization of the skin through Scanning Electron Microscope equipped with Energy Dispersive X-Ray Spectroscopy (EDS) probe is of special importance in order to achieve a definite diagnosis in case of suspected electrocution. We selected five cases in which the electrocution was extremely likely considering the circumstances of the death. In each case a forensic autopsy was performed. Then, the skin specimens were stained with Hematoxylin Eosin and Perls. On the other hand, the skin lesions were examined with a scanning electron microscope equipped with EDS probe in order to evaluate the morphological ultrastructural features and the presence of deposits on the surface of the skin. The typical skin injury of the electrocution (current mark) were macroscopically detected in all of the cases. The microscopic examination of the skin lesions revealed the typical spherical vacuoles in the horny layer and, in the epidermis, the elongation of the cell nuclei as well as necrosis. Perls staining was negative in 4 out 6 cases. Ultrastructural morphology revealed the evident vacuolization of the horny layer, elongation of epidermic cells, coagulation of the elastic fibers. In the specimens collected from the site of contact with the conductor of case 1 and 2, the presence of the Kα peaks of iron was detected. In the corresponding specimens taken from cases 2, 4, 5 the microanalysis showed the Kα peaks of titanium. In case 3, titanium and carbon were found. In the suspicion of electrocution, the integrated use of different tools is recommended

  15. Diffracted X-ray tracking for monitoring intramolecular motion in individual protein molecules using broad band X-ray

    Energy Technology Data Exchange (ETDEWEB)

    Ichiyanagi, Kouhei; Sasaki, Yuji C. [Department of Advanced Materials Science, Graduate School of Frontier Sciences, The University of Tokyo, 609 Kiban Building 5-1-5 Kashiwanoha, Kahiwashi, Chiba 277-8561 (Japan); Japan Science and Technology Agency, CREST, CREST, Sasaki-Team, 609 Kiban Building, 5-1-5 Kashiwanoha, Kashiwa, Chiba 277-8561 (Japan); Sekiguchi, Hiroshi; Hoshino, Masato; Kajiwara, Kentaro; Senba, Yasunori; Ohashi, Haruhiko; Ohta, Noboru [Japan Synchrotron Radiation Research Institute, SPring-8, 1-1-1 Kouto, Sayo, Hyogo 679-5198 (Japan); Hoshisashi, Kentaro; Jae-won, Chang; Tokue, Maki; Matsushita, Yufuku [Department of Advanced Materials Science, Graduate School of Frontier Sciences, The University of Tokyo, 609 Kiban Building 5-1-5 Kashiwanoha, Kahiwashi, Chiba 277-8561 (Japan); Nishijima, Masaki; Inoue, Yoshihisa [Department of Applied Chemistry and Office for University-Industry Collaboration, Osaka University, 2-1 Yamadaoka, Suita, Osaka 565-0871 (Japan); Yagi, Naoto [Japan Science and Technology Agency, CREST, CREST, Sasaki-Team, 609 Kiban Building, 5-1-5 Kashiwanoha, Kashiwa, Chiba 277-8561 (Japan); Japan Synchrotron Radiation Research Institute, SPring-8, 1-1-1 Kouto, Sayo, Hyogo 679-5198 (Japan)

    2013-10-15

    Diffracted X-ray tracking (DXT) enables the tilting and twisting motions of single protein molecules to be monitored with micro- to milliradian resolution using a highly brilliant X-ray source with a wide energy bandwidth. We have developed a technique to monitor single molecules using gold nanocrystals attached to individual protein molecules using the BL28B2 beamline at SPring-8. In this paper we present the installation of a single toroidal X-ray mirror at BL28B2 to focus X-rays in an energy range of 10–20 keV (△E/E = 82% for an X-ray with a wide energy bandwidth). With this beamline we tracked diffraction spots from gold nanocrystals over a wide angle range than that using quasi-monochromatic X-rays. Application of the wide angle DXT technique to biological systems enabled us to observe the on-site motions of single protein molecules that have been functionalized in vivo. We further extend the capability of DXT by observing the fractional tilting and twisting motions of inner proteins under various conditions. As a proof of this methodology and to determine instrumental performance the intramolecular motions of a human serum albumin complex with 2-anthracenecarboxylic acid was investigated using the BL28B2 beamline. The random tilting and twisting intramolecular motions are shown to be directly linked to the movement of individual protein molecules in the buffer solution.

  16. 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.

  17. Extended X-ray absorption fine structure and X-ray diffraction studies on supported Ni catalysts

    International Nuclear Information System (INIS)

    Aldea, N.; Marginean, P.; Yaning, Xie; Tiandou, Hu; Tao, Liu; Wu, Zhongua; ZhenYa, Dai

    1999-01-01

    In the first part of this paper, we present a study based on EXAFS spectroscopy. This method can yield structural information about the local environment around a specific atomic constituent in the amorphous materials, the location and chemical state of any catalytic atom on any support or point defect structures, in alloys and composites. EXAFS is a specific technique of the scattering of X-ray on materials. The present study is aimed toward elucidation of the local structure of Ni atoms and their interaction with oxide support. The second goal of the paper consists in X-ray diffraction on the same samples. X-ray diffraction method that is capable to determine average particle size, microstrains, probability of faults as well as particle size distribution function of supported Ni catalysts is presented. The method is based on the Fourier analysis of a single X-Ray diffraction profile. The results obtained on supported nickel catalysts, which are used in H/D isotopic exchange reactions are reported. The global structure is obtained with a new fitting method based on the Generalised Fermi Function facilities for approximation and Fourier transform of the experimental X-Ray line profiles. Both types of measurements were performed on Beijing Synchrotron Radiation Facilities (BSRF). (authors)

  18. X-ray diffraction, Raman, and photoacoustic studies of ZnTe nanocrystals

    Science.gov (United States)

    Ersching, K.; Campos, C. E. M.; de Lima, J. C.; Grandi, T. A.; Souza, S. M.; da Silva, D. L.; Pizani, P. S.

    2009-06-01

    Nanocrystalline ZnTe was prepared by mechanical alloying. X-ray diffraction (XRD), energy dispersive spectroscopy, Raman spectroscopy, and photoacoustic absorption spectroscopy techniques were used to study the structural, chemical, optical, and thermal properties of the as-milled powder. An annealing of the mechanical alloyed sample at 590 °C for 6 h was done to investigate the optical properties in a defect-free sample (close to bulk form). The main crystalline phase formed was the zinc-blende ZnTe, but residual trigonal tellurium and hexagonal ZnO phases were also observed for both as-milled and annealed samples. The structural parameters, phase fractions, average crystallite sizes, and microstrains of all crystalline phases were obtained from Rietveld analyses of the X-ray patterns. Raman results corroborate the XRD results, showing the longitudinal optical phonons of ZnTe (even at third order) and those modes of trigonal Te. Nonradiative surface recombination and thermal bending heat transfer mechanisms were proposed from photoacoustic analysis. An increase in effective thermal diffusivity coefficient was observed after annealing and the carrier diffusion coefficient, the surface recombination velocity, and the recombination time parameters remained the same.

  19. An autonomous CZT module for X-ray diffraction imaging

    International Nuclear Information System (INIS)

    Montemont, G.; Monnet, O.; Stanchina, S.; Verger, L.; Kosciesza, D.; Schlomka, J.P.

    2013-01-01

    We present the development of a CZT-based detection module dedicated to X-ray diffraction imaging. This kind of application requires a good energy and spatial resolution in order to resolve Bragg peaks. In a first part, we present the detector configuration used and dimensioning constraints. As the input energy range is comprised between 20 and 150 keV, we use 5 mm thick high resistivity CZT crystals. The 660 mm 2 detection area is segmented on both sides into 192 anodes and 12 cathodes. Signals from both sides are read jointly in order to perform multi parametric event corrections (depth of interaction, charge sharing, induction sharing). In order to be integrated easily inside an X-ray imaging system, the system has been conceived to be completely autonomous: it is powered by a single 12 V supply and is interfaced with the external system by Ethernet for communication and RS485 for synchronization. In a second part, we describe the system readout architecture and then the implementation of the data processing. An FPGA circuit embeds a digital processing chain that carries out readout ASIC interfacing and advanced multi parametric data corrections. Gain, offset but also depth of interaction and charge sharing are corrected on the flow. Incoming events from different channels are clustered together by comparing their location and time of occurrence. The FPGA also embeds a processor running an operating system that controls the system, carries out all calibrations, automated tests and acquisitions. Eventually, we show the results obtained and demonstrate the relative influence of depth of interaction and charge sharing. Homogeneity of detector behavior is also discussed and the reproducibility of the performance between modules is presented. The average energy resolution at 25 C is 2.4 % FWHM at 122 keV and 3.8 % FWHM at 60 keV and the average efficiency is 73 %. (authors)

  20. IL 12: Femtosecond x-ray powder diffraction

    International Nuclear Information System (INIS)

    Woerner, M.; Zamponi, F.; Rothhardt, P.; Ansari, Z.; Dreyer, J.; Freyer, B.; Premont-Schwarz, M.; Elsaesser, T.

    2010-01-01

    A chemical reaction generates new compounds out of one or more initial species. On a molecular level, the spatial arrangement of electrons and nuclei changes. While the structure of the initial and the product molecules can be measured routinely, the transient structures and molecular motions during a reaction have remained unknown in most cases. This knowledge, however, is a key element for the exact understanding of the reaction. The ultimate dream is a 'reaction microscope' which allows for an in situ imaging of the molecules during a reaction. We report on the first femtosecond x-ray powder diffraction experiment in which we directly map the transient electronic charge density in the unit cell of a crystalline solid with 30 pico-meter spatial and 100 femtosecond temporal resolution. X-ray diffraction from polycrystalline powder samples, the Debye Scherrer diffraction technique, is a standard method for determining equilibrium structures. The intensity of the Debye Scherrer rings is determined by the respective x-ray structure factor which represents the Fourier transform of the spatial electron density. In our experiments, the transient intensity and angular positions of up to 20 Debye Scherrer reactions from a polycrystalline powder are measured and unravel for the first time a concerted electron and proton transfer in hydrogen-bonded ionic (NH 4 ) 2 SO 4 crystals. Photoexcitation of ammonium sulfate induces a sub-100 fs electron transfer from the sulfate groups into a highly conned electron channel along the z-axis of the unit cell. The latter geometry is stabilized by transferring protons from the adjacent ammonium groups into the channel. Time-dependent charge density maps derived from the diffraction data display a periodic modulation of the channels charge density by low-frequency lattice motions with a concerted electron and proton motion between the channel and the initial proton binding site. A deeper insight into the underlying microscopic

  1. X-ray diffraction using the time structure of the SRS

    International Nuclear Information System (INIS)

    Tanner, B.K.

    1983-01-01

    The subject is discussed under the headings: introduction (advances in the techniques of X-ray topography; comparison with transmission electron microscopy); stroboscopic X-ray topography; stroboscopic X-ray topography of travelling surface acoustic waves; possible general diffraction experiments. (U.K.)

  2. Sequential x-ray diffraction topography at 1-BM x-ray optics testing beamline at the advanced photon source

    Energy Technology Data Exchange (ETDEWEB)

    Stoupin, Stanislav, E-mail: sstoupin@aps.anl.gov; Shvyd’ko, Yuri; Trakhtenberg, Emil; Liu, Zunping; Lang, Keenan; Huang, Xianrong; Wieczorek, Michael; Kasman, Elina; Hammonds, John; Macrander, Albert; Assoufid, Lahsen [Advanced Photon Source, Argonne National Laboratory, Argonne, IL 60439 (United States)

    2016-07-27

    We report progress on implementation and commissioning of sequential X-ray diffraction topography at 1-BM Optics Testing Beamline of the Advanced Photon Source to accommodate growing needs of strain characterization in diffractive crystal optics and other semiconductor single crystals. The setup enables evaluation of strain in single crystals in the nearly-nondispersive double-crystal geometry. Si asymmetric collimator crystals of different crystallographic orientations were designed, fabricated and characterized using in-house capabilities. Imaging the exit beam using digital area detectors permits rapid sequential acquisition of X-ray topographs at different angular positions on the rocking curve of a crystal under investigation. Results on sensitivity and spatial resolution are reported based on experiments with high-quality Si and diamond crystals. The new setup complements laboratory-based X-ray topography capabilities of the Optics group at the Advanced Photon Source.

  3. High-Resolution Detector For X-Ray Diffraction

    Science.gov (United States)

    Carter, Daniel C.; Withrow, William K.; Pusey, Marc L.; Yost, Vaughn H.

    1988-01-01

    Proposed x-ray-sensitive imaging detector offers superior spatial resolution, counting-rate capacity, and dynamic range. Instrument based on laser-stimulated luminescence and reusable x-ray-sensitive film. Detector scans x-ray film line by line. Extracts latent image in film and simultaneously erases film for reuse. Used primarily for protein crystallography. Principle adapted to imaging detectors for electron microscopy and fluorescence spectroscopy and general use in astronomy, engineering, and medicine.

  4. Performances for confocal X-ray diffraction technology based on polycapillary slightly focusing X-ray optics

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Hehe; 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: stxbeijing@163.com [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); Sun, Weiyuan; Li, Yude; Lin, Xiaoyan; Zhao, Weigang; Zhao, Guangcui; Luo, Ping; Pan, Qiuli; 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)

    2013-09-21

    The confocal X-ray diffraction (XRD) technology based on a polycapillary slightly focusing X-ray lens (PSFXRL) in excitation channel and a polycapillary parallel X-ray lens (PPXRL) with a long input focal distance in detection channel was developed. The output focal spot of the PSFXRL and the input focal spot of the PPXRL were adjusted in confocal configuration, and only the X-rays from the volume overlapped by these foci could be accordingly detected. This confocal configuration was helpful in decreasing background. The convergence of the beam focused by the PSFXRL and divergence of the beam which could be collected by the PPXRL with a long input focal distance were both about 9 mrad at 8 keV. This was helpful in improving the resolution of lattice spacing of this confocal XRD technology. The gain in power density of such PSFXRL and PPXRL was about 120 and 7 at 11 keV, respectively, which was helpful in using the low power source to perform XRD analysis efficiently. The performances of this confocal XRD technology were provided, and some common plastics were analyzed. The experimental results demonstrated that the confocal diffraction technology base on polycapillary slightly focusing X-ray optics had wide potential applications.

  5. Two digital X-ray imaging systems for applications in X-ray diffraction

    International Nuclear Information System (INIS)

    Bateman, J.E.; Connolly, J.F.; Stephenson, R.; Flesher, A.C.; Bryant, C.J.; Lincoln, A.D.; Tucker, P.A.; Swanton, S.W.

    1986-08-01

    Two digital X-ray imaging systems developed at the Rutherford Appleton Laboratory are described:- the Mark I and the Mark II. Both use a bidimensionally sensitive Multiwire proportional counter as the basic X-ray image transducer coupled to a digital microcomputer system. The Mark I system provides the advantages of high speed, high sensitivity digital imaging directly into the computer with the potential for software control of the sample orientation and environment. The Mark II system adds the novel features of signal averaging and multi-frame exposures. (author)

  6. 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.

  7. Application of energy dispersive X-ray fluorescence technique for investigations of trace element composition in medicinal plants from Manipur

    International Nuclear Information System (INIS)

    Joseph, Daisy; Singh, Toudam Sony; Singh, Rajmohan

    2009-01-01

    Seven medicinal plants from remote areas of Manipur were analyzed for their trace elemental composition using an X-ray spectrometer consisting of a radioisotope source of 109 Cd and Si (Li) X-ray detector of resolution 170 eV at 5.9 keV Mn K-X-ray and its associated electronics. In most samples Ca, Mn, Fe and Sr were predominantly seen and Cu, Zn and Pb were detected at trace levels. The presence and significance of the elements in these medicinal plants will be presented and discussed in the following sections of the paper. (author)

  8. X-ray diffraction imaging of material microstructures

    KAUST Repository

    Varga, Laszlo; Varga, Bonbien; Calo, Victor

    2016-01-01

    Various examples are provided for x-ray imaging of the microstructure of materials. In one example, a system for non-destructive material testing includes an x-ray source configured to generate a beam spot on a test item; a grid detector configured

  9. X-ray diffraction analysis of mudstone from nw sudan

    International Nuclear Information System (INIS)

    Salih, Suad Z.Elabdeen

    1997-03-01

    This study deals with the theoretical and experimental aspects of the x-ray diffraction technique (XRD). The XRD technique is used to investigate fine structure of matter, and it is most efficient method for the determination of the mineralogical composition of rocks. The XRD technique is used also to investigate the clay mineralogical of mud-stones of the Nubian sandstones of north western Sudan. The XRD results revealed that the mud-stone samples are composed, in decreasing abundance's of kaolinite, smectite, chlorite and illite. Non-clay minerals reported include quartz, feldspars and geothite. Kaolinite dominates in most of samples with percentages ranging between 78-96%. Smectite comes second in abundance and ranges between 10-24%, followed by chlorite and illite which showed the lowest abundance's. The dominance of kaolinite over smectite indicates that intense chemical weathering and leaching occurred under warm humid climate interrupted by dry periods. Most probably these clay minerals were produced by inheritance and partly by neo formation. The variation of the chemical composition of these mud stones is due basically to differences in clay mineralogy which was controlled by source rock geology, weathering physicochemical behavior of elements, local environment and climatic condition in the past. (Author)

  10. X-Ray Powder Diffraction with Guinier - Haegg Focusing Cameras

    Energy Technology Data Exchange (ETDEWEB)

    Brown, Allan

    1970-12-15

    The Guinier - Haegg focusing camera is discussed with reference to its use as an instrument for rapid phase analysis. An actual camera and the alignment procedure employed in its setting up are described. The results obtained with the instrument are compared with those obtained with Debye - Scherrer cameras and powder diffractometers. Exposure times of 15 - 30 minutes with compounds of simple structure are roughly one-sixth of those required for Debye - Scherrer patterns. Coupled with the lower background resulting from the use of a monochromatic X-ray beam, the shorter exposure time gives a ten-fold increase in sensitivity for the detection of minor phases as compared with the Debye - Scherrer camera. Attention is paid to the precautions taken to obtain reliable Bragg angles from Guinier - Haegg film measurements, with particular reference to calibration procedures. The evaluation of unit cell parameters from Guinier - Haegg data is discussed together with the application of tests for the presence of angle-dependent systematic errors. It is concluded that with proper calibration procedures and least squares treatment of the data, accuracies of the order of 0.005% are attainable. A compilation of diffraction data for a number of compounds examined in the Active Central Laboratory at Studsvik is presented to exemplify the scope of this type of powder camera.

