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

  1. [Application of in situ micro energy dispersive X-ray fluorescence analysis in mineralogy].

    PubMed

    Yang, Hai; Ge, Liang-Quan; Gu, Yi; Zhang, Qing-Xian; Xiong, Sheng-Qing

    2013-11-01

    Thirteen rock samples were collected for studying the variation of element content in the mineral during the alteration process from Xinjiang, China. The IED-6000 in situ micro energy dispersive X-ray fluorescence developed by CDUT was applied to get chemical and physical data from minerals. The non-destructive spectrometer is based on a low-power Mo-anode X-ray tube and a Si-PIN peltier cooled X-ray detector. The unique design of the tube's probe allows very close coupling of polycapillary and makes the use of micro-area measurement feasible and efficient. The spectrometer can be integrated into any microscope for analysis. The long axis diameter of beam spot is about 110 microm. According to micro-EDXRF measurement, the tetrahedrite was corrected to pyrite, improving the efficiency and accuracy of the mineral identification. The feldspar of mineralized rock sample is rich in Cu and Zn which can be used as prospecting indicator elements. Element content of Cr, Mn and Co shows negative correlation with the degree of mineralization.

  2. Geopolymerisation Kinetics. 1. In situ Energy-Dispersive X-ray Diffractometry

    SciTech Connect

    Provis,J.; van Deventer, J.

    2007-01-01

    In situ energy-dispersive X-ray diffractometry, using a polychromatic synchrotron beam and a 'laboratory-sized' sample, is used to provide a direct measurement of the kinetics of geopolymerisation. The effects of sample SiO{sub 2}/Al{sub 2}O{sub 3} ratio, Na/(Na+K) ratio and reaction temperature are investigated. The results obtained support recent propositions that the initial gel phase formed during geopolymerisation is later transformed to a second, probably more-ordered gel phase, and provide detailed information regarding the rate of formation of the first gel phase during the first 3 h of reaction. Increasing the SiO{sub 2}/Al{sub 2}O{sub 3} ratio generally decreases the initial rate of reaction, with the highest SiO{sub 2}/Al{sub 2}O{sub 3} ratio samples showing what appears to be a pause in the reaction corresponding roughly to the solidification of the geopolymeric binder. Mixed (Na,K)-aluminosilicate geopolymers with moderate SiO{sub 2}/Al{sub 2}O{sub 3} ratios behave similarly to pure Na- or K-aluminosilicate compositions of higher SiO{sub 2}/Al{sub 2}O{sub 3} ratio. Fitting a simplified first-order rate expression to the overall reaction process at different temperatures allows the calculation of an effective overall activation energy, which may be useful in comparing geopolymerisation of slurries with different compositions.

  3. X-ray Energy Dispersive Spectrometry during in-situ Liquid Cell Studies using an Analytical Electron Microscope

    SciTech Connect

    Zaluzec, Nestor J.; Burke, M. Grace; Haigh, Sarah J.; Kulzick, Matthew

    2014-04-01

    The use of analytical spectroscopies during scanning/transmission electron microscope (S/TEM) investigations of micro- and nano-scale structures has become a routine technique in the arsenal of tools available to today's materials researchers. Essential to implementation and successful application of spectroscopy to characterization is the integration of numerous technologies, which include electron optics, specimen holders, and associated detectors. While this combination has been achieved in many instrument configurations, the integration of X-ray energy-dispersive spectroscopy and in situ liquid environmental cells in the S/TEM has to date been elusive. In this work we present the successful incorporation/modifications to a system that achieves this functionality for analytical electron microscopy.

  4. Effect of hydration on the structure of solid-supported Niosomal membranes investigated by in situ energy dispersive X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Caracciolo, Giulio; Pozzi, Daniela; Caminiti, Ruggero; Marianecci, Carlotta; Moglioni, Simone; Carafa, Maria; Amenitsch, Heinz

    2008-09-01

    The supramolecular structure of Niosomal vesicles (Niosomes) made of a binary mixture of polysorbate 20 (Tween 20) and Cholesterol in aqueous solution was investigated by means of synchrotron small angle X-ray scattering (SAXS). Solid-supported Niosomal membranes at full hydration exhibit the same structural properties, as determined by in situ energy dispersive X-ray diffraction (EDXD), than their counterpart in solution. Both Niosomes and solid-supported Niosomal membranes are made of highly swollen bilayers rich in Tween 20 coexisting with Cholesterol crystallites. EDXD patterns from oriented samples suggest that at least some Cholesterol crystals are aligned along the normal to the solid support.

  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. Ability of different restorative materials to prevent in situ secondary caries: analysis by polarized light-microscopy and energy-dispersive X-ray.

    PubMed

    Paradella, Thaís Cachuté; Koga-Ito, Cristiane Yumi; Jorge, Antonio Olavo Cardoso

    2008-08-01

    Secondary caries is the main cause of direct restoration replacement. The purpose of this study was to analyze enamel adjacent to different restorative materials after in situ cariogenic challenge using polarized-light microscopy (PLM), scanning electron microscopy (SEM) and energy-dispersive X-ray analysis (EDS). Twelve volunteers, with a low level of dental plaque, a low level of mutans streptococci, and normal salivary flow, wore removable palatal acrylic appliances containing enamel specimens restored with Z250 composite, Freedom composite, Fuji IX glass-ionomer cement, or Vitremer resin-modified glass-ionomer for 14 days. Volunteers dripped one drop of 20% sucrose solution (n = 10) or distilled water (control group) onto each specimen 8 times per day. Specimens were removed from the appliances and submitted to PLM for examination of the lesion area (in mm(2)), followed by dehydration, gold-sputtering, and submission to SEM and EDS. The calcium (Ca) and phosphorus (P) contents were evaluated in weight per cent (%wt). Differences were found between Z250 and Vitremer, and between Z250 and FujiIX, when analyzed using PLM. Energy-dispersive X-ray analysis results showed differences between the studied materials regarding Ca %wt. In conclusion, enamel adjacent to glass-ionomer cement presented a higher Ca %wt, but this material did not completely prevent enamel secondary caries under in situ cariogenic challenge.

  7. Chain-length dependent growth dynamics of n-alkanes on silica investigated by energy-dispersive x-ray reflectivity in situ and in real-time

    NASA Astrophysics Data System (ADS)

    Weber, C.; Frank, C.; Bommel, S.; Rukat, T.; Leitenberger, W.; Schäfer, P.; Schreiber, F.; Kowarik, S.

    2012-05-01

    We compare the growth dynamics of the three n-alkanes C36H74, C40H82, and C44H90 on SiO2 using real-time and in situ energy-dispersive x-ray reflectivity. All molecules investigated align in an upright-standing orientation on the substrate and exhibit a transition from layer-by-layer growth to island growth after about 4 monolayers under the conditions employed. Simultaneous fits of the reflected intensity at five distinct points in reciprocal space show that films formed by longer n-alkanes roughen faster during growth. This behavior can be explained by a chain-length dependent height of the Ehrlich-Schwoebel barrier. Further x-ray diffraction measurements after growth indicate that films consisting of longer n-alkanes also incorporate more lying-down molecules in the top region. While the results reveal behavior typical for chain-like molecules, the findings can also be useful for the optimization of organic field effect transistors where smooth interlayers of n-alkanes without coexistence of two or more molecular orientations are required.

  8. Copper phosphonatoethanesulfonates: temperature dependent in situ energy dispersive X-ray diffraction study and influence of the pH on the crystal structures.

    PubMed

    Feyand, Mark; Hübner, Annika; Rothkirch, André; Wragg, David S; Stock, Norbert

    2012-11-19

    The system Cu(2+)/H2O3P-C2H4-SO3H/NaOH was investigated using in situ energy dispersive X-ray diffraction (EDXRD) to study the formation and temperature induced phase transformation of previously described copper phosphonosulfonates. Thus, the formation of [Cu2(O3P-C2H4-SO3)(OH)(H2O)]·3H2O (4) at 90 °C is shown to proceed via a previously unknown intermediate [Cu2(O3P-C2H4-SO3)(OH)(H2O)]·4H2O (6), which could be structurally characterized from high resolution powder diffraction data. Increase of the reaction temperature to 150 °C led to a rapid phase transformation to [Cu2(O3P-C2H4-SO3)(OH)(H2O)]·H2O (1), which was also studied by in situ EDXRD. The comparison of the structures of 1, 4, and 6 allowed us to establish a possible reaction mechanism. In addition to the in situ crystallization studies, microwave assisted heating for the synthesis of the copper phosphonosulfonates was employed, which allowed the growth of larger crystals of [NaCu(O3P-C2H4-SO3)(H2O)2] (5) suitable for single crystal X-ray diffraction. Through the combination of force field calculations and Rietveld refinement we were able to determine the crystal structure of [Cu1.5(O3P-C2H4-SO3)] 2H2O (3) and thus structurally characterize all compounds known up to now in this well investigated system. With the additional structural data we are now able to describe the influence of the pH on the structure formation.

  9. In-situ energy dispersive x-ray diffraction study of the growth of CuO nanowires by annealing method

    SciTech Connect

    Srivastava, Himanshu; Ganguli, Tapas; Deb, S. K.; Sant, Tushar; Poswal, H. K.; Sharma, Surinder M.

    2013-10-14

    The in-situ growth of CuO nanowires was studied by Energy Dispersive X-ray Diffraction (EDXRD) to observe the mechanism of growth. The study was carried out for comparison at two temperatures—at 500 °C, the optimum temperature of the nanowires growth, and at 300 °C just below the temperature range of the growth. The in situ observation revealed the successive oxidation of Cu foil to Cu{sub 2}O layer and finally to CuO layer. Further analysis showed the presence of a compressive stress in CuO layer due to interface at CuO and Cu{sub 2}O layers. The compressive stress was found to increase with the growth of the nanowires at 500 °C while it relaxed with the growth of CuO layer at 300 °C. The present results do not support the existing model of stress relaxation induced growth of nanowires. Based on the detailed Transmission Electron Microscope, Scanning Electron Microscope, and EDXRD results, a microstructure based growth model has been suggested.

  10. In situ energy-dispersive X-ray diffraction for the synthesis optimization and scale-up of the porous zirconium terephthalate UiO-66.

    PubMed

    Ragon, Florence; Horcajada, Patricia; Chevreau, Hubert; Hwang, Young Kyu; Lee, U-Hwang; Miller, Stuart R; Devic, Thomas; Chang, Jong-San; Serre, Christian

    2014-03-03

    The synthesis optimization and scale-up of the benchmarked microporous zirconium terephthalate UiO-66(Zr) were investigated by evaluating the impact of several parameters (zirconium precursors, acidic conditions, addition of water, and temperature) over the kinetics of crystallization by time-resolved in situ energy-dispersive X-ray diffraction. Both the addition of hydrochloric acid and water were found to speed up the reaction. The use of the less acidic ZrOCl2·8H2O as the precursor seemed to be a suitable alternative to ZrCl4·xH2O, avoiding possible reproducibility issues as a consequence of the high hygroscopic character of ZrCl4. ZrOCl2·8H2O allowed the formation of smaller good quality UiO-66(Zr) submicronic particles, paving the way for their use within the nanotechnology domain, in addition to higher reaction yields, which makes this synthesis route suitable for the preparation of UiO-66(Zr) at a larger scale. In a final step, UiO-66(Zr) was prepared using conventional reflux conditions at the 0.5 kg scale, leading to a rather high space-time yield of 490 kg m(-3) day(-1), while keeping physicochemical properties similar to those obtained from smaller scale solvothermally prepared batches.

  11. Adsorption of N/S heterocycles in the flexible metal-organic framework MIL-53(Fe(III)) studied by in situ energy dispersive X-ray diffraction.

    PubMed

    Van de Voorde, Ben; Munn, Alexis S; Guillou, Nathalie; Millange, Franck; De Vos, Dirk E; Walton, Richard I

    2013-06-14

    The adsorption of N/S-containing heterocyclic organic molecules in the flexible iron(III) terephthalate MIL-53, Fe(III)(OH)(0.6)F(0.4)(O2C-C6H4-CO2)·(H2O), from the liquid phase was studied with in situ energy dispersive X-ray diffraction (EDXRD), in order to follow the adsorption-induced expansion of the structure. For comparison with the diffraction data, liquid phase adsorption isotherms were recorded for uptake of benzothiophene, benzothiazole and indole in isopropanol and in heptane. The solvent not only influences pore opening but is also a competing guest. The in situ EDXRD experiments allow the kinetics of guest uptake and the competition with solvent to be monitored directly. Indole uptake is limited; this adsorbate is barely capable of opening the closed, either hydrated or dehydrated, MIL-53(Fe) structure, or of penetrating the isopropanol-containing material in the concentration range under study. When isopropanol is used as a solvent, the guest molecules benzothiophene and benzothiazole must be present at a certain threshold concentration before substantial adsorption into the metal-organic framework takes place, eventually resulting in full opening of the structure. The fully expanded structures of benzothiophene or benzothiazole loaded MIL-53(Fe) materials have Imcm symmetry and a unit cell volume of ca. 1600 Å(3), and upon uptake of the guest molecules by the closed form (unit cell volume ~1000 Å(3)) no intermediate crystalline phases are seen. Successful uptake by MIL-53(Fe) requires that the adsorbate is primarily a good hydrogen bond acceptor; additionally, based on UV-visible spectroscopy, a charge-transfer interaction between the S atoms of benzothiophene and the aromatic rings in the MOF pore wall is proposed.

  12. 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.

  13. Spectral and raw quasi in-situ energy dispersive X-ray data captured via a TEM analysis of an ODS austenitic stainless steel sample under 1 MeV Kr(2+) high temperature irradiation.

    PubMed

    Brooks, Adam J; Yao, Zhongwen

    2017-10-01

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

  14. 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.

  15. Rate Dependent Multi-Mechanism Discharge of Ag0.50VOP 4·1.8H2O: Insights from In Situ Energy Dispersive X-ray Diffraction

    DOE PAGES

    Huie, Matthew M.; Bock, David C.; Zhong, Zhong; ...

    2016-09-01

    Ag0.50VOPO4·1.8H2O (silver vanadium phosphate, SVOP) demonstrates a counterintuitive higher initial loaded voltage under higher discharge current. Energy dispersive X-ray diffraction (EDXRD) from synchrotron radiation was used to create tomographic profiles of cathodes at various depths of discharge for two discharge rates. SVOP displays two reduction mechanisms, reduction of a vanadium center accompanied by lithiation of the structure, or reduction-displacement of a silver cation to form silver metal. In-situ EDXRD provides the opportunity to observe spatially resolved changes to the parent SVOP crystal and formation of Ag0 during reduction. At a C/170 discharge rate V5+ reduction is the preferred initial reactionmore » resulting in higher initial loaded voltage. At a discharge rate of C/400 reduction of Ag+ with formation of conductive Ag0 occurs earlier during discharge. Discharge rate also affects the spatial location of reduction products. The faster discharge rate initiates reduction close to the current collector with non-uniform distribution of silver metal resulting in isolated cathode areas. The slower rate develops a more homogenous distribution of reduced SVOP and silver metal. This study illuminates the roles of electronic and ionic conductivity limitations within a cathode at the mesoscale and how they impact the course of reduction processes and loaded voltage.« less

  16. Visualization of structural evolution and phase distribution of a lithium vanadium oxide (Li1.1V3O8) electrode via an operando and in situ energy dispersive X-ray diffraction technique

    DOE PAGES

    Zhang, Qing; Bruck, Andrea M.; Bock, David C.; ...

    2017-05-03

    We present Li1+nV3O8 (n = 0–0.2) has been extensively investigated as a cathode material for Li ion batteries because of its superior electrochemical properties including high specific energy and good rate capability. In this paper, a synchrotron based energy dispersive X-ray diffraction (EDXRD) technique was employed to profile the phase transitions and the spatial phase distribution of a Li1.1V3O8 electrode during electrochemical (de)lithiation in situ and operando. As annealing temperature during the preparation of the Li1.1V3O8 material has a strong influence on the morphology and crystallinity, and consequently influences the electrochemical outcomes of the material, Li1.1V3O8 materials prepared at twomore » different temperatures, 500 and 300°C (LVO500 and LVO300), were employed in this study. The EDXRD spectra of LVO500 and LVO300 cells pre-discharged at C/18, C/40 and C/150 were recorded in situ, and phase localization and relative intensity of the peaks were compared. For cells discharged at the C/18 rate, although α and β phases were distributed uniformly within the LVO500 electrode, they were localized on two sides of the LVO300 electrode. Discharging rates of C/40 and C/150 led to homogeneous β phase formation in both LVO500 and LVO300 electrodes. Furthermore, the phase distribution as a function of position and (de)lithiation extent was mapped operando as the LVO500 cell was (de)lithiated. In conclusion, the operando data indicate that (1) the lithiation reaction initiated from the side of the electrode facing the Li anode and proceeded towards the side facing the steel can, (2) during discharge the phase transformation from a Li-poor to a Li-rich α phase and the formation of a β phase can proceed simultaneously in the electrode after the first formation of a β phase, and (3) the structural evolution occurring during charging is not the reverse of that during discharge and takes place homogenously throughout the electrode.« less

  17. Energy-dispersive small-angle X-ray scattering with cone collimation using X-ray capillary optics

    NASA Astrophysics Data System (ADS)

    Li, Fangzuo; Liu, Zhiguo; Sun, Tianxi

    2016-09-01

    Energy-dispersive small-angle X-ray scattering (ED-SAXS) with an innovative design of cone collimation based on an ellipsoidal single-bounce capillary (ESBC) and a polycapillary parallel X-ray lens (PPXRL) had been explored. Using this new cone collimation system, scattering angle 2θ has a theoretical minimum angle related to the mean half-opening angle of the hollow cone beam of 1.42 mrad, and with the usable X-ray energy ranging from 4 to 30 keV, the resulting observable scattering vector q is down to a minimum value of about 0.003 Å-1 (or a Bragg spacing of about 2100 Å). However, the absorption of lower energies by X-ray capillary optics, sample transmission, and detector response function limits the application range to lower energy. Cone collimation ED-SAXS experiments carried out on pure water, Lupolen, and in situ temperature-dependent measurement of diacetylenic acid/melamine micelle solid were presented at three different scattering angles 2θ of 0.18°, 0.70° and 1.18° to illustrate the new opportunities offered by this technique as well as its limitations. Also, a comparison has been made by replacing the PPXRL with a pinhole, and the result shows that cone collimation ED-SAXS based on ESBC with PPXRL was helpful in improving the signal-to-noise ratio (i.e., reducing the parasitic background scattering) than ESBC with a pinhole. The cone collimation instrument based on X-ray capillary optics could be considered as a promising tool to perform SAXS experiments, especially cone collimation ED-SAXS has potential application for the in situ temperature-dependent studying on the kinetics of phase transitions.

  18. Systematic and in situ energy dispersive X-ray diffraction investigations on the formation of lanthanide phosphonatobutanesulfonates: Ln(O(3)P-C(4)H(8)-SO(3))(H(2)O) (Ln = La-Gd).

    PubMed

    Feyand, Mark; Näther, Christian; Rothkirch, André; Stock, Norbert

    2010-12-06

    Using the flexible linker H(2)O(3)P-C(4)H(8)-SO(3)H (H(3)L) and rare earth ions Ln(3+) (Ln = La, Ce, Pr, Nd, Sm, Eu, Gd) we were able to synthesize the new isostructural inorganic organic hybrid compounds Ln(O(3)P-C(4)H(8)-SO(3))(H(2)O). High-throughput experiments were employed to study the influence of the molar ratios Ln:H(3)L and pH on the product formation. The crystal structure of the compounds Sm(O(3)P-C(4)H(8)-SO(3))(H(2)O) (1) and Pr(O(3)P-C(4)H(8)-SO(3))(H(2)O) (2) were determined by single crystal diffraction. The structures are built up from chains of edge-sharing LnO(8)-polyhedra that are connected by the phosphonate and sulfonate groups into layers. These layers are linked by the -(CH(2))(4)- group to form a three-dimensional framework. The synthesis of compound 1 was scaled up in a conventional oven as well as in a microwave reactor system. A modification of a microwave reactor system allowed its integration into the beamline F3 at HASYLAB, DESY, Hamburg. The crystallization was investigated in situ by means of energy dispersive X-ray diffraction using conventional as well as microwave heating methods applying temperatures varying from 110 to 150 °C. The formation of Sm(O(3)P-C(4)H(8)-SO(3))(H(2)O) takes place in two steps. In the first step a crystalline intermediate was observed, which transforms completely into compound 1. The method by Sharp and Hancock was used to determine the rate constants, reaction exponents, and the Arrhenius activation energy for both reaction steps. Comparing both heating methods, microwave heating leads to fully crystallized reaction product after shorter reaction times, but neither the temperature nor the heating method has significant influence on the induction time.

  19. 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

    NASA Astrophysics Data System (ADS)

    Akdoğan, E. K.; Şavklıyıldız, İ.; Biçer, H.; Paxton, W.; Toksoy, F.; Zhong, Z.; Tsakalakos, T.

    2013-06-01

    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 °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 °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 °C was 3 A, corresponding to instantaneous absorbed power density of 570 W/cm3. Densification of 8YSZ was accompanied by anomalous elastic volume expansions of the unit cell by 0.45% and 2.80% at 847 °C and 905 °C, respectively. The anomalous expansion at 905 °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 (ɛ) at room temperature, as computed from tetragonal (112) and (211) reflections, are ɛ(112) = 0.05% and ɛ(211) = 0.13%, respectively. Time dependence of (211) and (112) peak widths (β) show a decrease with both exhibiting a singularity at 905 °C. An anisotropy in (112) and (211) peak widths of {β(112)/β(211)} = (3:1) magnitude was observed. No phase transformation occurred at 905 °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 superposition of mass fluxes due to Fickian diffusion, thermodiffusion (Soret effect), and electromigration, which in turn are a consequence of a superposition of chemical

  20. 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

  1. Phase development in the hardening process of two calcium phosphate bone cements: an energy dispersive X-ray diffraction study

    SciTech Connect

    Generosi, A.; Smirnov, V.V.; Rau, J.V.; Albertini, V. Rossi; Ferro, D.; Barinov, S.M.

    2008-03-04

    This work was aimed at the application of an energy dispersive X-ray diffraction technique to study the kinetics of phase development during the setting and hardening reactions in two calcium phosphate bone cements. The cements under study are based on either tricalcium phosphate or tetracalcium phosphate initial solid phase, and a magnesium carbonate-phosphoric acid liquid phase as the hardening liquid. The application of the energy dispersive X-ray diffraction method allowed to collect the diffraction patterns from the cement pastes in situ starting from 1 min of the setting and hardening process. The only crystallized phase in both cements was apatite-like phase, the primary crystallization process proceeds during a few seconds of the setting reaction. Both the compressive strength and the pH value changes during the hardening period can be attributed to the transformations occurring in the intergranular X-ray amorphous phase.

  2. Energy dispersive X-Ray fluorescence determination of thorium in phosphoric acid solutions

    NASA Astrophysics Data System (ADS)

    Mirashi, N. N.; Dhara, Sangita; Kumar, S. Sanjay; Chaudhury, Satyajeet; Misra, N. L.; Aggarwal, S. K.

    2010-07-01

    Energy dispersive X-ray fluorescence studies on determination of thorium (in the range of 7 to 137 mg/mL) in phosphoric acid solutions obtained by dissolution of thoria in autoclave were made. Fixed amounts of Y internal standard solutions, after dilution with equal amount of phosphoric acid, were added to the calibration as well as sample solutions. Solution aliquots of approximately 2-5 µL were deposited on thick absorbent sheets to absorb the solutions and the sheets were presented for energy dispersive X-ray fluorescence measurements. A calibration plot was made between intensity ratios (Th Lα/Y Kα) against respective amounts of thorium in the calibration solutions. Thorium amounts in phosphoric acid samples were determined using their energy dispersive X-ray fluorescence spectra and the above calibration plot. The energy dispersive X-ray fluorescence results, thus obtained, were compared with the corresponding gamma ray spectrometry results and were found to be within average deviation of 2.6% from the respective gamma ray spectrometry values. The average precision obtained in energy dispersive X-ray fluorescence determinations was found to be 4% (1 σ). The energy dispersive X-ray fluorescence method has an advantage over gamma ray spectrometry for thorium determination as the amount of sample required and measurement time is far less compared to that required in gamma ray spectrometry.

  3. Analysis of the Deformation Behavior of Magnesium-Rare Earth Alloys Mg-2 pct Mn-1 pct Rare Earth and Mg-5 pct Y-4 pct Rare Earth by In Situ Energy-Dispersive X-ray Synchrotron Diffraction and Elasto-Plastic Self-Consistent Modeling

    NASA Astrophysics Data System (ADS)

    Lentz, Martin; Klaus, Manuela; Coelho, Rodrigo S.; Schaefer, Nobert; Schmack, Florian; Reimers, Walter; Clausen, Bjørn

    2014-11-01

    The deformation behavior of the Mg-RE alloys ME21 and WE54 was investigated. Although both alloys contain rare earth elements, which alter and weaken the texture, the flow curves of the alloys deviate significantly, especially in uniaxial compression test. Apart from the higher strength of the WE54 alloy, the compression flow curve does not exhibit the typical sigmoidal shape, which is associated with tension twinning. However, optical microscopy, X-ray texture measurements, and EBSD analysis reveal the activity of tension twinning. The combination of in situ energy-dispersive X-ray synchrotron diffraction and EPSC modeling was used to analyze these differences. The investigation reveals that twin propagation is decelerated in the WE54 alloy, which requires a change of the twinning scheme from the `finite initial fraction' to the `continuity' assumption. Furthermore, an enhanced activity of the < c+ a> pyramidal slip system was observed in case of the WE54 alloy.

  4. 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.

  5. 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.

  6. 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.

  7. Single photon energy dispersive x-ray diffraction

    NASA Astrophysics Data System (ADS)

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

    2014-03-01

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

  8. 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.

  9. Single photon energy dispersive x-ray diffraction.

    PubMed

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

    2014-03-01

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

  10. 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.

  11. 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.

  12. 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.

  13. Internal conversion in energy dispersive X-ray analysis of actinide-containing materials.

    PubMed

    Wiss, Thierry; Thiele, Hartmut; Cremer, Bert; Ray, Ian

    2007-06-01

    The use of X-ray elemental analysis tools like energy dispersive X-ray (EDS) is described in the context of the investigation of nuclear materials. These materials contain radioactive elements, particularly alpha-decaying actinides that affect the quantitative EDS measurement by producing interferences in the X-ray spectra. These interferences originating from X-ray emission are the result of internal conversion by the daughter atoms from the alpha-decaying actinides. The strong interferences affect primarily the L X-ray lines from the actinides (in the typical energy range used for EDS analysis) and would require the use of the M lines. However, it is typically at the energy of the actinide's M lines that the interferences are dominant. The artifacts produced in the X-ray analysis are described and illustrated by some typical examples of analysis of actinide-bearing material.

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

    NASA Astrophysics Data System (ADS)

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

    2017-08-01

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

  15. 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.

  16. 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.…

  17. 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.…

  18. Analysis of titanium and zirconium in red mud with energy dispersive x-ray spectrometry

    SciTech Connect

    Kobya, M.; Ertugrul, M.; Dogan, O.; Simsek, O.

    1996-11-01

    An energy dispersive x-ray fluorescence technique was used for the determination of Titanium (Ti) and Zirconium (Zr) in red mud by using a standard addition method. An annular {sup 241}Am source is employed for excitation of K shells of elements. 13 refs., 2 figs., 1 tab.

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

    PubMed Central

    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

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

    PubMed

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

    2016-12-01

    Here we report the influence of key experimental parameters on atomically resolved energy dispersive X-ray spectroscopy (EDX). In particular, we examine the role of the probe forming convergence semi-angle, sample thickness, lattice spacing, and dwell/collection time. We show that an optimum specimen-dependent probe forming convergence angle exists to maximize the signal-to-noise ratio of the atomically resolved signal in EDX mapping. Furthermore, we highlight that it can be important to select an appropriate dwell time to efficiently process the X-ray signal. These practical considerations provide insight for experimental parameters in atomic resolution energy dispersive X-ray analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Energy dispersive x-ray fluorescence analyzer with several x-ray tubes

    NASA Astrophysics Data System (ADS)

    Borisov, G. I.; Kondratenko, R. I.; Mikhin, V. A.; Odinov, B. V.; Pukhov, A. V.

    2005-07-01

    X-ray flurescent analyzer (XFA) has been developed and fabricated for determining sulphur, vanadium and nickel in oil. The instrument is equipped with three x-ray tubes with transmission Ti, Cu and Ag anodes, and aluminum, copper, and germanium filters, respectively, and one common switchable power supply. To excite characteristic radiation of determined elements, the characteristic radiation of the tube anode (titan, copper) is used, or the charactersitic radiation of the filter (germanium). XFA is fitted with one small-size electrically cooled semiconductor detector. The measuring device is based on a wide-angle geometry of characteristic radiation excitation and registration, where the x-ray tube focus illuminates the sample, and the registering detector 'sees' the illuminated area within the plane angle of 90° (it corresponds to 0.146 of 4p). Under such geometry, the dependence of the count rate for excited characteristic photons on the position of sample under study has a smooth maximum in the calculated sample position point. For one, the rate count changes by less than 1%. Quantitative results are obtained through the regression method. The instrument underwent metrology testing. It is designed for operation both in the laboratory and industrial environment. The instrument has been delivered for operation to the "Druzhba" pipeline.

  2. 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.

  3. Breast tissue contrast-simulating materials using energy-dispersive X-ray diffraction.

    PubMed

    Alkhateeb, Shyma M; Abdelkader, Mohamed H; Bradley, David A; Pani, Silvia

    2012-07-01

    Breast lesions and normal tissues have different molecular arrangements that affect their diffraction patterns. Different mouldable and non-mouldable materials were analysed using an energy dispersive X-ray diffraction system based on a conventional X-ray source (operated at 70 kVp) and a CdTe detector (Amptek XT-100), including a conventional spectroscopic chain. Combinations of materials were identified to have a contrast comparable to that achieved in diffraction imaging for different breast tissues at the momentum transfer values carrying the greatest amount of information (1.1 nm(-1) and 1.6 nm(-1)).

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

    NASA Astrophysics Data System (ADS)

    Egan, Christopher K.; Wilson, Matthew D.; Veale, Matthew C.; Seller, Paul; Jacques, Simon D. M.; Cernik, Robert J.

    2014-04-01

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

  5. Place of HgI/sub 2/ energy-dispersive x-ray detectors

    SciTech Connect

    Dabrowski, A.J.; Huth, G.C.; Iwanczyk, J.S.; Kusmiss, J.H.; Barton, J.S.; Szymczyk, J.M.; Schnepple, W.F.; Lynn, R.

    1982-01-01

    After a review of solid-state conduction counters, in general, and of the history of mercuric iodide, in particular, the theory of operation of solid-state energy-dispersive HgI/sub 2/ detectors is dicusssed. The main factors which limit energy resolution in solid-state compound detectors are considered, including statistical fluctuations in charge generation, the window effect, trapping, inhomogeneities in the detector material, and electronic noise. Potential applications of room-temperature HgI/sub 2/ x-ray detectors are listed, and general considerations are discussed for x-ray fluorescence analysis with HgI/sub 2/. Directions of current investigations are given. (LEW)

  6. 20-element HgI[sub 2] energy dispersive x-ray array detector system

    SciTech Connect

    Iwanczyk, J.S.; Dorri, N.; Wang, M.; Szczebiot, R.W.; Dabrowski, A.J. ); Hedman, B.; Hodgson, K.O. . Stanford Synchrotron Radiation Lab.); Patt, B.E. )

    1992-10-01

    This paper describes recent progress in the development of HgI[sub 2] energy dispersive x-ray 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 alpha]) 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 form diluted samples simulating proteins with nickel.

  7. 20 element HgI sub 2 energy dispersive x-ray array detector system

    SciTech Connect

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

    1991-01-01

    This paper describes recent progress in the development of HgI{sub 2} 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.

  8. 20 element HgI{sub 2} energy dispersive x-ray array detector system

    SciTech Connect

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

    1991-12-31

    This paper describes recent progress in the development of HgI{sub 2} 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.

  9. Energy dispersive X-ray analysis on an absolute scale in scanning transmission electron microscopy.

    PubMed

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

    2015-10-01

    We demonstrate absolute scale agreement between the number of X-ray counts in energy dispersive X-ray spectroscopy using an atomic-scale coherent electron probe and first-principles simulations. Scan-averaged spectra were collected across a range of thicknesses with precisely determined and controlled microscope parameters. Ionization cross-sections were calculated using the quantum excitation of phonons model, incorporating dynamical (multiple) electron scattering, which is seen to be important even for very thin specimens. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. 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.

  11. Use of MCNP code in energy dispersive X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    Trojek, T.; Čechák, T.

    2007-10-01

    Monte Carlo simulations enable us to improve the applicability of analytical techniques based on emission of characteristic radiation. In particular, the MCNP4C2 code was tested for interpretation of measured data obtained with the use of energy dispersive X-ray fluorescence analysis. This paper describes MCNP outputs and compares them with the results of analytical calculations or experiments. Then the application of Monte Carlo simulations to the prediction of measurement results is shown, and the MCNP results are verified.

  12. Analysis of some Nigerian solid mineral ores by energy-dispersive X-ray fluorescence spectroscopy

    NASA Astrophysics Data System (ADS)

    Obiajunwa, E. I.

    2001-11-01

    Determination of major, minor and trace elements in some Nigerian solid mineral ores by energy-dispersive X-ray fluorescence (EDXRF) spectroscopy is described. Concentration values of major, minor and trace elements for Z>18 are reported. The mineral ores studied include (i) tantalite-coloumbite minerals, (ii) bismuth minerals and (iii) lead minerals. The accuracy and precision of the technique for chemical analysis was assured by analysing the geological standards mica-Fe (biotite) and NBS 278 (obsidian).

  13. 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.

  14. Rate Dependent Multi-Mechanism Discharge of Ag0.50VOP 4·1.8H2O: Insights from In Situ Energy Dispersive X-ray Diffraction

    SciTech Connect

    Huie, Matthew M.; Bock, David C.; Zhong, Zhong; Bruck, Andrea M.; Yin, Jiefu; Takeuchi, Esther S.; Takeuchi, Kenneth J.; Marschilok, Amy C.

    2016-09-01

    Ag0.50VOPO4·1.8H2O (silver vanadium phosphate, SVOP) demonstrates a counterintuitive higher initial loaded voltage under higher discharge current. Energy dispersive X-ray diffraction (EDXRD) from synchrotron radiation was used to create tomographic profiles of cathodes at various depths of discharge for two discharge rates. SVOP displays two reduction mechanisms, reduction of a vanadium center accompanied by lithiation of the structure, or reduction-displacement of a silver cation to form silver metal. In-situ EDXRD provides the opportunity to observe spatially resolved changes to the parent SVOP crystal and formation of Ag0 during reduction. At a C/170 discharge rate V5+ reduction is the preferred initial reaction resulting in higher initial loaded voltage. At a discharge rate of C/400 reduction of Ag+ with formation of conductive Ag0 occurs earlier during discharge. Discharge rate also affects the spatial location of reduction products. The faster discharge rate initiates reduction close to the current collector with non-uniform distribution of silver metal resulting in isolated cathode areas. The slower rate develops a more homogenous distribution of reduced SVOP and silver metal. This study illuminates the roles of electronic and ionic conductivity limitations within a cathode at the mesoscale and how they impact the course of reduction processes and loaded voltage.

  15. High-resolution microcalorimeter energy-dispersive spectrometer for x-ray microanalysis and particle analysis

    SciTech Connect

    Wollman, D. A.; Hilton, G. C.; Irwin, K. D.; Dulcie, L. L.; Bergren, N. F.; Martinis, John M.; Newbury, Dale E.; Woo, Keung-Shan; Liu, Benjamin Y. H.; Diebold, Alain C.

    1998-11-24

    We have developed a high-resolution microcalorimeter energy-dispersive spectrometer (EDS) at NIST that provides improved x-ray microanalysis of contaminant particles and defects important to the semiconductor industry. Using our microcalorimeter EDS mounted on a scanning electron microscope (SEM), we have analyzed a variety of specific sized particles on Si wafers, including 0.3 {mu}m diameter W particles and 0.1 {mu}m diameter Al{sub 2}O{sub 3} particles. To compare the particle analysis capabilities of microcalorimeter EDS to that of semiconductor EDS and Auger electron spectroscopy (AES), we report measurements of the Al-K{alpha}/Si-K{alpha} x-ray peak intensity ratio for 0.3 {mu}m diameter Al{sub 2}O{sub 3} particles on Si as a function of electron beam energy. We also demonstrate the capability of microcalorimeter EDS for chemical shift measurements.

  16. 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??.

  17. Silica granuloma: scanning electron microscopy and energy dispersive X-ray microanalysis.

    PubMed

    Chun, S I; Cho, S W

    1991-02-01

    A 46-year-old woman had 1-month-old erythematous papules on the left elbow and both knees where acupuncture with gold needles had been performed twenty years earlier. She also had a 2-month-old pruritic scar lesion on the nape. Histopathologic findings showed sarcoidal granulomas. The presence of silica components in the granulomas was confirmed by scanning electron microscopy (SEM) of the lesion on the nape and energy dispersive X-ray microanalysis (EDXA) of the lesions on the nape and the left elbow. We suggest that acupuncture with gold needles may be one cause of silica granuloma.

  18. Application of energy dispersive X-ray fluorescence spectrometry (EDX) in a case of methomyl ingestion.

    PubMed

    Kinoshita, Hiroshi; Tanaka, Naoko; Jamal, Mostofa; Kumihashi, Mitsuru; Okuzono, Ryota; Tsutsui, Kunihiko; Ameno, Kiyoshi

    2013-04-10

    We applied energy dispersive X-ray fluorescence spectrometry (EDX) in a case of poisoning by methomyl, a carbamate pesticide. Quantitative GC/MS analysis showed that the concentration of methomyl-oxime in the femoral blood was 4.0 μg/ml. The elemental analysis by EDX identified the high peak of silicon and sulfur in the stomach contents. We concluded that the cause of his death was methomyl poisoning. This indicates that screening of stomach contents by EDX provides useful information for the forensic diagnosis.

  19. A new approach to synchrotron energy-dispersive X-ray diffraction computed tomography.

    PubMed

    Lazzari, Olivier; Egan, Christopher K; Jacques, Simon D M; Sochi, Taha; Di Michiel, Marco; Cernik, Robert J; Barnes, Paul

    2012-07-01

    A new data collection strategy for performing synchrotron energy-dispersive X-ray diffraction computed tomography has been devised. This method is analogous to angle-dispersive X-ray diffraction whose diffraction signal originates from a line formed by intersection of the incident X-ray beam and the sample. Energy resolution is preserved by using a collimator which defines a small sampling voxel. This voxel is translated in a series of parallel straight lines covering the whole sample and the operation is repeated at different rotation angles, thus generating one diffraction pattern per translation and rotation step. The method has been tested by imaging a specially designed phantom object, devised to be a demanding validator for X-ray diffraction imaging. The relative strengths and weaknesses of the method have been analysed with respect to the classic angle-dispersive technique. The reconstruction accuracy of the method is good, although an absorption correction is required for lower energy diffraction because of the large path lengths involved. The spatial resolution is only limited to the width of the scanning beam owing to the novel collection strategy. The current temporal resolution is poor, with a scan taking several hours. The method is best suited to studying large objects (e.g. for engineering and materials science applications) because it does not suffer from diffraction peak broadening effects irrespective of the sample size, in contrast to the angle-dispersive case.

