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Sample records for in-situ energy-dispersive x-ray

  1. Soil characterization by energy dispersive X-ray fluorescence: sampling strategy for in situ analysis.

    PubMed

    Custo, Graciela; Boeykens, Susana; Dawidowski, L; Fox, L; Gómez, D; Luna, F; Vázquez, Cristina

    2005-07-01

    This work describes a sampling strategy that will allow the use of portable EDXRF (energy dispersive X-ray fluorescence) instruments for "in situ" soil analysis. The methodology covers a general approach to planning field investigations for any type of environmental studies and it was applied for a soil characterization study in the zone of Campana, Argentina, by evaluating data coming from an EDXRF spectrometer with a radioisotope excitation source. Simulating non-treated sampled as "in situ" samples and a soil characterization for Campana area was intended. "In situ" EDXRF methodology is a powerful analytical modality with the advantage of providing data immediately, allowing a fast general screening of the soil composition. PMID:16038489

  2. In situ energy dispersive x-ray reflectometry measurements on organic solar cells upon working

    NASA Astrophysics Data System (ADS)

    Paci, B.; Generosi, A.; Albertini, V. Rossi; Perfetti, P.; de Bettignies, R.; Firon, M.; Leroy, J.; Sentein, C.

    2005-11-01

    The change in the morphology of plastic solar cells was studied by means of time-resolved energy dispersive x-ray reflectivity (XRR). This unconventional application of the XRR technique allowed the follow up of in situ morphological evolution of an organic photovoltaic device upon working. The study consisted of three steps: A preliminary set of XRR measurements on various samples representing the intermediate stages of cell construction, which provided accurate data regarding the electronic densities of the different layers; the verification of the morphological stability of the device under ambient condition; a real-time collection of XRR patterns, both in the dark and during 15h in artificial light conditions which allowed the changes in the system morphology at the electrode-active layer interface to be monitored. In this way, a progressive thickening of this interface, responsible for a reduction in the performances of the device, was observed directly.

  3. In situ energy-dispersive x-ray diffraction system for time-resolved thin-film growth studies

    NASA Astrophysics Data System (ADS)

    Ellmer, K.; Mientus, R.; Weiß, V.; Rossner, H.

    2003-03-01

    Energy-dispersive x-ray diffraction (EDXRD) with synchrotron light can be used for in situ-structural analysis during polycrystalline thin-film growth, due to its fast data collection and the fixed diffraction angle. An in situ deposition and analysis set-up for the investigation of nucleation and growth of thin films during magnetron sputtering was constructed and installed at the synchrotron radiation source Hamburger Synchrotronstrahlungs Labor (Hamburg). The polychromatic synchrotron beam passes the sputtering chamber through Kapton windows and hits the substrate with the growing film. The diffracted beam, observed under a fixed diffraction angle of between 1° and 10° was energy-analysed by a high-purity germanium detector. The measurement time for a single XRD spectrum can be as short as 10 s for a beam line at a bending magnet, which allows a time-resolved monitoring of film growth. The performance of the in situ EDXRD set-up is demonstrated for the growth of zinc oxide and tin-doped indium oxide films prepared by reactive magnetron sputtering from ceramic and metallic targets. From the position and the width of the diffraction lines the internal mechanical strain and the grain size of the growing films can be derived. The prospects for thin-film growth investigations using such an instrument are assessed.

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

    NASA Astrophysics Data System (ADS)

    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.

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

    NASA Astrophysics Data System (ADS)

    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

  6. In situ measurement of the deuterium (hydrogen) charging of a palladium electrode during electrolysis by energy dispersive x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Felici, R.; Bertalot, L.; DeNinno, A.; LaBarbera, A.; Violante, V.

    1995-05-01

    A method to determine the concentration of deuterium inside a palladium cathode during the electrolysis of LiOD-heavy water solution is described. This method is based on the measurement of the host metal lattice parameter which is linearly related to the concentration in a wide range. A hard-x-ray beam which is able to cross two glass walls and few centimeters of water solutions without suffering a strong attenuation has been used. The measurement of the lattice parameter is performed in situ, during the electrolysis, by using energy dispersive x-ray diffraction. The sample volume illuminated by the x-ray beam is limited to a small region close to the surface and depends on the incident photon energy. In principle, this allows one to study the dynamics of the charging process and to determine the concentration profile in the range from few up to tens of micrometers. The deuterium concentration, determined by this method, was then checked by degassing the cathode in a known volume and was always found in a very good agreement, showing that the charging was uniform for the whole sample.

  7. Spatially resolved energy dispersive x-ray spectroscopic method for in-situ evaluation of mechanical properties during the growth of a C - Pt composite nanowire

    SciTech Connect

    Banerjee, Amit; Banerjee, S. S.

    2014-05-15

    A core-shell type C-Pt composite nanowire is fabricated using focused ion and electron beam induced chemical vapor deposition techniques. Using information from spatially resolved energy dispersive x-ray spectra, we detect the resonance vibration in the C-Pt composite nanowire. We use this method to measure the Young's moduli of the constituents (C, Pt) of the composite nanowire and also estimate the density of the FEB CVD grown Pt shell surrounding the C core. By measuring the resonance characteristics of the composite nanowire we estimate a Pt shell growth rate of ∼0.9 nms{sup −1}. The study is analyzed to suggest that the Pt shell growth mechanism is primarily governed by the sticking coefficient of the organometallic vapor on the C nanowire core.

  8. Spatially resolved energy dispersive x-ray spectroscopic method for in-situ evaluation of mechanical properties during the growth of a C - Pt composite nanowire

    NASA Astrophysics Data System (ADS)

    Banerjee, Amit; Banerjee, S. S.

    2014-05-01

    A core-shell type C-Pt composite nanowire is fabricated using focused ion and electron beam induced chemical vapor deposition techniques. Using information from spatially resolved energy dispersive x-ray spectra, we detect the resonance vibration in the C-Pt composite nanowire. We use this method to measure the Young's moduli of the constituents (C, Pt) of the composite nanowire and also estimate the density of the FEB CVD grown Pt shell surrounding the C core. By measuring the resonance characteristics of the composite nanowire we estimate a Pt shell growth rate of ˜0.9 nms-1. The study is analyzed to suggest that the Pt shell growth mechanism is primarily governed by the sticking coefficient of the organometallic vapor on the C nanowire core.

  9. In situ strain profiling of elastoplastic bending in Ti-6Al-4V alloy by synchrotron energy dispersive x-ray diffraction

    SciTech Connect

    Croft, M.; Shukla, V.; Akdogan, E. K.; Sadangi, R.; Ignatov, A.; Balarinni, L.; Tsakalakos, T.; Jisrawi, N.; Zhong, Z.; Horvath, K.

    2009-05-01

    Elastic and plastic strain evolution under four-point bending has been studied by synchrotron energy dispersive x-ray diffraction. Measured strain profiles across the specimen thickness showed an increasing linear elastic strain gradient under increasing four-point bending load up to approx2 kN. The bulk elastic modulus of Ti-6Al-4V was determined as 118 GPa. The onset of plastic deformation was found to set in at a total in-plane strain of approx0.008, both under tension and compression. Plastic deformation under bending is initiated in the vicinity of the surface and at a stress of 1100 MPa, and propagates inward, while a finite core region remains elastically deformed up to 3.67 kN loading. The onset of the plastic regime and the plastic regime itself has been verified by monitoring the line broadening of the (100) peak of alpha-Ti. The effective compression/tension stress-strain curve has been obtained from the scaling collapse of strain profile data taken at seven external load levels. A similar multiple load scaling collapse of the plastic strain variation has also been obtained. The level of precision in strain measurement reported herein was evaluated and found to be 1.5x10{sup -5} or better.

  10. Portable energy dispersive X-ray fluorescence and X-ray diffraction and radiography system for archaeometry

    NASA Astrophysics Data System (ADS)

    Mendoza Cuevas, Ariadna; Perez Gravie, Homero

    2011-03-01

    Starting on a laboratory developed portable X-ray fluorescence (PXRF) spectrometer; three different analytical results can be performed: analysis of chemical elements, analysis of major chemical crystalline phase and structural analysis, which represents a contribution to a new, low cost development of portable X-ray analyzer; since these results are respectively obtained with independent equipments for X-ray fluorescence, X-ray diffraction and radiography. Detection limits of PXRF were characterized using standard reference materials for ceramics, glass, bronze and bones, which are the main materials requiring quantitative analysis in art and archeological objects. A setup for simultaneous energy dispersive X-ray fluorescence and diffraction (ED (XRF-XRD)) in the reflection mode has been tested for in situ and non-destructive analysis according to the requirements of art objects inspection. The system uses a single low power X-ray tube and an X-ray energy dispersive detector to measure X-ray diffraction spectrum at a fixed angle. Application to the identification of jadeite-jade mineral in archeological objects by XRD is presented. A local high resolution radiography image obtained with the same low power X-ray tube allows for studies in painting and archeological bones.

  11. Single atom identification by energy dispersive x-ray spectroscopy

    SciTech Connect

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

    2012-04-09

    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.

  12. Electrochemical Reduction of Ag2VP2O8 Composite Electrodes Visualized via In situ Energy Dispersive X-ray Diffraction (EDXRD). Unexpected Conductive Additive Effects

    SciTech Connect

    Kirshenbaum, Kevin C.; Bock, David C.; Zhong, Zhong; Marschilok, Amy C.; Takeuchi, Kenneth J.; Takeuchi, Esther

    2015-07-29

    In our study, we characterize the deposition of silver metal nanoparticles formed during discharge of Li/Ag2VP2O8 cells with composite cathodes containing conductive carbon additive. Using in situ energy dispersive X-ray diffraction (EDXRD) of an intact battery, the location and distribution of silver metal nanoparticles generated upon reduction-displacement deposition within an Ag2VP2O8 cathode containing a pre-existing percolation network can be observed for the first time. Our study yielded unexpected results where higher rate initial discharge generated a more effective conductive matrix. This stands in contrast to cells with cathodes with no conductive additive where a low rate initial discharge proved more effective. Our results provide evidence that using conductive additives in conjunction with an in situ reduction-displacement deposition of silver metal provides a path toward the ultimate goal of complete electrical contact and full utilization of all electroactive particles.

  13. Anomalous lattice expansion in yttria stabilized zirconia under simultaneous applied electric and thermal fields: A time-resolved in situ energy dispersive x-ray diffractometry study with an ultrahigh energy synchrotron probe

    SciTech Connect

    Akdogan, E. K.; Savkl Latin-Small-Letter-Dotless-I y Latin-Small-Letter-Dotless-I ld Latin-Small-Letter-Dotless-I z, I.; Bicer, H.; Paxton, W.; Toksoy, F.; Tsakalakos, T.; Zhong, Z.

    2013-06-21

    Nonisothermal densification in 8% yttria doped zirconia (8YSZ) particulate matter of 250 nm median particle size was studied under 215 V/cm dc electric field and 9 Degree-Sign C/min heating rate, using time-resolved in-situ high temperature energy dispersive x-ray diffractometry with a polychromatic 200 keV synchrotron probe. Densification occurred in the 876-905 Degree-Sign C range, which resulted in 97% of the theoretical density. No local melting at particle-particle contacts was observed in scanning electron micrographs, implying densification was due to solid state mass transport processes. The maximum current draw at 905 Degree-Sign C was 3 A, corresponding to instantaneous absorbed power density of 570 W/cm{sup 3}. Densification of 8YSZ was accompanied by anomalous elastic volume expansions of the unit cell by 0.45% and 2.80% at 847 Degree-Sign C and 905 Degree-Sign C, respectively. The anomalous expansion at 905 Degree-Sign C at which maximum densification was observed is characterized by three stages: (I) linear stage, (II) anomalous stage, and (III) anelastic recovery stage. The densification in stage I (184 s) and II (15 s) was completed in 199 s, while anelastic relaxation in stage III lasted 130 s. The residual strains ({epsilon}) at room temperature, as computed from tetragonal (112) and (211) reflections, are {epsilon}{sub (112)} = 0.05% and {epsilon}{sub (211)} = 0.13%, respectively. Time dependence of (211) and (112) peak widths ({beta}) show a decrease with both exhibiting a singularity at 905 Degree-Sign C. An anisotropy in (112) and (211) peak widths of {l_brace} {beta}{sub (112)}/{beta}{sub (211)}{r_brace} = (3:1) magnitude was observed. No phase transformation occurred at 905 Degree-Sign C as verified from diffraction spectra on both sides of the singularity, i.e., the unit cell symmetry remains tetragonal. We attribute the reduction in densification temperature and time to ultrafast ambipolar diffusion of species arising from the

  14. Measuring Performance of Energy-Dispersive X-ray Systems.

    PubMed

    Statham

    1998-11-01

    : As Si(Li) detector technology has matured, many of the fundamental problems have been addressed in the competition among manufacturers and there is now an expectation, implied by many textbooks, that all energy-dispersive X-ray (EDX) detectors are made and will perform in the same way. Although there has been some convergence in Si(Li) systems and these are still the most common, manufacturing recipes still differ and there are many alternative EDX devices, such as microcalorimeters and room temperature detectors, that have both advantages and disadvantages over Si(Li). Rather than emphasizing differences in technologies, performance measures should reveal benefits relevant to the intended application. The instrument is inevitably going to be a "black box" of integrated components; this article reviews some of the methods that have been applied and introduces some new techniques that can be used to assess performance without resorting to complex software or sophisticated mathematical algorithms. Sensitivity, resolution, artefacts, and stability are discussed with particular application to compositional analysis using electron beam excitation of X-rays in the 100-eV to 10-keV energy region. PMID:10087283

  15. Energy Dispersive X-Ray and Electrochemical Impedance Spectroscopies for Performance and Corrosion Analysis of PEMWEs

    NASA Astrophysics Data System (ADS)

    Steen, S. M., Iii; Zhang, F.-Y.

    2014-11-01

    Proton exchange membrane water electrolyzers (PEMWEs) are a promising energy storage technology due to their high efficiency, compact design, and ability to be used in a renewable energy system. Before they are able to make a large commercial impact, there are several hurdles facing the technology today. Two powerful techniques for both in-situ and ex- situ characterizations to improve upon their performance and better understand their corrosion are electrochemical impedance spectroscopy and energy dispersive x-ray spectroscopy, respectively. In this paper, the authors use both methods in order to characterize the anode gas diffusion layer (GDL) in a PEMWE cell and better understand the corrosion that occurs in the oxygen electrode during electrolysis.

  16. Focal construct geometry for high intensity energy dispersive x-ray diffraction based on x-ray capillary optics.

    PubMed

    Li, Fangzuo; Liu, Zhiguo; Sun, Tianxi; Jiang, Bowen; Zhu, Yu

    2016-03-14

    We presented a focal construct geometry (FCG) method for high intensity energy dispersive X-ray diffraction by utilizing a home-made ellipsoidal single-bounce capillary (ESBC) and a polycapillary parallel X-ray lens (PPXRL). The ESBC was employed to focus the X-rays from a conventional laboratory source into a small focal spot and to produce an annular X-ray beam in the far-field. Additionally, diffracted polychromatic X-rays were confocally collected by the PPXRL attached to a stationary energy-resolved detector. Our FCG method based on ESBC and PPXRL had achieved relatively high intensity diffraction peaks and effectively narrowed the diffraction peak width which was helpful in improving the potential d-spacing resolution for material phase analysis. PMID:26979685

  17. Focal construct geometry for high intensity energy dispersive x-ray diffraction based on x-ray capillary optics

    NASA Astrophysics Data System (ADS)

    Li, Fangzuo; Liu, Zhiguo; Sun, Tianxi; Jiang, Bowen; Zhu, Yu

    2016-03-01

    We presented a focal construct geometry (FCG) method for high intensity energy dispersive X-ray diffraction by utilizing a home-made ellipsoidal single-bounce capillary (ESBC) and a polycapillary parallel X-ray lens (PPXRL). The ESBC was employed to focus the X-rays from a conventional laboratory source into a small focal spot and to produce an annular X-ray beam in the far-field. Additionally, diffracted polychromatic X-rays were confocally collected by the PPXRL attached to a stationary energy-resolved detector. Our FCG method based on ESBC and PPXRL had achieved relatively high intensity diffraction peaks and effectively narrowed the diffraction peak width which was helpful in improving the potential d-spacing resolution for material phase analysis.

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

    NASA Astrophysics Data System (ADS)

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

    2010-04-01

    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.

  19. Single photon energy dispersive x-ray diffraction

    SciTech Connect

    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

    2014-03-15

    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.

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

    NASA Technical Reports Server (NTRS)

    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.

  1. Analysis of tincal ore waste by energy dispersive X-ray fluorescence (EDXRF) Technique

    NASA Astrophysics Data System (ADS)

    Kalfa, Orhan Murat; Üstündağ, Zafer; Özkırım, Ilknur; Kagan Kadıoğlu, Yusuf

    2007-01-01

    Etibank Borax Plant is located in Kırka-Eskişehir, Turkey. The borax waste from this plant was analyzed by means of energy dispersive X-ray fluorescence (EDXRF). The standard addition method was used for the determination of the concentration of Al, Fe, Zn, Sn, and Ba. The results are presented and discussed in this paper.

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

    ERIC Educational Resources Information Center

    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.…

  3. Energy Dispersive X-ray Tomography for 3D Elemental Mapping of Individual Nanoparticles.

    PubMed

    Slater, Thomas J A; Lewis, Edward A; Haigh, Sarah J

    2016-01-01

    Energy dispersive X-ray spectroscopy within the scanning transmission electron microscope (STEM) provides accurate elemental analysis with high spatial resolution, and is even capable of providing atomically resolved elemental maps. In this technique, a highly focused electron beam is incident upon a thin sample and the energy of emitted X-rays is measured in order to determine the atomic species of material within the beam path. This elementally sensitive spectroscopy technique can be extended to three dimensional tomographic imaging by acquiring multiple spectrum images with the sample tilted along an axis perpendicular to the electron beam direction. Elemental distributions within single nanoparticles are often important for determining their optical, catalytic and magnetic properties. Techniques such as X-ray tomography and slice and view energy dispersive X-ray mapping in the scanning electron microscope provide elementally sensitive three dimensional imaging but are typically limited to spatial resolutions of > 20 nm. Atom probe tomography provides near atomic resolution but preparing nanoparticle samples for atom probe analysis is often challenging. Thus, elementally sensitive techniques applied within the scanning transmission electron microscope are uniquely placed to study elemental distributions within nanoparticles of dimensions 10-100 nm. Here, energy dispersive X-ray (EDX) spectroscopy within the STEM is applied to investigate the distribution of elements in single AgAu nanoparticles. The surface segregation of both Ag and Au, at different nanoparticle compositions, has been observed. PMID:27403838

  4. X-ray photo-emission and energy dispersive spectroscopy of HA coated titanium

    SciTech Connect

    Drummond, J.L.; Steinberg, A.D.; Krauss, A.R.

    1997-08-01

    The purpose of this study was to determine the chemical composition changes of hydroxyapatite (HA) coated titanium using surface analysis (x-ray photo-emission) and bulk analysis (energy dispersive spectroscopy). The specimens examined were controls, 30 minutes and 3 hours aged specimens in distilled water or 0.2M sodium phosphate buffer (pH 7.2) at room temperature. Each x-ray photo-emission cycle consisted of 3 scans followed by argon sputtering for 10 minutes for a total of usually 20 cycles, corresponding to a sampling depth of {approximately} 1500 {angstrom}. The energy dispersive spectroscopy analysis was on a 110 by 90 {mu}m area for 500 sec. Scanning electron microscopy examination showed crystal formation (3P{sub 2}O{sub 5}*2CAO*?H{sub 2}O by energy dispersive spectroscopy analysis) on the HA coating for the specimens aged in sodium phosphate buffer. The x-ray photo-emission results indicated the oxidation effect of water on the titanium (as TiO{sub 2}) and the effect of the buffer to increase the surface concentration of phosphorous. No differences in the chemical composition were observed by energy dispersive spectroscopy analysis. The crystal growth was only observed for the sodium phosphate buffer specimens and only on the HA surface.

  5. The 20 element HgI2 energy dispersive x ray array detector system

    NASA Astrophysics Data System (ADS)

    Iwanczyk, J. A.; Dorri, N.; Wang, M.; Szczebiot, R. W.; Dabrowski, A. J.; Hedman, B.; Hodgson, K. O.; Patt, B. E.

    1991-11-01

    This paper describes recent progress in the development of HgI2 energy dispersive x-ray detector arrays and associated miniaturized processing electronics for synchrotron radiation research applications. The experimental results with a 20 element array detector were obtained under realistic synchrotron beam conditions at SSRL. An energy resolution of 250 eV (FWHM) at 5.9 keV (Mn-K(sub a)) was achieved. Energy resolution and throughput measurements versus input count rate and energy of incoming radiation have been measured. Extended X-ray Absorption Fine Structure (EXAFS) spectra were taken from diluted samples simulating proteins with nickel.

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

    NASA Technical Reports Server (NTRS)

    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.

  7. Superconducting Detector System for High-Resolution Energy-Dispersive Soft X-Ray Spectroscopy

    SciTech Connect

    Friedrich, S; Niedermayr, T; Drury, O; Funk, T; Frank, M; Labov, S E; Cramer, S

    2001-02-21

    Synchrotron-based soft x-ray spectroscopy is often limited by detector performance. Grating spectrometers have the resolution, but lack the efficiency for the analysis of dilute samples. Semiconducting Si(Li) or Ge detectors are efficient, but often lack the resolution to separate weak signals from strong nearby lines in multi-element samples. Superconducting tunnel junctions (STJs) operated at temperatures below 1 K can be used as high-resolution high-efficiency x-ray detectors. They combine high energy resolution around 10 eV FWHM with the broad band efficiency of energy-dispersive detectors. We have designed a two-stage adiabatic demagnetization refrigerator (ADR) to operate STJ detectors in x-ray fluorescence measurements at beam line 4 of the ALS. We demonstrate the capabilities of such a detector system for fluorescence analysis of dilute metal sites in proteins and inorganic model compounds.

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

    NASA Astrophysics Data System (ADS)

    Ghammraoui, B.; Tabary, J.; Pouget, S.; Paulus, C.; Moulin, V.; Verger, L.; Duvauchelle, Ph.

    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.

  9. Determination of carrier yields for neutron activation analysis using energy dispersive X-ray spectrometry

    USGS Publications Warehouse

    Johnson, R.G.; Wandless, G.A.

    1984-01-01

    A new method is described for determining carrier yield in the radiochemical neutron activation analysis of rare-earth elements in silicate rocks by group separation. The method involves the determination of the rare-earth elements present in the carrier by means of energy-dispersive X-ray fluorescence analysis, eliminating the need to re-irradiate samples in a nuclear reactor after the gamma ray analysis is complete. Results from the analysis of USGS standards AGV-1 and BCR-1 compare favorably with those obtained using the conventional method. ?? 1984 Akade??miai Kiado??.

  10. Distinction between entrance and exit wounds by energy dispersive X-ray fluorescence spectrometry.

    PubMed

    Tanaka, Naoko; Kinoshita, Hiroshi; Takakura, Ayaka; Jamal, Mostofa; Ito, Asuka; Kumihashi, Mitsuru; Tsutsui, Kunihiko; Kimura, Shoji; Ameno, Kiyoshi

    2016-09-01

    We investigated gunshot wounds in two autopsy cases using energy dispersive X-ray spectrometry (EDX). Lead and copper were detected in the entrance wound of one case and lead, antimony, and copper were detected in that of the other case. In the exit wounds of both cases, lead, antimony, and copper were below detection limits. These findings indicate that the detection of metallic elements, such as lead, antimony, and copper, which are found in bullets, may be useful for differentiating entrance from exit wounds using EDX. PMID:27591531

  11. In-situ mechanical testing during X-ray diffraction

    SciTech Connect

    Van Swygenhoven, Helena Van Petegem, Steven

    2013-04-15

    Deforming metals during recording X-ray diffraction patterns is a useful tool to get a deeper understanding of the coupling between microstructure and mechanical behaviour. With the advances in flux, detector speed and focussing techniques at synchrotron facilities, in-situ mechanical testing is now possible during powder diffraction and Laue diffraction. The basic principle is explained together with illustrative examples.

  12. The SLcam: a full-field energy dispersive X-ray camera

    NASA Astrophysics Data System (ADS)

    Bjeoumikhov, A.; Buzanich, G.; Langhoff, N.; Ordavo, I.; Radtke, M.; Reinholz, U.; Riesemeier, H.; Scharf, O.; Soltau, H.; Wedell, R.

    2012-11-01

    The color X-ray camera (SLcam®) is a full-field single photon imager. As stand-alone camera, it is applicable for energy and space-resolved X-ray detection measurements. The exchangeable poly-capillary optics in front of a beryllium entrance window conducts X-ray photons from the probe to distinguished energy dispersive pixels on a pnCCD. The dedicated software enables the acquisition and the online processing of the spectral data for all 69696 pixels, leading to a real-time visualization of the element distribution in a sample. No scanning system is employed. A first elemental composition image of the sample is visible within minutes while statistics is improving in the course of time. Straight poly-capillary optics allows for 1:1 imaging with a space resolution of 50 μm and no limited depth of sharpness, ideal to map uneven objects. Using conically shaped optics, a magnification of 6 times was achieved with a space resolution of 10 μm. We present a measurement with a laboratory source showing the camera capability to perform fast full-field X-ray Fluorescence (FF-XRF) imaging with an easy, portable and modular setup.

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

    SciTech Connect

    Daley, T.D.; Gibson, D. )

    1990-03-01

    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.

  14. X-ray coherent scattering form factors of tissues, water and plastics using energy dispersion

    NASA Astrophysics Data System (ADS)

    King, B. W.; Landheer, K. A.; Johns, P. C.

    2011-07-01

    A key requirement for the development of the field of medical x-ray scatter imaging is accurate characterization of the differential scattering cross sections of tissues and phantom materials. The coherent x-ray scattering form factors of five tissues (fat, muscle, liver, kidney, and bone) obtained from butcher shops, four plastics (polyethylene, polystyrene, lexan (polycarbonate), nylon), and water have been measured using an energy-dispersive technique. The energy-dispersive technique has several improvements over traditional diffractometer measurements. Most notably, the form factor is measured on an absolute scale with no need for scaling factors. Form factors are reported in terms of the quantity x = λ-1sin (θ/2) over the range 0.363-9.25 nm-1. The coherent form factors of muscle, liver, and kidney resemble those of water, while fat has a narrower peak at lower x, and bone is more structured. The linear attenuation coefficients of the ten materials have also been measured over the range 30-110 keV and parameterized using the dual-material approach with the basis functions being the linear attenuation coefficients of polymethylmethacrylate and aluminum.

  15. Determination of selenium in biological samples with an energy-dispersive X-ray fluorescence spectrometer.

    PubMed

    Li, Xiaoli; Yu, Zhaoshui

    2016-05-01

    Selenium is both a nutrient and a toxin. Selenium-especially organic selenium-is a core component of human nutrition. Thus, it is very important to measure selenium in biological samples. The limited sensitivity of conventional XRF hampers its widespread use in biological samples. Here, we describe the use of high-energy (100kV, 600W) linearly polarized beam energy-dispersive X-Ray fluorescence spectroscopy (EDXRF) in tandem with a three-dimensional optics design to determine 0.1-5.1μgg(-1) levels of selenium in biological samples. The effects of various experimental parameters such as applied voltage, acquisition time, secondary target and various filters were thoroughly investigated. The detection limit of selenium in biological samples via high-energy (100kV, 600W) linearly polarized beam energy-dispersive X-ray fluorescence spectroscopy was decreased by one order of magnitude versus conventional XRF (Paltridge et al., 2012) and found to be 0.1μg/g. To the best of our knowledge, this is the first report to describe EDXRF measurements of Se in biological samples with important implications for the nutrition and analytical chemistry communities. PMID:26922394

  16. Quantitative energy-dispersive x-ray diffraction for identification of counterfeit medicines: a preliminary study

    NASA Astrophysics Data System (ADS)

    Crews, Chiaki C. E.; O'Flynn, Daniel; Sidebottom, Aiden; Speller, Robert D.

    2015-06-01

    The prevalence of counterfeit and substandard medicines has been growing rapidly over the past decade, and fast, nondestructive techniques for their detection are urgently needed to counter this trend. In this study, energy-dispersive X-ray diffraction (EDXRD) combined with chemometrics was assessed for its effectiveness in quantitative analysis of compressed powder mixtures. Although EDXRD produces lower-resolution diffraction patterns than angular-dispersive X-ray diffraction (ADXRD), it is of interest for this application as it carries the advantage of allowing the analysis of tablets within their packaging, due to the higher energy X-rays used. A series of caffeine, paracetamol and microcrystalline cellulose mixtures were prepared with compositions between 0 - 100 weight% in 20 weight% steps (22 samples in total, including a centroid mixture), and were pressed into tablets. EDXRD spectra were collected in triplicate, and a principal component analysis (PCA) separated these into their correct positions in the ternary mixture design. A partial least-squares (PLS) regression model calibrated using this training set was validated using both segmented cross-validation, and with a test set of six samples (mixtures in 8:1:1 and 5⅓:2⅓:2⅓ ratios) - the latter giving a root-mean square error of prediction (RMSEP) of 1.30, 2.25 and 2.03 weight% for caffeine, paracetamol and cellulose respectively. These initial results are promising, with RMSEP values on a par with those reported in the ADXRD literature.