  11. X-Ray Powder Diffraction with Guinier - Haegg Focusing Cameras

    International Nuclear Information System (INIS)

    Brown, Allan

    1970-12-01

    The Guinier - Haegg focusing camera is discussed with reference to its use as an instrument for rapid phase analysis. An actual camera and the alignment procedure employed in its setting up are described. The results obtained with the instrument are compared with those obtained with Debye - Scherrer cameras and powder diffractometers. Exposure times of 15 - 30 minutes with compounds of simple structure are roughly one-sixth of those required for Debye - Scherrer patterns. Coupled with the lower background resulting from the use of a monochromatic X-ray beam, the shorter exposure time gives a ten-fold increase in sensitivity for the detection of minor phases as compared with the Debye - Scherrer camera. Attention is paid to the precautions taken to obtain reliable Bragg angles from Guinier - Haegg film measurements, with particular reference to calibration procedures. The evaluation of unit cell parameters from Guinier - Haegg data is discussed together with the application of tests for the presence of angle-dependent systematic errors. It is concluded that with proper calibration procedures and least squares treatment of the data, accuracies of the order of 0.005% are attainable. A compilation of diffraction data for a number of compounds examined in the Active Central Laboratory at Studsvik is presented to exemplify the scope of this type of powder camera

  12. Federated repositories of X-ray diffraction images.

    Science.gov (United States)

    Androulakis, Steve; Schmidberger, Jason; Bate, Mark A; DeGori, Ross; Beitz, Anthony; Keong, Cyrus; Cameron, Bob; McGowan, Sheena; Porter, Corrine J; Harrison, Andrew; Hunter, Jane; Martin, Jennifer L; Kobe, Bostjan; Dobson, Renwick C J; Parker, Michael W; Whisstock, James C; Gray, Joan; Treloar, Andrew; Groenewegen, David; Dickson, Neil; Buckle, Ashley M

    2008-07-01

    There is a pressing need for the archiving and curation of raw X-ray diffraction data. This information is critical for validation, methods development and improvement of archived structures. However, the relatively large size of these data sets has presented challenges for storage in a single worldwide repository such as the Protein Data Bank archive. This problem can be avoided by using a federated approach, where each institution utilizes its institutional repository for storage, with a discovery service overlaid. Institutional repositories are relatively stable and adequately funded, ensuring persistence. Here, a simple repository solution is described, utilizing Fedora open-source database software and data-annotation and deposition tools that can be deployed at any site cheaply and easily. Data sets and associated metadata from federated repositories are given a unique and persistent handle, providing a simple mechanism for search and retrieval via web interfaces. In addition to ensuring that valuable data is not lost, the provision of raw data has several uses for the crystallographic community. Most importantly, structure determination can only be truly repeated or verified when the raw data are available. Moreover, the availability of raw data is extremely useful for the development of improved methods of image analysis and data processing.

  13. X-ray topography under conditions of monochromatic spherical wave diffraction

    International Nuclear Information System (INIS)

    Aristov, V.V.; Polovinkina, V.I.; Ibhikawa, Tetsuya; Kiduta, Seishi.

    1981-01-01

    An X-ray topographic scheme was developed in which there is a large distance between the X-ray source and the specimen. A monochromatic X-ray beam with an angular divergence 6 x 10 - 5 rad obtained by double successive diffraction in the (n 1 , +n 2 ) setting was used. This scheme enables diffraction focusing of a weakly absorbed wave field onto the exit surface of the crystal to be performed. Topographs of a wedge-shaped silicon crystal were obtained. Interference effects such as focusing, anomalous and ordinary Pendelloesung effects peculiar to X-ray spherical wave diffraction were observed in the topographs with high resolution. (author)

  14. Characterization of Polycrystalline Materials Using Synchrotron X-ray Imaging and Diffraction Techniques

    DEFF Research Database (Denmark)

    Ludwig, Wolfgang; King, A.; Herbig, M.

    2010-01-01

    The combination of synchrotron radiation x-ray imaging and diffraction techniques offers new possibilities for in-situ observation of deformation and damage mechanisms in the bulk of polycrystalline materials. Minute changes in electron density (i.e., cracks, porosities) can be detected using...... propagation based phase contrast imaging, a 3-D imaging mode exploiting the coherence properties of third generation synchrotron beams. Furthermore, for some classes of polycrystalline materials, one may use a 3-D variant of x-ray diffraction imaging, termed x-ray diffraction contrast tomography. X-ray...

  15. Liquid ammonia: Molecular correlation functions from x-ray diffraction

    International Nuclear Information System (INIS)

    Narten, A.H.

    1977-01-01

    For nearly spherical molecules the x-ray scattering from liquids yields structure and correlation functions for molecular centers. The distribution of electron density in an ammonia molecular is very nearly spherical, and orientational correlation between molecules in the liquid is not ''seen'' by x rays. Structure and correlation functions for molecular centers (nitrogen atoms) are derived from x-ray data on liquid NH 3 at 4 degreeC and tabulated. They provide a sensitive test for future work on a molecular theory of liquid ammonia

  16. 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)

  17. In situ determination of K, Ca, S and Si in fresh sugar cane leaves by handheld Energy Dispersive X-Ray Fluorescence Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Guerra, Marcelo B.B.; Adame, Andressa; Almeida, Eduardo de; Brasil, Marcos A.S.; Krug, Francisco J., E-mail: fjkrug@cena.usp.br [Centro de Energia Nuclear na Agricultura, Piracicaba, SP (Brazil); Schaefer, Carlos E.G.R. [Departamento de Solos, Universidade Federal de Viçosa, MG (Brazil)

    2018-05-01

    A portable energy dispersive X-ray fluorescence spectrometer was evaluated in the in situ analysis of fresh sugar cane leaves for real time plant nutrition diagnosis. Fresh leaf fragments (n = 10 sugar cane varieties; 20 fragments per leaf; 2 measurement sites per fragment) were irradiated and the averaged data from X-ray characteristic emission lines intensities (for K, Ca, S and Si Kα lines) were in close agreement with mass fraction data obtained by a validated comparative method. The linear correlation coefficients (r) ranged from 0.9575 for Ca to 0.9851 for Si. The obtained limits of detection were at least two-fold lower than the critical nutrient levels. Manganese can also be properly determined, but validation still requires more robust calibration models. The proposed method is a straightforward approach towards the fast evaluation of the nutritional profile of plants avoiding time-consuming steps, which involve drying, grinding, weighing, and acid digestion. (author)

  18. High-resolution X-ray diffraction with no sample preparation.

    Science.gov (United States)

    Hansford, G M; Turner, S M R; Degryse, P; Shortland, A J

    2017-07-01

    It is shown that energy-dispersive X-ray diffraction (EDXRD) implemented in a back-reflection geometry is extremely insensitive to sample morphology and positioning even in a high-resolution configuration. This technique allows high-quality X-ray diffraction analysis of samples that have not been prepared and is therefore completely non-destructive. The experimental technique was implemented on beamline B18 at the Diamond Light Source synchrotron in Oxfordshire, UK. The majority of the experiments in this study were performed with pre-characterized geological materials in order to elucidate the characteristics of this novel technique and to develop the analysis methods. Results are presented that demonstrate phase identification, the derivation of precise unit-cell parameters and extraction of microstructural information on unprepared rock samples and other sample types. A particular highlight was the identification of a specific polytype of a muscovite in an unprepared mica schist sample, avoiding the time-consuming and difficult preparation steps normally required to make this type of identification. The technique was also demonstrated in application to a small number of fossil and archaeological samples. Back-reflection EDXRD implemented in a high-resolution configuration shows great potential in the crystallographic analysis of cultural heritage artefacts for the purposes of scientific research such as provenancing, as well as contributing to the formulation of conservation strategies. Possibilities for moving the technique from the synchrotron into museums are discussed. The avoidance of the need to extract samples from high-value and rare objects is a highly significant advantage, applicable also in other potential research areas such as palaeontology, and the study of meteorites and planetary materials brought to Earth by sample-return missions.

  19. 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...

  20. Determination of some elements along the length of pine needles by means of the scanning energy dispersive x-ray fluorescence (EDXRF) method

    International Nuclear Information System (INIS)

    Viksna, A.; Katkevics, J.; Nulle, S.

    1998-01-01

    The scanning energy dispersive X-ray fluorescence (EDXDF) is used to measure the distribution of trace elements along the length of single pine needles. The current set up allows simultaneous determination up to 15 trace elements. The pilot experiments showed that the distribution of some elements varied along length of the pine needle. Concentration variations of trace elements with the needle age and needle position within the foliage crown were also observed. This could be one way of studying the annual physiological cycle of needles. The scanning EDXRF method was compared with graphite furnace atomic absorption spectrometry (GFAAS). (authors)

  1. 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

  2. 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.

  3. Viability utilization of one Se sup(75) source in the analysis of uranium, thorium and rare earths for use on energy dispersive x-ray fluorescence

    International Nuclear Information System (INIS)

    Nova Mussel, W. da.

    1989-01-01

    This work is a study about the viable utilization of one Se sup(75) source as an excitation source for the use of Energy Dispersive X-Ray Fluorescence (EDXRF), in the analysis of Uranium, Thorium and the Rare Earths. The following arrangement was build up: a HPGE detector, two Se sup(75) sources in 30 sup(0) positions of castle, deadtime of 5%. Using this arrangement the calibration curve for U and Th was measured and the angular correlation coeficient was r+ 0,999, and for the Rare Earths was superior r+ 0,960. The answer given for this system was considered very fine. (author)

  4. Modelling the X-ray powder diffraction of nitrogen-expanded austenite using the Debye formula

    DEFF Research Database (Denmark)

    Oddershede, Jette; Christiansen, Thomas; Ståhl, Kenny

    2008-01-01

    Stress-free and homogeneous samples of nitrogen-expanded austenite, a defect-rich f.c.c. structure with a high interstitial nitrogen occupancy (between 0.36 and 0.61), have been studied using X-ray powder diffraction and Debye simulations. The simulations confirm the presence of deformation...... to be indistinguishable to X-ray powder diffraction....

  5. X-Ray Diffraction and the Discovery of the Structure of DNA

    Science.gov (United States)

    Crouse, David T.

    2007-01-01

    A method is described for teaching the analysis of X-ray diffraction of DNA through a series of steps utilizing the original methods used by James Watson, Francis Crick, Maurice Wilkins and Rosalind Franklin. The X-ray diffraction pattern led to the conclusion of the basic helical structure of DNA and its dimensions while basic chemical principles…

  6. 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...

  7. 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.

  8. Qualitative analysis of powder x-ray diffraction data

    International Nuclear Information System (INIS)

    Raftery, T.

    1999-01-01

    based methods of considering significant lines such as with the Hanawalt, Fink and alphabetical index; computer based search-match based on FOM and the more recent graphically based full pattern methods of phase identification. No single approach is foolproof. a range of techniques is recommended if a high level of success is required. Copyright (1999) Australian X-ray Analytical Association Inc

  9. On the theory of time-resolved x-ray diffraction

    DEFF Research Database (Denmark)

    Henriksen, Niels Engholm; Møller, Klaus Braagaard

    2008-01-01

    We derive the basic theoretical formulation for X-ray diffraction with pulsed fields, using a fully quantized description of light and matter. Relevant time scales are discussed for coherent as well as incoherent X-ray pulses, and we provide expressions to be used for calculation...... of the experimental diffraction signal for both types of X-ray sources. We present a simple analysis of time-resolved X-ray scattering for direct bond breaking in diatomic molecules. This essentially analytical approach highlights the relation between the signal and the time-dependent quantum distribution...

  10. New opportunities for 3D materials science of polycrystalline materials at the micrometre lengthscale by combined use of X-ray diffraction and X-ray imaging

    DEFF Research Database (Denmark)

    Ludwig, W.; King, A.; Reischig, P.

    2009-01-01

    Non-destructive, three-dimensional (3D) characterization of the grain structure in mono-phase polycrystalline materials is an open challenge in material science. Recent advances in synchrotron based X-ray imaging and diffraction techniques offer interesting possibilities for mapping 3D grain shapes....... A recent extension of this methodology, termed X-ray diffraction contrast tomography (DCT), combines the principles of X-ray diffraction imaging, three-dimensional X-ray diffraction microscopy (3DXRD) and image reconstruction from projections. DCT provides simultaneous access to 3D grain shape...

  11. Two digital X-ray imaging systems for applications in X-ray diffraction

    International Nuclear Information System (INIS)

    Bateman, J.E.; Connolly, J.F.; Stephenson, R.; Flesher, A.C.; Tucker, P.A.; Swanton, S.W.

    1987-01-01

    Two digital X-ray imaging systems developed at the Rutherford Appleton Laboratory are described: the Mark I and the Mark II. Both use a bidimensionally sensitive multiwire proportional counter (MWPC) as the basic X-ray image transducer coupled, in the case of the Mark I to a Digital LSI 11-23 microcomputer system via CAMAC, and in the case of the Mark II to a Digital LSI 11-73 microcomputer system via custom-built data acquisition hardware mounted directly on the Q-bus of the microcomputer. The Mark I system provides the advantages of high speed, high sensitivity digital imaging directly into the computer with the potential for software control of the sample orientation and environment. The Mark II system adds the novel features of signal averaging and multiframe exposures. The dedicated digital memories have a resolution of 512x512 pixels of 16 bits, matching well to the spatial resolution of the xenon-filled MWPC (0.5 mm fwhm over an aperture of 200 mm x 200 mm). A 512x512x4 bit video graphics system displays the images in grey scales or colour. (orig.)

  12. The phase problem and perspectives of surface X-ray diffraction

    International Nuclear Information System (INIS)

    Tajiri, Hiroo; Takahashi, Toshio

    2009-01-01

    The emergence of synchrotron radiation sources has accelerated the application of diffraction techniques to surface sciences. Surface X-ray diffraction has become the state-of-the-art technique for determining ordered structures of atoms on crystal surfaces. We introduce surface X-ray diffraction briefly from the historical point of view and describe the concept that not only determine constellation of surface atoms but also view surface atoms as image. The progress in experimental and theoretical studies of surface X-ray diffraction including crystallographic direct methods is reviewed. (author)

  13. Three-dimensional visualization of a human chromosome using coherent x-ray diffraction

    International Nuclear Information System (INIS)

    Nishino, Yoshinori; Ishikawa, Tetsuya; Takahashi, Yukio; Imamoto, Naoko; Maeshima, Kazuhiro

    2010-01-01

    We succeeded in observing a human chromosome in two- and three-dimensions using x-ray diffraction microscopy. X-ray diffraction microscopy is a lens-less imaging technique utilizing coherent x-ray diffraction, and can overcome various limitations in conventional lens-based x-ray microscopy. Biological applications of the method have been limited to 2D observation, and 3D observation has been long waited. We found that the reconstructed chromosome images contain high-density axial structure, which has not been observed under unstained or unlabeled conditions. The result experimentally demonstrates the effectiveness of x-ray diffraction microscopy in observing internal structures of unstained biological samples with high image contrast. (author)

  14. Single shot diffraction of picosecond 8.7-keV x-ray pulses

    Directory of Open Access Journals (Sweden)

    F. H. O’Shea

    2012-02-01

    Full Text Available We demonstrate multiphoton, single shot diffraction images of x rays produced by inverse Compton scattering a high-power CO_{2} laser from a relativistic electron beam, creating a pulse of 8.7 keV x rays. The tightly focused, relatively high peak brightness electron beam and high photon density from the 2 J CO_{2} laser yielded 6×10^{7} x-ray photons over the full opening angle in a single shot. Single shot x-ray diffraction is performed by passing the x rays though a vertical slit and on to a flat silicon (111 crystal. 10^{2} diffracted photons were detected. The spectrum of the detected x rays is compared to simulation. The diffraction and detection of 10^{2} x rays is a key step to a more efficient time resolved diagnostic in which the number of observed x rays might reach 10^{4}; enabling a unique, flexible x-ray source as a sub-ps resolution diagnostic for studying the evolution of chemical reactions, lattice deformation and melting, and magnetism.

  15. 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

  16. X-ray Laue diffraction with allowance for second derivatives of amplitudes in dynamical diffraction equations

    International Nuclear Information System (INIS)

    Balyan, M.K.

    2014-01-01

    Asymmetrical Laue diffraction in a perfect crystal with a plane entrance surface is considered. The second derivatives of amplitudes in the direction, perpendicular to diffraction plane in the dynamical diffraction equations are taken into account. Using the corresponding Green function a general form for the amplitude of diffracted wave in the crystal is derived. The sizes of the source in both directions as well as the source of crystal distance and non-monochromaticity of the radiation incident on the crystal are taken into account. On the basis of obtained expression the coherent properties of the field depending on the sizes of the source and on the width of the spectrum of the incident radiation are analyzed. Taking into account the second derivatives of amplitudes with respect to the direction, perpendicular to the diffraction plane, the time dependent propagation equations for an X-ray pulse in a perfect crystal are given

  17. Measurement of thickness of thin films by the X-ray diffraction method

    International Nuclear Information System (INIS)

    Srinivasan, C.; Balasingh, C.; Singh, A.K.

    1979-07-01

    X-ray diffraction method can be used to measure the thickness of thin films (coatings). The principle and the experimental details of the x-ray diffraction methods are described. The intensities of the diffracted beams are derived assuming a random orientation of the crystallites in the diffracting medium. Consequently, the expressions are not valid when the sample has preferred orientation. To check the performance of the method, thicknesses of nickel deposits on mild steel plates were determined by the x-ray diffraction method and the results compared with those obtained by the weighing method and metallographic examination. The weighing method which gives an accuracy of +- 0.1 micron is taken as the standard. The x-ray diffraction methods and the metallographic examinations give values within +- 1 micron of the value obtained by the weighing method. (author)

  18. Detectors for X-ray diffraction and scattering: a user's overview

    International Nuclear Information System (INIS)

    Bruegemann, Lutz; Gerndt, E.K.E.

    2004-01-01

    An overview of the applications of X-ray detectors to material research is given. Four experimental techniques and their specific detector requirements are described. Detector types are classified and critical parameters described in the framework of X-ray diffraction and X-ray scattering experiments. The article aims at building a bridge between detector end-users and detector developers. It gives limits of critical detector parameters, like angular resolution, energy resolution, dynamic range, and active area

  19. The application of energy-dispersive X-Ray fluorescence spectrometry (EDXRF) to the analysis of ceramic glasses

    International Nuclear Information System (INIS)

    Ben Abdelwahed, Haifa; Reguigui, Nafaa; Ghdira, Lotfi; Khosrof, S.

    2005-01-01

    The measurement of energies and intensities of fluorescent X-rays emitted from a given material when atoms are bombarded with suitable projectiles like electrons, protons, α particles or photons has been successfully used for non-destructive elemental analysis in many applications, especially in the analysis of ceramic glasses. Use of radioisotopes as a source of excitation radiation in combination with high resolution semiconductor detectors in x-ray fluorescence has found wide applications in elemental analysis. A radioisotope excited X-ray fluorescence spectrometer consisting of a standard 5.45mm Si(Li) detector having a resolution of 200 eV at 5.9 keV coupled to a TRUMP-8K multichannel analyzer has been used. Tow sources of annular geometry using 10 mCi 109Cd and 10 mCi 55Fe together with PC AXIL software have been used for this study of tile-pavement glasses of ''Ksar Said'' in Tunisia. Analytical data shows that those tile pavement witch are broken in the 19th century from France (Marseille) have not the same composition of Tunisian tile pavement. Referring to our data, The kind of that analyzed glasses is of alkaline lead. we found also, through this study, the elemental compositions of different pigments (green, blue, brownish, yellow, white and red) used to color that tile-pavement glasses

  20. The application of energy-dispersive X-Ray Fluorescence spectrometry (EDXRF) to the analysis of ceramic glasses

    International Nuclear Information System (INIS)

    Ben Abdelwahed, H.; Reguigui, N.; Ghidira, L.; Khosrof, S.