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

    PubMed

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

    2009-01-01

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

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

    PubMed Central

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

    2009-01-01

    The development of an innovative detector technology for photon-counting in X-ray imaging is reported. This new generation of detectors, based on pixellated cadmium telluride (CdTe) and cadmium zinc telluride (CZT) detector arrays electrically connected to application specific integrated circuits (ASICs) for readout, will produce fast and highly efficient photon-counting and energy-dispersive X-ray imaging. There are a number of applications that can greatly benefit from these novel imagers including mammography, planar radiography, and computed tomography (CT). Systems based on this new detector technology can provide compositional analysis of tissue through spectroscopic X-ray imaging, significantly improve overall image quality, and may significantly reduce X-ray dose to the patient. A very high X-ray flux is utilized in many of these applications. For example, CT scanners can produce ~100 Mphotons/mm2/s in the unattenuated beam. High flux is required in order to collect sufficient photon statistics in the measurement of the transmitted flux (attenuated beam) during the very short time frame of a CT scan. This high count rate combined with a need for high detection efficiency requires the development of detector structures that can provide a response signal much faster than the transit time of carriers over the whole detector thickness. We have developed CdTe and CZT detector array structures which are 3 mm thick with 16×16 pixels and a 1 mm pixel pitch. These structures, in the two different implementations presented here, utilize either a small pixel effect or a drift phenomenon. An energy resolution of 4.75% at 122 keV has been obtained with a 30 ns peaking time using discrete electronics and a 57Co source. An output rate of 6×106 counts per second per individual pixel has been obtained with our ASIC readout electronics and a clinical CT X-ray tube. Additionally, the first clinical CT images, taken with several of our prototype photon-counting and energy-dispersive

  2. X-ray fluorescence and energy dispersive x-ray diffraction for the quantification of elemental concentrations in breast tissue.

    PubMed

    Geraki, K; Farquharson, M J; Bradley, D A

    2004-01-07

    This paper presents improvements on a previously reported method for the measurement of elements in breast tissue specimens (Geraki et al 2002 Phys. Med. Biol. 47 2327-39). A synchrotron-based system was used for the detection of the x-ray fluorescence (XRF) emitted from iron, copper, zinc and potassium in breast tissue specimens, healthy and cancerous. Calibration models resulting from the irradiation of standard aqueous solutions were used for the quantification of the elements. The present developments concentrate on increasing the convergence between the tissue samples and the calibration models, therefore improving accuracy. For this purpose the composition of the samples in terms of adipose and fibrous tissue was evaluated, using an energy dispersive x-ray diffraction (EDXRD) system. The relationships between the attenuation and scatter properties of the two tissue components and water were determined through Monte Carlo simulations. The results from the simulations and the EDXRD measurements allowed the XRF data from each specimen to be corrected according to its composition. The statistical analysis of the elemental concentrations of the different groups of specimens reveals that all four elements are found in elevated levels in the tumour specimens. The increase is less pronounced for iron and copper and most for potassium and zinc. Other observed features include the substantial degree of inhomogeneity of elemental distributions within the volume of the specimens, varying between 4% and 36% of the mean, depending on the element and the type of the sample. The accuracy of the technique, based on the measurement of a standard reference material, proved to be between 3% and 22% depending on the element, which presents only a marginal improvement (1%-3%) compared to the accuracy of the previously reported results. The measurement precision was between 1% and 9% while the calculated uncertainties on the final elemental concentrations ranged between 10% and 16%.

  3. 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.

  4. 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.

  5. [Application of the racial algorithm in energy dispersive X-ray fluorescence overlapped spectrum analysis].

    PubMed

    Zeng, Guo-Qiang; Luo, Yao-Yao; Ge, Liang-Quan; Zhang, Qing-Xian; Gu, Yi; Cheng, Feng

    2014-02-01

    In the energy dispersive X-ray fluorescence spectrum analysis, scintillation detector such as NaI (Tl) detector usually has a low energy resolution at around 8%. The low energy resolution causes problems in spectral data analysis especially in the high background and low counts condition, it is very limited to strip the overlapped spectrum, and the more overlapping the peaks are, the more difficult to peel the peaks, and the qualitative and quantitative analysis can't be carried out because we can't recognize the peak address and peak area. Based on genetic algorithm and immune algorithm, we build a new racial algorithm which uses the Euclidean distance as the judgment of evolution, the maximum relative error as the iterative criterion to be put into overlapped spectrum analysis, then we use the Gaussian function to simulate different overlapping degrees of the spectrum, and the racial algorithm is used in overlapped peak separation and full spectrum simulation, the peak address deviation is in +/- 3 channels, the peak area deviation is no more than 5%, and it is proven that this method has a good effect in energy dispersive X-ray fluorescence overlapped spectrum analysis.

  6. 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.

  7. 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.

  8. Identification of inorganic dust particles in bronchoalveolar lavage macrophages by energy dispersive x-ray microanalysis.

    PubMed

    Johnson, N F; Haslam, P L; Dewar, A; Newman-Taylor, A J; Turner-Warwick, M

    1986-01-01

    This study shows that energy dispersive x-ray microprobe analysis to identify and quantify intracellular particles in macrophages obtained by the minimally invasive method of bronchoalveolar lavage (BAL) can detect inorganic dust exposures of many different kinds. Bronchoalveolar lavage macrophages from 22 patients have been examined. Twelve patients had occupational exposure to asbestos, talc, silica, hard metal or printing ink, while 10 had no known history of dust exposure. X-ray microprobe analysis identified particles which related to the known exposures, superimposed on a background of other particles related to smoking (kaolinite and mica) or to the general environment (silicon, titanium, and iron). The particle identification provided useful objective confirmation of the known exposures, except for silica, which could not be distinguished from the general background levels. X-ray microanalysis using BAL macrophages can be helpful for clarification of mixed dust exposures, to identify particles when light microscopy indicates retained dust in patients with no known history of exposure, and to monitor retained particles after removal from exposure.

  9. A novel portable energy dispersive X-ray fluorescence spectrometer with triaxial geometry

    NASA Astrophysics Data System (ADS)

    Pessanha, S.; Alves, M.; Sampaio, J. M.; Santos, J. P.; Carvalho, M. L.; Guerra, M.

    2017-01-01

    The X-ray fluorescence technique is a powerful analytical tool with a broad range of applications such as quality control, environmental contamination by heavy metals, cultural heritage, among others. For the first time, a portable energy dispersive X-ray fluorescence spectrometer was assembled, with orthogonal triaxial geometry between the X-ray tube, the secondary target, the sample and the detector. This geometry reduces the background of the measured spectra by reducing significantly the Bremsstrahlung produced in the tube through polarization in the secondary target and in the sample. Consequently, a practically monochromatic excitation energy is obtained. In this way, a better peak-background ratio is obtained compared to similar devices, improving the detection limits and leading to superior sensitivity. The performance of this setup is compared with the one of a benchtop setup with triaxial geometry and a portable setup with planar geometry. Two case studies are presented concerning the analysis of a 18th century paper document, and the bone remains of an individual buried in the early 19th century.

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

    SciTech Connect

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

    2016-07-27

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

  11. 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

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

    PubMed Central

    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.

    2016-01-01

    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

  13. Atomic-scale chemical quantification of oxide interfaces using energy-dispersive X-ray spectroscopy

    SciTech Connect

    Lu, Ping; Van Benthem, Mark; Xiong, Jie; Jia, Quanxi

    2013-04-29

    Atomic-scale quantification of chemical composition across oxide interfaces is important for understanding physical properties of epitaxial oxide nanostructures. Energy-dispersive X-ray spectroscopy (EDS) in an aberration-corrected scanning transmission electron microscope was used to quantify chemical composition across the interface of ferromagnetic La{sub 0.7}Sr{sub 0.3}MnO{sub 3} and antiferromagnetic BiFeO{sub 3} quantum structure. This research demonstrates that chemical composition at atomic columns can be quantified by Gaussian peak-fitting of EDS compositional profiles across the interface. Cation diffusion was observed at both A- and B-sublattice sites; and asymmetric chemical profiles exist across the interface, consistent with the previous studies.

  14. 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.

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

    PubMed

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

    2016-01-27

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

  16. 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).

  17. Welders' pneumoconiosis: tissue elemental microanalysis by energy dispersive x ray analysis.

    PubMed Central

    Funahashi, A; Schlueter, D P; Pintar, K; Bemis, E L; Siegesmund, K A

    1988-01-01

    Histological examination on lung tissue obtained from 10 symptomatic welders was performed by two certified pathologists without the knowledge of the patients' clinical condition. In all cases, there was some degree of interstitial fibrosis; in five the degree of fibrosis was considered to be moderate to pronounced. The tissue was also analysed by energy dispersive x ray analysis and elemental contents were compared with age matched controls. There was a large amount of iron in the lungs of welders but the silicon content did not differ from the control subjects. No specific foreign element was detected. It is concluded that (1) interstitial pulmonary fibrosis is seen in some welders and (2) the cause of fibrosis does not appear to be coexisting silicosis. Images PMID:3342182

  18. 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.

  19. Development of a prototype pipework scanning system based upon energy dispersive X-ray diffraction (EDXRD)

    NASA Astrophysics Data System (ADS)

    Garrity, D. J.; De Rosa, A. J.; Bradley, D. A.; Jarman, S. E.; Jenneson, P. M.; Vincent, S. M.

    2010-07-01

    A prototype pipework scanning system based upon energy dispersive X-ray diffraction (EDXRD) has been produced, for which system development and preliminary results are presented here. This apparatus has been developed from experience with 2D and 3D bench-top EDXRD systems and comprises a conventional industrial X-ray tube coupled to a bespoke design of tungsten collimators and compact CdTe detector. It is designed as a robust system, rather than delicate lab-based system, to investigate sections of stainless steel pipework for structural changes induced through quenching the steel in liquid nitrogen, and damaging effects such as chloride-induced stress corrosion cracking (SCC). Given the properties of tungsten, namely its brittle nature, a complex programme of electro-discharge machining (EDM) has been devised to precisely manufacture the collimators from a series of sintered tungsten blocks. Preliminary measurements have focused on calibrating the system using the extreme ferrite and austenite phases, meeting a pre-requisite benchmark for attempting more challenging measurements such as the austenite to martensite transformation and investigations of SCC in these sections of pipework.

  20. Can we detect Li K X-ray in lithium compounds using energy dispersive spectroscopy?

    PubMed

    Hovington, Pierre; Timoshevskii, Vladimir; Burgess, Simon; Demers, Hendrix; Statham, Peter; Gauvin, Raynald; Zaghib, Karim

    2016-11-01

    Lithium is the key element for the development of battery and new technology and the development of an analytical technique to spatially and quantitatively resolve this element is of key importance. Detection of Li K in pure metallic lithium is now possible in the Scanning Electron Microscope (SEM) with newly designed Energy Dispersive Spectroscopy (EDS). However, this work is clearly showing, for the first time using EDS, the detection of Li K in several binary lithium compounds (LiH, Li3 N, Li2 S, LiF and LiCl). Experimental Li K X-rays intensity is compared with a specially modified Monte Carlo simulation program showing discrepancies between theoretical and experimental Li K measurements. The effect of chemical bounding on the X-rays emission using density functional theory with the all-electron linearized augmented plane wave is showing that the emission of Li K from the binary compounds studied should be, at least, 12 times lower than in metallic Li. SCANNING 38:571-578, 2016. © 2016 Wiley Periodicals, Inc.

  1. Biomedical and agricultural applications of energy dispersive X-ray spectroscopy in electron microscopy.

    PubMed

    Wyroba, Elżbieta; Suski, Szymon; Miller, Karolina; Bartosiewicz, Rafał

    2015-09-01

    Energy dispersive X-ray spectroscopy (EDS) in electron microscopy has been widely used in many research areas since it provides precise information on the chemical composition of subcellular structures that may be correlated with their high resolution images. In EDS the characteristic X-rays typical of each element are analyzed and the new detectors - an example of which we describe - allow for setting precisely the area of measurements and acquiring signals as a point analysis, as a linescan or in the image format of the desired area. Mapping of the elements requires stringent methods of sample preparation to prevent redistribution/loss of the elements as well as elimination of the risk of overlapping spectra. Both qualitative and quantitative analyses may be performed at a low probe current suitable for thin biological samples. Descriptions of preparation techniques, drawbacks and precautions necessary to obtain reliable results are provided, including data on standards, effects of specimen roughness and quantification. Data on EPMA application in different fields of biomedical and agricultural studies are reviewed. In this review we refer to recent EDS/EPMA applications in medical diagnostics, studies on air pollution and agrochemicals as well as on plant models used to monitor the environment.

  2. Risk and benefit of diffraction in Energy Dispersive X-ray fluorescence mapping

    NASA Astrophysics Data System (ADS)

    Nikonow, Wilhelm; Rammlmair, Dieter

    2016-11-01

    Energy dispersive X-ray fluorescence mapping (μ-EDXRF) is a fast and non-destructive method for chemical quantification and therefore used in many scientific fields. The combination of spatial and chemical information is highly valuable for understanding geological processes. Problems occur with crystalline samples due to diffraction, which appears according to Bragg's law, depending on the energy of the X-ray beam, the incident angle and the crystal parameters. In the spectra these peaks can overlap with element peaks suggesting higher element concentrations. The aim of this study is to investigate the effect of diffraction, the possibility of diffraction removal and potential geoscientific applications for X-ray mapping. In this work the μ-EDXRF M4 Tornado from Bruker was operated with a Rh-tube and polychromatic beam with two SDD detectors mounted each at ± 90° to the tube. Due to the polychromatic beam the Bragg condition fits for several mineral lattice planes. Since diffraction depends on the angle, it is shown that a novel correction approach can be applied by measuring from two different angles and calculating the minimum spectrum of both detectors gaining a better limit of quantification for this method. Furthermore, it is possible to use the diffraction information for separation of differently oriented crystallites within a monomineralic aggregate and obtain parameters like particle size distribution for the sample, as it is done by thin section image analysis in cross-polarized light. Only with μ-EDXRF this can be made on larger samples without preparation of thin sections.

  3. Characterization of energy dispersive semiconductor detectors for x-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Hopman, Theodore Lambert

    Since the development of the electron microprobe in the 1950s by Castaing, characteristic x-ray emission lines have been used to determine chemical compositions of samples. Energy-dispersive detectors allow simultaneous multi-element analysis; continued improvements in detector technology have lowered limits of detection and allowed the effects of physical processes in the detector to become apparent. A well-characterized detector, in terms of its geometry and its response to x-rays, is essential for accurate and precise chemical analysis. In this work, scans with a collimated 55Fe radionuclide source allowed the geometry of Si(Li) detectors to be determined. Across the surface of the detector the response function was uniform, indicating it is due primarily to detector physics and/or processing electronics. Monochromatized x-rays over an energy range of 1--10 keV were used to generate simple spectra in Si(Li) and silicon drift detectors with analog and digital pulse processing systems. Monte Carlo simulations of detector response allowed approximate contributions from physical processes to be seen individually. Transport of energetic electrons, electron diffusion at metal-semiconductor junctions, and differences in detector structure together determine variation with energy of spectral features. The Si K photoelectron escape step at ˜1.8 keV, previously attributed to electron transport only, is found to be affected by diffusion. The diffusion tail to the low-energy side of the primary peak is found to have a component due to escape of Si L Auger electrons. Escape peak intensities in SDD and Si(Li) detectors agree only when contact photoelectron contributions are taken into account.

  4. 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.

  5. 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.

  6. 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.

  7. 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.

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

    Treesearch

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

    2014-01-01

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

  9. A Review of Energy Dispersive X-Ray Fluorescence (EDXRF) as an Analytical Tool in Numismatic Studies.

    PubMed

    Navas, María José; Asuero, Agustín García; Jiménez, Ana María

    2016-01-01

    Energy dispersive X-ray fluorescence spectrometry (EDXRF) as an analytical technique in studies of ancient coins is summarized and reviewed. Specific EDXRF applications in historical studies, in studies of the corrosion of coins, and in studies of the optimal working conditions of some laser-based treatment for the cleaning of coins are described.

  10. In situ X-ray-based imaging of nano materials

    DOE PAGES

    Weker, Johanna Nelson; Huang, Xiaojing; Toney, Michael F.

    2016-02-13

    We study functional nanomaterials that are heterogeneous and understanding their behavior during synthesis and operation requires high resolution diagnostic imaging tools that can be used in situ. Over the past decade, huge progress has been made in the development of X-ray based imaging, including full field and scanning microscopy and their analogs in coherent diffractive imaging. Currently, spatial resolution of about 10 nm and time resolution of sub-seconds are achievable. For catalysis, X-ray imaging allows tracking of particle chemistry under reaction conditions. In energy storage, in situ X-ray imaging of electrode particles is providing important insight into degradation processes. Recently,more » both spatial and temporal resolutions are improving to a few nm and milliseconds and these developments will open up unprecedented opportunities.« less

  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. 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.

  13. 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.

  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. 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.

  16. 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.

  17. Development of mercuric iodide energy dispersive x-ray array detectors

    SciTech Connect

    Iwanczyk, J.S.; Warburton, W.K.; Dabrowski, A.J.; Hedman, B.; Hodgson, K.O.; Patt, B.E.

    1988-02-01

    There are various areas of synchrotron radiation research particularly Extended X-Ray Absorption Fine Structure (EXAFS) on dilute solutions and anomalous scattering, which would strongly benefit from the availability of energy dispersive detector arrays with high energy resolution and good spatial resolution. The goal of this development project is to produce high energy resolution mercuric iodide (HgI/sub 2/) detector sub-modules, consisting of several elements. These sub-modules can later be grouped into larger arrays of 100-400 elements. A prototype 5 element HgI/sub 2/ array detector was constructed and tested. Dimensions of each element were 7.3 mm x 0.7 mm. An energy resolution of 335 eV (FWHM) for Mn0K..cap alpha.. at 5.9 keV has been measured. The novel fiber-optic pulsed light feedback has been introduced into the charge preamplifiers in order to minimize electronic crosstalk between channels.

  18. Mercuric iodide detector systems for identifying substances by x-ray energy dispersive diffraction

    SciTech Connect

    Iwanczyk, J.S.; Patt, B.E.; Wang, Y.J.; Croft, M.; Kalman, Z.; Mayo, W.

    1995-08-01

    The use of mercuric iodide arrays for energy-dispersive x-ray diffraction (EDXRD) spectroscopy is now being investigated by the authors for inspection of specific crystalline powders in substances ranging from explosives to illicit drugs. Mercuric iodide has been identified as the leading candidate for replacing the Ge detectors previously employed in the development of this technique because HgI{sub 2} detectors: operate at or near room temperature; without the bulky apparatus associated with cryogenic cooling; and offer excellent spectroscopy performance with extremely high efficiency. Furthermore, they provide the practicality of constructing optimal array geometries necessary for these measurements. Proof of principle experiments have been performed using a single-HgI{sub 2} detector spectrometer. An energy resolution of 655 eV (FWHM) has been obtained for 60 keV gamma line from an {sup 241}Am source. The EDXRD signatures of various crystalline powdered compounds have been measured and the spectra obtained show the excellent potential of mercuric iodide for this application.

  19. 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.

  20. 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.

  1. Minimum detectable limits of measuring bone mineral density using an energy dispersive X-ray diffraction system

    NASA Astrophysics Data System (ADS)

    Allday, A. W.; Farquharson, M. J.

    2001-06-01

    In the clinical environment, the most common method of assessing bone mineral density (BMD) loss is dual energy X-ray absorptiometry (DEXA), which relies on the transmission of X-ray photons through the volume of interest. Energy dispersive X-ray diffraction (EDXRD), which utilises coherent X-ray scattering, potentially is a more accurate method. As part of the development of a precision EDXRD system, an experiment was performed using a range of bone and fat mix phantoms, which were also used for DEXA evaluation. The results are presented here and suggest initial minimum detectable limits of the order of 5% BMD loss for the EDXRD experiment and 10-15% for the DEXA assessment.

  2. THE SAP3 COMPUTER PROGRAM FOR QUANTITATIVE MULTIELEMENT ANALYSIS BY ENERGY DISPERSIVE X-RAY FLUORESCENCE

    SciTech Connect

    Nielson, K. K.; Sanders, R. W.

    1982-04-01

    SAP3 is a dual-function FORTRAN computer program which performs peak analysis of energy-dispersive x-ray fluorescence spectra and then quantitatively interprets the results of the multielement analysis. It was written for mono- or bi-chromatic excitation as from an isotopic or secondary excitation source, and uses the separate incoherent and coherent backscatter intensities to define the bulk sample matrix composition. This composition is used in performing fundamental-parameter matrix corrections for self-absorption, enhancement, and particle-size effects, obviating the need for specific calibrations for a given sample matrix. The generalized calibration is based on a set of thin-film sensitivities, which are stored in a library disk file and used for all sample matrices and thicknesses. Peak overlap factors are also determined from the thin-film standards, and are stored in the library for calculating peak overlap corrections. A detailed description is given of the algorithms and program logic, and the program listing and flow charts are also provided. An auxiliary program, SPCAL, is also given for use in calibrating the backscatter intensities. SAP3 provides numerous analysis options via seventeen control switches which give flexibility in performing the calculations best suited to the sample and the user needs. User input may be limited to the name of the library, the analysis livetime, and the spectrum filename and location. Output includes all peak analysis information, matrix correction factors, and element concentrations, uncertainties and detection limits. Twenty-four elements are typically determined from a 1024-channel spectrum in one-to-two minutes using a PDP-11/34 computer operating under RSX-11M.

  3. Determination of calcium and iodine in gall bladder stone using energy dispersive X-ray fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Ekinci, Neslihan; Şahin, Yusuf

    2002-01-01

    Energy dispersive X-ray fluorescence techniques were used to analyze gall bladder stones. Enrichment of Ca and I was observed in the gall bladder stone taken from a patient. The concentration of Ca has been determined with an annular 55Fe radioactive source and the concentration of I with an annular 241Am radioactive source using the standard addition method in 2π geometry. A Si(Li)-detector was used to measure Ca and I concentrations in the gall bladder stones.

  4. In situ soft X-ray absorption spectroscopy of flames

    NASA Astrophysics Data System (ADS)

    Frank, Jonathan H.; Shavorskiy, Andrey; Bluhm, Hendrik; Coriton, Bruno; Huang, Erxiong; Osborn, David L.

    2014-10-01

    The feasibility of in situ soft X-ray absorption spectroscopy for imaging carbonaceous species in hydrocarbon flames is demonstrated using synchrotron radiation. Soft X-rays are absorbed by core level electrons in all carbon atoms regardless of their molecular structure. Core electron spectroscopy affords distinct advantages over valence spectroscopy, which forms the basis of traditional laser diagnostic techniques for combustion. In core level spectroscopy, the transition linewidths are predominantly determined by the instrument response function and the decay time of the core-hole, which is on the order of a femtosecond. As a result, soft X-ray absorption measurements can be performed in flames with negligible Doppler and collisional broadening. Core level spectroscopy has the further advantage of measuring all carbonaceous species regardless of molecular structure in the far-edge region, whereas near-edge features are molecule specific. Interferences from non-carbon flame species are unstructured and can be subtracted. In the present study, absorption measurements in the carbon K-edge region are demonstrated in low-pressure ( P total = 20-30 Torr) methane jet flames. Two-dimensional imaging of the major carbonaceous species, CH4, CO2, and CO, is accomplished by tuning the synchrotron radiation to the respective carbon K-edge, near-edge X-ray absorption fine structure (NEXAFS) transitions and scanning the burner.

  5. 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.

  6. In situ synchrotron based x-ray techniques as monitoring tools for atomic layer deposition

    SciTech Connect

    Devloo-Casier, Kilian Detavernier, Christophe; Dendooven, Jolien

    2014-01-15

    Atomic layer deposition (ALD) is a thin film deposition technique that has been studied with a variety of in situ techniques. By exploiting the high photon flux and energy tunability of synchrotron based x-rays, a variety of new in situ techniques become available. X-ray reflectivity, grazing incidence small angle x-ray scattering, x-ray diffraction, x-ray fluorescence, x-ray absorption spectroscopy, and x-ray photoelectron spectroscopy are reviewed as possible in situ techniques during ALD. All these techniques are especially sensitive to changes on the (sub-)nanometer scale, allowing a unique insight into different aspects of the ALD growth mechanisms.

  7. 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.

  8. Study of heavy metals and other elements in macrophyte algae using energy-dispersive X-ray fluorescence

    SciTech Connect

    Carvalho, M.L.; Amorim, P.; Marques, M.I.M.; Ramos, M.T.; Ferreira, J.G.

    1997-04-01

    Fucus vesiculosus L. seaweeds from three estuarine stations were analyzed by X-ray fluorescence, providing results for the concentration of total K, Ca, Ti, Mn, Fe, Co, Ni, Cu, Zn, As, Br, Sr, and Pb. Four different structures of the algae (base, stipe, reproductive organs, and growing tips) were analyzed to study the differential accumulation of heavy metals by different parts of Fucus. Some elements (e.g., Cu and Fe) are preferentially accumulated in the base of the algae, whereas others (e.g., As) exhibit higher concentrations in the reproductive organs and growing tips. The pattern of accumulation in different structures is similar for Cu, Zn, and Pb, but for other metals there is considerable variability in accumulation between parts of the plant. This is important in determining which structures of the plant should be used for biomonitoring. For samples collected at stations subject to differing metal loads, the relative elemental composition is approximately constant, notwithstanding significant variation in absolute values. The proportion of metals in Fucus is similar to that found in other estuaries, where metal concentrations are significantly lower. Energy-dispersive X-ray fluorescence has been shown to be a suitable technique for multielement analysis in this type of sample. No chemical pretreatment is required, minimizing sample contamination. The small amount of sample required, and the wide range of elements that can be detected simultaneously make energy-dispersive X-ray fluorescence a valuable tool for pollution studies.

  9. New reference and test materials for the characterization of energy dispersive X-ray spectrometers at scanning electron microscopes.

    PubMed

    Rackwitz, Vanessa; Krumrey, Michael; Laubis, Christian; Scholze, Frank; Hodoroaba, Vasile-Dan

    2015-04-01

    Checking the performance of energy dispersive X-ray spectrometers as well as validation of the results obtained with energy dispersive X-ray spectrometry (EDX) at a scanning electron microscope (SEM) involve the use of (certified) reference and dedicated test materials. This paper gives an overview on the test materials mostly employed by SEM/EDX users and accredited laboratories as well as on those recommended in international standards. The new BAM reference material EDS-CRM, which is currently in the process of certification, is specifically designed for the characterization of EDS systems at a SEM through calibration of the spectrometer efficiency in analytical laboratories in a simple manner. The certification of the spectra by means of a reference EDS is described. The focus is on the traceability of EDS efficiency which is ensured by measurements of the absolute detection efficiency of silicon drift detectors (SDD) and Si(Li) detectors at the laboratory of the PTB using the electron storage ring BESSY II as a primary X-ray source standard. A new test material in development at BAM for testing the performance of an EDS in the energy range below 1 keV is also briefly presented.

  10. Automatic energy dispersive x-ray analyzer for defining the small quantities of chemical elements

    SciTech Connect

    Landman, K.; Antipov, A.; Veits, B.

    1993-12-31

    The results of analyzer development, which represents an analysing complex for high sensitive x-ray fluorescence analysis is presented. Results of research of detection limits of a wide range of elements is described.

  11. In situ synchrotron x-ray photon beam characterization

    SciTech Connect

    Kyele, Nicholas R.; Silfhout, Roelof G. van; Manolopoulos, Spyros; Nikitenko, S.

    2007-03-15

    We have investigated two in situ methods of measuring x-ray beam parameters such as integrated intensity, position, and intensity distribution. These virtually transparent methods both rely on the collection of scattered radiation from a thin amorphous foil. The scattered radiation is collected by an active pixel sensor placed below the foil, well out of the direction of the beam path. These methods measure a cross-sectional image of the beam as opposed to a profile or beam centroid position provided by existing in situ detection methods. We present the results of measurements taken at a third generation synchrotron radiation source and provide analytical methods of deriving beam profile, position, and absolute intensity.

  12. 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.

  13. Band reject filtration of the excitation spectrum at energy dispersive X-ray spectroscopy of weak signals

    NASA Astrophysics Data System (ADS)

    Tur'yanskii, A. G.; Gizha, S. S.; Senkov, V. M.; Pirshin, I. V.; Stanishevskii, Ya. M.

    2016-09-01

    The possibility of the efficient band reject filtration of the continuous X-ray excitation spectrum in the energy range E ≥ 8 keV is demonstrated. This makes it possible to strongly increase the sensitivity of energy dispersive X-ray spectroscopy at detecting of weak fluorescence lines. Spectral rejection is implemented by transmitting a primary beam through highly oriented pyrolytic graphite with given structural parameters. Diffraction extinction in pyrolytic graphite ensures the possibility of reducing the intensity by more than 20 dB and rejecting the spectral band with a width of 1 keV. The reduction of statistical fluctuations of the background of elastically scattered radiation is achieved when the bottom of the formed spectral valley is adjusted to the analyzed fluorescence line. The proposed scheme of band reject filtration also allows the suppression of intense characteristic lines in the primary and scattered radiation spectra.

  14. Energy dispersive x-ray diffractometry as a tool alternative to differential scanning calorimetry for investigating polymer phase transitions

    NASA Astrophysics Data System (ADS)

    Rossi-Albertini, V.; Isopo, A.; Caminiti, R.; Tentolini, U.

    2002-02-01

    Recently, a technique based on energy dispersive x-ray diffraction has been proposed to follow the polymer phase transitions. However, the potentialities of this method were not clear, as well as the experimental conditions in which it is more convenient than differential scanning calorimetry, generally used for the same purpose. In the present letter, the answer to this question is provided. It is shown that the two methods are complementary, rather than equivalent, the heating rate being the relevant parameter to establish which is preferable. The demonstration of this statement is given through the observation of the complex thermal properties of a reference sample studied in both ways at progressively lower heating rates. The connection between such unusual application of x-ray diffraction and the differential scanning calorimetry is discussed in terms of the two possible definitions of entropy.

  15. Uranium aerosols at a nuclear fuel fabrication plant: Characterization using scanning electron microscopy and energy dispersive X-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Hansson, E.; Pettersson, H. B. L.; Fortin, C.; Eriksson, M.

    2017-05-01

    Detailed aerosol knowledge is essential in numerous applications, including risk assessment in nuclear industry. Cascade impactor sampling of uranium aerosols in the breathing zone of nuclear operators was carried out at a nuclear fuel fabrication plant. Collected aerosols were evaluated using scanning electron microscopy and energy dispersive X-ray spectroscopy. Imaging revealed remarkable variations in aerosol morphology at the different workshops, and a presence of very large particles (up to ≅ 100 × 50 μm2) in the operator breathing zone. Characteristic X-ray analysis showed varying uranium weight percentages of aerosols and, frequently, traces of nitrogen, fluorine and iron. The analysis method, in combination with cascade impactor sampling, can be a powerful tool for characterization of aerosols. The uranium aerosol source term for risk assessment in nuclear fuel fabrication appears to be highly complex.

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

    PubMed

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

    2017-05-01

    The increasing use of energy dispersive X-ray spectroscopy in atomic resolution scanning transmission electron microscopy invites the question of whether its success in precision composition determination at lower magnifications can be replicated in the atomic resolution regime. In this paper, we explore, through simulation, the prospects for composition measurement via the model system of AlxGa1-xAs, discussing the approximations used in the modelling, the variability in the signal due to changes in configuration at constant composition, and the ability to distinguish between different compositions. Results are presented in such a way that the number of X-ray counts, and thus the expected variation due to counting statistics, can be gauged for a range of operating conditions. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. 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.

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

    PubMed

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

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

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

    NASA Astrophysics Data System (ADS)

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

    2017-05-01

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

  20. Determination of metal components in marine sediments using energy-dispersive X-ray fluorescence (ED-XRF) spectrometry.

    PubMed

    Tung, Joanne Wai Ting

    2004-11-01

    A rapid energy-dispersive X-ray fluorescence (ED-XRF) spectrometric method for the analysis of metal components of marine sediments has been presented. Calibrations were made using synthetic matrix. The agreement of the results for sediment standard reference materials with reference values is satisfactory. Major advantages of the non-destructive ED-XRF technique over conventional chemical digestion methods include the applicability to analyzing the major oxide components, as well as to trace metals, and the avoidance of hazardous chemicals. The method has been applied to the routine analysis of Hong Kong marine sediment.

  1. [Results of an investigation of enamel fragments from Benvenuto Cellini's "Saliera" using energy-dispersive X-ray microanalysis (EDX)].

    PubMed

    Ditrich, Hans

    2009-01-01

    A blackmail letter was submitted in the context of the theft of Cellini's salt cellar (Saliera) from the Museum of Fine Arts in Vienna. Dark blue enamel fragments were included in this letter as a proof of authenticity. The comparison of this material with enamel believed to originate from the original artwork, using microspectrography and energy-dispersive X-ray microanalysis (EDX) in the scanning electron microscope showed similar elemental composition. Accordingly, the further investigations could concentrate on this blackmail attempt in spite of numerous other confession letters received.

  2. 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.

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

    SciTech Connect

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

    2016-06-30

    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 (EDS) mapping in aberration-corrected scanning transmission electron microscope (STEM) 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.

  4. 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.

  5. Discrimination of land-use types in a catchment by energy dispersive X-ray fluorescence and principal component analysis.

    PubMed

    Melquiades, F L; Andreoni, L F S; Thomaz, E L

    2013-07-01

    Differences in composition and chemical elemental concentration are important information for soil samples classification. The objective of this study is to present a direct methodology, that is non-destructive and without complex sample preparation, in order to discriminate different land-use types and soil degradation, employing energy dispersive X-ray fluorescence and multivariate analysis. Sample classification results from principal component analysis, utilizing spectral data and elemental concentration values demonstrate that the methodology is efficient to discriminate different land-use types. Copyright © 2013 Elsevier Ltd. All rights reserved.

  6. The HgI sub 2 energy dispersive x-ray array detectors and minaturized processing electronics project

    SciTech Connect

    Iwanczyk, J.S.; Dorri, N.; Wang, M.; Szawlowski . Inst. of Physics); Patt, W.K. ); Hedman, B.; Hodgson, K.O. . Stanford Synchrotron Radiation Lab.)

    1990-04-01

    This paper describes recent progress in the development of HgI{sub 2} energy dispersive x-ray detector arrays for synchrotron radiation research and their associated miniaturized processing electronics. Deploying a 5 element HgI{sub 2} array detector under realistic operating conditions at SSRL, an energy resolution of 252 eV FWHM at 5.9 keV (Mn-K{alpha}) was obtained. The authors also report energy resolution and throughput measurements versus input count rate. The results from the HgI{sub 2} system are then compared to those obtained under identical conditions from a commercial 13 element Ge detector array.

  7. Energy Dispersive X-ray Diffraction (EDXRD) of Li1.1V3O8 Electrochemical Cell

    SciTech Connect

    Zhang, Qing; Bruck, Andrea M.; Bock, David C.; Li, Jing; Stach, Eric A.; Takeuchi, Esther S.; Takeuchi, Kenneth J.; Marschilok, Amy C.

    2017-01-01

    ABSTRACT

    In this study, we conducted the first energy dispersive x-ray diffraction (EDXRD) experiments on Li/Li1.1V3O8coin cells discharged to different lithiation levels in order to investigate the phase transitions upon electrochemical reduction. The phase transformation from layered Li-poor α to Li-rich α to defect rock-salt β phase was confirmed with cells of different lithiation stages. No spatial localization of phase formation was observed throughout the cathodes under the conditions of this measurement.

  8. 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

  9. 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.

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

    SciTech Connect

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

    1996-07-01

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

  11. Anisotropic Thermal Expansion of Zirconium Diboride: An Energy-Dispersive X-Ray Diffraction Study

    SciTech Connect

    Paxton, William A.; Özdemir, Tevfik E.; Şavklıyıldız, İlyas; Whalen, Terence; Biçer, Hülya; Akdoğan, Enver Koray; Zhong, Zhong; Tsakalakos, Thomas

    2016-01-01

    Zirconium diboride (ZrB2) is an attractive material due to its thermal and electrical properties. In recent years, ZrB2has been investigated as a superior replacement for sapphire when used as a substrate for gallium nitride devices. Like sapphire, ZrB2has an anisotropic hexagonal structure which defines its directionally dependent properties. However, the anisotropic behavior of ZrB2is not well understood. In this paper, we use energy-dispersive synchrotron X-ray diffraction to measure the thermal expansion of polycrystalline ZrB2powder from 300 to 1150 K. Nine Bragg reflections are fit using Pseudo-Voigt peak profiles and used to compute theaandclattice parameters using a nonlinear least-squares approximation. The temperature-dependent instantaneous thermal expansion coefficients are determined for eacha-axis andc-axis direction and are described by the following equations:αa= (4.1507×10-6+5.1086×10-9(T-293.15))/(1+4.1507×10-6(T-293.15
  12. The Oxford-Diamond In Situ Cell for studying chemical reactions using time-resolved X-ray diffraction.

    PubMed

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

    2012-08-01

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

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

    NASA Astrophysics Data System (ADS)

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

    2012-08-01

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

  14. High Pressure Studies Using Energy Dispersive Diffraction of High Energy X-Rays.

    DTIC Science & Technology

    1987-02-01

    Work 38 8 - Contributions to Conferences and Meetings 39 9- References 40 LIST OF FIGURES Figure 1 - Calculated resolution for the spectrum of silicon ...10 - Energy dispersive spectrum of silicon powder collected at 20 - 8.5" 20 Figure 11 - EDXRD spectrum of TiB obtained using Synchrotron Radiation 23...energy required for creating an electron-hole pair in the semiconductor crystal of the detector (2.96 eV for germanium ). F the Fano factor, reflecting

  15. Residual strain gradient determination in metal matrix composites by synchrotron X-ray energy dispersive diffraction

    NASA Technical Reports Server (NTRS)

    Kuntz, Todd A.; Wadley, Haydn N. G.; Black, David R.

    1993-01-01

    An X-ray technique for the measurement of internal residual strain gradients near the continuous reinforcements of metal matrix composites has been investigated. The technique utilizes high intensity white X-ray radiation from a synchrotron radiation source to obtain energy spectra from small (0.001 cu mm) volumes deep within composite samples. The viability of the technique was tested using a model system with 800 micron Al203 fibers and a commercial purity titanium matrix. Good agreement was observed between the measured residual radial and hoop strain gradients and those estimated from a simple elastic concentric cylinders model. The technique was then used to assess the strains near (SCS-6) silicon carbide fibers in a Ti-14Al-21Nb matrix after consolidation processing. Reasonable agreement between measured and calculated strains was seen provided the probe volume was located 50 microns or more from the fiber/matrix interface.

  16. Electron cyclotron resonance ion source plasma characterization by energy dispersive x-ray imaging

    NASA Astrophysics Data System (ADS)

    Rácz, R.; Mascali, D.; Biri, S.; Caliri, C.; Castro, G.; Galatà, A.; Gammino, S.; Neri, L.; Pálinkás, J.; Romano, F. P.; Torrisi, G.