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

    NASA Astrophysics Data System (ADS)

    Ellmer, K.; Mientus, R.; Weiß, V.; Rossner, H.

    2001-07-01

    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° and 10°, 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.

  18. Towards hybrid pixel detectors for energy-dispersive or soft X-ray photon science.

    PubMed

    Jungmann-Smith, J H; Bergamaschi, A; Brückner, M; Cartier, S; Dinapoli, R; Greiffenberg, D; Huthwelker, T; Maliakal, D; Mayilyan, D; Medjoubi, K; Mezza, D; Mozzanica, A; Ramilli, M; Ruder, Ch; Schädler, L; Schmitt, B; Shi, X; Tinti, G

    2016-03-01

    JUNGFRAU (adJUstiNg Gain detector FoR the Aramis User station) is a two-dimensional hybrid pixel detector for photon science applications at free-electron lasers and synchrotron light sources. The JUNGFRAU 0.4 prototype presented here is specifically geared towards low-noise performance and hence soft X-ray detection. The design, geometry and readout architecture of JUNGFRAU 0.4 correspond to those of other JUNGFRAU pixel detectors, which are charge-integrating detectors with 75 µm × 75 µm pixels. Main characteristics of JUNGFRAU 0.4 are its fixed gain and r.m.s. noise of as low as 27 e(-) electronic noise charge (<100 eV) with no active cooling. The 48 × 48 pixels JUNGFRAU 0.4 prototype can be combined with a charge-sharing suppression mask directly placed on the sensor, which keeps photons from hitting the charge-sharing regions of the pixels. The mask consists of a 150 µm tungsten sheet, in which 28 µm-diameter holes are laser-drilled. The mask is aligned with the pixels. The noise and gain characterization, and single-photon detection as low as 1.2 keV are shown. The performance of JUNGFRAU 0.4 without the mask and also in the charge-sharing suppression configuration (with the mask, with a `software mask' or a `cluster finding' algorithm) is tested, compared and evaluated, in particular with respect to the removal of the charge-sharing contribution in the spectra, the detection efficiency and the photon rate capability. Energy-dispersive and imaging experiments with fluorescence X-ray irradiation from an X-ray tube and a synchrotron light source are successfully demonstrated with an r.m.s. energy resolution of 20% (no mask) and 14% (with the mask) at 1.2 keV and of 5% at 13.3 keV. The performance evaluation of the JUNGFRAU 0.4 prototype suggests that this detection system could be the starting point for a future detector development effort for either applications in the soft X-ray energy regime or for an energy-dispersive

  19. Compositional analysis of Ceramic Glaze by Laser Induced Breakdown Spectroscopy and Energy Dispersive X-Ray

    NASA Astrophysics Data System (ADS)

    Khedr, A.; Abdel-kareem, O.; Elnabi, S. H.; Harith, M. A.

    2011-09-01

    Laser induced breakdown spectroscopy (LIBS) has been applied for the analysis of Egyptian Islamic glaze ceramic sample. The sample dating back to Fatimid period (969-1169AD), and collected from Al-Fustat excavation store in Cairo. The analysis of contaminated pottery sample has been performed to draw mapping for the elemental compositions by LIBS technique. LIBS measurements have been done by the fundamental wavelength (1064 nm) of Nd: YAG laser for the elemental analysis and performing the cleaning processes of the pottery sample. In addition, complementary analyses were carried out by scanning electron microscopy linked with energy dispersive X-ray microanalysis (SEM/EDX) to obtain verification of chemical results. The morphological surfaces before and after cleaning has been done by Optical Microscopy (OM).

  20. Energy dispersive x-ray diffraction of charge density waves via chemical filtering

    SciTech Connect

    Feng Yejun; Somayazulu, M. S.; Jaramillo, R.; Rosenbaum, T.F.; Isaacs, E.D.; Hu Jingzhu; Mao Hokwang

    2005-06-15

    Pressure tuning of phase transitions is a powerful tool in condensed matter physics, permitting high-resolution studies while preserving fundamental symmetries. At the highest pressures, energy dispersive x-ray diffraction (EDXD) has been a critical method for geometrically confined diamond anvil cell experiments. We develop a chemical filter technique complementary to EDXD that permits the study of satellite peaks as weak as 10{sup -4} of the crystal Bragg diffraction. In particular, we map out the temperature dependence of the incommensurate charge density wave diffraction from single-crystal, elemental chromium. This technique provides the potential for future GPa pressure studies of many-body effects in a broad range of solid state systems.

  1. Evaluation on determination of iodine in coal by energy dispersive X-ray fluorescence

    USGS Publications Warehouse

    Wang, B.; Jackson, J.C.; Palmer, C.; Zheng, B.; Finkelman, R.B.

    2005-01-01

    A quick and inexpensive method of relative high iodine determination from coal samples was evaluated. Energy dispersive X-ray fluorescence (EDXRF) provided a detection limit of about 14 ppm (3 times of standard deviations of the blank sample), without any complex sample preparation. An analytical relative standard deviation of 16% was readily attainable for coal samples. Under optimum conditions, coal samples with iodine concentrations higher than 5 ppm can be determined using this EDXRF method. For the time being, due to the general iodine concentrations of coal samples lower than 5 ppm, except for some high iodine content coal, this method can not effectively been used for iodine determination. More work needed to meet the requirement of determination of iodine from coal samples for this method. Copyright ?? 2005 by The Geochemical Society of Japan.

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

    PubMed

    Chen, Z; Weyland, M; Sang, X; Xu, W; Dycus, J H; LeBeau, J M; D'Alfonso, A J; Allen, L J; Findlay, S D

    2016-09-01

    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. PMID:27258645

  3. Characterization of small noble metal electrodes by voltammetry and energy dispersive x ray analysis

    NASA Astrophysics Data System (ADS)

    Strein, Timothy G.; Ewing, Andrew G.

    1993-01-01

    Construction and characterization of platinum and gold electrodes with total structural diameters of 1-2 micrometers is described. These small voltammetric probes have been constructed by direct electroreduction of noble metals onto the tips of etched carbon fiber microdisk electrodes. Voltammetry, electron microscopy, energy-dispersive x-ray analysis, and pulsed amperometric detection have been used to characterize these electrodes. Dopamine concentrations have been determined over a range of 10(exp -4) to 10(exp -3) M in the biological buffer system which contains 25 mM glucose, a compound known to adsorb strongly to electrodes. Amperometric monitoring at a constant potential with these small results in signal decay of 20% to 40% in a ten minute experiment. Pulsed amperometric detection minimizes electrode fouling, resulting in 5% or less signal decay over the same ten minute period.

  4. Portable apparatus for in situ x-ray diffraction and fluorescence analyses of artworks.

    PubMed

    Eveno, Myriam; Moignard, Brice; Castaing, Jacques

    2011-10-01

    A portable X-ray fluorescence/X-ray diffraction (XRF/XRD) system for artwork studies has been designed constructed and tested. It is based on Debye Scherrer XRD in reflection that takes advantage of many recent improvements in the handling of X-rays (polycapillary optics; advanced two-dimensional detection). The apparatus is based on a copper anode air cooled X-ray source, and the XRD analysis is performed on a 5-20 μm thick layer from the object surface. Energy dispersive XRF elemental analysis can be performed at the same point as XRD, giving elemental compositions that support the interpretation of XRD diagrams. XRF and XRD analyses were tested to explore the quality and the limits of the analytical technique. The XRD diagrams are comparable in quality with diagrams obtained with conventional laboratory equipment. The mineral identification of materials in artwork is routinely performed with the portable XRF-XRD system. Examples are given for ceramic glazes containing crystals and for paintings where the determination of pigments is still a challenge for nondestructive analysis. For instance, lead compounds that provide a variety of color pigments can be easily identified as well as a pigment such as lapis lazuli that is difficult to identify by XRF alone. More than 70 works of art have been studied in situ in museums, monuments, etc. In addition to ceramics and paintings, these works include bronzes, manuscripts, etc., which permit improvement in the comprehension of ancient artistic techniques. PMID:21615981

  5. Analysis of nuclear materials by energy dispersive x-ray fluorescence and spectral effects of alpha decay

    SciTech Connect

    Worley, Christopher G

    2009-01-01

    Energy dispersive X-ray fluorescence (EDXRF) spectra collected from alpha emitters are complicated by artifacts inherent to the alpha decay process, particularly when using portable instruments. For example, {sup 239}Pu EDXRF spectra exhibit a prominent uranium L X-ray emission peak series due to sample alpha decay rather than source-induced X-ray fluorescence. A portable EDXRF instrument was used to collect spectra from plutonium, americium, and a Pu-contaminated steel sample. The plutonium sample was also analyzed by wavelength dispersive XRF to demonstrate spectral differences observed when using these very different instruments.

  6. Energy dispersive X-ray diffraction in the diamond anvil, high-pressure apparatus - Comparison of synchrotron and conventional X-ray sources

    NASA Technical Reports Server (NTRS)

    Spain, I. L.; Black, D. R.

    1985-01-01

    The use of both conventional fixed-anode X-ray sources and synchrotron radiation to carry out energy-dispersive X-ray diffraction experiments at high pressure in a diamond anvil cell, is discussed. The photon flux at the sample and at the detector for the two cases are compared and the results are presented in graphs. It is shown that synchrotron radiation experiments can be performed with nearly two orders of magnitude increase in data rate if superior detectors and detector electronics are available.

  7. Combination of Raman, Infrared, and X-Ray Energy-Dispersion Spectroscopies and X-Ray Diffraction to Study a Fossilization Process

    NASA Astrophysics Data System (ADS)

    de Sousa Filho, Francisco Eduardo; da Silva, João Hermínio; Feitosa Saraiva, Antônio Álamo; Brito, Deyvid Dennys S.; Viana, Bartolomeu Cruz; de Oliveira Abagaro, Bruno Tavares; de Tarso Cavalcante Freire, Paulo

    2011-12-01

    X-ray diffraction was combined with X-ray energy-dispersion, Fourier-transform infrared, and Raman spectroscopies to study the fossilization of a Cretaceous specimen of the plant Brachyphyllum castilhoi, a fossil from the Ipubi Formation, in the Araripe Sedimentary Basin, Northeastern Brazil. Among the possible fossilization processes, which could involve pyrite, silicon oxide, calcium oxide, or other minerals, we were able to single out pyritization as the central mechanism producing the fossil, more than 100 million years ago. In addition to expanding the knowledge of the Ipubi Formation, this study shows that, when combined with other experimental techniques, Raman spectroscopy is a valuable tool at the paleontologist's disposal.

  8. Fast GPU-based absolute intensity determination for energy-dispersive X-ray Laue diffraction

    NASA Astrophysics Data System (ADS)

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

    2016-01-01

    This paper presents a novel method for fast determination of absolute intensities in the sites of Laue spots generated by a tetragonal hen egg-white lysozyme crystal after exposure to white synchrotron radiation during an energy-dispersive X-ray Laue diffraction experiment. The Laue spots are taken by means of an energy-dispersive X-ray 2D pnCCD detector. Current pnCCD detectors have a spatial resolution of 384 × 384 pixels of size 75 × 75 μm2 each and operate at a maximum of 400 Hz. Future devices are going to have higher spatial resolution and frame rates. The proposed method runs on a computer equipped with multiple Graphics Processing Units (GPUs) which provide fast and parallel processing capabilities. Accordingly, our GPU-based algorithm exploits these capabilities to further analyse the Laue spots of the sample. The main contribution of the paper is therefore an alternative algorithm for determining absolute intensities of Laue spots which are themselves computed from a sequence of pnCCD frames. Moreover, a new method for integrating spectral peak intensities and improved background correction, a different way of calculating mean count rate of the background signal and also a new method for n-dimensional Poisson fitting are presented.We present a comparison of the quality of results from the GPU-based algorithm with the quality of results from a prior (base) algorithm running on CPU. This comparison shows that our algorithm is able to produce results with at least the same quality as the base algorithm. Furthermore, the GPU-based algorithm is able to speed up one of the most time-consuming parts of the base algorithm, which is n-dimensional Poisson fitting, by a factor of more than 3. Also, the entire procedure of extracting Laue spots' positions, energies and absolute intensities from a raw dataset of pnCCD frames is accelerated by a factor of more than 3.

  9. Analysis of energy dispersive x-ray diffraction profiles for material identification, imaging and system control

    NASA Astrophysics Data System (ADS)

    Cook, Emily Jane

    2008-12-01

    This thesis presents the analysis of low angle X-ray scatter measurements taken with an energy dispersive system for substance identification, imaging and system control. Diffraction measurements were made on illicit drugs, which have pseudo- crystalline structures and thus produce diffraction patterns comprising a se ries of sharp peaks. Though the diffraction profiles of each drug are visually characteristic, automated detection systems require a substance identification algorithm, and multivariate analysis was selected as suitable. The software was trained with measured diffraction data from 60 samples covering 7 illicit drugs and 5 common cutting agents, collected with a range of statistical qual ities and used to predict the content of 7 unknown samples. In all cases the constituents were identified correctly and the contents predicted to within 15%. Soft tissues exhibit broad peaks in their diffraction patterns. Diffraction data were collected from formalin fixed breast tissue samples and used to gen erate images. Maximum contrast between healthy and suspicious regions was achieved using momentum transfer windows 1.04-1.10 and 1.84-1.90 nm_1. The resulting images had an average contrast of 24.6% and 38.9% compared to the corresponding transmission X-ray images (18.3%). The data was used to simulate the feedback for an adaptive imaging system and the ratio of the aforementioned momentum transfer regions found to be an excellent pa rameter. Investigation into the effects of formalin fixation on human breast tissue and animal tissue equivalents indicated that fixation in standard 10% buffered formalin does not alter the diffraction profiles of tissue in the mo mentum transfer regions examined, though 100% unbuffered formalin affects the profile of porcine muscle tissue (a substitute for glandular and tumourous tissue), though fat is unaffected.

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

    NASA Technical Reports Server (NTRS)

    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.

  11. A study of the behavior of bromide in artificial pits using in situ X-ray microprobe analysis

    SciTech Connect

    Isaacs, H.S.; Kaneko, M.

    1997-12-31

    An in situ X-ray microprobe analysis of Type 316 stainless steel artificial pits has been carried out with a bromide/chloride solution. A high intensity 8 micron diameter polychromatic X-ray beam was scanned across the steel solution interface within the artificial pit. The resulting X-ray fluorescence was analyzed using an energy dispersive X-ray detector. In contrast to the light Cl atom, Br could be detected, making it possible to monitor the behavior of halides in the artificial pits and in the salt layer at the interface. It was found that Br was more active than Cl. At high potentials, elemental Br was produced as an oxidation product, whereas without added bromide, chloride only formed a salt layer. Br also concentrated at the salt steel interface at potentials below where it was oxidized.

  12. Two facets of the x-ray microanalysis at low voltage: The secondary fluorescence x-rays emission and the microcalorimeter energy-dispersive spectrometer

    NASA Astrophysics Data System (ADS)

    Demers, Hendrix

    The best spatial resolution, for a microanalysis with a scanning electron microscope (SEND, is achieved by using a low voltage electron beam. But the x-ray microanalysis was developed for high electron beam energy (greater than 10 keV). Also, the specimen will often contain light and medium elements and the analyst will have to use a mixture of K, L, and sometime M x-ray peaks for the x-ray microanalysis. With a mixture of family lines, it will be common to have secondary fluorescence x-rays emission by K--L and L--K interactions. The accuracy of the fluorescence correction models presently used by the analyst are not well known for these interactions. This work shows that the modified secondary fluorescence x-rays emission correction models can improve the accuracy of the microanalysis for K--L and L--K interactions. The general equation derived in this work allows the identification of three factors which influence the secondary fluorescence x-rays emission. The fluorescence production factor epsilonƒ can be used to predict the importance of the secondary fluorescence x-rays emission. A large value of epsilonƒ indicates that a fluorescence correction is needed. Another disadvantage of using a low voltage is that there are more frequent occurrences of x-ray peaks overlap. A new microanalysis instruments that combines the high-spatial resolution and high-energy resolution for x-ray detection is needed. The microcalorimeter energy-dispersive spectrometer (muEDS) should improve the low voltage microanalysis, but the maturity of this technology has to be evaluated first. One of the first commercial muEDS for x-ray microanalysis in a SEM is studied and analyzed in this work. This commercial muEDS has an excellent energy resolution (˜ 15 eV) and can detect x-rays of low energy. This x-ray detector can be used as a high-spatial resolution and high-energy resolution microanalysis instrument. There are still hurdles that this technology must overcome before its

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

    SciTech Connect

    Forslind, B.

    1988-06-01

    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.

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

    NASA Astrophysics Data System (ADS)

    Li, Fangzuo; Liu, Zhiguo; Sun, Tianxi

    2016-04-01

    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 (ICo/IRa) and effective atomic numbers (Zeff) of SiC ceramics with the confocal energy dispersive X-ray fluorescence (EDXRF) spectrometer. A calibration curve of the relationship between ICo/IRa and Zeff 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 Zeff differing from each other by only 0.01. The linear relationship between the variation of Zeff 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 ΔCC, ΔCSi, and ΔCO 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.

  15. Elemental analysis of mining wastes by energy dispersive X-ray fluorescence (EDXRF)

    NASA Astrophysics Data System (ADS)

    Gonzalez-Fernandez, O.; Queralt, I.; Carvalho, M. L.; Garcia, G.

    2007-08-01

    An energy dispersive X-ray fluorescence (EDXRF) tri-axial geometry experimental spectrometer has been employed to determine the concentrations of 13 different elements (K, Ca, Ti, Cr, Mn, Fe, Co, Ni, Cu, Zn, Rb, Sr and Pb) in mine wastes from different depths of two mine tailings from the Cartagena-La Union (Spain) mining district. The elements were determined and quantified using the fundamental parameters method. The concentrations of Cr, Ni, Cu, Zn and Pb were compared to the values from the European and Spanish legislation to evaluate the environmental risk and to classify the wastes as inert wastes or as wastes that have to be control land-filled. The results obtained demonstrate that these wastes can be considered as inert for the considered elements, apart from the concentration levels of Zn and Pb. Whilst Zn slightly overpasses the regulatory levels, Pb mean value exceeds three to six times the value to be considered as Class I potential land-filling material.

  16. An energy dispersive x-ray scattering and molecular dynamics study of liquid dimethyl carbonate

    NASA Astrophysics Data System (ADS)

    Gontrani, Lorenzo; Russina, Olga; Marincola, Flaminia Cesare; Caminiti, Ruggero

    2009-12-01

    In this work, we report on the first x-ray diffraction study on liquid dimethyl carbonate. Diffraction spectra were collected with an energy-dispersive instrument, whose wide Q-range allows the structure determination of weakly ordered systems (such as liquids). The structural correlation in this liquid ranges up to about 20 Å. The observed patterns are interpreted with a structural model derived from classical molecular dynamics simulations. The simulations were run using OPLS force field, only slightly modified to restrain bond distances to the experimental values. The model structure function and radial distribution functions, averaged among the productive trajectory frames, are in very good agreement with the corresponding experimental ones. Molecular dynamics results show that the deviations from C2v cis-cis structure, predicted by ab initio calculations and observed by electron diffraction in the gas phase, are small. By analyzing the intra- and intermolecular pair distribution functions, it was possible to assign the peaks of the experimental radial distribution function to specific structural correlations, and to compute the different average intermolecular coordination numbers. The intermolecular methyl-carbonyl oxygen distance is thoroughly discussed to assess the presence of weak C-H⋯ṡO hydrogen bonds.

  17. Microcalorimeter-type energy dispersive X-ray spectrometer for a transmission electron microscope.

    PubMed

    Hara, Toru; Tanaka, Keiichi; Maehata, Keisuke; Mitsuda, Kazuhisa; Yamasaki, Noriko Y; Ohsaki, Mitsuaki; Watanabe, Katsuaki; Yu, Xiuzhen; Ito, Takuji; Yamanaka, Yoshihiro

    2010-01-01

    A new energy dispersive X-ray spectrometer (EDS) with a microcalorimeter detector equipped with a transmission electron microscope (TEM) has been developed for high- accuracy compositional analysis in the nanoscale. A superconducting transition-edge-sensor-type microcalorimeter is applied as the detector. A cryogen-free cooling system, which consists of a mechanical and a dilution refrigerator, is selected to achieve long-term temperature stability. In order to mount these detector and refrigerators on a TEM, the cooling system is specially designed such that these two refrigerators are separated. Also, the detector position and arrangement are carefully designed to avoid adverse affects between the superconductor detector and the TEM lens system. Using the developed EDS system, at present, an energy resolution of 21.92 eV full-width-at-half maximum has been achieved at the Cr K alpha line. This value is about seven times better than that of the current typical commercial Si(Li) detector, which is usually around 140 eV. The developed microcalorimeter EDS system can measure a wide energy range, 1-20 keV, at one time with this high energy resolution that can resolve peaks from most of the elements. Although several further developments will be needed to enable practical use, highly accurate compositional analysis with high energy resolution will be realized by this microcalorimeter EDS system. PMID:19717388

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

    NASA Astrophysics Data System (ADS)

    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.

  19. Multi-element analysis of pyrite ores using polarized energy-dispersive X-ray fluorescence spectrometry.

    PubMed

    Ustündağ, Zafer; Ustündağ, Ilknur; Kağan Kadioğlu, Yusuf

    2007-07-01

    X-ray fluorescence (XRF) spectrometry is used worldwide in geological material analysis. This study, applies polarized energy-dispersive X-ray fluorescence (PEDXRF) Spectrometer and compares in the samples of Rize-Cayeli and Mardin pyrite ores. The samples of pyrite ore were collected from the Rize and Mardin in Turkey. The prepared samples were analyzed using a PEDXRF spectrometer. The result of the analysis shows the presence of many elements including rare-earth elements (from Na to Th). The accuracy and precision of the technique for chemical analysis is demonstrated by analyzing USGS standards, GEOL, GBW 7109 and GBW-7309 sediment. PMID:17459714

  20. Backscattered electron imaging and windowless energy dispersive x-ray microanalysis: a new technique for gallstone analysis

    SciTech Connect

    Kaufman, H.S.; Lillemoe, K.D.; Magnuson, T.H.; Frasca, P.; Pitt, H.A. )

    1990-12-01

    Scanning electron microscopy with or without conventional energy dispersive x-ray microanalysis is currently used to identify gallstone microstructure and inorganic composition. Organic calcium salts are among many biliary constituents thought to have a role in gallstone nidation and growth. However, current analytical techniques which identify these salts are destructive and compromise gallstone microstructural data. We have developed a new technique for gallstone analysis which provides simultaneous structural and compositional identification of calcium salts within gallstones. Backscattered electron imaging is used to localize calcium within cholesterol at minimum concentrations of 0.01%. Windowless energy dispersive x-ray microanalysis produces elemental spectra of gallstone calcium salts which are qualitatively and quantitatively different. These combined techniques provide simultaneous structural and compositional information obtained from intact gallstone cross-sections and have been used to identify calcium salts in gallstones obtained at cholecystectomy from 106 patients.

  1. Characterization of Japanese color sticks by energy dispersive X-ray fluorescence, X-ray diffraction and Fourier transform infrared analysis

    NASA Astrophysics Data System (ADS)

    Manso, M.; Valadas, S.; Pessanha, S.; Guilherme, A.; Queralt, I.; Candeias, A. E.; Carvalho, M. L.

    2010-04-01

    This work comprises the use of energy dispersive X-ray fluorescence (EDXRF), X-ray diffraction (XRD) and Fourier transformed infrared (FTIR) techniques for the study of the composition of twentieth century traditional Japanese color sticks. By using the combination of analytical techniques it was possible to obtain information on inorganic and organic pigments, binders and fillers present in the sticks. The colorant materials identified in the sticks were zinc and titanium white, chrome yellow, yellow and red ochre, vermillion, alizarin, indigo, Prussian and synthetic ultramarine blue. The results also showed that calcite and barite were used as inorganic mineral fillers while Arabic gum was the medium used. EDXRF offered great potential for such investigations since it allowed the identification of the elements present in the sample preserving its integrity. However, this information alone was not enough to clearly identify some of the materials in study and therefore it was necessary to use XRD and FTIR techniques.

  2. In situ x-ray reflectivity and grazing incidence x-ray diffraction study of L 1(0) ordering in (57)Fe/Pt multilayers.

    PubMed

    Raghavendra Reddy, V; Gupta, Ajay; Gome, Anil; Leitenberger, Wolfram; Pietsch, U

    2009-05-01

    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(0) phase formation in [Fe(19 Å)/Pt(25 Å)]( × 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(0) phase, (ii) the ordered fct L 1(0) FePt peaks start to appear at 320 °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 Mössbauer spectroscopies are used to study the magnetic properties of the as-deposited and 400 °C annealed multilayers. The magnetic data for the 400 °C annealed sample indicate that the magnetization is at an angle of ∼50° from the plane of the film. PMID:21825468

  3. ENERGY-DISPERSIVE, X-RAY REFLECTIVITY DENSITY MEASUREMENTS OF POROUS SIO2 XEROGELS

    EPA Science Inventory

    X-ray reflectivity has been used to nondestructively measure the density of thin, porous, SiO2-based xerogels. Critical angle, defined by total external reflection, was measured for multiple x-ray energies to correct for sample misalignment error in me determination of the densit...

  4. [Influence of the Experiment Energy Dispersive X-Ray Fluorescence Measurement of Uranium by Different Excitation Source].

    PubMed

    Xiong, Chao; Ge, Liang-quan; Liu, Duan; Zhang, Qing-xian; Gu, Yi; Luo, Yao-yao; Zhao, Jian-kun

    2016-03-01

    Aiming at the self-excitation effect on the interference of measurements which exist in the process of Energy dispersive X-ray fluorescence method for uranium measurement. To solve the problem of radioactive isotopes only used as excitation source in determination of uranium. Utilizing the micro X-ray tube to test Self-excitation effect to get a comparison of the results obtained by three different uranium ore samples--109 Cd, 241 Am and Mirco X-ray tube. The results showed that self-excitation effect produced the area measure of characteristic X-ray peak is less than 1% of active condition, also the interference of measurements can be negligible. Photoelectric effect cross-section excited by 109 Cd is higher, corresponding fluorescence yield is higher than excited by 241 Am as well due to characteristics X-ray energy of 109 Cd, 22.11 & 24.95 KeV adjacent to absorption edge energy of L(α), 21.75 KeV, based on the above, excitation efficiency by 109 Cd is higher than 241 Am; The fact that measurement error excited by 241 Am is significantly greater than by 109 Cd is mainly due to peak region overlap between L energy peaks of uranium and Scattering peak of 241 Am, 26.35 keV, These factors above caused the background of measured Spectrum higher; The error between the uranium content in ore samples which the X-ray tube as the excitation source and the chemical analysis results is within 10%. Conclusion: This paper come to the conclusion that the technical quality of uranium measurement used X-ray tube as excitation source is superior to that in radioactive source excitation mode. PMID:27400534

  5. Standardless Quantitative Electron-Excited X-ray Microanalysis by Energy-Dispersive Spectrometry: What Is Its Proper Role?

    PubMed

    Newbury

    1998-11-01

    : Electron beam X-ray microanalysis with semiconductor energy-dispersive spectrometry (EDS) performed with standards and calculated matrix corrections can yield quantitative results with a distribution such that 95% of analyses fall within +/-5% relative for major and minor constituents. Standardless methods substitute calculations for the standard intensities, based either on physical models of X-ray generation and propagation (first principles) or on mathematical fits to remotely measured standards (fitted standards). Error distributions have been measured for three different standardless analysis procedures with a suite of microanalysis standards including metal alloys, glasses, minerals, ceramics, and stoichiometric compounds. For the first-principles standardless procedure, the error distribution placed 95% of analyses within +/-50% relative, whereas for two commercial fitted standards procedures, the error distributions placed 95% of analyses within +/-25% relative. The implication of these error distributions for the accuracy of analytical results is considered, and recommendations for the use of standardless analysis are given. PMID:10087281

  6. Standardless Quantitative Electron-Excited X-ray Microanalysis by Energy-Dispersive Spectrometry: What Is Its Proper Role?

    NASA Astrophysics Data System (ADS)

    Newbury, Dale E.

    1998-11-01

    : Electron beam X-ray microanalysis with semiconductor energy-dispersive spectrometry (EDS) performed with standards and calculated matrix corrections can yield quantitative results with a distribution such that 95% of analyses fall within ±5% relative for major and minor constituents. Standardless methods substitute calculations for the standard intensities, based either on physical models of X-ray generation and propagation (first principles) or on mathematical fits to remotely measured standards (fitted standards). Error distributions have been measured for three different standardless analysis procedures with a suite of microanalysis standards including metal alloys, glasses, minerals, ceramics, and stoichiometric compounds. For the first-principles standardless procedure, the error distribution placed 95% of analyses within ±50% relative, whereas for two commercial fitted standards procedures, the error distributions placed 95% of analyses within ±25% relative. The implication of these error distributions for the accuracy of analytical results is considered, and recommendations for the use of standardless analysis are given.