    2005-01-01

    The measurement of energies and intensities of fluorescent X-rays emitted from a given material when atoms are bombarded with suitable projectiles like electrons, protons,α particles or photons have been successfully used for non destructive elemental analysis in many applications, especially in the analysis of ceramic glasses. Use of radioisotopes as a source of excitation radiation in combination with high resolution semiconductor detectors in x-ray fluorescence has found wide applications in elemental analysis. A radioisotope excited X-ray fluorescence spectrometer consisting of a standard 5.45mm Si(Li) detector having a resolution of 200 eV at 5.9 KeV coupled to a TRUMP -8K multichannel analyser has been used. Two sources of annular geometry using 10 mCi 109 CD and 10 mCi 55 Fe together with PC AXIL software have been used for this study of tile-pavement glasses of ''Ksar Said'' in Tunisia. Analytical data shows that those tile pavements which are broken in the 19th century from France (Marseille) have not the same composition of Tunisian tile pavement. Referring to our data, the kind of that analysed glasses is of alkaline lead. We found also, through this study, the elemental compositions of different pigments (green, blue, brownish, yellow, white and red) used to color those tile-pavement glasses

  1. Grazing Incidence X-ray Scattering and Diffraction

    Indian Academy of Sciences (India)

    IAS Admin

    several materials as a function of angle of incidence, αi with X-rays of wavelength ..... are several advantages of using this formulation for the description of surface ..... print of the surface (as shown at the botton of Figure. 5). A Soller collimator ...

  2. [X-ray diffraction experiments with condenser matter

    International Nuclear Information System (INIS)

    Coppens, P.

    1990-01-01

    This report discusses research on the following topics: high-T c superconductors; The response of crystal to an applied electric field; quasicrystals; surface structure and kinetics of surface layer formation; EXAFS studies of superconductors and heterostructures; effect of iron on the crystal structure of perovskite; x-ray detector development; and SAXS experiments

  3. Structural Investigations of Nanowires Using X-Ray Diffraction

    DEFF Research Database (Denmark)

    Stankevic, Tomas

    Advancements in growth of the nanowire-based devices opened another dimension of possible structures and material combinations, which nd their applications in a wide variety of elds, including everyday life. Characterization of such devices brings its own challenges and here we show that X-rays oer...

  4. X-ray powder diffraction in forensic practice

    Czech Academy of Sciences Publication Activity Database

    Kotrlý, M.; Bezdička, Petr

    2006-01-01

    Roč. 13, č. 3 (2006), s. 153-155 ISSN 1210-8529 R&D Projects: GA MV RN20052005001 Institutional research plan: CEZ:AV0Z40320502 Keywords : X-ray powder microdiffraction * pigments * forensic practice Subject RIV: CA - Inorganic Chemistry

  5. Refractive x-ray lens for high pressure diffraction

    International Nuclear Information System (INIS)

    Ohishi, Yasuo

    2001-01-01

    A stacked compound refractive x-ray lens was designed to produce a efficiently focused (φ 2 and a peak gain of 12, is well matched to these requirements. It is composed of many plastic chips made by molding, which is allowing many identical chips to be made precisely. Other advantages of this lens include high throughput, simple energy tunability and easy installation. (author)

  6. Chemometric classification of gunshot residues based on energy dispersive X-ray microanalysis and inductively coupled plasma analysis with mass-spectrometric detection

    International Nuclear Information System (INIS)

    Steffen, S.; Otto, M.; Niewoehner, L.; Barth, M.; Brozek-Mucha, Z.; Biegstraaten, J.; Horvath, R.

    2007-01-01

    A gunshot residue sample that was collected from an object or a suspected person is automatically searched for gunshot residue relevant particles. Particle data (such as size, morphology, position on the sample for manual relocation, etc.) as well as the corresponding X-ray spectra and images are stored. According to these data, particles are classified by the analysis-software into different groups: 'gunshot residue characteristic', 'consistent with gunshot residue' and environmental particles, respectively. Potential gunshot residue particles are manually checked and - if necessary - confirmed by the operating forensic scientist. As there are continuing developments on the ammunition market worldwide, it becomes more and more difficult to assign a detected particle to a particular ammunition brand. As well, the differentiation towards environmental particles similar to gunshot residue is getting more complex. To keep external conditions unchanged, gunshot residue particles were collected using a specially designed shooting device for the test shots revealing defined shooting distances between the weapon's muzzle and the target. The data obtained as X-ray spectra of a number of particles (3000 per ammunition brand) were reduced by Fast Fourier Transformation and subjected to a chemometric evaluation by means of regularized discriminant analysis. In addition to the scanning electron microscopy in combination with energy dispersive X-ray microanalysis results, isotope ratio measurements based on inductively coupled plasma analysis with mass-spectrometric detection were carried out to provide a supplementary feature for an even lower risk of misclassification

  7. 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.

  8. 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.

  9. Chemometric classification of gunshot residues based on energy dispersive X-ray microanalysis and inductively coupled plasma analysis with mass-spectrometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Steffen, S. [Bundeskriminalamt (BKA), Forensic Science Institute KT23, Thaerstr. 11, D - 65193 Wiesbaden (Germany); Otto, M. [TU Bergakademie Freiberg (TU BAF), Institute for Analytical Chemistry, Leipziger Str. 29, D - 09599 Freiberg (Germany)], E-mail: matthias.otto@chemie.tu-freiberg.de; Niewoehner, L.; Barth, M. [Bundeskriminalamt (BKA), Forensic Science Institute KT23, Thaerstr. 11, D - 65193 Wiesbaden (Germany); Brozek-Mucha, Z. [Instytut Ekspertyz Sadowych (IES), Westerplatte St. 9, PL - 31-033 Krakow (Poland); Biegstraaten, J. [Nederlands Forensisch Instituut (NFI), Fysische Technologie, Laan van Ypenburg 6, NL-2497 GB Den Haag (Netherlands); Horvath, R. [Kriminalisticky a Expertizny Ustav (KEU PZ), Institute of Forensic Science, Sklabinska 1, SK - 812 72 Bratislava (Slovakia)

    2007-09-15

    A gunshot residue sample that was collected from an object or a suspected person is automatically searched for gunshot residue relevant particles. Particle data (such as size, morphology, position on the sample for manual relocation, etc.) as well as the corresponding X-ray spectra and images are stored. According to these data, particles are classified by the analysis-software into different groups: 'gunshot residue characteristic', 'consistent with gunshot residue' and environmental particles, respectively. Potential gunshot residue particles are manually checked and - if necessary - confirmed by the operating forensic scientist. As there are continuing developments on the ammunition market worldwide, it becomes more and more difficult to assign a detected particle to a particular ammunition brand. As well, the differentiation towards environmental particles similar to gunshot residue is getting more complex. To keep external conditions unchanged, gunshot residue particles were collected using a specially designed shooting device for the test shots revealing defined shooting distances between the weapon's muzzle and the target. The data obtained as X-ray spectra of a number of particles (3000 per ammunition brand) were reduced by Fast Fourier Transformation and subjected to a chemometric evaluation by means of regularized discriminant analysis. In addition to the scanning electron microscopy in combination with energy dispersive X-ray microanalysis results, isotope ratio measurements based on inductively coupled plasma analysis with mass-spectrometric detection were carried out to provide a supplementary feature for an even lower risk of misclassification.

  10. 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...

  11. 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).

  12. 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.

  13. 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.

  14. Physical methods for studying minerals and solid materials: X-ray, electron and neutron diffraction; scanning and transmission electron microscopy; X-ray, electron and ion spectrometry

    International Nuclear Information System (INIS)

    Eberhart, J.-P.

    1976-01-01

    The following topics are discussed: theoretical aspects of radiation-matter interactions; production and measurement of radiations (X rays, electrons, neutrons); applications of radiation interactions to the study of crystalline materials. The following techniques are presented: X-ray and neutron diffraction, electron microscopy, electron diffraction, X-ray fluorescence analysis, electron probe microanalysis, surface analysis by electron emission spectrometry (ESCA and Auger electrons), scanning electron microscopy, secondary ion emission analysis [fr

  15. Characterization of diffraction gratings by use of a tabletop soft-x-ray laser

    International Nuclear Information System (INIS)

    Seminario, Max; Rocca, Jorge J.; Depine, Ricardo A.; Bach, Benny; Bach, Bernie

    2001-01-01

    We have demonstrated the use of a high-repetition-rate 46.9-mm tabletop laser to characterize diffraction gratings designed for grazing-incidence operation in the soft-x-ray spectral region. The efficiencies for various diffraction orders were measured as a function of angle of incidence and compared with the results of model simulations. This measurement technique provides benchmarks with which to improve electromagnetic codes used in the design of soft-x-ray diffraction gratings. The results illustrate the potential of compact tabletop soft-x-ray lasers for use as a new tool for characterization of short-wavelength optics at the manufacturer's site

  16. Review - X-ray diffraction measurements in high magnetic fields and at high temperatures

    Directory of Open Access Journals (Sweden)

    Yoshifuru Mitsui, Keiichi Koyama and Kazuo Watanabe

    2009-01-01

    Full Text Available A system was developed measuring x-ray powder diffraction in high magnetic fields up to 5 T and at temperatures from 283 to 473 K. The stability of the temperature is within 1 K over 6 h. In order to examine the ability of the system, the high-field x-ray diffraction measurements were carried out for Si and a Ni-based ferromagnetic shape-memory alloy. The results show that the x-ray powder diffraction measurements in high magnetic fields and at high temperatures are useful for materials research.

  17. Electronic structure of nanoscale Cu/Pt alloys: A combined X-ray diffraction and X-ray absorption investigations

    International Nuclear Information System (INIS)

    Chen Xing; Chu Wangsheng; Cai Quan; Xia Dingguo; Wu Zhonghua; Wu Ziyu

    2006-01-01

    PVP-protected Cu/Pt clusters were prepared by glycol/water reduction method and characterized with transmission electron microscopy (TEM), X-ray diffraction (XRD) and absorption spectra. TEM and XRD analysis show that the Cu/Pt clusters with different molar ratio have fcc structure with particle size of about 4 nm, while the lattice parameters in these clusters reduce with increasing Cu concentration. From the X-ray absorption near edge structure (XANES) at Cu-K edge and Pt-L 2,3 edge, we demonstrate that the d-electronic states of Cu and Pt are affected by the local environment as a function of Cu/Pt molar ratio. With increasing Cu concentration, Pt loses a fraction of 5d electrons and the hybridization between p- and d-states at Cu sites is enhanced

  18. Electronic structure of nanoscale Cu/Pt alloys: A combined X-ray diffraction and X-ray absorption investigations

    Energy Technology Data Exchange (ETDEWEB)

    Chen Xing [Beijing Synchrotron Radiation Facility, Institute of High Energy Physics, CAS, Beijing (China); Graduate School of the Chinese Academy of Sciences, 100864 Beijing (China); Chu Wangsheng [Beijing Synchrotron Radiation Facility, Institute of High Energy Physics, CAS, Beijing (China); University of Science and Technology of China, Hefei, 230036 (China); Cai Quan [Beijing Synchrotron Radiation Facility, Institute of High Energy Physics, CAS, Beijing (China); Graduate School of the Chinese Academy of Sciences, 100864 Beijing (China); Xia Dingguo [College of Environmental and Energy Engineering, Beijing University of Technology, 100022 Beijing (China); Wu Zhonghua [Beijing Synchrotron Radiation Facility, Institute of High Energy Physics, CAS, Beijing (China); Wu Ziyu [Beijing Synchrotron Radiation Facility, Institute of High Energy Physics, CAS, Beijing (China) and National Center for Nanoscience and Technology (China)]. E-mail: wuzy@ihep.ac.cn

    2006-11-15

    PVP-protected Cu/Pt clusters were prepared by glycol/water reduction method and characterized with transmission electron microscopy (TEM), X-ray diffraction (XRD) and absorption spectra. TEM and XRD analysis show that the Cu/Pt clusters with different molar ratio have fcc structure with particle size of about 4 nm, while the lattice parameters in these clusters reduce with increasing Cu concentration. From the X-ray absorption near edge structure (XANES) at Cu-K edge and Pt-L{sub 2,3} edge, we demonstrate that the d-electronic states of Cu and Pt are affected by the local environment as a function of Cu/Pt molar ratio. With increasing Cu concentration, Pt loses a fraction of 5d electrons and the hybridization between p- and d-states at Cu sites is enhanced.

  19. Degradation of periodic multilayers as seen by small-angle x-ray scattering and x-ray diffraction

    CERN Document Server

    Rafaja, D; Simek, D; Zdeborova, L; Valvoda, V

    2002-01-01

    The capabilities of small-angle x-ray scattering (SAXS) and wide-angle x-ray diffraction (XRD) to recognize structural changes in periodic multilayers were compared on Fe/Au multilayers with different degrees of structural degradation. Experimental results have shown that both methods are equally sensitive to the multilayer degradation, i.e., to the occurrence of non-continuous interfaces, to short-circuits in the multilayer structure and to the multilayer precipitation. XRD yielded additional information on the multilayer crystallinity, whilst SAXS could better recognize fragments of a long-range periodicity (remnants of the original multilayer structure). Changes in the multilayer structure were initiated by successive annealing at 200 and 300 deg. C. Experimental data were complemented by numerical simulations performed using a combination of optical theory and the distorted wave Born approximation for SAXS or the kinematical Born approximation for XRD.

  20. X-ray diffraction studies of NbTe2 single crystal

    Indian Academy of Sciences (India)

    Unknown

    X-ray (EDAX) and remaining structural characterization was also accomplished by X-ray diffraction (XRD) studies. Lattice parameters, volume and ... The layered structure compound, NbTe2, is one of the typical materials which lead to charge .... financial assistance to carry out this work. References. Brown B E 1966 Acta ...

  1. Interaction between lipid monolayers and poloxamer 188: An X-ray reflectivity and diffraction study

    DEFF Research Database (Denmark)

    Wu, G.H.; Majewski, J.; Ege, C.

    2005-01-01

    The mechanism by which poloxamer 188 (P188) seals a damaged cell membrane is examined using the lipid monolayer as a model system. X-ray reflectivity and grazing-incidence x-ray diffraction results show that at low nominal lipid density, P188, by physically occupying the available area and phase ...

  2. Microprocessor-based system for automatic X-ray diffraction and fluorescence

    International Nuclear Information System (INIS)

    Souza, A.M. de; Carmo, L.C.S. do; Pereira, V.J.E.; Soares, E.A.

    1984-01-01

    A data acquisition and processing device appropriate for X-ray analysis and goniometer control was built. The Z-80 based system as well as the whole architeture is described. The advantages and new possibilities of the automated instrument as compared to the traditional ones are listed. The X-ray diffraction and fluorescence techniques can take advantage of the automation. (Author) [pt

  3. 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

  4. High-energy X-ray diffraction studies of disordered materials

    International Nuclear Information System (INIS)

    Kohara, Shinji; Suzuya, Kentaro

    2003-01-01

    With the arrival of the latest generation of synchrotron sources and the introduction of advanced insertion devices (wigglers and undulators), the high-energy (E≥50 keV) X-ray diffraction technique has become feasible, leading to new approaches in the quantitative study of the structure of disordered materials. High-energy X-ray diffraction has several advantages: higher resolution in real space due to a wide range of scattering vector Q, smaller correction terms (especially the absorption correction), reduction of truncation errors, the feasibility of running under extreme environments, including high-temperatures and high-pressures, and the ability to make direct comparisons between X-ray and neutron diffraction data. Recently, high-energy X-ray diffraction data have been combined with neutron diffraction data from a pulsed source to provide more detailed and reliable structural information than that hitherto available

  5. Nondestructive, energy-dispersive, x-ray fluorescence analysis of actinide stream concentrations from reprocessed nuclear fuels

    International Nuclear Information System (INIS)

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

    1979-01-01

    In one plan for reprocessing LWR spent fuel, after separation from fission products and transplutonics, part of the U and all of the Pu in a nitrate solution will form a coprocessed stream which is then evaporated and sent to a hold tank for accounting. The remaining U fraction will be purified and sent to a separate storage tank. These two streams can be monitored using x-ray fluorescence analysis. This report discusses equipment, spectra, cell calibration, and dynamic concentration measurements. 7 figures

  6. 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

  7. Curved anode wire chambers for x-ray diffraction applications

    International Nuclear Information System (INIS)

    Perez-Mendez, V.; Wiedenbeck, P.; Wagner, C.N.J.; Woelfel, E.

    1983-01-01

    Curved position sensitive proportional detectors are described. The first has a radius of curvature of 135 mm and a 60 0 angular range. The second has a radius of curvature of 360 mm and a 45 0 angular range. For high quantum efficiency for x-ray energies up to 60 keV, a relatively large x-ray path and high gas pressure are required. The anode wires are suspended in circular arcs by the interaction of a current flowing through them and a magnetic field provided by two permanent magnets placed above and below the wire running parallel to it over the full length of the curved chambers. Anode wire stability under the combined action of the magnetic and electrostatic forces is discussed

  8. Preferred orientation determination using line source x-ray diffraction

    International Nuclear Information System (INIS)

    Kimmel, G.; Shmarjahu, D.

    1977-10-01

    A texture goniometer has been attached to a diffractometer connected to a line-focus x-ray source. Reasonable results are obtained for the texture of rolled sheets and the test procedure is given. To illustrate the test procedure, the determination of preferred orientation in cold-rolled copper is described, as compared with random powder of sintered copper. Improvements of the measurements are proposed

  9. 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)

  10. Synchrotron Radiation and Energy Dispersive X-Ray Fluorescence Applications on Elemental Distribution in Human Hair and Bones

    International Nuclear Information System (INIS)

    Carvalho, M.L.; Marques, A.F.; Brito, J.

    2003-01-01

    This work is an application of synchrotron microprobe X- Ray fluorescence in order to study elemental distribution along human hair samples of contemporary citizens. Furthermore, X-Ray fluorescence spectrometry is also used to analyse human bones of different historical periods: Neolithic and contemporary subjects. The elemental content in the bones allowed us to conclude about environmental contamination, dietary habits and health status influence in the corresponding citizens. All samples were collected post-mortem. Quantitative analysis was performed for Mn, Fe, Co, Ni, Cu, Zn, Br, Rb, Sr and Pb. Mn and Fe concentration were much higher in bones from pre-historic periods. On the contrary, Pb bone concentrations of contemporary subjects are much higher than in pre-historical ones, reaching 100 μg g-1, in some cases. Very low concentrations for Co, Ni, Br and Rb were found in all the analysed samples. Cu concentrations, allows to distinguish Chalcolithic bones from the Neolithic ones. The distribution of trace elements along human hair was studied for Pb and the obtained pattern was consistent with the theoretical model, based on the diffusion of this element from the root and along the hair. Therefore, the higher concentrations in hair for Pb of contemporary individuals were also observed in the bones of citizens of the same sampling sites. All samples were analysed directly without any chemical treatment

  11. 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

  12. Reflectivity and diffraction of X rays applied to organic thin films

    International Nuclear Information System (INIS)

    Rieutord, Francois

    1987-01-01

    This research thesis reports the study of organic thin films by using X-ray-based technologies, and more particularly X-ray reflectivity. After some recalls on X ray diffraction, and on the fabrication of Langmuir-Blodgett films, the author shows how, by combining three X-ray-based techniques, it is possible to study a volume structure of a thin film. He describes the technique of measurement by X- ray reflexivity, its experimental implementation, and methods for result interpretation. In the next part, the author reports the study of peculiar interference effects which are noticed in reflexivity on Langmuir-Blodgett films, and then describes the nature of these films by correlating results of X ray reflexivity with direct observations performed by electronic microscopy on replica [fr

  13. State-of-the-art and problems of X-ray diffraction analysis of biomacromolecules

    International Nuclear Information System (INIS)

    Andreeva, N. S.