    2017-07-01

    Pinhole and CCD based quasi-optical x-ray imaging technique was applied to investigate the plasma of an electron cyclotron resonance ion source (ECRIS). Spectrally integrated and energy resolved images were taken from an axial perspective. The comparison of integrated images taken of argon plasma highlights the structural changes affected by some ECRIS setting parameters, like strength of the axial magnetic confinement, RF frequency and microwave power. Photon counting analysis gives precise intensity distribution of the x-ray emitted by the argon plasma and by the plasma chamber walls. This advanced technique points out that the spatial positions of the electron losses are strongly determined by the kinetic energy of the electrons themselves to be lost and also shows evidences how strongly the plasma distribution is affected by slight changes in the RF frequency.

  17. 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.

  18. 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.

  19. In Situ X-Ray Analysis of Protein Crystals in Low-Birefringent And X-Ray Transmissive Plastic Microchannels

    SciTech Connect

    Ng, J.D.; Clark, P.J.; Stevens, R.C.; Kuhn, P.

    2009-05-22

    Plastic microchannel crystallization template designs made from inexpensive cyclic olefin copolymers have been shown to be low-birefringent, X-ray transmissive and compatible with microfluidic fabrication in restricted geometry. The model proteins thaumatin, lysozyme and bacteriorhodopsin demonstrated the feasibility of conducting counter-diffusion equilibration within the new plastic configuration. Crystals of each of these proteins were directly evaluated in situ using synchrotron radiation and their diffraction quality was evaluated without invasive manipulation or cryofreezing. Protein crystals able to produce complete X-ray data sets were used to calculate electron-density maps for structure determination. Fluidic crystallization in the plastic platform was also coupled with a commercialized automated imager and an in situ X-ray scanner that allowed optical and X-ray inspection of crystallization hits. The results demonstrate the feasibility of rapid nanovolume counter-diffusion crystallization experiments without the need for additional instrumentation.

  20. High-throughput and time-resolved energy-dispersive X-ray diffraction (EDXRD) study of the formation of CAU-1-(OH)2: microwave and conventional heating.

    PubMed

    Ahnfeldt, Tim; Moellmer, Jens; Guillerm, Vincent; Staudt, Reiner; Serre, Christian; Stock, Norbert

    2011-05-27

    Aluminium dihydroxyterephthalate [Al(8)(OH)(4)(OCH(3))(8)(BDC(OH)(2))(6)]⋅x H(2)O (denoted CAU-1-(OH)(2)) was synthesized under solvothermal conditions and characterized by X-ray powder diffraction, IR spectroscopy, sorption measurements, as well as thermogravimetric and elemental analysis. CAU-1-(OH)(2) is isoreticular to CAU-1 and its pores are lined with OH groups. It is stable under ambient conditions and in water, and it exhibits permanent porosity and two types of cavities with effective diameters of approximately 1 and 0.45 nm. The crystallization of CAU-1-(OH)(2) was studied by in situ energy-dispersive X-ray diffraction (EDXRD) experiments in the 120-145 °C temperature range. Two heating methods-conventional and microwave-were investigated. The latter leads to shorter induction periods as well as shorter reaction times. Whereas CAU-1-(OH)(2) is formed at all investigated temperatures using conventional heating, it is only observed below 130 °C using microwave heating. The calculation of the activation energy of the crystallization of CAU-1-(OH)(2) exhibits similar values for microwave and conventional synthesis. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

    1. Energy-dispersive X-ray fluorescence analysis of moss and soil from abandoned mining of Pb-Zn ores.

      PubMed

      Koz, B

      2014-09-01

      This research investigates heavy metal pollution around one of the most important mining areas in Turkey, the Sebinkarahisar (Giresun) lead-zinc mining, by means of analyzing moss and soil samples collected in the neighborhood of the copper mining at different distances. Energy dispersive X-ray fluorescence spectrometry (Epsilon 5, PANalytical, Almelo, The Netherlands) is utilized in the experiments. The results have indicated that the both moss and soil samples contain aluminum, vanadium, chromium, manganese, iron, nickel, copper, zinc, arsenic, barium, cerium, tungsten, and lead. The comparison of the heavy metal concentrations with the typical measurements in the world and with the limit values for the human health has revealed the critical heavy metal pollution levels in the region. The possible consequences of these results are briefly discussed from the point of potential hazards to ecology and human health.

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

      NASA Astrophysics Data System (ADS)

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

      2017-09-01

      Multilayer tungsten carbide wear resistant coatings were analyzed by laser induced breakdown spectroscopy (LIBS) and energy dispersive X-ray (EDX) spectroscopy. Coaxial laser cladding technique was utilized to produce tungsten carbide coating deposited on low alloy steel substrate with additional inconel 625 interlayer. EDX and LIBS techniques were used for elemental profiling of major components (Ni, W, C, Fe, etc.) in the coating. A good correlation between EDX and LIBS data was observed while LIBS provided additional information on light element distribution (carbon). A non-uniform distribution of tungsten carbide grains along coating depth was detected by both LIBS and EDX. In contrast, horizontal elemental profiling showed a uniform tungsten carbide particles distribution. Depth elemental profiling by layer-by-layer LIBS analysis was demonstrated to be an effective method for studying tungsten carbide grains distribution in wear resistant coating without any sample preparation.

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

      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.

    4. 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.

    5. Scanning electron microscopy and energy-dispersive X-ray microanalysis of Penicillium brevicompactum treated with cobalt.

      PubMed

      Farrag, Rasha M; Mohamadein, Mohamed M; Mekawy, Amal A

      2008-01-01

      Scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) were used to study the morphology and elemental composition of the conidia, phialids and hyphae of Penicillium brevicompactum grown in the presence of cobalt concentrations of 0, 50, 200, 500, 800 and 1000 ppm (mg/l). Cobalt uptake was through the hyphae, phialids and the conidia with maximum uptake being by the conidia at a concentration of 1000 ppm. EDX revealed the increase in the percentage of calcium and magnesium in the hyphae, conidia and phialids, compared to corresponding controls, accompanying the increase in cobalt uptake. Alternatively a decrease in sulfur percentage was observed. This study might reflect the possibility of using SEM-EDX as a new technique in understanding the mechanism of tolerance.

    6. 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

    7. Nail Damage (Severe Onychodystrophy) Induced by Acrylate Glue: Scanning Electron Microscopy and Energy Dispersive X-Ray Investigations

      PubMed Central

      Pinteala, Tudor; Chiriac, Anca Eduard; Rosca, Irina; Larese Filon, Francesca; Pinteala, Mariana; Chiriac, Anca; Podoleanu, Cristian; Stolnicu, Simona; Coros, Marius Florin; Coroaba, Adina

      2017-01-01

      Background Scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) techniques have been used in various fields of medical research, including different pathologies of the nails; however, no studies have focused on obtaining high-resolution microscopic images and elemental analysis of disorders caused by synthetic nails and acrylic adhesives. Methods Damaged/injured fingernails caused by the use of acrylate glue and synthetic nails were investigated using SEM and EDX methods. Results SEM and EDX proved that synthetic nails, acrylic glue, and nails damaged by contact with acrylate glue have a different morphology and different composition compared to healthy human nails. Conclusions SEM and EDX analysis can give useful information about the aspects of topography (surface sample), morphology (shape and size), hardness or reflectivity, and the elemental composition of nails. PMID:28232921

    8. 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.

    9. Energy-dispersive and x-ray photoelectron spectroscopy and electron microscopy of new quininium-plastic membrane electrodes.

      PubMed

      Shoukry, Adel F; Maraffie, Hayat M; Al-Shatti, Laila A

      2007-10-01

      New quininium (Qn) plastic membrane electrodes of the conventional type were constructed and characterized. They are based on incorporation of Qn-reineckate (QnRn) ion-pair, Qn-phosphotungstate (Qn3-PT), or Qn-phosphomolybdate (Qn3PM) ion associate into a poly(vinyl chloride) membrane. The electrodes are selective for Qn and have been successfully used for the determination of Qn2SO4 in pharmaceutical tablets. Nevertheless, they showed, as almost all other ion-selective electrodes, limited life times. Energy dispersive- (EDS) and X-ray photoelectron spectroscopy (XPS), as well as electron microscopy were applied to investigate the cause of this limitation in the life times of the electrodes. The results indicated that the electrodes lose their activity after prolonged soaking as a result of leaching of the ion exchanger from the membranes into the test solution in addition to deformation at the surface of the expired electrode.

    10. [Line scanning analysis of white porcelain from Gong Kiln in early Tang dynasty by energy disperse X-ray fluorescence].

      PubMed

      Ling, Xue; Mao, Zhen-wei; Feng, Min; Hu, Yao-wu; Wang, Chang-sui; Liu, Hong-miao

      2005-07-01

      Gong kiln, for its long porcelain-firing history, was one of three representative white porcelain kilns in northern China. In order to improve the quality and whiteness of white porcelain, a decorating layer or cosmetic earth was laid on the body surface in Gong kiln during early Tang dynasty, which was able to blot out rough surface and weaken the influence of fuscous body upon surface color. In this paper the main chemical composition of the white porcelain's profile was analyzed by using energy disperse X-Ray fluorescence. The result showed that different materials were used as cosmetic earth during early Tang dynasty, in accordance with the phenomenon under optical microscope. In addition, the glaze belongs to calcium glaze in which plant ash was added.

    11. Quick analysis of organic matter in soil by energy-dispersive X-ray fluorescence and multivariate analysis.

      PubMed

      Morona, Franslley; Dos Santos, Felipe R; Brinatti, André M; Melquiades, Fábio L

      2017-09-08

      The rapid, simple and accurate determination of soil quality indicators is fundamental for improvements in precision agriculture and consequently in production efficiency. The objectives of this study were to determine the organic matter (OM) and total organic carbon (TOC) concentrations in agricultural soil and to discriminate soil provenance by energy-dispersive X-ray fluorescence (EDXRF) combined with principal component analysis and partial least square regression. The conventional methods used for the determination of OM and TOC concentrations are the gravimetric and Walkley-Black methods, respectively. Figures of merit such as sensitivity, detection and quantification limits, accuracy and precision were evaluated. Samples were differentiated by their provenance, and the quality of the prediction model shows that EDXRF combined with multivariate analysis is a promising methodology to fulfil the lack of rapid and accurate analytical methods for the assessment of OM and TOC concentrations in agricultural soils. Copyright © 2017 Elsevier Ltd. All rights reserved.

    12. 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.

    13. 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.

    14. Bismuth tri- and tetraarylcarboxylates: crystal structures, in situ X-ray diffraction, intermediates and luminescence.

      PubMed

      Feyand, Mark; Köppen, Milan; Friedrichs, Gernot; Stock, Norbert

      2013-09-09

      A systematic investigation of the systems Bi(3+)/carboxylic acid/HNO3 for the tri- and tetracarboxylic acids pyromellitic acid (H4Pyr), trimellitic acid (H3Tri) and trimesic acid (H3BTC) acid led to the discovery of five new bismuth carboxylates. Structural characterisation allowed the influence of the linker geometry and the Bi(3+):linker molar ratio in the starting solution on the crystal structure to be determined. The crystallisation of three selected compounds was investigated by in situ energy-dispersive X-ray diffraction. Three new crystalline intermediates were observed within minutes, and two of them could be isolated by quenching of the reaction mixture. Their crystal structures were determined from laboratory and synchrotron X-ray powder diffraction data and allowed a possible reaction pathway to be established. In depth characterisation of the luminescence properties of the three bismuth pyromellate compounds was carried out. Fluorescence and phosphorescence could be assigned to (mainly) ligand- and metal-based transitions. The polymorphs of Bi(HPyr) exhibit different luminescence properties, although their structures are very similar. Surprisingly, doping of the three host structures with Eu(3+) and Tb(3+) ions was only successful for one of the polymorphs.

    15. 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

    16. Photometric study of single-shot energy-dispersive x-ray diffraction at a laser plasma facility

      SciTech Connect

      Hoidn, O. R.; Seidler, G. T.

      2014-01-15

      The low repetition rates and possible shot-to-shot variations in laser-plasma studies place a high value on single-shot diagnostics. For example, white-beam scattering methods based on broadband backlighter x-ray sources are used to determine changes in the structure of laser-shocked crystalline materials by the evolution of coincidences of reciprocal lattice vectors and kinematically allowed momentum transfers. Here, we demonstrate that white-beam techniques can be extended to strongly disordered dense plasma and warm dense matter systems where reciprocal space is only weakly structured and spectroscopic detection is consequently needed to determine the static structure factor and thus, the ion-ion radial distribution function. Specifically, we report a photometric study of energy-dispersive x-ray diffraction (ED-XRD) for structural measurement of high energy density systems at large-scale laser facilities such as OMEGA and the National Ignition Facility. We find that structural information can be obtained in single-shot ED-XRD experiments using established backlighter and spectrometer technologies.

    17. 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.

    18. Atomic-resolution chemical mapping of ordered precipitates in Al alloys using energy-dispersive X-ray spectroscopy.

      PubMed

      Wenner, Sigurd; Jones, Lewys; Marioara, Calin D; Holmestad, Randi

      2017-05-01

      Scanning transmission electron microscopy (STEM) coupled with energy-dispersive X-ray spectroscopy (EDS) is a common technique for chemical mapping in thin samples. Obtaining high-resolution elemental maps in the STEM is jointly dependent on stepping the sharply focused electron probe in a precise raster, on collecting a significant number of characteristic X-rays over time, and on avoiding damage to the sample. In this work, 80kV aberration-corrected STEM-EDS mapping was performed on ordered precipitates in aluminium alloys. Probe and sample instability problems are handled by acquiring series of annular dark-field (ADF) images and simultaneous EDS volumes, which are aligned and non-rigidly registered after acquisition. The summed EDS volumes yield elemental maps of Al, Mg, Si, and Cu, with sufficient resolution and signal-to-noise ratio to determine the elemental species of each atomic column in a periodic structure, and in some cases the species of single atomic columns. Within the uncertainty of the technique, S and β" phases were found to have pure elemental atomic columns with compositions Al2CuMg and Al2Mg5Si4, respectively. The Q' phase showed some variation in chemistry across a single precipitate, although the majority of unit cells had a composition Al6Mg6Si7.2Cu2.

    19. 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.

    20. A deconvolution approach for the enhancement of spatial resolution in energy dispersive x-ray diffraction and related imaging methods

      NASA Astrophysics Data System (ADS)

      Schlesinger, S.; Bomsdorf, H.

      2013-07-01

      A reconstruction approach is presented, allowing the improvement of spatial resolution of images obtained by sequential pixel scanning techniques. Based on a series of measurements taken under different object positions, the signal contributions from individual voxels of significantly reduced size are calculated. Mathematically, the type of reconstruction used can be regarded as a deconvolution or solving an inverse problem. Due to the specific shape of the convolution kernel in the x-ray diffraction example treated here the problem turns out to be ill-posed, and thus its solution using measured (noisy) data requires the application of a suitable regularization method. Detailed studies on this issue led to the development of a novel iterative algorithm, combining several deconvolution runs with preceding and intermediate image processing steps. The Tikhonov method was used for regularization. Depending on the object under investigation, the original Euclidean norm (least-squares fit) was advantageously replaced by the 1-norm (least absolute deviation, LAD problem). The method presented here was developed to overcome resolution limitations in spatially resolved x-ray diffraction measurements on extended objects as used, e.g., for material analysis or the detection of illicit substances in baggage inspection applications. Nevertheless, the technique may easily be utilized for resolution enhancement within other imaging modalities, provided the task can be written as a deconvolution problem and the corresponding convolution kernel is known. According to the features of our experimental setup the developed reconstruction algorithm is explained for energy dispersive x-ray diffraction with pencil beam irradiation as an example application. The spatial resolution enhancement is demonstrated, using simulated and measured data sets corresponding to objects of different material composition.

    1. Micromechanical characterization of shales through nanoindentation and energy dispersive x-ray spectrometry

      DOE PAGES

      Veytskin, Yuriy B.; Tammina, Vamsi K.; Bobko, Christopher P.; ...

      2017-03-01

      Shales are heterogeneous sedimentary rocks which typically comprise a variable mineralogy (including compacted clay particles sub-micrometer in size), silt grains, and nanometer sized pores collectively arranged with transversely isotropic symmetry. Moreover, a detailed understanding of the micro- and sub-microscale geomechanics of these minerals is required to improve models of shale strength and stiffness properties. In this paper, we propose a linked experimental–computational approach and validate a combination of grid nanoindentation and Scanning Electron Microscopy (SEM) with Energy and Wavelength Dispersive X-ray Spectrometry (EDS/WDS) at the same spatial locations to identify both the nano-mechanical morphology and local mineralogy of these nanocomposites.more » The experimental parameters of each method are chosen to assess a similar volume of material. By considering three different shales of varying mineralogy and mechanical diversity, we show through the EMMIX statistical iterative technique that the constituent phases, including highly compacted plate- or sheet-like clay particles, carbonates, silicates, and sulfides, have distinct nano-mechanical morphologies and associated indentation moduli and hardness. Nanoindentation-based strength homogenization analysis determines an average clay packing density, friction coefficient, and solid cohesion for each tested shale sample. Comparison of bulk to microscale geomechanical properties, through bulk porosimetry measurements, reveals a close correspondence between bulk and microscale clay packing densities. Determining the mechanical microstructure and material properties is useful for predictive microporomechanical models of the stiffness and strength properties of shale. Furthermore, the experimental and computational approaches presented here also apply to other chemically and mechanically complex materials exhibiting nanogranular, composite behavior.« less

    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. Monte Carlo simulation of energy-dispersive x-ray fluorescence and applications

      NASA Astrophysics Data System (ADS)

      Li, Fusheng

      Four key components with regards to Monte Carlo Library Least Squares (MCLLS) have been developed by the author. These include: a comprehensive and accurate Monte Carlo simulation code - CEARXRF5 with Differential Operators (DO) and coincidence sampling, Detector Response Function (DRF), an integrated Monte Carlo - Library Least-Squares (MCLLS) Graphical User Interface (GUI) visualization System (MCLLSPro) and a new reproducible and flexible benchmark experiment setup. All these developments or upgrades enable the MCLLS approach to be a useful and powerful tool for a tremendous variety of elemental analysis applications. CEARXRF, a comprehensive and accurate Monte Carlo code for simulating the total and individual library spectral responses of all elements, has been recently upgraded to version 5 by the author. The new version has several key improvements: input file format fully compatible with MCNP5, a new efficient general geometry tracking code, versatile source definitions, various variance reduction techniques (e.g. weight window mesh and splitting, stratifying sampling, etc.), a new cross section data storage and accessing method which improves the simulation speed by a factor of four and new cross section data, upgraded differential operators (DO) calculation capability, and also an updated coincidence sampling scheme which including K-L and L-L coincidence X-Rays, while keeping all the capabilities of the previous version. The new Differential Operators method is powerful for measurement sensitivity study and system optimization. For our Monte Carlo EDXRF elemental analysis system, it becomes an important technique for quantifying the matrix effect in near real time when combined with the MCLLS approach. An integrated visualization GUI system has been developed by the author to perform elemental analysis using iterated Library Least-Squares method for various samples when an initial guess is provided. This software was built on the Borland C++ Builder

    4. In situ Monitoring of Synchrotron X-Ray-Induced Radiolysis Effects on Chromium Species Using X-Ray Absorption Spectroscopy

      NASA Astrophysics Data System (ADS)

      Men, S.; Anderson, A. J.; Mayanovic, R. A.

      2017-05-01

      Synchrotron X-ray radiolysis-induced redox in a chromium aqueous solution was monitored using in situ X-ray absorption spectroscopy. The radiolysis in the fluid sample within a specifically designed hydrothermal diamond anvil cell caused the oxidation of Cr(III) to Cr(VI) upon heating from room temperature to 400°C, and reduction of Cr(VI) to Cr(III) at 500°C. The two fitted components of the pre-edge features of the Cr K-edge spectra were used to identify the presence of Cr(VI) in the solution.

    5. 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.

    6. 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.

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

      SciTech Connect

      Nomura, Ryuichi; Uesugi, Kentaro

      2016-04-15

      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.

    8. 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.

    9. X-ray induced chemical reaction revealed by in-situ X-ray diffraction and scanning X-ray microscopy in 15 nm resolution (Conference Presentation)

      NASA Astrophysics Data System (ADS)

      Ge, Mingyuan; Liu, Wenjun; Bock, David; De Andrade, Vincent; Yan, Hanfei; Huang, Xiaojing; Marschilok, Amy; Takeuchi, Esther; Xin, Huolin; Chu, Yong S.

      2016-09-01

      The detection sensitivity of synchrotron-based X-ray techniques has been largely improved due to the ever increasing source brightness, which have significantly advanced ex-situ and in-situ research for energy materials, such as lithium-ion batteries. However, the strong beam-matter interaction arisen from the high beam flux can significantly modify the material structure. The parasitic beam-induced effect inevitably interferes with the intrinsic material property, which brings difficulties in interpreting experimental results, and therefore requires comprehensive evaluation. Here we present a quantitative in-situ study of the beam-effect on one electrode material Ag2VO2PO4 using four different X-ray probes with different radiation dose rate. The material system we reported exhibits interesting and reversible radiation-induced thermal and chemical reactions, which was further evaluated under electron microscopy to illustrate the underlying mechanism. The work we presented here will provide a guideline in using synchrotron X-rays to distinguish the materials' intrinsic behavior from extrinsic structure changed induced by X-rays, especially in the case of in-situ and operando study where the materials are under external field of either temperature or electric field.

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

      NASA Astrophysics Data System (ADS)

      Baker, John

      1991-05-01

      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.

    11. Misfit strain of oxygen precipitates in Czochralski silicon studied with energy-dispersive X-ray diffraction

      SciTech Connect

      Gröschel, A. Will, J.; Bergmann, C.; Magerl, A.

      2014-06-21

      Annealed Czochralski Silicon wafers containing SiO{sub x} precipitates have been studied by high energy X-ray diffraction in a defocused Laue setup using a laboratory tungsten tube. The energy dispersive evaluation of the diffracted Bragg intensity of the 220 reflection within the framework of the statistical dynamical theory yields the static Debye-Waller factor E of the crystal, which gives access to the strain induced by the SiO{sub x} precipitates. The results are correlated with precipitate densities and sizes determined from transmission electron microscopy measurements of equivalent wafers. This allows for the determination of the constrained linear misfit ε between precipitate and crystal lattice. For samples with octahedral precipitates the values ranging from ε = 0.39 (+0.28/−0.12) to ε = 0.48 (+0.34/−0.16) indicate that self-interstitials emitted into the matrix during precipitate growth contribute to the lattice strain. In this case, the expected value calculated from literature values is ε = 0.26 ± 0.05. Further, the precise evaluation of Pendellösung oscillations in the diffracted Bragg intensity of as-grown wafers reveals a thermal Debye-Waller parameter for the 220 reflection B{sup 220}(293 K) of 0.5582 ± 0.0039 Å{sup 2} for a structure factor based on spherically symmetric scattering contributions.

    12. The detection of food soils on stainless steel using energy dispersive X-ray and Fourier transform infrared spectroscopy.

      PubMed

      Whitehead, K A; Benson, P S; Verran, J

      2011-09-01

      Organic soiling is a major issue in the food processing industries, causing a range of biofouling and microbiological problems. Energy dispersive X-ray (EDX) and Fourier transform infra red spectroscopy (FT-IR) were used to quantify and determine the biochemical groups of food soils on stainless steel surfaces. EDX quantified organic material on surfaces where oily based residues predominated, but was limited in its usefulness since other food soils were difficult to detect. FT-IR provided spectral 'fingerprints' for each of the soils tested. Key soiling components were associated with specific peaks, viz. oils at 3025 cm(-1)-3011 cm(-1), proteins at 1698 cm(-1)-1636 cm(-1) and carbohydrates at 1658 cm(-1)-1596 cm(-1), 783 cm(-1)-742 cm(-1). High concentrations of some soils (10%) were needed for detection by both EDX and FT-IR. The two techniques may be of use for quantifying and identifying specific recalcitrant soils on surfaces to improve cleaning and hygiene regimes.

    13. 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.

    14. 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.

    15. Determination of Zn in Dry Feeds for Cats and Dogs by Energy-Dispersive X-Ray Fluorescence Spectrometry.

      PubMed

      Ávila, Dayara Virgnía L; Souza, Sidnei O; Costa, Silvânio Silvério L; Araujo, Rennan Geovanny O; Garcia, Carlos Alexandre B; Alves, José do Patrocínio H; Passos, Elisangela A

      2016-11-01

      This work describes an analytical method for Zn determination in dry feeds for cats and dogs by energy-dispersive X-ray fluorescence (EDXRF). Samples of dry feed were powdered and prepared in the form of pellets for direct analysis by EDXRF. The LOQ (10σ) was 0.4 mg/kg. The samples were also analyzed by inductively coupled plasma-optical emission spectrometry (ICP-OES) as an independent comparative method. Application of a paired t-test showed no significant differences between Zn concentrations obtained by EDXRF and ICP-OES (at a 95% confidence level). Analysis of variance was also applied to the results and revealed no significant differences between the two techniques (at a 95% confidence level). The precision, expressed as the RSD (n = 3), was RSD < 4.55%. This analytical method provides a simple, rapid, accurate, and precise determination of Zn in dry feeds for cats and dogs by EDXRF as direct, solid-sample analysis.

    16. Scanning electron microscopy and energy-dispersive X-ray analysis of defects in mature rat incisor enamel after thyroparathyroidectomy.

      PubMed

      Chardin, H; Acevedo, A C; Risnes, S

      1998-04-01

      The surface and the structure of the erupted enamel of the continuously growing rat incisor were studied by scanning electron microscopy (SEM) to analyse the effect of thyroparathyroidectomy on enamel formation. Ten male 21-day-old Wistar rats were thyroparathyroidectomized and five sham-operated rats were used as controls. Two months after surgery the rats were perfused with 1% glutaraldehyde and their mandibles dissected. The erupted ends of the incisors were cut off and routinely processed for SEM. An energy-dispersive analysis of X-rays (EDX analysis) was performed for the calcium:iron ratio of the enamel surface defects. Thyroparathyroidectomy induced surface defects and structural abnormalities in the outer layer of the mature erupted enamel. It was established that the surface and structural defects were related. The EDX analysis of the outer enamel showed that the enamel defects were associated with an abnormal elevation of the iron content. The SEM appearance and the EDX analyses indicated that these defects were hypomineralized and rich in iron. The reddish colour of the enamel is due to the high concentrations of iron.

    17. Scanning electron microscopy and energy-dispersive X-ray microanalysis studies of several human calculi containing calcium phosphate crystals.

      PubMed

      Kodaka, T; Debari, K; Sano, T; Yamada, M

      1994-01-01

      Human calcium phosphate calculi: two sialoliths, a urolith, a rhinolith, and a tonsillolith were investigated by scanning electron microscopy (SEM) and energy-dispersive X-ray analysis (EDX). The sialoliths and urolith had appositional shells with thick cortices, respectively, around several nuclei composed of calcospherulites and a rubber-film fragment. The rhinolith had a thin cortex with appositional laminations around a glomerulus-like mass of calcified cotton-like strings. The tonsillolith had a rough cortex with appositional laminations. Its porous interior was composed of numerous calcified conglomerates with microorganisms and calcified masses with fine appositional laminations around the conglomerates. The major crystals were identified as biological apatites (AP) with a sand-grain rather than a needle-like shape, and plate-shaped octacalcium phosphate (OCP). The AP deposits of the rhinolith probably were associated with magnesium (Mg) phosphates or contained Mg. No OCP was found in the rhinolith. The AP deposits were mainly formed by extracellular calcification. Hexahedral crystals, identified as Mg-containing whitlockite (WH), were precipitated in the internal spaces of the AP and OCP deposits. The rhinolith nucleus consisted of WH crystal deposits only.

    18. Determination of Nickel and Manganese Contaminants in Pharmaceutical Iron Supplements Using Energy Dispersive X-ray Fluorescence.

      PubMed

      Cardoso, Pedro; Amaro, Pedro; Santos, José Paulo; de Assis, Joaquim T; Carvalho, Maria Luisa

      2017-03-01

      In this study, we investigate the capability of energy dispersive X-ray fluorescence (EDXF) spectrometry in a triaxial geometry apparatus as a fast and nondestructive determination method of both dominant and contaminant elements in pharmaceutical iron supplements. The following iron supplements brands with their respective active ingredients were analyzed: Neutrofer fólico (iron gylcinate), Anemifer (iron(II) sulfate monohydrate), Noripurum (iron(III)-hydroxide polymaltose complex), Sulferbel (iron(II) sulfate monohydrate), and Combiron Fólico (carbonyl iron). Although we observe a good agreement between the iron content obtained by the present method and that indicated in the supplement's prescribed dose, we observe contamination by manganese and nickel of up to 180 μg and 36 μg, respectively. These contents correspond to 7.2% and 14.4% of the permitted daily exposure of manganese and nickel, respectively, for an average adult individual as determined by the European Medicine Agency (EMEA). The method was successfully validated against the concentrations of several certified reference materials of biological light matrices with similar concentrations of contaminants. Moreover, we also validated our method by comparing the concentrations with those obtained with the inductively coupled plasma-atomic emission technique.

    19. 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

    20. 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.

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

      PubMed

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

      2012-10-01

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

    2. 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

      2014-02-04

      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.

    3. Energy dispersive X-ray fluorescence analysis of mine waters from the Migori Gold Mining Belt in Southern Nyanza, Kenya.

      PubMed

      Odumo, O B; Mustapha, A O; Patel, J P; Angeyo, H K

      2011-09-01

      Analyses of water samples from Mikei, Osiri, Masara and Macalder (Makalda) gold mines of the Migori gold mining belt of Southwestern Kenya were done to determine the level of heavy metals using the Energy Dispersive X-ray Fluorescence technique. The concentrations of the heavy metals were; copper (29.34 ± 5.01-14,975.59 ± 616.14 μg/L); zinc (33.69 ± 4.29-683.15 ± 32.93 μg/L); arsenic (958.16 ± 60.14-18,047.52 ± 175.00 μg/L) and lead (19.51 ± 5.5-214.53 ± 6.29 μg/L). High levels of arsenic and lead were noted. These heavy metals are not only dangerous to the lives of miners and the local inhabitants; they are also a threat to aquatic life since these waters finally find their way into Lake Victoria.

    4. Integrated sorption-energy-dispersive X-ray fluorescence detection for automatic determination of lead and cadmium in low-concentration solutions.

      PubMed

      Pérez-Serradilla, J A; Luque de Castro, M D

      2007-11-01

      Sorbent material packed in a PTFE laboratory-made flow cell located in the specimen holder of an energy-dispersive X-ray fluorescence (EDXRF) detector has been used for in situ solid-phase extraction (SPE) preconcentration-detection of metals. The flow cell was connected to a single-channel flow-injection (FI) manifold (for full automation of the steps and proper development of the method) by two PTFE tubes of 0.5-mm inner diameter introduced into the spectrometer specimen holder by a small orifice without distortion or modification of the instrument. The optical window open in the PTFE flow cell was adjusted to the X-ray irradiation zone of the spectrometer and fixed to it. The approach was tested by using both Pb and Cd aqueous solutions and a Dowex 50 cation-exchange resin as a sorbent, and flushing the sample through the flow cell for EDXRF measurements after removal of the sample matrix. The limits of detection and the limits of quantification (LOQs) thus obtained were 0.15 and 0.5 microg for Pb and 0.3 and 0.8 microg for Cd, respectively, values that allow the approach to be used for the analysis of drinking water by injecting a 100-mL sample into the FI manifold, taking into account the EC drinking water directives. The linear dynamic ranges are between the LOQ and 600 microg for both analytes. The method was validated by the standard addition method using tap-water samples. In addition, the integrated SPE-EDXRF approach enables the study of the variables influencing the sorption step-namely the effects of the volume of sample flushed through the column, concentrations of the analytes in the sample, breakthrough volume of the resin, elution profiles, sample pH and retention and elution flow rates-in an automatic, cheap, fast and precise way.

    5. 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.

    6. Low-energy shelf response in thin energy-dispersive X-ray detectors from Compton scattering of hard X-rays

      NASA Astrophysics Data System (ADS)

      Michel-Hart, N.; Elam, W. T.

      2017-08-01

      Silicon drift detectors have been successfully employed in both soft and hard X-ray spectroscopy. The response function to incident radiation at soft X-ray levels has been well studied and modeled, but less research has been published on response functions for these detectors to hard X-ray input spectra above 20 keV. When used with hard X-ray sources a significant low energy, non-peak response exists which can adversely affect detection limits for lighter elements in, for example, X-ray fluorescence spectroscopy. We present a numerical model that explains the non-peak response function of silicon drift detectors to hard X-rays based on incoherent Compton scattering within the detector volume. Experimental results are presented and numerically compared to model results.

    7. Trace elements as tumor biomarkers and prognostic factors in breast cancer: a study through energy dispersive x-ray fluorescence

      PubMed Central

      2012-01-01

      Background The application and better understanding of traditional and new breast tumor biomarkers and prognostic factors are increasing due to the fact that they are able to identify individuals at high risk of breast cancer, who may benefit from preventive interventions. Also, biomarkers can make possible for physicians to design an individualized treatment for each patient. Previous studies showed that trace elements (TEs) determined by X-Ray Fluorescence (XRF) techniques are found in significantly higher concentrations in neoplastic breast tissues (malignant and benign) when compared with normal tissues. The aim of this work was to evaluate the potential of TEs, determined by the use of the Energy Dispersive X-Ray Fluorescence (EDXRF) technique, as biomarkers and prognostic factors in breast cancer. Methods By using EDXRF, we determined Ca, Fe, Cu, and Zn trace elements concentrations in 106 samples of normal and breast cancer tissues. Cut-off values for each TE were determined through Receiver Operating Characteristic (ROC) analysis from the TEs distributions. These values were used to set the positive or negative expression. This expression was subsequently correlated with clinical prognostic factors through Fisher’s exact test and chi-square test. Kaplan Meier survival curves were also evaluated to assess the effect of the expression of TEs in the overall patient survival. Results Concentrations of TEs are higher in neoplastic tissues (malignant and benign) when compared with normal tissues. Results from ROC analysis showed that TEs can be considered a tumor biomarker because, after establishing a cut-off value, it was possible to classify different tissues as normal or neoplastic, as well as different types of cancer. The expression of TEs was found statistically correlated with age and menstrual status. The survival curves estimated by the Kaplan-Meier method showed that patients with positive expression for Cu presented a poor overall survival (p

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

      PubMed Central

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

      2017-01-01

      The full strain and stress tensor determination in a triaxially stressed single crystal using X-ray diffraction requires a series of lattice spacing measurements at different crystal orientations. This can be achieved using a tunable X-ray source. This article reports on a novel experimental procedure for single-shot full strain tensor determination using polychromatic synchrotron radiation with an energy range from 5 to 23 keV. Microbeam X-ray Laue diffraction patterns were collected from a copper micro-bending beam along the central axis (centroid of the cross section). Taking advantage of a two-dimensional energy-dispersive X-ray detector (pnCCD), the position and energy of the collected Laue spots were measured for multiple positions on the sample, allowing the measurement of variations in the local microstructure. At the same time, both the deviatoric and hydrostatic components of the elastic strain and stress tensors were calculated. PMID:28656042

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

      PubMed

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

      2017-06-01

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

    10. 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.

    11. Lung dust content in idiopathic pulmonary fibrosis: a study with scanning electron microscopy and energy dispersive x ray analysis.

      PubMed Central

      Monsó, E; Tura, J M; Pujadas, J; Morell, F; Ruiz, J; Morera, J

      1991-01-01

      Examination with an optical microscope and polarised light is not sensitive enough to detect low diameter asbestos fibres. This limitation implies that some cases of asbestosis can be erroneously diagnosed as idiopathic pulmonary fibrosis (IPF) if asbestos bodies are not found in the standard examination of abnormal tissue. To determine whether IPF is over-diagnosed, a study was carried out with scanning electron microscopy (SEM) and energy dispersive x ray analysis (EDXA) on 25 samples previously diagnosed as IPF at the standard examination. Scanning electron microscopy will show the presence of low diameter fibres in the lung without tissue destruction, and these fibres can be identified using EDXA. The quantitative and qualitative results for lung tissue from patients diagnosed as having IPF were compared with the results of the examination of 25 samples of normal lung. Most of the samples from patients diagnosed as having IPF showed only occasional inorganic particles (less than 10 particles/SEM field at 160 x), results equivalent to the results obtained in normal lung. Two cases of IPF, however, showed innumerable asbestos fibres (greater than 100 fibres/SEM field). One of these two patients had an antecedent of brief exposure to asbestos. No environmental antecedent was found in the second patient. Asbestosis was the final diagnosis for these two patients. The examination of inorganic particles in normal lungs showed mainly non-fibrous silicates (61.4%) and particles of heavy elements (34.9%). Only one asbestos fibre was found (0.9%). It is concluded that standard pathological techniques overdiagnose IPF in a few cases in which asbestos bodies are not found with the optical microscope. Images PMID:2039745

    12. Chemical elements characterization of root canal sealers using scanning electron microscopy and energy dispersive X-ray analysis.

      PubMed

      Sampaio, Felipe Cavalcanti; Alencar, Ana Helena Gonçalves; Guedes, Orlando Aguirre; Veloso, Heloisa Helena Pinho; Santos, Tatiane Oliveira; Estrela, Carlos

      2014-03-01

      The aim of this study was to evaluate the chemical elements composition of root canal filling materials using Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray analysis (EDX). Eighteen standard polyethylene tubes were filled with the following materials: Sealapex(®), Sealer 26(®), MTA Fillapex(®), Pulp Canal Sealer(®), Endofill(®) and AH Plus(®). After 48 hours at 37°C and 95% relative humidity, the samples were surface-sputtered with gold and analyzed using SEM at 5000X magnification. Their chemical composition and element distributionwere determined using EDX. Results were evaluated qualitatively (SEM images and elemental mapping) and quantitatively (weight percentage). Calcium oxide- and hydroxide-based sealers (Sealapex(®) and Sealer 26(®)) had calcium peaks of 53.58 wt% and 65.00 wt%. MTA Fillapex(®) had 30.58 wt% of calcium and high amounts of silicon (31.02 wt%) and bismuth (27.38 wt%). Zinc oxide- and eugenol-based sealers, Pulp Canal Sealer(®) and Endofill(®), had 67.74 wt% and 63.16 wt% of zinc each. AH Plus(®) had a higher amount of zirconium (64.24 wt%). All materials had elements other than those described by the manufacturers. Surface analysis using EDX revealed that regularity varied, element distribution was uniform, and particles had similar sizes and variable shapes. Most chemical elements were those described by the manufacturers, but percentages were different. The surface of root canal sealers had different regularity findings, uniform distribution and particles of similar sizes but variable shapes.

    13. In Situ Mineralogical Analysis of Planetary Materials Using X-Ray Diffraction and X-Ray Fluorescence

      NASA Technical Reports Server (NTRS)

      Sarrazin, P.; Blake, D.; Vaniman, D.; Chang, Sherwood (Technical Monitor)

      1996-01-01

      pinhole camera (transmission geometry, flat two-dimensional detector perpendicular to the direct beam), the instrument (which we call CHEMIN, for Chemistry and Mineralogy) uses an X-ray sensitive CCD detector which will allow concurrent positional and energy-dispersive analysis of collected photons. Thus XRF (energy) and XRD (geometry) analysis of transmitted X-rays will be performed at the same time. Tests performed with single minerals and simple mixtures give promising results. Refinements of the prototype promise interpretable results on complex samples.