  7. Low energy x-ray spectra measured with a mercuric iodide energy dispersive spectrometer in a scanning electron microscope

    SciTech Connect

    Iwanczyk, J.S.; Dabrowski, A.J.; Huth, G.C.; Bradley, J.G.; Conley, J.M.; Albee, A.L.

    1985-01-01

    A mercuric iodide energy dispersive x-ray spectrometer, with Peltier cooling provided for the detector and input field effect transistor, has been developed and tested in a scanning electron microscope. X-ray spectra were obtained with the 15 keV electron beam. An energy resolution of 225 eV (FWHM) for Mn-K/sub ..cap alpha../ at 5.9 keV and 195 eV (FWHM) for Mg-K line at 1.25 keV has been measured. Overall system noise level was 175 eV (FWHM). The detector system characterization with a carbon target demonstrated good energy sensitivity at low energies and lack of significant spectral artifacts at higher energies. 16 refs., 5 figs.

  8. Low energy X-ray spectra measured with a mercuric iodide energy dispersive spectrometer in a scanning electron microscope

    NASA Technical Reports Server (NTRS)

    Iwanczyk, J. S.; Dabrowski, A. J.; Huth, G. C.; Bradley, J. G.; Conley, J. M.

    1986-01-01

    A mercuric iodide energy dispersive X-ray spectrometer, with Peltier cooling provided for the detector and input field effect transistor, has been developed and tested in a scanning electron microscope. X-ray spectra were obtained with the 15 keV electron beam. An energy resolution of 225 eV (FWHM) for Mn-K(alpha) at 5.9 keV and 195 eV (FWHM) for the Mg-K line at 1.25 keV has been measured. Overall system noise level was 175 eV (FWHM). The detector system characterization with a carbon target demonstrated good energy sensitivity at low energies and lack of significant spectral artifacts at higher energies.

  9. A new background subtraction method for energy dispersive X-ray fluorescence spectra using a cubic spline interpolation

    NASA Astrophysics Data System (ADS)

    Yi, Longtao; Liu, Zhiguo; Wang, Kai; Chen, Man; Peng, Shiqi; Zhao, Weigang; He, Jialin; Zhao, Guangcui

    2015-03-01

    A new method is presented to subtract the background from the energy dispersive X-ray fluorescence (EDXRF) spectrum using a cubic spline interpolation. To accurately obtain interpolation nodes, a smooth fitting and a set of discriminant formulations were adopted. From these interpolation nodes, the background is estimated by a calculated cubic spline function. The method has been tested on spectra measured from a coin and an oil painting using a confocal MXRF setup. In addition, the method has been tested on an existing sample spectrum. The result confirms that the method can properly subtract the background.

  10. Probing Heterogeneous Chemistry of Individual Atmospheric Particles Using Scanning Electron Microscopy and Energy-Dispersive X-ray Analysis

    SciTech Connect

    Krueger, Brenda J.; Grassian, Vicki H.; Iedema, Martin J.; Cowin, James P.; Laskin, Alexander

    2003-10-01

    In this paper, we demonstrate the utility of single-particle analysis to investigate the chemistry of isolated, individual particles of atmospheric relevance such as NaCl, sea salt, CaCO3, and SiO2. A variety of state-of-th-art scanning electron microscopy techniques, including environmental scanning electon microscopy and computer-controlled scanning electron microscopy/energy-dispersive X-ray analysis, were utilized for monitoring and quantifying phase transitions of individual particles, morphology, and compositional changes of individual particles as they react with nitric acid.

  11. Benzyne-functionalized graphene and graphite characterized by Raman spectroscopy and energy dispersive X-ray analysis

    PubMed Central

    Magedov, Igor V.; Frolova, Lilia V.; Ovezmyradov, Mekan; Bethke, Donald; Shaner, Eric A.; Kalugin, Nikolai G.

    2012-01-01

    The benzyne functionalization of chemical vapor deposition grown large area graphene and graphite was performed using a mixture of o-trimethylsilylphenyl triflate and cesium fluoride that react with the carbon surface. The reaction requires at least 2 days of treatment before the appearance of Raman and energy-dispersive X-ray spectral signatures that verify modification. Raman spectra of modified graphene and graphite show a rich structure of lines corresponding to C=C-C, C-H, and low frequency modes of surface-attached benzyne rings. PMID:23505324

  12. Dose-rate controlled energy dispersive x-ray spectroscopic mapping of the metallic components in a biohybrid nanosystem

    NASA Astrophysics Data System (ADS)

    Zhu, Yuanyuan; Munro, Catherine J.; Olszta, Matthew J.; Edwards, Danny J.; Braunschweig, Adam B.; Knecht, Marc R.; Browning, Nigel D.

    2016-08-01

    In this work, we showcase that through precise control of the electron dose rate, state-of-the-art large solid angle energy dispersive x-ray spectroscopy mapping in aberration-corrected scanning transmission electron microscope is capable of faithful and unambiguous chemical characterization of the Pt and Pd distribution in a peptide-mediated nanosystem. This low-dose-rate recording scheme adds another dimension of flexibility to the design of elemental mapping experiments, and holds significant potential for extending its application to a wide variety of beam sensitive hybrid nanostructures.

  13. Electro-deposition of Cu studied with in situ electrochemical scanning transmission x-ray microscopy

    NASA Astrophysics Data System (ADS)

    Hitchcock, A. P.; Qin, Z.; Rosendahl, S. M.; Lee, V.; Reynolds, M.; Hosseinkhannazer, H.

    2016-01-01

    Soft X-ray scanning transmission X-ray microscopy (STXM) was used to investigate Cu deposition onto, and stripping from a Au surface. Cu 2p spectromicroscopy was used to analyze initial and final states (ex situ processing) and follow the processes in situ. The in situ experiments were carried out using a static electrochemical cell with an electrolyte layer thickness of ˜1 μm. A new apparatus for in situ electrochemical STXM is described.

  14. A semianalytic model to extract differential linear scattering coefficients of breast tissue from energy dispersive x-ray diffraction measurements

    SciTech Connect

    LeClair, Robert J.; Boileau, Michel M.; Wang Yinkun

    2006-04-15

    The goal of this work is to develop a technique to measure the x-ray diffraction signals of breast biopsy specimens. A biomedical x-ray diffraction technology capable of measuring such signals may prove to be of diagnostic use to the medical field. Energy dispersive x-ray diffraction measurements coupled with a semianalytical model were used to extract the differential linear scattering coefficients [{mu}{sub s}(x)] of breast tissues on absolute scales. The coefficients describe the probabilities of scatter events occurring per unit length of tissue per unit solid angle of detection. They are a function of the momentum transfer argument, x=sin({theta}/2)/{lambda}, where {theta}=scatter angle and {lambda}=incident wavelength. The technique was validated by using a 3 mm diameter 50 kV polychromatic x-ray beam incident on a 5 mm diameter 5 mm thick sample of water. Water was used because good x-ray diffraction data are available in the literature. The scatter profiles from 6 deg. to 15 deg. in increments of 1 deg. were measured with a 3 mmx3 mmx2 mm thick cadmium zinc telluride detector. A 2 mm diameter Pb aperture was placed on top of the detector. The target to detector distance was 29 cm and the duration of each measurement was 10 min. Ensemble averages of the results compare well with the gold standard data of A. H. Narten [''X-ray diffraction data on liquid water in the temperature range 4 deg. C-200 deg. C, ORNL Report No. 4578 (1970)]. An average 7.68% difference for which most of the discrepancies can be attributed to the background noise at low angles was obtained. The preliminary measurements of breast tissue are also encouraging.

  15. Note: High-pressure in situ x-ray laminography using diamond anvil cell

    NASA Astrophysics Data System (ADS)

    Nomura, Ryuichi; Uesugi, Kentaro

    2016-04-01

    A high-pressure in situ X-ray laminography technique was developed using a newly designed, laterally open diamond anvil cell. A low X-ray beam of 8 keV energy was used, aiming at future application to dual energy X-ray chemical imaging techniques. The effects of the inclination angle and the imaging angle range were evaluated at ambient pressure using the apparatus. Sectional images of ruby ball samples were successfully reconstructed at high pressures, up to approximately 50 GPa. The high-pressure in situ X-ray laminography technique is expected to provide new insights into the deep Earth sciences.

  16. Note: High-pressure in situ x-ray laminography using diamond anvil cell.

    PubMed

    Nomura, Ryuichi; Uesugi, Kentaro

    2016-04-01

    A high-pressure in situ X-ray laminography technique was developed using a newly designed, laterally open diamond anvil cell. A low X-ray beam of 8 keV energy was used, aiming at future application to dual energy X-ray chemical imaging techniques. The effects of the inclination angle and the imaging angle range were evaluated at ambient pressure using the apparatus. Sectional images of ruby ball samples were successfully reconstructed at high pressures, up to approximately 50 GPa. The high-pressure in situ X-ray laminography technique is expected to provide new insights into the deep Earth sciences. PMID:27131721

  17. Methodology toward 3D micro X-ray fluorescence imaging using an energy dispersive charge-coupled device detector.

    PubMed

    Garrevoet, Jan; Vekemans, Bart; Tack, Pieter; De Samber, Björn; Schmitz, Sylvia; Brenker, Frank E; Falkenberg, Gerald; Vincze, Laszlo

    2014-12-01

    A new three-dimensional (3D) micro X-ray fluorescence (μXRF) methodology based on a novel 2D energy dispersive CCD detector has been developed and evaluated at the P06 beamline of the Petra-III storage ring (DESY) in Hamburg, Germany. This method is based on the illumination of the investigated sample cross-section by a horizontally focused beam (vertical sheet beam) while fluorescent X-rays are detected perpendicularly to the sheet beam by a 2D energy dispersive (ED) CCD detector allowing the collection of 2D cross-sectional elemental images of a certain depth within the sample, limited only by signal self-absorption effects. 3D elemental information is obtained by a linear scan of the sample in the horizontal direction across the vertically oriented sheet beam and combining the detected cross-sectional images into a 3D elemental distribution data set. Results of the 3D μXRF analysis of mineral inclusions in natural deep Earth diamonds are presented to illustrate this new methodology. PMID:25346101

  18. Total reflection X-ray fluorescence and energy-dispersive X-ray fluorescence analysis of runoff water and vegetation from abandoned mining of Pb Zn ores

    NASA Astrophysics Data System (ADS)

    Marques, A. F.; Queralt, I.; Carvalho, M. L.; Bordalo, M.

    2003-12-01

    The present work reports on the heavy metal content: Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Cd and Pb in running waters and vegetation around abandoned mining areas. Two species of mosses ( Dicranum sp. and Pleurocarpus sp.) and three different species of wild grass ( Bromus sp., Rumex sp. and Pseudoavena sp.) growing on the surrounding areas of old lead-zinc mines (Aran Valley, Pyrenees, NE Spain) have been analyzed. Both water and vegetation were collected in two different sampling places: (a) near the mine gallery water outlets and (b) on the landfill close to the abandoned mineral concentration factories. For the heavy metal content determination, two different techniques were used: total reflection X-ray fluorescence for water analysis and energy-dispersive X-ray fluorescence for vegetation study. Surface waters around mine outlets exhibit anomalous content of Co, Ni, Zn, Cd. Stream waters running on mining landfills exhibit higher Cu, Zn, Cd and Pb than those of the waters at the mine gallery outlets. The results allow us to assess the extent of the environmental impact of the mining activities on the water quality. The intake of these elements by vegetation was related with the sampling place, reflecting the metal water content and the substrate chemistry. Accumulation of metals in mosses is higher than those exhibited in wild grasses. Furthermore, different levels of accumulation were found in different wild grass. Rumex sp. presented the lowest metal concentrations, while Pseudoavena sp. reported the highest metal content.

  19. Design and Performance of a TES X-ray Microcalorimeter Array for Energy Dispersive Spectroscopy on Scanning Transmission Electron Microscope

    NASA Astrophysics Data System (ADS)

    Muramatsu, Haruka; Nagayoshi, K.; Hayashi, T.; Sakai, K.; Yamamoto, R.; Mitsuda, K.; Yamasaki, N. Y.; Maehata, K.; Hara, T.

    2016-02-01

    We discuss the design and performance of a transition edge sensor (TES) X-ray microcalorimeter array for scanning transmission electron microscope (STEM)-energy dispersive X-ray spectroscopy (EDS). The TES X-ray microcalorimeter has better energy resolution compared to conventional silicon drift detector and STEM-EDS utilizing a TES detector makes it possible to map the distribution of elements on a specimen in addition to analyze the composition. The requirement for a TES detector is a high counting rate (> 20 kcps), wide energy band (0.5-15 keV) and good energy resolution (< 10 eV) full width at half maximum. The major improvement of this development is to increase the maximum counting rate. In order to accommodate the high counting rate, we adopted an 8 × 8 format, 64-pixel array and common biasing scheme for the readout method. We did all design and fabrication of the device in house. With the device we have fabricated most recently, the pulse decay time is 40 \\upmu s which is expected to achieve 50 kcps. For a single pixel, the measured energy resolution was 7.8 eV at 5.9 keV. This device satisfies the requirements of counting rate and energy resolution, although several issues remain where the performance must be confirmed.

  20. Design and Performance of a TES X-ray Microcalorimeter Array for Energy Dispersive Spectroscopy on Scanning Transmission Electron Microscope

    NASA Astrophysics Data System (ADS)

    Muramatsu, Haruka; Nagayoshi, K.; Hayashi, T.; Sakai, K.; Yamamoto, R.; Mitsuda, K.; Yamasaki, N. Y.; Maehata, K.; Hara, T.

    2016-07-01

    We discuss the design and performance of a transition edge sensor (TES) X-ray microcalorimeter array for scanning transmission electron microscope (STEM)-energy dispersive X-ray spectroscopy (EDS). The TES X-ray microcalorimeter has better energy resolution compared to conventional silicon drift detector and STEM-EDS utilizing a TES detector makes it possible to map the distribution of elements on a specimen in addition to analyze the composition. The requirement for a TES detector is a high counting rate (>20 kcps), wide energy band (0.5-15 keV) and good energy resolution (<10 eV) full width at half maximum. The major improvement of this development is to increase the maximum counting rate. In order to accommodate the high counting rate, we adopted an 8 × 8 format, 64-pixel array and common biasing scheme for the readout method. We did all design and fabrication of the device in house. With the device we have fabricated most recently, the pulse decay time is 40 μs which is expected to achieve 50 kcps. For a single pixel, the measured energy resolution was 7.8 eV at 5.9 keV. This device satisfies the requirements of counting rate and energy resolution, although several issues remain where the performance must be confirmed.

  1. Design and Performance of a TES X-ray Microcalorimeter Array for Energy Dispersive Spectroscopy on Scanning Transmission Electron Microscope

    NASA Astrophysics Data System (ADS)

    Muramatsu, Haruka; Nagayoshi, K.; Hayashi, T.; Sakai, K.; Yamamoto, R.; Mitsuda, K.; Yamasaki, N. Y.; Maehata, K.; Hara, T.

    2016-07-01

    We discuss the design and performance of a transition edge sensor (TES) X-ray microcalorimeter array for scanning transmission electron microscope (STEM)-energy dispersive X-ray spectroscopy (EDS). The TES X-ray microcalorimeter has better energy resolution compared to conventional silicon drift detector and STEM-EDS utilizing a TES detector makes it possible to map the distribution of elements on a specimen in addition to analyze the composition. The requirement for a TES detector is a high counting rate (>20 kcps), wide energy band (0.5-15 keV) and good energy resolution (<10 eV) full width at half maximum. The major improvement of this development is to increase the maximum counting rate. In order to accommodate the high counting rate, we adopted an 8 × 8 format, 64-pixel array and common biasing scheme for the readout method. We did all design and fabrication of the device in house. With the device we have fabricated most recently, the pulse decay time is 40 \\upmu s which is expected to achieve 50 kcps. For a single pixel, the measured energy resolution was 7.8 eV at 5.9 keV. This device satisfies the requirements of counting rate and energy resolution, although several issues remain where the performance must be confirmed.

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

    NASA Astrophysics Data System (ADS)

    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.

  3. Electrochemical in-situ reaction cell for X-ray scattering, diffraction and spectroscopy

    SciTech Connect

    Braun, Artur; Granlund, Eric; Cairns, Elton J.

    2003-01-27

    An electrochemical in-situ reaction cell for hard X-ray experiments with battery electrodes is described. Applications include the small angle scattering, diffraction, and near-edge spectroscopy of lithium manganese oxide electrodes.

  4. Detector solid angle formulas for use in x-ray energy dispersive spectrometry.

    SciTech Connect

    Zaluzec, N. J.; Materials Science Division

    2009-01-01

    With the advent of silicon drift X-ray detectors, a range of new geometries has become possible in electron optical columns. Because of their compact size, these detectors can potentially achieve high geometrical collection efficiencies; however, using traditional approximations detector solid angle calculations rapidly break down and at times can yield nonphysical values. In this article we present generalized formulas that can be used to calculate the variation in detection solid angle for contemporary Si(Li) as well as new silicon drift configurations.

  5. Measurement of Trace Constituents by Electron-Excited X-Ray Microanalysis with Energy-Dispersive Spectrometry.

    PubMed

    Newbury, Dale E; Ritchie, Nicholas W M

    2016-06-01

    Electron-excited X-ray microanalysis performed with scanning electron microscopy and energy-dispersive spectrometry (EDS) has been used to measure trace elemental constituents of complex multielement materials, where "trace" refers to constituents present at concentrations below 0.01 (mass fraction). High count spectra measured with silicon drift detector EDS were quantified using the standards/matrix correction protocol embedded in the NIST DTSA-II software engine. Robust quantitative analytical results for trace constituents were obtained from concentrations as low as 0.000500 (mass fraction), even in the presence of significant peak interferences from minor (concentration 0.01≤C≤0.1) and major (C>0.1) constituents. Limits of detection as low as 0.000200 were achieved in the absence of peak interference. PMID:27329308

  6. Energy dispersive X-ray spectroscopy analysis of Si sidewall surface etched by deep-reactive ion etching

    NASA Astrophysics Data System (ADS)

    Matsutani, Akihiro; Nishioka, Kunio; Sato, Mina

    2016-06-01

    We investigated the composition of a passivation film on a sidewall etched by deep-reactive ion etching (RIE) using SF6/O2 and C4F8 plasma, by energy-dispersive X-ray (EDX) spectroscopy. It was found that the compositions of carbon and fluorine in the passivation film on the etched sidewall depend on the width and depth of the etched trench. It is important to understand both the plasma behavior and the passivation film composition to carry out fabrication by deep-RIE. We consider that these results of the EDX analysis of an etched sidewall will be useful for understanding plasma behavior in order to optimize the process conditions of deep-RIE.

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

    SciTech Connect

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

    1989-03-01

    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.

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

    SciTech Connect

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

    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.

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

    NASA Astrophysics Data System (ADS)

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

    2015-08-01

    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

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

    USGS Publications Warehouse

    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.

  11. Electron probe energy dispersive X-ray microanalysis (EDXA) in the investigation of fossil bone: the case of Java man.

    PubMed

    Bartsiokas, A; Day, M H

    1993-05-22

    Doubts about the attribution of the Trinil femur to Homo erectus on anatomical grounds have a long history. Here, for the first time, published stratigraphic information and chemical evidence based on the Ca/P ratios confirm that the anatomical doubts are justified. The Trinil femur apparently belongs to a more recent stratum above the 'fossil layer' (Hauptknochenschicht, HK) in which the Trinil calotte was found. It is concluded that the Trinil Femur I belongs to Homo sapiens, whereas the Trinil Femora II-V and the calotte belong to H. erectus. The chemical evidence derives from the use of electron probe energy dispersive X-ray microanalysis (EDXA), a technique that can be virtually non-destructive and therefore may be used on scarce fossil evidence. PMID:8391701

  12. Energy dispersive x-ray analysis of the cornea. Application to paraffin sections of normal and diseased corneas

    SciTech Connect

    Robinson, M.R.; Streeten, B.W.

    1984-11-01

    The distribution of chemical elements in the normal human cornea was studied by energy dispersive x-ray analysis and scanning electron microscopy of routinely prepared paraffin sections. Calcium, phosphorus, and sulfur were consistently present in quantities above background and varied in concentration regionally. Analysis of fresh-frozen tissue, an approximation of the in vivo state, gave a similar elemental profile to paraffin sections, except for the loss of diffusable electrolytes in the latter. After fixation, S was the most abundant element and was highest in Descemet's membrane. Corneas with granular, lattice, macular, and Fuchs endothelial dystrophies, band keratopathy, and spheroidal degeneration were also examined. Characteristic patterns of abnormal S and Ca distribution were found in each of the dystrophies. The relative proportions of Ca, P, and S gave diagnostic profiles for distinguishing band keratopathy and spheroidal degeneration.

  13. Non-destructive analysis of didymium and praseodymium molybdate crystals using energy dispersive X-ray fluorescence technique

    NASA Astrophysics Data System (ADS)

    Bhat, C. K.; Joseph, Daisy; Pandita, Sanjay; Kotru, P. N.

    2016-08-01

    Analysis of didymium (Di) and praseodymium molybdate crystals were carried out using energy dispersive X-ray fluorescence (EDXRF). The assigned empirical chemical formulae of the composites were tested and verified by the EDXRF technique by estimating experimental major elemental concentration ratios. On the Basis of these ratios, the established formulae for some of the composite materials have been verified and suggestions made for their refinement. Non-destructive technique used in this analysis enables to retain the original crystal samples and makes rapid simultaneous scan of major elements such as La, Pr, Ned and Mo as well as impurities such as Ce. Absence of samarium(Sm) in the spectrum during analysis of didymium molybdate crystals indicated an incomplete growth of mixed rare earth single crystal. These crystals (e.g.,Di) are shown to be of modified stoichiometry with Ce as trace impurity.

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

    PubMed

    Smith, Kevin T; Balouet, Jean Christophe; Shortle, Walter C; Chalot, Michel; Beaujard, François; Grudd, Håkan; Vroblesky, Don A; Burken, 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. PMID:24034830

  15. Energy-dispersive X-ray diffraction using an annular beam.

    PubMed

    Dicken, A J; Evans, J P O; Rogers, K D; Greenwood, C; Godber, S X; Prokopiou, D; Stone, N; Clement, J G; Lyburn, I; Martin, R M; Zioupos, P

    2015-05-18

    We demonstrate material phase identification by measuring polychromatic diffraction spots from samples at least 20 mm in diameter and up to 10 mm thick with an energy resolving point detector. Within our method an annular X-ray beam in the form of a conical shell is incident with its symmetry axis normal to an extended polycrystalline sample. The detector is configured to receive diffracted flux transmitted through the sample and is positioned on the symmetry axis of the annular beam. We present the experiment data from a range of different materials and demonstrate the acquisition of useful data with sub-second collection times of 0.5 s; equating to 0.15 mAs. Our technique should be highly relevant in fields that demand rapid analytical methods such as medicine, security screening and non-destructive testing. PMID:26074592

  16. Energy dispersive X-ray microanalysis, fluoride release, and antimicrobial properties of glass ionomer cements indicated for atraumatic restorative treatment

    PubMed Central

    Saxena, Sudhanshu; Tiwari, Sonia

    2016-01-01

    Aim: The aim of this study was to compare constituents of glass powder, fluoride release, and antimicrobial properties of new atraumatic restorative treatment material with zirconia fillers and conventional glass ionomer cement (GIC) type IX. Materials and Methods: Thisin vitro study comparing Zirconomer and Fuji IX was executed in three parts: (1) energy dispersive X-ray microanalysis of glass powders (2) analysis of fluoride release at 1st, 3rd, 7th, 15th, and 30th day, and (3) antimicrobial activity against Streptococcus mutans, Lactobacillus casei, and Candida albicans at 48 hours. Data was analyzed using unpaired t-test and two way analysis of variance followed by least significant difference post hoc test. A P value of < 0.05 was considered statistically significant. Results: Energy dispersive X-ray microanalysis revealed that, in both Zirconomer and Fuji IX glass powders, mean atomic percentage of oxygen was more than 50%. According to the weight percentage, zirconium in Zirconomer and silica in Fuji IX were the second main elements. Calcium, zinc, and zirconium were observed only in Zirconomer. At all the time intervals, statistically significant higher amount of fluoride release was observed with Zirconomer than Fuji IX. At 48 hours, mean ± standard deviation (SD) of zone of inhibition against Streptococcus mutans was 11.14 ± 0.77 mm and 8.51 ± 0.43 mm for Zirconomer and Fuji IX, respectively. Against Lactobacillus casei, it was 14.06 ± 0.71 mm for Zirconomer and 11.70 ± 0.39 mm for Fuji IX. No antifungal activity was observed against Candida albicans by Zirconomer and Fuji IX. Conclusion: Zirconomer had higher antibacterial activity against Streptococcus mutans and Lactobacillus casei, which may be attributed to its composition and higher fluoride release. However, it failed to show antifungal effect againstCandida albicans. PMID:27583226

  17. Energy dispersive X-ray analysis of titanium dioxide nanoparticle distribution after intravenous and subcutaneous injection in mice.

    PubMed

    Patri, Anil; Umbreit, Thomas; Zheng, J; Nagashima, K; Goering, Peter; Francke-Carroll, Sabine; Gordon, Edward; Weaver, James; Miller, Terry; Sadrieh, Nakissa; McNeil, Scott; Stratmeyer, Mel

    2009-11-01

    In an effort to understand the disposition and toxicokinetics of nanoscale materials, we used EDS (energy dispersive X-ray spectroscopy) to detect and map the distribution of titanium dioxide (TiO2) in tissue sections from mice following either subcutaneous (s.c.) or intravenous (i.v.) injection. TiO2 nanoparticles were administered at a dose of 560 mg/kg (i.v.) or 5600 mg/kg (s.c.) to Balb/c female mice on two consecutive days. Tissues (liver, kidney, lung, heart, spleen, and brain) were examined by light microscopy, TEM (transmission electron microscopy), SEM (scanning electron microscopy), and EDS following necropsy one day after treatment. Particle agglomerates were detected by light microscopy in all tissues examined, EDS microanalysis was used to confirm that these tissues contained elemental titanium and oxygen. The TEM micrographs and EDS spectra of the aggregates were compared with in vitro measurements of TiO2 nanoparticle injection solution (i.e., in water). The nanoparticles were also characterized using dynamic light scattering in water, 10 mM NaCl, and phosphate buffered saline (PBS). In low ionic strength solvents (water and 10 mM NaCl), the TiO2 particles had average hydrodynamic diameters ranging from 114-122 nm. In PBS, however, the average diameter increases to 1-2 microm, likely due to aggregation analogous to that observed in tissue by TEM and EDS. This investigation demonstrates the suitability of energy dispersive X-ray spectroscopy (EDS) for detection of nanoparticle aggregates in tissues and shows that disposition of TiO2 nanoparticles depends on the route of administration (i.v. or s.c.). PMID:19626582

  18. Determination of selenium at trace levels in geologic materials by energy-dispersive X-ray fluorescence spectrometry

    USGS Publications Warehouse

    Wahlberg, J.S.

    1981-01-01

    Low levels of selenium (0.1-500 ppm) in both organic and inorganic geologic materials can be semiquantitatively measured by isolating Se as a thin film for presentation to an energy-dispersive X-ray fluorescence spectrometer. Suitably pulverized samples are first digested by fusing with a mixture of Na2CO3 and Na2O2. The fusion cake is dissolved in distilled water, buffered with NH4Cl, and filtered to remove Si and the R2O3 group. A carrier solution of Na2TeO4, plus solid KI, hydrazine sulfate and Na2SO3, is added to the filtrate. The solution is then vacuum-filtered through a 0.45-??m pore-size filter disc. The filter, with the thin film of precipitate, is supported between two sheets of Mylar?? film for analysis. Good agreement is shown between data reported in this study and literature values reported by epithermal neutron-activation analysis and spectrofluorimetry. The method can be made quantitative by utilizing a secondary precipitation to assure complete recovery of the Se. The X-ray method offers fast turn-around time and a reasonably high production rate. ?? 1981.

  19. In situ/operando soft x-ray spectroscopy characterization of ion solvation and catalysis

    NASA Astrophysics Data System (ADS)

    Liu, Yi-Sheng; Guo, Jinghua

    Many important systems especially in energy-related regime are based on the complexity of material architecture, chemistry and interactions among constituents within. To understand and thus ultimately control the varying applications calls for in-situ/operando characterization tools. We will present the recent development of the in-situ/operando soft X-ray spectroscopic in the studies of catalytic and alkali ion solvation under bias condition, and reveal how to overcome the challenge that soft X-rays cannot easily peek into the high-pressure catalytic cells or liquid electrochemical cells. Also the different feasible detection approaches can provide surface and bulk sensitivity experimentally from those in-situ cells. The unique design of in-situ/operando soft X-ray spectroscopy instrumentation and fabrication principle with examples in Ca, Na, Mg based solutions at ambient pressure/temperature and high temperature (~250°C) gas catalysis will be shown.

  20. Scanning force microscope for in situ nanofocused X-ray diffraction studies

    PubMed Central

    Ren, Zhe; Mastropietro, Francesca; Davydok, Anton; Langlais, Simon; Richard, Marie-Ingrid; Furter, Jean-Jacques; Thomas, Olivier; Dupraz, Maxime; Verdier, Marc; Beutier, Guillaume; Boesecke, Peter; Cornelius, Thomas W.