    2006-01-01

    The state-of-the-art of X-ray diffraction studies of biomacromolecules is briefly characterized, and the challenge imposed by science is discussed. These studies are characterized by a wide scope and extensive use. This field of science is of great interest and is developed in many countries. The main purpose is to solve practical problems in medicine consisting in the design of drugs against various diseases. X-ray diffraction analysis of enzymes brought the pharmaceutical industry to a new level, thus allowing the rational design of drugs against formerly untreatable diseases. Modern X-ray diffraction studies of biomacromolecules laid the basis for a new science called structural biology. This method allows one to solve fundamental problems of physical chemistry for a new state of matter existing in living systems. Here, science poses numerous problems in analysis of X-ray diffraction data on biological macromolecules. Many of theses problems are in their infancy

  14. Quantitative method of X-ray diffraction phase analysis of building materials

    International Nuclear Information System (INIS)

    Czuba, J.; Dziedzic, A.

    1978-01-01

    Quantitative method of X-ray diffraction phase analysis of building materials, with use of internal standard, has been presented. The errors committed by determining the content of particular phases have been also given. (author)

  15. Unified Theory for Decoding the Signals from X-Ray Florescence and X-Ray Diffraction of Mixtures.

    Science.gov (United States)

    Chung, Frank H

    2017-05-01

    For research and development or for solving technical problems, we often need to know the chemical composition of an unknown mixture, which is coded and stored in the signals of its X-ray fluorescence (XRF) and X-ray diffraction (XRD). X-ray fluorescence gives chemical elements, whereas XRD gives chemical compounds. The major problem in XRF and XRD analyses is the complex matrix effect. The conventional technique to deal with the matrix effect is to construct empirical calibration lines with standards for each element or compound sought, which is tedious and time-consuming. A unified theory of quantitative XRF analysis is presented here. The idea is to cancel the matrix effect mathematically. It turns out that the decoding equation for quantitative XRF analysis is identical to that for quantitative XRD analysis although the physics of XRD and XRF are fundamentally different. The XRD work has been published and practiced worldwide. The unified theory derives a new intensity-concentration equation of XRF, which is free from the matrix effect and valid for a wide range of concentrations. The linear decoding equation establishes a constant slope for each element sought, hence eliminating the work on calibration lines. The simple linear decoding equation has been verified by 18 experiments.

  16. Direct analysis of plutonium metal for gallium, iron, and nickel by energy dispersive x-ray spectrometry

    International Nuclear Information System (INIS)

    Bramlet, H.L.; Doyle, J.H.

    1981-01-01

    An x-ray secondary target method for routine determination of gallium, iron, and nickel in plutonium metal is described that has significant advantages over wet chemical analysis. Coupons requiring minimal preparation for analysis are produced as a breakaway tab on the plutonium ingot. All three elements are determined on the same coupon. Gallium is determined using an arsenic secondary target followed by iron and nickel using a zinc target. The analysis times are 5 minutes for gallium and 15 minutes for the combined iron and nickel. The method of analysis was evaluated in the range of from 0.5 to 1.5% gallium. Iron was investigated over the range of 67 to 3000 ppM and nickel from 64 to 110 ppM

  17. Study of the solid solution formation in mixed oxides by X-ray diffraction

    International Nuclear Information System (INIS)

    Riella, H.G.

    1984-01-01

    A method to determine the plutonium distribution in mixed oxides - UO 2 /PuO 2 is described. The distribution function and the medium size of crystallite are obtained from the X-ray diffraction profile. Through the deconvolution by Fourier analysis, the X-ray diffraction profile is obtained without the influence of the difractrometer. Some experimental results for different samples of UO 2 -PuO 2 discussed. (Author) [pt

  18. On the evaluation of X-ray diffraction experiments by the regularization method

    Energy Technology Data Exchange (ETDEWEB)

    Trubin, V.A.; Szasz, A. (Lab. of Surface and Interface Physics, Eoetvoes Univ., Budapest (Hungary))

    1991-05-16

    The characteristic property of diffractometers as the presence of occasional and systematic errors in measured patterns requires such an evaluation which is as informative as possible. This circumstance gives rise to the problem of optimal planning of the experiment. The X-ray diffraction optimization problem with application of the regularization method is studied. The proposal permits to determine more accurately the unknown true characteristics of the X-ray diffraction experiment. (orig.).

  19. On the evaluation of X-ray diffraction experiments by the regularization method

    International Nuclear Information System (INIS)

    Trubin, V.A.; Szasz, A.

    1991-01-01

    The characteristic property of diffractometers as the presence of occasional and systematic errors in measured patterns requires such an evaluation which is as informative as possible. This circumstance gives rise to the problem of optimal planning of the experiment. The X-ray diffraction optimization problem with application of the regularization method is studied. The proposal permits to determine more accurately the unknown true characteristics of the X-ray diffraction experiment. (orig.)

  20. Analysis of Catalonian silver coins from the Spanish War of Independence period (1808-1814) by Energy Dispersive X-ray Fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Pitarch, A., E-mail: apitarch@ija.csic.e [Laboratory of X-Ray Analytical Applications, Institute of Earth Sciences ' Jaume Almera' - ICTJA, Spanish Council for Scientific Research - CSIC, Lluis Sole Sabaris s/n, 08028 Barcelona (Spain); Queralt, I. [Laboratory of X-Ray Analytical Applications, Institute of Earth Sciences ' Jaume Almera' - ICTJA, Spanish Council for Scientific Research - CSIC, Lluis Sole Sabaris s/n, 08028 Barcelona (Spain); Alvarez-Perez, A. [Department of Geology, Faculty of Sciences, Autonomous University of Barcelona, 08193 Bellaterra, Barcelona (Spain)

    2011-02-01

    Between the years 1808 and 1814, the Spanish War of Independence took place. This period, locally known as 'Guerra del Frances', generated the need for money and consequently five mints were opened around the Catalan territory. To mark the 200th anniversary of the beginning of the war, an extensive campaign of Energy Dispersive X-ray Fluorescence measurements of some of these 'emergency coins' was carried out. Apart from the silver (major constituent of all the studied coins) it has been possible to recognize copper as main metal alloying element. Likewise, the presence of zinc, tin, lead, gold, platinum, antimony, nickel and iron has been also identified. The obtained results have been useful not only for the characterization of the alloys, but also to determine the differences and analogies between the emissions and for historical explanations.

  1. Characterization of chemical elements in soil submitted to different systems use and management by energy dispersive x-ray fluorescence spectrometry (EDXRF)

    International Nuclear Information System (INIS)

    Wastowski, Arci Dirceu; Rosa, Genesio Mario da; Cherubin, Mauricio Roberto; Rigon, Joao Paulo Gonsiorkiewicz

    2010-01-01

    This study aimed to evaluate the chemical elements levels in soil, submitted to different management systems and use by the Energy Dispersive X-Ray Fluorescence Spectrometry - EDXRF. The systems were T1 - agroforestry (SAF), T2 - native field (CN), T3 - native forest (NM), T4 - tillage forest (PF); T5 - conventional tillage system (SPC) and T6 - system tillage (NT). Samples were collected at 0-10 and 10-20 cm, dried and ground for analysis in EDX-720. The soil showed no difference in the average concentrations of chemical elements analyzed in the profiles, but the systems presented different concentrations of metal elements, and T3 had the highest K, Ca and Zn at 0-10 cm and higher contents of K, Ca, Cu, Zn and Mn in the layer of 10-20 cm. (author)

  2. A study of accumulation of trace metals in coffee plants grown on ultisols fertilized with rock phosphates by energy dispersive x-ray fluorescence (EDXRF) technique

    International Nuclear Information System (INIS)

    Joseph, Daisy; Lal, Madan; D'Souza, T.J.

    1995-01-01

    Trace elements in soil and leaves of coffee plants have been analysed by a non-destructive Energy Dispersive X-ray Fluorescence (EDXRF) technique to study their accumulation due to repeated rock phosphate fertilization. Analysis of standard reference materials of soil and leaves through EDXRF yielded values within 5% error of the certified values. This method was therefore used to determine the trace metals (Fe, Cu, Zn, Rb, Sr, Nb, Zr and Y) concentrations of soils, rock phosphates and leaves of coffee grown in experimental ultisols. Results indicate that rock phosphate fertilization over a period of 10 years did not contribute significantly to high trace metal concentration in plants. (author). 6 refs., 5 tabs., 5 figs

  3. Analysis of Heavy Metal in Electrocoagulated Metal Hydroxide Sludge (EMHS from the Textile Industry by Energy Dispersive X-Ray Fluorescence (EDXRF

    Directory of Open Access Journals (Sweden)

    Tanveer Mehedi Adyel

    2012-12-01

    Full Text Available Environmental pollution due to discharges of heavy metal containing sludge from textile industries is a common nuisance in Bangladesh, where no treatment of sludge is carried out before final disposals. Energy Dispersive X-ray Fluorescence (EDXRF was employed in the present study to analyze the heavy metal content of Electrocoagulated Metal Hydroxide Sludge (EMHS collected from a composite textile industry. Thirteen heavy metals, viz., Mn, Ti, Cu, Zn, Ni, Sr, V, Cr, Zr, Hg, Cd, Nb and Ga, were detected. Mn, Ni, Cu, Zn and Cd exceeded the permissible limit to apply the EMHS in agricultural land. Cr, Ni, Cu and Zn were compared to the values of the European legislation to evaluate the environmental risk and to classify the wastes as inert wastes or as wastes that have to be control landfilled. EMHS was categorized as class I and needs to be deposited in controlled landfills.

  4. Application of energy dispersive X-ray fluorescence spectrometry to polychrome terracotta sculptures from the Alcobaça Monastery, Portugal

    Directory of Open Access Journals (Sweden)

    Agnès Le Gac

    2014-01-01

    Full Text Available Portable energy dispersive X-ray fluorescence spectrometry (EDXRF was used in the Alcobaça Monastery, in order to study the chromatic coatings applied to terracotta statues that belong to two seventeenth-century monumental groupings. The main goal of this scientific approach consisted in determining the elemental composition of the constitutive layers and in trying to reconstitute the existing polychromy, taking into account the technical aspects observed at naked eye. The measurements carried out by EDXRF allowed a first material characterization of these artworks. By comparing the results obtained in each statue, it was possible to attest the application of a seventeenth-century coating to each one and at least a subsequent intervention in the form of a refurbishment or a new polychromy. According to the materials employed in their production, it appears that the refurbishment is likely dated from the 19th century while the new polychromy is still dated from the 18th century.

  5. Nondestructive multielement analyses of airborne particulates by combined uses of instrumental neutron activation analysis and energy dispersive X-ray fluorescence analysis

    International Nuclear Information System (INIS)

    Mamuro, Tetsuo; Matsuda, Yatsuka; Mizohata, Akira

    1974-01-01

    Combined uses of instrumental neutron activation analysis and energy dispersive X-ray fluorescence analysis make it possible to analyze nondestructively a considerably large number of elements in airborne particulates. We have confirmed that up to 45 elements can be analyzed without any chemical procedures for urban airborne particulate samples. As the radiation spectrometry by semiconductor detectors and the automatic data reduction by electronic computation are quite common to the two techniques, combined uses of them produce no special annoyance. Several elements can be analyzed by both of them and therefore the reliability of the analytical results can be comfirmed by comparing the data obtained by them with each other. It is noted that this confirmation can be made for the very same sample. In this article are described our experiences of multielement analyses of airborne particulates and some problems to be solved in further studies. (auth.)

  6. Nanometer-scale, quantitative composition mappings of InGaN layers from a combination of scanning transmission electron microscopy and energy dispersive x-ray spectroscopy

    International Nuclear Information System (INIS)

    Pantzas, K; Voss, P L; Ougazzaden, A; Patriarche, G; Largeau, L; Mauguin, O; Troadec, D; Gautier, S; Moudakir, T; Suresh, S

    2012-01-01

    Using elastic scattering theory we show that a small set of energy dispersive x-ray spectroscopy (EDX) measurements is sufficient to experimentally evaluate the scattering function of electrons in high-angle annular dark field scanning transmission microscopy (HAADF-STEM). We then demonstrate how to use this function to transform qualitative HAADF-STEM images of InGaN layers into precise, quantitative chemical maps of the indium composition. The maps obtained in this way combine the resolution of HAADF-STEM and the chemical precision of EDX. We illustrate the potential of such chemical maps by using them to investigate nanometer-scale fluctuations in the indium composition and their impact on the growth of epitaxial InGaN layers. (paper)

  7. 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.)

  8. 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.

  9. Device for high-temperature X-ray diffraction analysis. Ustrojstvo dlya vysokotemperaturnogo rentgenostrukturnogo analiza

    Energy Technology Data Exchange (ETDEWEB)

    Epifanov, V G; Zavilinskij, A V; Pet' kov, V V; Polenur, A V

    1975-01-07

    Device for high-temperature X-ray diffraction analysis, containing a vacuum chamber with a window for X-ray transit, in which sample- and standard-holders, heater, thermal shields and means for standard and sample temperature measurement are located, is proposed. In order to increase the working temperature level and the structural change detection accuracy the heater is located between the sample- and standard-holders. The standard-holder is linked with the mechanism of control of its position in relation to the heater. The device is intended for investigating phase transformations by differential thermal analysis method with the simultaneous diffraction pattern detection using X-ray diffractometry method.

  10. Neutron and X-ray diffraction from modulated structures

    International Nuclear Information System (INIS)

    Harris, P.

    1994-07-01

    This thesis describes X-ray and neutron scattering experiments performed on two examples of modulated structures. After an introduction to the subject of modulated structures, the thesis is divided in three parts. A single crystal elastic neutron scattering experiment between 4.2 and 115 Κ has been performed and four-circle X-ray data have been collected at 8 Κ for the monoclinic low-temperature phase of the layered perovskite PAMC. The results from the neutron scattering experiment indicate that magnetoelastic effects influence the ordering of the crystal. The X-ray experiments have made it possible to determine the crystal structure in the low-temperature phase. The superspace group is P2 1 /b(β-30)Os, with β = 1/3. A small-angle neutron scattering experiment has been performed on the magnetic structure of manganese silicide. When a magnetic field is applied, the modulation vectors turn towards the field direction, showing domain growth and diverging peak widths as they approach the field direction. Phase 'A' is established to have the modulation vectors directed perpendicular to the field direction. Cooling in zero field shows increasing peak widths at low temperatures, indicating a lock-in transition below the lowest reached temperature. To be able to analyse the data of the magnetic order in MnSi, and analytical calculation of the three dimensional resolution function for a small-angle neutron scattering spectrometer has been performed. The calculation is done by application of a combination of phase space analysis and Gaussian approximations for the neutron distribution as well as for the transmission functions of the different apertures. A finite mosaic spread of the crystal and finite correlation widths of the Bragg reflections have been included in the cross section. (au) (3 tabs., 48 ills., 100 refs.)

  11. X-ray diffraction study of surface-layer structure in parallel grazing rays

    International Nuclear Information System (INIS)

    Shtypulyak, N.I.; Yakimov, I.I.; Litvintsev, V.V.

    1989-01-01

    An x-ray diffraction method is described for study of thin polycrystalline and amorphous films and surface layers in an extremely asymmetrical diffraction system in parallel grazing rays using a DRON-3.0 diffractometer. The minimum grazing angles correspond to diffraction under conditions of total external reflection and a layer depth of ∼ 2.5-8 nm

  12. X-ray and Neutron Diffraction in the Study of Organic Crystalline Hydrates

    Directory of Open Access Journals (Sweden)

    Katharina Fucke

    2010-07-01

    Full Text Available A review. Diffraction methods are a powerful tool to investigate the crystal structure of organic compounds in general and their hydrates in particular. The laboratory standard technique of single crystal X-ray diffraction gives information about the molecular conformation, packing and hydrogen bonding in the crystal structure, while powder X-ray diffraction on bulk material can trace hydration/dehydration processes and phase transitions under non-ambient conditions. Neutron diffraction is a valuable complementary technique to X-ray diffraction and gives highly accurate hydrogen atom positions due to the interaction of the radiation with the atomic nuclei. Although not yet often applied to organic hydrates, neutron single crystal and neutron powder diffraction give precise structural data on hydrogen bonding networks which will help explain why hydrates form in the first place.

  13. Background removal in X-ray fiber diffraction patterns

    International Nuclear Information System (INIS)

    Millane, R.P.; Arnott, S.

    1985-01-01

    Background can be a major source of error in measurement of diffracted intensities in fiber diffraction patterns. Errors can be large when poorly oriented less-crystalline specimens give diffraction patterns with little uncontaminated background. A method for estimating and removing a general global background in such cases is described and illustrated with an example. (orig.)

  14. 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.

  15. Evaluation of In-Vacuum Imaging Plate Detector for X-Ray Diffraction Microscopy

    International Nuclear Information System (INIS)

    Nishino, Yoshinori; Takahashi, Yukio; Yamamoto, Masaki; Ishikawa, Tetsuya

    2007-01-01

    We performed evaluation tests of a newly developed in-vacuum imaging plate (IP) detector for x-ray diffraction microscopy. IP detectors have advantages over direct x-ray detection charge-coupled device (CCD) detectors, which have been commonly used in x-ray diffraction microscopy experiments, in the capabilities for a high photon count and for a wide area. The detector system contains two IPs to make measurement efficient by recording data with the one while reading or erasing the other. We compared speckled diffraction patterns of single particles taken with the IP and a direct x-ray detection CCD. The IP was inferior to the CCD in spatial resolution and in signal-to-noise ratio at a low photon count

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

    International Nuclear Information System (INIS)

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

    2013-01-01

    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 mm 2 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. - Highlights: • Demonstration of an EDXRF imaging system based on a 2D-MHSP detector for biological analysis • Evaluation of the drift of the dental amalgam constituents, throughout the teeth • Observation of Hg diffusion, due to hydroxyapatite crystal defects that compose the teeth tissues

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

    Energy Technology Data Exchange (ETDEWEB)

    Silva, A.L.M. [I3N, Physics Dept, University of Aveiro, 3810-193 Aveiro (Portugal); Figueroa, R.; Jaramillo, A. [Physics Department, Universidad de La Frontera, Temuco (Chile); Carvalho, M.L. [Atomic Physics Centre, University of Lisbon, 1649-03 Lisboa (Portugal); Veloso, J.F.C.A., E-mail: joao.veloso@ua.pt [I3N, Physics Dept, University of Aveiro, 3810-193 Aveiro (Portugal)

    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 mm{sup 2} 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. - Highlights: • Demonstration of an EDXRF imaging system based on a 2D-MHSP detector for biological analysis • Evaluation of the drift of the dental amalgam constituents, throughout the teeth • Observation of Hg diffusion, due to hydroxyapatite crystal defects that compose the teeth tissues.

  18. 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.