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

      NASA Astrophysics Data System (ADS)

      Donais, Mary Kate; Van Pevenage, Jolien; Sparks, Andrew; Redente, Monica; George, David B.; Moens, Luc; Vincze, Laszlo; Vandenabeele, Peter

      2016-12-01

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

    15. 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.

    16. Determination of the sequence of intersecting lines from laser toner and seal ink by Fourier transform infrared microspectroscopy and scanning electron microscope / energy dispersive X-ray mapping.

      PubMed

      Wang, Yuanfeng; Li, Bing

      2012-06-01

      The aim of this study was to verify that the combination of Fourier transform infrared microspectroscopy and scanning electron microscope / energy dispersive X-ray mapping could be applied to line intersection problems. The spectral data of red seal ink, laser toner and their intersections, such as peak location and peak intensity, were described. Relative peak height ratios of different chemical components in intersecting lines were used to distinguish the sequences. Energy dispersive X-ray mapping characteristics of intersecting areas were also detailed. The results show that both the laser toner and the seal ink appear on the surface of intersections, regardless of the sequence. The distribution of the two inks on the surface is influenced not only by the sequence of heterogeneous lines but also by diffusion. Fourier transform infrared microspectroscopy and scanning electron microscope/energy dispersive X-ray mapping are able to explore the chemical components and the corresponding elemental distribution in the intersections. The combination of these two techniques has provided a reliable method for sequencing intersecting lines of red seal ink and laser toner, and more importantly, this method may be a basis for sequencing superimposed lines from other writing instruments.

    17. 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.

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

      DOE PAGES

      Alonso-Mori, Roberto; Kern, Jan; Gildea, Richard J.; ...

      2012-11-05

      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 wellmore » 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. Furthermore, 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.« less

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

      PubMed

      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

      2012-11-20

      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. Kβ(1,3) XES spectra of Mn(II) and Mn(2)(III,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.

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

      SciTech Connect

      Alonso-Mori, Roberto; Kern, Jan; Gildea, Richard J.; Sokaras, Dimosthenis; Weng, Tsu -Chien; Lassalle-Kaiser, Benedikt; Tran, Rosalie; Hattne, Johan; Laksmono, Hartawan; Hellmich, Julia; Glockner, 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, Sebastien; Williams, Garth J.; Zouni, Athina; Messinger, Johannes; Glatzel, Pieter; Sauter, Nicholas K.; Yachandra, Vittal K.; Yano, Junko; Bergmann, Uwe

      2012-11-05

      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. Furthermore, 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.

    1. [Research on the content prediction model for the determination of nickel in soil by portable energy dispersive X-ray fluorescence analyzer].

      PubMed

      Wang, Guang-Xi; Li, Dan; Lai, Wan-Chang; Zhai, Juan; Yang, Zhong-Jian; Hou, Xin; Cao, Fa-Ming

      2013-08-01

      The present paper discusses the influence of matrix effect on measurement results when portable energy dispersive X-ray fluorescence analyzer is used for the determination of Ni in soil. Based on the scattered X-ray intensity of WL(alpha) emitted from the X-ray tube on the sample, a correction method was proposed, and it combines with the correction of absorption element, which can effectively overcome the matrix effect. The correlation coefficient of the content prediction model based on this method is 0.999 and the residual standard deviation is 2.541. The average relative error is 3.90 when the content prediction model is used to measure the content of Ni in the national standard soil samples, so the results coincide well with standard values, and the precision is high.

    2. 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.

    3. Application of in situ x-ray absorption and fluorescence measurements to analyze solutions in a simulated pit

      SciTech Connect

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

      1991-12-31

      X-ray energy-dispersive spectroscopy has been used to study the compositions of metal ions in solutions developed during localized corrosion. An electrochemical cell was designed to simulate a corrosion pit, maintaining one-dimensional diffusion and fulfilling the requirements for x-ray fluorescence measurements. The working electrode consisted of a dissolving thin foil of Type 304 stainless steel sealed between Mylar sheets through which the x-ray beam passed. Concentration gradients within the artificial pit were quantitatively determined.

    4. Application of in situ x-ray absorption and fluorescence measurements to analyze solutions in a simulated pit

      SciTech Connect

      Isaacs, H.S.; Davenport, A.J.; Cho, J.H. ); Rivers, M.L.; Sutton, S.R. . Dept. of Geophysical Sciences)

      1991-01-01

      X-ray energy-dispersive spectroscopy has been used to study the compositions of metal ions in solutions developed during localized corrosion. An electrochemical cell was designed to simulate a corrosion pit, maintaining one-dimensional diffusion and fulfilling the requirements for x-ray fluorescence measurements. The working electrode consisted of a dissolving thin foil of Type 304 stainless steel sealed between Mylar sheets through which the x-ray beam passed. Concentration gradients within the artificial pit were quantitatively determined.

    5. 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.

    6. 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.

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

      PubMed

      Toyoshima, Ryo; Kondoh, Hiroshi

      2015-03-04

      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.

    8. Evaluation of Root Canal Dentin Erosion after Different Irrigation Methods Using Energy-dispersive X-ray Spectroscopy.

      PubMed

      Wang, Zhejun; Maezono, Hazuki; Shen, Ya; Haapasalo, Markus

      2016-12-01

      The purpose of this study was to examine the level of erosion in root dentin caused by different irrigation methods and protocols. Thirty-five extracted upper molar teeth were instrumented and divided into 7 groups to undergo treatment by different methods: negative control, GentleWave System (Sonendo Inc, Laguna Hills, CA), and syringe needle irrigation following different protocols. The teeth were instrumented to size #25/.08 or #30/.09 for needle irrigation groups and to ProTaper size S1 for the GentleWave group under 5% sodium hypochlorite (NaOCl). The needle irrigation groups were subjected to final rinses of 2 minutes of 3% NaOCl + 2 minutes of 8% EDTA (3% N2 + 8% E2), 2 minutes of 3% NaOCl + 2 minutes of 8% EDTA + 1 minute of 3% NaOCl (3% N2 + 8% E2 + 3% N1), 2 minutes of 5% NaOCl + 2 minutes of 17% EDTA (5% N2 + 17% E2), 2 minutes of 5% NaOCl + 2 minutes of 17% EDTA + 1 minute of 5% NaOCl (5% N2 + 17% E2 + 5% N1), and 5 minutes of 5% NaOCl + 5 minutes of 17% EDTA + 5 minutes of 5% NaOCl (5% N5 + 17% E5 + 5% N5), respectively. The root canal surface was observed by scanning electron microscopy, and the dentin composition was analyzed by continuous line scanning for 300 μm into dentin using energy-dispersive X-ray spectroscopy. A slight but statistically significant decrease of calcium and an increase of carbon was measured in the 5% N2 + 17% E2 group in comparison with the control; no significant difference was found among GentleWave, 3% N2 + 8% E2, and 5% N2 + 17% E2 (P > .05). A final 1-minute rinse with 3% or 5% NaOCl reduced calcium and phosphorus to a significantly lower level than in groups without a 1-minute final rinse (P < .05). Final irrigation with 5% NaOCl for 5 minutes removed almost all calcium and phosphorus. Scanning electron microscopy showed canal wall erosion when an additional final irrigation with NaOCl was done. NaOCl followed by final EDTA irrigation performed either by syringe needle or the Gentle

    9. 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).

    10. Simulation of an energy-dispersion x-ray spectrometer in the computational medium X-Energo

      SciTech Connect

      Plotnikov, R.I.; Savel`ev, S.K.; Fedorov, S.I.

      1995-01-01

      The description of the calculation part of the simulation medium X-Energo is presented. It contains mathematical models included in the medium X-Energo for the determinating major processes taking place in an X-ray spectrometer, namely, the formation of an X-ray radiation spectrum, the interaction of this radiation with filter and sample materials, and the detector response to the signal. 6 refs.

    11. 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.

    12. In situ laser heating and radial synchrotron x-ray diffraction in a diamond anvil cell

      SciTech Connect

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

      2007-06-15

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

    13. In situ laser heating and radial synchrotron x-ray diffraction in a diamond anvil cell.

      PubMed

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

      2007-06-01

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

    14. In situ X-ray-based imaging of nano materials

      SciTech Connect

      Weker, Johanna Nelson; Huang, Xiaojing; Toney, Michael F.

      2016-02-13

      We study functional nanomaterials that are heterogeneous and understanding their behavior during synthesis and operation requires high resolution diagnostic imaging tools that can be used in situ. Over the past decade, huge progress has been made in the development of X-ray based imaging, including full field and scanning microscopy and their analogs in coherent diffractive imaging. Currently, spatial resolution of about 10 nm and time resolution of sub-seconds are achievable. For catalysis, X-ray imaging allows tracking of particle chemistry under reaction conditions. In energy storage, in situ X-ray imaging of electrode particles is providing important insight into degradation processes. Recently, both spatial and temporal resolutions are improving to a few nm and milliseconds and these developments will open up unprecedented opportunities.

    15. Simple load frame for in situ computed tomography and x-ray tomographic microscopy

      SciTech Connect

      Breunig, T.M. ); Stock, S.R.; Brown, R.C. )

      1993-05-01

      In many instances, the response of a sample to external stimuli must be observed repeatedly during the course of an experiment. The sequence in which features are formed is often critical to proper identification of the mechanisms operating, for example, in fatigue and fracture. Merely observing what is visible at the surface of the sample can be misleading or can provide inadequate information about what governs fatigue crack growth or about what controls the fracture process. X-ray imaging allows one to observe the interior of samples and is an attractive technique to use with in situ stressing of test specimens. Here, a simple compact, inexpensive load frame is described for in situ x-ray computed tomography and for very high resolution computed tomography, termed x-ray tomographic microscopy. The load frame is evaluated, and its use is illustrated by observations of crack closure as a function of load in a notched tensile sample of Al-Li-2090.

    16. 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

    17. 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.

    18. Modular deposition chamber for in situ X-ray experiments during RF and DC magnetron sputtering.

      PubMed

      Krause, Bärbel; Darma, Susan; Kaufholz, Marthe; Gräfe, Hans Hellmuth; Ulrich, Sven; Mantilla, Miguel; Weigel, Ralf; Rembold, Steffen; Baumbach, Tilo

      2012-03-01

      A new sputtering system for in situ X-ray experiments during DC and RF magnetron sputtering is described. The outstanding features of the system are the modular design of the vacuum chamber, the adjustable deposition angle, the option for plasma diagnostics, and the UHV sample transfer in order to access complementary surface analysis methods. First in situ diffraction and reflectivity measurements during RF and DC deposition of vanadium carbide demonstrate the performance of the set-up.

    19. Composition Analysis of III-Nitrides at the Nanometer Scale: Comparison of Energy Dispersive X-ray Spectroscopy and Atom Probe Tomography

      NASA Astrophysics Data System (ADS)

      Bonef, Bastien; Lopez-Haro, Miguel; Amichi, Lynda; Beeler, Mark; Grenier, Adeline; Robin, Eric; Jouneau, Pierre-Henri; Mollard, Nicolas; Mouton, Isabelle; Monroy, Eva; Bougerol, Catherine

      2016-10-01

      The enhancement of the performance of advanced nitride-based optoelectronic devices requires the fine tuning of their composition, which has to be determined with a high accuracy and at the nanometer scale. For that purpose, we have evaluated and compared energy dispersive X-ray spectroscopy (EDX) in a scanning transmission electron microscope (STEM) and atom probe tomography (APT) in terms of composition analysis of AlGaN/GaN multilayers. Both techniques give comparable results with a composition accuracy better than 0.6 % even for layers as thin as 3 nm. In case of EDX, we show the relevance of correcting the X-ray absorption by simultaneous determination of the mass thickness and chemical composition at each point of the analysis. Limitations of both techniques are discussed when applied to specimens with different geometries or compositions.

    20. 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.

    1. An energy-dispersive X-ray analysis and SEM study of debris remaining on endodontic instruments after ultrasonic cleaning and autoclave sterilization.

      PubMed

      Parirokh, Masoud; Asgary, Saeed; Eghbal, Mohammad Jafar

      2005-08-01

      This study was carried out to investigate metallic and non-metallic debris remaining on endodontic files after ultrasonic cleaning and autoclave processing. Forty-eight unused rotary and hand endodontic files, including eight different brands, were tested. Instruments were cleaned with ultrasound, autoclaved and before and after each step were observed by scanning electron microscopy (SEM). Adherent debris was analysed by energy-dispersive X-ray analysis (EDXA). All of the instruments before ultrasound cleaning were contaminated with metallic and non-metallic debris. Although most non-metallic debris was removed by ultrasonic cleaning, most of the metallic debris remained even after the final step of sterilization.

    2. Data on Heavy metal in coastal sediments from South East Coast of Tamilnadu, India using Energy Dispersive X-ray Fluorescence (EDXRF) Technique.

      PubMed

      Chandramohan, J; Senthilkumar, G; Gandhi, M Suresh; Ravisankar, R

      2016-12-01

      This article contains the chemical and geographical data and figures for the chemical data in sediments of East Coast (Pattipulam to Dhevanampattinam) of Tamilnadu. The obtained data are related to the research article "Heavy Metal Assessment in Sediment Samples Collected From Pattipulam to Dhevanampattinam along the East Coast of Tamil Nadu Using EDXRF Technique" (Chandramohan et al., 2016) [1]. Chemical data are collected from Energy dispersive X-ray fluorescence spectrometer (EDXRF). Furthermore, the obtained chemical data describes it in more detail in the figures.

    3. Component analyses of urinary nanocrystallites of uric acid stone formers by combination of high-resolution transmission electron microscopy, fast Fourier transformation, energy dispersive X-ray spectroscopy, X-ray diffraction and Fourier transform infrared spectroscopy.

      PubMed

      Sun, Xin-Yuan; Xue, Jun-Fa; Xia, Zhi-Yue; Ouyang, Jian-Ming

      2015-06-01

      This study aimed to analyse the components of nanocrystallites in urines of patients with uric acid (UA) stones. X-ray diffraction (XRD), Fourier transform infrared spectroscopy, high-resolution transmission electron microscopy (HRTEM), fast Fourier transformation (FFT) of HRTEM, and energy dispersive X-ray spectroscopy (EDS) were performed to analyse the components of these nanocrystallites. XRD and FFT showed that the main component of urinary nanocrystallites was UA, which contains a small amount of calcium oxalate monohydrate and phosphates. EDS showed the characteristic absorption peaks of C, O, Ca and P. The formation of UA stones was closely related to a large number of UA nanocrystallites in urine. A combination of HRTEM, FFT, EDS and XRD analyses could be performed accurately to analyse the components of urinary nanocrystallites.

    4. 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.

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

      PubMed

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

      2017-02-01

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

    6. Electron paramagnetic resonance, scanning electron microscopy with energy dispersion X-ray spectrometry, X-ray powder diffraction, and NMR characterization of iron-rich fired clays.

      PubMed

      Presciutti, Federica; Capitani, Donatella; Sgamellotti, Antonio; Brunetti, Brunetto Giovanni; Costantino, Ferdinando; Viel, Stéphane; Segre, Annalaura

      2005-12-01

      The aim of this study is to clarify the structure of an iron-rich clay and the structural changes involved in the firing process as a preliminary step to get information on ancient ceramic technology. To this purpose, illite-rich clay samples fired at different temperatures were characterized using a multitechnique approach, i.e., by electron paramagnetic resonance, scanning electron microscopy with electron dispersion X-ray spectrometry, X-ray powder diffraction, magic angle spinning and multiple quantum magic angle spinning NMR. During firing, four main reaction processes occur: dehydration, dehydroxylation, structural breakdown, and recrystallization. When the results are combined from all characterization methods, the following conclusions could be obtained. Interlayer H2O is located close to aluminum in octahedral sites and is driven off at temperatures lower than 600 degrees C. Between 600 and 700 degrees C dehydroxylation occurs whereas, between 800 and 900 degrees C, the aluminum in octahedral sites disappears, due to the breakdown of the illite structure, and all iron present is oxidized to Fe3+. In samples fired at 1000 and 1100 degrees C iron clustering was observed as well as large single crystals of iron with the occurrence of ferro- or ferrimagnetic effects. Below 900 degrees C the aluminum in octahedral sites presents a continuous distribution of chemical shift, suggesting the presence of slightly distorted sites. Finally, over the whole temperature range, the presence of at least two tetrahedral aluminum sites was revealed, characterized by different values of the quadrupolar coupling constant.

    7. 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.

    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. Reactor for nano-focused x-ray diffraction and imaging under catalytic in situ conditions

      NASA Astrophysics Data System (ADS)

      Richard, M.-I.; Fernández, S.; Hofmann, J. P.; Gao, L.; Chahine, G. A.; Leake, S. J.; Djazouli, H.; De Bortoli, Y.; Petit, L.; Boesecke, P.; Labat, S.; Hensen, E. J. M.; Thomas, O.; Schülli, T.

      2017-09-01

      A reactor cell for in situ studies of individual catalyst nanoparticles or surfaces by nano-focused (coherent) x-ray diffraction has been developed. Catalytic reactions can be studied in flow mode in a pressure range of 10-2-103 mbar and temperatures up to 900 °C. This instrument bridges the pressure and materials gap at the same time within one experimental setup. It allows us to probe in situ the structure (e.g., shape, size, strain, faceting, composition, and defects) of individual nanoparticles using a nano-focused x-ray beam. Here, the setup was used to observe strain and facet evolution of individual model Pt catalysts during in situ experiments. It can be used for heating other (non-catalytically active) nanoparticles (e.g., nanowires) in inert or reactive gas atmospheres or vacuum as well.

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

      DTIC Science & Technology

      2015-09-08

      AFRL-RX-WP-JA-2016-0273 A ROTATIONAL AND AXIAL MOTION SYSTEM LOAD FRAME INSERT FOR IN SITU HIGH ENERGY X - RAY STUDIES (POSTPRINT...SUBTITLE A ROTATIONAL AND AXIAL MOTION SYSTEM LOAD FRAME INSERT FOR IN SITU HIGH ENERGY X - RAY STUDIES (POSTPRINT) 5a. CONTRACT NUMBER FA8650-14...final publication is available at http://dx.doi.org/10.1063/1.4927855 14. ABSTRACT (Maximum 200 words) High energy x - ray characterization methods hold

    12. In situ fine tuning of bendable soft x-ray mirrors using a lateral shearing interferometer

      NASA Astrophysics Data System (ADS)

      Merthe, Daniel J.; Goldberg, Kenneth A.; Yashchuk, Valeriy V.; McKinney, Wayne R.; Celestre, Richard; Mochi, Iacopo; MacDougall, James; Morrison, Gregory Y.; Rekawa, Senajith B.; Anderson, Erik; Smith, Brian V.; Domning, Edward E.; Padmore, Howard

      2013-05-01

      Broadly applicable, in situ at-wavelength metrology methods for x-ray optics are currently under development at the Advanced Light Source. We demonstrate the use of quantitative wavefront feedback from a lateral shearing interferometer for the suppression of aberrations. With the high sensitivity provided by the interferometer we were able to optimally tune the bending couples of a single elliptical mirror (NA=2.7 mrad) in order to focus a beam of soft x-rays (1.24 keV) to a nearly diffraction-limited beam waist size of 156(±10) nm.

    13. Effect of bleaching agents having a neutral pH on the surface of mineral trioxide aggregate using electron microscopy and energy dispersive X-ray microanalysis

      PubMed Central

      Kazia, Nooh; Suvarna, Nithin; Shetty, Harish Kumar; Kumar, Pradeep

      2016-01-01

      Aim: To investigate the effect of bleaching agents having a neutral pH on the surface of mineral trioxide aggregate (MTA) used as a coronal seal material for nonvital bleaching, beneath the bleaching agent, with the help of energy dispersive X-ray microanalysis and scanning electron microscopy (SEM). Materials and Methods: Six samples of plastic tubes filled with white MTA (Angelus white) were kept in 100% humidity for 21 days. Each sample was divided into 2 and made into 12 samples. These were then divided into three groups. Group A was exposed to Opalescence Boost 40% hydrogen peroxide (HP) (Ultradent). Group B to Opalescence 10% carbamide peroxide (Ultradent) and Group C (control group) not exposed to any bleaching agent. After recommended period of exposure to bleaching agents according to manufacturers’ instructions, the samples were observed under SEM with an energy dispersive X-ray microanalysis system (JSM-6380 LA). Results: There were no relevant changes in color and no statistically significant surface structure changes of the MTA in both the experimental groups. Conclusion: The present findings suggest that even high concentration HP containing bleaching agents with neutral pH can be used on the surface of MTA without causing structural changes. The superior sealing ability of MTA and the high alkalinity would prevent cervical resorption postbleaching. PMID:27656061

    14. Hard X-ray-induced damage on carbon-binder matrix for in situ synchrotron transmission X-ray microscopy tomography of Li-ion batteries.

      PubMed

      Lim, Cheolwoong; Kang, Huixiao; De Andrade, Vincent; De Carlo, Francesco; Zhu, Likun

      2017-05-01

      The electrode of Li-ion batteries is required to be chemically and mechanically stable in the electrolyte environment for in situ monitoring by transmission X-ray microscopy (TXM). Evidence has shown that continuous irradiation has an impact on the microstructure and the electrochemical performance of the electrode. To identify the root cause of the radiation damage, a wire-shaped electrode is soaked in an electrolyte in a quartz capillary and monitored using TXM under hard X-ray illumination. The results show that expansion of the carbon-binder matrix by the accumulated X-ray dose is the key factor of radiation damage. For in situ TXM tomography, intermittent X-ray exposure during image capturing can be used to avoid the morphology change caused by radiation damage on the carbon-binder matrix.

    15. 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).

    16. 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.

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

      PubMed

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

      2011-01-07

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

    18. 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.

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

      PubMed Central

      Gumí-Audenis, B.; Carlà, F.; Vitorino, M. V.; Panzarella, A.; Porcar, L.; Boilot, M.; Guerber, S.; Bernard, P.; Rodrigues, M. S.; Sanz, F.; Giannotti, M. I.; Costa, L.

      2015-01-01

      A fast atomic force microscope (AFM) has been developed that can be installed as a sample holder for grazing-incidence X-ray experiments at solid/gas or solid/liquid interfaces. It allows a wide range of possible investigations, including soft and biological samples under physiological conditions (hydrated specimens). The structural information obtained using the X-rays is combined with the data gathered with the AFM (morphology and mechanical properties), providing a unique characterization of the specimen and its dynamics in situ during an experiment. In this work, lipid monolayers and bilayers in air or liquid environment have been investigated by means of AFM, both with imaging and force spectroscopy, and X-ray reflectivity. In addition, this combination allows the radiation damage induced by the beam on the sample to be studied, as has been observed on DOPC and DPPC supported lipid bilayers under physiological conditions. PMID:26524300

    20. Hydrothermal formation of tobermorite studied by in situ X-ray diffraction under autoclave condition.

      PubMed

      Kikuma, Jun; Tsunashima, Masamichi; Ishikawa, Tetsuji; Matsuno, Shin-ya; Ogawa, Akihiro; Matsui, Kunio; Sato, Masugu

      2009-09-01

      Hydrothermal formation of tobermorite from a pre-cured cake has been investigated by transmission X-ray diffraction (XRD) using high-energy X-rays from a synchrotron radiation source in combination with a newly designed autoclave cell. The autoclave cell has a large and thin beryllium window for wide-angle X-ray diffraction; nevertheless, it withstands a steam pressure of more than 1.2 MPa, which enables in situ XRD measurements in a temperature range of 373 to 463 K under a saturated steam pressure. Formation and/or decomposition of several components has been successfully observed during 7.5 h of reaction time. From the intensity changes of the intermediate materials, namely non-crystalline C-S-H and hydroxylellestadite, two pathways for tobermorite formation have been confirmed. Thus, the newly developed autoclave cell can be used for the analyses of reaction mechanisms under specific atmospheres and temperatures.

    1. IN SITU STUDIES OF CORROSION USING X-RAY ABSORPTION NEAR SPECTROSCOPY (XANES)

      SciTech Connect

      ISAACS, H.S.; SCHMUKI, P.; VIRTANEN, S.

      2001-03-25

      Applications of x-ray absorption near-edge spectroscopy (XANES) and the design of cells for in situ corrosion studies are reviewed. Passive films studies require very thin metal or alloy layers be used having a thickness of the order of the films formed because of penetration of the x-ray beam into the metal substrate. The depth of penetration in water also limits the thickness of solutions that can be used because of water reduces the x-ray intensity. Solution thickness must also be limited in studies of conversion layer formation studies because the masking of the Cr in solution. Illustrative examples are taken from the anodic behavior of Al-Cr alloys, the growth of passive films on Fe and stainless steels, and the formation of chromate conversion layers on Al.

    2. 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.

    3. 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.

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

      PubMed

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

      2010-01-01

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

    5. 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.

    6. 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.

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

      SciTech Connect

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

      2016-01-15

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

    8. 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.

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

      PubMed

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

      2009-09-01

      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 A 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.

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

      PubMed

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

      2014-10-01

      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 CoCl2 aqueous solution by X-ray absorption and emission spectroscopy is presented.

    11. 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.

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

      PubMed Central

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

      2015-01-01

      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

    13. 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.

    14. 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.

    15. 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.

    16. A portable molecular beam epitaxy system for in situ x-ray investigations at synchrotron beamlines.

      PubMed

      Slobodskyy, T; Schroth, P; Grigoriev, D; Minkevich, A A; Hu, D Z; Schaadt, D M; Baumbach, T

      2012-10-01

      A portable synchrotron molecular beam epitaxy (MBE) system is designed and applied for in situ investigations. The growth chamber is equipped with all the standard MBE components such as effusion cells with shutters, main shutter, cooling shroud, manipulator, reflection high energy electron diffraction setup, and pressure gauges. The characteristic feature of the system is the beryllium windows which are used for in situ x-ray measurements. An UHV sample transfer case allows in vacuo transfer of samples prepared elsewhere. We describe the system design and demonstrate its performance by investigating the annealing process of buried InGaAs self-organized quantum dots.

    17. A portable molecular beam epitaxy system for in situ x-ray investigations at synchrotron beamlines

      SciTech Connect

      Slobodskyy, T.; Schroth, P.; Grigoriev, D.; Minkevich, A. A.; Baumbach, T.; Hu, D. Z.; Schaadt, D. M.

      2012-10-15

      A portable synchrotron molecular beam epitaxy (MBE) system is designed and applied for in situ investigations. The growth chamber is equipped with all the standard MBE components such as effusion cells with shutters, main shutter, cooling shroud, manipulator, reflection high energy electron diffraction setup, and pressure gauges. The characteristic feature of the system is the beryllium windows which are used for in situ x-ray measurements. An UHV sample transfer case allows in vacuo transfer of samples prepared elsewhere. We describe the system design and demonstrate its performance by investigating the annealing process of buried InGaAs self-organized quantum dots.

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

      NASA Astrophysics Data System (ADS)

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

      2003-01-01

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

    20. Assessment of Ca and P content variation in enamel during an eight-week bleaching protocol using energy dispersive X-ray fluorescence

      NASA Astrophysics Data System (ADS)

      Sorozini, M.; Dos Santos, R. S.; Silva, E. M.; Dos Anjos, M. J.; Perez, C. R.

      2017-05-01

      Tooth bleaching is a simple technique performed with gels based on hydrogen peroxide molecules responsible for removing the tooth structure's pigmentation. The effects of the overuse of these agents on the tooth structure are not well established. Energy dispersive X-ray fluorescence (EDXRF) can be employed to analyze objects of biological origin as bone and tooth. It is very suitable analytical technique to detect demineralization processes in these tissues. The objective of this study was to use x-ray fluorescence to evaluate the effects on mineral content of enamel submitted to eight-week protocols of home bleaching gels (10% carbamide peroxide and 9.5% hydrogen peroxide), as well as bleaching strips. Four enamel fragments obtained from five teeth were subjected to bleaching for 8 weeks: Group 1- artificial saliva; Group 2-10% carbamide peroxide gel, 6 h daily; Group 3-9.5% hydrogen peroxide gel, two 30-minute applications; and Group 4-bleaching strips, twice daily for 30 min. The change in mineral content was assessed weekly using X-ray fluorescence (Artax 200). Differences were basically found in Group 4 for the concentrations of Ca and P after treatment with bleaching strips containing 10% hydrogen peroxide. For the Ca/P ratio, the differences were found in Group 2-15% carbamide peroxide (p < 0.05). X-ray fluorescence proved to be a suitable method for the evaluation of the mineral content, presenting the advantage of being able to evaluate the same area at different stages of the methodology.

    1. 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].

    2. 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.

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

      PubMed

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

      2012-11-16

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

    4. A structural and kinetic study by energy dispersion X-ray diffraction: interaction between 1,4-dihydropyridines and biological membranes

      NASA Astrophysics Data System (ADS)

      Boffi, Federico; Caminiti, Ruggero; Sadun, Claudia; Capuani, Silvia; Giovannelli, Aldo; Congiu Castellano, A.

      1998-04-01

      Application of energy dispersive X-ray diffraction to the study of the main transition phase of the pure and doped DMPC ( Lα-dimyristoylphosphatidylcholine; 1,2-ditetradecanoyl- sn-glycero-3-phosphatidylcholine) bilayers is reported. The aim is to provide an investigative tool to follow the structural variation induced in these systems by temperature and by insertion of doping substances. Hydrophobic compounds such as 1,4-dihydropyridines are used as doping molecules; Nifedipine and Lacidipine show different physical-chemical properties, modifying in a different way the membrane bilayer and its main transition phase. The results show that this technique is useful for studying these kinds of systems (membrane bilayer or biopolymer), giving information on structural variations that occur in a relatively short time.

    5. 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.

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

      NASA Astrophysics Data System (ADS)

      Barbes, Damien; Tabary, Joachim; Paulus, Caroline; Hazemann, Jean-Louis; Verger, Loïck

      2017-03-01

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

    7. The effect of primycin on the intracellular monovalent ion and water contents of rat hepatocytes as revealed by energy dispersive X-ray microanalysis and interference microscopy.

      PubMed

      Horváth, I; Nagy, I; Lustyik, G; Váradi, G

      1983-01-01

      Using energy-dispersive X-ray microanalytic and interference microscopic techniques, the intracellular concentration of the monovalent ions (Na+, K+, Cl+) as well as the intracytoplasmic and intracellular water contents were studied in normal and adrenalectomized rat hepatocytes with and without primycin treatment. Although primycin influenced significantly only the intracellular potassium content of the adrenalectomized group, it exerted a marked influence on the intranuclear water content in both the normal and adrenalectomized rats. The intranuclear water content increased significantly in the primycin-treated animals. The conclusion is drawn that the increased level of hydration of the nuclear substances reflects a 'decondensation' of the chromatin which on the other hand, may represent the basis for the various effects of primycin on the induction of certain hepatic enzymes.

    8. Iron Bacteria in Drinking-Water Distribution Systems: Elemental Analysis of Gallionella Stalks, Using X-Ray Energy-Dispersive Microanalysis

      PubMed Central

      Ridgway, H. F.; Means, E. G.; Olson, B. H.

      1981-01-01

      “Iron” bacteria belonging to the genus Gallionella were observed by scanning electron microscopy in water samples and attached to pipe surfaces in a Southern California drinking-water distribution system. The cells were recognized by their characteristic elongated helical stalks composed of numerous intertwined microfibrils. Many of the stalks were partially coated with insoluble ferric salt deposits. Stalks recovered directly from water samples were analyzed for their elemental composition by using X-ray energy-dispersive microanalysis. Silicon, aluminum, calcium, and iron were the predominant elements present in the stalks. Smaller quantities of the elements phosphorous, sulfur, chlorine, copper, and zinc were also detected. Manganese, though present in measurable quantities in the water supply, was not detected in the stalks, suggesting that this organism is unable to utilize this element as an electron donor. This represents the first such analysis of Gallionella stalks recovered from environmental samples without prior subculturing in artificial laboratory media. Images PMID:16345695

    9. Indium segregation in N-polar InGaN quantum wells evidenced by energy dispersive X-ray spectroscopy and atom probe tomography

      NASA Astrophysics Data System (ADS)

      Bonef, Bastien; Catalano, Massimo; Lund, Cory; Denbaars, Steven P.; Nakamura, Shuji; Mishra, Umesh K.; Kim, Moon J.; Keller, Stacia

      2017-04-01

      Energy dispersive X-ray spectroscopy (EDX) in scanning transmission electron microscopy and atom probe tomography are used to characterize N-polar InGaN/GaN quantum wells at the nanometer scale. Both techniques first evidence the incorporation of indium in the initial stage of the barrier layer growth and its suppression by the introduction of H2 during the growth of the barrier layer. Accumulation of indium at step edges on the vicinal N-polar surface is also observed by both techniques with an accurate quantification obtained by atom probe tomography (APT) and its 3D reconstruction ability. The use of EDX allows for a very accurate interpretation of the APT results complementing the limitations of both techniques.

    10. 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.

    11. 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.

    12. Determination of the geometric blurring of an energy dispersive X-ray diffraction (EDXRD) system and its use in the simulation of experimentally derived diffraction profiles

      NASA Astrophysics Data System (ADS)

      Luggar, R. D.; Horrocks, J. A.; Speller, R. D.; Lacey, R. J.

      1996-02-01

      A computational model has been developed to calculate the geometric blurring distribution of an energy dispersive X-ray diffraction (EDXRD) system. The scattering volume, trapezoid in the horizontal plane, is divided into typically of the order 10 4 elements and the blurring contribution of each element considered in an iterative procedure to build up a distribution for the entire trapezoid. The resultant distribution is asymmetric and peaks at angle below that nominally set. A correction for the focal spot intensity distribution has been included. The blurring distribution has been used as a filter to the Joint Committee on Powder Diffraction Standards (JCPDS) data for several materials to predict the experimentally derived diffraction profiles. A good agreement has been demonstrated between the simulated and measured spectra with a significant improvement on previous models assuming a Gaussian blurring distribution. The model can be used to predict the spectral blurring for any EDXRD system irrespective of the application.

    13. Energy-dispersive x-ray fluorescence spectroscopy and inductively coupled plasma emission spectrometry evaluated for multielement analysis in complex biological matrices.

      PubMed

      Irons, R D; Schenk, E A; Giauque, R D

      1976-12-01

      Energy-dispersive x-ray spectroscopy and inductively coupled plasma emission spectrometry were evaluated as methods for routine multielement analysis of biological material. Standard samples included Standard Reference Materials (National Bureau of Standards), compounded mixtures, and supplements that provided a wide range of elemental concentrations for analysis. Elements included in this study were Zn, Pb, Ni, Mn, Fe, Mg, Cu, Ca, As, Se, Br, Rb, and Sr. Standards were analyzed as unknowns by participating laboratories. The two methods were evaluated for sensitivity, precision, and accuracy, and the results compared to those obtained for atomic absorption spectrometric analysis of identical standard unknowns. Both methods compared favorably and both were determined to be highly reliable for such an application. Advantages and disadvantages of each method are compared and discussed.

    14. A false report of product tampering involving a rodent and soft drink can: light microscopy, image analysis and scanning electron microscopy/energy dispersive X-ray analysis.

      PubMed

      Platek, F; Ranieri, N; Wolnik, K A

      1997-11-01

      The "Pepsi Tamperings" of 1993 resulted in a large number of cases involving foreign objects reportedly found inside canned soft drinks. Although the majority of cases involved medical syringes and metallic objects, one case involved the report of a mouse found inside a can of Caffeine-Free Diet Pepsi. Using light and polarized light microscopy and computer-assisted image analysis, trace evidence and tooth structure from the suspect mouse were matched to scratches and indentions on the suspect can. Scanning electron microscopy and energy dispersive X-ray analysis were used to compare and match particles of gnawed metal from the lid of the suspect can to other particles recovered from the muzzle and stomach of the suspect mouse. The forensic analyses in this case proved the mouse could not have been canned in the soft drink product and refuted the defendant's sworn statements.

    15. An in situ electrochemical soft X-ray spectromicroscopy investigation of Fe galvanically coupled to Au.

      PubMed

      Gianoncelli, A; Kaulich, B; Kiskinova, M; Prasciolu, M; Urzo, B D; Bozzini, B

      2011-06-01

      In this paper we report a pioneering electrochemical study of the galvanic coupling of Au and Fe in neutral aqueous solutions containing sulphate and fluoride ions, carried out by synchrotron-based in situ soft X-ray imaging and X-ray absorption microspectroscopy. The investigation was performed at the TwinMic X-ray Microscopy station at Elettra synchrotron facility combining X-ray imaging with μ-XAS with sub-micron lateral resolution. Using a purposely developed model thin-layer wet cell the morphology and chemical evolution of Fe electrodes in contact with aqueous solutions containing Na2SO4 and NaF have been investigated. The obtained results shed light on fundamental aspects regarding stability of Fe-based metallic bipolar plates in different electrochemical environments, an important issue for durability of polymer-electrolyte fuel cells. Imaging morphological features typical of the relevant electrochemical processes with chemical contrast, yields details on the spatial distribution and speciation of Fe resulting from corrosion of the Fe electrodes in the working fuel cells.

    16. Synchrotron x-ray microdiffraction reveals intrinsic structural features of amyloid deposits in situ.

      PubMed

      Briki, Fatma; Vérine, Jérôme; Doucet, Jean; Bénas, Philippe; Fayard, Barbara; Delpech, Marc; Grateau, Gilles; Riès-Kautt, Madeleine

      2011-07-20

      Amyloidoses are increasingly recognized as a major public health concern in Western countries. All amyloidoses share common morphological, structural, and tinctorial properties. These consist of staining by specific dyes, a fibrillar aspect in electron microscopy and a typical cross-β folding in x-ray diffraction patterns. Most studies that aim at deciphering the amyloid structure rely on fibers generated in vitro or extracted from tissues using protocols that may modify their intrinsic structure. Therefore, the fine details of the in situ architecture of the deposits remain unknown. Here, we present to our knowledge the first data obtained on ex vivo human renal tissue sections using x-ray microdiffraction. The typical cross-β features from fixed paraffin-embedded samples are similar to those formed in vitro or extracted from tissues. Moreover, the fiber orientation maps obtained across glomerular sections reveal an intrinsic texture that is correlated with the glomerulus morphology. These results are of the highest importance to understanding the formation of amyloid deposits and are thus expected to trigger new incentives for tissue investigation. Moreover, the access to intrinsic structural parameters such as fiber size and orientation using synchrotron x-ray microdiffraction, could provide valuable information concerning in situ mechanisms and deposit formation with potential benefits for diagnostic and therapeutic purposes. Copyright © 2011 Biophysical Society. Published by Elsevier Inc. All rights reserved.

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

      DOE PAGES

      Lee, J. H.; Tung, I. C.; Chang, S. -H.; ...

      2016-01-05

      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-raymore » 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. Finally, 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.« less

    18. Performing elemental microanalysis with high accuracy and high precision by scanning electron microscopy/silicon drift detector energy-dispersive X-ray spectrometry (SEM/SDD-EDS).