    2014-01-01

    A compact scanning force microscope has been developed for in situ combination with nanofocused X-ray diffraction techniques at third-generation synchrotron beamlines. Its capabilities are demonstrated on Au nano-islands grown on a sapphire substrate. The new in situ device allows for in situ imaging the sample topography and the crystallinity by recording simultaneously an atomic force microscope (AFM) image and a scanning X-ray diffraction map of the same area. Moreover, a selected Au island can be mechanically deformed using the AFM tip while monitoring the deformation of the atomic lattice by nanofocused X-ray diffraction. This in situ approach gives access to the mechanical behavior of nanomaterials. PMID:25178002

  1. Gold nephropathy. Ultrastructural, fluorescent, and energy-dispersive x-ray microanalysis study

    SciTech Connect

    Ainsworth, S.K.; Swain, R.P.; Watabe, N.; Brackett, N.C. Jr.; Pilia, P.; Hennigar, G.R.

    1981-07-01

    The nephrotic syndrome developed in a patient receiving therapy with gold for rheumatoid arthritis. The results of a histopathological examination of the renal biopsy specimen were unremarkable. Immunofluorescent studies showed deposits of immunoglobulins and C3 in a granular pattern in the glomerular basement membranes. Ultrastructurally, the discrete osmiophilic immune complexes were epimembranous. By x-ray microanalysis, gold that was complexed with sulfur was present in proximal tubular cytoplasmic vacuoles and nuclei. Gold and sulfur could not be demonstrated in glomerular epimembranous deposits. The results of these studies suggest that immune complex deposition does not involve gold and sulfur acting as haptens. Gold-salt therapy may result in damage to proximal tubules that leak renal tubular antigens, which in turn complex with autoantibody and produce an autoimmune membranous nephropathy. The evidence for this mechanism is not convincing. Although the data indicate an immune-complex cause for gold-salt nephropathy, the incident antigen (or antigens) and mechanism of action remain unidentified.

  2. Effect of x-ray energy dispersion in digital subtraction imaging at the iodine K-edge--A Monte Carlo study

    SciTech Connect

    Prino, F.; Ceballos, C.; Cabal, A.; Sarnelli, A.; Gambaccini, M.; Ramello, L.

    2008-01-15

    The effect of the energy dispersion of a quasi-monochromatic x-ray beam on the performance of a dual-energy x-ray imaging system is studied by means of Monte Carlo simulations using MCNPX (Monte Carlo N-Particle eXtended) version 2.6.0. In particular, the case of subtraction imaging at the iodine K-edge, suitable for angiographic imaging application, is investigated. The average energies of the two beams bracketing the iodine K-edge are set to the values of 31.2 and 35.6 keV corresponding to the ones obtained with a compact source based on a conventional x-ray tube and a mosaic crystal monochromator. The energy dispersion of the two beams is varied between 0 and 10 keV of full width at half-maximum (FWHM). The signal and signal-to-noise ratio produced in the simulated images by iodine-filled cavities (simulating patient vessels) drilled in a PMMA phantom are studied as a function of the x-ray energy dispersion. The obtained results show that, for the considered energy separation of 4.4 keV, no dramatic deterioration of the image quality is observed with increasing x-ray energy dispersion up to a FWHM of about 2.35 keV. The case of different beam energies is also investigated by means of fast simulations of the phantom absorption.

  3. Electrochemical cell for in-situ x-ray characterization

    SciTech Connect

    Doughty, D.H.; Ingersoll, D.; Rodriguez, M.A.

    1998-08-04

    An electrochemical cell suitable for in-situ XRD analysis is presented. Qualitative information such as phase formation and phase stability can be easily monitored using the in-situ cell design. Quantitative information such as lattice parameters and kinetic behavior is also straightforward. Analysis of the LiMn&sub2;O&sub4; spinel using this cell design shows that the lattice undergoes two major structural shrinkages at approx. 4.0 V and approx. 4.07 V during charging. These shrinkages correlate well with the two electrochemical waves observed and indicate the likelihood of two separate redox processes which charging and discharging.

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

    NASA Astrophysics Data System (ADS)

    Bottaini, C.; Mirão, J.; Figuereido, M.; Candeias, A.; Brunetti, A.; Schiavon, N.

    2015-01-01

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

  5. In situ X-ray microprobe study of salt layers during anodic dissolution of stainless steel in chloride solution

    SciTech Connect

    Isaacs, H.S.; Cho, J.H.; Rivers, M.L.; Sutton, S.R.

    1995-04-01

    Salt layers play an important role in many electrochemical dissolution processes. The composition of salt films formed on austenitic stainless steel have, for the first time, been determined using in situ energy dispersive X-ray fluorescence microanalysis during dissolution in a chloride solution. The electrode was the cross section of a nickel/chromium steel foil sandwiched between plastic sheets. The foil was electrochemically dissolved producing a pit 1.6 mm deep. The electrode configuration simulated localized corrosion with a one-dimensional diffusion geometry. X-ray fluorescence intensities of chromium K{sub {alpha}}, iron K{sub {alpha}}, an nickel K{sub {beta}} energies were measured as the steel/solution interface traversed a 6 {mu}m, polychromatic, high-intensity X-ray beam. Qualitative determinations were made of the composition of the salt layer and the composition of the saturated solution. Salt layer thickness was found to increase with increased applied potentials. The salt layer was found to be rich in iron and depleted in nickel and, particularly, chromium. The effective diffusion coefficients of the dissolved species were determined from the composition of the saturated solution at the interface. Nickel showed the highest and chromium the lowest effective diffusion coefficient.

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

    NASA Astrophysics Data System (ADS)

    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.

  7. An atomic layer deposition chamber for in situ x-ray diffraction and scattering analysis

    SciTech Connect

    Geyer, Scott M.; Methaapanon, Rungthiwa; Kim, Woo-Hee; Bent, Stacey F.; Johnson, Richard W.; Van Campen, Douglas G.; Metha, Apurva

    2014-05-15

    The crystal structure of thin films grown by atomic layer deposition (ALD) will determine important performance properties such as conductivity, breakdown voltage, and catalytic activity. We report the design of an atomic layer deposition chamber for in situ x-ray analysis that can be used to monitor changes to the crystal structural during ALD. The application of the chamber is demonstrated for Pt ALD on amorphous SiO{sub 2} and SrTiO{sub 3} (001) using synchrotron-based high resolution x-ray diffraction, grazing incidence x-ray diffraction, and grazing incidence small angle scattering.

  8. DIBENZYLAMMONIUM AND SODIUM DIBENZYLDITHIOCARBAMATES AS PRECIPITANTS FOR PRECONCENTRATION OF TRACE ELEMENTS IN WATER FOR ANALYSIS BY ENERGY DISPERSIVE X-RAY FLUORESCENCE

    EPA Science Inventory

    Precipitation with combined dibenzylammonium dibenzyldithiocarbamate and sodium dibenzyldithiocarbamate at pH 5.0 can be used to separate 22 trace elements from water. Membrane filtration on the precipitate yielded a thin sample, suitable for analysis by energy dispersive X-ray f...

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

    DOEpatents

    Gibson, David M.; Gibson, Walter M.; Huang, Huapeng

    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.

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

    SciTech Connect

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

    2014-07-21

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

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

    NASA Astrophysics Data System (ADS)

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

    2014-07-01

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

  12. In-situ observations of catalytic surface reactions with soft x-rays under working conditions

    NASA Astrophysics Data System (ADS)

    Toyoshima, Ryo; Kondoh, Hiroshi

    2015-03-01

    Catalytic chemical reactions proceeding on solid surfaces are an important topic in fundamental science and industrial technologies such as energy conversion, pollution control and chemical synthesis. Complete understanding of the heterogeneous catalysis and improving its efficiency to an ultimate level are the eventual goals for many surface scientists. Soft x-ray is one of the prime probes to observe electronic and structural information of the target materials. Most studies in surface science using soft x-rays have been performed under ultra-high vacuum conditions due to the technical limitation, though the practical catalytic reactions proceed under ambient pressure conditions. However, recent developments of soft x-ray based techniques operating under ambient pressure conditions have opened a door to the in-situ observation of materials under realistic environments. The near-ambient-pressure x-ray photoelectron spectroscopy (NAP-XPS) using synchrotron radiation enables us to observe the chemical states of surfaces of condensed matters under the presence of gas(es) at elevated pressures, which has been hardly conducted with the conventional XPS technique. Furthermore, not only the NAP-XPS but also ambient-pressure compatible soft x-ray core-level spectroscopies, such as near-edge absorption fine structure (NEXAFS) and x-ray emission spectroscopy (XES), have been significantly contributing to the in-situ observations. In this review, first we introduce recent developments of in-situ observations using soft x-ray techniques and current status. Then we present recent new findings on catalytically active surfaces using soft x-ray techniques, particularly focusing on the NAP-XPS technique. Finally we give a perspective on the future direction of this emerging technique.

  13. Exposure and analysis of microparticles embedded in silica aerogel keystones using NF3-mediated electron beam-induced etching and energy-dispersive X-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Martin, Aiden A.; Lin, Ting; Toth, Milos; Westphal, Andrew J.; Vicenzi, Edward P.; Beeman, Jeffrey; Silver, Eric H.

    2016-07-01

    In 2006, NASA's Stardust spacecraft delivered to Earth dust particles collected from the coma of comet 81P/Wild 2, with the goal of furthering the understanding of solar system formation. Stardust cometary samples were collected in a low-density, nanoporous silica aerogel making their study technically challenging. This article demonstrates the identification, exposure, and elemental composition analysis of particles analogous to those collected by NASA's Stardust mission using in-situ SEM techniques. Backscattered electron imaging is shown by experimental observation and Monte Carlo simulation to be suitable for locating particles of a range of sizes relevant to Stardust (down to submicron diameters) embedded within silica aerogel. Selective removal of the silica aerogel encapsulating an embedded particle is performed by cryogenic NF3-mediated electron beam-induced etching. The porous, low-density nature of the aerogel results in an enhanced etch rate compared with solid material, making it an effective, nonmechanical method for the exposure of particles. After exposure, elemental composition of the particle was analyzed by energy-dispersive X-ray spectroscopy using a high spectral resolution microcalorimeter. Signals from fluorine contamination are shown to correspond to nonremoved silica aerogel and only in residual concentrations.

  14. Exposure and analysis of microparticles embedded in silica aerogel keystones using NF3-mediated electron beam-induced etching and energy-dispersive X-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Martin, Aiden A.; Lin, Ting; Toth, Milos; Westphal, Andrew J.; Vicenzi, Edward P.; Beeman, Jeffrey; Silver, Eric H.

    2016-04-01

    In 2006, NASA's Stardust spacecraft delivered to Earth dust particles collected from the coma of comet 81P/Wild 2, with the goal of furthering the understanding of solar system formation. Stardust cometary samples were collected in a low-density, nanoporous silica aerogel making their study technically challenging. This article demonstrates the identification, exposure, and elemental composition analysis of particles analogous to those collected by NASA's Stardust mission using in-situ SEM techniques. Backscattered electron imaging is shown by experimental observation and Monte Carlo simulation to be suitable for locating particles of a range of sizes relevant to Stardust (down to submicron diameters) embedded within silica aerogel. Selective removal of the silica aerogel encapsulating an embedded particle is performed by cryogenic NF3-mediated electron beam-induced etching. The porous, low-density nature of the aerogel results in an enhanced etch rate compared with solid material, making it an effective, nonmechanical method for the exposure of particles. After exposure, elemental composition of the particle was analyzed by energy-dispersive X-ray spectroscopy using a high spectral resolution microcalorimeter. Signals from fluorine contamination are shown to correspond to nonremoved silica aerogel and only in residual concentrations.

  15. Atomic-scale chemical imaging and quantification of metallic alloy structures by energy-dispersive X-ray spectroscopy.

    PubMed

    Lu, Ping; Zhou, Lin; Kramer, M J; Smith, David J

    2014-01-01

    Determination of atomic-scale crystal structure for nanostructured intermetallic alloys, such as magnetic alloys containing Al, Ni, Co (alnico) and Fe, is crucial for understanding physical properties such as magnetism, but technically challenging due to the small interatomic distances and the similar atomic numbers. By applying energy-dispersive X-ray spectroscopy (EDS) mapping to the study of two intermetallic phases of an alnico alloy resulting from spinodal decomposition, we have determined atomic-scale chemical composition at individual lattice sites for the two phases: one is the B2 phase with Fe0.76Co0.24 -Fe0.40Co0.60 ordering and the other is the L2(1) phase with Ni0.48Co0.52 at A-sites, Al at B(Ι)-sites and Fe0.20Ti0.80 at B(ΙΙ)-sites, respectively. The technique developed through this study represents a powerful real-space approach to investigate structure chemically at the atomic scale for a wide range of materials systems. PMID:24492747

  16. NASA Li/CF(x) cell problem analysis: Scanning electron microscopy with energy dispersive x ray spectrometry

    NASA Technical Reports Server (NTRS)

    Baker, John

    1991-01-01

    An analysis was made of Lithium/carbon fluoride cell parts for possible chloride contamination induced by exposure to thionyl chloride (SOCl2); various samples were submitted for analysis. Only a portion of the analysis which has been conducted is covered, herein, namely analysis by scanning electron microscopy with energy dispersive x ray spectrometry (SEM/EDS). A strip of nickel was exposed to SOCl2 vapors to observe variations in surface concentrations of sulfur and chlorine with time. By detecting chlorine one can not infer contamination by SOCl2 only that contamination is present. Six samples of stainless steel foil were analyzed for chlorine using EDS. Chlorine was not detected on background samples but was detected on the samples which had been handled including those which had been cleaned. Cell covers suspected of being contaminated while in storage and covers which were not exposed to the same storage conditions were analyzed for chlorine. Although no chlorine was found on the covers from cells, it was found on all stored covers. Results are presented with techniques shown for analysis and identification. Relevant photomicrographs are presented.

  17. Distribution of toxic elements in teeth treated with amalgam using μ-energy dispersive X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Guerra, M.; Ferreira, C.; Carvalho, M. L.; Santos, J. P.; Pessanha, S.

    2016-08-01

    Over the years, the presence of mercury in amalgam fillings has raised some safety concerns. Amalgam is one of the most commonly used tooth fillings and contains approximately 50% of elemental mercury and 50% of other metals, mostly silver, tin and copper. Amalgam can release small amounts of mercury vapor over time, and patients can absorb these vapors by inhaling or ingesting them. In this study, 10 human teeth treated with dental amalgam were analyzed using energy dispersive X-ray fluorescence (EDXRF) to study the diffusion of its constituents, Ag, Cu, Sn and Hg. The used EDXRF setup, makes use of a polycapillary lens to focus radiation up to 25 μm allowing the mapping of the elemental distribution in the samples. Quantification was performed using the inbuilt software based on the Fundamental Parameters method for bulk samples, considering a hydroxyapatite matrix. The teeth were longitudinally cut and each slice was scanned from the surface enamel to the inner region (dentin and pulp cavity). Mercury concentration profiles show strong levels of this element close to the amalgam region, decreasing significantly in the dentin, and increasing again up to 40,000 μg·g- 1 in the cavity were the pulp used to exist when the tooth was vital.

  18. Atomic-scale Chemical Imaging and Quantification of Metallic Alloy Structures by Energy-Dispersive X-ray Spectroscopy

    PubMed Central

    Lu, Ping; Zhou, Lin; Kramer, M. J.; Smith, David J.

    2014-01-01

    Determination of atomic-scale crystal structure for nanostructured intermetallic alloys, such as magnetic alloys containing Al, Ni, Co (alnico) and Fe, is crucial for understanding physical properties such as magnetism, but technically challenging due to the small interatomic distances and the similar atomic numbers. By applying energy-dispersive X-ray spectroscopy (EDS) mapping to the study of two intermetallic phases of an alnico alloy resulting from spinodal decomposition, we have determined atomic-scale chemical composition at individual lattice sites for the two phases: one is the B2 phase with Fe0.76Co0.24 -Fe0.40Co0.60 ordering and the other is the L21 phase with Ni0.48Co0.52 at A-sites, Al at BΙ-sites and Fe0.20Ti0.80 at BΙΙ-sites, respectively. The technique developed through this study represents a powerful real-space approach to investigate structure chemically at the atomic scale for a wide range of materials systems. PMID:24492747

  19. Scanning Electron Microscopy Findings With Energy-Dispersive X-ray Investigations of Cosmetically Tinted Contact Lenses

    PubMed Central

    Hotta, Fumika; Imai, Shoji; Miyamoto, Tatsuro; Mitamura-Aizawa, Sayaka; Mitamura, Yoshinori

    2015-01-01

    Objective: To investigate the surfaces and principal elements of the colorants of cosmetically tinted contact lenses (Cos-CLs). Methods: We analyzed the surfaces and principal elements of the colorants of five commercially available Cos-CLs using scanning electron microscopy with energy-dispersive x-ray analysis. Results: In two Cos-CLs, the anterior and posterior surfaces were smooth, and colorants were found inside the lens. One lens showed colorants located to a depth of 8 to 14 μm from the anterior side of the lens. In the other lens, colorants were found in the most superficial layer on the posterior surface, although a coated layer was observed. The colorants in the other three lenses were deposited on either lens surface. Although a print pattern was uniform in embedded type lenses, uneven patterns were apparent in dot-matrix design lenses. Colorants used in all lenses contained chlorine, iron, and titanium. In the magnified scanning electron microscopy images of a certain lens, chlorine is exuded and spread. Conclusions: Cosmetically tinted contact lenses have a wide variety of lens surfaces and colorants. Colorants may be deposited on the lens surface and consist of an element that has tissue toxicity. PMID:25799458

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

    SciTech Connect

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

    2007-11-15

    An in situ x-ray diffraction (XRD) setup is designed and installed in the materials science beam line of the Pelletron accelerator at the Inter-University Accelerator Centre for in situ studies of phase change in swift heavy ion irradiated materials. A high vacuum chamber with suitable windows for incident and diffracted X-rays is integrated with the goniometer and the beamline. Indigenously made liquid nitrogen (LN{sub 2}) temperature sample cooling unit is installed. The snapshots of growth of particles with fluence of 90 MeV Ni ions were recorded using in situ XRD experiment, illustrating the potential of this in situ facility. A thin film of C{sub 60} was used to test the sample cooling unit. It shows that the phase of the C{sub 60} film transforms from a cubic lattice (at room temperature) to a fcc lattice at around T=255 K.

  1. Probing electrode/electrolyte interfaces in situ by X-ray spectroscopies: old methods, new tricks.

    PubMed

    Wu, Cheng Hao; Weatherup, Robert S; Salmeron, Miquel B

    2015-11-11

    Electrode/electrolyte interfaces play a vital role in various electrochemical systems, but in situ characterization of such buried interfaces remains a major challenge. Several efforts to develop techniques or to modify existing techniques to study such interfaces are showing great promise to overcome this challenge. Successful examples include electrochemical scanning tunneling microscopy (EC-STM), surface-sensitive vibrational spectroscopies, environmental transmission electron microscopy (E-TEM), and surface X-ray scattering. Other techniques such as X-ray core-level spectroscopies are element-specific and chemical-state-specific, and are being widely applied in materials science research. Herein we showcase four types of newly developed strategies to probe electrode/electrolyte interfaces in situ with X-ray core-level spectroscopies. These include the standing wave approach, the meniscus approach, and two liquid cell approaches based on X-ray photoelectron spectroscopy and soft X-ray absorption spectroscopy. These examples demonstrate that with proper modifications, many ultra-high-vacuum based techniques can be adapted to study buried electrode/electrolyte interfaces and provide interface-sensitive, element- and chemical-state-specific information, such as solute distribution, hydrogen-bonding network, and molecular reorientation. At present, each method has its own specific limitations, but all of them enable in situ and operando characterization of electrode/electrolyte interfaces that can provide important insights into a variety of electrochemical systems. PMID:26514115

  2. Functional materials analysis using in situ and in operando X-ray and neutron scattering

    PubMed Central

    Peterson, Vanessa K.; Papadakis, Christine M.

    2015-01-01

    In situ and in operando studies are commonplace and necessary in functional materials research. This review highlights recent developments in the analysis of functional materials using state-of-the-art in situ and in operando X-ray and neutron scattering and analysis. Examples are given covering a number of important materials areas, alongside a description of the types of information that can be obtained and the experimental setups used to acquire them. PMID:25866665

  3. Functional materials analysis using in situ and in operando X-ray and neutron scattering.

    PubMed

    Peterson, Vanessa K; Papadakis, Christine M

    2015-03-01

    In situ and in operando studies are commonplace and necessary in functional materials research. This review highlights recent developments in the analysis of functional materials using state-of-the-art in situ and in operando X-ray and neutron scattering and analysis. Examples are given covering a number of important materials areas, alongside a description of the types of information that can be obtained and the experimental setups used to acquire them. PMID:25866665

  4. Gas cell for in situ soft X-ray transmission-absorption spectroscopy of materials

    SciTech Connect

    Drisdell, W. S.; Kortright, J. B.

    2014-07-15

    A simple gas cell design, constructed primarily from commercially available components, enables in situ soft X-ray transmission-absorption spectroscopy of materials in contact with gas at ambient temperature. The cell has a minimum X-ray path length of 1 mm and can hold gas pressures up to ∼300 Torr, and could support higher pressures with simple modifications. The design enables cycling between vacuum and gas environments without interrupting the X-ray beam, and can be fully sealed to allow for measurements of air-sensitive samples. The cell can attach to the downstream port of any appropriate synchrotron beamline, and offers a robust and versatile method for in situ measurements of certain materials. The construction and operation of the cell are discussed, as well as sample preparation and proper spectral analysis, illustrated by examples of spectral measurements. Potential areas for improvement and modification for specialized applications are also mentioned.

  5. Nitride-MBE system for in situ synchrotron X-ray measurements

    NASA Astrophysics Data System (ADS)

    Sasaki, Takuo; Ishikawa, Fumitaro; Yamaguchi, Tomohiro; Takahasi, Masamitu

    2016-05-01

    A molecular beam epitaxy (MBE) chamber dedicated to nitride growth was developed at the synchrotron radiation facility SPring-8. This chamber has two beryllium windows for incident and outgoing X-rays, and is directly connected to an X-ray diffractometer, enabling in situ synchrotron X-ray measurements during the nitride growth. Experimental results on initial growth dynamics in GaN/SiC, AlN/SiC, and InN/GaN heteroepitaxy were presented. We achieved high-speed and high-sensitivity reciprocal space mapping with a thickness resolution of atomic-layer scale. This in situ measurement using the high-brilliance synchrotron light source will be useful for evaluating structural variations in the initial growth stage of nitride semiconductors.

  6. In-situ Measurements of Colloid Transport and Retention Using Synchroton X-ray Fluorescence

    Technology Transfer Automated Retrieval System (TEKTRAN)

    The physics regarding the retention and mobilization of colloids in saturated and unsaturated conditions remains poorly understood, partially due to the inability to measure colloid concentrations in-situ. In this study, we attached Cd+2 ions to clay colloids, and used synchrotron x-rays to cause th...

  7. A furnace and environmental cell for the in situ investigation of molten salt electrolysis using high-energy X-ray diffraction.

    PubMed

    Styles, Mark J; Rowles, Matthew R; Madsen, Ian C; McGregor, Katherine; Urban, Andrew J; Snook, Graeme A; Scarlett, Nicola V Y; Riley, Daniel P

    2012-01-01

    This paper describes the design, construction and implementation of a relatively large controlled-atmosphere cell and furnace arrangement. The purpose of this equipment is to facilitate the in situ characterization of materials used in molten salt electrowinning cells, using high-energy X-ray scattering techniques such as synchrotron-based energy-dispersive X-ray diffraction. The applicability of this equipment is demonstrated by quantitative measurements of the phase composition of a model inert anode material, which were taken during an in situ study of an operational Fray-Farthing-Chen Cambridge electrowinning cell, featuring molten CaCl(2) as the electrolyte. The feasibility of adapting the cell design to investigate materials in other high-temperature environments is also discussed. PMID:22186642

  8. Facility for combined in situ magnetron sputtering and soft x-ray magnetic circular dichroism

    SciTech Connect

    Telling, N. D.; Laan, G. van der; Georgieva, M. T.; Farley, N. R. S.

    2006-07-15

    An ultrahigh vacuum chamber that enables the in situ growth of thin films and multilayers by magnetron sputtering techniques is described. Following film preparation, x-ray absorption spectroscopy (XAS) and x-ray magnetic circular dichroism (XMCD) measurements are performed by utilizing an in vacuum electromagnet. XMCD measurements on sputtered thin films of Fe and Co yield spin and orbital moments that are consistent with those obtained previously on films measured in transmission geometry and grown in situ by evaporation methods. Thin films of FeN prepared by reactive sputtering are also examined and reveal an apparent enhancement in the orbital moment for low N content samples. The advantages of producing samples for in situ XAS and XMCD studies by magnetron sputtering are discussed.

  9. Note: Sample chamber for in situ x-ray absorption spectroscopy studies of battery materials

    SciTech Connect

    Pelliccione, CJ; Timofeeva, EV; Katsoudas, JP; Segre, CU

    2014-12-01

    In situ x-ray absorption spectroscopy (XAS) provides element-specific characterization of both crystalline and amorphous phases and enables direct correlations between electrochemical performance and structural characteristics of cathode and anode materials. In situ XAS measurements are very demanding to the design of the experimental setup. We have developed a sample chamber that provides electrical connectivity and inert atmosphere for operating electrochemical cells and also accounts for x-ray interactions with the chamber and cell materials. The design of the sample chamber for in situ measurements is presented along with example XAS spectra from anode materials in operating pouch cells at the Zn and Sn K-edges measured in fluorescence and transmission modes, respectively. (C) 2014 AIP Publishing LLC.

  10. Characterization of the interfacial geomechanics in gas shales via integrated Raman spectroscopy, nanoindentation and energy dispersive X-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Ferralis, N.; Abedi, S.; Grossman, J. C.; Ulm, F.

    2012-12-01

    The geomechanical characterization of gas shales at the microscale is currently enabled by the use of grid-based nanoindentation techniques. However, the inability to probe the chemical and mineral heterogeneity of gas shales limits the identification of the geomechanical properties of individual components and phases within the probed region. The development of an integrated multiphysics approach that combines geomechanical and chemical information is crucial for the characterization of interfaces between phases, leading to the identification of regions with low yield strain. Here we present a comprehensive investigation where a spatially aligned coupled multiphysics analysis of gas shales is used to identify relevant the geomechanics of mineral and organic phases and their interfaces. This method uses grid-based nanondentation to extract the geomechanical information. Raman spectroscopy is used to identify the majority of inorganic components (calcite, quartz, anatase, pyrite, clay) as well as to characterize the diversity and maturity in the organic component (kerogen). Energy dispersive X-ray is used in combination with Raman to identify clay. With the use of clustering analysis statistical tools a correlation analysis over the full range of data (geomechanics and chemical data), we identify several mineral phases, and we clearly associate the mechanical properties (defined in terms of hardness, modulus and yield strain) with each phase. With this innovative multiphysics analysis we were able to identify interfacial phases between inorganic phases, with distinct hardness and yield strain. We find that regions between calcite-rich or quartz rich phases and clay-rich phases showed a lower than of that of the corresponding boundary phases. Hence this approach provides a viable method for the identification of the "weakest links" in gas shales with the highest probability of fracture.

  11. Gunshot residue testing in suicides: Part I: Analysis by scanning electron microscopy with energy-dispersive X-ray.

    PubMed

    Molina, D Kimberley; Martinez, Michael; Garcia, James; DiMaio, Vincent J M

    2007-09-01

    Several different methods can be employed to test for gunshot residue (GSR) on a deceased person's hands, including scanning electron microscopy with energy-dispersive x-ray spectroscopy (SEM-EDX) and inductively coupled plasma-atomic emission spectrometry (ICP-AES). Each of these techniques has been extensively studied, especially on living individuals. The current studies (Part I and Part II) were designed to compare the use and utility of the different GSR testing techniques in a medical examiner setting. In Part I, the hands of deceased persons who died from undisputed suicidal handgun wounds were tested for GSR by SEM-EDX over a 4-year period. A total of 116 cases were studied and analyzed for caliber of weapon, proximity of wound, and results of GSR testing, including spatial deposition upon the hands. It was found that in only 50% of cases with a known self-inflicted gunshot wound was SEM-EDX positive for at least 1 specific particle for GSR. In 18% of the cases there was a discernible pattern (spatial distribution) of the particles on the hand such that the manner in which the weapon was held could be determined. Since only 50% of cases where the person is known to have fired a weapon immediately prior to death were positive for GSR by SEM-EDX, this test should not be relied upon to determine whether a deceased individual has discharged a firearm. Furthermore, in only 18% of cases was a discernible pattern present indicating how the firearm was held. The low sensitivity, along with the low percentage of cases with a discernible pattern, limits the usefulness of GSR test results by SEM-EDX in differentiating self-inflicted from non-self-inflicted wounds. PMID:17721163

  12. In situ x-ray, electrochemical, and modeling investigation of the oxygen electrode activation.

    SciTech Connect

    Yildiz, B.; Chang, K.-C.; Meyers, D.; Carter, J. D.; You, H.