  19. 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)

  20. Separation and determination of arsenic and selenium in natural water samples by energy dispersive X-ray fluorescence

    International Nuclear Information System (INIS)

    Moreira, Silvana; Gregorio, Mauricio Abud

    2002-01-01

    This work had as main objective to study a method for separation and determination of Arsenic (III) and (V), and Selenium (IV) and (VI) present in aqueous solutions at trace level. For this purpose a preconcentration method based on the adsorption of the elements in activated charcoal loaded with zirconium (ZrC * ) was used. The ion As (III) was better absorbed onto 200 mg ZrC * in pH 8, while, the ion As (V) presented better results when the absorption was carried out onto 100 mg ZrC * with the pH adjusted for 2. The ions Se (IV) and Se (VI) presented a better absorption when the solutions were adjusted for pH 4, but with different masses of ZrC * , 200 mg for Se (IV) and for Se (VI) just 100 mg. The detection limits obtained by the X-ray fluorescence were 0.050 mg.L -1 and 0.009 mg.L -1 for As (III) and As (V), respectively. In the case of selenium the limits were 0.011 mg.L -1 and 0.016 mg.L -1 for Se (IV) and (VI) species, respectively. The errors obtained by this methodology were smaller than 2% for the ion As (III) and smaller than 1% for As (V), Se (IV) and Se (VI). (author)

  1. Combining operando synchrotron X-ray tomographic microscopy and scanning X-ray diffraction to study lithium ion batteries

    Science.gov (United States)

    Pietsch, Patrick; Hess, Michael; Ludwig, Wolfgang; Eller, Jens; Wood, Vanessa

    2016-06-01

    We present an operando study of a lithium ion battery combining scanning X-ray diffraction (SXRD) and synchrotron radiation X-ray tomographic microscopy (SRXTM) simultaneously for the first time. This combination of techniques facilitates the investigation of dynamic processes in lithium ion batteries containing amorphous and/or weakly attenuating active materials. While amorphous materials pose a challenge for diffraction techniques, weakly attenuating material systems pose a challenge for attenuation-contrast tomography. Furthermore, combining SXRD and SRXTM can be used to correlate processes occurring at the atomic level in the crystal lattices of the active materials with those at the scale of electrode microstructure. To demonstrate the benefits of this approach, we investigate a silicon powder electrode in lithium metal half-cell configuration. Combining SXRD and SRXTM, we are able to (i) quantify the dissolution of the metallic lithium electrode and the expansion of the silicon electrode, (ii) better understand the formation of the Li15Si4 phase, and (iii) non-invasively probe kinetic limitations within the silicon electrode. A simple model based on the 1D diffusion equation allows us to qualitatively understand the observed kinetics and demonstrates why high-capacity electrodes are more prone to inhomogeneous lithiation reactions.

  2. Combining operando synchrotron X-ray tomographic microscopy and scanning X-ray diffraction to study lithium ion batteries

    Science.gov (United States)

    Pietsch, Patrick; Hess, Michael; Ludwig, Wolfgang; Eller, Jens; Wood, Vanessa

    2016-01-01

    We present an operando study of a lithium ion battery combining scanning X-ray diffraction (SXRD) and synchrotron radiation X-ray tomographic microscopy (SRXTM) simultaneously for the first time. This combination of techniques facilitates the investigation of dynamic processes in lithium ion batteries containing amorphous and/or weakly attenuating active materials. While amorphous materials pose a challenge for diffraction techniques, weakly attenuating material systems pose a challenge for attenuation-contrast tomography. Furthermore, combining SXRD and SRXTM can be used to correlate processes occurring at the atomic level in the crystal lattices of the active materials with those at the scale of electrode microstructure. To demonstrate the benefits of this approach, we investigate a silicon powder electrode in lithium metal half-cell configuration. Combining SXRD and SRXTM, we are able to (i) quantify the dissolution of the metallic lithium electrode and the expansion of the silicon electrode, (ii) better understand the formation of the Li15Si4 phase, and (iii) non-invasively probe kinetic limitations within the silicon electrode. A simple model based on the 1D diffusion equation allows us to qualitatively understand the observed kinetics and demonstrates why high-capacity electrodes are more prone to inhomogeneous lithiation reactions. PMID:27324109

  3. 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.)

  4. 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.

  5. 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.

  6. Mineralogy of the clay fraction of soils from the moray cusco archaeological site: a study by energy dispersive X-ray fluorescence, X-ray diffractometry and Mössbauer spectroscopy

    International Nuclear Information System (INIS)

    Cerón Loayza, María L.; Bravo Cabrejos, Jorge A.; Mejía Santillán, Mirian E.

    2011-01-01

    The purpose of this work is to report the advances in the elemental and structural characterization of the clay fraction of soils from the terraces of the Moray Archaeological site, located 38 km north of the city of Cusco, Cusco Region. One sample was collected from each of the twelve terraces of this site and its clay fraction was separated by sedimentation. Previously the pH of the raw samples was measured resulting that all of the samples were from alkaline to strongly alkaline. Energy dispersive X-ray fluorescence (EDXRF) was used for the elemental characterization, and X-ray diffractometry (XRD) and transmission Mössbauer spectroscopy (TMS), using the γ 14.4 keV nuclear resonance transition in 57 Fe, were used for the structural characterization of the clays and clay minerals present in each sample. The EDXRF analyses of all the samples show the presence of relatively high concentrations of sulfur in some of the samples and relatively high concentrations of calcium in all of the samples, which may be related to the high alkalinity of the samples. By XRD it is observed the presence of quartz, calcite, gypsum, cronstedtite, 2:1 phyllosilicates, and iron oxides. The mineralogical analysis of Fe by TMS shows that it is present in the form of hematite and occupying Fe 2 +  and Fe 3 +  sites in phyllosilicates, cronstedtite, and other minerals not yet identified.

  7. Mineralogy of the clay fraction of soils from the moray cusco archaeological site: a study by energy dispersive X-ray fluorescence, X-ray diffractometry and Moessbauer spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-11-15

    The purpose of this work is to report the advances in the elemental and structural characterization of the clay fraction of soils from the terraces of the Moray Archaeological site, located 38 km north of the city of Cusco, Cusco Region. One sample was collected from each of the twelve terraces of this site and its clay fraction was separated by sedimentation. Previously the pH of the raw samples was measured resulting that all of the samples were from alkaline to strongly alkaline. Energy dispersive X-ray fluorescence (EDXRF) was used for the elemental characterization, and X-ray diffractometry (XRD) and transmission Moessbauer spectroscopy (TMS), using the {gamma} 14.4 keV nuclear resonance transition in {sup 57}Fe, were used for the structural characterization of the clays and clay minerals present in each sample. The EDXRF analyses of all the samples show the presence of relatively high concentrations of sulfur in some of the samples and relatively high concentrations of calcium in all of the samples, which may be related to the high alkalinity of the samples. By XRD it is observed the presence of quartz, calcite, gypsum, cronstedtite, 2:1 phyllosilicates, and iron oxides. The mineralogical analysis of Fe by TMS shows that it is present in the form of hematite and occupying Fe{sup 2 + } and Fe{sup 3 + } sites in phyllosilicates, cronstedtite, and other minerals not yet identified.

  8. 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.

  9. 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.

  10. Characterization of particulate matter from the Metropolitan Zone of the Valley of Mexico by scanning electron microscopy and energy-dispersive x-ray analysis

    International Nuclear Information System (INIS)

    Martiez, T.; Lartigue, J.; Avila-Perez, P.; Carapio-Morales, L.; Zarazua, G.; Tejeda, S.

    2005-01-01

    The urban air pollution issue is a concern in many Mega cities, because of hazardous effect to human health. The Metropolitan Zone of the Valley of Mexico (MZMV) is one of the ten largest urban areas around the World with a population of 24.4 million people by the year 2000. One or the 'six criteria pollutants' regulated by Norm (because the hazardous effect to human health) are those commonly designed as Total Suspended Particles (TSP) and Respirable Particles (RP) lower than 10 μm (coarse, PM10 and fine PM2.5). Particulate matter consists of solids or liquid aerosol particles suspended in the air and has diverse chemical composition related to the sources. Under ambient conditions of sampling analysis particulate matter exists almost exclusively in solid phase but can include liquid aerosols such as the heavier components of diesel combustion products and nitric acid. In general particulate matter includes dust, dirt, soot, smoke and liquid droplets emitted in the air by sources such as factories, power plants, cars, fire, construction activities, aircrafts and winds blown dust. In this work the survey of TSP particles an PM10 was carried out with an automatic high volume sampler with an average flow rate of 1.5 m 3 min -1 during 24 h in five monitoring stations of the national network system chosen trying to cover the fourth cardinal directions and the central zone: Xalostoc (XAL) at NE; Tlanepantla (TLA) at NW; Merced (MER) at the downtown; Cerro de la Estrella (CES) at SE and Pedregal (PED) at SW. A sample of l cm 2 was cut from each filter and mounted with a graphite tape on an aluminum sample-holder. The analysis of 100 induvidual particles of each sample were done by scanning electron microscopy and energy-dispersive X-ray microanalysis (EDX). The analysis was performed using a scanning electron microscope PHILLIPS Model XL-30. X-ray analysis is carried out with an energy-dispersive Si(Li) detector Model Saphire, SUTW (super ultra thin window), allowing

  11. Advanced x-ray stress analysis method for a single crystal using different diffraction plane families

    International Nuclear Information System (INIS)

    Imafuku, Muneyuki; Suzuki, Hiroshi; Sueyoshi, Kazuyuki; Akita, Koichi; Ohya, Shin-ichi

    2008-01-01

    Generalized formula of the x-ray stress analysis for a single crystal with unknown stress-free lattice parameter was proposed. This method enables us to evaluate the plane stress states with any combination of diffraction planes. We can choose and combine the appropriate x-ray sources and diffraction plane families, depending on the sample orientation and the apparatus, whenever diffraction condition is satisfied. The analysis of plane stress distributions in an iron single crystal was demonstrated combining with the diffraction data for Fe{211} and Fe{310} plane families

  12. 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

  13. Applications of synchrotron x-ray diffraction topography to fractography

    International Nuclear Information System (INIS)

    Bilello, J.C.

    1983-01-01

    Fractographs have been taken using a variety of probes each of which produces different types of information. Methods which have been used to examine fracture surfaces include: (a) optical microscopy, particularly interference contrast methods, (b) scanning electron microscopy (SEM), (c) SEM with electron channelling, (d) SEM with selected-area electron channelling, (e) Berg-Barrett (B-B) topography, and now (f) synchrotron x-radiation fractography (SXRF). This review concentrated on the role that x-ray methods can play in such studies. In particular, the ability to nondestructively assess the subsurface microstructure associated with the fracture to depths of the order of 5 to 10 μm becomes an important attribute for observations of a large class of semi-brittle metals, semiconductors and ceramics

  14. X-ray and neutron diffraction studies of crystallinity in hydroxyapatite coatings.

    Science.gov (United States)

    Girardin, E; Millet, P; Lodini, A

    2000-02-01

    To standardize industrial implant production and make comparisons between different experimental results, we have to be able to quantify the crystallinity of hydroxyapatite. Methods of measuring crystallinity ratio were developed for various HA samples before and after plasma spraying. The first series of methods uses X-ray diffraction. The advantage of these methods is that X-ray diffraction equipment is used widely in science and industry. In the second series, a neutron diffraction method is developed and the results recorded are similar to those obtained by the modified X-ray diffraction methods. The advantage of neutron diffraction is the ability to obtain measurements deep inside a component. It is a nondestructive method, owing to the very low absorption of neutrons in most materials. Copyright 2000 John Wiley & Sons, Inc.

  15. High Pressure X-Ray Diffraction Studies on Nanocrystalline Materials

    Science.gov (United States)

    Palosz, B.; Stelmakh, S.; Grzanka, E.; Gierlotka, S.; Pielaszek, R.; Bismayer, U.; Werner, S.; Palosz, W.

    2003-01-01

    Application of in situ high pressure powder diffraction technique for examination of specific structural properties of nanocrystals based on the experimental data of SiC nanocrystalline powders of 2 to 30 nrn diameter in diameter is presented. Limitations and capabilities of the experimental techniques themselves and methods of diffraction data elaboration applied to nanocrystals with very small dimensions (nanoparticles of different grain size.

  16. Comparative study of macrotexture analysis using X-ray diffraction and electron backscattered diffraction techniques

    International Nuclear Information System (INIS)

    Serna, Marilene Morelli

    2002-01-01

    The macrotexture is one of the main characteristics in metallic materials, which the physical properties depend on the crystallographic direction. The analysis of the macrotexture to middles of the decade of 80 was just accomplished by the techniques of Xray diffraction and neutrons diffraction. The possibility of the analysis of the macrotexture using, the technique of electron backscattering diffraction in the scanning electronic microscope, that allowed to correlate the measure of the orientation with its location in the micro structure, was a very welcome tool in the area of engineering of materials. In this work it was studied the theoretical aspects of the two techniques and it was used of both techniques for the analysis of the macrotexture of aluminum sheets 1050 and 3003 with intensity, measured through the texture index 'J', from 2.00 to 5.00. The results obtained by the two techniques were shown reasonably similar, being considered that the statistics of the data obtained by the technique of electron backscatter diffraction is much inferior to the obtained by the X-ray diffraction. (author)

  17. Measurements of transient electron density distributions by femtosecond X-ray diffraction

    International Nuclear Information System (INIS)

    Freyer, Benjamin

    2013-01-01

    This thesis concerns measurements of transient charge density maps by femtosecond X-ray diffraction. Different X-ray diffraction methods will be considered, particularly with regard to their application in femtosecond X-ray diffraction. The rotation method is commonly used in stationary X-ray diffraction. In the work in hand an X-ray diffraction experiment is demonstrated, which combines the method with ultrafast X-ray pulses. This experiment is the first implementation which makes use of the rotation method to map transient intensities of a multitude of Bragg reflections. As a prototype material Bismuth is used, which previously was studied frequently by femtosecond X-ray diffraction by measuring Bragg reflections successively. The experimental results of the present work are compared with the literature data. In the second part a powder-diffraction experiment will be presented, which is used to study the dynamics of the electron-density distribution on ultrafast time scales. The experiment investigates a transition metal complex after photoexcitation of the metal to ligand charge transfer state. Besides expected results, i. e. the change of the bond length between the metal and the ligand and the transfer of electronic charge from the metal to the ligand, a strong contribution of the anion to the charge transfer was found. Furthermore, the charge transfer has predominantly a cooperative character. That is, the excitation of a single complex causes an alteration of the charge density of several neighboring units. The results show that more than 30 transition-metal complexes and 60 anions contribute to the charge transfer. This collective response is a consequence of the strong coulomb interactions of the densely packed ions.

  18. X-ray radiation damage of organic semiconductor thin films during grazing incidence diffraction experiments

    Energy Technology Data Exchange (ETDEWEB)

    Neuhold, A., E-mail: alfred.neuhold@tugraz.at [Institute of Solid State Physics, Graz University of Technology, Graz (Austria); Novak, J.; Flesch, H.-G.; Moser, A.; Djuric, T. [Institute of Solid State Physics, Graz University of Technology, Graz (Austria); Grodd, L.; Grigorian, S.; Pietsch, U. [Institute of Physics, University Siegen (Germany); Resel, R. [Institute of Solid State Physics, Graz University of Technology, Graz (Austria)

    2012-08-01

    Since modern synchrotrons with highly intense X-ray beams are in use to investigate organic materials, the stability of soft matter materials during beam exposure is a crucial issue. Grazing incidence X-ray diffraction and specular X-ray reflectivity measurements were performed on thin films of organic semiconducting materials, like poly(3-hexylthiophene) (P3HT), sexithiophene and pentacene. These films were irradiated with an average flux density between 10{sup 15} and 10{sup 16} photons/(s mm{sup 2}) and evidenced a different stability in synchrotron X-ray radiation. The semi-crystalline P3HT showed a clear intensity decrease of the 1 0 0 Bragg peak and 0 2 0 Bragg peak compared to the rather stable diffraction features of the molecular crystals sexithiophene and pentacene. The difference in synchrotron X-ray radiation stability is explained by the interaction of the X-ray beam with the individual chemical components in the molecules as well as by the different crystallinities of the materials. Furthermore, the semi-crystalline P3HT film exhibited an increase of film thickness after irradiation and the surface roughness slightly decreased. To summarize, this study shows a strong influence of synchrotron X-ray radiation to specific organic thin films like e.g. P3HT, while others like pentacene and sexithiophene are observed as quite stable.

  19. Microbeam high-resolution diffraction and x-ray standing wave methods applied to semiconductor structures

    International Nuclear Information System (INIS)

    Kazimirov, A; Bilderback, D H; Huang, R; Sirenko, A; Ougazzaden, A

    2004-01-01

    A new approach to conditioning x-ray microbeams for high angular resolution x-ray diffraction and scattering techniques is introduced. We combined focusing optics (one-bounce imaging capillary) and post-focusing collimating optics (miniature Si(004) channel-cut crystal) to generate an x-ray microbeam with a size of 10 μm and ultimate angular resolution of 14 μrad. The microbeam was used to analyse the strain in sub-micron thick InGaAsP epitaxial layers grown on an InP(100) substrate by the selective area growth technique in narrow openings between the oxide stripes. For the structures for which the diffraction peaks from the substrate and the film overlap, the x-ray standing wave technique was applied for precise measurements of the strain with a Δd/d resolution of better than 10 -4 . (rapid communication)

  20. Three-Dimensional X-Ray Diffraction Technique for Metals Science

    DEFF Research Database (Denmark)

    Zhang, Yubin; Fan, Guohua

    2017-01-01

    The three-dimensional X-ray diffraction (3DXRD) is a new, advanced technique for materials characterization. This technique utilizes high-energy synchrotron X-rays to characterize the 3D crystallographic structure and strain/stress state of bulk materials. As the measurement is non......-destructive, the microstructural evolution as a function of time can be followed, i.e. it allows 4D (x, y, z characterizations, t). The high brilliance of synchrotron X-rays ensures that diffraction signals from volumes of micrometer scale can be quickly detected and distinguished from the background noise, i.e. its spatial...... implemented in several large synchrotron facilities, e.g. the Advanced Photon Source (APS) in USA and the Spring-8 in Japan. Another family of 3DXRD technique that utilizes white beam synchrotron X-rays has also been developed in parallel in cooperation between Oak Ridge National Laboratory and APS...

  1. New tubes and techniques for flash X-ray diffraction and high contrast radiography

    International Nuclear Information System (INIS)

    Charbonnier, F.M.; Barbour, J.P.; Brewster, J.L.

    High energy electrons are particularly efficient in producing characteristic X-rays and soft polychromatic. A line of wide spectrum beryllium window flash X-ray tubes, ranging from 150 to 600kV, has been developed to exploit this property. Laue and Debye Scherrer flash X-ray diffraction patterns have been obtained using a single 30 ns pulse exposure. X-ray diffraction tests obtained are shown. Extremely high contrast flash radiography of small, low density objects has been obtained using industrial film without screen. Alternatively, particularly at high voltages and for subjects which include a broad range of materials and thicknesses, special film techniques can be used to produce extremely wide latitudes. Equipment, techniques and results are discussed

  2. Information extracting and processing with diffraction enhanced imaging of X-ray

    International Nuclear Information System (INIS)

    Chen Bo; Chinese Academy of Science, Beijing; Chen Chunchong; Jiang Fan; Chen Jie; Ming Hai; Shu Hang; Zhu Peiping; Wang Junyue; Yuan Qingxi; Wu Ziyu

    2006-01-01

    X-ray imaging at high energies has been used for many years in many fields. Conventional X-ray imaging is based on the different absorption within a sample. It is difficult to distinguish different tissues of a biological sample because of their small difference in absorption. The authors use the diffraction enhanced imaging (DEI) method. The authors took images of absorption, extinction, scattering and refractivity. In the end, the authors presented pictures of high resolution with all these information combined. (authors)

  3. Dynamical x-ray diffraction studies of interfacial strain in superlattices grown by molecular beam epitaxy

    International Nuclear Information System (INIS)

    Vandenberg, J.M.; Chu, S.N.G.; Hamm, R.A.; Panish, M.B.; Ritter, D.; Mancrander, A.T.