      PubMed

      Newbury, Dale E; Ritchie, Nicholas W M

      Electron-excited X-ray microanalysis performed in the scanning electron microscope with energy-dispersive X-ray spectrometry (EDS) is a core technique for characterization of the microstructure of materials. The recent advances in EDS performance with the silicon drift detector (SDD) enable accuracy and precision equivalent to that of the high spectral resolution wavelength-dispersive spectrometer employed on the electron probe microanalyzer platform. SDD-EDS throughput, resolution, and stability provide practical operating conditions for measurement of high-count spectra that form the basis for peak fitting procedures that recover the characteristic peak intensities even for elemental combination where severe peak overlaps occur, such PbS, MoS2, BaTiO3, SrWO4, and WSi2. Accurate analyses are also demonstrated for interferences involving large concentration ratios: a major constituent on a minor constituent (Ba at 0.4299 mass fraction on Ti at 0.0180) and a major constituent on a trace constituent (Ba at 0.2194 on Ce at 0.00407; Si at 0.1145 on Ta at 0.0041). Accurate analyses of low atomic number elements, C, N, O, and F, are demonstrated. Measurement of trace constituents with limits of detection below 0.001 mass fraction (1000 ppm) is possible within a practical measurement time of 500 s.

    19. 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.

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

      PubMed

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

      2013-11-05

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

    1. 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.

    2. In situ Raman and X-ray spectroscopies to monitor microbial activities under high hydrostatic pressure.

      PubMed

      Oger, Phil M; Daniel, Isabelle; Picard, Aude

      2010-02-01

      Until recently, monitoring of cells and cellular activities at high hydrostatic pressure (HHP) was mainly limited to ex situ observations. Samples were analyzed prior to and following the depressurization step to evaluate the effect of the pressure treatment. Such ex situ measurements have several drawbacks: (i) it does not allow for kinetic measurements and (ii) the depressurization step often leads to artifactual measurements. Here, we describe recent advances in diamond anvil cell (DAC) technology to adapt it to the monitoring of microbial processes in situ. The modified DAC is asymmetrical, with a single anvil and a diamond window to improve imaging quality and signal collection. Using this novel DAC combined to Raman and X-ray spectroscopy, we monitored the metabolism of glucose by baker's yeast and the reduction of selenite by Agrobacterium tumefaciens in situ under HHP. In situ spectroscopy is also a promising tool to study piezophilic microorganisms.

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

      PubMed

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

      2016-12-01

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

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

      NASA Astrophysics Data System (ADS)

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

      2010-06-01

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

    5. 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.

    6. In situ X-ray diffraction study on the growth kinetics of NiO nanoparticles.

      PubMed

      Meneses, C T; Almeida, J M A; Sasaki, J M

      2010-05-01

      The growth kinetics of NiO nanoparticles have been studied by in situ X-ray diffraction using two detection systems (conventional and imaging plate). NiO nanoparticles were formed by thermal decomposition after heating of an amorphous compound formed by the coprecipitation method. It was found that the detection method using an imaging plate is more efficient than the conventional detection mode for observing changes in the crystallite growth of nanocrystalline materials. Studies have been carried out to investigate the effects of the heating rates on the particles growth. The results suggest that the growth process of the particles is accelerated when the samples are treated at low heating rates. The evolution of particles size and the diffusion coefficient obtained from X-ray powder diffraction patterns are discussed in terms of the thermal conditions for the two types of detection.

    7. Diffraction imaging for in situ characterization of double-crystal X-ray monochromators

      SciTech Connect

      Stoupin, Stanislav; Liu, Zunping; Heald, Steve M.; Brewe, Dale; Meron, Mati

      2015-10-30

      In this paper, imaging of the Bragg-reflected X-ray beam is proposed and validated as an in situ method for characterization of the performance of double-crystal monochromators under the heat load of intense synchrotron radiation. A sequence of images is collected at different angular positions on the reflectivity curve of the second crystal and analyzed. The method provides rapid evaluation of the wavefront of the exit beam, which relates to local misorientation of the crystal planes along the beam footprint on the thermally distorted first crystal. The measured misorientation can be directly compared with the results of finite element analysis. Finally, the imaging method offers an additional insight into the local intrinsic crystal quality over the footprint of the incident X-ray beam.

    8. 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.

    9. 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

      2006-11-07

      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.

    10. 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.

    11. In situ/Operando studies of electrocatalysts using hard X-ray spectroscopy

      DOE PAGES

      Lassalle-Kaiser, Benedikt; Gul, Sheraz; Kern, Jan; ...

      2017-05-02

      This review focuses on the use of X-ray absorption and emission spectroscopy techniques using hard X-rays to study electrocatalysts under in situ/operando conditions. The importance and the versatility of methods in the study of electrodes in contact with the electrolytes are described, when they are being cycled through the catalytic potentials during the progress of the oxygen-evolution, oxygen reduction and hydrogen evolution reactions. The catalytic oxygen evolution reaction is illustrated with examples using three oxides, Co, Ni and Mn, and two sulfides, Mo and Co. These are used as examples for the hydrogen evolution reaction. A bimetallic, bifunctional oxygen evolvingmore » and oxygen reducing Ni/Mn oxide is also presented. The various advantages and constraints in the use of these techniques and the future outlook are discussed.« less

    12. In situ X-ray diffraction studies of (de)lithiation mechanism in silicon nanowire anodes.

      PubMed

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

      2012-06-26

      Silicon is a promising anode material for Li-ion batteries due to its high theoretical specific capacity. From previous work, silicon nanowires (SiNWs) are known to undergo amorphorization during lithiation, and no crystalline Li-Si product has been observed. In this work, we use an X-ray transparent battery cell to perform in situ synchrotron X-ray diffraction on SiNWs in real time during electrochemical cycling. At deep lithiation voltages the known metastable Li(15)Si(4) phase forms, and we show that avoiding the formation of this phase, by modifying the SiNW growth temperature, improves the cycling performance of SiNW anodes. Our results provide insight on the (de)lithiation mechanism and a correlation between phase evolution and electrochemical performance for SiNW anodes.

    13. 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.

    14. Diffraction imaging for in situ characterization of double-crystal X-ray monochromators

      DOE PAGES

      Stoupin, Stanislav; Liu, Zunping; Heald, Steve M.; ...

      2015-10-30

      In this paper, imaging of the Bragg-reflected X-ray beam is proposed and validated as an in situ method for characterization of the performance of double-crystal monochromators under the heat load of intense synchrotron radiation. A sequence of images is collected at different angular positions on the reflectivity curve of the second crystal and analyzed. The method provides rapid evaluation of the wavefront of the exit beam, which relates to local misorientation of the crystal planes along the beam footprint on the thermally distorted first crystal. The measured misorientation can be directly compared with the results of finite element analysis. Finally,more » the imaging method offers an additional insight into the local intrinsic crystal quality over the footprint of the incident X-ray beam.« less

    15. 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.

    16. Automated scanning electron microscopy and x-ray microanalysis for in situ quantification of gadolinium deposits in skin.

      PubMed

      Thakral, Charu; Abraham, Jerrold L

      2007-10-01

      Gadolinium (Gd) has been identified as a possible causative agent of an emerging cutaneous and systemic fibrosing disorder, nephrogenic systemic fibrosis (NSF), which can cause serious disability and even death. To date, there are only two known associations with this disorder--renal insufficiency and Gd enhanced magnetic resonance imaging (MRI). We developed an automated quantitative scanning electron microscopy (SEM) and Energy dispersive x-ray spectroscopy (EDS) method for Gd in tissue of NSF patients. Freshly cut paraffin block surfaces examined using the variable pressure mode under standardized conditions and random search of the tissue area allow in situ detection and semiquantitative morphometric (volumetric) analysis of insoluble higher atomic number features using backscattered electron imaging. We detected Gd ranging from 1 to 2270 cps/mm2 in 57 cutaneous biopsies of NSF. Gd was associated with P, Ca, and usually Na in tissue deposits. Our method reproducibly determines the elemental composition, relative concentration, and spatial distribution of detected features within the tissue. However, we cannot detect features below our spatial resolution, nor concentrations below the detection limit of our SEM/EDS system. The findings confirm transmetallation and release of toxic Gd ions in NSF and allow dose-response analysis at the histologic level.

    17. 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

    18. In situ EXAFS, X-ray diffraction and photoluminescence for high-pressure studies.

      PubMed

      Sapelkin, A V; Bayliss, S C; Russell, D; Clark, S M; Dent, A J

      2000-07-01

      A new facility for simultaneous extended X-ray absorption of fine structure (EXAFS), X-ray diffraction and photoluminescence measurements under high pressures has been developed for use on station 9.3 at the Daresbury Laboratory Synchrotron Radiation Source. This high-pressure facility can be used at any suitable beamline at a synchrotron source. Full remote operation of the rig allows simultaneous collection of optical and structural data while varying the pressure. The set-up is very flexible and can be tailored for a particular experiment, such as time- or temperature-dependent measurements. A new approach to the collection of high-pressure EXAFS data is also presented. The approach significantly shortens the experimental times and allows a dramatic increase in the quality of EXAFS data collected. It also opens up the possibility for EXAFS data collection at any pressure which can be generated using a diamond cell. The high quality of data collected is demonstrated with a GaN case study. Particular attention will be paid to the use of energy-dispersive EXAFS and quick-scanning EXAFS techniques under pressure.

    19. Fast Atomic-Scale Elemental Mapping of Crystalline Materials by STEM Energy-Dispersive X-Ray Spectroscopy Achieved with Thin Specimens [Fast Atomic-Scale Chemical Imaging of Crystalline Materials by STEM Energy-Dispersive X-ray Spectroscopy Achieved with Thin Specimens].

      DOE PAGES

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

      2017-02-23

      Elemental mapping at the atomic-scale by scanning transmission electron microscopy (STEM) using energy-dispersive X-ray spectroscopy (EDS) provides a powerful real-space approach to chemical characterization of crystal structures. However, applications of this powerful technique have been limited by inefficient X-ray emission and collection, which require long acquisition times. Recently, using a lattice-vector translation method, we have shown that rapid atomic-scale elemental mapping using STEM-EDS can be achieved. This method provides atomic-scale elemental maps averaged over crystal areas of ~few 10 nm2with the acquisition time of ~2 s or less. Here we report the details of this method, and, in particular,more » investigate the experimental conditions necessary for achieving it. It shows, that in addition to usual conditions required for atomic-scale imaging, a thin specimen is essential for the technique to be successful. Phenomenological modeling shows that the localization of X-ray signals to atomic columns is a key reason. The effect of specimen thickness on the signal delocalization is studied by multislice image simulations. The results show that the X-ray localization can be achieved by choosing a thin specimen, and the thickness of less than about 22 nm is preferred for SrTiO3in [001] projection for 200 keV electrons.« less

    20. 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.

    1. 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

    2. 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.

    3. Fiber-optic based in situ atomic spectroscopy for manufacturing of x-ray optics

      NASA Astrophysics Data System (ADS)

      Atanasoff, George; Metting, Christopher J.; von Bredow, Hasso

      2016-09-01

      The manufacturing of multilayer Laue (MLL) components for X-ray optics by physical vapor deposition (PVD) requires high precision and accuracy that presents a significant process control challenge. Currently, no process control system provides the accuracy, long-term stability and broad capability for adoption in the manufacturing of X-ray optics. In situ atomic absorption spectroscopy is a promising process control solution, capable of monitoring the deposition rate and chemical composition of extremely thin metal silicide films during deposition and overcoming many limitations of the traditional methods. A novel in situ PVD process control system for the manufacturing of high-precision thin films, based on combined atomic absorption/emission spectrometry in the vicinity of the deposited substrate, is described. By monitoring the atomic concentration in the plasma region independently from the film growth on the deposited substrate, the method allows deposition control of extremely thin films, compound thin films and complex multilayer structures. It provides deposition rate and film composition measurements that can be further utilized for dynamic feedback process control. The system comprises a reconfigurable hardware module located outside the deposition chamber with hollow cathode light sources and a fiber-optic-based frame installed inside the deposition chamber. Recent experimental results from in situ monitoring of Al and Si thin films deposited by DC and RF magnetron sputtering at a variety of plasma conditions and monitoring configurations are presented. The results validate the operation of the system in the deposition of compound thin films and provide a path forward for use in manufacturing of X-Ray optics.

    4. 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.

    5. MAX200x: In-situ X-ray Measurements at High Pressure and High Temperatures.

      NASA Astrophysics Data System (ADS)

      Lathe, C.; Mueller, H. J.; Wehber, M.; Lauterjung, J.; Schilling, F. R.

      2009-05-01

      Twenty years ago geoscientists from all over the world launched in-situ X-ray diffraction experiments under extreme pressure and temperature conditions at synchrotron beamlines. One of the first apparatus was installed at HASYLAB, MAX80, a single-stage multi-anvil system. MAX80 allows in-situ diffraction studies in conjunction with the simultaneous measurement of elastic properties up to 12 GPa and 1600 K. This very successful experiment, unique in Europe, is operated by Helmholtz Centre Potsdam and is used by more than twenty groups from different countries every year. Experiments for both, applied and basic research are conducted, ranging from life-sciences, chemistry, physics, over material sciences to geosciences. Today new materials and the use of high brilliant synchrotron sources allow constructing double-stage multi-anvil systems for X-ray diffraction to reach much higher pressures. The newly designed high-flux hard wiggler (HARWI-II) beamline is an ideal X-ray source for this kind of experiments. As only the uppermost few kilometres of the Earth (less than 0.1% of its radius) are accessible for direct observations (e.g. deep drilling), sophisticated techniques are required to observe and to understand the processes in the deep interior of our planet. In-situ studies are an excellent tool to investigate ongoing geodynamic processes within the laboratory. One of the fundamental regions to study geodynamic processes seems to be the so-called transition zone, the boundary between upper and lower Earth's mantle between 410 and 670 km depth. Mineral reactions, phase transitions, as wheel as fluid rock interaction in this area might have the potential to strongly influence and control the dynamic motions within our whole planet. Around 25 GPa and 2 000 K are required to simulate these processes in the laboratory. The new MAX200x will be an excellent tool for these ambitious experiments.

    6. MEASURING THE PLASTIC RESPONSE IN POLYCRSYTALLINE MATERIALS USING IN-SITU X-RAY DIFFRACTION

      SciTech Connect

      Hawreliak, J; Butterfield, M; El-Dasher, B; McNaney, J; Lorenzana, H

      2008-10-01

      The insight provided by ultra-fast lattice level measurements during high strain rate high pressure experiments is key to understanding kinetic material properties like plasticity. In-situ x-ray diffraction provides a diagnostic technique which can be used to study the governing physical phenomena of plasticity at the relevant time and spatial scale. Here we discuss the recent development of a geometry capable of investigating plasticity in polycrystalline foils. We also present some preliminary data of investigations into shock compressed rolled copper foils.

    7. Confocal X-ray fluorescence spectrometer for in-situ analyses of paintings

      NASA Astrophysics Data System (ADS)

      Trojek, Tomáš; Prokeš, Radek; Šefců, Radka; Bilavčíková, Hana; Čechák, Tomáš

      2017-08-01

      This paper describes the properties of the newly constructed device for confocal X-ray fluorescence analysis that was tested with a sample plate consisting of 19 combinations of two single pigment layers. The preparation of this experimental wooden board with layered systems was based on knowledge of the panel painting techniques of Bohemian collections from the National Gallery in Prague dating back to the 14th and 15th centuries. The design of the confocal setup allows its transport and the in-situ measurement of paintings in depositories or even in exhibition areas. The advantages of our confocal setup with movable collimating optics are also described.

    8. 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.

    9. 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.

    10. In-situ probing of lattice response in shock compressed materials using x-ray diffraction

      SciTech Connect

      Hawreliak, J; Butterfield, M; Davies, H; El-Dasher, B; Higginbotham, A; Kalantar, D; Kimminau, G; McNaney, J; Milathianaki, D; Murphy, W; Nagler, B; Lorenzana, H; Park, N; Remington, B; Thorton, L; Whitcher, T; Wark, J; Lorenzana, H

      2007-07-17

      Lattice level measurements of material response under extreme conditions are required to build a phenomenological understanding of the shock response of solids. We have successfully used laser produced plasma x-ray sources coincident with laser driven shock waves to make in-situ measurements of the lattice response during shock compression for both single crystal and polycrystalline materials. Using a detailed analysis of shocked single crystal iron which has undergone the {alpha} - {var_epsilon} phase transition we can constrain the transition mechanism to be consistent with a compression and shuffle of alternate lattice planes.

    11. IN-SITU PROBING OF LATTICE RESPONSE IN SHOCK COMPRESSED MATERIALS USING X-RAY DIFFRACTION

      SciTech Connect

      Hawreliak, James; Butterfield, Martin; El-Dasher, Bassem; Kalantar, Daniel; McNaney, James; Remington, Bruce; Lorenzana, Hector; Davies, Huw; Park, Nigel; Thorton, Lee; Higginbotham, Andrew; Kimminau, Giles; Murphy, William; Nagler, Bob; Whitcher, Thomas; Wark, Justin; Milathianaki, Despina

      2007-12-12

      Lattice level measurements of material response under extreme conditions are required to build a phenomenological understanding of the shock response of solids. We have successfully used laser produced plasma x-ray sources coincident with laser driven shock waves to make in-situ measurements of the lattice response during shock compression for both single crystal and polycrystalline materials. Using a detailed analysis of shocked single crystal iron which has undergone the {alpha}-{epsilon} phase transition we can constrain the transition mechanism to be consistent with a compression and shuffle of alternate lattice planes.

    12. Fiducial marker application method for position alignment of in situ multimodal x-ray experiments and reconstructions

      SciTech Connect

      Shade, Paul A.; Menasche, David B; Bernier, Joel V.; Kenesei, Peter; Park, Jun-Sang; Suter, Robert; Schuren, Jay C.; Turner, Todd J.

      2016-04-01

      An evolving suite of X-ray characterization methods are presently available to the materials community, providing a great opportunity to gain new insight into material behavior and provide critical validation data for materials models. Two critical and related issues are sample repositioning during an in situ experiment and registration of multiple data sets after the experiment. To address these issues, a method is described which utilizes a focused ion-beam scanning electron microscope equipped with a micromanipulator to apply gold fiducial markers to samples for X-ray measurements. The method is demonstrated with a synchrotron X-ray experiment involving in situ loading of a titanium alloy tensile specimen.

    13. In Situ Industrial Bimetallic Catalyst Characterization using Scanning Transmission Electron Microscopy and X-ray Absorption Spectroscopy at One Atmosphere and Elevated Temperature.

      PubMed

      Prestat, Eric; Kulzick, Matthew A; Dietrich, Paul J; Smith, Mr Matthew; Tien, Mr Eu-Pin; Burke, M Grace; Haigh, Sarah J; Zaluzec, Nestor J

      2017-08-18

      We have developed a new experimental platform for in situ scanning transmission electron microscope (STEM) energy dispersive X-ray spectroscopy (EDS) which allows real time, nanoscale, elemental and structural changes to be studied at elevated temperature (up to 1000 °C) and pressure (up to 1 atm). Here we demonstrate the first application of this approach to understand complex structural changes occurring during reduction of a bimetallic catalyst, PdCu supported on TiO2 , synthesized by wet impregnation. We reveal a heterogeneous evolution of nanoparticle size, distribution, and composition with large differences in reduction behavior for the two metals. We show that the data obtained is complementary to in situ STEM electron energy loss spectroscopy (EELS) and when combined with in situ X-ray absorption spectroscopy (XAS) allows correlation of bulk chemical state with nanoscale changes in elemental distribution during reduction, facilitating new understanding of the catalytic behavior for this important class of materials. © 2017 The Authors. Published by Wiley-VCH Verlag GmbH & Co. KGaA.

    14. 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.

    15. 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.

    16. 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.

    17. Identification of key deformation mechanisms of polyethylene materials via in-situ x-ray scattering

      NASA Astrophysics Data System (ADS)

      Hermel-Davidock, Theresa; Degroot, Willem; Demirors, Mehmet; Landes, Brian; Patel, Rajen; Peltier, Tracy

      2006-03-01

      Changes in the microstructure of ethylene based copolymers can be used to modify and enhance their mechanical performance. In this study, the effects of comonomer content, molecular weight, and molecular weight distribution on the mechanical performance of select polyethylene polymers were examined. Two key performance parameters for commercial polymer materials, especially in the area of blown film applications, are tear resistance and puncture resistance. However, polyethylene films exhibiting very different Dart and Elmendorf tear values cannot be differentiated by standard tensile test methods even though they exhibit very similar morphology. Alternative methods to link morphology and mechanical response need to be found. Wide-angle and small-angle x-ray scattering was collected during in-situ tensile testing to understand how compositional and structural differences affect the mechanical response of semicrystalline polyethylene polymers. Microstructural changes observed during the in-situ deformation process are correlated to Elmendorf tear and Dart impact performance for both intrinsic and blown film samples.

    18. Identification of key deformation mechanisms of polyethylene materials via in-situ x-ray scattering

      NASA Astrophysics Data System (ADS)

      Hermel-Davidock, Theresa; Landes, Brian; Demirors, Mehmet

      2008-03-01

      Changes in the microstructure of ethylene based copolymers can be used to modify and enhance their mechanical performance. In this study, the effects of comonomer content, molecular weight, and molecular weight distribution on the mechanical performance of select polyethylene polymers were examined. Two key performance parameters for commercial polymer materials, especially in the area of blown film applications, are tear resistance and puncture resistance. However, polyethylene films which exhibit very similar morphology often exhibit very different Dart and Elmendorf tear values which cannot be differentiated by standard tensile test methods. Alternative methods to link morphology and mechanical response need to be found. Wide-angle and small-angle x-ray scattering was collected during in-situ tensile testing to understand how compositional and structural differences affect the mechanical response of semicrystalline polyethylene polymers. Microstructural changes observed during the in-situ deformation process are correlated to Elmendorf tear performance for both intrinsic and blown film samples.

    19. Orthoclase surface structure dissolution measured in situ by x-ray reflectivity and atomic force microscopy.

      SciTech Connect

      Sturchio, N. C.; Fenter, P.; Cheng, L.; Teng, H.

      2000-11-28

      Orthoclase (001) surface topography and interface structure were measured during dissolution by using in situ atomic force microscopy (AFM) and synchrotrons X-ray reflectivity at pH 1.1-12.9 and T = 25-84 C. Terrace roughening at low pH and step motion at high pH were the main phenomena observed, and dissolution rates were measured precisely. Contrasting dissolution mechanisms are inferred for low- and high-pH conditions. These observations clarify differences in alkali feldspar dissolution mechanisms as a function of pH, demonstrate a new in situ method for measuring face-specific dissolution rates on single crystals, and improve the fundamental basis for understanding alkali feldspar weathering processes.

    20. 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

    1. 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

    2. X-Ray Diffraction and Fluorescence Measurements for In-situ Planetary Instruments

      NASA Astrophysics Data System (ADS)

      Hansford, G.; Hill, K. S.; Vernon, D.; Ambrosi, R. M.; Bridges, J.; Hutchinson, I.

      2010-12-01

      The X-Ray Diffraction (XRD) instruments are core components of the forthcoming NASA Mars Science Laboratory (MSL) and ESA/NASA EXOMARS missions and will provide the first demonstrations of an XRF/XRD instrument’s capabilities in-situ on an extraterrestrial planetary surface. The University of Leicester team is part of the Italy-UK collaboration that is responsible for building the ExoMars X-Ray Diffraction instrument, Mars XRD. The ExoMars X-ray diffraction instrument incorporates an 55-Fe radioisotope source and three fixed-position CCDs to simultaneously acquire an X-Ray fluorescence spectrum and a diffraction pattern providing a measurement of both elemental and mineralogical composition [1]. The CCDs cover an angular range from 6 to 65-deg enabling the analysis of silicates, from clays, or other phyllosilicates characterised by varying d-spacings, to oxides, and carbonates or evaporites. The identification of hydrous minerals may help identify past Martian hydrothermal systems capable of preserving traces of life. Here we present some initial findings from XRF and XRD tests carried out at the University of Leicester using an 55-Fe source and X-ray sensitive CCD [1]. The XRD/XRD test system consists of a single CCD on a motorised arm, an 55-Fe X-ray source, source collimator and a sample table which approximately replicate the reflection geometry of the XRD instrument. It was used to test geological reference standard materials and Martian analogues. Incidence angle and CCD angles on both the diffraction and fluorescence results were evaluated. A key area of interest is the effect of sample roughness on the XRD/XRF results. We present results from testing pressed powder pellet samples of varying surface roughness, and a comparison with model results [2]. So far we have found that increased roughness causes a reduced intensity at lower take-off angles. Several methods for measuring surface roughness of the samples have been used including an Alicona Infinite

    3. 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.

    4. 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

    5. 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.

    6. 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.

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

      PubMed

      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 CuIn(x)Ga(1-x)Se2 (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. 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.

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

      PubMed

      Bae, Sungchul; Kanematsu, Manabu; Hernández-Cruz, Daniel; Moon, Juhyuk; Kilcoyne, David; Monteiro, Paulo J M

      2016-12-01

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

    10. 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

    11. Corrosion of an alloy studied in situ with synchrotron x-ray diffraction

      NASA Astrophysics Data System (ADS)

      Renner, Frank; Lee, Tien-Lin; Kolb, Dieter M.; Stierle, Andreas; Dosch, Helmut; Zegenhagen, Jorg

      2004-03-01

      Corrosion processes are mostly electrochemical in nature. For the basic understanding of corrosion and similar technical processes, in-situ structural methods capable of atomic resolution, such as scanning probe microscopy or hard X-ray techniques are necessary. We used in-situ X-ray diffraction and in addition ex-situ AFM, to study Cu_3Au(111) single crystal surfaces in 0.1M H_2SO4 electrolyte as a function of electrode potential in the sub-critical regime. This binary metal alloys serves as model systems for more complicated technically utilized metal alloys. During the initial electrochemical corrosion, Cu atoms are dissolved and a passivating layer is formed. The experiments show the formation of an epitaxial and highly strained ultra-thin Cu_xAu_1-x(111) phase on the surface at a potential where Cu dissolution starts. At higher potentials, thicker epitaxial Au islands are growing on the surface. AFM images reveal a surface, densely packed with Au islands of a homogeneous size-distribution. On a prolonged timescale, a percolating, porous morphology of the surface evolves by ripening, even at an electrode potential well below the critical potential.

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

      SciTech Connect

      Kroner, Anna B. Gilbert, Martin; Duller, Graham; Cahill, Leo; Leicester, Peter; Woolliscroft, Richard; Shotton, Elizabeth J.; Mohammed, Khaled M. H.

      2016-07-27

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

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

      PubMed Central

      Bae, Sungchul; Kanematsu, Manabu; Hernández-Cruz, Daniel; Moon, Juhyuk; Kilcoyne, David; Monteiro, Paulo J. M.

      2016-01-01

      The understanding and control of early hydration of tricalcium silicate (C3S) is of great importance to cement science and concrete technology. However, traditional characterization methods are incapable of providing morphological and spectroscopic information about in situ hydration at the nanoscale. Using soft X-ray spectromicroscopy, we report the changes in morphology and molecular structure of C3S at an early stage of hydration. In situ C3S hydration in a wet cell, beginning with induction (~1 h) and acceleration (~4 h) periods of up to ~8 h, was studied and compared with ex situ measurements in the deceleration period after 15 h of curing. Analysis of the near-edge X-ray absorption fine structure showed that the Ca binding energy and energy splitting of C3S changed rapidly in the early age of hydration and exhibited values similar to calcium silicate hydrate (C–S–H). The formation of C–S–H nanoseeds in the C3S solution and the development of a fibrillar C–S–H morphology on the C3S surface were visualized. Following this, silicate polymerization accompanied by C–S–H precipitation produced chemical shifts in the peaks of the main Si K edge and in multiple scattering. However, the silicate polymerization process did not significantly affect the Ca binding energy of C–S–H. PMID:28774096

    14. Forensic analysis of soil and sediment traces by scanning electron microscopy and energy-dispersive X-ray analysis: an experimental investigation.

      PubMed

      Pye, Kenneth; Croft, Debra

      2007-01-05

      This paper reports the results of a series of experiments carried out to determine the precision of soil trace comparisons based on elemental peak height ratios determined by energy-dispersive X-ray analysis (EDXRA) in a variable pressure scanning electron microscope (VP-SEM). Experiments were conducted on 'bulk' soil aggregates, ground powders prepared from the <150 microm soil fractions and on smears of both the bulk soil and <150 microm material placed on cotton cloth. X-ray count data were obtained using area scans and spot analyses at different magnifications. The effects on elemental peak height ratios of varying the SEM chamber pressure, beam spot size, emission current and accelerating voltage were also examined. The peak height ratios for oxygen, silicon, aluminium, potassium, calcium and iron were found to show little variation as a function of chamber pressure, spot size and emission current over the ranges examined, but a strong dependency on accelerating voltage was observed. Within-sample variation in results, expressed by the percentage coefficient of variation, was found to be lowest for area scan analyses of the ground <150 microm fractions and greatest for the spot analyses of the bulk soil aggregates and the <150 microm fractions. We conclude that comparison of elemental peak height ratios determined by EDXRA can be a useful tool for rapid screening of soil samples, especially when combined with investigation of other attributes of the soil traces such as colour, fabric and the composition, shapes and surface textures of individual particles or aggregates within the soil traces. If sufficient material is available and can be readily separated without contamination or loss, higher resolution and more precise elemental data should be obtained by methods such as inductively coupled plasma atomic-emission spectrometry (ICP-AES) or mass-spectrometry (ICP-MS).

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

      PubMed

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

      2012-06-04

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

    16. Determination of inorganic nutrients in wheat flour by laser-induced breakdown spectroscopy and energy dispersive X-ray fluorescence spectrometry

      NASA Astrophysics Data System (ADS)

      Peruchi, Lidiane Cristina; Nunes, Lidiane Cristina; de Carvalho, Gabriel Gustinelli Arantes; Guerra, Marcelo Braga Bueno; de Almeida, Eduardo; Rufini, Iolanda Aparecida; Santos, Dário; Krug, Francisco José

      2014-10-01

      Laser-induced breakdown spectroscopy (LIBS) and energy dispersive X-ray fluorescence spectrometry (EDXRF) were evaluated for the determination of P, K, Ca, Mg, S, Fe, Cu, Mn and Zn in pressed pellets of wheat flours. EDXRF and LIBS calibration models were built with analytes mass fractions determined by inductively coupled plasma optical emission spectrometry after microwave-assisted acid digestion in a set of 25 wheat flour laboratory samples. Test samples consisted of pressed pellets prepared from wheat flour mixed with 30% mm- 1 cellulose binder. Experiments were carried out with a LIBS setup consisted of a Q-switched Nd:YAG laser and a spectrometer with Echelle optics and ICCD, and a benchtop EDXRF system fitted with a Rh target X-ray tube and a Si(Li) semiconductor detector. The correlation coefficients from the linear calibration models of P, K, Ca, Mg, S, Fe, Mn and Zn determined by LIBS and/or EDXRF varied from 0.9705 for Zn to 0.9990 for Mg by LIBS, and from 0.9306 for S to 0.9974 for K by EDXRF. The coefficients of variation of measurements varied from 1.2 to 20% for LIBS, and from 0.3 to 24% for EDXRF. The predictive capabilities based on RMSEP (root mean square error of prediction) values were appropriate for the determination of P, Ca, Mg, Fe, Mn and Zn by LIBS, and for P, K, S, Ca, Fe, and Zn by EDXRF. In general, results from the analysis of NIST SRM 1567a Wheat flour by LIBS and EDXRF were in agreement with their certified mass fractions.

    17. Characterization of individual submicrometer aerosol particles collected in Incheon, Korea, by quantitative transmission electron microscopy energy-dispersive X-ray spectrometry

      NASA Astrophysics Data System (ADS)

      Geng, Hong; Kang, Sujin; Jung, Hae-Jin; ChoëL, Marie; Kim, Hyekyeong; Ro, Chul-Un

      2010-08-01

      For the last decade the Monte Carlo calculation method has been proven to be an excellent tool for accurately simulating electron-solid interactions in atmospheric individual particles of micrometer size. Although it was designed for application to scanning electron microscopy, in the present study it is demonstrated that the Monte Carlo calculation can also be applied in a quantitative single particle analysis using transmission electron microscopy (TEM) with an ultrathin window energy-dispersive X-ray (EDX) spectrometer with a high accelerating voltage (200 kV). By utilizing an iterative reverse Monte Carlo simulation combined with successive approximation, atomic elemental concentrations (including low-Z elements) of submicrometer standard particles were determined with high accuracy for electron beam refractory particles such as NaCl, KCl, SiO2, Fe2O3, Na2SO4, K2SO4, CaCO3, and CaSO4. On the basis of quantitative X-ray analysis together with morphological information from TEM images, overall 1638 submicrometer individual particles from 10 sets of aerosol samples collected in Incheon, Korea, were identified. The most frequently encountered particle types are carbonaceous and (NH4)2SO4/NH4HSO4-containing particles, followed by mineral (e.g., aluminosilicate, SiO2, CaCO3), sea salt, K-rich (e.g., K2SO4 and KCl), Fe-rich, fly ash, and transition or heavy-metal-containing (e.g., ZnSO4, ZnCl2, PbSO4) particles. The relative abundances of the submicrometer particle types vary among samples collected in different seasons and also depend on different air mass transport routes. This study demonstrates that the quantitative TEM-EDX individual particle analysis is a useful and reliable technique in characterizing urban submicrometer aerosol particles.

    18. Migration of iron and manganese into CCA-treated wood in soil contact and the resulting error in leaching results when using energy dispersive x-ray fluorescence spectrometers

      Treesearch

      Tor P. Schultz; Darrel D. Nicholas; Stan Lebow

      2003-01-01

      In a laboratory leaching study, we found that chromated copper arsenate (CCA) treated wood, which had been exposed to one of five soils examined, unexpectedly appeared to gain significant Cr (47%) when measured with an energy-dispersive x-ray fluorescence instrument (American Wood-Preservers' Association (AWPA) Method A9-01 2001). Analysis of some of the leached...

    19. Note: Experiments in hard x-ray chemistry: In situ production of molecular hydrogen and x-ray induced combustion

      SciTech Connect

      Pravica, Michael; Bai Ligang; Liu Yu; Galley, Martin; Robinson, John; Park, Changyong; Hatchett, David

      2012-03-15

      We have successfully loaded H{sub 2} into a diamond anvil cell at high pressure using the synchrotron x-ray induced decomposition of NH{sub 3}BH{sub 3}. In a second set of studies, radiation-assisted release of O{sub 2} from KCLO{sub 3}, H{sub 2} release from NH{sub 3}BH{sub 3}, and reaction of these gases in a mixture of the reactants to form liquid water using x-rays at ambient conditions was observed. Similar observations were made using a KCLO{sub 3} and NaBH{sub 4} mixture. Depending on reaction conditions, an explosive or far slower reaction producing water was observed.

    20. 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.

    1. Chemical and morphological study of gunshot residue persisting on the shooter by means of scanning electron microscopy and energy dispersive X-ray spectrometry.

      PubMed

      Brożek-Mucha, Zuzanna

      2011-12-01

      Persistence of gunshot residue (GSR) simultaneously collected from hands, face and hair, and clothing of the shooting person was examined. Samples were collected from five shooters in nine time intervals after a single shoot with a Luger 9 mm pistol, in the range of 0-4 h and examined with scanning electron microscopy and energy dispersive X-ray spectrometry. Numbers of particles, frequencies of occurrence of certain compositions of particles, and their sizes in function of the time intervals were inspected. The greatest numbers of particles were observed in samples collected from hands right after shooting, but they decrease quickly with time. In samples collected from the face smaller initial numbers of particles were found, but they lasted at a similar level longer. The estimated half-life times of particles were less than 1 h for samples taken from the hands, over 1 h for clothing and about 2-3 h for the face. In samples collected at longer intervals after shooting, there were particles present of small sizes and irregular shapes. The results demonstrate that including evidence collected from the suspect's face and hair may increase the probability of detection of GSR in cases when the suspect has not been apprehended immediately after the investigated incident.

    2. Correlative Energy-Dispersive X-Ray Spectroscopic Tomography and Atom Probe Tomography of the Phase Separation in an Alnico 8 Alloy

      SciTech Connect

      Guo, Wei; Sneed, Brian T.; Zhou, Lin; Tang, Wei; Kramer, Matthew J.; Cullen, David A.; Poplawsky, Jonathan D.

      2016-12-21

      Alnico alloys have long been used as strong permanent magnets because of their ferromagnetism and high coercivity. Understanding their structural details allows for better prediction of the resulting magnetic properties. However, quantitative three-dimensional characterization of the phase separation in these alloys is still challenged by the spatial quantification of nanoscale phases. Herein, we apply a dual tomography approach, where correlative scanning transmission electron microscopy (STEM) energy-dispersive X-ray spectroscopic (EDS) tomography and atom probe tomography (APT) are used to investigate the initial phase separation process of an alnico 8 alloy upon non-magnetic annealing. STEM-EDS tomography provides information on the morphology and volume fractions of Fe–Co-rich and Νi–Al-rich phases after spinodal decomposition in addition to quantitative information of the composition of a nanoscale volume. Subsequent analysis of a portion of the same specimen by APT offers quantitative chemical information of each phase at the sub-nanometer scale. Furthermore, APT reveals small, 2–4 nm Fe-rich α1 phases that are nucleated in the Ni-rich α2 matrix. From this information, we show that phase separation of the alnico 8 alloy consists of both spinodal decomposition and nucleation and growth processes. Lastly, we discuss the complementary benefits and challenges associated with correlative STEM-EDS and APT.

    3. Measurement Error in Atomic-Scale Scanning Transmission Electron Microscopy-Energy-Dispersive X-Ray Spectroscopy (STEM-EDS) Mapping of a Model Oxide Interface.

      PubMed

      Spurgeon, Steven R; Du, Yingge; Chambers, Scott A

      2017-06-01

      With the development of affordable aberration correctors, analytical scanning transmission electron microscopy (STEM) studies of complex interfaces can now be conducted at high spatial resolution at laboratories worldwide. Energy-dispersive X-ray spectroscopy (EDS) in particular has grown in popularity, as it enables elemental mapping over a wide range of ionization energies. However, the interpretation of atomically resolved data is greatly complicated by beam-sample interactions that are often overlooked by novice users. Here we describe the practical factors-namely, sample thickness and the choice of ionization edge-that affect the quantification of a model perovskite oxide interface. Our measurements of the same sample, in regions of different thickness, indicate that interface profiles can vary by as much as 2-5 unit cells, depending on the spectral feature. This finding is supported by multislice simulations, which reveal that on-axis maps of even perfectly abrupt interfaces exhibit significant delocalization. Quantification of thicker samples is further complicated by channeling to heavier sites across the interface, as well as an increased signal background. We show that extreme care must be taken to prepare samples to minimize channeling effects and argue that it may not be possible to extract atomically resolved information from many chemical maps.

    4. Role of trace elements (Zn, Sr, Fe) in bone development: energy dispersive X-ray fluorescence study of rat bone and tooth tissue.