    2006-01-01

    Oxygen electrodes of solid oxide electrochemical cells have been shown to improve under strong cathodic and anodic polarization. Our study investigates the mechanism causing such improvement, using in situ x-ray and electrochemical characterization and electrochemical impedance modeling of the oxygen electrodes. Several porous and dense thin-film model electrodes of La{sub 0.8}Sr{sub 0.2}MnO{sub 3} (LSM) and La{sub 0.8}Sr{sub 0.2}MnO{sub 3} (LCM) on single crystal yttria-stabilized zirconia (YSZ) electrolytes have been analyzed in situ at the Advanced Photon Source (APS) using x-ray reflectivity and x-ray absorption near edge spectroscopy (XANES) at the Mn K-edge and La LII-edge. In situ x-ray reflectivity analysis show that no clear correlation between the polarization of the electrode and any further changes in the roughness of the LSM/YSZ interface exist. XANES measurements illustrate that the cathodic or anodic dc polarization at high temperature induces no detectable changes in Mn chemical state either in the bulk or at the surface of the LCM and LSM electrodes on YSZ, while the La chemical state changes reversibly at the electrode surface. This field-induced chemical change of La at the surface of electrodes is assumed to be a cause of the electrochemical activation through enhanced surface exchange of oxygen on the doped lanthanum manganite electrodes.

  13. Matrix effects in the energy dispersive X-ray analysis of CaO-Al(2)O(3)-MgO inclusions in steel.

    PubMed

    Pistorius, Petrus Christiaan; Verma, Neerav

    2011-12-01

    Energy dispersive X-ray microanalysis of micron-sized inclusions in steel is of considerable industrial importance. Measured spectra and Monte Carlo simulations show a significant effect of the steel matrix on analysis of CaO-Al(2)O(3)-MgO inclusions: the steel matrix filters the softer (Al and Mg) characteristic X-rays, increasing the relative height of the Ca peak. Bulk matrix correction methods would not result in correct inclusion compositions, but operating at a lower acceleration voltage shifts the effect to smaller inclusion sizes. PMID:22051086

  14. In situ observation of cellular organelles with a contact x-ray microscope

    NASA Astrophysics Data System (ADS)

    Kado, M.; Kishimoto, M.; Tamotsu, S.; Yasuda, K.; Shinohara, K.

    2013-10-01

    A contact x-ray microscope coupled with a highly intense laser plasma soft x-ray source has been developed and in situ observations of cellular organelles have been conducted. The soft x-rays were generated by irradiating a high power laser pulse onto a thin-foiled gold target and about 1.3×1015 photons/sr were obtained, which allowed the inner structures of live wet biological cells to be imaged. Single shot flash imaging is a key technique to image cellular organelles of live biological cells avoiding degradation of the spatial resolution of the images resulting from motion blur and radiation damage. The use of a fluorescence microscope to identify cellular organelles in conjunction with the soft x-ray microscope has allowed several cellular organelles to be identified precisely in the soft x-ray images. Combining the fluorescence microscope with the soft x-ray microscope will be very useful and will establish the technique as a powerful tool to analyze living function of biological cells.

  15. In Situ Synchrotron X-Ray Techniques for the Study of Lithium Battery Materials

    SciTech Connect

    McBreen, J.; Mukerjee, S.; Yang, X. Q.; Sun, X., Ein-Eli, Y.

    1998-11-01

    The combination of in situ X-ray diffraction (XRD) and x-ray absorption spectroscopy (XAS) is a very powerful technique in the study of lithium battery cathode materials. XRD identifies the phase changes that occur during cycling and XAS gives information on the redox charge compensation processes that occur on the transition metal oxides. Because of its element specific nature XAS can identify the occurrence of redox processes on the various cations in doped oxide cathode materials. Since XAS probes short range order and is particularly useful in the study of amorphous tin based composite oxide anode materials.

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

    NASA Astrophysics Data System (ADS)

    Pitarch, A.; Queralt, I.

    2010-05-01

    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 [1]. 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.

  17. Amalgam tattoo: report of an unusual clinical presentation and the use of energy dispersive X-ray analysis as an aid to diagnosis

    SciTech Connect

    McGinnis, J.P. Jr.; Greer, J.L.; Daniels, D.S.

    1985-01-01

    An unusual appearing gingival amalgam pigmentation (amalgam tattoo) that completely surrounded the maxillary right first premolar in a 13-year-old boy is presented. Because of the wide distribution and apparent clinical progression of the discoloration, an excisional biopsy was performed. The histopathologic diagnosis of amalgam pigmentation was confirmed in paraffin sections by energy dispersive X-ray microanalysis. Silver, tin, and mercury were detected in the specimen.

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

    SciTech Connect

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

    2007-06-29

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

  19. In Situ X-Ray Probing Reveals Fingerprints of Surface Platinum Oxide

    SciTech Connect

    Friebel, Daniel

    2011-08-24

    In situ x-ray absorption spectroscopy (XAS) at the Pt L{sub 3} edge is a useful probe for Pt-O interactions at polymer electrolyte membrane fuel cell (PEMFC) cathodes. We show that XAS using the high energy resolution fluorescence detection (HERFD) mode, applied to a well-defined monolayer Pt/Rh(111) sample where the bulk penetrating hard x-rays probe only surface Pt atoms, provides a unique sensitivity to structure and chemical bonding at the Pt-electrolyte interface. Ab initio multiple-scattering calculations using the FEFF8 code and complementary extended x-ray absorption fine structure (EXAFS) results indicate that the commonly observed large increase of the white-line at high electrochemical potentials on PEMFC cathodes originates from platinum oxide formation, whereas previously proposed chemisorbed oxygen-containing species merely give rise to subtle spectral changes.

  20. In situ X-ray snapshot analysis of transient molecular adsorption in a crystalline channel

    NASA Astrophysics Data System (ADS)

    Kubota, Ryou; Tashiro, Shohei; Shiro, Motoo; Shionoya, Mitsuhiko

    2014-10-01

    Molecular adsorption is a fundamental phenomenon in porous materials and is usually characterized by the efficiency and selectivity of molecular separations and reactions. However, for functional porous materials, analysis of the dynamic behaviour of molecular adsorbents is a major challenge. Here, we use in situ single-crystal X-ray diffraction to analyse multi-step molecular adsorption in a crystalline nanochannel of a metal-macrocycle framework. The pore surface of the metal-macrocycle framework crystal contains five different enantiomerically paired binding pockets, to which the adsorption of a (1R)-1-(3-chlorophenyl)ethanol solution was monitored with time. The resulting X-ray snapshot analyses suggest that the guest adsorption process takes a two-step pathway before equilibrium, in which the guest molecule is temporarily trapped by a neighbouring binding site. This demonstrates the potential for using X-ray analyses to visualize a transient state during a non-covalent self-assembly process.

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

    SciTech Connect

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

    2009-09-01

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

  2. Energy-dispersive X-ray emission spectroscopy using an X-ray free-electron laser in a shot-by-shot mode

    PubMed Central

    Alonso-Mori, Roberto; Kern, Jan; Gildea, Richard J.; Sokaras, Dimosthenis; Weng, Tsu-Chien; Lassalle-Kaiser, Benedikt; Tran, Rosalie; Hattne, Johan; Laksmono, Hartawan; Hellmich, Julia; Glöckner, Carina; Echols, Nathaniel; Sierra, Raymond G.; Schafer, Donald W.; Sellberg, Jonas; Kenney, Christopher; Herbst, Ryan; Pines, Jack; Hart, Philip; Herrmann, Sven; Grosse-Kunstleve, Ralf W.; Latimer, Matthew J.; Fry, Alan R.; Messerschmidt, Marc M.; Miahnahri, Alan; Seibert, M. Marvin; Zwart, Petrus H.; White, William E.; Adams, Paul D.; Bogan, Michael J.; Boutet, Sébastien; Williams, Garth J.; Zouni, Athina; Messinger, Johannes; Glatzel, Pieter; Sauter, Nicholas K.; Yachandra, Vittal K.; Yano, Junko; Bergmann, Uwe

    2012-01-01

    The ultrabright femtosecond X-ray pulses provided by X-ray free-electron lasers open capabilities for studying the structure and dynamics of a wide variety of systems beyond what is possible with synchrotron sources. Recently, this “probe-before-destroy” approach has been demonstrated for atomic structure determination by serial X-ray diffraction of microcrystals. There has been the question whether a similar approach can be extended to probe the local electronic structure by X-ray spectroscopy. To address this, we have carried out femtosecond X-ray emission spectroscopy (XES) at the Linac Coherent Light Source using redox-active Mn complexes. XES probes the charge and spin states as well as the ligand environment, critical for understanding the functional role of redox-active metal sites. Kβ1,3 XES spectra of MnII and Mn2III,IV complexes at room temperature were collected using a wavelength dispersive spectrometer and femtosecond X-ray pulses with an individual dose of up to >100 MGy. The spectra were found in agreement with undamaged spectra collected at low dose using synchrotron radiation. Our results demonstrate that the intact electronic structure of redox active transition metal compounds in different oxidation states can be characterized with this shot-by-shot method. This opens the door for studying the chemical dynamics of metal catalytic sites by following reactions under functional conditions. The technique can be combined with X-ray diffraction to simultaneously obtain the geometric structure of the overall protein and the local chemistry of active metal sites and is expected to prove valuable for understanding the mechanism of important metalloproteins, such as photosystem II. PMID:23129631

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

    PubMed

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

    2016-01-01

    In situ studies of oxide molecular beam epitaxy by synchrotron x-ray scattering has been made possible by upgrading an existing UHV/molecular beam epitaxy (MBE) six-circle diffractometer system. For oxide MBE growth, pure ozone delivery to the chamber has been made available, and several new deposition sources have been made available on a new 12 in. CF (ConFlat, a registered trademark of Varian, Inc.) flange. X-ray diffraction has been used as a major probe for film growth and structures for the system. In the original design, electron diffraction was intended for the secondary diagnostics available without the necessity of the x-ray and located at separate positions. Deposition of films was made possible at the two diagnostic positions. And, the aiming of the evaporation sources is fixed to the point between two locations. Ozone can be supplied through two separate nozzles for each location. Also two separate thickness monitors are installed. Additional features of the equipment are also presented together with the data taken during typical oxide film growth to illustrate the depth of information available via in situ x-ray techniques. PMID:26827327

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

    SciTech Connect

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

    2016-01-01

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

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

    PubMed

    Wang, Hongchang; Kashyap, Yogesh; Laundy, David; Sawhney, Kawal

    2015-07-01

    In situ metrology overcomes many of the limitations of existing metrology techniques and is capable of exceeding the performance of present-day optics. A novel technique for precisely characterizing an X-ray bimorph mirror and deducing its two-dimensional (2D) slope error map is presented. This technique has also been used to perform fast optimization of a bimorph mirror using the derived 2D piezo response functions. The measured focused beam size was significantly reduced after the optimization, and the slope error map was then verified by using geometrical optics to simulate the focused beam profile. This proposed technique is expected to be valuable for in situ metrology of X-ray mirrors at synchrotron radiation facilities and in astronomical telescopes. PMID:26134795

  6. Electrochemical flowcell for in-situ investigations by soft x-ray absorption and emission spectroscopy

    SciTech Connect

    Schwanke, C.; Lange, K. M.; Golnak, R.; Xiao, J.

    2014-10-15

    A new liquid flow-cell designed for electronic structure investigations at the liquid-solid interface by soft X-ray absorption and emission spectroscopy is presented. A thin membrane serves simultaneously as a substrate for the working electrode and solid state samples as well as for separating the liquid from the surrounding vacuum conditions. In combination with counter and reference electrodes this approach allows in-situ studies of electrochemical deposition processes and catalytic reactions at the liquid-solid interface in combination with potentiostatic measurements. As model system in-situ monitoring of the deposition process of Co metal from a 10 mM CoCl{sub 2} aqueous solution by X-ray absorption and emission spectroscopy is presented.

  7. Investigation of x-ray photon counting using a silicon-PIN diode and its application to energy-dispersive computed tomography

    NASA Astrophysics Data System (ADS)

    Kodama, Hajime; Sato, Eiichi; Sagae, Michiaki; Hagiwara, Osahiko; Matsukiyo, Hiroshi; Osawa, Akihiro; Enomoto, Toshiyuki; Watanabe, Manabu; Kusachi, Shinya; Sato, Shigehiro; Ogawa, Akira

    2013-09-01

    X-ray photon counting was performed using a readymade silicon-PIN photodiode (Si-PIN-PD) at tube voltages ranging from 42 to 60 kV, and X-ray photons are directly detected using the 100 MHz Si-PIN-PD without a scintillator. Photocurrent from the diode is amplified using charge-sensitive and shaping amplifiers. Using a multichannel analyzer, X-ray spectra at a tube voltage of 60 kV could easily be measured. The photon-counting computed tomography (PCCT) is accomplished by repeated linear scans and rotations of an object, and projection curves of the object are obtained by the linear scan. In the PC-CT, we confirmed the energy-dispersive effect with changes in lower-level voltage of the event pulse using a comparator.

  8. In situ x-ray investigation of freestanding nanoscale Cu-Nb multilayers under tensile load.

    SciTech Connect

    Aydiner, C. C.; Misra, A.; Brown, D. W.; Mara, N. A.; Almer, J. D

    2009-01-01

    The yield behavior in a freestanding sputter-deposited Cu/Nb multilayer with 30 nm nominal individual layer thickness has been investigated with in situ synchrotron x-ray diffraction during tensile loading. A pronounced elastic-plastic transition is observed with the fraction of plastically yielded grains increasing gradually with strain. Near synchronous yielding is observed in the Cu and Nb grains. The gradual progression in yield behavior is interpreted in terms of residual stresses, and elastic and plastic anisotropy.

  9. Development of in situ, at-wavelength metrology for soft x-ray nano-focusing

    SciTech Connect

    Yuan, Sheng Sam; Yashchuk, Valeriy V.; Goldberg, Kenneth A.; Celestre, Richard; McKinney, Wayne R.; Morrison, Gregory Y.; Warwick, Tony; Padmore, Howard A.

    2010-09-19

    At the Advanced Light Source (ALS), we are developing broadly applicable, high-accuracy, in situ, at-wavelength wavefront slope measurement techniques for Kirkpatrick-Baez (KB) mirror nano-focusing. We describe here details of the metrology beamline endstation, the at-wavelength tests, and an original alignment method that have already allowed us to precisely set a bendable KB mirror to achieve a FWHM focused spot size of ~;;120 nm, at 1-nm soft x-ray wavelength.

  10. In-situ synchrotron x-ray transmission microscopy of the sintering of multilayers

    NASA Astrophysics Data System (ADS)

    Yan, Zilin; Guillon, Olivier; Martin, Christophe L.; Wang, Steve; Lee, Chul-Seung; Bouvard, Didier

    2013-06-01

    This letter reports on in-situ characterization of the high temperature sintering of multilayer ceramic capacitors by high-resolution synchrotron x-ray imaging. Microstructural evolution was obtained in real time by a continuous recording of 2-dimensional radiographs. Anisotropic strains were measured for different layers. Quantification of defects was conducted with 3-dimensional nano-computed tomography. These in-situ observations prove that electrode discontinuities occur at the early stage of sintering and originate from initial heterogeneities linked to the particulate nature of the starting powders.

  11. In Situ Soft X-ray Spectroscopy Characterization of Interfacial Phenomena in Energy Materials and Devices

    NASA Astrophysics Data System (ADS)

    Guo, Jinghua; Liu, Yi-Sheng; Kapilashrami, Mukes; Glans, Per-Anders; Bora, Debajeet; Braun, Artur; Velasco Vélez, Juan Jesús; Salmeron, Miquel; ALS/LBNL Team; EMPA, MSD/LBNL Collaboration

    2015-03-01

    Advanced energy technology arises from the understanding in basic science, thus rest in large on in-situ/operando characterization tools for observing the physical and chemical interfacial processes, which has been largely limited in a framework of thermodynamic and kinetic concepts or atomic and nanoscale. In many important energy systems such as energy conversion, energy storage and catalysis, advanced materials and functionality in devices are based on the complexity of material architecture, chemistry and interactions among constituents within. To understand and thus ultimately control the energy conversion and energy storage applications calls for in-situ/operando characterization tools. Soft X-ray spectroscopy offers a number of very unique features. We will present our development of the in-situ/operando soft X-ray spectroscopic tools of catalytic and electrochemical reactions in recent years, and reveal how to overcome the challenge that soft X-rays cannot easily peek into the high-pressure catalytic cells or liquid electrochemical cells. In this presentation a number of examples are given, including the nanocatalysts and the recent experiment performed for studying the hole generation in a specifically designed photoelectrochemical cell under operando conditions. The ALS is supported by the the U.S. Department of Energy.

  12. THIN-FILM DENSITY DETERMINATION OF TANTALUM, TANTALUM OXIDES, AND XEROGELS BY MULTIPLE RADIATION ENERGY DISPERSIVE X-RAY REFLECTIVITY

    EPA Science Inventory

    X-ray reflectivity provides a nondestructive technique for measuring density in thin films. A conventional laboratory, Bragg-Brentano geometry diffractometer was employed to show the generalized feasibility of this technique. X-ray tubes with chromium, copper, and molybdenum targ...

  13. X-ray energy dispersive spectroscopy of uranium ore using a TES microcalorimeter mounted on a field-emission scanning electron microscope

    NASA Astrophysics Data System (ADS)

    Maehata, Keisuke; Idemitsu, Kazuya; Tanaka, Keiichi

    2011-08-01

    Energy dispersive spectroscopic measurements of uranium ore were conducted using a superconducting phase transition-edge-thermosensor (TES) microcalorimeter mounted on a field-emission scanning electron microscope (SEM) to demonstrate its potential for high-precision microanalysis. The effective solid angle for X-ray detection is found to be larger than 2 msr by precise adjustments in the X-ray polycapillary alignment. The observed detection signal pulses with decay time constant of 50 μs enable maximum count rates larger than 300 counts per second. The energy resolution was determined to be 14.6 eV FWHM at Al Kα X-ray energies of 1487 eV. Distinct peaks appear in the resulting X-ra y energy spectrum associated with U-Mα, U-Mβ and U-Mγ X-rays emitted by the uranium ore specimens. This spectrum includes weaker peaks corresponding to C-Kα, Fe-Lα, Cu-L and Sr L α1 X rays.

  14. Determination of trace elements in Syrian medicinal plants and their infusions by energy dispersive X-ray fluorescence and total reflection X-ray fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Khuder, A.; Sawan, M. Kh.; Karjou, J.; Razouk, A. K.

    2009-07-01

    X-ray fluorescence (XRF) and total-reflection X-ray fluorescence (TXRF) techniques suited well for a multi-element determination of K, Ca, Mn, Fe, Cu, Zn, Rb, and Sr in some Syrian medicinal plant species. The accuracy and the precision of both techniques were verified by analyzing the Standard Reference Materials (SRM) peach-1547 and apple leaves-1515. A good agreement between the measured concentrations of the previously mentioned elements and the certified values were obtained with errors less than 10.7% for TXRF and 15.8% for XRF. The determination of Br was acceptable only by XRF with an error less than 24%. Furthermore, the XRF method showed a very good applicability for the determination of K, Ca, Mn, Fe, Cu, Zn, Rb, Sr, and Br in infusions of different Syrian medicinal plant species, namely anise ( Anisum vulgare), licorice root ( Glycyrrhiza glabra), and white wormwood ( Artemisia herba-alba).

  15. Electron-excited energy dispersive X-ray spectrometry at high speed and at high resolution: silicon drift detectors and microcalorimeters.

    PubMed

    Newbury, Dale E

    2006-12-01

    Two recent developments in X-ray spectrometer technology provide dramatic improvements in analytical capabilities that impact the frontiers of electron microscopy. Silicon drift detectors (SDD) use the same physics as silicon (lithium) energy dispersive spectrometers [Si(Li) EDS] but differ in design: only 10% of the thickness of the Si(Li) EDS with an anode area below 0.1 mm2 and a complex rear surface electrode pattern that creates a lateral internal charge collection field. The SDD equals or betters the Si(Li) EDS in most measures of performance. For output versus input count rate, the SDD exceeds the Si(Li) EDS by a factor of 5 to 10 for the same resolution. This high throughput can benefit analytical measurements that are count limited, such as X-ray mapping and trace measurements. The microcalorimeter EDS determines the X-ray energy by measuring the temperature rise in a metal absorber. Operating at 100 mK, the microcalorimeter EDS achieves resolution of 2-5 eV over a photon energy range of 200 eV to 10 keV in energy dispersive operation, eliminating most peak interference situations and providing high peak-to-background to detect low fluorescence yield peaks. Chemical bonding effects on low energy (< 2 keV) peak shapes can be measured. PMID:19830945

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

    SciTech Connect

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

    2013-12-15

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

  17. In situ compressive damage of cement paste characterized by lab source X-ray computer tomography

    SciTech Connect

    Wan, Keshu; Xue, Xiaobo

    2013-08-15

    This paper aims at illustrating the potential of lab source X-ray CT for studying the damage behavior of cement based materials through in situ load experiments. This approach permits quantifying the microstructure prior and during loading. The load damage is separated from the specimen deformation using an image interpolation method. A quantitative relationship between external load and internal specimen damage is analyzed using the statistical information of gray scale values of the CT data. Local damage degrees are defined on 3D subset, and the 3D spatial distribution of damage information is clarified in this research. - Highlights: • On line damage is characterized by lab source X-ray CT. • Loading damage is separated with the specimen deformation. • Local damage is analyzed using gray scale values of the CT data. • 3D spatial distribution of the local damage information is clarified.

  18. Rapid in situ X-ray position stabilization via extremum seeking feedback.

    PubMed

    Zohar, S; Venugopalan, N; Kissick, D; Becker, M; Xu, S; Makarov, O; Stepanov, S; Ogata, C; Sanishvili, R; Fischetti, R F

    2016-03-01

    X-ray beam stability is crucial for acquiring high-quality data at synchrotron beamline facilities. When the X-ray beam and defining apertures are of similar dimensions, small misalignments driven by position instabilities give rise to large intensity fluctuations. This problem is solved using extremum seeking feedback control (ESFC) for in situ vertical beam position stabilization. In this setup, the intensity spatial gradient required for ESFC is determined by phase comparison of intensity oscillations downstream from the sample with pre-existing vertical beam oscillations. This approach compensates for vertical position drift from all sources with position recovery times <6 s and intensity stability through a 5 µm aperture measured at 1.5% FWHM over a period of 8 hours. PMID:26917131

  19. In situ x-ray diffraction measurements of the capillary fountain jet produced via ultrasonic atomization

    NASA Astrophysics Data System (ADS)

    Yano, Yohko F.; Douguchi, Junya; Kumagai, Atsushi; Iijima, Takao; Tomida, Yukinobu; Miyamoto, Toshiaki; Matsuura, Kazuo

    2006-11-01

    In situ x-ray diffraction measurements were carried out for investigating the liquid structure in the ultrasonic fountain jet to consider the mechanism of the "ultrasonic ethanol separation" reported by Sato et al. [J. Chem. Phys. 114, 2382 (2001)]. For pure liquids (water and ethanol), it was found that the high frequency ultrasound does not affect the liquid structure microscopically. For the 20mol% ethanol-water mixture, the estimated ethanol mole fraction in the ultrasonic fountain jet by using the position of the main maximum in the x-ray diffraction profile coincided with that in the reservoir. This result suggests that the ethanol separation is not caused by any distorted liquid structure under the ultrasound irradiation and occurs when or after the generation of the liquid droplet mist.

  20. In situ x-ray diffraction measurements of the capillary fountain jet produced via ultrasonic atomization.

    PubMed

    Yano, Yohko F; Douguchi, Junya; Kumagai, Atsushi; Iijima, Takao; Tomida, Yukinobu; Miyamoto, Toshiaki; Matsuura, Kazuo

    2006-11-01

    In situ x-ray diffraction measurements were carried out for investigating the liquid structure in the ultrasonic fountain jet to consider the mechanism of the "ultrasonic ethanol separation" reported by Sato et al. [J. Chem. Phys. 114, 2382 (2001)]. For pure liquids (water and ethanol), it was found that the high frequency ultrasound does not affect the liquid structure microscopically. For the 20 mol % ethanol-water mixture, the estimated ethanol mole fraction in the ultrasonic fountain jet by using the position of the main maximum in the x-ray diffraction profile coincided with that in the reservoir. This result suggests that the ethanol separation is not caused by any distorted liquid structure under the ultrasound irradiation and occurs when or after the generation of the liquid droplet mist. PMID:17100459

  1. In situ x-ray photoelectron spectroscopy for electrochemical reactions in ordinary solvents

    SciTech Connect

    Masuda, Takuya; Yoshikawa, Hideki; Kobata, Masaaki; Kobayashi, Keisuke; Noguchi, Hidenori; Kawasaki, Tadahiro; Uosaki, Kohei

    2013-09-09

    In situ electrochemical X-ray photoelectron spectroscopy (XPS) apparatus, which allows XPS at solid/liquid interfaces under potential control, was constructed utilizing a microcell with an ultra-thin Si membrane, which separates vacuum and a solution. Hard X-rays from a synchrotron source penetrate into the Si membrane surface exposed to the solution. Electrons emitted at the Si/solution interface can pass through the membrane and be analyzed by an analyzer placed in vacuum. Its operation was demonstrated for potential-induced Si oxide growth in water. Effect of potential and time on the thickness of Si and Si oxide layers was quantitatively determined at sub-nanometer resolution.

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

    SciTech Connect

    Antonio, M.R.; Soderholm, L.; Song, I.

    1995-06-12

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

  3. X-ray microscopy for in situ characterization of 3D nanostructural evolution in the laboratory

    NASA Astrophysics Data System (ADS)

    Hornberger, Benjamin; Bale, Hrishikesh; Merkle, Arno; Feser, Michael; Harris, William; Etchin, Sergey; Leibowitz, Marty; Qiu, Wei; Tkachuk, Andrei; Gu, Allen; Bradley, Robert S.; Lu, Xuekun; Withers, Philip J.; Clarke, Amy; Henderson, Kevin; Cordes, Nikolaus; Patterson, Brian M.

    2015-09-01

    X-ray microscopy (XRM) has emerged as a powerful technique that reveals 3D images and quantitative information of interior structures. XRM executed both in the laboratory and at the synchrotron have demonstrated critical analysis and materials characterization on meso-, micro-, and nanoscales, with spatial resolution down to 50 nm in laboratory systems. The non-destructive nature of X-rays has made the technique widely appealing, with potential for "4D" characterization, delivering 3D micro- and nanostructural information on the same sample as a function of sequential processing or experimental conditions. Understanding volumetric and nanostructural changes, such as solid deformation, pore evolution, and crack propagation are fundamental to understanding how materials form, deform, and perform. We will present recent instrumentation developments in laboratory based XRM including a novel in situ nanomechanical testing stage. These developments bridge the gap between existing in situ stages for micro scale XRM, and SEM/TEM techniques that offer nanometer resolution but are limited to analysis of surfaces or extremely thin samples whose behavior is strongly influenced by surface effects. Several applications will be presented including 3D-characterization and in situ mechanical testing of polymers, metal alloys, composites and biomaterials. They span multiple length scales from the micro- to the nanoscale and different mechanical testing modes such as compression, indentation and tension.

  4. In situ X-ray monitoring of damage accumulation in SiC/RBSN tensile specimens

    NASA Technical Reports Server (NTRS)

    Baaklini, George Y.; Bhatt, Ramkrishna T.

    1991-01-01

    The room-temperature tensile testing of silicon carbide fiber reinforced reaction-bonded silicon nitride (SiC/RBSN) composite specimens was monitored by using in-situ X-ray film radiography. Radiographic evaluation before, during, and after loading provided data on the effect of preexisting volume flaws (high density impurities, and local density variations) on the fracture behavior of composites. Results from (O)1, (O)3, (O)5, and (O)8 composite specimens showed that X-ray film radiography can monitor damage accumulations during tensile loading. Matrix cracking, fiber-matrix debonding, and fiber pullout were imaged throughout the tensile loading history of the specimens. Further, in-situ film radiography was found to be a helpful and practical technique for estimating interfacial shear strength between the SiC fiber and the RBSN matrix by the matrix crack spacing method. It is concluded that pretest, in-situ, and post-test radiography can provide for a greater understanding of ceramic matrix composite mechanical behavior, a verification of related experimental procedures, and a validation and development of related analytical models.

  5. In situ X-ray monitoring of damage accumulation in SiC/RBSN tensile specimens

    SciTech Connect

    Baaklini, G.Y.; Bhatt, R.T.

    1991-08-01

    The room-temperature tensile testing of silicon carbide fiber reinforced reaction-bonded silicon nitride (SiC/RBSN) composite specimens was monitored by using in-situ X-ray film radiography. Radiographic evaluation before, during, and after loading provided data on the effect of preexisting volume flaws (high density impurities, and local density variations) on the fracture behavior of composites. Results from (O)1, (O)3, (O)5, and (O)8 composite specimens showed that X-ray film radiography can monitor damage accumulations during tensile loading. Matrix cracking, fiber-matrix debonding, and fiber pullout were imaged throughout the tensile loading history of the specimens. Further, in-situ film radiography was found to be a helpful and practical technique for estimating interfacial shear strength between the SiC fiber and the RBSN matrix by the matrix crack spacing method. It is concluded that pretest, in-situ, and post-test radiography can provide for a greater understanding of ceramic matrix composite mechanical behavior, a verification of related experimental procedures, and a validation and development of related analytical models. 14 refs.