    1992-01-01

    This paper reports on dynamical X-ray diffraction studies that have been carried out for lattice-matched InGaAs/InP superlattices grown by modified molecular beam epitaxy (MBE) techniques. The (400) X-ray satellite pattern, which is predominantly affected by the strain modulation, was analyzed. The strain and thickness of the actual layers including the presence of strained interfacial regions were determined

  4. Model experiment of in vivo synchrotron X-ray diffraction of human kidney stones

    Energy Technology Data Exchange (ETDEWEB)

    Ancharov, A.I. [Institute of Solid State Chemistry and Mechanochemistry SB RAS, Novosibirsk (Russian Federation)]. E-mail: ancharov@mail.ru; Potapov, S.S. [Institute of Mineralogy UB RAS, Miass (Russian Federation); Moiseenko, T.N. [The State Regional Clinical Hospital, Novosibirsk (Russian Federation); Feofilov, I.V. [The State Regional Clinical Hospital, Novosibirsk (Russian Federation); Nizovskii, A.I. [Boreskov Institute of Catalysis SB RAS, Novosibirsk (Russian Federation)

    2007-05-21

    The diffraction of synchrotron radiation (SR) was used to explore the phase composition of kidney stones placed into a specific object phantom, which imitated the human body. As an imitation of the patient breath, the kidney stone was moved vertically and rotated to an angle of 15{sup o} during the recording of the X-ray pattern. It was shown that rotation and displacement did not distort the X-ray pattern.

  5. Model experiment of in vivo synchrotron X-ray diffraction of human kidney stones

    International Nuclear Information System (INIS)

    Ancharov, A.I.; Potapov, S.S.; Moiseenko, T.N.; Feofilov, I.V.; Nizovskii, A.I.

    2007-01-01

    The diffraction of synchrotron radiation (SR) was used to explore the phase composition of kidney stones placed into a specific object phantom, which imitated the human body. As an imitation of the patient breath, the kidney stone was moved vertically and rotated to an angle of 15 o during the recording of the X-ray pattern. It was shown that rotation and displacement did not distort the X-ray pattern

  6. Ultrafast Structural Dynamics in InSb Probed by Time-Resolved X-Ray Diffraction

    International Nuclear Information System (INIS)

    Chin, A.H.; Shank, C.V.; Chin, A.H.; Schoenlein, R.W.; Shank, C.V.; Glover, T.E.; Leemans, W.P.; Balling, P.

    1999-01-01

    Ultrafast structural dynamics in laser-perturbed InSb are studied using time-resolved x-ray diffraction with a novel femtosecond x-ray source. We report the first observation of a delay in the onset of lattice expansion, which we attribute to energy relaxation processes and lattice strain propagation. In addition, we observe direct indications of ultrafast disordering on a subpicosecond time scale. copyright 1999 The American Physical Society

  7. Diffractive-refractive optics: (+,-,-,+) X-ray crystal monochromator with harmonics separation

    Czech Academy of Sciences Publication Activity Database

    Hrdý, Jaromír; Mikulík, P.; Oberta, Peter

    2011-01-01

    Roč. 18, č. 2 (2011), s. 299-301 ISSN 0909-0495 R&D Projects: GA MPO FR-TI1/412 Institutional research plan: CEZ:AV0Z10100522 Keywords : diffractive-refractive optics * x-ray synchrotron radiation monochromator * x-ray crystal monochromator * harmonics separation Subject RIV: BH - Optics, Masers, Lasers Impact factor: 2.726, year: 2011

  8. Nano-fabrication of diffractive optics for soft X-ray and atom beam focusing

    International Nuclear Information System (INIS)

    Rehbein, S.

    2002-01-01

    Nano-structuring processes are described for manufacturing diffractive optics for the condenser-monochromator set-up of the transmission X-ray microscope (TXM) and for the scanning transmission X-ray microscope (STXM) at the BESSY II electron storage ring in Berlin. Furthermore, a process for manufacturing free-standing nickel zone plates for helium atom beam focusing experiments is presented. (author)

  9. The discovery of X-ray diffraction by crystals and its great impact on science

    International Nuclear Information System (INIS)

    Mai Zhenhong

    2012-01-01

    In April 1912, Friedrich, Knipping and Laue discovered X-ray diffraction in a CuSO 4 crystal. Later, Laue derived the famous Laue equations which explain the diffraction phenomenon. For this, Laue was awarded a Nobel Prize for Physics in 1914. In 1912 W. H. Bragg and W. L. Bragg received news of Laue 's discovery, and from X-ray diffraction experiments in a ZnS crystal they derived the famous Bragg equation. For this work, father and son were together awarded the Nobel Prize for Physics in 1915, To commemorate the 100th anniversary of the discovery of X-ray diffraction, this article reviews the important contributions of the early pioneers and their historic impact on science and technology worldwide. (author)

  10. Materials identification using a small-scale pixellated x-ray diffraction system

    International Nuclear Information System (INIS)

    O’Flynn, D; Crews, C; Drakos, I; Christodoulou, C; Speller, R D; Wilson, M D; Veale, M C; Seller, P

    2016-01-01

    A transmission x-ray diffraction system has been developed using a pixellated, energy-resolving detector (HEXITEC) and a small-scale, mains operated x-ray source (Amptek Mini-X). HEXITEC enables diffraction to be measured without the requirement of incident spectrum filtration, or collimation of the scatter from the sample, preserving a large proportion of the useful signal compared with other diffraction techniques. Due to this efficiency, sufficient molecular information for material identification can be obtained within 5 s despite the relatively low x-ray source power. Diffraction data are presented from caffeine, hexamine, paracetamol, plastic explosives and narcotics. The capability to determine molecular information from aspirin tablets inside their packaging is demonstrated. Material selectivity and the potential for a sample classification model is shown with principal component analysis, through which each different material can be clearly resolved. (paper)

  11. Size effect in X-ray and electron diffraction patterns from hydroxyapatite particles

    International Nuclear Information System (INIS)

    Suvorova, E.I.; Buffat, P.-A.

    2001-01-01

    High-resolution transmission electron microscopy (HRTEM), electron microdiffraction, and X-ray diffraction were used to study hydroxyapatite specimens with particle sizes from a few nanometers to several hundreds of nanometers. Diffuse scattering (without clear reflections in transmission diffraction patterns) or strongly broadened peaks in X-ray diffraction patterns are characteristic for agglomerated hydroxyapatite nanocrystals. However, HRTEM and microdiffraction showed that this cannot be considered as an indication of the amorphous state of the matter but rather as the demonstration of size effect and the morphological and structural features of hydroxyapatite nanocrystals

  12. Mechanical characterisation of surface layers by x-ray diffraction -application to tribology

    International Nuclear Information System (INIS)

    Farrahi, G.H.

    1996-01-01

    The results presented in this paper show that X-ray diffraction can be employed for the characterisation of surface layer damage through residual stresses and work hardening by some tribological actions such as fretting and dry sliding. X-ray diffraction technique can also be employed for a rapid and non-destructive measurement of hardness of hardened steel. The diffraction profile analysis can offer a good indication about the materials characteristics and the microstructural evolution caused by heat treatment or by mechanical loading

  13. Examining the ground layer of St. Anthony from Padua 19th century oil painting by Raman spectroscopy, scanning electron microscopy and X-ray diffraction

    International Nuclear Information System (INIS)

    Vančo, Ľubomír; Kadlečíková, Magdaléna; Breza, Juraj; Čaplovič, Ľubomír; Gregor, Miloš

    2013-01-01

    Highlights: ► Raman spectroscopic examination of uncovered and covered paint layers of a real painting. ► Deconvolution of Raman peaks of lead white. ► Comparison of results with energy-dispersive analysis and X-ray diffraction. - Abstract: In this paper we studied the material composition of the ground layer of a neoclassical painting. We used Raman spectroscopy (RS) as a prime method. Thereafter scanning electron microscopy combined with energy dispersive spectroscopy (SEM–EDS) and X-ray powder diffraction (XRD) were employed as complementary techniques. The painting inspected was of the side altar in King St. Stephen's Church in Galanta (Slovakia), signed and dated by Jos. Chr. Mayer 1870. Analysis was carried out on both covered and uncovered ground layers. Four principal compounds (barite, lead white, calcite, dolomite) and two minor compounds (sphalerite, quartz) were identified. This ground composition is consistent with the 19th century painting technique used in Central Europe consisting of white pigments and white fillers. Transformation of lead white occurred under laser irradiation. Subdominant Raman peaks of the components were measured. The observed results elucidate useful partnership of RS and SEM–EDS measurements supported by X-ray powder diffraction as well as possibilities and limitations of non-destructive analysis of covered lower layers by RS.

  14. In-situ X-ray diffraction : a useful tool to investigate hydride-formation reactions

    NARCIS (Netherlands)

    Notten, P.H.L.; Daams, J.L.C.; Veirman, de A.E.M.; Staals, A.A.

    1994-01-01

    A high-pressure X-ray diffraction (XRD) cell has been designed which allowed us to study simultaneously hydrogen absorption/desorption isotherms and XRD powder diffraction patterns on (de)hydrided intermetallic compounds. The hydride formation reaction was investigated in the case of LaNi5 under

  15. Small angle X ray diffraction investigation of twinned opal_like structures

    NARCIS (Netherlands)

    Samusev, A.K.; Sinev, I.S.; Samusev, K.B.; Rybin, M.V.; Mistonov, A.A.; Grigoryeva, N.A.; Grigoriev, S.V.; Petukhov, A.V.; Byelov, D.; Trofimova, E.Y.; Kurdyukov, D.A.; Golubev, V.G.; Limonov, M.F.

    2012-01-01

    Small angle X ray diffraction from synthetic opal films has been investigated as a function of the orientation of the sample. All the observed (hkl) diffraction reflections have been interpreted. The reconstruct tion of the reciprocal lattice of the studied opal films has been carried out. The

  16. Analytic theory of soft x-ray diffraction by lamellar multilayer gratings

    NARCIS (Netherlands)

    Kozhevnikov, I.V.; van der Meer, R.; Bastiaens, Hubertus M.J.; Boller, Klaus J.; Bijkerk, Frederik

    2011-01-01

    An analytic theory describing soft x-ray diffraction by Lamellar Multilayer Gratings (LMG) has been developed. The theory is derived from a coupled waves approach for LMGs operating in the single-order regime, where an incident plane wave can only excite a single diffraction order. The results from

  17. X-ray diffraction investigation of the sulphur induced 4x1 reconstruction of Ni(110)

    DEFF Research Database (Denmark)

    Foss, M.; Feidenhans'l, R.; Nielsen, M.

    1993-01-01

    The atomic structure of the Ni(110)4 x 1-S reconstruction has been determined on the basis of surface X-ray diffraction measurements. An analysis of the in-plane diffraction data shows that the model consists of Ni rows along the [001] direction, two for every 4 x 1 unit cell, corresponding to 0....

  18. New structural studies of liquid crystal by reflectivity and resonant X-ray diffraction

    International Nuclear Information System (INIS)

    Fernandes, P.

    2007-04-01

    This memory presents three structural studies of smectic Liquid Crystals by reflectivity and resonant diffraction of X-rays. It is divided in five chapters. In the first a short introduction to Liquid Crystals is given. In particular, the smectic phases that are the object of this study are presented. The second chapter is consecrated to the X-ray experimental techniques that were used in this work. The three last chapters present the works on which this thesis can be divided. Chapter three demonstrates on free-standing films of MHPOBC (historic liquid crystal that possesses the antiferroelectric sub-phases) the possibility to extend the technique of resonant X-ray diffraction to liquid crystals without resonant element. In the fourth chapter the structure of the B 2 liquid crystal phase of bent-core molecules (or banana molecules) is elucidated by using resonant X-ray diffraction combined with polarization analysis of the diffracted beam. A model of the polarization of the resonant beam diffracted by four different structures proposed for the B 2 phase is developed in this chapter. In the fifth chapter a smectic binary mixture presenting a very original critical point of phase separation is studied by X-ray reflectivity and optical microscopy. A concentration gradient in the direction perpendicular to the plane of the film seems to be induced by the free-standing film geometry. The results of a simplified model of the system are compatible with this interpretation

  19. Takagi-Taupin description of x-ray dynamical diffraction from diffractive optics with large numerical aperture

    International Nuclear Information System (INIS)

    Yan Hanfei; Maser, Joerg; Macrander, Albert; Shen Qun; Vogt, Stefan; Stephenson, G. Brian; Kang, Hyon Chol

    2007-01-01

    We present a formalism of x-ray dynamical diffraction from volume diffractive optics with large numerical aperture and high aspect ratio, in an analogy to the Takagi-Taupin equations [Acta Crystallogr. 15, 1311 (1962); Bull. Soc. Fr. Mineral. Crystallogr. 87, 469 (1964)] for strained single crystals. We derive a set of basic equations for dynamical diffraction from volume diffractive optics, which enable us to study the focusing property of these optics with various grating profiles. We study volume diffractive optics that satisfy the Bragg condition to various degrees, namely, flat, tilted, and wedged geometries, and derive the curved geometries required for ultimate focusing. We show that the curved geometries satisfy both the Bragg condition everywhere and phase requirement for point focusing and effectively focus hard x rays to a scale close to the wavelength. Our calculations were made for an x-ray wavelength of 0.064 nm (19.5 keV)

  20. X-ray diffraction and X-ray K absorption near edge studies of copper (II) complexes with amino acids

    Science.gov (United States)

    Sharma, P. K.; Mishra, Ashutosh; Malviya, Varsha; Kame, Rashmi; Malviya, P. K.

    2017-05-01

    Synthesis of copper (II) complexes [CuL1L2X].nH2O, where n=1, 2,3 (X=Cl,Br,NO3) (L1is 2,2’-bipyridine and L2 is L-tyrosine) by the chemical root method. The XRD data for the samples have been recorded. EXAFS spectra have also been recorded at the K-edge of Cu using the dispersive beam line BL-8 at 2.5 Gev Indus-2 Synchrotron radiation source at RRCAT, Indore, India. XRD and EXAFS data have been analysed using the computer software. X-ray diffraction studies of all complexes indicate their crystalline nature. Lattice parameter, bond length, particle size have been determined from XRD data.

  1. The materials science synchrotron beamline EDDI for energy-dispersive diffraction analysis

    International Nuclear Information System (INIS)

    Genzel, Ch.; Denks, I.A.; Gibmeier, J.; Klaus, M.; Wagener, G.

    2007-01-01

    In April 2005 the materials science beamline EDDI (Energy Dispersive DIffraction) at the Berlin synchrotron storage ring BESSY started operation. The beamline is operated in the energy-dispersive mode of diffraction using the high energy white photon beam provided by a superconducting 7 T multipole wiggler. Starting from basic information on the beamline set-up, its measuring facilities and data processing concept, the wide range of applications for energy-dispersive diffraction is demonstrated by a series of examples coming from different fields in materials sciences. It will be shown, that the EDDI beamline is especially suitable for the investigation of structural properties and gradients in the near surface region of polycrystalline materials. In particular, this concerns the analysis of multiaxial residual stress fields in the highly stressed surface zone of technical parts. The high photon flux further facilitates fast in situ experiments at room as well as high temperature to monitor for example the growth kinetics and reaction in thin film growth

  2. Use of X-ray fluorescence energy dispersive technique in the lead determination and other metals in excrements of otters (Lontra longicaudis)

    International Nuclear Information System (INIS)

    Moraes, Liz Mary B.; Silva, Richard M.C.; Nascimento Filho, Virgilio F.; Ferreira, Carla Josef; Adriano, Leonardo R.; Ferreira, Jose Roberto

    2005-01-01

    This work had for objective to evaluate the contamination for Pb and other metals (Ti, Mn, Fe, Ni, Cu and Zn) in excrement samples of a neotropical otter population specie, found in river Betari, Alto Vale do Ribeira basin, Southeast Sao Paulo State. This river is a tributary of the Ribeira de Iguape river and part of its passage meets inside of the Parque Estadual Turistico do Alto Ribeira, one of the most conserved area of Brazilian Atlantic Forest. As the diet of these animals is based in fishes, it is an environmental interest in the determination of Pb in its excrements, since that is accumulating on the tropical chain path and in this region (in the decade of 1970) had the implanted a Pb extraction from galena mining. The analysis of the samples requires frequently the chemical digestion, with the disadvantages of being weak and expense. Aiming at to eliminate these disadvantages, the objective of the work was to use the X-ray fluorescence energy dispersive technique (EDXRF), for demanding a minimum preparation of the sample. Six excrement samples had been frozen, lyophilized and cryogenically milled, and after analyzed as pellet form, using a X-ray tube (target Mo, Zr filter, 25 kV/10 mA) and Si(Li) semiconductor spectrometer. The concentration was varied from 5.0 to 15.4 μg g -1 and it was possible also quantified other metals, showing maximum concentrations: Ti - 308, Mn - 38, Fe - 1131, Ni - 44, Cu . 2.8 and Zn . 92.4 μg g -1 . (author)

  3. Direct rapid analysis of trace bioavailable soil macronutrients by chemometrics-assisted energy dispersive X-ray fluorescence and scattering spectrometry.

    Science.gov (United States)

    Kaniu, M I; Angeyo, K H; Mwala, A K; Mangala, M J

    2012-06-04

    Precision agriculture depends on the knowledge and management of soil quality (SQ), which calls for affordable, simple and rapid but accurate analysis of bioavailable soil nutrients. Conventional SQ analysis methods are tedious and expensive. We demonstrate the utility of a new chemometrics-assisted energy dispersive X-ray fluorescence and scattering (EDXRFS) spectroscopy method we have developed for direct rapid analysis of trace 'bioavailable' macronutrients (i.e. C, N, Na, Mg, P) in soils. The method exploits, in addition to X-ray fluorescence, the scatter peaks detected from soil pellets to develop a model for SQ analysis. Spectra were acquired from soil samples held in a Teflon holder analyzed using (109)Cd isotope source EDXRF spectrometer for 200 s. Chemometric techniques namely principal component analysis (PCA), partial least squares (PLS) and artificial neural networks (ANNs) were utilized for pattern recognition based on fluorescence and Compton scatter peaks regions, and to develop multivariate quantitative calibration models based on Compton scatter peak respectively. SQ analyses were realized with high CMD (R(2)>0.9) and low SEP (0.01% for N and Na, 0.05% for C, 0.08% for Mg and 1.98 μg g(-1) for P). Comparison of predicted macronutrients with reference standards using a one-way ANOVA test showed no statistical difference at 95% confidence level. To the best of the authors' knowledge, this is the first time that an XRF method has demonstrated utility in trace analysis of macronutrients in soil or related matrices. Copyright © 2012 Elsevier B.V. All rights reserved.

  4. Direct rapid analysis of trace bioavailable soil macronutrients by chemometrics-assisted energy dispersive X-ray fluorescence and scattering spectrometry

    International Nuclear Information System (INIS)

    Kaniu, M.I.; Angeyo, K.H.; Mwala, A.K.; Mangala, M.J.

    2012-01-01

    Highlights: ► Chemometrics-assisted EDXRFS spectroscopy realizes direct, rapid and accurate analysis of trace bioavailable macronutrients in soils. ► The method is minimally invasive, involves little sample preparation, short analysis times and is relatively insensitive to matrix effects. ► This opens up the ability to rapidly characterize large number of samples/matrices with this method. - Abstract: Precision agriculture depends on the knowledge and management of soil quality (SQ), which calls for affordable, simple and rapid but accurate analysis of bioavailable soil nutrients. Conventional SQ analysis methods are tedious and expensive. We demonstrate the utility of a new chemometrics-assisted energy dispersive X-ray fluorescence and scattering (EDXRFS) spectroscopy method we have developed for direct rapid analysis of trace ‘bioavailable’ macronutrients (i.e. C, N, Na, Mg, P) in soils. The method exploits, in addition to X-ray fluorescence, the scatter peaks detected from soil pellets to develop a model for SQ analysis. Spectra were acquired from soil samples held in a Teflon holder analyzed using 109 Cd isotope source EDXRF spectrometer for 200 s. Chemometric techniques namely principal component analysis (PCA), partial least squares (PLS) and artificial neural networks (ANNs) were utilized for pattern recognition based on fluorescence and Compton scatter peaks regions, and to develop multivariate quantitative calibration models based on Compton scatter peak respectively. SQ analyses were realized with high CMD (R 2 > 0.9) and low SEP (0.01% for N and Na, 0.05% for C, 0.08% for Mg and 1.98 μg g −1 for P). Comparison of predicted macronutrients with reference standards using a one-way ANOVA test showed no statistical difference at 95% confidence level. To the best of the authors’ knowledge, this is the first time that an XRF method has demonstrated utility in trace analysis of macronutrients in soil or related matrices.