      PubMed

      Maciejewska, Karina; Drzazga, Zofia; Kaszuba, Michał

      2014-01-01

      Osteoporosis is one of the most common debilitating disease around the world and it is more and more established among young people. There are well known recommendations for nutrition of newborns and children concerning adequate calcium and vitamin D intake in order to maintain proper bone density. Nevertheless, important role in structure and function of a healthy bone tissue is played by an integration between all constituents including elements other than Ca, like trace elements, which control vital processes in bone tissue. It is important from scientific point of view as well as prevention of bone diseases, to monitor the mineralization process considering changes of the concentration of minerals during first stage of bone formation. This work presents studies of trace element (zinc, strontium, and iron) concentration in bones and teeth of Wistar rats at the age of 7, 14, and 28 days. Energy dispersive X-ray fluorescence (EDXRF) was used to examine mandibles, skulls, femurs, tibiae, and incisors. The quantitative analysis was performed using fundamental parameters method (FP). Zn and Sr concentrations were highest for the youngest individuals and decreased with age of rats, while Fe content was stable in bone matrix for most studied bones. Our results reveal the necessity of monitoring concentration of not only major, but also minor elements, because the trace elements play special role in the first period of bone development.

    5. Test method for the presence or absence of Pb in electrical components using energy-dispersive micro X-ray fluorescence.

      PubMed

      Araki, Wakako; Mizoroki, Kaoru; Oki, Mitsuhiro; Takenaka, Miyuki

      2005-07-01

      The micro-EDXRF (energy dispersive X-ray fluorescence) method was applied to the screening of Pb in micrometer-area samples, such as a Cu contact in electrical components that had been coated by Pb-free Sn-Ag-Cu solder. The reliability of the screening method was evaluated by a comparison with a scanning electron microscope (SEM) observation and a precious chemical analysis method of inductively coupled plasma mass spectrometry (ICP-MS). Some factors that affect the testing reliability, such as the thickness of the solder, the segregation of Pb and Ag, etc. were found by SEM observations. By adjusting some calculation parameters, screening of the micrometer area (0.1 mm) was performed using the fundamental parameter (FP) method for a thin film in conjunction with micro-EDXRF. The measurement error ranged by 25% for the thin film-FP method. The resulted detection limit was 0.04 wt% for Pb, depending on the solder thickness. This method can be successively applied for quality control to check the purity of a Pb-free Sn-Ag-Cu solder coating in electrical components.

    6. Post-mortem interval estimation of human skeletal remains by micro-computed tomography, mid-infrared microscopic imaging and energy dispersive X-ray mapping

      PubMed Central

      Hatzer-Grubwieser, P.; Bauer, C.; Parson, W.; Unterberger, S. H.; Kuhn, V.; Pemberger, N.; Pallua, Anton K.; Recheis, W.; Lackner, R.; Stalder, R.; Pallua, J. D.

      2015-01-01

      In this study different state-of-the-art visualization methods such as micro-computed tomography (micro-CT), mid-infrared (MIR) microscopic imaging and energy dispersive X-ray (EDS) mapping were evaluated to study human skeletal remains for the determination of the post-mortem interval (PMI). PMI specific features were identified and visualized by overlaying molecular imaging data and morphological tissue structures generated by radiological techniques and microscopic images gained from confocal microscopy (Infinite Focus (IFM)). In this way, a more distinct picture concerning processes during the PMI as well as a more realistic approximation of the PMI were achieved. It could be demonstrated that the gained result in combination with multivariate data analysis can be used to predict the Ca/C ratio and bone volume (BV) over total volume (TV) for PMI estimation. Statistical limitation of this study is the small sample size, and future work will be based on more specimens to develop a screening tool for PMI based on the outcome of this multidimensional approach. PMID:25878731

    7. Development of a microanalytical energy dispersive X-ray fluorescence method for compositional characterization of (U, Pu)O2 samples

      NASA Astrophysics Data System (ADS)

      Dhara, Sangita; Sanjay Kumar, S.; Jayachandran, Kavitha; Kamat, J. V.; Kumar, Ashok; Radhakrishna, J.; Misra, N. L.

      2017-05-01

      Elemental compositional characterization of (U, Pu)O2 samples is an important aspect for quality control of nuclear fuels. A microanalytical Energy Dispersive X-ray Fluorescence (EDXRF) method has been developed for the determination of plutonium and uranium. The method involves sample dissolution, addition of internal standard(s) into the sample solution, taking about 50 μg of the sample on absorbent sheets, drying and sealing the specimens in such a manner that no loose radioactive particle comes out, during the analysis. Such approach does not require putting the instrument inside the glove box. These specimens were presented for the EDXRF measurements using Rh Kα as the excitation source. The amount of uranium and plutonium in samples were calculated using two different internal standards Ga and Y. The Pu weight percent (wt%) was calculated with respect to (U + Pu) in the samples. The results obtained were in good agreement with the biamperometric analysis results of the samples. The average precision observed was within 1% (1σ, n = 4) and the deviation of the EDXRF determined values from expected values was within 2%. The detection limits obtained for Pu and U were 4 μg.

    8. A case of hut lung: scanning electron microscopy with energy dispersive x-ray spectroscopy analysis of a domestically acquired form of pneumoconiosis.

      PubMed

      Mukhopadhyay, Sanjay; Gujral, Manmeet; Abraham, Jerrold L; Scalzetti, Ernest M; Iannuzzi, Michael C

      2013-07-01

      Hut lung is a pneumoconiosis caused by exposure to smoke derived from biomass fuels used for cooking in poorly ventilated huts. We report, to our knowledge, the first analysis of the dust deposited in the lungs in hut lung by scanning electron microscopy with energy dispersive x-ray spectroscopy (SEM/EDS). A Bhutanese woman presented with shortness of breath and an abnormal chest radiograph. Chest CT scan showed innumerable tiny bilateral upper lobe centrilobular nodules. Transbronchial biopsy revealed mild interstitial fibrosis with heavy interstitial deposition of black dust. SEM/EDS showed that the dust was carbonaceous, with smaller yet substantial numbers of silica and silicate particles. Additional history revealed use of a wood/coal-fueled stove in a small, poorly ventilated hut for 45 years. The possibility of hut lung should be considered in women from countries where use of biomass-fueled stoves for cooking is common. Our findings support the classification of this condition as a mixed-dust pneumoconiosis.

    9. Analysis of trace elements during different developmental stages of somatic embryogenesis in Plantago ovata Forssk using energy dispersive X-ray fluorescence.

      PubMed

      Saha, Priyanka; Raychaudhuri, Sarmistha Sen; Sudarshan, Mathummal; Chakraborty, Anindita

      2010-06-01

      Energy dispersive X-ray fluorescence (ED-XRF) technique has been used for the determination of trace element profile during different developmental stages of somatic embryogenic callus of an economically important medicinal plant, Plantago ovata Forssk. Somatic embryogenesis is a plant tissue culture-based technique, which is used for plant regeneration and crop improvement. In the present investigation, elemental content was analysed using ED-XRF technique during different developmental stages and also determine the effect of additives--casein hydrolysate and coconut water on the trace elemental profile of embryogenic callus tissue of P. ovata. Subsequent experiments showed significant alteration in the concentration of K, Ca, Mn, Fe, Zn, Cu, Br, and Sr in both the embryogenic and non-embryogenic callus. Higher K, Ca, Fe, Cu, and Zn accumulation was in embryogenic tissue stage compared to other stages, suggesting these elements are crucial for successful embryogenesis. The results suggest that this information could be useful for formulating a media for in vitro embryo induction of P. ovata.

    10. Energy-dispersive X-ray spectrometry combined with directly suspended droplet microextraction for determination of dissolved silicate in surface water via silicomolybdenum blue complex.

      PubMed

      Pytlakowska, Katarzyna

      2014-10-01

      Energy-dispersive X-ray fluorescence spectrometry (EDXRF) is a well-established analytical technique successfully applied with good precision and accuracy to determination of many elements. However, in the case of elements of low atomic number, such as silicon, direct determination is hampered due to low fluorescence yield and relatively low energy easily absorbed by sample matrix. An indirect method for determining surface water silicate is thus proposed. The method is based on silicate determination via molybdenum present in silicomolybdenum blue complex. Determination follows directly suspended droplet microextraction. Optimum conditions for both microextraction and EDXRF measurement were studied. A good ratio of silicon to molybdenum (1-41) and a sensitive Kα line of molybdenum make it possible to determine low concentrations of silicate. Under optimized conditions, good linearity, up to 3 μg mL(-1) (r=0.9990), and good detection limit (6 ng mL(-1)) were achieved. The total RSD for the EDXRF determination of silicate following DSDME was 6.7%. Taking into account all steps preceding the determination and the uncertainty of XRF measurements, the proposed method can be recognized as precise. The enrichment factor was 140. The developed method was used to determine dissolved silicate content in surface water samples. The accuracy and repeatability of the proposed procedure were checked by standard addition method and compared to the results obtained using ICP-OES technique. The recovery (92.2-96%) was satisfactory and indicates usefulness of the developed procedure.

    11. Correlative Energy-Dispersive X-Ray Spectroscopic Tomography and Atom Probe Tomography of the Phase Separation in an Alnico 8 Alloy

      DOE PAGES

      Guo, Wei; Sneed, Brian T.; Zhou, Lin; ...

      2016-12-21

      Alnico alloys have long been used as strong permanent magnets because of their ferromagnetism and high coercivity. Understanding their structural details allows for better prediction of the resulting magnetic properties. However, quantitative three-dimensional characterization of the phase separation in these alloys is still challenged by the spatial quantification of nanoscale phases. Herein, we apply a dual tomography approach, where correlative scanning transmission electron microscopy (STEM) energy-dispersive X-ray spectroscopic (EDS) tomography and atom probe tomography (APT) are used to investigate the initial phase separation process of an alnico 8 alloy upon non-magnetic annealing. STEM-EDS tomography provides information on the morphology andmore » volume fractions of Fe–Co-rich and Νi–Al-rich phases after spinodal decomposition in addition to quantitative information of the composition of a nanoscale volume. Subsequent analysis of a portion of the same specimen by APT offers quantitative chemical information of each phase at the sub-nanometer scale. Furthermore, APT reveals small, 2–4 nm Fe-rich α1 phases that are nucleated in the Ni-rich α2 matrix. From this information, we show that phase separation of the alnico 8 alloy consists of both spinodal decomposition and nucleation and growth processes. Lastly, we discuss the complementary benefits and challenges associated with correlative STEM-EDS and APT.« less

    12. Chemical Differentiation of Osseous and Nonosseous Materials Using Scanning Electron Microscopy-Energy-Dispersive X-Ray Spectrometry and Multivariate Statistical Analysis.

      PubMed

      Meizel-Lambert, Cayli J; Schultz, John J; Sigman, Michael E

      2015-11-01

      Identification of osseous materials is generally established on gross anatomical features. However, highly fragmented or taphonomically altered materials may be problematic and may require chemical analysis. This research was designed to assess the use of scanning electron microscopy-energy-dispersive X-ray spectrometry (SEM/EDX), elemental analysis, and multivariate statistical analysis (principal component analysis) for discrimination of osseous and nonosseous materials of similar chemical composition. Sixty samples consisting of osseous (human and nonhuman bone and dental) and non-osseous samples were assessed. After outliers were removed a high overall correct classification of 97.97% was achieved, with 99.86% correct classification for osseous materials. In addition, a blind study was conducted using 20 samples to assess the applicability for using this method to classify unknown materials. All of the blind study samples were correctly classified resulting in 100% correct classification, further demonstrating the efficiency of SEM/EDX and statistical analysis for differentiation of osseous and nonosseous materials. © 2015 American Academy of Forensic Sciences.

    13. Scanning electron microscopy coupled with energy-dispersive X-ray spectrometry for quick detection of sulfur-oxidizing bacteria in environmental water samples

      NASA Astrophysics Data System (ADS)

      Sun, Chengjun; Jiang, Fenghua; Gao, Wei; Li, Xiaoyun; Yu, Yanzhen; Yin, Xiaofei; Wang, Yong; Ding, Haibing

      2017-01-01

      Detection of sulfur-oxidizing bacteria has largely been dependent on targeted gene sequencing technology or traditional cell cultivation, which usually takes from days to months to carry out. This clearly does not meet the requirements of analysis for time-sensitive samples and/or complicated environmental samples. Since energy-dispersive X-ray spectrometry (EDS) can be used to simultaneously detect multiple elements in a sample, including sulfur, with minimal sample treatment, this technology was applied to detect sulfur-oxidizing bacteria using their high sulfur content within the cell. This article describes the application of scanning electron microscopy imaging coupled with EDS mapping for quick detection of sulfur oxidizers in contaminated environmental water samples, with minimal sample handling. Scanning electron microscopy imaging revealed the existence of dense granules within the bacterial cells, while EDS identified large amounts of sulfur within them. EDS mapping localized the sulfur to these granules. Subsequent 16S rRNA gene sequencing showed that the bacteria detected in our samples belonged to the genus Chromatium, which are sulfur oxidizers. Thus, EDS mapping made it possible to identify sulfur oxidizers in environmental samples based on localized sulfur within their cells, within a short time (within 24 h of sampling). This technique has wide ranging applications for detection of sulfur bacteria in environmental water samples.

    14. Quick Detection of Sulfur Bacteria in Environmental Water Sample with SEM(scanning electron microscopy) coupled with Energy Dispersive X-ray Spectrometry

      NASA Astrophysics Data System (ADS)

      Sun, C.; Ding, H.; Wang, Y.; Jiang, F.; Li, X.; Gao, W.; Yin, X.

      2015-12-01

      Sulfur-oxidizing bacteria play important roles in global sulfur cycle. Sulfur bacteria detection has been largely dependent on targeted gene sequencing technology or traditional cell cultivation which usually takes from days to months to finish. This cannot meet the requirements of some time-sensitive samples and/or complicated environmental samples. Since Energy-Dispersive X-ray Spectrometry (EDS) can be used to simultaneously detect multiple elements including sulfur in a sample with minimal sample treatment, the technology was applied to detect sulfur bacteria through the high sulfur content in the bacteria cell. We report the application of SEM (scanning electron microscopy) imaging coupled with EDS mapping for direct and quick detection of sulfur oxidizer in contaminated environmental water samples. The presence of sulfur bacteria can be confirmed within 24 hours after sampling. Subsequent 16S RNA gene sequencing results found the bacteria detected had over 99% similarity to Chromatium Okenii, confirming the bacterium was a sulfur oxidizer. The developed technique made it possible to quickly detect sulfur oxidizer in environmental sample and could have wide applications in sulfur bacteria detection in environmental water samples.

    15. Scanning electron microscopy with energy dispersive X-ray spectrophotometry analysis of reciprocating and continuous rotary nickel-titanium instruments following root canal retreatment.

      PubMed

      Kalyoncuoğlu, Elif; Keskin, Cangül; Uzun, İsmail; Bengü, Aydın S; Guler, Buğra

      2016-01-01

      This study aimed to evaluate superficial defects and the composition of Reciproc R25 and ProTaper Retreatment file systems (Dentsply Maillefer, Ballaigues, Switzerland) used for retreatment. A total of 100 maxillary incisor teeth were randomly divided into the following two groups: Reciproc R25 (n = 25) and ProTaper Retreatment instrument (n = 75) groups. The nickel-titanium (Ni-Ti) compositions of the files before and after use were analyzed using energy dispersive X-ray spectrophotometry (EDX). Chi-square, Mann-Whitney U, and Kruskal-Wallis tests were used to analyze the data. ProTaper Retreatment instrument group showed a significantly higher number of defects than the Reciproc group (P < 0.05). No instrument fracture was detected. The presence of debris was observed in both groups before use, although the level was significantly higher in the ProTaper Retreatment group, which consisted of metals (P < 0.05). There was no significant difference between new and used instruments with regard to Ni-Ti composition (P < 0.05). EDX analysis showed that both the Reciproc and ProTaper Retreatment instruments had a Ni-Ti composition that was within the standards specified by the American Society of Testing and Materials. This study confirmed the use of both the Reciproc R25 file and ProTaper Retreatment file system for root canal filling removal in straight root canals as a safe procedure. (J Oral Sci 58, 401-406, 2016).

    16. Surface analysis of ProFile instruments by scanning electron microscopy and X-ray energy-dispersive spectroscopy: a preliminary study.

      PubMed

      Martins, R C; Bahia, M G A; Buono, V T L

      2002-10-01

      The purpose of this preliminary study was to analyze surface irregularities on ProFile nickel-titanium (NiTi) rotary instruments before use, after sterilization by two different methods and after instrumentation of molar root canals. Five new ProFile NiTi rotary instruments with 0.04 taper, size 20, five instruments with 0.04 taper, size 25 and five with 0.06 taper, size 20 were analyzed by scanning electron microscopy (SEM) and X-ray energy-dispersive spectroscopy (EDS). The instruments were then divided into two groups: three of each taper and size were sterilized in a dry heat sterilizer, whilst two of each taper and size were sterilized in an autoclave. After inspection by the same techniques, the files were used to instrument six molar root canals, and again analyzed by SEM/EDS. Together with the usual machining defects, a variable amount of material containing mainly carbon and sulphur was found on the surface of new instruments. This material was not removed by standard cleaning and sterilization procedures. The use of the files for instrumentation of root canals eliminated a considerable amount of the adhered substance, but deposits rich in calcium and phosphorus accumulated on the remaining impurities. The adherence of dentine on surface deposits found on new ProFile instruments requires special cleaning, prior to sterilization.

    17. Investigation of Sn surface segregation during GeSn epitaxial growth by Auger electron spectroscopy and energy dispersive x-ray spectroscopy

      SciTech Connect

      Tsukamoto, Takahiro; Suda, Yoshiyuki; Hirose, Nobumitsu; Kasamatsu, Akifumi; Mimura, Takashi; Matsui, Toshiaki

      2015-02-02

      The mechanism of Sn surface segregation during the epitaxial growth of GeSn on Si (001) substrates was investigated by Auger electron spectroscopy and energy dispersive X-ray spectroscopy. Sn surface segregation depends on the growth temperature and Sn content of GeSn layers. During Sn surface segregation, Sn-rich nanoparticles form and move on the surface during the deposition, which results in a rough surface owing to facet formation. The Sn-rich nanoparticles moving on the surface during the deposition absorb Sn from the periphery and yield a lower Sn content, not on the surface but within the layer, because the Sn surface segregation and the GeSn deposition occur simultaneously. Sn surface segregation can occur at a lower temperature during the deposition compared with that during postannealing. This suggests that the Sn surface segregation during the deposition is strongly promoted by the migration of deposited Ge and Sn adatoms on the surface originating from the thermal effect of substrate temperature, which also suggests that limiting the migration of deposited Ge and Sn adatoms can reduce the Sn surface segregation and improve the crystallinity of GeSn layers.

    18. Ca/P concentration ratio at different sites of normal and osteoporotic rabbit bones evaluated by Auger and energy dispersive X-ray spectroscopy.

      PubMed

      Kourkoumelis, Nikolaos; Balatsoukas, Ioannis; Tzaphlidou, Margaret

      2012-03-01

      Osteoporosis is a systemic skeletal disorder associated with reduced bone mineral density and the consequent high risk of bone fractures. Current practice relates osteoporosis largely with absolute mass loss. The assessment of variations in chemical composition in terms of the main elements comprising the bone mineral and its effect on the bone's quality is usually neglected. In this study, we evaluate the ratio of the main elements of bone mineral, calcium (Ca), and phosphorus (P), as a suitable in vitro biomarker for induced osteoporosis. The Ca/P concentration ratio was measured at different sites of normal and osteoporotic rabbit bones using two spectroscopic techniques: Auger electron spectroscopy (AES) and energy-dispersive X-ray spectroscopy (EDX). Results showed that there is no significant difference between samples from different genders or among cortical bone sites. On the contrary, we found that the Ca/P ratio of trabecular bone sections is comparable to cortical sections with induced osteoporosis. Ca/P ratio values are positively related to induced bone loss; furthermore, a different degree of correlation between Ca and P in cortical and trabecular bone is evident. This study also discusses the applicability of AES and EDX to the semiquantitative measurements of bone mineral's main elements along with the critical experimental parameters.

    19. Post-mortem interval estimation of human skeletal remains by micro-computed tomography, mid-infrared microscopic imaging and energy dispersive X-ray mapping.

      PubMed

      Longato, S; Wöss, C; Hatzer-Grubwieser, P; Bauer, C; Parson, W; Unterberger, S H; Kuhn, V; Pemberger, N; Pallua, Anton K; Recheis, W; Lackner, R; Stalder, R; Pallua, J D

      2015-04-07

      In this study different state-of-the-art visualization methods such as micro-computed tomography (micro-CT), mid-infrared (MIR) microscopic imaging and energy dispersive X-ray (EDS) mapping were evaluated to study human skeletal remains for the determination of the post-mortem interval (PMI). PMI specific features were identified and visualized by overlaying molecular imaging data and morphological tissue structures generated by radiological techniques and microscopic images gained from confocal microscopy (Infinite Focus (IFM)). In this way, a more distinct picture concerning processes during the PMI as well as a more realistic approximation of the PMI were achieved. It could be demonstrated that the gained result in combination with multivariate data analysis can be used to predict the Ca/C ratio and bone volume (BV) over total volume (TV) for PMI estimation. Statistical limitation of this study is the small sample size, and future work will be based on more specimens to develop a screening tool for PMI based on the outcome of this multidimensional approach.

    20. Application of Scanning Electron Microscopy/Energy-Dispersive X-Ray Spectroscopy for Characterization of Detrital Minerals in Karst Cave Speleothems.

      PubMed

      Zupančič, Nina; Miler, Miloš; Šebela, Stanka; Jarc, Simona

      2016-02-01

      Micro-scale observations in karst caves help to identify different processes that shaped local morphology. Scanning electron microscopy/energy-dispersive X-ray spectroscopy inspection of speleothems from two karst caves in Slovenia, Predjama and Črna Jama, confirmed the presence of sub-angular to sub-rounded detrital fragments of clay minerals, feldspars, quartz, Fe-oxides/hydroxides, rutile and Nb-rutile, xenotime, kassite, allanite, fluorapatite, epidote, ilmenite, monazite, sphene, and zircon, between 2 and 50 μm across. These occur in porous layers separating calcite laminae in the clayey coating on the layer below the surface of the speleothems, and are also incorporated within actual crystals. It is likely that they are derived from the weathered rocks of the Eocene flysch. Probably they were first transported into the caves by floodwaters forming cave sediments. Later, depending upon the climate conditions, they were moved by air currents or by water to the surface of active speleothems. They might also be redeposited from overlying soils enriched with wind-transported minerals from the flysch, or from higher passages filled with weathered flysch sediment, by drip water percolating through the fissured limestone. As some of the identified minerals are carriers of rare earth elements, Ti and Zr, their presence could affect any palaeoclimatic interpretations that are based upon the geochemical composition of the speleothems.

    1. Measurement Error in Atomic-Scale Scanning Transmission Electron Microscopy—Energy-Dispersive X-Ray Spectroscopy (STEM-EDS) Mapping of a Model Oxide Interface

      DOE PAGES

      Spurgeon, Steven R.; Du, Yingge; Chambers, Scott A.

      2017-04-05

      With the development of affordable aberration correctors, analytical scanning transmission electron microscopy (STEM) studies of complex interfaces can now be conducted at high spatial resolution at laboratories worldwide. Energy-dispersive X-ray spectroscopy (EDS) in particular has grown in popularity, as it enables elemental mapping over a wide range of ionization energies. However, the interpretation of atomically resolved data is greatly complicated by beam–sample interactions that are often overlooked by novice users. Here we describe the practical factors—namely, sample thickness and the choice of ionization edge—that affect the quantification of a model perovskite oxide interface. Our measurements of the same sample,more » in regions of different thickness, indicate that interface profiles can vary by as much as 2–5 unit cells, depending on the spectral feature. This finding is supported by multislice simulations, which reveal that on-axis maps of even perfectly abrupt interfaces exhibit significant delocalization. Quantification of thicker samples is further complicated by channeling to heavier sites across the interface, as well as an increased signal background. We show that extreme care must be taken to prepare samples to minimize channeling effects and argue that it may not be possible to extract atomically resolved information from many chemical maps.« less

    2. Computer-aided screening system for cervical precancerous cells based on field emission scanning electron microscopy and energy dispersive x-ray images and spectra

      NASA Astrophysics Data System (ADS)

      Jusman, Yessi; Ng, Siew-Cheok; Hasikin, Khairunnisa; Kurnia, Rahmadi; Osman, Noor Azuan Bin Abu; Teoh, Kean Hooi

      2016-10-01

      The capability of field emission scanning electron microscopy and energy dispersive x-ray spectroscopy (FE-SEM/EDX) to scan material structures at the microlevel and characterize the material with its elemental properties has inspired this research, which has developed an FE-SEM/EDX-based cervical cancer screening system. The developed computer-aided screening system consisted of two parts, which were the automatic features of extraction and classification. For the automatic features extraction algorithm, the image and spectra of cervical cells features extraction algorithm for extracting the discriminant features of FE-SEM/EDX data was introduced. The system automatically extracted two types of features based on FE-SEM/EDX images and FE-SEM/EDX spectra. Textural features were extracted from the FE-SEM/EDX image using a gray level co-occurrence matrix technique, while the FE-SEM/EDX spectra features were calculated based on peak heights and corrected area under the peaks using an algorithm. A discriminant analysis technique was employed to predict the cervical precancerous stage into three classes: normal, low-grade intraepithelial squamous lesion (LSIL), and high-grade intraepithelial squamous lesion (HSIL). The capability of the developed screening system was tested using 700 FE-SEM/EDX spectra (300 normal, 200 LSIL, and 200 HSIL cases). The accuracy, sensitivity, and specificity performances were 98.2%, 99.0%, and 98.0%, respectively.

    3. Scanning Electron Microscopy and Energy Dispersive X-ray Spectroscopy Studies on Processed Tooth Graft Material by Vacuum-ultrasonic Acceleration.

      PubMed

      Lee, Eun-Young; Kim, Eun-Suk; Kim, Kyung-Won

      2014-05-01

      The current gold standard for clinical jawbone formation involves autogenous bone as a graft material. In addition, demineralized dentin can be an effective graft material. Although demineralized dentin readily induces heterotopic bone formation, conventional decalcification takes three to five days, so, immediate bone grafting after extraction is impossible. This study evaluated the effect of vacuum ultrasonic power on the demineralization and processing of autogenous tooth material and documented the clinical results of rapidly processed autogenous demineralized dentin (ADD) in an alveolar defects patient. The method involves the demineralization of extracted teeth with detached soft tissues and pulp in 0.6 N HCl for 90 minutes using a heat controlled vacuum-ultrasonic accelerator. The characteristics of processed teeth were evaluated by scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDS). Bone grafting using ADD was performed for narrow ridges augmentation in the mandibular area. The new processing method was completed within two hours regardless of form (powder or block). EDS and SEM uniformly demineralized autotooth biomaterial. After six months, bone remodeling was observed in augmented sites and histological examination showed that ADD particles were well united with new bone. No unusual complications were encountered. This study demonstrates the possibility of preparing autogenous tooth graft materials within two hours, allowing immediate one-day grafting after extraction.

    4. Scanning Electron Microscopy-Energy-Dispersive X-Ray (SEM/EDX): A Rapid Diagnostic Tool to Aid the Identification of Burnt Bone and Contested Cremains.

      PubMed

      Ellingham, Sarah T D; Thompson, Tim J U; Islam, Meez

      2017-06-12

      This study investigates the use of Scanning electron microscopy-energy-dispersive X-ray (SEM-EDX) as a diagnostic tool for the determination of the osseous origin of samples subjected to different temperatures. Sheep (Ovis aries) ribs of two experimental groups (fleshed and defleshed) were burned at temperatures of between 100°C and 1100°C in 100°C increments and subsequently analyzed with the SEM-EDX to determine the atomic percentage of present elements. Three-factor ANOVA analysis showed that neither the exposure temperature, nor whether the burning occurred with or without soft tissue present had any significant influence on the bone's overall elemental makeup (p > 0.05). The Ca/P ratio remained in the osseous typical range of between 1.6 and 2.58 in all analyzed samples. This demonstrates that even faced with high temperatures, the overall gross elemental content and atomic percentage of elements in bone remain stable, creating a unique "fingerprint" for osseous material, even after exposure to extreme conditions. © 2017 American Academy of Forensic Sciences.

    5. Screening of cadmium and copper phytoremediation ability of Tagetes erecta, using biochemical parameters and scanning electron microscopy-energy-dispersive X-ray microanalysis.

      PubMed

      Goswami, Sunayana; Das, Suchismita

      2017-09-01

      Tagetes erecta thrived in phytotoxic levels of cadmium (Cd; 50-300 mg kg(-1) ) and copper (Cu; 150-400 mg kg(-1) ) for 21 d. It accumulated high metal contents in its above-ground tissues (3675 mg Cd kg(-1) dry wt and 3948 mg Cu kg(-1) dry wt) and showed greater root to shoot translocation and a high extraction coefficient, all of which pointed toward its potential as a hyperaccumulator. Both Cd stress and Cu stress reduced the plant biomass, foliar area, and number. In addition, there were significant declines in pigment contents as well as boosts in lipid peroxidation levels. However, the plant triggered a number of stress-mitigation strategies to abate reactive oxygen species formed as a result of Cd/Cu excess, mostly via significant augmentation of superoxide dismutase, catalase, glutathione peroxidase, and ascorbate peroxidase activities. Though the root and leaf anatomy revealed some signs of toxic symptoms at 50 mg Cd kg(-1) and at 150 mg Cu kg(-1) , as evidenced by scanning electron microscopy, the root showed maximum tolerance, with tolerance indexes of 85.4% and 91.7%, respectively. Energy-dispersive X-ray microanalysis showed specific Ca(2+) signals in both root and stomata, which could be associated with a specific signaling pathway leading to increased root metal uptake and stomatal closure. Environ Toxicol Chem 2017;36:2533-2542. © 2017 SETAC. © 2017 SETAC.

    6. An Energy-Dispersive X-Ray Fluorescence Spectrometry and Monte Carlo simulation study of Iron-Age Nuragic small bronzes ("Navicelle") from Sardinia, Italy

      NASA Astrophysics Data System (ADS)

      Schiavon, Nick; de Palmas, Anna; Bulla, Claudio; Piga, Giampaolo; Brunetti, Antonio

      2016-09-01

      A spectrometric protocol combining Energy Dispersive X-Ray Fluorescence Spectrometry with Monte Carlo simulations of experimental spectra using the XRMC code package has been applied for the first time to characterize the elemental composition of a series of famous Iron Age small scale archaeological bronze replicas of ships (known as the ;Navicelle;) from the Nuragic civilization in Sardinia, Italy. The proposed protocol is a useful, nondestructive and fast analytical tool for Cultural Heritage sample. In Monte Carlo simulations, each sample was modeled as a multilayered object composed by two or three layers depending on the sample: when all present, the three layers are the original bronze substrate, the surface corrosion patina and an outermost protective layer (Paraloid) applied during past restorations. Monte Carlo simulations were able to account for the presence of the patina/corrosion layer as well as the presence of the Paraloid protective layer. It also accounted for the roughness effect commonly found at the surface of corroded metal archaeological artifacts. In this respect, the Monte Carlo simulation approach adopted here was, to the best of our knowledge, unique and enabled to determine the bronze alloy composition together with the thickness of the surface layers without the need for previously removing the surface patinas, a process potentially threatening preservation of precious archaeological/artistic artifacts for future generations.

    7. X-Ray Diffraction and Fluorescence Measurements for In Situ Planetary Instruments

      NASA Astrophysics Data System (ADS)

      Hansford, G.; Hill, K. S.; Talboys, D.; Vernon, D.; Ambrosi, R.; Bridges, J.; Hutchinson, I.; Marinangeli, L.

      2011-12-01

      The ESA/NASA ExoMars mission, due for launch in 2018, has a combined X-ray fluorescence/diffraction instrument, Mars-XRD, as part of the onboard analytical laboratory. The results of some XRF (X-ray fluorescence) and XRD (X-ray diffraction) tests using a laboratory chamber with representative performance are reported. A range of standard geological reference materials and analogues were used in these tests. The XRD instruments are core components of the forthcoming NASA Mars Science Laboratory (MSL) and ESA/NASA ExoMars missions and will provide the first demonstrations of the capabilities of combined XRD/XRF instrumentation in situ on an extraterrestrial planetary surface. The University of Leicester team is part of the Italy-UK collaboration that is responsible for building the ExoMars X-ray diffraction instrument, Mars-XRD [1,2]. Mars-XRD incorporates an Fe-55 radioisotope source and three fixed-position charge-coupled devices (CCDs) to simultaneously acquire an X-ray fluorescence spectrum and a diffraction pattern providing a measurement of both elemental and mineralogical composition. The CCDs cover an angular range of 2θ = 6° to 73° enabling the analysis of a wide range of geologically important minerals including phyllosilicates, feldspars, oxides, carbonates and evaporites. The identification of hydrous minerals may help identify past Martian hydrothermal systems capable of preserving traces of life. Here we present some initial findings from XRF and XRD tests carried out at the University of Leicester using an Fe-55 source and X-ray sensitive CCD. The XRF/XRD test system consists of a single CCD on a motorised arm, an Fe-55 X-ray source, a collimator and a sample table which approximately replicate the reflection geometry of the Mars-XRD instrument. It was used to test geological reference standard materials and Martian analogues. This work was funded by the Science and Technology Facilities Council, UK. References [1] Marinangeli, L., Hutchinson, I

    8. 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.

    9. 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.

    10. 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.

    11. Novel in-situ x-ray diffraction measurement of ferrroelectric superlattice properties during growth

      NASA Astrophysics Data System (ADS)

      Bein, Benjamin; Hsing, Hsiang-Chun; Callori, Sara J.; Sinsheimer, John; Dawber, Matthew

      2015-03-01

      Ferroelectric domains, surface termination, average lattice parameter and bilayer thickness were monitored by in-situ x-ray diffraction during the growth of BaTiO3/SrTiO<3 (BTO/STO) superlattices by off-axis RF magnetron sputtering. A new x-ray diffraction technique was employed which makes effective use of the custom growth chamber, pilatus detector and synchrotron radiation available at beamline X21, NSLS, BNL. The technique allows for scan times substantially faster than the growth of a single layer of material, allowing continuous monitoring of multiple structural parameters as the film grows. The effect of electric boundary conditions was investigated by growing the same superlattice alternatively on STO substrates and 20nm SrRuO3 (SRO) thin films grown on STO substrates. Besides the fundamental knowledge gained from these studies, being able to monitor the structural parameters of a growing ferroelectric superlattice at this level of detail provides numerous insights which can guide the growth of higher quality ferroelectric superlattices in general. Supported by NSF: DMR-1055413.

    12. 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.

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

      PubMed

      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(R) 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.

    14. 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).

    15. In situ synchrotron X-ray diffraction study of hydrides in Zircaloy-4 during thermomechanical cycling

      NASA Astrophysics Data System (ADS)

      Cinbiz, Mahmut N.; Koss, Donald A.; Motta, Arthur T.; Park, Jun-Sang; Almer, Jonathan D.

      2017-04-01

      The d-spacing evolution of both in-plane and out-of-plane hydrides has been studied using in situ synchrotron radiation X-ray diffraction during thermo-mechanical cycling of cold-worked stress-relieved Zircaloy-4. The structure of the hydride precipitates is such that the δ{111} d-spacing of the planes aligned with the hydride platelet face is greater than the d-spacing of the 111 planes aligned with the platelet edges. Upon heating from room temperature, the δ{111} planes aligned with hydride plate edges exhibit bi-linear thermally-induced expansion. In contrast, the d-spacing of the (111) plane aligned with the hydride plate face initially contracts upon heating. These experimental results can be understood in terms of a reversal of stress state associated with precipitating or dissolving hydride platelets within the α-zirconium matrix.

    16. Compact low power infrared tube furnace for in situ X-ray powder diffraction.

      PubMed

      Doran, A; Schlicker, L; Beavers, C M; Bhat, S; Bekheet, M F; Gurlo, A

      2017-01-01

      We describe the development and implementation of a compact, low power, infrared heated tube furnace for in situ powder X-ray diffraction experiments. Our silicon carbide (SiC) based furnace design exhibits outstanding thermal performance in terms of accuracy control and temperature ramping rates while simultaneously being easy to use, robust to abuse and, due to its small size and low power, producing minimal impact on surrounding equipment. Temperatures in air in excess of 1100 °C can be controlled at an accuracy of better than 1%, with temperature ramping rates up to 100 °C/s. The complete "add-in" device, minus power supply, fits in a cylindrical volume approximately 15 cm long and 6 cm in diameter and resides as close as 1 cm from other sensitive components of our experimental synchrotron endstation without adverse effects.

    17. 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.

    18. Compact low power infrared tube furnace for in situ X-ray powder diffraction

      NASA Astrophysics Data System (ADS)

      Doran, A.; Schlicker, L.; Beavers, C. M.; Bhat, S.; Bekheet, M. F.; Gurlo, A.

      2017-01-01

      We describe the development and implementation of a compact, low power, infrared heated tube furnace for in situ powder X-ray diffraction experiments. Our silicon carbide (SiC) based furnace design exhibits outstanding thermal performance in terms of accuracy control and temperature ramping rates while simultaneously being easy to use, robust to abuse and, due to its small size and low power, producing minimal impact on surrounding equipment. Temperatures in air in excess of 1100 °C can be controlled at an accuracy of better than 1%, with temperature ramping rates up to 100 °C/s. The complete "add-in" device, minus power supply, fits in a cylindrical volume approximately 15 cm long and 6 cm in diameter and resides as close as 1 cm from other sensitive components of our experimental synchrotron endstation without adverse effects.

    19. Development of a combined portable x-ray fluorescence and Raman spectrometer for in situ analysis

      NASA Astrophysics Data System (ADS)

      Guerra, M.; Longelin, S.; Pessanha, S.; Manso, M.; Carvalho, M. L.

      2014-06-01

      In this work, we have built a portable X-ray fluorescence (XRF) spectrometer in a planar configuration coupled to a Raman head and a digital optical microscope, for in situ analysis. Several geometries for the XRF apparatus and digital microscope are possible in order to overcome spatial constraints and provide better measurement conditions. With this combined spectrometer, we are now able to perform XRF and Raman measurements in the same point without the need for sample collection, which can be crucial when dealing with cultural heritage objects, as well as forensic analysis. We show the capabilities of the spectrometer by measuring several standard reference materials, as well as other samples usually encountered in cultural heritage, geological, as well as biomedical studies.

    20. Advanced in situ metrology for x-ray beam shaping with super precision.

      PubMed

      Wang, Hongchang; Sutter, John; Sawhney, Kawal

      2015-01-26

      We report a novel method for in situ metrology of an X-ray bimorph mirror by using the speckle scanning technique. Both the focusing beam and the "tophat" defocussed beam have been generated by optimizing the bimorph mirror in a single iteration. Importantly, we have demonstrated that the angular sensitivity for measuring the slope error of an optical surface can reach accuracy in the range of two nanoradians. When compared with conventional ex-situ metrology techniques, the method enables a substantial increase of around two orders of magnitude in the angular sensitivity and opens the way to a previously inaccessible region of slope error measurement. Such a super precision metrology technique will be beneficial for both the manufacture of polished mirrors and the optimization of beam shaping.