  6. X-ray Photon Counting Using 100 MHz Ready-Made Silicon P-Intrinsic-N X-ray Diode and Its Application to Energy-Dispersive Computed Tomography

    NASA Astrophysics Data System (ADS)

    Kodama, Hajime; Watanabe, Manabu; Sato, Eiichi; Oda, Yasuyuki; Hagiwara, Osahiko; Matsukiyo, Hiroshi; Osawa, Akihiro; Enomoto, Toshiyuki; Kusachi, Shinya; Sato, Shigehiro; Ogawa, Akira

    2013-07-01

    X-ray photons are directly detected using a 100 MHz ready-made silicon P-intrinsic-N X-ray diode (Si-PIN-XD). The Si-PIN-XD is shielded using an aluminum case with a 25-µm-thick aluminum window and a BNC connector. The photocurrent from the Si-PIN-XD is amplified by charge sensitive and shaping amplifiers, and the event pulses are sent to a multichannel analyzer (MCA) to measure X-ray spectra. At a tube voltage of 90 kV, we observe K-series characteristic X-rays of tungsten. Photon-counting computed tomography (PC-CT) is accomplished by repeated linear scans and rotations of an object, and projection curves of the object are obtained by linear scanning at a tube current of 2.0 mA. The exposure time for obtaining a tomogram is 10 min with scan steps of 0.5 mm and rotation steps of 1.0°. At a tube voltage of 90 kV, the maximum count rate is 150 kcps. We carry out PC-CT using gadolinium media and confirm the energy-dispersive effect with changes in the lower level voltage of the event pulse using a comparator.

  7. In situ X-ray pair distribution function analysis of geopolymer gel nanostructure formation kinetics.

    PubMed

    White, Claire E; Provis, John L; Bloomer, Breaunnah; Henson, Neil J; Page, Katharine

    2013-06-14

    With the ever-increasing environmentally-driven demand for technologically advanced structural materials, geopolymer cement is fast becoming a viable alternative to traditional cements due to its proven engineering characteristics and the reduction in CO2 emitted during manufacturing (as much as 80% less CO2 emitted in manufacture, compared to ordinary Portland cement). Nevertheless, much remains unknown regarding the kinetics of reaction responsible for nanostructural evolution during the geopolymerisation process. Here, in situ X-ray total scattering measurements and pair distribution function (PDF) analysis are used to quantify the extent of reaction as a function of time for alkali-activated metakaolin/slag geopolymer binders, including the impact of various activators (alkali hydroxide/silicate) on the kinetics of the geopolymerisation reaction. Quantifying the reaction process in situ from X-ray PDF data collected during the initial ten hours can provide an estimate of the total reaction extent, but when combined with data obtained at longer times (128 days here) enables more accurate determination of the overall rate of reaction. To further assess the initial stages of the geopolymerisation reaction process, a pseudo-single step first order rate equation is fitted to the extent of reaction data, which reveals important mechanistic information regarding the role of free silica in the activators in the evolution of the binder systems. Hence, it is shown that in situ X-ray PDF analysis is an ideal experimental local structure tool to probe the reaction kinetics of complex reacting systems involving transitions between disordered/amorphous phases, of which geopolymerisation is an important example. PMID:23450172

  8. 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.

    PubMed

    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. PMID:25126753

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

    SciTech Connect

    Abboud, A.; Send, S.; Pashniak, N.; Pietsch, U.; Kirchlechner, C.; Micha, J. S.; Ulrich, O.; Keckes, J.

    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.

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

    PubMed

    Abboud, A; Kirchlechner, C; Send, S; Micha, J S; Ulrich, O; Pashniak, N; Strüder, L; Keckes, J; Pietsch, U

    2014-11-01

    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. PMID:25430118

  11. The Analysis of Particles at Low Accelerating Voltages (≤ 10 kV) With Energy Dispersive X-Ray Spectroscopy (EDS)

    PubMed Central

    Small, J. A.

    2002-01-01

    In recent years, there have been a series of advancements in electron beam instruments and x-ray detectors which may make it possible to improve significantly the quality of results from the quantitative electron-probe analysis of individual particles. These advances include: (1) field-emission gun electron beam instruments such as scanning electron microscopes (FEG-SEMs) that have high brightness electron guns with excellent performance at low beam energies, E0 ≤ 10 keV and (2) high-resolution energy-dispersive x-ray spectrometers, like the microcalorimeter detector, that provide high-resolution (< 10 eV) parallel x-ray collection. These devices make it possible to separate low energy (< 4 keV) x-ray lines including the K lines of carbon, nitrogen and oxygen and the L and M lines for elements with atomic numbers in the range of 25 to 83. In light of these advances, this paper investigates the possibility of using accelerating voltages ≤ 10 kV, as a method to improve the accuracy of elemental analysis for micrometer-sized particles.

  12. In-situ X-ray characterization of the reaction of lithium with InSe

    SciTech Connect

    Levy-Clement, C.; Dahn, J.R.; McKinnon, W.R.; Rioux, J.

    1984-12-01

    The reaction at room temperature of Li with InSe in Li/InSe electrochemical cells was studied using in-situ X-ray diffraction. Li reacts with InSe first to form Li/sub 2/Se and In, then reacts with the In to form InLi. An intermediate phase appears in each of these two steps. The first intermediate phase may be an intercalation compound Li /SUB x/ InSe, the second some In-Li alloy.

  13. In-Situ Silver Acetylide Silver Nitrate Explosive Deposition Measurements Using X-Ray Fluorescence.

    SciTech Connect

    Covert, Timothy Todd

    2014-09-01

    The Light Initiated High Explosive facility utilized a spray deposited coating of silver acetylide - silver nitrate explosive to impart a mechanical shock into targets of interest. A diagnostic was required to measure the explosive deposition in - situ. An X - ray fluorescence spectrometer was deployed at the facility. A measurement methodology was developed to measure the explosive quantity with sufficient accuracy. Through the use of a tin reference material under the silver based explosive, a field calibration relationship has been developed with a standard deviation of 3.2 % . The effect of the inserted tin material into the experiment configuration has been explored.

  14. In situ x-ray diffraction of shock-driven deformation and phase transformation in titanium

    NASA Astrophysics Data System (ADS)

    Bolme, Cynthia; Lazicki, Amy; Brown, Don; Gleason, Arianna; Cerreta, Ellen; Morrow, Ben; Ali, Suzanne; Swift, Damian; Nagler, Bob; Galtier, Eric; Granados, Eduardo; Milathianaki, Despina; Heimann, Phil

    2015-06-01

    Titanium alloys are employed in demanding engineering applications due to their high strength-to-weight ratio and their resistance to corrosion. Pure titanium and titanium with high levels of oxygen impurities were studied under laser-driven shock compression at the Matter in Extreme Conditions endstation at the Linac Coherent Light Source. In situ x-ray diffraction data were acquired during compression, showing the lattice-level response of titanium as it underwent plastic deformation and phase transformation. The kinetics of these processes and the influence of oxygen impurities on the deformation behavior will be presented.

  15. In-situ x-ray absorption study of copper films in ground watersolutions

    SciTech Connect

    Kvashnina, K.O.; Butorin, S.M.; Modin, A.; Soroka, I.; Marcellini, M.; Nordgren, J.; Guo, J.-H.; Werme, L.

    2007-10-29

    This study illustrates how the damage from copper corrosion can be reduced by modifying the chemistry of the copper surface environment. The surface modification of oxidized copper films induced by chemical reaction with Cl{sup -} and HCO{sub 3}{sup -} in aqueous solutions was monitored by in situ X-ray absorption spectroscopy. The results show that corrosion of copper can be significantly reduced by adding even a small amount of sodium bicarbonate. The studied copper films corroded quickly in chloride solutions, whereas the same solution containing 1.1 mM HCO{sub 3}{sup -} prevented or slowed down the corrosion processes.

  16. In situ X-ray absorption study of copper films in ground water solutions

    NASA Astrophysics Data System (ADS)

    Kvashnina, K. O.; Butorin, S. M.; Modin, A.; Soroka, I.; Marcellini, M.; Nordgren, J.; Guo, J.-H.; Werme, L.

    2007-10-01

    This study illustrates how the damage from copper corrosion can be reduced by modifying the chemistry of the copper surface environment. The surface modification of oxidized copper films induced by chemical reaction with Cl - and HCO3- in aqueous solutions was monitored by in situ X-ray absorption spectroscopy. The results show that corrosion of copper can be significantly reduced by adding even a small amount of sodium bicarbonate. The studied copper films corroded quickly in chloride solutions, whereas the same solution containing 1.1 mM HCO3- prevented or slowed down the corrosion processes.

  17. Development of a speckle-based portable device for in situ metrology of synchrotron X-ray mirrors

    PubMed Central

    Kashyap, Yogesh; Wang, Hongchang; Sawhney, Kawal

    2016-01-01

    A portable device for in situ metrology of synchrotron X-ray mirrors based on the near-field speckle scanning technique has been developed. Ultra-high angular sensitivity is achieved by scanning a piece of abrasive paper or filter membrane in the X-ray beam. In addition to the compact setup and ease of implementation, a user-friendly graphical user interface has been developed to ensure that optimizing active X-ray mirrors is simple and fast. The functionality and feasibility of this device have been demonstrated by characterizing and optimizing X-ray mirrors. PMID:27577767

  18. Development of a speckle-based portable device for in situ metrology of synchrotron X-ray mirrors.

    PubMed

    Kashyap, Yogesh; Wang, Hongchang; Sawhney, Kawal

    2016-09-01

    A portable device for in situ metrology of synchrotron X-ray mirrors based on the near-field speckle scanning technique has been developed. Ultra-high angular sensitivity is achieved by scanning a piece of abrasive paper or filter membrane in the X-ray beam. In addition to the compact setup and ease of implementation, a user-friendly graphical user interface has been developed to ensure that optimizing active X-ray mirrors is simple and fast. The functionality and feasibility of this device have been demonstrated by characterizing and optimizing X-ray mirrors. PMID:27577767

  19. [Energy-dispersive x-ray fluorescence spectrometry--a forensic chemistry method for determination of shooting distance].

    PubMed

    Havel, J

    2003-10-01

    The article follows up the experiences Energo-dispersive X-ray fluorescence spectrometry (EDXRF) as the forensic necrochemical method as the tool for detection of metals (gunshot residues--GSR) in connection with gunshot-wounds of persons--authors: dipl. Ing. J. Havel and dipl. Ing. K. Zelenka and Energo-dispersive X-ray fluorescence spectrometry (EDXRF) as the forensic method as the tool for identification of inlets (gunshot--entries) and outlets (gunshot--exits)--author: dipl. Ing. J. Havel. PMID:14661530

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

    SciTech Connect

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

    1987-01-01

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

  1. In situ azimuthal rotation device for linear dichroism measurements in scanning transmission x-ray microscopy

    NASA Astrophysics Data System (ADS)

    Hernández-Cruz, D.; Hitchcock, A. P.; Tyliszczak, T.; Rousseau, M.-E.; Pézolet, M.

    2007-03-01

    A novel miniature rotation device used in conjunction with a scanning transmission x-ray microscope is described. It provides convenient in situ sample rotation to enable measurements of linear dichroism at high spatial resolution. The design, fabrication, and mechanical characterization are presented. This device has been used to generate quantitative maps of the spatial distribution of the orientation of proteins in several different spider and silkworm silks. Specifically, quantitative maps of the dichroic signal at the C 1s→π*amide transition in longitudinal sections of the silk fibers give information about the spatial orientation, degree of alignment, and spatial distribution of protein peptide bonds. A new approach for analyzing the dichroic signal to extract orientation distributions, in addition to magnitudes of aligned components, is presented and illustrated with results from Nephila clavipes dragline spider silk measured using the in situ rotation device.

  2. Mass Spectrometry Guided In Situ Proteolysis to Obtain Crystals for X-ray Structure Determination

    SciTech Connect

    Gheyi, Tarun; Rodgers, Logan; Romero, Richard; Sauder, J. Michael; Burley, Stephen K.

    2012-04-30

    A strategy for increasing the efficiency of protein crystallization/structure determination with mass spectrometry has been developed. This approach combines insights from limited proteolysis/mass spectrometry and crystallization via in situ proteolysis. The procedure seeks to identify protease-resistant polypeptide chain segments from purified proteins on the time-scale of crystal formation, and subsequently crystallizing the target protein in the presence of the optimal protease at the right relative concentration. We report our experience with 10 proteins of unknown structure, two of which yielded high-resolution X-ray structures. The advantage of this approach comes from its ability to select only those structure determination candidates that are likely to benefit from application of in situ proteolysis, using conditions most likely to result in formation of a stable proteolytic digestion product suitable for crystallization.

  3. Experimental novaculite deformation: interpretation of in-situ X-ray diffraction data using EPSC models

    NASA Astrophysics Data System (ADS)

    Thomas, S.; Willenweber, A.; Cline, C. J.; Sas, M.; Pape, D.; Erickson, B.; Bright, T.; Burnley, P. C.

    2012-12-01

    The deformation behavior of fine-grained polycrystalline quartz (novaculite) was studied experimentally using in-situ X-ray diffraction and theoretically by elastic plastic self consistent modeling (EPSC). Previous experimental work has shown that different subpopulations of crystals experience different stress levels during high pressure deformation and reflection stresses may lead to poor approximations of macroscopic sample stresses, since in-situ diffraction data originates from grain scale phenomena rather than macroscopic sample properties [1]. In this context EPSC models have been utilized to interpret diffraction data, i.e., to independently derive the macroscopic sample load and to directly compare results with diffraction data. In our study a series of novaculite samples with 645 ± 50 wt ppm H2O was deformed in different regimes of disclocation-creep, at 2.5 GPa and up to ~1000 °C, in the D-DIA apparatus at the NSLS X17B2 beamline. In-situ synchrotron X-ray diffraction was used to monitor the sample stress state during controlled deformation and to observe the strain behavior of the individual lattice reflections of novaculite. Lattice strains were calculated from measured lattice spacings. The macroscopic sample strain was determined by sample radiographs. The strains provide information about how individual grains or grain populations react to stress depending on their orientation within the aggregate. We observe a reproducible elastic slope across the series of experiments and a temperature dependence of individual lattice strains and yield strength. In addition, EPSC models were calculated to theoretically determine macroscopic sample stresses and to match measured rheological sample properties with simulations. Depending on deformation conditions measured elastic lattice strains could be matched by activating basal and/or prism and/or pyramidal slip systems of the crystal structure. Here, we present EPSC models, compare macroscopic stresses

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

    SciTech Connect

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

    2015-05-14

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

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

    PubMed Central

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

    2015-01-01

    The lipid cubic phase (LCP) continues to grow in popularity as a medium in which to generate crystals of membrane (and soluble) proteins for high-resolution X-ray crystallographic structure determination. To date, the PDB includes 227 records attributed to the LCP or in meso method. Among the listings are some of the highest profile membrane proteins, including the β2-adrenoreceptor–Gs protein complex that figured in the award of the 2012 Nobel Prize in Chemistry to Lefkowitz and Kobilka. The most successful in meso protocol to date uses glass sandwich crystallization plates. Despite their many advantages, glass plates are challenging to harvest crystals from. However, performing in situ X-ray diffraction measurements with these plates is not practical. Here, an alternative approach is described that provides many of the advantages of glass plates and is compatible with high-throughput in situ measurements. The novel in meso in situ serial crystallography (IMISX) method introduced here has been demonstrated with AlgE and PepT (alginate and peptide transporters, respectively) as model integral membrane proteins and with lysozyme as a test soluble protein. Structures were solved by molecular replacement and by experimental phasing using bromine SAD and native sulfur SAD methods to resolutions ranging from 1.8 to 2.8 Å using single-digit microgram quantities of protein. That sulfur SAD phasing worked is testament to the exceptional quality of the IMISX diffraction data. The IMISX method is compatible with readily available, inexpensive materials and equipment, is simple to implement and is compatible with high-throughput in situ serial data collection at macromolecular crystallography synchrotron beamlines worldwide. Because of its simplicity and effectiveness, the IMISX approach is likely to supplant existing in meso crystallization protocols. It should prove particularly attractive in the area of ligand screening for drug discovery and development. PMID

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

    PubMed

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

    2015-06-01

    The lipid cubic phase (LCP) continues to grow in popularity as a medium in which to generate crystals of membrane (and soluble) proteins for high-resolution X-ray crystallographic structure determination. To date, the PDB includes 227 records attributed to the LCP or in meso method. Among the listings are some of the highest profile membrane proteins, including the β2-adrenoreceptor-Gs protein complex that figured in the award of the 2012 Nobel Prize in Chemistry to Lefkowitz and Kobilka. The most successful in meso protocol to date uses glass sandwich crystallization plates. Despite their many advantages, glass plates are challenging to harvest crystals from. However, performing in situ X-ray diffraction measurements with these plates is not practical. Here, an alternative approach is described that provides many of the advantages of glass plates and is compatible with high-throughput in situ measurements. The novel in meso in situ serial crystallography (IMISX) method introduced here has been demonstrated with AlgE and PepT (alginate and peptide transporters, respectively) as model integral membrane proteins and with lysozyme as a test soluble protein. Structures were solved by molecular replacement and by experimental phasing using bromine SAD and native sulfur SAD methods to resolutions ranging from 1.8 to 2.8 Å using single-digit microgram quantities of protein. That sulfur SAD phasing worked is testament to the exceptional quality of the IMISX diffraction data. The IMISX method is compatible with readily available, inexpensive materials and equipment, is simple to implement and is compatible with high-throughput in situ serial data collection at macromolecular crystallography synchrotron beamlines worldwide. Because of its simplicity and effectiveness, the IMISX approach is likely to supplant existing in meso crystallization protocols. It should prove particularly attractive in the area of ligand screening for drug discovery and development. PMID:26057665

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

    NASA Astrophysics Data System (ADS)

    Chakraborty, R.; Serdy, J.; West, B.; Stuckelberger, M.; Lai, B.; Maser, J.; Bertoni, M. I.; Culpepper, M. L.; Buonassisi, T.

    2015-11-01

    In situ characterization of micro- and nanoscale defects in polycrystalline thin-film materials is required to elucidate the physics governing defect formation and evolution during photovoltaic device fabrication and operation. X-ray fluorescence spectromicroscopy is particularly well-suited to study defects in compound semiconductors, as it has a large information depth appropriate to study thick and complex materials, is sensitive to trace amounts of atomic species, and provides quantitative elemental information, non-destructively. Current in situ methods using this technique typically require extensive sample preparation. In this work, we design and build an in situ temperature stage to study defect kinetics in thin-film solar cells under actual processing conditions, requiring minimal sample preparation. Careful selection of construction materials also enables controlled non-oxidizing atmospheres inside the sample chamber such as H2Se and H2S. Temperature ramp rates of up to 300 °C/min are achieved, with a maximum sample temperature of 600 °C. As a case study, we use the stage for synchrotron X-ray fluorescence spectromicroscopy of CuInxGa1-xSe2 (CIGS) thin-films and demonstrate predictable sample thermal drift for temperatures 25-400 °C, allowing features on the order of the resolution of the measurement technique (125 nm) to be tracked while heating. The stage enables previously unattainable in situ studies of nanoscale defect kinetics under industrially relevant processing conditions, allowing a deeper understanding of the relationship between material processing parameters, materials properties, and device performance.

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

    SciTech Connect

    Chakraborty, R. E-mail: buonassisi@mit.edu; Serdy, J.; Culpepper, M. L.; Buonassisi, T. E-mail: buonassisi@mit.edu; West, B.; Stuckelberger, M.; Bertoni, M. I.; Lai, B.; Maser, J.

    2015-11-15

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

  9. ENERGY DISPERSIVE X-RAY FLUORESCENCE ANALYSIS OF DUST COLLECTED USING A VERTICAL ELUTRIATOR COTTON DUST SAMPLER

    EPA Science Inventory

    X-ray fluorescence (XRF) spectroscopy has been used to analyze trace element concentrations in cotton dusts collected on verticle elutriator filter media. Twenty-three samples collected from ten bales of cotton processed in a model card room have been analyzed. The major elements...

  10. An analytic model for the response of a CZT detector in diagnostic energy dispersive x-ray spectroscopy

    SciTech Connect

    LeClair, Robert J.; Wang Yinkun; Zhao Peiying; Boileau, Michel; Wang, Lilie; Fleurot, Fabrice

    2006-05-15

    A CdZnTe detector (CZTD) can be very useful for measuring diagnostic x-ray spectra. The semiconductor detector does, however, exhibit poor hole transport properties and fluorescence generation upon atomic de-excitations. This article describes an analytic model to characterize these two phenomena that occur when a CZTD is exposed to diagnostic x rays. The analytical detector response functions compare well with those obtained via Monte Carlo calculations. The response functions were applied to 50, 80, and 110 kV x-ray spectra. Two 50 kV spectra were measured; one with no filtration and the other with 1.35 mm Al filtration. The unfiltered spectrum was numerically filtered with 1.35 mm of Al in order to see whether the recovered spectrum resembled the filtered spectrum actually measured. A deviation curve was obtained by subtracting one curve from the other on an energy bin by bin basis. The deviation pattern fluctuated around the zero line when corrections were applied to both spectra. Significant deviations from zero towards the lower energies were observed when the uncorrected spectra were used. Beside visual observations, the exposure obtained using the numerically attenuated unfiltered beam was compared to the exposure calculated with the actual filtered beam. The percent differences were 0.8% when corrections were applied and 25% for no corrections. The model can be used to correct diagnostic x-ray spectra measured with a CdZnTe detector.

  11. Simulations of in situ x-ray diffraction from uniaxially compressed highly textured polycrystalline targets

    SciTech Connect

    McGonegle, David Wark, Justin S.; Higginbotham, Andrew; Milathianaki, Despina; Remington, Bruce A.

    2015-08-14

    A growing number of shock compression experiments, especially those involving laser compression, are taking advantage of in situ x-ray diffraction as a tool to interrogate structure and microstructure evolution. Although these experiments are becoming increasingly sophisticated, there has been little work on exploiting the textured nature of polycrystalline targets to gain information on sample response. Here, we describe how to generate simulated x-ray diffraction patterns from materials with an arbitrary texture function subject to a general deformation gradient. We will present simulations of Debye-Scherrer x-ray diffraction from highly textured polycrystalline targets that have been subjected to uniaxial compression, as may occur under planar shock conditions. In particular, we study samples with a fibre texture, and find that the azimuthal dependence of the diffraction patterns contains information that, in principle, affords discrimination between a number of similar shock-deformation mechanisms. For certain cases, we compare our method with results obtained by taking the Fourier transform of the atomic positions calculated by classical molecular dynamics simulations. Illustrative results are presented for the shock-induced α–ϵ phase transition in iron, the α–ω transition in titanium and deformation due to twinning in tantalum that is initially preferentially textured along [001] and [011]. The simulations are relevant to experiments that can now be performed using 4th generation light sources, where single-shot x-ray diffraction patterns from crystals compressed via laser-ablation can be obtained on timescales shorter than a phonon period.

  12. In situ high-resolution X-ray photoelectron spectroscopy - Fundamental insights in surface reactions

    NASA Astrophysics Data System (ADS)

    Papp, Christian; Steinrück, Hans-Peter

    2013-11-01

    Since the advent of third generation synchrotron light sources optimized for providing soft X-rays up to 2 keV, X-ray photoelectron spectroscopy (XPS) has been developed to be an outstanding tool to study surface properties and surface reactions at an unprecedented level. The high resolution allows identifying various surface species, and for small molecules even the vibrational fine structure can be resolved in the XP spectra. The high photon flux reduces the required measuring time per spectrum to the domain of a few seconds or even less, which enables to follow surface processes in situ. Moreover, it also provides access to very small coverages down to below 0.1% of a monolayer, enabling the investigation of minority species or processes at defect sites. The photon energy can be adjusted according to the requirement of a particular experiment, i.e., to maximize or minimize the surface sensitivity or the photoionization cross-section of the substrate or the adsorbate. For a few instruments worldwide, a next step forward was taken by combining in situ high-resolution spectrometers with supersonic molecular beams. These beams allow to control and vary the kinetic and internal energies of the incident molecules and provide a local pressure of up to ~10-5 mbar, which can be switched on and off in a controllable way, thus offering a well-defined time structure to study adsorption or reaction processes.

  13. An experimental system for high temperature X-ray diffraction studies with in situ mechanical loading

    PubMed Central

    Oswald, Benjamin B.; Schuren, Jay C.; Pagan, Darren C.; Miller, Matthew P.

    2013-01-01

    An experimental system with in situ thermomechanical loading has been developed to enable high energy synchrotron x-ray diffraction studies of crystalline materials. The system applies and maintains loads of up to 2250 N in uniaxial tension or compression at a frequency of up to 100 Hz. The furnace heats the specimen uniformly up to a maximum temperature of 1200 °C in a variety of atmospheres (oxidizing, inert, reducing) that, combined with in situ mechanical loading, can be used to mimic processing and operating conditions of engineering components. The loaded specimen is reoriented with respect to the incident beam of x-rays using two rotational axes to increase the number of crystal orientations interrogated. The system was used at the Cornell High Energy Synchrotron Source to conduct experiments on single crystal silicon and polycrystalline Low Solvus High Refractory nickel-based superalloy. The data from these experiments provide new insights into how stresses evolve at the crystal scale during thermomechanical loading and complement the development of high-fidelity material models. PMID:23556825

  14. In situ x-ray photoemission studies of the oxidation of Y-Ba-Cu films

    SciTech Connect

    Price, R.J.; Jackman, R.B.; Foord, J.S.

    1988-12-15

    X-ray photoemission has been used to investigate the formation of Y-Ba-Cu films on Si(100) and as an in situ probe of their subsequent oxidation to yield the associated oxide ceramic. The layers are prepared by coevaporation of the metallic components under ultrahigh vacuum, and pure alloy phases can be deposited at 300 K; reaction with the underlying substrate resulting in loss of Cu and incorporation by Si in the film takes place, however, at higher temperatures. Room-temperature oxidation stabilizes the film against this interaction and results in the preferential oxidation and surface segregation of barium at the expense of Cu. This segregation process becomes even more apparent during higher temperature (approx.600 K) oxidation reactions. Chemical shifts and associated effects in x-ray photoelectron spectra are used to infer information on the chemical changes that occur in the film as oxidation proceeds. The thin-film phases prepared in situ in this work reveal a very similar surface composition to bulk superconducting samples prepared ex situ. This suggests that the surface segregation in bulk samples does not simply result from reaction with species such as water vapor, but instead may represent an equilibrium state of the oxide-oxygen interface.

  15. In Situ X-ray Reflectivity Studies of Protein Adsorption onto Functionalized Surfaces

    NASA Astrophysics Data System (ADS)

    Richter, Andrew

    2007-03-01

    The adsorption of protein films onto solid surfaces, both artificial and naturally occurring, have been widely studied using a variety of techniques due to their importance in medicine, biomedical applications, and the general understanding of protein structure and function. What have yet to be performed are in situ, time-resolved, high-resolution structural studies of these systems. We have begun a project that uses the technique of in situ x-ray reflectivity to obtain highly resolved structural information with time resolution on the order of minutes. This talk will present our first findings of serum albumin and immunoglobulin G films on hydrophobic self-assembled monolayers. The protein films are readily observable, showing extensive denaturing after adsorption with a slow decay of density into the aqueous solution. Additionally, a thin low-density region that occurs between the hydrophobic film and the solution persists after protein deposition. Comparisons to films that are removed from solution, the influence of solution concentration, the effects of x-ray damage, and the time scales for protein film formation and evolution will also be discussed.

  16. Scanning electron microscopy/energy dispersive spectrometry fixedbeam or overscan x-ray microanalysis of particles can miss the real structure: x-ray spectrum image mapping reveals the true nature

    NASA Astrophysics Data System (ADS)

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

    2013-05-01

    The typical strategy for analysis of a microscopic particle by scanning electron microscopy/energy dispersive spectrometry x-ray microanalysis (SEM/EDS) is to use a fixed beam placed at the particle center or to continuously overscan to gather an "averaged" x-ray spectrum. While useful, such strategies inevitably concede any possibility of recognizing microstructure within the particle, and such fine scale structure is often critical for understanding the origins, behavior, and fate of particles. Elemental imaging by x-ray mapping has been a mainstay of SEM/EDS analytical practice for many years, but the time penalty associated with mapping with older EDS technology has discouraged its general use and reserved it more for detailed studies that justified the time investment. The emergence of the high throughput, high peak stability silicon drift detector (SDD-EDS) has enabled a more effective particle mapping strategy: "flash" x-ray spectrum image maps can now be recorded in seconds that capture the spatial distribution of major (concentration, C > 0.1 mass fraction) and minor (0.01 <= C <= 0.1) constituents. New SEM/SDD-EDS instrument configurations feature multiple SDDs that view the specimen from widely spaced azimuthal angles. Multiple, simultaneous measurements from different angles enable x-ray spectrometry and mapping that can minimize the strong geometric effects of particles. The NIST DTSA-II software engine is a powerful aid for quantitatively analyzing EDS spectra measured individually as well as for mapping information (available free for Java platforms at: http://www.cstl.nist.gov/div837/837.02/epq/dtsa2/index.html).