  5. Data processing software suite SITENNO for coherent X-ray diffraction imaging using the X-ray free-electron laser SACLA

    International Nuclear Information System (INIS)

    Sekiguchi, Yuki; Oroguchi, Tomotaka; Takayama, Yuki; Nakasako, Masayoshi

    2014-01-01

    The software suite SITENNO is developed for processing diffraction data collected in coherent X-ray diffraction imaging experiments of non-crystalline particles using an X-ray free-electron laser. Coherent X-ray diffraction imaging is a promising technique for visualizing the structures of non-crystalline particles with dimensions of micrometers to sub-micrometers. Recently, X-ray free-electron laser sources have enabled efficient experiments in the ‘diffraction before destruction’ scheme. Diffraction experiments have been conducted at SPring-8 Angstrom Compact free-electron LAser (SACLA) using the custom-made diffraction apparatus KOTOBUKI-1 and two multiport CCD detectors. In the experiments, ten thousands of single-shot diffraction patterns can be collected within several hours. Then, diffraction patterns with significant levels of intensity suitable for structural analysis must be found, direct-beam positions in diffraction patterns determined, diffraction patterns from the two CCD detectors merged, and phase-retrieval calculations for structural analyses performed. A software suite named SITENNO has been developed to semi-automatically apply the four-step processing to a huge number of diffraction data. Here, details of the algorithm used in the suite are described and the performance for approximately 9000 diffraction patterns collected from cuboid-shaped copper oxide particles reported. Using the SITENNO suite, it is possible to conduct experiments with data processing immediately after the data collection, and to characterize the size distribution and internal structures of the non-crystalline particles

  6. Combined X-ray and neutron fibre diffraction studies of biological and synthetic polymers

    International Nuclear Information System (INIS)

    Parrot, I.M.; Urban, V.; Gardner, K.H.; Forsyth, V.T.

    2005-01-01

    The fibrous state is a natural one for polymer molecules which tend to assume regular helical conformations rather than the globular structures characteristic of many proteins. Fibre diffraction therefore has broad application to the study of a wide range of biological and synthetic polymers. The purpose of this paper is to illustrate the general scope of the method and in particular to demonstrate the impact of a combined approach involving both X-ray and neutron diffraction methods. While the flux of modern X-ray synchrotron radiation sources allows high quality datasets to be recorded with good resolution within a very short space of time, neutron studies can provide unique information through the ability to locate hydrogen or deuterium atoms that are often difficult or impossible to locate using X-ray methods. Furthermore, neutron fibre diffraction methods can, through the ability to selectively label specific parts of a structure, be used to highlight novel aspects of polymer structure that can not be studied using X-rays. Two examples are given. The first describes X-ray and neutron diffraction studies of conformational transitions in DNA. The second describes structural studies of the synthetic high-performance polymer poly(p-phenylene terephthalamide) (PPTA), known commercially as Kevlar[reg] or Twaron[reg

  7. Combined X-ray and neutron fibre diffraction studies of biological and synthetic polymers.

    Energy Technology Data Exchange (ETDEWEB)

    Parrot, I. M. [Institut Laue-Langevin (ILL); Urban, Volker S [ORNL; Gardner, K. H. [DuPont Experimental Station; Forsyth, V. T. [Institut Laue Langevin and Keele University

    2005-04-01

    The fibrous state is a natural one for polymer molecules which tend to assume regular helical conformations rather than the globular structures characteristic of many proteins. Fibre diffraction therefore has broad application to the study of a wide range of biological and synthetic polymers. The purpose of this paper is to illustrate the general scope of the method and in particular to demonstrate the impact of a combined approach involving both X-ray and neutron diffraction methods. While the flux of modern X-ray synchrotron radiation sources allows high quality datasets to be recorded with good resolution within a very short space of time, neutron studies can provide unique information through the ability to locate hydrogen or deuterium atoms that are often difficult or impossible to locate using X-ray methods. Furthermore, neutron fibre diffraction methods can, through the ability to selectively label specific parts of a structure, be used to highlight novel aspects of polymer structure that can not be studied using X-rays. Two examples are given. The first describes X-ray and neutron diffraction studies of conformational transitions in DNA. The second describes structural studies of the synthetic high-performance polymer poly(p-phenylene terephthalamide) (PPTA), known commercially as Kevlar{reg_sign} or Twaron{reg_sign}.

  8. Combined X-ray and neutron fibre diffraction studies of biological and synthetic polymers

    Science.gov (United States)

    Parrot, I. M.; Urban, V.; Gardner, K. H.; Forsyth, V. T.

    2005-08-01

    The fibrous state is a natural one for polymer molecules which tend to assume regular helical conformations rather than the globular structures characteristic of many proteins. Fibre diffraction therefore has broad application to the study of a wide range of biological and synthetic polymers. The purpose of this paper is to illustrate the general scope of the method and in particular to demonstrate the impact of a combined approach involving both X-ray and neutron diffraction methods. While the flux of modern X-ray synchrotron radiation sources allows high quality datasets to be recorded with good resolution within a very short space of time, neutron studies can provide unique information through the ability to locate hydrogen or deuterium atoms that are often difficult or impossible to locate using X-ray methods. Furthermore, neutron fibre diffraction methods can, through the ability to selectively label specific parts of a structure, be used to highlight novel aspects of polymer structure that can not be studied using X-rays. Two examples are given. The first describes X-ray and neutron diffraction studies of conformational transitions in DNA. The second describes structural studies of the synthetic high-performance polymer poly(p-phenylene terephthalamide) (PPTA), known commercially as Kevlar® or Twaron®.

  9. Combined X-ray and neutron fibre diffraction studies of biological and synthetic polymers

    Energy Technology Data Exchange (ETDEWEB)

    Parrot, I.M. [Institut Laue Langevin, 6 Rue Jules Horowitz, 38042 Grenoble Cedex 9 (France); Institute of Science and Technology in Medicine, Keele University Medical School, Staffordshire ST4 7QB (United Kingdom); Urban, V. [Oak Ridge National Laboratory, P.O. Box 2008, Oak Ridge, TN 37831-6100 (United States); Gardner, K.H. [Department of Materials Science and Engineering University of Delaware, Newark, DE 19719 (United States); Forsyth, V.T. [Institut Laue Langevin, 6 Rue Jules Horowitz, 38042 Grenoble Cedex 9 (France) and Institute of Science and Technology in Medicine, Keele University Medical School, Staffordshire ST4 7QB (United Kingdom)]. E-mail: tforsyth@ill.fr

    2005-08-15

    The fibrous state is a natural one for polymer molecules which tend to assume regular helical conformations rather than the globular structures characteristic of many proteins. Fibre diffraction therefore has broad application to the study of a wide range of biological and synthetic polymers. The purpose of this paper is to illustrate the general scope of the method and in particular to demonstrate the impact of a combined approach involving both X-ray and neutron diffraction methods. While the flux of modern X-ray synchrotron radiation sources allows high quality datasets to be recorded with good resolution within a very short space of time, neutron studies can provide unique information through the ability to locate hydrogen or deuterium atoms that are often difficult or impossible to locate using X-ray methods. Furthermore, neutron fibre diffraction methods can, through the ability to selectively label specific parts of a structure, be used to highlight novel aspects of polymer structure that can not be studied using X-rays. Two examples are given. The first describes X-ray and neutron diffraction studies of conformational transitions in DNA. The second describes structural studies of the synthetic high-performance polymer poly(p-phenylene terephthalamide) (PPTA), known commercially as Kevlar[reg] or Twaron[reg].

  10. Computed tomography of x-ray index of refraction using the diffraction enhanced imaging method

    International Nuclear Information System (INIS)

    Dilmanian, F.A.; Ren, B.; Wu, X.Y.; Orion, I.; Zhong, Z.; Thomlinson, W.C.; Chapman, L.D.

    2000-01-01

    Diffraction enhanced imaging (DEI) is a new, synchrotron-based, x-ray radiography method that uses monochromatic, fan-shaped beams, with an analyser crystal positioned between the subject and the detector. The analyser allows the detection of only those x-rays transmitted by the subject that fall into the acceptance angle (central part of the rocking curve) of the monochromator/analyser system. As shown by Chapman et al , in addition to the x-ray attenuation, the method provides information on the out-of-plane angular deviation of x-rays. New images result in which the image contrast depends on the x-ray index of refraction and on the yield of small-angle scattering, respectively. We implemented DEI in the tomography mode at the National Synchrotron Light Source using 22 keV x-rays, and imaged a cylindrical acrylic phantom that included oil-filled, slanted channels. The resulting 'refraction CT image' shows the pure image of the out-of-plane gradient of the x-ray index of refraction. No image artefacts were present, indicating that the CT projection data were a consistent set. The 'refraction CT image' signal is linear with the gradient of the refractive index, and its value is equal to that expected. The method, at the energy used or higher, has the potential for use in clinical radiography and in industry. (author)

  11. 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

  12. Growth of ω inclusions in Ti alloys: An X-ray diffraction study

    International Nuclear Information System (INIS)

    Šmilauerová, J.; Harcuba, P.; Pospíšil, J.; Matěj, Z.; Holý, V.

    2013-01-01

    We investigated the size and crystal structure of nanometer-sized ω inclusions in single crystals of β-Ti alloys by X-ray diffraction pole-figure measurements and reciprocal space mapping. We studied the topotactical relation of the β and ω crystal lattices, and from the positions and shapes of the diffraction maxima of the ω lattice determined the mean size of the ω inclusions and the misfit of the inclusion lattice with respect to the host lattice, as well as their changes during ageing. The lattice of the ω inclusions exhibits a large positive misfit already before ageing and the misfit is subsequently reduced during the ageing process. Using the theories of elasticity and X-ray scattering we simulated diffuse X-ray scattering around the β diffraction maxima and demonstrated that the diffuse scattering is caused mainly by local elastic strains in the β host phase around the ω inclusions

  13. Determination of the strain hardening rate of metals and alloys by X ray diffraction

    International Nuclear Information System (INIS)

    Cadalbert, Robert

    1977-01-01

    This report for engineering graduation is based on the study of X ray diffraction line profile which varies with the plastic strain rate of the metal. After some generalities of strain hardening (consequence of a plastic deformation on the structure of a polycrystalline metal, means to study a strain hardened structure, use of X ray diffraction to analyse the strain hardened crystalline structure), the author reports the strain hardening rate measurement by using X ray diffraction. Several aspects are addressed: principles, experimental technique, apparatus, automation and programming of the measurement cycle, method sensitivity and precision. In the next part, the author reports applications: measurement of the strain hardening rate in different materials (tubes with hexagonal profile, cylindrical tubes in austenitic steel), and study of the evolution of strain hardening with temperature [fr

  14. Synchrotron X-ray diffraction analysis for quantitative defect evaluation in GaP/Si nanolayers

    Energy Technology Data Exchange (ETDEWEB)

    Nguyen Thanh, T.; Robert, C. [Université Européenne de Bretagne, INSA, FOTON, UMR 6082, F-35708 RENNES (France); Létoublon, A., E-mail: Antoine.letoublon@insa-rennes.fr [Université Européenne de Bretagne, INSA, FOTON, UMR 6082, F-35708 RENNES (France); Cornet, C. [Université Européenne de Bretagne, INSA, FOTON, UMR 6082, F-35708 RENNES (France); Quinci, T. [Université Européenne de Bretagne, INSA, FOTON, UMR 6082, F-35708 RENNES (France); CEA LCP, INES, 50 av. du Lac Léman, Savoie Technolac, 73375 Le Bourget du Lac (France); Giudicelli, E.; Almosni, S. [Université Européenne de Bretagne, INSA, FOTON, UMR 6082, F-35708 RENNES (France); Boudet, N. [CRG-D2AM, ESRF and Inst. Néel, CNRS-UJF, 25 Av des Martyrs, 38042 Grenoble (France); Ponchet, A. [CEMES, CNRS, Université de Toulouse, 29 rue J. Marvig BP 94347, 31055 Toulouse Cedex 4 (France); Kuyyalil, J. [Université Européenne de Bretagne, INSA, FOTON, UMR 6082, F-35708 RENNES (France); Danila, M. [National Institute for Research and Development in Microtechnologies (IMT), 126A Erou Iancu Nicolae Street, 077190, Bucharest (Romania); Durand, O.; Bertru, N.; Le Corre, A. [Université Européenne de Bretagne, INSA, FOTON, UMR 6082, F-35708 RENNES (France)

    2013-08-31

    In the context of III–V monolithic integration on silicon, synchrotron X-ray diffraction has been employed in this study using a bi-dimensional large area hybrid pixel detector (XPAD third generation) to characterize defects in the GaP layers. Despite a very coherent interface (low plastic relaxation) of GaP/Si, 2 types of defect are detected. Micro-twins contributions are evidenced and quantitatively evaluated from additional reflections analysis. Antiphase domains are evidenced using the Williamson-Hall-like plot method applied to transverse scans extracted directly from single XPAD images taken on specular GaP reflections. - Highlights: ► Antiphase domain evidence and characterization in GaP/Si using X-ray diffraction ► Microtwin evidence and characterization ► Synchrotron diffraction ► Large area X-ray hybrid pixel detector.

  15. Submicron x-ray diffraction and its applications to problems in materials and environmental science

    Science.gov (United States)

    Tamura, N.; Celestre, R. S.; MacDowell, A. A.; Padmore, H. A.; Spolenak, R.; Valek, B. C.; Meier Chang, N.; Manceau, A.; Patel, J. R.

    2002-03-01

    The availability of high brilliance third generation synchrotron sources together with progress in achromatic focusing optics allows us to add submicron spatial resolution to the conventional century-old x-ray diffraction technique. The new capabilities include the possibility to map in situ, grain orientations, crystalline phase distribution, and full strain/stress tensors at a very local level, by combining white and monochromatic x-ray microbeam diffraction. This is particularly relevant for high technology industry where the understanding of material properties at a microstructural level becomes increasingly important. After describing the latest advances in the submicron x-ray diffraction techniques at the Advanced Light Source, we will give some examples of its application in material science for the measurement of strain/stress in metallic thin films and interconnects. Its use in the field of environmental science will also be discussed.

  16. Submicron X-Ray Diffraction and its Applications to Problems in Materials and Environmental Science

    Energy Technology Data Exchange (ETDEWEB)

    Patel, J. R.

    2002-08-16

    The availability of high brilliance 3rd generation synchrotron sources together with progress in achromatic focusing optics allow to add submicron spatial resolution to the conventional century-old X-ray diffraction technique. The new capabilities include the possibility to map in-situ, grain orientations, crystalline phase distribution and full strain/stress tensors at a very local level, by combining white and monochromatic X-ray microbeam diffraction. This is particularly relevant for high technology industry where the understanding of material properties at a microstructural level becomes increasingly important. After describing the latest advances in the submicron X-ray diffraction techniques at the ALS, we will give some examples of its application in material science for the measurement of strain/stress in metallic thin films and interconnects. Its use in the field of environmental science will also be discussed.

  17. Submicron X-ray diffraction and its applications to problems in materials and environmental science

    Energy Technology Data Exchange (ETDEWEB)

    Tamura, N.; Celestre, R.S.; MacDowell, A.A.; Padmore, H.A.; Spolenak, R.; Valek, B.C.; Meier Chang, N.; Manceau, A.; Patel, J.R.

    2002-03-26

    The availability of high brilliance 3rd generation synchrotron sources together with progress in achromatic focusing optics allow to add submicron spatial resolution to the conventional century-old X-ray diffraction technique. The new capabilities include the possibility to map in-situ, grain orientations, crystalline phase distribution and full strain/stress tensors at a very local level, by combining white and monochromatic X-ray microbeam diffraction. This is particularly relevant for high technology industry where the understanding of material properties at a microstructural level becomes increasingly important. After describing the latest advances in the submicron X-ray diffraction techniques at the ALS, we will give some examples of its application in material science for the measurement of strain/stress in metallic thin films and interconnects. Its use in the field of environmental science will also be discussed.

  18. Note: Application of a pixel-array area detector to simultaneous single crystal x-ray diffraction and x-ray absorption spectroscopy measurements

    International Nuclear Information System (INIS)

    Sun, Cheng-Jun; Brewe, Dale L.; Heald, Steve M.; Zhang, Bangmin; Chen, Jing-Sheng; Chow, G. M.; Venkatesan, T.

    2014-01-01

    X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS) are two main x-ray techniques in synchrotron radiation facilities. In this Note, we present an experimental setup capable of performing simultaneous XRD and XAS measurements by the application of a pixel-array area detector. For XRD, the momentum transfer in specular diffraction was measured by scanning the X-ray energy with fixed incoming and outgoing x-ray angles. By selecting a small fixed region of the detector to collect the XRD signal, the rest of the area was available for collecting the x-ray fluorescence for XAS measurements. The simultaneous measurement of XRD and X-ray absorption near edge structure for Pr 0.67 Sr 0.33 MnO 3 film was demonstrated as a proof of principle for future time-resolved pump-probe measurements. A static sample makes it easy to maintain an accurate overlap of the X-ray spot and laser pump beam

  19. Direct observation of ultrafast atomic motion using time-resolved X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Shymanovich, U.

    2007-11-13

    This thesis is dedicated to the study of the atomic motion in laser irradiated solids on a picosecond to subpicosecond time-scale using the time-resolved X-ray diffraction technique. In the second chapter, the laser system, the laser-plasma based X-ray source and the experimental setup for optical pump / X-ray probe measurements were presented. Chapter 3 is devoted to the characterization and comparison of different types of X-ray optics. Chapter 4 presented the time-resolved X-ray diffraction experiments performed for this thesis. The first two sections of this chapter discuss the measurements of initially unexpected strain-induced transient changes of the integrated reflectivity of the X-ray probe beam. The elimination of the strain-induced transient changes of the integrated reflectivity represented an important prerequisite to perform the study of lattice heating in Germanium after femtosecond optical excitation by measuring the transient Debye-Waller effect. The third section describes the investigations of acoustic waves upon ultrafast optical excitation and discusses the two different pressure contributions driving them: the thermal and the electronic ones. (orig.)

  20. Direct observation of ultrafast atomic motion using time-resolved X-ray diffraction

    International Nuclear Information System (INIS)

    Shymanovich, U.

    2007-01-01

    This thesis is dedicated to the study of the atomic motion in laser irradiated solids on a picosecond to subpicosecond time-scale using the time-resolved X-ray diffraction technique. In the second chapter, the laser system, the laser-plasma based X-ray source and the experimental setup for optical pump / X-ray probe measurements were presented. Chapter 3 is devoted to the characterization and comparison of different types of X-ray optics. Chapter 4 presented the time-resolved X-ray diffraction experiments performed for this thesis. The first two sections of this chapter discuss the measurements of initially unexpected strain-induced transient changes of the integrated reflectivity of the X-ray probe beam. The elimination of the strain-induced transient changes of the integrated reflectivity represented an important prerequisite to perform the study of lattice heating in Germanium after femtosecond optical excitation by measuring the transient Debye-Waller effect. The third section describes the investigations of acoustic waves upon ultrafast optical excitation and discusses the two different pressure contributions driving them: the thermal and the electronic ones. (orig.)