    1. Titanium boride equation of state determined by in-situ X-ray diffraction.

      PubMed

      Ono, Shigeaki; Kikegawa, Takumi

      2016-12-01

      The equation of state (EOS) of titanium boride, TiB2, was investigated by in situ X-ray diffraction in a diamond anvil cell and multianvil high-pressure apparatus. The pressure-volume-temperature (P-V-T) data were collected at up to 111 GPa and room temperature for the diamond-anvil cell experiments and at up to 15 GPa and 1300 K for the multianvil experiments. No phase transition was observed through the entire range of experimental conditions. The pressure-volume data at room temperature were fitted using a Vinet EOS to obtain the isothermal bulk modulus, BT0 = 256.7 GPa, and its pressure derivative, B' T0 = 3.83. When fitting a thermal EOS using the P-V-T data for the multianvil experiments, we find that [Formula: see text] = 0.095 (GPa/K) and α 0 = 2.49 × 10(-5) K(-1).

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

      NASA Astrophysics Data System (ADS)

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

      2012-02-01

      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.

    3. Development of a combined portable x-ray fluorescence and Raman spectrometer for in situ analysis.

      PubMed

      Guerra, M; Longelin, S; Pessanha, S; Manso, M; Carvalho, M L

      2014-06-01

      In this work, we have built a portable X-ray fluorescence (XRF) spectrometer in a planar configuration coupled to a Raman head and a digital optical microscope, for in situ analysis. Several geometries for the XRF apparatus and digital microscope are possible in order to overcome spatial constraints and provide better measurement conditions. With this combined spectrometer, we are now able to perform XRF and Raman measurements in the same point without the need for sample collection, which can be crucial when dealing with cultural heritage objects, as well as forensic analysis. We show the capabilities of the spectrometer by measuring several standard reference materials, as well as other samples usually encountered in cultural heritage, geological, as well as biomedical studies.

    4. In situ synchrotron x-ray studies of ferroelectric thin films.

      SciTech Connect

      Fong, D. D.; Eastman, J. A.; Stephenson, G. B.; Fuoss, P. H.; Streiffer, S. K.; Thompson, C.; Auciello, O.; Materials Science Division; Northern Illinois Univ.

      2005-03-01

      In situ synchrotron X-ray scattering was used to observe both the growth of PbTiO{sub 3} films by metal-organic chemical vapor deposition and the behavior of the ferroelectric phase transition as a function of film thickness. The dependences of growth mode and deposition rate on gas flows and substrate temperature were determined by homoepitaxial growth studies on thick films (>50 nm). These studies facilitated the growth of thin coherently strained PbTiO{sub 3} films on SrTiO{sub 3} (001) substrates, with thicknesses ranging from 2 to 42 nm. Experiments on the ferroelectric phase transition as a function of film thickness were carried out in these films under controlled mechanical and electrical boundary conditions.

    5. In situ synchrotron X-ray diffraction study of hydrides in Zircaloy-4 during thermomechanical cycling

      DOE PAGES

      Cinbiz, Mahmut N.; Koss, Donald A.; Motta, Arthur T.; ...

      2017-02-20

      The d-spacing evolution of both in-plane and out-of-plane hydrides has been studied using in situ synchrotron radiation X-ray diffraction during thermo-mechanical cycling of cold-worked stress-relieved Zircaloy-4. The structure of the hydride precipitates is such that the δ{111} d-spacing of the planes aligned with the hydride platelet face is greater than the d-spacing of the 111 planes aligned with the platelet edges. Upon heating from room temperature, the δ{111} planes aligned with hydride plate edges exhibit bi-linear thermally-induced expansion. In contrast, the d-spacing of the (111) plane aligned with the hydride plate face initially contracts upon heating. Furthermore, these experimental resultsmore » can be understood in terms of a reversal of stress state associated with precipitating or dissolving hydride platelets within the α-zirconium matrix.« less

    6. In Situ Study of Silicon Electrode Lithiation with X-ray Reflectivity

      DOE PAGES

      Cao, Chuntian; Steinrück, Hans-Georg; Shyam, Badri; ...

      2016-10-26

      Surface sensitive X-ray reflectivity (XRR) measurements were performed to investigate the electrochemical lithiation of a native oxide terminated single crystalline silicon (100) electrode in real time during the first galvanostatic discharge cycle. This allows us to gain nanoscale, mechanistic insight into the lithiation of Si and the formation of the solid electrolyte interphase (SEI). We describe an electrochemistry cell specifically designed for in situ XRR studies and have determined the evolution of the electron density profile of the lithiated Si layer (LixSi) and the SEI layer with subnanometer resolution. We propose a three-stage lithiation mechanism with a reaction limited, layer-by-layermore » lithiation of the Si at the LixSi/Si interface.« less

    7. In Situ Study of Silicon Electrode Lithiation with X-ray Reflectivity

      SciTech Connect

      Cao, Chuntian; Steinrück, Hans-Georg; Shyam, Badri; Stone, Kevin H.; Toney, Michael F.

      2016-10-26

      Surface sensitive X-ray reflectivity (XRR) measurements were performed to investigate the electrochemical lithiation of a native oxide terminated single crystalline silicon (100) electrode in real time during the first galvanostatic discharge cycle. This allows us to gain nanoscale, mechanistic insight into the lithiation of Si and the formation of the solid electrolyte interphase (SEI). We describe an electrochemistry cell specifically designed for in situ XRR studies and have determined the evolution of the electron density profile of the lithiated Si layer (LixSi) and the SEI layer with subnanometer resolution. We propose a three-stage lithiation mechanism with a reaction limited, layer-by-layer lithiation of the Si at the LixSi/Si interface.

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

      NASA Astrophysics Data System (ADS)

      Zalkind, S.; Rafailov, G.; Halevy, I.; Livneh, T.; Rubin, A.; Maimon, H.; Schweke, D.

      2017-03-01

      The oxidation kinetics of U-0.1 wt%Cr at oxygen pressures of 150 Torr and the temperature range of 90-150 °C was studied by means of in-situ X-ray diffraction (XRD). A "breakaway" in the oxidation kinetics is found at ∼0.25 μm, turning from a parabolic to a linear rate law. At the initial stage of oxidation the growth plane of UO2(111) is the prominent one. As the oxide thickens, the growth rate of UO2(220) plane increases and both planes grow concurrently. The activation energies obtained for the oxide growth are Qparabolic = 17.5 kcal/mol and Qlinear = 19 kcal/mol. Enhanced oxidation around uranium carbide (UC) inclusions is clearly observed by scanning electron microscopy (SEM).

    9. Orthorhombic boron oxide under pressure: In situ study by X-ray diffraction and Raman scattering

      NASA Astrophysics Data System (ADS)

      Cherednichenko, Kirill A.; Le Godec, Yann; Kalinko, Aleksandr; Mezouar, Mohamed; Solozhenko, Vladimir L.

      2016-11-01

      High-pressure phase of boron oxide, orthorhombic β-B2O3, has been studied in situ by synchrotron X-ray diffraction to 22 GPa and Raman scattering to 46 GPa at room temperature. The bulk modulus of β-B2O3 has been found to be 169(3) GPa that is in good agreement with our ab initio calculations. Raman and IR spectra of β-B2O3 have been measured at ambient pressure; all experimentally observed bands have been attributed to the theoretically calculated ones, and the mode assignment has been performed. Based on the data on Raman shift as a function of pressure, combined with equation-of-state data, the Grüneisen parameters of all experimentally observed Raman bands have been calculated. β-B2O3 enriched by 10B isotope has been synthesized, and the effect of boron isotopic substitution on Raman spectra has been studied.

    10. 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.

    11. Compact x-ray microradiograph for in situ imaging of solidification processes: Bringing in situ x-ray micro-imaging from the synchrotron to the laboratory

      SciTech Connect

      Rakete, C.; Baumbach, C.; Goldschmidt, A.; Samberg, D.; Schroer, C. G.; Breede, F.; Stenzel, C.; Zimmermann, G.; Pickmann, C.; Houltz, Y.; Lockowandt, C.; Svenonius, O.; Wiklund, P.; Mathiesen, R. H.

      2011-10-15

      A laboratory based high resolution x-ray radiograph was developed for the investigation of solidification dynamics in alloys. It is based on a low-power microfocus x-ray tube and is potentially appropriate for x-ray diagnostics in space. The x-ray microscope offers a high spatial resolution down to approximately 5 {mu}m. Dynamic processes can be resolved with a frequency of up to 6 Hz. In reference experiments, the setup was optimized to yield a high contrast for AlCu-alloys. With samples of about 150 {mu}m thickness, high quality image sequences of the solidification process were obtained with high resolution in time and space.

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

      SciTech Connect

      Li, Meimei; Almer, Jonathan D.; Yang, Yong; Tan, Lizhen

      2016-01-01

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

    13. Structural study on Ni nanowires in an anodic alumina membrane by using in situ heating extended x-ray absorption fine structure and x-ray diffraction techniques.

      PubMed

      Cai, Quan; Zhang, Junxi; Chen, Xing; Chen, Zhongjun; Wang, Wei; Mo, Guang; Wu, Zhonghua; Zhang, Lide; Pan, Wei

      2008-03-19

      Polycrystalline Ni nanowires have been prepared by electrochemical deposition in an anodic alumina membrane template with a nanopore size of about 60 nm. In situ heating extended x-ray absorption fine structure and x-ray diffraction techniques are used to probe the atomic structures. The nanowires are identified as being mixtures of nanocrystallites and amorphous phase. The nanocrystallites have the same thermal expansion coefficient, of 1.7 × 10(-5) K(-1), as Ni bulk; however, the amorphous phase has a much larger thermal expansion coefficient of 3.5 × 10(-5) K(-1). Details of the Ni nanowire structures are discussed in this paper.

    14. Nondestructive characterization of municipal-solid-waste-contaminated surface soil by energy-dispersive X-ray fluorescence and low-Z (atomic number) particle electron probe X-ray microanalysis.

      PubMed

      Gupta, Dhrubajyoti; Ghosh, Rita; Mitra, Ajoy K; Roy, Subinit; Sarkar, Manoranjan; Chowdhury, Subhajit; Bhowmik, Asit; Mukhopadhyay, Ujjal; Maskey, Shila; Ro, Chul-Un

      2011-11-01

      The long-term environmental impact of municipal solid waste (MSW) landfilling is still under investigation due to the lack of detailed characterization studies. A MSW landfill site, popularly known as Dhapa, in the eastern fringe of the metropolis of Kolkata, India, is the subject of present study. A vast area of Dhapa, adjoining the current core MSW dump site and evolving from the raw MSW dumping in the past, is presently used for the cultivation of vegetables. The inorganic chemical characteristics of the MSW-contaminated Dhapa surface soil (covering a 2-km stretch of the area) along with a natural composite (geogenic) soil sample (from a small countryside farm), for comparison, were investigated using two complementary nondestructive analytical techniques, energy-dispersive X-ray fluorescence (EDXRF) for bulk analysis and low-Z (atomic number) particle electron probe X-ray microanalysis (low-Z particle EPMA) for single-particle analysis. The bulk concentrations of K, Rb, and Zr remain almost unchanged in all the soil samples. The Dhapa soil is found to be polluted with heavy metals such as Cu, Zn, and Pb (highly elevated) and Ti, Cr, Mn, Fe, Ni, and Sr (moderately elevated), compared to the natural countryside soil. These high bulk concentration levels of heavy metals were compared with the Ecological Soil Screening Levels for these elements (U.S. Environment Protection Agency) to assess the potential risk on the immediate biotic environment. Low-Z particle EPMA results showed that the aluminosilicate-containing particles were the most abundant, followed by SiO2, CaCO3-containing, and carbonaceous particles in the Dhapa samples, whereas in the countryside sample only aluminosilicate-containing and SiO2 particles were observed. The mineral particles encountered in the countryside sample are solely of geogenic origin, whereas those from the Dhapa samples seem to have evolved from a mixture of raw dumped MSW, urban dust, and other contributing factors such as wind

    15. Elemental analysis of human amniotic fluid and placenta by total-reflection X-ray fluorescence and energy-dispersive X-ray fluorescence: child weight and maternal age dependence

      NASA Astrophysics Data System (ADS)

      Carvalho, M. L.; Custódio, P. J.; Reus, U.; Prange, A.

      2001-11-01

      This work is an attempt to evaluate the possible influence of the mother's age in trace element concentrations in human amniotic fluid and placenta and whether these concentrations are correlated to the weight of the newborn infants. Total-reflection X-ray fluorescence (TXRF) was used to analyze 16 amniotic fluid samples, and the placenta samples were analyzed by energy dispersive X-ray fluorescence (EDXRF). The whole samples were collected during delivery from healthy mothers and healthy infants and full-term pregnancies. According to the age of the mother, three different groups were considered: 20-25, 25-30 and 30-40 years old. Only two mothers were aged more than 35 years. The weight of the infants ranged from 2.56 to 4.05 kg and three groups were also considered: 2.5-3, 3-3.5 and 3.5-4 kg. The organic matrix of the amniotic fluid samples was removed by treatment with HNO 3 followed by oxygen plasma ashing. Yttrium was used as the internal standard for TXRF analysis. Placenta samples were lyophilized and analyzed by EDXRF without any chemical treatment. Very low levels of Ni and Sr were found in the amniotic fluid samples, and were independent of the age of the mother and weight of the child. Cr, Mn, Se and Pb were at the level of the detection limit. Zn, considered one of the key elements in neonatal health, was not significantly different in the samples analyzed; however, it was weakly related to birth weigh. The concentrations obtained ranged from 0.11 to 0.92 mg/l and 30 to 65 μg/g in amniotic fluid and placenta, respectively. The only two elements which seemed to be significantly correlated with mother's age and newborn weight were Ca and Fe for both types of sample: Ca levels were increased in heavier children and older mothers; however, Fe increased with increasing maternal age, but decreased for heavier babies. The same conclusions were obtained for placenta and amniotic fluid samples. Cu is closely associated with Fe in its function in the organism

    16. Orthogonal identification of gunshot residue with complementary detection principles of voltammetry, scanning electron microscopy, and energy-dispersive X-ray spectroscopy: sample, screen, and confirm.

      PubMed

      O'Mahony, Aoife M; Samek, Izabela A; Sattayasamitsathit, Sirilak; Wang, Joseph

      2014-08-19

      Field-deployable voltammetric screening coupled with complementary laboratory-based analysis to confirm the presence of gunshot residue (GSR) from the hands of a subject who has handled, loaded, or discharged a firearm is described. This protocol implements the orthogonal identification of the presence of GSR utilizing square-wave stripping voltammetry (SWSV) as a rapid screening tool along with scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) to confirm the presence of the characteristic morphology and metal composition of GSR particles. This is achieved through the judicious modification of the working electrode of a carbon screen-printed electrode (CSPE) with carbon tape (used in SEM analysis) to fix and retain a sample. A comparison between a subject who has handled and loaded a firearm and a subject who has had no contact with GSR shows the significant variations in voltammetric signals and the presence or absence of GSR-consistent particles and constituent metals. This initial electrochemical screening has no effect on the integrity of the metallic particles, and SEM/EDX analysis conducted prior to and postvoltammetry show no differences in analytical output. The carbon tape is instrumental in retaining the GSR sample after electrochemical analysis, supported by comparison with orthogonal detection at a bare CSPE. This protocol shows great promise as a two-tier detection system for the presence of GSR from the hands of a subject, whereby initial screening can be conducted rapidly onsite by minimally trained operators; confirmation can follow at the same substrate to substantiate the voltammetric results.

    17. Scanning Electron Microscopy and Energy-Dispersive X-Ray Microanalysis of Set CEM Cement after Application of Different Bleaching Agents.

      PubMed

      Samiei, Mohammad; Janani, Maryam; Vahdati, Amin; Alemzadeh, Yalda; Bahari, Mahmoud

      2017-01-01

      The present study evaluated the element distribution in completely set calcium-enriched mixture (CEM) cement after application of 35% carbamide peroxide, 40% hydrogen peroxide and sodium perborate as commercial bleaching agents using an energy-dispersive x-ray microanalysis (EDX) system. The surface structure was also observed using the scanning electron microscope (SEM). Twenty completely set CEM cement samples, measuring 4×4 mm(2), were prepared in the present in vitro study and randomly divided into 4 groups based on the preparation technique as follows: the control group; 35% carbamide peroxide group in contact for 30-60 min for 4 times; 40% hydrogen peroxide group with contact time of 15-20 min for 3 times; and sodium perborate group, where the powder and liquid were mixed and placed on CEM cement surface 4 times. Data were analyzed at a significance level of 0.05 through the one Way ANOVA and Tukey's post hoc tests. EDX showed similar element distribution of oxygen, sodium, calcium and carbon in CEM cement with the use of carbamide peroxide and hydroxide peroxide; however, the distribution of silicon was different (P<0.05). In addition, these bleaching agents resulted in significantly higher levels of oxygen and carbon (P<0.05) and a lower level of calcium (P<0.05) compared to the control group. SEM of the control group showed plate-like and globular structure. Sodium perborate was similar to control group due to its weak oxidizing properties. Globular structures and numerous woodpecker holes were observed on the even surface on the carbamide peroxide group. The mean elemental distribution of completely set CEM cement was different when exposed to sodium perborate, carbamide peroxide and hydrogen peroxide.

    18. Determination of heavy metals concentrations in airborne particulates matter (APM) from Manjung district, Perak using energy dispersive X-ray fluorescence (EDXRF) spectrometer

      NASA Astrophysics Data System (ADS)

      Arshad, Nursyairah; Hamzah, Zaini; Wood, Ab. Khalik; Saat, Ahmad; Alias, Masitah

      2015-04-01

      Airborne particulates trace metals are considered as public health concern as it can enter human lungs through respiratory system. Generally, any substance that has been introduced to the atmosphere that can cause severe effects to living things and the environment is considered air pollution. Manjung, Perak is one of the development districts that is active with industrial activities. There are many industrial activities surrounding Manjung District area such as coal fired power plant, quarries and iron smelting which may contribute to the air pollution into the environment. This study was done to measure the concentrations of Hg, U, Th, K, Cu, Fe, Cr, Zn, As, Se, Pb and Cd in the Airborne Particulate Matter (APM) collected at nine locations in Manjung District area within 15 km radius towards three directions (North, North-East and South-East) in 5 km intervals. The samples were collected using mini volume air sampler with cellulose filter through total suspended particulate (TSP). The sampler was set up for eight hours with the flow rate of 5 L/min. The filter was weighed before and after sample collection using microbalance, to get the amount of APM and kept in desiccator before analyzing. The measurement was done using calibrated Energy Dispersive X-Ray Fluorescence (EDXRF) Spectrometer. The air particulate concentrations were found below the Malaysia Air Quality Guidelines for TSP (260 µg/m3). All of the metals concentrations were also lower than the guidelines set by World Health Organization (WHO), Ontario Ministry of the Environment and Argonne National Laboratory, USA NCRP (1975). From the concentrations, the enrichment factor were calculated.

    19. Energy dispersive X-ray fluorescence and scattering assessment of soil quality via partial least squares and artificial neural networks analytical modeling approaches.

      PubMed

      Kaniu, M I; Angeyo, K H; Mwala, A K; Mwangi, F K

      2012-08-30

      Soil quality assessment (SQA) calls for rapid, simple and affordable but accurate analysis of soil quality indicators (SQIs). Routine methods of soil analysis are tedious and expensive. Energy dispersive X-ray fluorescence and scattering (EDXRFS) spectrometry in conjunction with chemometrics is a potentially powerful method for rapid SQA. In this study, a 25 m Ci (109)Cd isotope source XRF spectrometer was used to realize EDXRFS spectrometry of soils. Glycerol (a simulate of "organic" soil solution) and kaolin (a model clay soil) doped with soil micro (Fe, Cu, Zn) and macro (NO(3)(-), SO(4)(2-), H(2)PO(4)(-)) nutrients were used to train multivariate chemometric calibration models for direct (non-invasive) analysis of SQIs based on partial least squares (PLS) and artificial neural networks (ANN). The techniques were compared for each SQI with respect to speed, robustness, correction ability for matrix effects, and resolution of spectral overlap. The method was then applied to perform direct rapid analysis of SQIs in field soils. A one-way ANOVA test showed no statistical difference at 95% confidence interval between PLS and ANN results compared to reference soil nutrients. PLS was more accurate analyzing C, N, Na, P and Zn (R(2)>0.9) and low SEP of (0.05%, 0.01%, 0.01%, and 1.98 μg g(-1)respectively), while ANN was better suited for analysis of Mg, Cu and Fe (R(2)>0.9 and SEP of 0.08%, 4.02 μg g(-1), and 0.88 μg g(-1) respectively).

    20. Quantitative determinations and imaging in different structures of buried human bones from the XVIII-XIXth centuries by energy dispersive X-ray fluorescence - Postmortem evaluation.

      PubMed

      Guimarães, D; Dias, A A; Carvalho, M; Carvalho, M L; Santos, J P; Henriques, F R; Curate, F; Pessanha, S

      2016-08-01

      In this work, a non-commercial triaxial geometry energy dispersive X-ray Fluorescence (EDXRF) setup and a benchtop µ-XRF system were used to identify postmortem contamination in buried bones. For two of the individuals, unusually high concentrations of Cu and Pb, but also Zn (in one individual) were observed. The pigments of the burial shroud coverings have been identified as the source of contamination. Accurate and precise quantitative results were obtained by nondestructive process using fundamental parameters method taking into account the matrix absorption effects. A total of 30 bones from 13 individuals, buried between the mid-XVIIIth to early XIXth centuries, were analyzed to study the elemental composition and elemental distribution. The bones were collected from a church in Almada (Portugal), called Ermida do Espírito Santo, located near the Tagus River and at the sea neighbourhood. The triaxial geometry setup was used to quantify Ca, Fe, Cu, Zn, Br, Sr and Pb of powder pressed bone pellets (n=9 for each bone). Cluster analysis was performed considering the elemental concentrations for the different bones. There was a clear association between some bones regarding Fe, Cu, Zn, Br and Pb content but not a categorization between cortical and trabecular bones. The elemental distribution of Cu, Zn and Pb were assessed by the benchtop μ-analysis, the M4 Tornado, based on a polycapillary system which provides multi-elemental 2D maps. The results showed that contamination was mostly on the surface of the bone confirming that it was related to the burial shroud covering the individuals.

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

      PubMed Central

      Saini, Monika; Chandra, Suresh; Singh, Yashpal; Basu, Bikramjit; Tripathi, Arvind

      2010-01-01

      Objective: Porcelain chipping from porcelain fused to metal restoration has been Achilles heel till date. There has been advent of newer ceramics in past but but none of them has been a panacea for Porcelain fracture. An optimal firing is thus essential for the clinical success of the porcelain-fused to metal restoration. The aim of the present study was to evaluate ceramo-metal interface at different firing temperature using XRD and SEM-EDS analysis. Clinical implication of the study was to predict the optimal firing temperature at which porcelain should be fused with metal in order to possibly prevent the occasional failure of the porcelain fused to metal restorations. Materials and Methods: To meet the above-mentioned goal, porcelain was fused to metal at different firing temperatures (930–990°C) in vacuum. The microstructural observations of interface between porcelain and metal were evaluated using X-ray diffraction and scanning electron microscopy with energy dispersive spectroscopy. Results: Based on the experimental investigation of the interaction zone of porcelain fused to metal samples, it was observed that as the firing temperature was increased, the pores became less in number as well as the size of the pores decreased at the porcelain/metal interface upto 975°C but increased in size at 990°C. The least number of pores with least diameter were found in samples fired at 975°C. Several oxides like Cr2O3, NiO, and Al2O3 and intermetallic compounds (CrSi2, AlNi3) were also formed in the interaction zone. Conclusions It is suggested that the presence of pores may trigger the crack propagation along the interface, causing the failure of the porcelain fused to metal restoration during masticatory action. PMID:22114406

    2. Characterisation of ferromagnetic magnetic storage media surfaces by complementary particle induced X-ray analysis and time of flight-energy dispersive elastic recoil detection analysis

      NASA Astrophysics Data System (ADS)

      Zhang, Yanwen; Elfman, Mikael; Winzell, Thomas; Whitlow, Harry J.

      1999-04-01

      Thin (10 nm-1 μm) films of ferromagnetic material constitute an important class of materials that are difficult to analyse by conventional ion beam analytical (IBA) techniques because they are based on the ferromagnetic elements (Co, Fe, Mn, Ni, and Cr). The similar or overlapping isotope masses makes it difficult to separate the elemental signals using time of flight and energy dispersive elastic recoil detection (ToF-E ERD). In this exploratory study we have investigated the use of Particle Induced X-ray Emission (PIXE) measurements to refine the mass dispersive depth profile information from ToF-E ERD. The surfaces of two commercial magnetic media were investigated. One sample was a 3 {1}/{2}'' double density diskette with a coating of ferrite particles in an organic binder. The other sample was a complex C/Co/Cr/Ni-P/Al multilayer structure taken from a standard hard disc. The Lund nuclear microprobe with a 2.55 MeV proton beam was used for PIXE analysis. ToF-ERD measurements were carried out using a 55 MeV 127I 10+ ion beam incident at 67.5° to the surface normal. The time of flight and kinetic energy of recoils ejected at 45° to the ion beam direction was measured in a detector telescope. The findings demonstrate that by detailed analysis of the PIXE spectra it is possible to remove the ambiguities in mass assignment of the ToF-ERD data associated with the ferromagnetic elements.

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

      PubMed

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

      2012-01-01

      The aim of this study was to investigate the effects of some acidic drinks on dentin erosion, using methods of surface profile (SP) analysis and energy-dispersive X-ray fluorescence spectrometry (EDXRF). One hundred standardized dentin slabs obtained from bovine incisor roots were used. Dentin slabs measuring 5x5 mm were ground flat, polished and half of each specimen surface was protected with nail polish. For 60 min, the dentin surfaces were immersed in 50 mL of 5 different drinks (Gatorade®, Del Valle Mais orange juice®, Coca-Cola®, Red Bull® and white wine), 20 blocks in each drink. The pH of each beverage was measured. After the erosive challenge, the nail polish was removed and SP was analyzed. The mineral concentration of dentin surfaces was determined by means of EDXRF. Data were analyzed statistically by ANOVA and Tukey's test (α=0.05). SP analysis showed that Red-Bull had the highest erosive potential (p<0.05). EDXRF results exhibited a decrease in phosphate in the groups immersed in Red-Bull, orange juice and white wine (p<0.05), and no significant difference in calcium content between the reference surface and eroded surface. In conclusion, this study demonstrated that all studied beverages promoted erosion on root dentin and Red Bull had the highest erosive potential. There was no correlation between pH of beverages and their erosive potential and only the P content changed after erosive challenge.

    4. Microbiological or chemical models of enamel secondary caries compared by polarized-light microscopy and energy dispersive X-ray spectroscopy.

      PubMed

      Paradella, Thaís Cachuté; de Sousa, Fernando Augusto Cervantes Garcia; Koga-Ito, Cristiane Yumi; Jorge, Antonio Olavo Cardoso

      2009-08-01

      Different secondary caries models may present different results. The purpose of this study was to compare different in vitro secondary caries models, evaluating the obtained results by polarized-light microscopy (PLM), scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDS). Standardized human enamel specimens (n = 12) restored with different materials (Z250 conventional composite resin-CRZ, Freedom polyacid-modified composite resin-CRF, Vitremer resin-modified glass-ionomer-GIV, and Fuji IX conventional glass-ionomer cement-GIF) were submitted to microbiological (MM) or chemical caries models (CM). The control group was not submitted to any caries model. For MM, specimens were immersed firstly in sucrose broth inoculated with Streptococcus mutans ATCC 35688, incubated at 37 degrees C/5% CO(2) for 14 days and then in remineralizing solution for 14 days. For CM, specimens were submitted to chemical pH-cycling. Specimens were ground, submitted to PLM and then were dehydrated, gold-sputtered and submitted to SEM and EDS. Results were statistically analyzed by Kruskall-Wallis and Student-Newman-Keuls tests (alpha = 0.05). No differences between in vitro caries models were found. Morphological differences in enamel demineralization were found between composite resin and polyacid-modified composite resin (CRZ and CRF) and between the resin-modified glass-ionomer and the glass-ionomer cement (GIF and GIV). GIF showed higher calcium concentration and less demineralization, differing from the other materials. In conclusion, the glass-ionomer cement showed less caries formation under both in vitro caries models evaluated.

    5. Scanning Electron Microscopy and Energy-Dispersive X-Ray Microanalysis of Set CEM Cement after Application of Different Bleaching Agents

      PubMed Central

      Samiei, Mohammad; Janani, Maryam; Vahdati, Amin; Alemzadeh, Yalda; Bahari, Mahmoud

      2017-01-01

      Introduction: The present study evaluated the element distribution in completely set calcium-enriched mixture (CEM) cement after application of 35% carbamide peroxide, 40% hydrogen peroxide and sodium perborate as commercial bleaching agents using an energy-dispersive x-ray microanalysis (EDX) system. The surface structure was also observed using the scanning electron microscope (SEM). Methods and Materials: Twenty completely set CEM cement samples, measuring 4×4 mm2, were prepared in the present in vitro study and randomly divided into 4 groups based on the preparation technique as follows: the control group; 35% carbamide peroxide group in contact for 30-60 min for 4 times; 40% hydrogen peroxide group with contact time of 15-20 min for 3 times; and sodium perborate group, where the powder and liquid were mixed and placed on CEM cement surface 4 times. Data were analyzed at a significance level of 0.05 through the one Way ANOVA and Tukey’s post hoc tests. Results: EDX showed similar element distribution of oxygen, sodium, calcium and carbon in CEM cement with the use of carbamide peroxide and hydroxide peroxide; however, the distribution of silicon was different (P<0.05). In addition, these bleaching agents resulted in significantly higher levels of oxygen and carbon (P<0.05) and a lower level of calcium (P<0.05) compared to the control group. SEM of the control group showed plate-like and globular structure. Sodium perborate was similar to control group due to its weak oxidizing properties. Globular structures and numerous woodpecker holes were observed on the even surface on the carbamide peroxide group. Conclusion: The mean elemental distribution of completely set CEM cement was different when exposed to sodium perborate, carbamide peroxide and hydrogen peroxide. PMID:28512484

    6. 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

    7. In Situ Synchrotron X-ray Study of Ultrasound Cavitation and Its Effect on Solidification Microstructures

      SciTech Connect

      Mi, Jiawei; Tan, Dongyue; Lee, Tung Lik

      2014-12-11

      Considerable progress has been made in studying the mechanism and effectiveness of using ultrasound waves to manipulate the solidification microstructures of metallic alloys. However, uncertainties remain in both the underlying physics of how microstructures evolve under ultrasonic waves, and the best technological approach to control the final microstructures and properties. We used the ultrafast synchrotron X-ray phase contrast imaging facility housed at the Advanced Photon Source, Argonne National Laboratory, US to study in situ the highly transient and dynamic interactions between the liquid metal and ultrasonic waves/bubbles. The dynamics of ultrasonic bubbles in liquid metal and their interactions with the solidifying phases in a transparent alloy were captured in situ. The experiments were complemented by the simulations of the acoustic pressure field, the pulsing of the bubbles, and the associated forces acting onto the solidifying dendrites. The study provides more quantitative understanding on how ultrasonic waves/bubbles influence the growth of dendritic grains and promote the grain multiplication effect for grain refinement.

    8. 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.

    9. In Situ Synchrotron X-ray Study of Ultrasound Cavitation and Its Effect on Solidification Microstructures

      NASA Astrophysics Data System (ADS)

      Mi, Jiawei; Tan, Dongyue; Lee, Tung Lik

      2015-08-01

      Considerable progress has been made in studying the mechanism and effectiveness of using ultrasound waves to manipulate the solidification microstructures of metallic alloys. However, uncertainties remain in both the underlying physics of how microstructures evolve under ultrasonic waves, and the best technological approach to control the final microstructures and properties. We used the ultrafast synchrotron X-ray phase contrast imaging facility housed at the Advanced Photon Source, Argonne National Laboratory, US to study in situ the highly transient and dynamic interactions between the liquid metal and ultrasonic waves/bubbles. The dynamics of ultrasonic bubbles in liquid metal and their interactions with the solidifying phases in a transparent alloy were captured in situ. The experiments were complemented by the simulations of the acoustic pressure field, the pulsing of the bubbles, and the associated forces acting onto the solidifying dendrites. The study provides more quantitative understanding on how ultrasonic waves/bubbles influence the growth of dendritic grains and promote the grain multiplication effect for grain refinement.

    10. First use of portable system coupling X-ray diffraction and X-ray fluorescence for in-situ analysis of prehistoric rock art.

      PubMed

      Beck, L; Rousselière, H; Castaing, J; Duran, A; Lebon, M; Moignard, B; Plassard, F

      2014-11-01

      Study of prehistoric art is playing a major role in the knowledge of human evolution. Many scientific methods are involved in this investigation including chemical analysis of pigments present on artefacts or applied to cave walls. In the past decades, the characterization of coloured materials was carried on by taking small samples. This procedure had two main disadvantages: slight but existing damage of the paintings and limitation of the number of samples. Thanks to the advanced development of portable systems, in-situ analysis of pigment in cave can be now undertaken without fear for this fragile Cultural Heritage. For the first time, a portable system combining XRD and XRF was used in an underground and archaeological environment for prehistoric rock art studies. In-situ non-destructive analysis of black prehistoric drawings and determination of their composition and crystalline structure were successfully carried out. Original results on pigments used 13,000 years ago in the cave of Rouffignac (France) were obtained showing the use of two main manganese oxides: pyrolusite and romanechite. The capabilities of the portable XRD-XRF system have been demonstrated for the characterization of pigments as well as for the analysis of rock in a cave environment. This first in-situ experiment combining X-ray diffraction and X-ray fluorescence open up new horizons and can fundamentally change our approach of rock art studies.

    11. 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.

    12. 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

    13. 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.

    14. In Situ X-ray Synchrotron Tomographic Imaging During the Compression of Hyperelastic Polymeric Materials

      SciTech Connect

      Patterson, Brian M.; Cordes, Nikolaus L.; Henderson, Kevin; Williams, Jason J.; Stannard, Tyler; Singh, Sudhanshu S.; Ovejero, Angel Rodriguez; Xiao, Xianghui; Robinson, Mathew; Chawla, Nikhilesh

      2016-01-01

      Cellular structures are present in many modern and natural materials and their proper utilization is crucial within many industries. Characterizing their structural and mechanical properties is complicated, in that they often have a stochastic cellular structure, and in addition, they often have hyperelastic (i.e., non-linear) mechanical properties. Understanding the 3D structure and the dynamic response of polymer foams to mechanical stress is key to predicting lifetime performance, damage pathways, and stress recovery. Therefore, to gain a more complete picture, experiments which are designed to understand their mechanical properties must simultaneously acquire performance metrics during loading. In situ synchrotron X-ray computed tomography (CT) can image these cellular materials in 3D during uniaxial compression at a 10-2 s-1 strain rate. By utilizing the high X-ray photon flux and high speed camera provided by beamline 2-BM at the Advanced Photon Source (APS), it is possible to collect a full 3D tomogram (900 radiographs as the sample is rotated 180°) within 1 s. Rotating the sample stage in a washing machine motion allows for a 1 s tomogram to be collected every fifth second. In this study, a series of 20 tomograms were collected as the sample was continuously stressed to a nominal 60% compression. Several types of silicone foams with various structures were used to explore this technique. Stress-strain curves, collected simultaneously with the 3D tomograms, can be used to directly correlate the morphology with the mechanical performance and visualize in real-time, the buckling of ligaments. In addition, this method allows for the accurate measurement of the Poisson’s ratio as a function of compression. Coupling this moderate strain rate 3D data with finite element analysis provides a direct comparison between the true mechanical response and the modeled performance and adds a level of robustness that is not possible with other techniques

    15. 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.

    16. 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.

    17. Phase relations in partially molten lower mantle material investigated in-situ by X-ray fluorescence

      NASA Astrophysics Data System (ADS)

      Lo Nigro, G.; Andrault, D.; Petitgirard, S.; Garbarino, G.

      2009-12-01

      It is widely accepted that the early Earth was partially molten due to the high energy dissipated by terrestrial accretion and giant meteoritic impacts. After core formation, subsequent cooling of the magma ocean has led to fractional crystallization of the primitive mantle. Melting relations of silicates have been extensively investigated using the multi-anvil press, for pressures between 3 and 25 GPa [1, 2]. Using the quench technique, it has been shown that the pressure affects significantly the solidus and liquidus curves, and most probably the composition of the eutectic liquid. At higher pressures, the use of laser-heated diamond anvil cell (LH-DAC) technique is required with the intrinsic limitation of very small samples recovered, which gives rise to higher experimental uncertainties for the chemical analysis. We propose a new in-situ method, based on the use of geochemical tracers, to determine the melting relations at lower mantle conditions of pressure and temperature. First, we investigated partial melting up to more than 3000K, for pressures between 25 and up to more than 100 GPa, using LH-DAC coupled with angle dispersive X-ray diffraction at the ID27 beamline of the ESRF [3]. The starting material of chondritic composition resulted in an assemblage of (Mg,Fe)SiO3 perovskite, (Mg,Fe)O ferropericlase and CaSiO3 perovskite. Partial melting was evidenced from (i) disappearance on the 2D diffraction images of sets of diffraction rings representative of a given mineral, (ii) changes in diffraction intensities for the integrated patterns, and (iii) changes in the relation between sample-temperature and laser-power. For a given temperature condition, once partial melting has been evidenced, we kept constant temperature for several minutes in order to enable chemical segregation in the laser power; elements participating to the melt are expected to migrate preferentially and concentrate at the centre of the laser hot spot, while solid species should remain at

    18. X ray attenuation measurements for high-temperature materials characterization and in situ monitoring of damage accumulation

      NASA Astrophysics Data System (ADS)

      Baaklini, George Youssef

      1991-10-01

      The development and application is examined of x ray attenuation measurement systems that are capable of (1) characterizing density variations in high temperature materials, e.g., monolithic ceramics, ceramic and intermetallic matrix composites and (2) noninvasively monitoring damage accumulation and failure sequences in ceramic matrix composites under room temperature tensile testing. Results are presented in the development of (1) a point scan digital radiography system and (2) an in-situ x ray material testing system. The former is used to characterize silicon carbide and silicon nitride specimens and the latter is used to image the failure behavior of silicon carbide fiber reinforced reaction bonded silicon nitride matrix composites. Further, state of the art x ray computed tomography is studied to determine its capabilities and limitations in characterizing density variations of subscale engine components, e.g., a silicon carbide rotor, a silicon nitride blade, and a silicon carbide fiber reinforced beta titanium matrix rod, rotor, and ring. Microfocus radiography, conventional radiography, scanning acoustic microscopy, and metallography are used to substantiate the x ray computed tomography findings. Point scan digital radiography is a viable technique for characterization density variations in monolithic ceramic specimens. But it is very limited and time consuming in characterizing ceramic matrix composities. Precise x ray attenuation measurements, reflecting minute density variations, are achieved by photon counting and by using micro collimators at the source and the detector. X ray computed tomography is found to be a unique x ray attenuation measurement technique capable of providing cross sectional spatial density information in monolithic ceramics and metal matrix composites. X ray computed tomography is proven to accelerate generic composite component development. Radiographic evaluation before, during and after loading show the effect of preexisting

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

      SciTech Connect

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

      2016-08-15

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

    20. 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.

    1. 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.