  17. Relationship between dislocations and residual stresses in cold-drawn pearlitic steel analyzed by energy-dispersive X-ray diffraction

    SciTech Connect

    Sato, Shigeo; Wagatsuma, Kazuaki; Suzuki, Shigeru; Kumagai, Masayoshi; Imafuku, Muneyuki; Tashiro, Hitoshi; Kajiwara, Kentaro; Shobu, Takahiasa

    2013-09-15

    We analyzed the dislocation distribution of cold-drawn pearlitic-steel wire by using the line-profile analysis based on the energy dispersive X-ray diffraction (EDXD). Although this line-profile analysis requires a high resolution in reciprocal space, the resolution for EDXD is generally poor due to the energy resolution of the detector. Our analysis demonstrated that the resolution in the reciprocal space can be maximized at small scattering angles. Using the line-profile analysis based on the EDXD, the microstructural parameters such as the crystallite size and the dislocation density of the ferrite phase in the pearlitic steel were successfully analyzed. In addition, the distribution of the residual stress of the ferrite phase of a pearlitic steel wire was also analyzed using the EDXD measurement. - Highlights: • Energy dispersive X-ray diffraction is applied to the line-profile analysis. • Distribution of dislocations in ferrite in the pearlitic steel wire is analyzed. • Relationship between dislocations and residual stress is discussed.

  18. Development of in-line furnace for in-situ nanoscale resolution x-ray microscopy

    NASA Astrophysics Data System (ADS)

    Eng, Christopher; Chen-Wiegart, Yu-Chen K.; Wang, Jun

    2013-09-01

    Full field transmission x-ray microscopy (TXM) is a newly developed x-ray imaging technique to provide quantitative and non-destructive 3D characterization of the complex microstructure of materials at nanometer resolution. A key missing component is an in situ apparatus enabling the imaging of the complex structural evolution of the materials and to correlate the structural change with a material's functionality under real operating conditions. This work describes the design of an environmental cell which satisfies the requirements for in situ TXM studies. The limited space within the TXM presents a spatial constraint which prohibits the use of conventional heaters, as well as requiring consideration in designing for safe and controlled operation of the system and alignment of the cell with the beam. A gravity drip-fed water cooling jacket was installed in place around the heating module to maintain critical components of the microscope at safe operating temperatures. A motion control system consisting of pulse width modulated DC motor driven XYZ translation stages was developed to facilitate fine alignment of the cell. Temperature of the sample can be controlled remotely and accurately through a controller to temperatures as high as 1200 K. Heating zone measurement was carried out and shows a 500 x 500 x 500 μm3 homogeneous zone volume for sample area, which is a critical parameter to ensure accurate observation of structural evolution at nanometer scale with a sample in size of tens of microns. Application on Ni particles for in situ oxidation experiment and dehydrogenation of aluminum hydride is also discussed.

  19. Misidentification of major constituents by automatic qualitative energy dispersive X-ray microanalysis: a problem that threatens the credibility of the analytical community.

    PubMed

    Newbury, Dale E

    2005-12-01

    Automatic qualitative analysis for peak identification is a standard feature of virtually all modern computer-aided analysis software for energy dispersive X-ray spectrometry with electron excitation. Testing of recently installed systems from four different manufacturers has revealed the occasional occurrence of misidentification of peaks of major constituents whose concentrations exceeded 0.1 mass fraction (10 wt%). Test materials where peak identification failures were observed included ZnS, KBr, FeS2, tantalum-niobium alloy, NIST Standard Reference Material 482 (copper-gold alloy), Bi2Te3, uranium-rhodium alloys, platinum-chromium alloy, GaAs, and GaP. These misidentifications of major constituents were exacerbated when the incident beam energy was 10 keV or lower, which restricted or excluded the excitation of the high photon energy K- and L-shell X-rays where multiple peaks, for example, Kalpha (K-L2,3)-Kbeta (K-M2,3); Lalpha (L3-M4,5)-Lbeta (L2-M4)-Lgamma (L2-N4), are well resolved and amenable to identification with high confidence. These misidentifications are so severe as to properly qualify as blunders that present a serious challenge to the credibility of this critical analytical technique. Systematic testing of a peak identification system with a suite of diverse materials can reveal the specific elements and X-ray peaks where failures are likely to occur. PMID:17481333

  20. Misidentification of Major Constituents by Automatic Qualitative Energy Dispersive X-ray Microanalysis: A Problem that Threatens the Credibility of the Analytical Community

    NASA Astrophysics Data System (ADS)

    Newbury*, Dale E.

    2005-12-01

    Automatic qualitative analysis for peak identification is a standard feature of virtually all modern computer-aided analysis software for energy dispersive X-ray spectrometry with electron excitation. Testing of recently installed systems from four different manufacturers has revealed the occasional occurrence of misidentification of peaks of major constituents whose concentrations exceeded 0.1 mass fraction (10 wt%). Test materials where peak identification failures were observed included ZnS, KBr, FeS2, tantalum-niobium alloy, NIST Standard Reference Material 482 (copper gold alloy), Bi2Te3, uranium rhodium alloys, platinum chromium alloy, GaAs, and GaP. These misidentifications of major constituents were exacerbated when the incident beam energy was 10 keV or lower, which restricted or excluded the excitation of the high photon energy K- and L-shell X-rays where multiple peaks, for example, K[alpha] (K-L2,3) K[beta] (K-M2,3); L[alpha] (L3-M4,5) L[beta] (L2-M4) L[gamma] (L2-N4), are well resolved and amenable to identification with high confidence. These misidentifications are so severe as to properly qualify as blunders that present a serious challenge to the credibility of this critical analytical technique. Systematic testing of a peak identification system with a suite of diverse materials can reveal the specific elements and X-ray peaks where failures are likely to occur.

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

    NASA Astrophysics Data System (ADS)

    Steffen, S.; Otto, M.; Niewoehner, L.; Barth, M.; Bro¿żek-Mucha, Z.; Biegstraaten, J.; Horváth, R.

    2007-09-01

    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.

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

    NASA Astrophysics Data System (ADS)

    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).

  3. Atomic Structure of Pt3Ni Nanoframe Electrocatalysts by in Situ X-ray Absorption Spectroscopy.

    PubMed

    Becknell, Nigel; Kang, Yijin; Chen, Chen; Resasco, Joaquin; Kornienko, Nikolay; Guo, Jinghua; Markovic, Nenad M; Somorjai, Gabor A; Stamenkovic, Vojislav R; Yang, Peidong

    2015-12-23

    Understanding the atomic structure of a catalyst is crucial to exposing the source of its performance characteristics. It is highly unlikely that a catalyst remains the same under reaction conditions when compared to as-synthesized. Hence, the ideal experiment to study the catalyst structure should be performed in situ. Here, we use X-ray absorption spectroscopy (XAS) as an in situ technique to study Pt3Ni nanoframe particles which have been proven to be an excellent electrocatalyst for the oxygen reduction reaction (ORR). The surface characteristics of the nanoframes were probed through electrochemical hydrogen underpotential deposition and carbon monoxide electrooxidation, which showed that nanoframe surfaces with different structure exhibit varying levels of binding strength to adsorbate molecules. It is well-known that Pt-skin formation on Pt-Ni catalysts will enhance ORR activity by weakening the binding energy between the surface and adsorbates. Ex situ and in situ XAS results reveal that nanoframes which bind adsorbates more strongly have a rougher Pt surface caused by insufficient segregation of Pt to the surface and consequent Ni dissolution. In contrast, nanoframes which exhibit extremely high ORR activity simultaneously demonstrate more significant segregation of Pt over Ni-rich subsurface layers, allowing better formation of the critical Pt-skin. This work demonstrates that the high ORR activity of the Pt3Ni hollow nanoframes depends on successful formation of the Pt-skin surface structure. PMID:26652294

  4. Neighborite Under High Pressure: In Situ Angle Dispersive X-ray Diffraction Study Using Synchrotron Radiation

    NASA Astrophysics Data System (ADS)

    Liu, H.; Chen, J.; Weidner, D.; Hu, J.; Meng, Y.; Mao, H.

    2003-12-01

    The neighborite (NaMgF3) is an ideal analogue model for silicate perovskite (MgSiO3) due to the similarities between their crystal and electronic structures. The advantage of the analogue study is that the weaker bonding feature of neighborite grants us the opportunity to simulate behavior of silicate perovskite at lower mantlei. e.high pressure and high temperature condition, at relatively lower P-T conditions. The previous high pressure studies for neighborite were reported by Zhao et al [1, 2]. Energy dispersive x-ray diffraction data were achieved within 10GPa and 1000oC, while angle dispersive x-ray diffraction data were obtained only at 4.9GPa and room temperature.More information of atomic position change is required to reveal the role of MgF6 octahedral framework tilting during its phase transition process responding to heating andcompressing. Thus the high-resolution monochromatic x-ray powder diffraction studies on NaMgF3 perovskite at high pressure were carried out using diamond anvil cell at X17C of National Synchrotron Light Source (Brookhaven) and HPCAT of Advance Photon Source (Argonne). The orthorhombic structure keeps stable under pressure up to 30 GPa, and the crystal structure is refined using Rietveld method. The result indicates that tilting angle of the MgF6 octahedral framework increases continually while the octahedral Mg-F bond length decreases slightly with increasing pressure.Difference between the tilting angles derived from macro-structure (lattice parameters) and from micro-structure (atomic positions), as well as the trend of change in the tilting angle with temperature and pressureare discussed. [1]. Zhao YS, Weidner DJ, Ko JD, Leinenweber K, Liu X, Li BS, Meng Y,Pacalo REG, Vaughan MT, Wang YB, Yeganehhaeri A,J.Geophys. Res. Solid Earth, 99 (1994) 2871. [2]. Zhao YS, Parise JB, Wang YB, Kusaba K, Vaughan MT, Weidner DJ, Kikegawa T, Chen J, Shimomura O,Am.Miner., 79 (1994) 615.

  5. Calibration of a compact XUV soft X-ray monochromator with a digital autocollimator in situ.

    PubMed

    Yuh, Jih Young; Lin, Shang Wei; Huang, Liang Jen; Lee, Long Life

    2016-09-01

    A digital autocollimator of resolution 0.1 µrad (0.02 arcsec) serves as a handy correction tool for calibrating the angular uncertainty during angular and lateral movements of gratings inside a monochromator chamber under ultra-high vacuum. The photon energy dispersed from the extreme ultraviolet (XUV) to the soft X-ray region of the synchrotron beamline at the Taiwan Light Source was monitored using molecular ionization spectra at high resolution as energy references that correlate with the fine angular steps during grating rotation. The angular resolution of the scanning mechanism was <0.3 µrad, which results in an energy shift of 80 meV at 867 eV. The angular uncertainties caused by the lateral movement during a grating exchange were decreased from 2.2 µrad to 0.1 µrad after correction. The proposed method provides a simple solution for on-site beamline diagnostics of highly precise multi-axis optical manipulating instruments at synchrotron facilities and in-house laboratories. PMID:27577780

  6. Near-isothermal furnace for in situ and real time X-ray radiography solidification experiments.

    PubMed

    Becker, M; Dreißigacker, C; Klein, S; Kargl, F

    2015-06-01

    In this paper, we present a newly developed near-isothermal X-ray transparent furnace for in situ imaging of solidification processes in thin metallic samples. We show that the furnace is ideally suited to study equiaxed microstructure evolution and grain interaction. To observe the growth dynamics of equiaxed dendritic structures, a minimal temperature gradient across the sample is required. A uniform thermal profile inside a circular sample is achieved by positioning the sample in the center of a cylindrical furnace body surrounded by a circular heater arrangement. Performance tests with the hypo-eutectic Al-15wt.%Cu and the near-eutectic Al-33wt.%Cu alloys validate the near-isothermal character of the sample environment. Controlled cooling rates of less than 0.5 K min(-1) up to 10 K min(-1) can be achieved in a temperature range of 720 K-1220 K. Integrated in our rotatable laboratory X-ray facility, X-RISE, the furnace provides a large field of view of 10.5 mm in diameter and a high spatial resolution of ∼4 μm. With the here presented furnace, equiaxed dendrite growth models can be rigorously tested against experiments on metal alloys by, e.g., enabling dendrite growth velocities to be determined as a function of undercooling or solutal fields in front of the growing dendrite to be measured. PMID:26133847

  7. Near-isothermal furnace for in situ and real time X-ray radiography solidification experiments

    NASA Astrophysics Data System (ADS)

    Becker, M.; Dreißigacker, C.; Klein, S.; Kargl, F.

    2015-06-01

    In this paper, we present a newly developed near-isothermal X-ray transparent furnace for in situ imaging of solidification processes in thin metallic samples. We show that the furnace is ideally suited to study equiaxed microstructure evolution and grain interaction. To observe the growth dynamics of equiaxed dendritic structures, a minimal temperature gradient across the sample is required. A uniform thermal profile inside a circular sample is achieved by positioning the sample in the center of a cylindrical furnace body surrounded by a circular heater arrangement. Performance tests with the hypo-eutectic Al-15wt.%Cu and the near-eutectic Al-33wt.%Cu alloys validate the near-isothermal character of the sample environment. Controlled cooling rates of less than 0.5 K min-1 up to 10 K min-1 can be achieved in a temperature range of 720 K-1220 K. Integrated in our rotatable laboratory X-ray facility, X-RISE, the furnace provides a large field of view of 10.5 mm in diameter and a high spatial resolution of ˜4 μm. With the here presented furnace, equiaxed dendrite growth models can be rigorously tested against experiments on metal alloys by, e.g., enabling dendrite growth velocities to be determined as a function of undercooling or solutal fields in front of the growing dendrite to be measured.

  8. Near-isothermal furnace for in situ and real time X-ray radiography solidification experiments

    SciTech Connect

    Becker, M. Dreißigacker, C.; Klein, S.; Kargl, F.

    2015-06-15

    In this paper, we present a newly developed near-isothermal X-ray transparent furnace for in situ imaging of solidification processes in thin metallic samples. We show that the furnace is ideally suited to study equiaxed microstructure evolution and grain interaction. To observe the growth dynamics of equiaxed dendritic structures, a minimal temperature gradient across the sample is required. A uniform thermal profile inside a circular sample is achieved by positioning the sample in the center of a cylindrical furnace body surrounded by a circular heater arrangement. Performance tests with the hypo-eutectic Al-15wt.%Cu and the near-eutectic Al-33wt.%Cu alloys validate the near-isothermal character of the sample environment. Controlled cooling rates of less than 0.5 K min{sup −1} up to 10 K min{sup −1} can be achieved in a temperature range of 720 K–1220 K. Integrated in our rotatable laboratory X-ray facility, X-RISE, the furnace provides a large field of view of 10.5 mm in diameter and a high spatial resolution of ∼4 μm. With the here presented furnace, equiaxed dendrite growth models can be rigorously tested against experiments on metal alloys by, e.g., enabling dendrite growth velocities to be determined as a function of undercooling or solutal fields in front of the growing dendrite to be measured.

  9. An apparatus for in situ x-ray scattering measurements during polymer injection molding

    NASA Astrophysics Data System (ADS)

    Rendon, Stanley; Fang, Jun; Burghardt, Wesley R.; Bubeck, Robert A.

    2009-04-01

    We report a novel instrument for synchrotron-based in situ x-ray scattering measurements during injection molding processing. It allows direct, real-time monitoring of molecular-scale structural evolution in polymer materials undergoing a complex processing operation. The instrument is based on a laboratory-scale injection molding machine, and employs customized mold tools designed to allow x-ray access during mold filling and subsequent solidification, while providing sufficient robustness to withstand high injection pressures. The use of high energy, high flux synchrotron radiation, and a fast detector allows sufficiently rapid data acquisition to resolve time-dependent orientation dynamics in this transient process. Simultaneous monitoring of temperature and pressure signals allows transient scattering data to be referenced to various stages of the injection molding cycle. Representative data on a commercial liquid crystalline polymer, Vectra® B950, are presented to demonstrate the features of this apparatus; however, it may find application in a wide range of polymeric materials such as nanocomposites, semicrystalline polymers and fiber-reinforced thermoplastics.

  10. Use of x-ray fluorescence for in-situ detection of metals

    NASA Astrophysics Data System (ADS)

    Elam, W. T. E.; Whitlock, Robert R.; Gilfrich, John V.

    1995-01-01

    X-ray fluorescence (XRF) is a well-established, non-destructive method of determining elemental concentrations at ppm levels in complex samples. It can operate in atmosphere with no sample preparation, and provides accuracies of 1% or better under optimum conditions. This report addresses two sets of issues concerning the use of x-ray fluorescence as a sensor technology for the cone penetrometer, for shipboard waste disposal, or for other in-situ, real- time environmental applications. The first issue concerns the applicability of XRF to these applications, and includes investigation of detection limits and matrix effects. We have evaluated the detection limits and quantitative accuracy of a sensor mock-up for metals in soils under conditions expected in the field. In addition, several novel ways of improving the lower limits of detection to reach the drinking water regulatory limits have been explored. The second issue is the engineering involved with constructing a spectrometer within the 1.75 inch diameter of the penetrometer pipe, which is the most rigorous physical constraint. Only small improvements over current state-of-the-art are required. Additional advantages of XRF are that no radioactive sources or hazardous materials are used in the sensor design, and no reagents or any possible sources of ignition are involved.

  11. Kinetics of Methane Hydrate Decomposition Studied via in Situ Low Temperature X-ray Powder Diffraction

    SciTech Connect

    Everett, Susan M; Rawn, Claudia J; Keffer, David J.; Mull, Derek L; Payzant, E Andrew; Phelps, Tommy Joe

    2013-01-01

    Gas hydrates are known to have a slowed decomposition rate at ambient pressure and temperatures below the melting point of ice termed self-preservation or anomalous preservation. As hydrate exothermically decomposes, gas is released and water of the clathrate cages transforms into ice. Two regions of slowed decomposition for methane hydrate, 180 200 K and 230 260 K, were observed, and the kinetics were studied by in situ low temperature x-ray powder diffraction. The kinetic constants for ice formation from methane hydrate were determined by the Avrami model within each region and activation energies, Ea, were determined by the Arrhenius plot. Ea determined from the data for 180 200 K was 42 kJ/mol and for 230 260 K was 22 kJ/mol. The higher Ea in the colder temperature range was attributed to a difference in the microstructure of ice between the two regions.

  12. In-situ x-ray characterization of wurtzite formation in GaAs nanowires

    SciTech Connect

    Krogstrup, Peter; Hannibal Madsen, Morten; Nygaard, Jesper; Feidenhans'l, Robert; Hu Wen; Kozu, Miwa; Nakata, Yuka; Takahasi, Masamitu

    2012-02-27

    In-situ monitoring of the crystal structure formation during Ga-assisted GaAs nanowire growth on Si(111) substrates has been performed in a combined molecular beam epitaxy growth and x-ray characterization experiment. Under Ga rich conditions, we show that an increase in the V/III ratio increases the formation rate of the wurtzite structure. Moreover, the response time for changes in the structural phase formation to changes in the beam fluxes is observed to be much longer than predicted time scales of adatom kinetics and liquid diffusion. This suggests that the morphology of the growth interface plays the key role for the relative growth structure formation rates.

  13. Hydride reorientation in Zircaloy-4 examined by in situ synchrotron X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Weekes, H. E.; Jones, N. G.; Lindley, T. C.; Dye, D.

    2016-09-01

    The phenomenon of stress-reorientation has been investigated using in situ X-ray diffraction during the thermomechanical cycling of hydrided Zircaloy-4 tensile specimens. Results have shown that loading along a sample's transverse direction (TD) leads to a greater degree of hydride reorientation when compared to rolling direction (RD)-aligned samples. The elastic lattice micro-strains associated with radially oriented hydrides have been revealed to be greater than those oriented circumferentially, a consequence of strain accommodation. Evidence of hydride redistribution after cycling, to α-Zr grains oriented in a more favourable orientation when under an applied stress, has also been observed and its behaviour has been found to be highly dependent on the loading axis. Finally, thermomechanical loading across multiple cycles has been shown to reduce the difference in terminal solid solubility of hydrogen during dissolution (TSSD,H) and precipitation (TSSP,H).

  14. In situ surface X-ray scattering of stepped surface of platinum: Pt(311).

    PubMed

    Nakahara, Akira; Nakamura, Masashi; Sumitani, Kazushi; Sakata, Osami; Hoshi, Nagahiro

    2007-10-23

    Surface structure of a stepped surface of Pt, Pt(311) (=2(100)-(111)), has been determined under potential control in 0.1 M HClO4 with the use of in situ surface X-ray scattering (SXS). The crystal truncation rods (CTRs) are reproduced well with the (1x2) missing-row model. Relaxation of surface layers, which is observed on the low-index planes of Pt, is not found on Pt(311) in the "adsorbed hydrogen region". CTRs at 0.10 (RHE) have the same feature as those at 0.50 V, showing that the surface layers of Pt(311) have no potential dependence. Scanning tunneling microscopy (STM) also supports the (1x2) structure of Pt(311) in 0.1 M HClO4. PMID:17902717

  15. Tracking the catalyzed growth process of nanowires by in situ x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Kirkham, Melanie; Wang, Zhong Lin; Snyder, Robert L.

    2010-07-01

    Quasi-one-dimensional nanostructures of silicon, oxides, and other materials show great promise for a variety of applications. These nanostructures are commonly grown using metal catalyst nanoparticles. This paper investigates the growth mechanism of Au-catalyzed Si nanowires through in situ x-ray diffraction, and the results are compared to previously studied Au-catalyzed ZnO nanorods. The Si nanowires were found to grow from molten catalyst particles, however, the ZnO nanorods were found to grow from solid catalyst particles through a surface diffusion process. From this comparison, the relative bonding types of the catalyst and source material are determined to have a significant effect on the growth mechanism.

  16. In situ X-ray polymerization: from swollen lamellae to polymer-surfactant complexes.

    PubMed

    Agzenai, Yahya; Lindman, Björn; Alfredsson, Viveka; Topgaard, Daniel; Renamayor, Carmen S; Pacios, Isabel E

    2014-01-30

    The influence of the monomer diallyldimethylammonium chloride (D) on the lamellar liquid crystal formed by the anionic surfactant aerosol OT (AOT) and water is investigated, determining the lamellar spacings by SAXS and the quadrupolar splittings by deuterium NMR, as a function of the D or AOT concentrations. The cationic monomer D induces a destabilization of the AOT lamellar structure such that, at a critical concentration higher than 5 wt %, macroscopic phase separation takes place. When the monomer, which is dissolved in the AOT lamellae, is polymerized in situ by X-ray initiation, a new collapsed lamellar phase appears, corresponding to the complexation of the surfactant with the resulting polymer. A theoretical model is employed to analyze the variation of the interactions between the AOT bilayers and the stability of the lamellar structure. PMID:24410395

  17. In situ synchrotron x-ray studies of LiMn{sub 2}O{sub 4} cathodes

    SciTech Connect

    McBreen, J.; Mukerjee, S.; Yang, X.Q.

    1997-05-01

    LiCoO{sub 2} cathodes are now used in most commercial lithium ion batteries. LiMn{sub 2}O{sub 4} is an attractive low cost alternative. However, it is difficult to make reproducibly. At Brookhaven National Laboratory two in situ synchrotron x-ray techniques, that are available at the National Synchrotron Light Source (NSLS), have been used to investigate LiMn{sub 2}O{sub 4}. The techniques are x-ray absorption and high resolution x-ray diffraction. With x-ray absorption it is possible to follow the changes in the Mn oxidation state and the changes in the Mn-O and Mn-Mn bond lengths on cycling. Also it is possible to detect amorphous phases. The high energy x-rays at the diffraction Beam Lines at the NSLS (up to 24 KeV) permit in situ x-ray diffraction, in the transmission mode, in thin lithium and lithium ion cells. The evolution of the structural chances that occur on cycling can be followed. These in situ measurements were done on Li/LiMn{sub 2}O{sub 4} cells with a liquid electrolyte (1 M LiPF{sub 6} in a 1:1:3 PC:EC:DMC solvent).

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

    SciTech Connect

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

    2003-01-24

    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 {mu}g 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.

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

    NASA Astrophysics Data System (ADS)

    Rojas-Rodriguez, I.; Herrera, A.; Vázquez-López, C.; Apolo, R.; González-Hernández, J.; Hernández-Landaverde, M. A.; Rodriguez, M. E.

    2004-02-01

    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.

  20. Determination of heavy metals in suspended waste water collected from Oued El Harrach Algiers River by Energy Dispersive X-Ray Fluorescence

    NASA Astrophysics Data System (ADS)

    Ouziane, S.; Amokrane, A.; Toumert, I.

    2013-12-01

    A preliminary study of the atmospheric pollution in the centre of Algiers is one of the important fields of applications in the environmental science. Nowadays, we need to evaluate the level of the contamination which has an unfavourable effect on physicochemical properties of soils and plants and namely also on human health. In the present work, water samples collected from Oued El-Harrach Algiers River, have been filtered in 0.45 μm Millipore filters to be analysed by Energy Dispersive X-Ray Fluorescence technique using 109Cd radioisotope source. Concentrations of the toxic elements like heavy metals are determined and compared with the published ones values by Yoshida [1] and those obtained using PIXE and NAA techniques [6].

  1. Atomic-Resolution X-ray Energy-Dispersive Spectroscopy Chemical Mapping of Substitutional Dy Atoms in a High-Coercivity Neodymium Magnet

    NASA Astrophysics Data System (ADS)

    Itakura, Masaru; Watanabe, Natsuki; Nishida, Minoru; Daio, Takeshi; Matsumura, Syo

    2013-05-01

    We have investigated local element distributions in a Dy-doped Nd2Fe14B hot-deformed magnet by atomic-column resolution chemical mapping using an X-ray energy-dispersive spectrometer (XEDS) attached to an aberration-corrected scanning transmission electron microscope (Cs-corrected STEM). The positions of the Nd and Dy atomic columns were visualized in the XEDS maps. The substitution of Dy was limited to a surface layer 2-3 unit cells thick in the Nd2Fe14B grains, and the Dy atoms preferentially occupied the 4f-Nd sites of Nd2Fe14B. These results provide further insights into the principal mechanism governing the coercivity enhancement due to Dy doping.

  2. Peritoneal "melanosis" associated with a ruptured ovarian dermoid cyst: report of a case with electron-probe energy dispersive X-ray analysis.

    PubMed

    Jaworski, R C; Boadle, R; Greg, J; Cocks, P

    2001-10-01

    A case of peritoneal "melanosis" due to a ruptured left ovarian dermoid cyst is described. Histology showed that the dermoid contained gastric mucosa associated with ulceration, necrosis, and hemorrhage. The areas of pigmentation within the dermoid, omentum, and peritoneal cavity were due to collections of heavily pigment-laden macrophages. The pigment lacked the histochemical features of either melanin or hemosiderin, but electron-probe energy dispersive x-ray analysis showed that the pigment contained a high concentration of iron. It is postulated that peptic ulceration with hemorrhage is the most likely source of the pigment and that the peritoneal pigmentation is secondary to spillage of the contents of the dermoid cyst. PMID:11603224

  3. Remineralization of demineralized enamel by toothpastes: a scanning electron microscopy, energy dispersive X-ray analysis, and three-dimensional stereo-micrographic study.

    PubMed

    Gjorgievska, Elizabeta S; Nicholson, John W; Slipper, Ian J; Stevanovic, Marija M

    2013-06-01

    Remineralization of hard dental tissues is thought to be a tool that could close the gap between prevention and surgical procedures in clinical dentistry. The purpose of this study was to examine the remineralizing potential of different toothpaste formulations: toothpastes containing bioactive glass, hydroxyapatite, or strontium acetate with fluoride, when applied to demineralized enamel. Results obtained by scanning electron microscopy (SEM) and SEM/energy dispersive X-ray analyses proved that the hydroxyapatite and bioactive glass-containing toothpastes were highly efficient in promoting enamel remineralization by formation of deposits and a protective layer on the surface of the demineralized enamel, whereas the toothpaste containing 8% strontium acetate and 1040 ppm fluoride as NaF had little, if any, remineralization potential. In conclusion, the treatment of demineralized teeth with toothpastes containing hydroxyapatite or bioactive glass resulted in repair of the damaged tissue. PMID:23659606

  4. Thickness measurement of semiconductor thin films by energy dispersive X-ray fluorescence benchtop instrumentation: Application to GaN epilayers grown by molecular beam epitaxy

    NASA Astrophysics Data System (ADS)

    Queralt, I.; Ibañez, J.; Marguí, E.; Pujol, J.

    2010-07-01

    The importance of thin films in modern high technology products, such as semiconductors, requires fast and non-destructive analysis. A methodology to determine the thickness of single layers with benchtop energy dispersive X-ray fluorescence (EDXRF) instrumentation is described and tested following analytical validation criteria. The experimental work was carried out on gallium nitride thin films epitaxially grown on sapphire substrate. The results of samples with layers in the range from 400 to 1000 nm exhibit a good correlation with the layer thickness determined by optical reflectance. Spectral data obtained using thin layered samples indicate the possibility to precisely evaluate layer thickness from 5 nm, with a low relative standard deviation (RSD < 2%) of the results. In view of the limits of optical reflectance for very thin layer determination, EDXRF analysis offers the potential for the thickness determination of such kind of samples.