  1. Control of synchrotron x-ray diffraction by means of standing acoustic waves

    International Nuclear Information System (INIS)

    Zolotoyabko, E.; Quintana, J.P.

    2004-01-01

    Synchrotron x-ray diffraction measurements in quartz crystals of different thickness excited by standing acoustic waves were carried out at the Advanced Photon Source of Argonne National Laboratory. We demonstrated the ability to significantly modify the quartz rocking curves for 20-25 keV x rays by changing the shear wave parameters in the frequency range between 15 and 105 MHz. Dynamic deformation introduced into the crystal lattice by acoustic waves resulted in a remarkable broadening of the rocking curves. The broadening effect strongly depends on the strength of the ultrasound, which can be easily regulated by changing the acoustic amplitude or frequency near the resonance. The maximum rocking curve broadening reached 17 times, which corresponds to the wavelength band, Δλ/λ=4x10 -3 , when used as a monochromator or analyzer for 20-25 keV x rays. The initial rocking curve shape is restored by sweeping the acoustic frequency within a 50-100 kHz range near the resonance. The tunable broadening effect allows effective manipulation of x-ray intensities in time domain. Time-resolved x-ray diffraction measurements under a 19.6 MHz acoustic wave excitation were performed by synchronizing the acoustic wave and x-ray burst periodicity. We used the fact that twice per period the standing wave produces a zero net deformation across the crystal thickness. By introducing an oscillating delay to the acoustic excitation, we were able to effectively change the phase of the acoustic wave relative to the x-ray burst periodicity. The x-ray diffraction intensity was strongly affected by tuning the timing of the x-ray arrivals to the minimum or maximum acoustic deformation. A deep modulation of x rays was observed in a wide frequency range between 0.1 Hz and 1 MHz, which certifies that acoustically excited quartz crystals can potentially be used as slow and fast x-ray modulators with high duty cycle

  2. Asian conference on x-rays and related techniques in research and industry. Proceedings

    International Nuclear Information System (INIS)

    1996-01-01

    This proceedings compile the paper presented at the conference. The papers for presentation are from wide spectrum stressing the interdisciplinary nature of the conference i.e. x-ray fluorescence spectrometry (XRF), x-ray diffraction (XRD), TEM, scanning electron microscope (SEM), energy dispersive x-ray (EDX), auger electron microscopy, electron back scatter diffraction (EBSD)

  3. X-ray diffraction patterns of metal aurocyanides

    International Nuclear Information System (INIS)

    Selig, W.S.; Smith, G.S.; Harding, K.K.; Summers, L.J.

    1989-06-01

    Aurocyanides of the following metal cations have been prepared: Ag, Hg(II), Ga, Fe(III), Tl(I), Bi, Pb, Mn(II), Ni, Zn, Cu(II), Cd, In, and Co(II). Most of the aurocyanides are of the type M[Au(CN) 2 ] x where M is the metal cation and x its valence. However, under some conditions mixed aurocyanides containing K may be formed, such as KCo[Au(CN) 2 ] 3 . Only Ag and Hg(II) form aurocyanides which are sufficiently insoluble for the potentiometric determination of the aurocyanide anion. The diffraction patterns of the various aurocyanides are reported. 12 refs., 16 tabs

  4. X-ray diffraction microscopy based on refractive optics

    DEFF Research Database (Denmark)

    Poulsen, Henning Friis; Jakobsen, A. C.; Simons, Hugh

    2017-01-01

    A formalism is presented for dark‐field X‐ray microscopy using refractive optics. The new technique can produce three‐dimensional maps of lattice orientation and axial strain within millimetre‐sized sampling volumes and is particularly suited to in situ studies of materials at hard X‐ray energies....... An objective lens in the diffracted beam magnifies the image and acts as a very efficient filter in reciprocal space, enabling the imaging of individual domains of interest with a resolution of 100 nm. Analytical expressions for optical parameters such as numerical aperture, vignetting, and the resolution...

  5. X-ray grazing incidence diffraction from multilayers

    Energy Technology Data Exchange (ETDEWEB)

    Tixier, S.; Boeni, P.; Swygenhoven, H. van; Horisberger, M. [Paul Scherrer Inst. (PSI), Villigen (Switzerland)

    1997-09-01

    Grazing incidence scattering geometries using synchrotron radiation have been applied in order to characterise the roughness profiles and the structural coherence of multilayers. The lateral correlation length of the roughness profiles was evaluated using diffuse reflectivity in the `out of plane` geometry. This type of measurement is the only diffuse reflectivity technique allowing large lateral momentum transfer. It is typically suitable for correlation lengths smaller than 1000 A. The lateral structural coherence length of Ni{sub 3}Al/Ni multilayers as a function of the layer thickness was obtained by grazing incidence diffraction (GID). 3 figs., 1 ref.

  6. Controlled molecules for X-ray diffraction experiments at free-electron lasers

    International Nuclear Information System (INIS)

    Stern, Stephan

    2013-12-01

    X-ray diffractive imaging is at the very heart of materials science and has been utilized for decades to solve unknown molecular structures. Nowadays, it serves as the key method of structural biology to solve molecular structures of large biological molecules comprising several thousand or even millions of atoms. However, X-ray diffraction from isolated molecules is very weak. Therefore, the regular and periodic arrangement of a huge number of identical copies of a certain molecule of interest within a crystal lattice has been a necessary condition in order to exploit Bragg diffraction of X-rays. This results in a huge increase in scattered signal and a strongly improved signal-to-noise ratio compared to diffraction from non-crystalline samples. The major bottleneck of structural biology is that many of biologically interesting molecules refuse to form crystals of sufficient size to be used at synchrotron X-ray lightsources. However, novel X-ray free-electron lasers (XFELs), which became operational very recently, promise to address this issue. X-ray pulses provided by XFELs are many orders of magnitude more intense than X-ray pulses from a synchrotron source and at the same time as short as only several tens of femtoseconds. Combined with wavelengths in the nm-pm range, XFELs are well-suited to study ultrafast atomic and molecular dynamics. Additionally, the ultrashort pulses can be utilized to circumvent the damage threshold which set a limit to the incident intensity in X-ray diffraction experiments before. At XFELs, though eventually destroying the investigated sample, no significant sample deterioration happens on the ultrashort timescale of the XFEL pulse and the measured diffraction pattern is due to an (almost) unharmed sample. In the framework of this thesis, the approach of utilizing the highly intense XFEL pulses for X-ray diffraction of weakly-scattering non-crystalline samples was taken to the limit of small isolated molecules. X-ray diffraction was

  7. Controlled molecules for X-ray diffraction experiments at free-electron lasers

    Energy Technology Data Exchange (ETDEWEB)

    Stern, Stephan

    2013-12-15

    X-ray diffractive imaging is at the very heart of materials science and has been utilized for decades to solve unknown molecular structures. Nowadays, it serves as the key method of structural biology to solve molecular structures of large biological molecules comprising several thousand or even millions of atoms. However, X-ray diffraction from isolated molecules is very weak. Therefore, the regular and periodic arrangement of a huge number of identical copies of a certain molecule of interest within a crystal lattice has been a necessary condition in order to exploit Bragg diffraction of X-rays. This results in a huge increase in scattered signal and a strongly improved signal-to-noise ratio compared to diffraction from non-crystalline samples. The major bottleneck of structural biology is that many of biologically interesting molecules refuse to form crystals of sufficient size to be used at synchrotron X-ray lightsources. However, novel X-ray free-electron lasers (XFELs), which became operational very recently, promise to address this issue. X-ray pulses provided by XFELs are many orders of magnitude more intense than X-ray pulses from a synchrotron source and at the same time as short as only several tens of femtoseconds. Combined with wavelengths in the nm-pm range, XFELs are well-suited to study ultrafast atomic and molecular dynamics. Additionally, the ultrashort pulses can be utilized to circumvent the damage threshold which set a limit to the incident intensity in X-ray diffraction experiments before. At XFELs, though eventually destroying the investigated sample, no significant sample deterioration happens on the ultrashort timescale of the XFEL pulse and the measured diffraction pattern is due to an (almost) unharmed sample. In the framework of this thesis, the approach of utilizing the highly intense XFEL pulses for X-ray diffraction of weakly-scattering non-crystalline samples was taken to the limit of small isolated molecules. X-ray diffraction was

  8. Coherent x-ray diffraction imaging of paint pigment particles by scanning a phase plate modulator

    International Nuclear Information System (INIS)

    Chu, Y.S.; Chen, B.; Zhang, F.; Berenguer, F.; Bean, R.; Kewish, C.; Vila-Comamala, J.; Rodenburg, J.; Robinson, I.

    2011-01-01

    We have implemented a coherent x-ray diffraction imaging technique that scans a phase plate to modulate wave-fronts of the x-ray beam transmitted by samples. The method was applied to measure a decorative alkyd paint containing iron oxide red pigment particles. By employing an iterative algorithm for wave-front modulation phase retrieval, we obtained an image of the paint sample that shows the distribution of the pigment particles and is consistent with the result obtained from a transmission x-ray microscope. The technique has been experimentally proven to be a feasible coherent x-ray imaging method with about 120 nm spatial resolution and was shown to work well with industrially relevant specimens.

  9. Correlation between protein sequence similarity and x-ray diffraction quality in the protein data bank.

    Science.gov (United States)

    Lu, Hui-Meng; Yin, Da-Chuan; Ye, Ya-Jing; Luo, Hui-Min; Geng, Li-Qiang; Li, Hai-Sheng; Guo, Wei-Hong; Shang, Peng

    2009-01-01

    As the most widely utilized technique to determine the 3-dimensional structure of protein molecules, X-ray crystallography can provide structure of the highest resolution among the developed techniques. The resolution obtained via X-ray crystallography is known to be influenced by many factors, such as the crystal quality, diffraction techniques, and X-ray sources, etc. In this paper, the authors found that the protein sequence could also be one of the factors. We extracted information of the resolution and the sequence of proteins from the Protein Data Bank (PDB), classified the proteins into different clusters according to the sequence similarity, and statistically analyzed the relationship between the sequence similarity and the best resolution obtained. The results showed that there was a pronounced correlation between the sequence similarity and the obtained resolution. These results indicate that protein structure itself is one variable that may affect resolution when X-ray crystallography is used.

  10. Diffractive-refractive optics: (+,-,-,+) X-ray crystal monochromator with harmonics separation.

    Science.gov (United States)

    Hrdý, Jaromír; Mikulík, Petr; Oberta, Peter

    2011-03-01

    A new kind of two channel-cut crystals X-ray monochromator in dispersive (+,-,-,+) position which spatially separates harmonics is proposed. The diffracting surfaces are oriented so that the diffraction is inclined. Owing to refraction the diffracted beam is sagittally deviated. The deviation depends on wavelength and is much higher for the first harmonics than for higher harmonics. This leads to spatial harmonics separation. The idea is supported by ray-tracing simulation.

  11. Long wave-length x-ray diffraction crystal and method of manufacturing same

    International Nuclear Information System (INIS)

    Zingaro, W.P.; Sicignano, A.

    1980-01-01

    An x-ray diffraction crystal of the Langemuir-Blodgett type capable of detecting radiation having a wavelength greater than 50 Arystroms and a method of making such a crystal are described. The crystal consists of a pair of alternate monolayers, one a heavy metal soap, and one a light metal soap. Selecting cation pairs with a significant difference in atomic number and dispersing power, such as Pb and Be, Mg, or Ca, increases the effective interplanar distance since the Pb planes cause the predominant x-ray diffraction. (LL)

  12. An introduction to three-dimensional X-ray diffraction microscopy

    DEFF Research Database (Denmark)

    Poulsen, Henning Friis

    2012-01-01

    Three-dimensional X-ray diffraction microscopy is a fast and nondestructive structural characterization technique aimed at studies of the individual crystalline elements (grains or subgrains) within millimetre-sized polycrystalline specimens. It is based on two principles: the use of highly...... penetrating hard X-rays from a synchrotron source and the application of tomographic reconstruction algorithms for the analysis of the diffraction data. In favourable cases, the position, morphology, phase and crystallographic orientation can be derived for up to 1000 elements simultaneously. For each grain...

  13. X-ray diffraction investigation of spin reorientation in SmFe2

    International Nuclear Information System (INIS)

    Gaviko, V.S.; Korolyov, A.V.; Mushnikov, N.V.

    1996-01-01

    Spontaneous magnetoelastic crystal lattice distortions in the spin reorientation region of high magnetostrictive SmFe 2 have been investigated by X-ray diffraction in the temperature range 80-300 K. Comparison of experimental shapes of X-ray diffraction lines with calculated shapes shows that, in the region of the spin reorientation transition, a mixture of left angle 110 right angle and left angle 111 right angle phases rather than the angular left angle uuw right angle -type phase is realized. The temperature dependence of the relative volume content of left angle 110 right angle and left angle 111 right angle phases is determined using least-squares fitting. (orig.)

  14. X-ray diffraction studies of chitosan acetate-based polymer electrolytes

    International Nuclear Information System (INIS)

    Osman, Z.; Ibrahim, Z.A.; Abdul Kariem Arof

    2002-01-01

    Chitosan is the product when partially deacetylated chitin dissolves in dilute acetic acid. This paper presents the x-ray diffraction patterns of chitosan acetate, plasticised chitosan acetate and plasticised-salted chitosan acetate films. The results show that the chitosan acetate based polymer electrolyte films are not completely amorphous but it is partially crystalline. X-ray diffraction study also confirms the occurrence of the complexation between chitosan and the salt and the interaction between salt and plasticizer. The salt-chitosan interaction is clearly justified by infrared spectroscopy. (Author)

  15. Determination of densities from chemical composition and X-Ray diffraction

    International Nuclear Information System (INIS)

    Azevedo, A.L.T. de

    1980-01-01

    X-ray diffraction method applied to retained austenite measurements gives volume per cent results, whereas the same kind of measurement made by Moessbauer Effect gives iron percentages. To compare both results one needs to convert the volume % to weight % or vice-versa. This necessitates, among other things, in determining the densities of the α and #betta# phases in the steel being studied. A method for calculating the densities, based on the application of the definition of density to just one unit cell, using X-ray diffraction and chemical results, are described. (Author) [pt

  16. Introducing the ARL X'Tra x-ray diffraction system

    International Nuclear Information System (INIS)

    Harris, L.

    2002-01-01

    Full text: The ARL X'Tra is a state-of-the-art solution for powder X-ray diffraction in a large range of applications such as pharmaceuticals and biosciences, chemicals, earth sciences, semi-conductors, metallurgy and ceramics. The X'Tra offers the latest technology in key diffraction components to produce a high performance instrument at an affordable price. This presentation examines some of the hardware and performance features of this instrument. Copyright (2002) Australian X-ray Analytical Association Inc

  17. Magnetic x-ray circular dichroism in spin-polarized photoelectron diffraction

    International Nuclear Information System (INIS)

    Waddill, G.D.; Tobin, J.G.

    1994-01-01

    The first structural determination with spin-polarized, energy-dependent photoelectron diffraction using circularly-polarized x-rays is reported for Fe films on Cu(001). Circularly-polarized x-rays produced spin-polarized photoelectrons from the Fe 2p doublet, and intensity asymmetries in the 2p 3/2 level are observed. Fully spin-specific multiple scattering calculations reproduced the experimentally-determined energy and angular dependences. A new analytical procedure which focuses upon intensity variations due to spin-dependent diffraction is introduced. A sensitivity to local geometric and magnetic structure is demonstrated

  18. Rapid determination of trace phosphorus, sulfur, chlorine, bromine and iodine by energy dispersive X-ray fluorescence analysis with monochromatic excitations

    International Nuclear Information System (INIS)

    Wakisaka, Tatsushi; Morita, Naoki; Hirabayashi, Tadashi; Nakahara, Taketoshi

    1998-01-01

    A useful and rapid procedure is described for the determination of trace phosphorus, sulfur, chlorine, bromine, and iodine by means of an energy dispersive X-ray fluorescence spectrometer (EDXRF) with monochromatic excitations. Using monochromatic excitations, the detection limits for phosphorus, sulfur, chlorine (Cr-Kα, 5.41 keV), bromine (Mo-Kα, 17.44 keV), and iodine (W-continuum, 40 keV) were found to be 4.6, 1.7, 0.7, 0.09 and 0.5 μg g -1 , respectively. The relative standard deviations in five replicate measurements were 0.9-1.3%. The proposed method was applied to the direct determination of sulfur in the NIST Residual Fuel Oil, and others. The results obtained by the proposed method were in good agreement with the certified values. Bromine in a seawater sample, as well as iodine and bromine in a brine sample were determined by the proposed method. The obtained results were in good agreement with those obtained by ion chromatography. (author)

  19. Characterization of the ashes from the 2014-2015 Turrialba Volcano eruptions by means of scanning electron microscopy and energy dispersive X-Ray spectroscopy

    International Nuclear Information System (INIS)

    Lucke, Oscar H.; Calderon, Ariadna

    2016-01-01

    The Turrialba Volcano is a stratovolcano located approximately 35 km northwest from San Jose, Costa Rica's capital city. A series of eruptions since October 29, 2014 until at least late 2015, has represented the most significant activity of this volcano since the 1860s. A significant volume of ash was dispersed with this eruptions that reached the most populous areas of the country. The characteristics of the ash particles are analyzed in order to establish the nature of the eruptive events that occurred on 2014 and 2015, and to monitor the evolution of the eruptive processes. The analysis was carried out utilizing optical microscopy and stereomicroscopy techniques, as well as novel scanning electron microscopy (SEM) methods that involve imaging and element composition analysis by means of Energy Dispersive X-Ray Spectroscopy (EDX). The evolution of the Turrialba eruptions is showed from phreatic events in 2014, with ashes composed entirely of non-juvenile fragments, to phreatomagmatic events starting on March 12, 2015 with the appearance of a significant fraction of juvenile components in the ash. (author)

  20. Morphological and chemical changes in dentin after using endodontic agents: Fourier transform Raman spectroscopy, energy-dispersive x-ray fluorescence spectrometry, and scanning electron microscopy study

    Science.gov (United States)

    Pascon, Fernanda Miori; Kantovitz, Kamila Rosamilia; Soares, Luís Eduardo Silva; Santo, Ana Maria do Espírito; Martin, Airton Abraha~o.; Puppin-Rontani, Regina Maria

    2012-07-01

    We examine the morphological and chemical changes in the pulp chamber dentin after using endodontic agents by scanning electron microscopy (SEM), Fourier transform Raman spectroscopy (FT-Raman), and micro energy-dispersive x-ray fluorescence spectrometry (μEDXRF). Thirty teeth were sectioned exposing the pulp chamber and divided by six groups (n=5): NT-no treatment; CHX-2% chlorhexidine; CHXE-2% chlorhexidine+17% EDTA E-17% EDTA; SH5-5.25% NaOCl; SH5E-5.25% NaOCl+17% EDTA. The inorganic and organic content was analyzed by FT-Raman. μEDXRF examined calcium (Ca) and phosphorus (P) content as well as Ca/P ratio. Impressions of specimens were evaluated by SEM. Data were submitted to Kruskal-Wallis and Dunn tests (pNT=SH5E>CHX>E>CHXE). CHXE and E presented the highest Ca/P ratio values compared to the other groups (p<0.05). The SEM images in the EDTA-treated groups had the highest number of open tubules. Erosion in the tubules was observed in CHX and SH5E groups. Endodontic agents change the inorganic and organic content of pulp chamber dentin. NaOCl used alone, or in association with EDTA, was the most effective agent considering chemical and morphological approaches.