  5. Effects of Pamidronate on Dental Enamel Formation Assessed by Light Microscopy, Energy-Dispersive X-Ray Analysis, Scanning Electron Microscopy, and Microhardness Testing.

    PubMed

    Soares, Ana P; do Espírito Santo, Renan F; Line, Sérgio R P; Pinto, Maria das G F; Santos, Pablo de M; Toralles, Maria Betania P; do Espírito Santo, Alexandre R

    2016-06-01

    The aim of the present work was to investigate birefringence and morphology of the secretory-stage enamel organic extracellular matrix (EOECM), and structural and mechanical properties of mature enamel of upper incisors from adult rats that had been treated with pamidronate disodium (0.5 mg/kg/week for 56 days), using transmitted polarizing and bright-field light microscopies (TPLM and BFLM), energy-dispersive X-ray (EDX) analysis, scanning electron microscopy (SEM) and microhardness testing. BFLM showed no morphological changes of the EOECM in pamidronate and control groups, but TPLM revealed a statistically significant reduction in optical retardation values of birefringence brightness of pamidronate-treated rats when compared with control animals (p0.05). The present study indicates that pamidronate can affect birefringence of the secretory-stage EOECM, which does not seem to be associated with significant changes in morphological and/or mechanical properties of mature enamel. PMID:27212049

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

    NASA Astrophysics Data System (ADS)

    Pitarch, A.; Queralt, I.; Alvarez-Perez, A.

    2011-02-01

    Between the years 1808 and 1814, the Spanish War of Independence took place. This period, locally known as "Guerra del Francès", 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.

  7. Liver concentrations of copper, zinc, iron and molybdenum in sheep and goats from northern Greece, determined by energy-dispersive X-ray fluorescence spectrometry.

    PubMed

    Papachristodoulou, Christina; Stamoulis, Konstantinos; Tsakos, Panagiotis; Vougidou, Christina; Vozikis, Vasileios; Papadopoulou, Chrissanthy; Ioannides, Konstantinos

    2015-04-01

    Energy-dispersive X-Ray fluorescence spectrometry was used to determine the concentrations of copper (Cu), zinc, iron and molybdenum in the liver of 76 sheep and goats from the regions of Macedonia-Thrace, northern Greece. In general, metal concentrations were in the adequate range, with one main exception of Cu-deficiency observed in all of the examined goat liver samples and Cu-toxicity found in 4 % of the sheep liver samples. One-way analysis of variance was carried out to determine significant differences among means depending on animal species, sex and age. Pearson correlation analysis was used to explore correlations between metal concentrations. The results obtained in the present study are discussed in the framework of diagnostic ranges, suggested for classifying the metal status of sheep and goats, and are compared with liver metal concentrations reported world-wide. PMID:25694162

  8. In Situ Density Measurement of Basaltic Melts at High Pressure by X-ray Absorption Method

    NASA Astrophysics Data System (ADS)

    Ando, R.; Ohtani, E.; Suzuki, A.; Urakawa, S.; Katayama, Y.

    2004-12-01

    Density of silicate melt at high pressure is one of the most important properties to understand magma migration in the planetary interior. However, because of experimental difficulties, the density of magma at high pressure is poorly known. Katayama et al. (1996) recently developed a new in situ density measurement method for metallic melts, based on the density dependency of X-ray absorption in the sample. In this study, we tried to measure the density of basaltic melt by this absorption method. When X-ray is transmitted to the sample, the intensity of the transmitted X-ray beam (I) is expressed as follows; I=I0exp(-μ ρ t), where I0 is the intensity of incident X-ray beam, μ is the mass absorption coefficient, ρ is the density of the sample, and t is the thickness of the sample. If t and μ are known, we can determine the density of the sample by measuring I and I0. This is the principle of the absorption method for density measurement. In this study, in order to determine t, we used a single crystalline diamond cylinder as a sample capsule, diamond is less compressive and less deformable so that even at high pressure t (thickness of the sample at the point x) is expressed as follows; t = 2*(R02-x2)1/2, R0 is the inner radius of cylinder at the ambient condition, and x is distance from a center of the capsule. And diamond also shows less absorption so that this make it possible to measure the density of silicate melt with smaller absorption coefficient than metallic melts. In order to know the μ of the sample, we measured both densities (ρ ) and absorptions (I/I0) for some glasses and crystals with same composition of the sample at the ambient condition, and calculated as fallows; μ =ln(I/I0)/ρ . Experiments were made at the beamline (BL22XU) of SPring-8. For generation of high pressure and high temperature, we used DIA-type cubic anvil apparatus (SMAP180) there. We used tungsten carbide anvils with the edge-length of 6 mm. The energy of monochromatic X-ray

  9. In situ ambient pressure X-ray photoelectron spectroscopy studies of lithium-oxygen redox reactions.

    PubMed

    Lu, Yi-Chun; Crumlin, Ethan J; Veith, Gabriel M; Harding, Jonathon R; Mutoro, Eva; Baggetto, Loïc; Dudney, Nancy J; Liu, Zhi; Shao-Horn, Yang

    2012-01-01

    The lack of fundamental understanding of the oxygen reduction and oxygen evolution in nonaqueous electrolytes significantly hinders the development of rechargeable lithium-air batteries. Here we employ a solid-state Li(4+x)Ti(5)O(12)/LiPON/Li(x)V(2)O(5) cell and examine in situ the chemistry of Li-O(2) reaction products on Li(x)V(2)O(5) as a function of applied voltage under ultra high vacuum (UHV) and at 500 mtorr of oxygen pressure using ambient pressure X-ray photoelectron spectroscopy (APXPS). Under UHV, lithium intercalated into Li(x)V(2)O(5) while molecular oxygen was reduced to form lithium peroxide on Li(x)V(2)O(5) in the presence of oxygen upon discharge. Interestingly, the oxidation of Li(2)O(2) began at much lower overpotentials (~240 mV) than the charge overpotentials of conventional Li-O(2) cells with aprotic electrolytes (~1000 mV). Our study provides the first evidence of reversible lithium peroxide formation and decomposition in situ on an oxide surface using a solid-state cell, and new insights into the reaction mechanism of Li-O(2) chemistry. PMID:23056907

  10. In Situ Ambient Pressure X-ray Photoelectron Spectroscopy Studies of Lithium-Oxygen Redox Reactions

    PubMed Central

    Lu, Yi-Chun; Crumlin, Ethan J.; Veith, Gabriel M.; Harding, Jonathon R.; Mutoro, Eva; Baggetto, Loïc; Dudney, Nancy J.; Liu, Zhi; Shao-Horn, Yang

    2012-01-01

    The lack of fundamental understanding of the oxygen reduction and oxygen evolution in nonaqueous electrolytes significantly hinders the development of rechargeable lithium-air batteries. Here we employ a solid-state Li4+xTi5O12/LiPON/LixV2O5 cell and examine in situ the chemistry of Li-O2 reaction products on LixV2O5 as a function of applied voltage under ultra high vacuum (UHV) and at 500 mtorr of oxygen pressure using ambient pressure X-ray photoelectron spectroscopy (APXPS). Under UHV, lithium intercalated into LixV2O5 while molecular oxygen was reduced to form lithium peroxide on LixV2O5 in the presence of oxygen upon discharge. Interestingly, the oxidation of Li2O2 began at much lower overpotentials (~240 mV) than the charge overpotentials of conventional Li-O2 cells with aprotic electrolytes (~1000 mV). Our study provides the first evidence of reversible lithium peroxide formation and decomposition in situ on an oxide surface using a solid-state cell, and new insights into the reaction mechanism of Li-O2 chemistry. PMID:23056907

  11. Oxidation Induced Doping of Nanoparticles Revealed by in Situ X-ray Absorption Studies.

    PubMed

    Kwon, Soon Gu; Chattopadhyay, Soma; Koo, Bonil; Dos Santos Claro, Paula Cecilia; Shibata, Tomohiro; Requejo, Félix G; Giovanetti, Lisandro J; Liu, Yuzi; Johnson, Christopher; Prakapenka, Vitali; Lee, Byeongdu; Shevchenko, Elena V

    2016-06-01

    Doping is a well-known approach to modulate the electronic and optical properties of nanoparticles (NPs). However, doping at nanoscale is still very challenging, and the reasons for that are not well understood. We studied the formation and doping process of iron and iron oxide NPs in real time by in situ synchrotron X-ray absorption spectroscopy. Our study revealed that the mass flow of the iron triggered by oxidation is responsible for the internalization of the dopant (molybdenum) adsorbed at the surface of the host iron NPs. The oxidation induced doping allows controlling the doping levels by varying the amount of dopant precursor. Our in situ studies also revealed that the dopant precursor substantially changes the reaction kinetics of formation of iron and iron oxide NPs. Thus, in the presence of dopant precursor we observed significantly faster decomposition rate of iron precursors and substantially higher stability of iron NPs against oxidation. The same doping mechanism and higher stability of host metal NPs against oxidation was observed for cobalt-based systems. Since the internalization of the adsorbed dopant at the surface of the host NPs is driven by the mass transport of the host, this mechanism can be potentially applied to introduce dopants into different oxidized forms of metal and metal alloy NPs providing the extra degree of compositional control in material design. PMID:27152970

  12. In Situ Ambient Pressure X-ray Photoelectron Spectroscopy Studies of Lithium-Oxygen Redox Reactions

    NASA Astrophysics Data System (ADS)

    Lu, Yi-Chun; Crumlin, Ethan J.; Veith, Gabriel M.; Harding, Jonathon R.; Mutoro, Eva; Baggetto, Loïc; Dudney, Nancy J.; Liu, Zhi; Shao-Horn, Yang

    2012-10-01

    The lack of fundamental understanding of the oxygen reduction and oxygen evolution in nonaqueous electrolytes significantly hinders the development of rechargeable lithium-air batteries. Here we employ a solid-state Li4+xTi5O12/LiPON/LixV2O5 cell and examine in situ the chemistry of Li-O2 reaction products on LixV2O5 as a function of applied voltage under ultra high vacuum (UHV) and at 500 mtorr of oxygen pressure using ambient pressure X-ray photoelectron spectroscopy (APXPS). Under UHV, lithium intercalated into LixV2O5 while molecular oxygen was reduced to form lithium peroxide on LixV2O5 in the presence of oxygen upon discharge. Interestingly, the oxidation of Li2O2 began at much lower overpotentials (~240 mV) than the charge overpotentials of conventional Li-O2 cells with aprotic electrolytes (~1000 mV). Our study provides the first evidence of reversible lithium peroxide formation and decomposition in situ on an oxide surface using a solid-state cell, and new insights into the reaction mechanism of Li-O2 chemistry.

  13. Dynamics of barite growth in porous media quantified by in situ synchrotron X-ray tomography

    NASA Astrophysics Data System (ADS)

    Godinho, jose; Gerke, kirill

    2016-04-01

    Current models used to formulate mineral sequestration strategies of dissolved contaminants in the bedrock often neglect the effect of confinement and the variation of reactive surface area with time. In this work, in situ synchrotron X-ray micro-tomography is used to quantify barite growth rates in a micro-porous structure as a function of time during 13.5 hours with a resolution of 1 μm. Additionally, the 3D porous network at different time frames are used to simulate the flow velocities and calculate the permeability evolution during the experiment. The kinetics of barite growth under porous confinement is compared with the kinetics of barite growth on free surfaces in the same fluid composition. Results are discussed in terms of surface area normalization and the evolution of flow velocities as crystals fill the porous structure. During the initial hours the growth rate measured in porous media is similar to the growth rate on free surfaces. However, as the thinner flow paths clog the growth rate progressively decreases, which is correlated to a decrease of local flow velocity. The largest pores remain open, enabling growth to continue throughout the structure. Quantifying the dynamics of mineral precipitation kinetics in situ in 4D, has revealed the importance of using a time dependent reactive surface area and accounting for the local properties of the porous network, when formulating predictive models of mineral precipitation in porous media.

  14. A standards-based method for compositional analysis by energy dispersive X-ray spectrometry using multivariate statistical analysis: application to multicomponent alloys.

    PubMed

    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. PMID:23298470

  15. Fast elemental screening of soil and sediment profiles using small-spot energy-dispersive X-ray fluorescence: application to mining sediments geochemistry.

    PubMed

    Gonzalez-Fernandez, Oscar; Queralt, Ignacio

    2010-09-01

    Elemental analysis of different sediment cores originating from the Cartagena-La Union mining district in Spain was carried out by means of a programmable small-spot energy-dispersive X-ray fluorescence (EDXRF) spectrometer to study the distribution of heavy metals along soil profiles. Cores were obtained from upstream sediments of a mining creek, from the lowland sedimentation plain, and from a mining landfill dump (tailings pile). A programmable two-dimensional (2D) stage and a focal spot resolution of 600 μm allow us to obtain complete core mapping. Geochemical results were verified using a more powerful wavelength-dispersion X-ray fluorescence (WDXRF) technique. The data obtained was processed in order to study the statistical correlations within the elemental compositions. The results obtained allow us to observe the differential in-depth distribution of heavy metals among the sampled zones. Dump site cores exhibit a homogeneous distribution of heavy metals, whereas the alluvial plain core shows accumulation of heavy metals in the upper part. This approach can be useful for the fast screening of heavy metals in depositional environments around mining sites. PMID:20828442

  16. Alterations of the intracellular water and ion concentrations in brain and liver cells during aging as revealed by energy dispersive X-ray microanalysis of bulk specimens

    SciTech Connect

    Lustyik, G.; Nagy, I.

    1985-01-01

    Age dependence of the intracellular concentrations of monovalent ions (Na+, K+ and Cl-) was examined in 1, 11 and 25-month-old rat brain and liver cells by using energy dispersive X-ray microanalysis. The in vivo concentrations of Na+, K+ and Cl- ions were calculated from two different measurements: The elemental concentrations were measured in freeze-dried tissue pieces, and the intracellular water content was determined by means of a recently developed X-ray microanalytic method, using frozen-hydrated and fractured bulk specimens as well as subsequent freeze-drying. All the single monovalent ion concentrations and consequently, also the total monovalent ion content showed statistically significant increases during aging in brain cortical neurons. A 3-6% loss of the intracellular water content was accompanied by a 25-45% increase of the monovalent ionic strengths by the age of 25 months. A membrane protective OH radical scavenger (centrophenoxine) reversed the dehydration in the nerve cells of old animals, resulting in a decrease of the intracellular ion concentrations. Aging has a less prominent effect on the water and ion contents of the hepatocytes. The degree of water loss of cytoplasm exceeds that of the nuclei in the liver, suggesting that dominantly the translational steps can be involved in the general age altered slowing down of the protein synthetic machinery, predicted by the membrane hypothesis of aging.

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

    NASA Astrophysics Data System (ADS)

    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.

  18. Combination of electron energy-loss spectroscopy and energy dispersive x-ray spectroscopy to determine indium concentration in InGaN thin film structures

    NASA Astrophysics Data System (ADS)

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

    2015-11-01

    We demonstrate a method to determine the indium concentration, x, of In x Ga1-x N thin films by combining plasmon excitation studies in electron energy-loss spectroscopy (EELS) with a novel way of quantification of the intensity of x-ray lines in energy-dispersive x-ray spectroscopy (EDXS). The plasmon peak in EELS of InGaN is relatively broad. We fitted a Lorentz function to the main plasmon peak to suppress noise and the influence from the neighboring Ga 3d transition in the spectrum, which improves the precision in the evaluation of the plasmon peak position. As the indium concentration of InGaN is difficult to control during high temperature growth due to partial In desorption, the nominal indium concentrations provided by the growers were not considered reliable. The indium concentration obtained from EDXS quantification using Oxford Instrument ISIS 300 x-ray standard quantification software often did not agree with the nominal indium concentration, and quantification using K and L lines was inconsistent. We therefore developed a self-consistent iterative procedure to determine the In content from thickness-dependent k-factors, as described in recent work submitted to Journal of Microscopy. When the plasmon peak position is plotted versus the indium concentration from EDXS we obtain a linear relationship over the whole compositional range, and the standard error from linear least-squares fitting shows that the indium concentration can be determined from the plasmon peak position to within Δx = ± 0.037 standard deviation.

  19. Data of low-dose phase-based X-ray imaging for in situ soft tissue engineering assessments

    PubMed Central

    Izadifar, Zohreh; Honaramooz, Ali; Wiebe, Sheldon; Belev, George; Chen, Xiongbiao; Chapman, Dean

    2016-01-01

    This article presents the data of using three phase-based X-ray imaging techniques to characterize biomaterial scaffold and soft tissues in situ, as reported in our study “Low-dose phase-based X-ray imaging techniques for in situ soft tissue engineering assessments” [1]. The examined parameters include the radiation dose, scan time, and image quality, which are all critical to longitudinal in situ live animal assessments. The data presented were obtained from three dimensional imaging of scaffolds in situ cartilage by means of synchrotron-based computed tomography-diffraction enhanced imaging (CT-DEI), analyzer based imaging (CT-ABI), and in-line phase contrast imaging (CT-PCI) at standard and low dose imaging modalities. PMID:26909381

  20. Data of low-dose phase-based X-ray imaging for in situ soft tissue engineering assessments.

    PubMed

    Izadifar, Zohreh; Honaramooz, Ali; Wiebe, Sheldon; Belev, George; Chen, Xiongbiao; Chapman, Dean

    2016-03-01

    This article presents the data of using three phase-based X-ray imaging techniques to characterize biomaterial scaffold and soft tissues in situ, as reported in our study "Low-dose phase-based X-ray imaging techniques for in situ soft tissue engineering assessments" [1]. The examined parameters include the radiation dose, scan time, and image quality, which are all critical to longitudinal in situ live animal assessments. The data presented were obtained from three dimensional imaging of scaffolds in situ cartilage by means of synchrotron-based computed tomography-diffraction enhanced imaging (CT-DEI), analyzer based imaging (CT-ABI), and in-line phase contrast imaging (CT-PCI) at standard and low dose imaging modalities. PMID:26909381

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

    NASA Astrophysics Data System (ADS)

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

    1999-06-01

    Thermoelectrically cooled semiconductor detectors, such as Si-PIN, Si-drift, Cd1-xZnxTe 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 2×3 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- xZn xTe 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 pollution

  2. In-situ non-ambient X-ray diffraction studies of indium tungstate

    SciTech Connect

    Baiz, Tamam I.; Heinrich, Christophe P.; Banek, Nathan A.; Vivekens, Boris L.; Lind, Cora

    2012-03-15

    In situ variable temperature and high pressure X-ray diffraction studies were carried out on indium tungstate (In{sub 2}W{sub 3}O{sub 12}). This material displays positive volume expansion in both its low temperature monoclinic and high temperature orthorhombic phases, with negative thermal expansion along the a axis and positive thermal expansion along the b and c axes. Upon hydrostatic compression in a diamond anvil cell, one crystalline to crystalline phase transition is observed in the range 1.9 to 2.7 GPa, and progressive irreversible amorphization occurs at pressures above 4.3 GPa. The crystalline high pressure phase appears to be isostructural to previously observed high pressure phases in other A{sub 2}M{sub 3}O{sub 12} compounds. - Graphical abstract: Variable pressure X-ray diffraction patterns of In{sub 2}W{sub 3}O{sub 12} collected in a diamond anvil cell. A phase transition is clearly observed between 2.2 and 2.7 GPa, followed by irreversible amorphization. Highlights: Black-Right-Pointing-Pointer The structure of In{sub 2}W{sub 3}O{sub 12} was studied as a function of temperature and pressure. Black-Right-Pointing-Pointer Uniaxial negative thermal expansion was observed above 250 Degree-Sign C. Black-Right-Pointing-Pointer A pressure-induced phase transition occurred between 2.2 and 2.7 GPa. Black-Right-Pointing-Pointer Pressure-induced irreversible amorphization was observed above 4.3 GPa.

  3. High-pressure behavior and thermoelastic properties of niobium studied by in situ x-ray diffraction

    SciTech Connect

    Zou, Yongtao E-mail: yongtaozou6@gmail.com; Li, Baosheng; Qi, Xintong; Wang, Xuebing; Chen, Ting; Li, Xuefei; Welch, David

    2014-07-07

    In situ synchrotron energy dispersive x-ray diffraction (XRD) experiments on Nb have been conducted at pressures up to 6.4 GPa and temperatures up to 1073 K. From the pressure-volume-temperature measurements, thermoelastic parameters were derived for the first time for Nb based on the thermal pressure (ΔP{sub th}) equation of state (EOS), modified high-T Birch-Murnaghan EOS, and Mie-Grüneisen-Debye EOS. With the pressure derivative of the bulk modulus K{sub T}{sup ´} fixed at 4.0, we obtained the ambient isothermal bulk modulus K{sub T0}=174(5) GPa, the temperature derivative of bulk modulus at constant pressure (∂K{sub T}/∂T){sub P}=-0.060(8) GPa K⁻¹ and at constant volume (∂K{sub T}/∂T){sub V}=-0.046(8) GPa K⁻¹, the volumetric thermal expansivity α{sub T}(T)=2.3(3)×10⁻⁵+0.3(2)×10⁻⁸T (K⁻¹), as well as the pressure dependence of thermal expansion (∂α/∂P){sub T}=(₋2.0±0.4)×10⁻⁶ K⁻¹ GPa⁻¹. Fitting the present data to the Mie-Grüneisen-Debye EOS with Debye temperature Θ₀=276.6 K gives γ₀=1.27(8) and K{sub T0}=171(3) GPa at a fixed value of q=3.0. The ambient isothermal bulk modulus and Grüneisen parameter derived from this work are comparable to previously reported values from both experimental and theoretical studies. An in situ high-resolution, angle dispersive XRD study on Nb did not indicate any anomalous behavior related to pressure-induced electronic topological transitions at ~5 GPa as has been reported previously.

  4. An in situ XAFS study--the formation mechanism of gold nanoparticles from X-ray-irradiated ionic liquid.

    PubMed

    Ma, Jingyuan; Zou, Yang; Jiang, Zheng; Huang, Wei; Li, Jiong; Wu, Guozhong; Huang, Yuying; Xu, Hongjie

    2013-07-28

    An in situ X-ray absorption fine structure (XAFS) experiment has been performed to observe the evolution of gold nanoparticles in the ionic liquid [BMIM][AuCl4], by hard X-ray irradiation. The ionic liquid acts as both a reducing agent and a protective ligand. A synchrotron-based X-ray plays the role of the irradiation source, which induces the reduction of the gold species, as well as being a real time probe for XAFS measurements. From the extended X-ray absorption fine structure (EXAFS) fitting results for a series of spectra of gold L3-edge, it can be seen clearly that there is a single Au-Cl bond breaking process before the formation of Au-Au bonds, which is different from previous reports on the formation of Au nanoparticles by several chemical methods. PMID:23765109

  5. Synchrotron X-Ray Microprobe In-Situ Analysis of Extraterrestrial Particles Collected in Aerogel on the MIR Space Station

    NASA Technical Reports Server (NTRS)

    Flynn, G. J.; Sutton, S. R.; Horz, F.

    2000-01-01

    Using in-situ x-ray fluorescence, we determined the Cr/Fe, Mn/Fe and Ni/Fe of a particle captured in aerogel on MIR are approximately chondritic, indicating an extraterrestrial origin. Impurity of the aerogel precluded determining the Cu and Zn.

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

    SciTech Connect

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

    1998-11-01

    system definitely requires an in situ XRD technique to study the detail structural changes of the system during charge and discharge. The in situ XRD technique was used by Reimers, Li,and Dahn to study the LiCoO{sub 2}, LiNiO{sub 2}, and LiMn{sub 2}O{sub 4} systems. Their results of these studies have demonstrated that in situ XRD can provide more detailed information about the cathode material structural changes during charge-discharge. Conventional x-ray sources were used in these studies and the beryllium windows were used in the in situ cells. Provisions were made to prevent corrosion of the beryllium windows during charge-discharge. For this reason, the in situ cells were often designed quite differently than a real battery. More seriously, the problem of beryllium corrosion restricted the voltage range of the cell below 4.5 V. This limited the use of this technique to study the effects of overcharge which is very important to the thermal stability of the cathodes. Using the plastic lithium battery technology, Amatucci, Tarascon, and Klein constructed an in situ XRD cell, which allows structural investigations at voltages greater than 5 V without any beryllium window corrosion. However, all of these in situ XRD studies using conventional x-ray sources probe the cell in reflection geometry. Therefore, the observed structural changes are predominantly from the top few microns of the electrode coating, which might not be representative for the whole coating during charge-discharge especially when the rate is high.

  7. Non-destructive in situ study of "Mad Meg" by Pieter Bruegel the Elder using mobile X-ray fluorescence, X-ray diffraction and Raman spectrometers

    NASA Astrophysics Data System (ADS)

    Van de Voorde, Lien; Van Pevenage, Jolien; De Langhe, Kaat; De Wolf, Robin; Vekemans, Bart; Vincze, Laszlo; Vandenabeele, Peter; Martens, Maximiliaan P. J.

    2014-07-01

    "Mad Meg", a figure of Flemish folklore, is the subject of a famous oil-on-panel painting by the Flemish renaissance artist Pieter Bruegel the Elder, exhibited in the Museum Mayer van den Bergh (Antwerp, Belgium). This article reports on the in situ chemical characterization of this masterpiece by using currently available state-of-the-art portable analytical instruments. The applied non-destructive analytical approach involved the use of a) handheld X-ray fluorescence instrumentation for retrieving elemental information and b) portable X-ray fluorescence/X-ray diffraction instrumentation and laser-based Raman spectrometers for obtaining structural/molecular information. Next to material characterization of the used pigments and of the different preparation layers of the painting, also the verification of two important historical iconographic hypotheses is performed concerning the economic way of painting by Brueghel, and whether or not he used blue smalt pigment for painting the boat that appears towards the top of the painting. The pigments identified are smalt pigment (65% SiO2 + 15% K2O + 10% CoO + 5% Al2O3) for the blue color present in all blue areas of the painting, probably copper resinate for the green colors, vermillion (HgS) as red pigment and lead white is used to form different colors. The comparison of blue pigments used on different areas of the painting gives no differences in the elemental fingerprint which confirms the existing hypothesis concerning the economic painting method by Bruegel.

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

    PubMed

    Maddox, B R; Akin, M C; Teruya, A; Hunt, D; Hahn, D; Cradick, J; Morgan, D V

    2016-08-01

    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(7) molybdenum Kα photons. PMID:27587130

  9. In situ alkali-silica reaction observed by x-ray microscopy

    SciTech Connect

    Kurtis, K.E.; Monteiro, P.J.M.; Brown, J.T.; Meyer-Ilse, W.

    1997-04-01

    In concrete, alkali metal ions and hydroxyl ions contributed by the cement and reactive silicates present in aggregate can participate in a destructive alkali-silica reaction (ASR). This reaction of the alkalis with the silicates produces a gel that tends to imbibe water found in the concrete pores, leading to swelling of the gel and eventual cracking of the affected concrete member. Over 104 cases of alkali-aggregate reaction in dams and spillways have been reported around the world. At present, no method exists to arrest the expansive chemical reaction which generates significant distress in the affected structures. Most existing techniques available for the examination of concrete microstructure, including ASR products, demand that samples be dried and exposed to high pressure during the observation period. These sample preparation requirements present a major disadvantage for the study of alkali-silica reaction. Given the nature of the reaction and the affect of water on its products, it is likely that the removal of water will affect the morphology, creating artifacts in the sample. The purpose of this research is to observe and characterize the alkali-silica reaction, including each of the specific reactions identified previously, in situ without introducing sample artifacts. For observation of unconditioned samples, x-ray microscopy offers an opportunity for such an examination of the alkali-silica reaction. Currently, this investigation is focusing on the effect of calcium ions on the alkali-silica reaction.

  10. Boron phosphide under pressure: In situ study by Raman scattering and X-ray diffraction

    SciTech Connect

    Solozhenko, Vladimir L.; Kurakevych, Oleksandr O.; Le Godec, Yann; Kurnosov, Aleksandr V.; Oganov, Artem R.

    2014-07-21

    Cubic boron phosphide, BP, has been studied in situ by X-ray diffraction and Raman scattering up to 55 GPa at 300 K in a diamond anvil cell. The bulk modulus of B{sub 0} = 174(2) GPa has been established, which is in excellent agreement with our ab initio calculations. The data on Raman shift as a function of pressure, combined with equation-of-state (EOS) data, allowed us to estimate the Grüneisen parameters of the TO and LO modes of zinc-blende structure, γ{sub G}{sup TO }= 1.26 and γ{sub G}{sup LO }= 1.13, just like in the case of other A{sup III}B{sup V} diamond-like phases, for which γ{sub G}{sup TO }> γ{sub G}{sup LO }≅ 1. We also established that the pressure dependence of the effective electro-optical constant α is responsible for a strong change in relative intensities of the TO and LO modes from I{sub TO}/I{sub LO} ∼ 0.25 at 0.1 MPa to I{sub TO}/I{sub LO} ∼ 2.5 at 45 GPa, for which we also find excellent agreement between experiment and theory.