    2. In-situ X-ray Nanocharacterization of Defect Kinetics in Chalcogenide Solar Cell Materials

      SciTech Connect

      Bertoni, Mariana; Lai, Barry; Masser, Jorg; Buonassisi, Tonio

      2016-09-21

      ) correlate positively, and In negatively with charge collection efficiency for cells with low Ga content, both at grain boundaries and in grain cores. For cells with high Ga content, the charge collection efficiency depends to much lesser extent on the elemental distribution. The objective is three folded: (1) develop an x-ray in-situ microscopy capability to simulate growth and processing conditions, (2) apply it to elucidate performance-governing defect kinetics in chalcogenide solar cell materials, and (3) to study approaches to engineer materials from the nanoscale up. The development of these capabilities will enable experimental characterization to take place under actual processing and operating conditions and it will have impact well beyond the proposed research, enabling future studies on a large variety of materials system where electronic properties depend on underlying structural or chemical inhomogeneities.

    3. Assessment of the effects of laser photobiomodulation on peri-implant bone repair through energy dispersive x-ray fluorescence: A study of dogs

      NASA Astrophysics Data System (ADS)

      Menezes, R. F.; Araújo, N. C.; Carneiro, V. S. M.; Moreno, L. M.; Guerra, L. A. P.; Santos Neto, A. P.; Gerbi, M. E. M.

      2016-03-01

      Bone neoformation is essential in the osteointegration of implants and has been correlated with the repair capacity of tissues, the blood supply and the function of the cells involved. Laser therapy accelerates the mechanical imbrication of peri-implant tissue by increasing osteoblastic activity and inducing ATP, osteopontin and the expression of sialoproteins. Objective: The aim of the present study was to assess peri-implant bone repair using the tibia of dogs that received dental implants and laser irradiation (AsGaAl 830nm - 40mW, CW, f~0.3mm) through Energy Dispersive X-ray Fluorescence (EDXRF). Methodology: Two groups were established: G1 (Control, n=20; two dental implants were made in the tibia of each animal; 10 animals); G2 (Experimental, n=20, two dental implants were made in the tibia each animal + Laser therapy; 10 animals). G2 was irradiated every 48 hours for two weeks, with a total of seven sessions. The first irradiation was conducted during the surgery, at which time a point in the surgical alveolus was irradiated prior to the placement of the implant and four new spatial positions were created to the North, South, East and West (NSEW) of the implant. The subsequent sessions involved irradiation at these four points and at one infra-implant point (in the direction of the implant apex). Each point received 4J/cm2 and a total dose of 20J/cm2 per session (treatment dose=140J/cm2). The specimens were removed 15 and 30 days after the operation for the EDXRF test. The Mann- Whitney statistical test was used to assess the results. Results: The increase in the calcium concentration in the periimplant region of the irradiated specimens (G2) was statistically significant (p < 0.05), when compared with the control group (G1). Conclusion: The results of the present study show that irradiation with the AsGaAl laser promoted an acceleration in bone repair in the peri-implant region.

    4. Chemical Analysis of Reaction Rims on Olivine Crystals in Natural Samples of Black Dacite Using Energy-Dispersive X-Ray Spectroscopy, Lassen Peak, CA.

      NASA Astrophysics Data System (ADS)

      Graham, N. A.

      2014-12-01

      Lassen Volcanic Center is the southernmost volcanic region in the Cascade volcanic arc formed by the Cascadia Subduction Zone. Lassen Peak last erupted in 1915 in an arc related event producing a black dacite material containing xenocrystic olivine grains with apparent orthopyroxene reaction rims. The reaction rims on these olivine grains are believed to have formed by reactions that ensued from a mixing/mingling event that occurred prior to eruption between the admixed mafic andesitic magma and a silicic dacite host material. Natural samples of the 1915 black dacite from Lassen Peak, CA were prepared into 15 polished thin sections and carbon coated for analysis using a FEI Quanta 250 Scanning Electron Microscope (SEM) to identify and measure mineral textures and disequilibrium reaction rims. Observed mineralogical textures related to magma mixing include biotite and amphibole grains with apparent dehydration/breakdown rims, pyroxene-rimmed quartz grains, high concentration of microlites in glass matrix, and pyroxene/amphibole reaction rims on olivine grains. Olivine dissolution is evidenced as increased iron concentration toward convolute edges of olivine grains as observed by Backscatter Electron (BSE) imagery and elemental mapping using NSS spectral imaging software. In an attempt to quantify the area of reaction rim growth on olivine grains within these samples, high-resolution BSE images of 30 different olivine grains were collected along with Energy-Dispersive X-Ray Spectroscopy (EDS) of different phases. Olivine cores and rims were extracted from BSE images using Photoshop and saved as separate image files. ImageJ software was used to calculate the area (μm2) of the core and rim of these grains. Average pyroxene reaction rim width for 30 grains was determined to be 11.68+/-1.65 μm. Rim widths of all 30 grains were averaged together to produce an overall average rim width for the Lassen Peak black dacite. By quantifying the reaction rims on olivine grains

    5. Soft x-ray spectrometer for in situ monitoring of thin-film growth

      NASA Astrophysics Data System (ADS)

      Skytt, Per; Englund, Carl J.; Wassdahl, Nial; Mancini, Derrick C.; Nordgren, Joseph

      1994-11-01

      We have designed and constructed a compact spectrometer dedicated to in-situ characterization of thin films during deposition, using soft x-ray emission spectroscopy. It consists of a Rowland-circle mounted spherical grating and entrance slit, or slit array to enhance throughput. A 2D position-sensitive detector (microchannel plate stack and resistive anode) is mounted tangent to the image of the slit(s) on the Rowland circle. The instrument covers an energy range of 240 - 700 eV using a 300 1/mm grating in the first order. Thus, the spectrometer simultaneously records K emission for low-Z elements C through F, while L emission for 3D metals can be recorded in first or higher orders. The resolution is approximately 300, allowing chemical analysis. Both detector and grating are housed in a vacuum chamber that is turbomolecularly pumped to a pressure below 10(superscript -6) Torr. The instrument can be attached to any process chamber using a standard UHV flange. The slit extends into the process chamber separated from the housing by a valve. This valve can be closed, or in one of two open positions where thin foils serve as vacuum windows to protect the detector and grating, and as filters to reduce background counts from UV light. The spectrometer has successfully monitored a variety of processes in situ, including growth of optical TiN films by reactive magnetron sputter deposition, synchrotron radiation induced CVD of metallic films, and hot-filament CVD growth of diamond.

    6. 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.

    7. Kinetics of methane hydrate decomposition studied via in situ low temperature X-ray powder diffraction.

      PubMed

      Everett, S Michelle; Rawn, Claudia J; Keffer, David J; Mull, Derek L; Payzant, E Andrew; Phelps, Tommy J

      2013-05-02

      Gas hydrate is known to have a slowed decomposition rate at ambient pressure and temperatures below the melting point of ice. As hydrate exothermically decomposes, gas is released and water of the clathrate cages transforms into ice. Based on results from the decomposition of three nominally similar methane hydrate samples, the kinetics of two regions, 180-200 and 230-260 K, within the overall decomposition range 140-260 K, were studied by in situ low temperature X-ray powder diffraction. The kinetic rate constants, k(a), and the reaction mechanisms, n, for ice formation from methane hydrate were determined by the Avrami model within each region, and activation energies, E(a), were determined by the Arrhenius plot. E(a) determined from the data for 180-200 K was 42 kJ/mol and for 230-260 K was 22 kJ/mol. The higher E(a) in the colder temperature range was attributed to a difference in the microstructure of ice between the two regions.

    8. Hydrazine reduction of transition metal oxides - In situ characterization using X-ray photoelectron spectroscopy

      NASA Technical Reports Server (NTRS)

      Littrell, D. M.; Tatarchuk, B. J.

      1986-01-01

      The transition metal oxides (TMOs) V2O5, FeO3, Co3O4, NiO, CuO, and ZnO were exposed to hydrazine at various pressures. The metallic surfaces were surveyed by in situ X-ray photoelectron spectroscopy to determine the irrelative rate of reduction by hydrazine. The most easily reducible oxide, CuO, could be reduced to the metallic state at room temperature and 10 to the -6th torr. The reaction is first order with respect to CuO, with an activation energy of about 35 kJ/mol. Two types of adsorption were seen to occur at 295 K: (1) a reversible component in which the measured N:Cu ratio increased to 0.60 at hydrazine pressures up to 0.5 torr, and (2) an irreversible component, with a N:Cu ratio of 0.28, which could not be removed by extended vacuum pumping. The results of this study are useful for the identification of TMO's that can be used as solid neatallizers of hydrazine spills, and for the preparation of metal surfaces for electroplating and evaporative thin-film coating.

    9. Rapid terrestrial core formation from in situ X-ray computed microtomography

      NASA Astrophysics Data System (ADS)

      Chen, B.; Zhang, D.; Leng, W.; Jackson, J. M.; Wang, Y.; Yu, T.; Liu, J.; Li, J.

      2011-12-01

      The timescale of the terrestrial core formation constrained from the hafnium-tungsten chronometer is within 30 million years after the Solar System formation (e.g. Kleine et al., 2002; Yin et al., 2002). Possible mechanisms for core formation include diapiric instability of iron-rich liquids and percolation of the liquids through the solid silicate matrix. Core-mantle segregation by diapiric instabilities is thought to be a more rapid and efficient core formation process compared with percolation (Stevenson, 1981; Rubie et al., 2007; Golabek et al., 2008). Our experimental results from in situ X-ray computed microtomography show that at 1-1.5 GPa the iron-sulfur and iron-carbon liquids sank through the underlying olivine layer at a speed consistent with the measured core formation timescale. Our three-dimensional tomography data taken at various heating stages revealed that the iron-rich liquid diapirs in olivine induced percolative flow channeling processes, which affects the rheology of olivine and thus facilitates the sinking of iron-rich diapirs. Numerical simulations of diapir sinking based on the tomography observations suggest that the percolative flow channeling process accompanying the iron diapirs could significantly reduce the time for core formation segregation by a factor of 2 or more, depending on the viscosity reduction ratio caused by the percolative flow. Our study sheds new light on core formation processes in the Earth and terrestrial-like planetary bodies, contributing to our understanding of the origin and dynamics of planetary cores.

    10. Strains in Thermally Growing Alumina Films Measured in-situ usingSynchrotron X-rays

      SciTech Connect

      Hou, P.Y.; Paulikas, A.P.; Veal, B.W.

      2006-01-02

      Strains in thermally grown oxides have been measured in-situ, as the oxides develop and evolve. Extensive data have been acquired from oxides grown in air at elevated temperatures on different model alloys that form Al{sub 2}O{sub 3}. Using synchrotron x-rays at the Advanced Photon Source (Beamline 12BM, Argonne National Laboratory), Debye-Scherrer diffraction patterns from the oxidizing specimen were recorded every 5 minutes during oxidation and subsequent cooling. The diffraction patterns were analyzed to determine strains in the oxides, as well as phase changes and the degree of texture. To study a specimen's response to stress perturbation, the oxidizing temperature was quickly cooled from 1100 to 950 C to impose a compressive thermal stress in the scale. This paper describes this new experimental approach and gives examples from oxidized {beta}-NiAl, Fe-20Cr-10Al, Fe-28Al-5Cr and H{sub 2}-annealed Fe-28Al-5Cr (all at. %) alloys to illustrate some current understanding of the development and relaxation of growth stresses in Al{sub 2}O{sub 3}.

    11. In situ X-ray Scattering and Dynamical Modeling of Pd Catalyst Nanoparticles Formed in Flames

      SciTech Connect

      Wang, Juan; Seifert, Sönke; Winans, Randall E.; Tolmachoff, Erik; Xin, Yuxuan; Chen, Dongping; Wang, Hai; Anderson, Scott L.

      2015-08-20

      It has previously been demonstrated that organopalladium precursors can break down under combustion conditions, forming nanoparticles that catalyze ignition. Here, we use in situ small-angle X-ray scattering (SAXS) to probe the formation and growth of palladium nanoparticles in an ethylene fl ame doped with 28 ppm (mol) of Pd(acetate) 2 . The particles appear to nucleate in the fl ame front and are observed by SAXS to grow in size and mass in the high-temperature region of the fl ame ( ~ 2200 K) with median diameters that evolve from 1.5 to 3.0 nm. Transmission electron microscopy of particles collected on a grid located outside the fl ame shows that the particles are metallic palladium with sizes comparable to those determined by SAXS. Molecular dynamics simulation of particles of selected sizes indicates that at the fl ame temperature the particles are molten and the average mass density of the particle material is notably smaller than that of bulk, liquid Pd at the melting point. Both experimental and computational results point to homogeneous nucleation and particle - particle coalescence as mechanisms for particle formation and growth. Aerosol dynamics simulation reproduces the time evolution of the particle size distribution and suggests that a substantial fraction of the particles must be electrically charged during their growth process.

    12. Scanning of Adsorption Hysteresis In Situ with Small Angle X-Ray Scattering

      PubMed Central

      Mitropoulos, Athanasios Ch.; Favvas, Evangelos P.; Stefanopoulos, Konstantinos L.; Vansant, Etienne F.

      2016-01-01

      Everett’s theorem-6 of the domain theory was examined by conducting adsorption in situ with small angle x-ray scattering (SAXS) supplemented by the contrast matching technique. The study focuses on the spectrum differences of a point to which the system arrives from different scanning paths. It is noted that according to this theorem at a common point the system has similar macroscopic properties. Furthermore it was examined the memory string of the system. We concluded that opposite to theorem-6: a) at a common point the system can reach in a finite (not an infinite) number of ways, b) a correction for the thickness of the adsorbed film prior to capillary condensation is necessary, and c) the scattering curves although at high-Q values coincide, at low-Q values are different indicating different microscopic states. That is, at a common point the system holds different metastable states sustained by hysteresis effects. These metastable states are the ones which highlight the way of a system back to a return point memory (RPM). Entering the hysteresis loop from different RPMs different histories are implanted to the paths toward the common point. Although in general the memory points refer to relaxation phenomena, they also constitute a characteristic feature of capillary condensation. Analogies of the no-passing rule and the adiabaticity assumption in the frame of adsorption hysteresis are discussed. PMID:27741263

    13. Rapid thermal processing chamber for in-situ x-ray diffraction

      SciTech Connect

      Ahmad, Md. Imteyaz; Van Campen, Douglas G.; Yu, Jiafan; Pool, Vanessa L.; Van Hest, Maikel F. A. M.; Toney, Michael F.; Fields, Jeremy D.; Parilla, Philip A.; Ginley, David S.

      2015-01-15

      Rapid thermal processing (RTP) is widely used for processing a variety of materials, including electronics and photovoltaics. Presently, optimization of RTP is done primarily based on ex-situ studies. As a consequence, the precise reaction pathways and phase progression during the RTP remain unclear. More awareness of the reaction pathways would better enable process optimization and foster increased adoption of RTP, which offers numerous advantages for synthesis of a broad range of materials systems. To achieve this, we have designed and developed a RTP instrument that enables real-time collection of X-ray diffraction data with intervals as short as 100 ms, while heating with ramp rates up to 100 °Cs{sup −1}, and with a maximum operating temperature of 1200 °C. The system is portable and can be installed on a synchrotron beamline. The unique capabilities of this instrument are demonstrated with in-situ characterization of a Bi{sub 2}O{sub 3}-SiO{sub 2} glass frit obtained during heating with ramp rates 5 °C s{sup −1} and 100 °C s{sup −1}, revealing numerous phase changes.

    14. 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.

    15. In situ X-ray observation and simulation of ratcheting-fatigue interactions in solder joints

      NASA Astrophysics Data System (ADS)

      Shi, Liting; Mei, Yunhui; Chen, Gang; Chen, Xu

      2017-01-01

      Reflow voids created by solder oxidation reduce the reliability of lap joints. In situ visualization of reflow voids in Sn-3Ag-0.5Cu (SAC305) lap-shear solder joints under cyclic stressing was realized by X-ray computed tomography (CT), while the ratcheting deformation of the solder joints was monitored by a non-contact displacement detecting system (NDDS). The results revealed that the shape evolution of reflow voids in solder joints, as characterized by the sphericity of the voids, can be divided into three stages: i.e., the initial stage with a sharp drop, a stable stage, and a rapidly declining stage. A new evolution law for describing the progress of sphericity was proposed, and was further introduced into a viscoplastic constitutive model based on the OW-AF nonlinear kinematic hardening rule. The damage-coupled OW-AF model yielded an accurate estimation of the whole-life ratcheting behavior of Sn-3Ag-0.5Cu (SAC305) lap-shear solder joints. [Figure not available: see fulltext.

    16. Ionic Liquids as a Reference Material Candidate for the Quick Performance Check of Energy Dispersive X-ray Spectrometers for the Low Energy Range below 1 keV

      PubMed Central

      2016-01-01

      Ionic liquids (ILs) are proposed as simple and efficient test materials to evaluate the performance of energy dispersive X-ray spectrometers (EDS) in the low energy range below 1 keV. By only one measurement, C Kα, N Kα, O Kα, and F Kα X-ray lines can be excited. Additionally, the S Kα line at 2.3 keV and, particularly, the S L series at 149 eV complete the picture with X-ray lines offered by the selected ILs. The well-known (certifiable) elemental composition of the ILs selected in the present study can be used to check the accuracy of results produced with the available EDS quantification routines in the low energy range, simultaneously, for several low atomic number elements. A comparison with other reference materials in use for testing the performance of EDS in the low energy range is included. PMID:27336962

    17. Distinct charge dynamics in battery electrodes revealed by in situ and operando soft X-ray spectroscopy

      PubMed Central

      Liu, Xiaosong; Wang, Dongdong; Liu, Gao; Srinivasan, Venkat; Liu, Zhi; Hussain, Zahid; Yang, Wanli

      2013-01-01

      Developing high-performance batteries relies on material breakthroughs. During the past few years, various in situ characterization tools have been developed and have become indispensible in studying and the eventual optimization of battery materials. However, soft X-ray spectroscopy, one of the most sensitive probes of electronic states, has been mainly limited to ex situ experiments for battery research. Here we achieve in situ and operando soft X-ray absorption spectroscopy of lithium-ion battery cathodes. Taking advantage of the elemental, chemical and surface sensitivities of soft X-rays, we discover distinct lithium-ion and electron dynamics in Li(Co1/3Ni1/3Mn1/3)O2 and LiFePO4 cathodes in polymer electrolytes. The contrast between the two systems and the relaxation effect in LiFePO4 is attributed to a phase transformation mechanism, and the mesoscale morphology and charge conductivity of the electrodes. These discoveries demonstrate feasibility and power of in situ soft X-ray spectroscopy for studying integrated and dynamic effects in batteries. PMID:24100759

    18. Distinct charge dynamics in battery electrodes revealed by in situ and operando soft X-ray spectroscopy.

      PubMed

      Liu, Xiaosong; Wang, Dongdong; Liu, Gao; Srinivasan, Venkat; Liu, Zhi; Hussain, Zahid; Yang, Wanli

      2013-01-01

      Developing high-performance batteries relies on material breakthroughs. During the past few years, various in situ characterization tools have been developed and have become indispensible in studying and the eventual optimization of battery materials. However, soft X-ray spectroscopy, one of the most sensitive probes of electronic states, has been mainly limited to ex situ experiments for battery research. Here we achieve in situ and operando soft X-ray absorption spectroscopy of lithium-ion battery cathodes. Taking advantage of the elemental, chemical and surface sensitivities of soft X-rays, we discover distinct lithium-ion and electron dynamics in Li(Co(¹/₃)Ni(¹/₃)Mn(¹/₃))O₂ and LiFePO₄ cathodes in polymer electrolytes. The contrast between the two systems and the relaxation effect in LiFePO₄ is attributed to a phase transformation mechanism, and the mesoscale morphology and charge conductivity of the electrodes. These discoveries demonstrate feasibility and power of in situ soft X-ray spectroscopy for studying integrated and dynamic effects in batteries.

    19. Recent progress on synchrotron-based in-situ soft X-ray spectroscopy for energy materials.

      PubMed

      Liu, Xiaosong; Yang, Wanli; Liu, Zhi

      2014-12-10

      Soft X-ray spectroscopy (SXS) techniques such as photoelectron spectroscopy, soft X-ray absorption spectroscopy and X-ray emission spectroscopy are efficient and direct tools to probe electronic structures of materials. Traditionally, these surface sensitive soft X-ray techniques that detect electrons or photons require high vacuum to operate. Many recent in situ instrument developments of these techniques have overcome this vacuum barrier. One can now study many materials and model devices under near ambient, semi-realistic, and operando conditions. Further developments of integrating the realistic sample environments with efficient and high resolution detection methods, particularly at the high brightness synchrotron light sources, are making SXS an important tool for the energy research community. In this progress report, we briefly describe the basic concept of several SXS techniques and discuss recent development of SXS instruments. We then present several recent studies, mostly in situ SXS experiments, on energy materials and devices. Using these studies, we would like to highlight that the integration of SXS and in situ environments can provide in-depth insight of material's functionality and help researchers in new energy material developments. The remaining challenges and critical research directions are discussed at the end. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

    20. Design and Operation of an In Situ High Pressure Reaction Cell for X-Ray Absorption Spectroscopy

      NASA Astrophysics Data System (ADS)

      Bare, Simon R.; Yang, N.; Kelly, S. D.; Mickelson, G. E.; Modica, F. S.

      2007-02-01

      The design and initial operation of an in situ catalysis reaction cell for x-ray absorption spectroscopy measurements at high pressure is described. The design is based on an x-ray transparent tube fabricated from beryllium. This forms a true plug flow reactor for catalysis studies. The reactor is coupled to a portable microprocessor-controlled versatile feed system, and incorporates on-line analysis of reaction products. XAFS data recorded during the reduction of a NiRe/carbon catalyst at 4 bar are used to illustrate the performance of the reactor.

    1. In situ X-ray diffraction based investigation of crystallization in solution deposited PZT thin films

      NASA Astrophysics Data System (ADS)

      Nittala, Krishna

      Solution deposited PZT based thin films have potential applications in embedded decoupling capacitors and pulse discharge capacitors. During solution deposition, precursor solution is deposited onto a substrate to obtain an amorphous film. The film is then crystallized by heating it at a high temperature (˜600 - 700°C). Conditions during the crystallization anneal such as precursor stoichiometry in solution, heating rate and adhesion layer in the substrate are known to influence phase and texture evolution in these films. However, a mechanistic understanding of the changes taking place in these thin films during crystallization is lacking. A better understanding of the crystallization processes in these thin films could enable tailoring the properties of thin films to suit specific applications. To explore the crystallization process in solution deposited PZT thin films, high temperature in situ laboratory and synchrotron X-ray diffraction based techniques were developed. Taking advantage of the high X-ray flux available at synchrotron facilities such as beamline 6-ID-B, Advanced Photon Source, Argonne National Laboratory, crystalline phases formed in the thin films during crystallization at the high heating rates (0.5 -- 60°C/s) typically used during film processing could be measured. Using a 2-D detector for these measurements allowed the simultaneous measurement of both phase and texture information during crystallization. Analytical treatment of the unconventional diffraction geometry used during the synchrotron based measurements was performed to develop methodologies for quantitative estimation of texture components. The nominal lead content in the starting solutions and the heating rate used during crystallization was observed to influence the sequence of phases formed during crystallization of the films. In films crystallized at fast heating rates, titanium segregation, probably due to diffusion of titanium from the adhesion layer, was observed. To

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

      SciTech Connect

      Shade, Paul A. Schuren, Jay C.; Turner, Todd J.; Blank, Basil; Kenesei, Peter; Goetze, Kurt; Lienert, Ulrich; Almer, Jonathan; Suter, Robert M.; Bernier, Joel V.; Li, Shiu Fai; Lind, Jonathan

      2015-09-15

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

    3. Geological Carbon Sequestration: new insights from in-situ Synchrotron X-ray Microtomography

      NASA Astrophysics Data System (ADS)

      Voltolini, M.; Kwon, T.; Ajo Franklin, J. B.

      2012-12-01

      In a world with rapidly increasing atmospheric CO2 concentrations, a variety of scalable technologies are being considered to mitigate emissions from the combustion of fossil fuels; among these approaches, geological carbon storage (GCS) is being actively tested at a variety of subsurface sites. Despite these activities, a mechanistic understanding of multiphase flow in scCO2/brine systems at the pore scale is still being developed. The distribution of scCO2 in the pore space controls a variety of processes at the continuum scale including CO2 dissolution rate (by way of brine/CO2 contact area), capillary trapping, and residual brine fraction. Virtually no dynamic measurements of the pore-scale distribution of scCO2 in real geological samples have been made in three dimensions leaving models describing multi-phase fluid dynamics, reactive transport, and geophysical properties reliant on analog systems (often using fewer spatial dimensions, different fluids, or lower pressures) or theoretical models describing phase configurations. We present dynamic pore-scale imagery of scCO2 invasion dynamics in a 3D geological sample, in this case a quartz-rich sandstone core extracted from the Domengine Fm, a regionally extensive unit which is currently a target for future GCS operations in the Sacramento Basin. This dataset, acquired using synchrotron X-ray micro tomography (SXR-μCT) and high speed radiography, was made possible by development of a controlled P/T flow-through triaxial cell compatible with X-ray imaging in the 8-40 keV range. These experiments successfully resolved scCO2 and brine phases at a spatial resolution of 4.47 μm while the sample was kept at in situ conditions (45°C, 9 MPa pore pressure, 14 MPa hydrostatic confining stress) during drainage and imbibition cycles. Image volumes of the dry, brine saturated, and partially scCO2 saturated sample were captured and were used to correlate aspects of rock microstructure to development of the invasion front

    4. In situ flow cell for combined X-ray absorption spectroscopy, X-ray diffraction, and mass spectrometry at high photon energies under solar thermochemical looping conditions

      NASA Astrophysics Data System (ADS)

      Rothensteiner, Matthäus; Jenni, Joel; Emerich, Hermann; Bonk, Alexander; Vogt, Ulrich F.; van Bokhoven, Jeroen A.

      2017-08-01

      An in situ/operando flow cell for transmission mode X-ray absorption spectroscopy (XAS), X-ray diffraction (XRD), and combined XAS/XRD measurements in a single experiment under the extreme conditions of two-step solar thermochemical looping for the dissociation of water and/or carbon dioxide was developed. The apparatus exposes materials to relevant conditions of both the auto-reduction and the oxidation sub-steps of the thermochemical cycle at ambient temperature up to 1773 K and enables determination of the composition of the effluent gases by online quadrupole mass spectrometry. The cell is based on a tube-in-tube design and is heated by means of a focusing infrared furnace. It was tested successfully for carbon dioxide splitting. In combined XAS/XRD experiments with an unfocused beam, XAS measurements were performed at the Ce K edge (40.4 keV) and XRD measurements at 64.8 keV and 55.9 keV. Furthermore, XRD measurements with a focused beam at 41.5 keV were carried out. Equimolar ceria-hafnia was auto-reduced in a flow of argon and chemically reduced in a flow of hydrogen/helium. Under reducing conditions, all cerium(iv) was converted to cerium(iii) and a cation-ordered pyrochlore-type structure was formed, which was not stable upon oxidation in a flow of carbon dioxide.

    5. High pressure and high temperature in situ X-ray diffraction studies in the Paris-Edinburgh cell using a laboratory X-ray source†

      NASA Astrophysics Data System (ADS)

      Toulemonde, Pierre; Goujon, Céline; Laversenne, Laetitia; Bordet, Pierre; Bruyère, Rémy; Legendre, Murielle; Leynaud, Olivier; Prat, Alain; Mezouar, Mohamed

      2014-04-01

      We have developed a new laboratory experimental set-up to study in situ the pressure-temperature phase diagram of a given pure element or compound, its associated phase transitions, or the chemical reactions involved at high pressure and high temperature (HP-HT) between different solids and liquids. This new tool allows laboratory studies before conducting further detailed experiments using more brilliant synchrotron X-ray sources or before kinetic studies. This device uses the diffraction of X-rays produced by a quasi-monochromatic micro-beam source operating at the silver radiation (λ(Ag)Kα 1, 2≈0.56 Å). The experimental set-up is based on a VX Paris-Edinburgh cell equipped with tungsten carbide or sintered diamond anvils and uses standard B-epoxy 5 or 7 mm gaskets. The diffracted signal coming from the compressed (and heated) sample is collected on an image plate. The pressure and temperature calibrations were performed by diffraction, using conventional calibrants (BN, NaCl and MgO) for determination of the pressure, and by crossing isochores of BN, NaCl, Cu or Au for the determination of the temperature. The first examples of studies performed with this new laboratory set-up are presented in the article: determination of the melting point of germanium and magnesium under HP-HT, synthesis of MgB2 or C-diamond and partial study of the P, T phase diagram of MgH2.

    6. Shock Melting of Iron Silicide as Determined by In Situ X-ray Diffraction.

      NASA Astrophysics Data System (ADS)

      Newman, M.; Kraus, R. G.; Wicks, J. K.; Smith, R.; Duffy, T. S.

      2016-12-01

      The equation of state of core alloys at pressures and temperatures near the solid-liquid coexistence curve is important for understanding the dynamics at the inner core boundary of the Earth and super-Earths. Here, we present a series of laser driven shock experiments on textured polycrystalline Fe-15Si. These experiments were conducted at the Omega and Omega EP laser facilities. Particle velocities in the Fe-15Si samples were measured using a line VISAR and were used to infer the thermodynamic state of the shocked samples. In situ x-ray diffraction measurements were used to probe the melting transition and investigate the potential decomposition of Fe-15Si in to hcp and B2 structures. This work examines the kinetic effects of decomposition due to the short time scale of dynamic compression experiments. In addition, the thermodynamic data collected in these experiments adds to a limited body of information regarding the equation of state of Fe-15Si, which is a candidate for the composition in Earth's outer core. Our experimental results show a highly textured solid phase upon shock compression to pressures ranging from 170 to 300 GPa. Below 320 GPa, we observe diffraction peaks consistent with decomposition of the D03 starting material in to an hcp and a cubic (potentially B2) structure. Upon shock compression above 320 GPa, the intense and textured solid diffraction peaks give way to diffuse scattering and loss of texture, consistent with melting along the Hugoniot. When comparing these results to that of pure iron, we can ascertain that addition of 15 wt% silicon increases the equilibrium melting temperature significantly, or that the addition of silicon significantly increases the metastability of the solid phase, relative to the liquid. This work was performed under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344.

    7. Evolution of magma textures during deformation: Insights from in situ X-ray tomography experiments

      NASA Astrophysics Data System (ADS)

      Degruyter, W.; Cordonnier, B.; Manga, M.; Haboub, A.; Andrews, B. J.; Dennen, R. L.; MacDowell, A.; Parkinson, D. Y.

      2012-12-01

      Pyroclasts provide snapshots of the state of the magma at fragmentation or emplacement. Their textures record the deformation and degassing magma underwent prior to quenching. Understanding the link between the final texture and the processes that created them requires experimental reproduction of volcanic conditions under constrained parameters. Technological advances at the X-ray tomography beamline at the Advanced Light Source, Lawrence Berkeley National Laboratory have now made it possible to visualize magma in 3D as it is being deformed at high temperature, which allows us to visualize and quantify the processes that form pyroclasts. We use a fast readout camera that allows tomography on a few minutes timescale in combination with a high temperature uni-axial apparatus transparent to tomography. We heated obsidian samples from Big Glass Mountain, California and andesitic glass from Pahoa, California at various temperatures up to 1400 K. After an initial foaming stage, the samples were subjected to pure shear flow at strain-rates varying between 10-6 s-1 and 10-2 s-1. Magma rheology measurements in the past have typically been restricted to bulk measurements and visualization before and after the experiment. This limits the ability to interpret the measured relationship between stress and strain-rate and the evolution of texture. The in situ scanning allows us to track the deformation or relaxation of individual bubbles, development of strain localization, crack initiation and makes it possible to directly correlate these processes to the bulk measurements of stress and strain. These new measurements will improve the interpretation of the textures found within the products produced by volcanic eruptions.

    8. Design and Operation of a High Pressure Reaction Cell for in situ X-ray Absorption Spectroscopy

      SciTech Connect

      Bare,S.; Yang, N.; Kelly, S.; Mickelson, G.; Modica, F.

      2007-01-01

      X-ray absorption spectroscopy measurements of catalytic reactions have been instrumental in advancing the understanding of catalytic processes. These measurements require an in situ catalysis reaction cell with unique properties. Here we describe the design and initial operation of an in situ/operando catalysis reaction cell for transmission X-ray absorption spectroscopy measurements. The cell is designed: to be an ideal catalytic reactor with no mass transfer effects; to give the same conversion and selectivity under similar space velocities as standard laboratory micro-reactors; to be operational temperatures up to 600 {sup o}C and pressures up to 14 bar; to be X-ray transparent allowing XAS measurement to be collected in transmission for all elements with Z {>=} 23 (vanadium K-edge at 5.5 keV); to measure the actual catalyst bed temperature; to not use o-ring seals, or water cooling; to be robust, compact, easy to assemble, and use, and relatively low cost to produce. The heart of the cell is fabricated from an X-ray transparent beryllium tube that forms a plug flow reactor. XAFS data recorded during the reduction of a Re/{gamma}-A{sub 2}O{sub 3} catalyst as a function of hydrogen pressure from 0.05 to 8 bar, and from a Pt-Sn/{gamma}-A{sub 2}O{sub 3} catalyst during n-heptane reforming are given as initial examples of the versatility of the reactor.

    9. 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

      2016-01-05

      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. Finally, 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.

    10. In situ synchrotron x-ray spectroscopy of ruthenium nanoparticles modified with selenium for an oxygen reduction reaction.

      SciTech Connect

      Inukai, J.; Cao, D.; Wieckowski, A.; Chang, K.-C.; Menzel, A.; Komanicky, V.; You, H.; Univ. Illinois; Univ. Yamanashi

      2007-11-15

      We used in situ Se K-edge X-ray spectroscopy to characterize Ru nanoparticles chemically modified with submonolayers of selenium (Se/Ru) [Cao et al. J. Electrochem. Soc. 2006, 153, A869]. X-ray powder diffraction verified that the Se/Ru catalyst had metallic Ru cores. The in situ X-ray absorption near edge structure taken at the open circuit potential showed that there were both elemental and oxidized selenium on the as-prepared Se/Ru samples. All selenium oxide was reduced to the elemental form of selenium by applying negative potentials. By applying positive potentials, selenium was subsequently reoxidized. The analysis of the extended X-ray absorption fine structure shows the appearance of selenium hydration (Se-OH{sub 2}) in a deaerated solution, which was not observed during the oxygen reduction reaction. We present evidence that Se-free Ru atoms play an important role in the ORR activity of the Se/Ru catalyst studied in this paper.

    11. In-situ synchrotron x-ray spectroscopy of ruthenium nanoparticles modified with selenium for oxygen reduction reaction.

      SciTech Connect

      Inukai, J.; Cao, D.; Wieckowski, A.; Chang, K.-C.; Menzel, A.; Komanicky, V.; You, H.; Materials Science Division; Univ. of Illinois; Univ. of Yamanashi

      2007-11-15

      We used in situ Se K-edge X-ray spectroscopy to characterize Ru nanoparticles chemically modified with submonolayers of selenium (Se/Ru) [Cao et al. J. Electrochem. Soc. 2006, 153, A869]. X-ray powder diffraction verified that the Se/Ru catalyst had metallic Ru cores. The in situ X-ray absorption near edge structure taken at the open circuit potential showed that there were both elemental and oxidized selenium on the as-prepared Se/Ru samples. All selenium oxide was reduced to the elemental form of selenium by applying negative potentials. By applying positive potentials, selenium was subsequently reoxidized. The analysis of the extended X-ray absorption fine structure shows the appearance of selenium hydration (Se-OH{sub 2}) in a deaerated solution, which was not observed during the oxygen reduction reaction. We present evidence that Se-free Ru atoms play an important role in the ORR activity of the Se/Ru catalyst studied in this paper.

    12. Reactive sputter magnetron reactor for preparation of thin films and simultaneous in situ structural study by X-ray diffraction.

      PubMed

      Bürgi, J; Neuenschwander, R; Kellermann, G; García Molleja, J; Craievich, A F; Feugeas, J

      2013-01-01

      The purpose of the designed reactor is (i) to obtain polycrystalline and∕or amorphous thin films by controlled deposition induced by a reactive sputtering magnetron and (ii) to perform a parallel in situ structural study of the deposited thin films by X-ray diffraction, in real time, during the whole growth process. The designed reactor allows for the control and precise variation of the relevant processing parameters, namely, magnetron target-to-sample distance, dc magnetron voltage, and nature of the gas mixture, gas pressure and temperature of the substrate. On the other hand, the chamber can be used in different X-ray diffraction scanning modes, namely, θ-2θ scanning, fixed α-2θ scanning, and also low angle techniques such as grazing incidence small angle X-ray scattering and X-ray reflectivity. The chamber was mounted on a standard four-circle diffractometer located in a synchrotron beam line and first used for a preliminary X-ray diffraction analysis of AlN thin films during their growth on the surface of a (100) silicon wafer.

    13. Evaluation of dual energy x-ray absorptiometry for in situ measurement of bone mineral density of equine metacarpi.

      PubMed

      McClure, S R; Glickman, L T; Glickman, N W; Weaver, C M

      2001-05-01

      To determine the accuracy and precision of dual energy x-ray absorptiometry (DEXA) for measuring bone mineral density in horses in situ. Sample Population-12 randomly selected forelimbs from 12 horses. Metacarpi were scanned in 2 planes and DEXA measurements obtained for 6 regions of interest (ROI). Each ROI was isolated and bone density measured by Archimedes' principle. Linear regression analysis was used to determine the correlation between the 2 measurements at each ROI. An additional metacarpus was measured 10 times to determine the coefficient of variation for both techniques. Dual energy x-ray absorptiometry and bone density were significantly associated at multiple ROI. The addition of age, weight, and soft tissue or bone thickness improved these associations. Repeated measurements had a low coefficient of variation. Dual energy x-ray absorptiometry can be used to accurately and precisely measure the bone density in the equine metacarpus. Dual energy x-ray absorptiometry appears suitable for serial in vivo measurement of bone density of the equine metacarpus. Dual energy x-ray absorptiometry may be used for studies to evaluate the effects of diet or drugs on bone density or density changes from bone remodeling that develop prior to stress fractures.

    14. Characterization of toners and inkjets by laser ablation spectrochemical methods and Scanning Electron Microscopy-Energy Dispersive X-ray Spectroscopy

      NASA Astrophysics Data System (ADS)

      Trejos, Tatiana; Corzo, Ruthmara; Subedi, Kiran; Almirall, José

      2014-02-01

      Detection and sourcing of counterfeit currency, examination of counterfeit security documents and determination of authenticity of medical records are examples of common forensic document investigations. In these cases, the physical and chemical composition of the ink entries can provide important information for the assessment of the authenticity of the document or for making inferences about common source. Previous results reported by our group have demonstrated that elemental analysis, using either Laser Ablation-Inductively Coupled Plasma-Mass Spectrometry (LA-ICP-MS) or Laser Ablation Induced Breakdown Spectroscopy (LIBS), provides an effective, practical and robust technique for the discrimination of document substrates and writing inks with minimal damage to the document. In this study, laser-based methods and Scanning Electron Microscopy-Energy Dispersive X-Ray Spectroscopy (SEM-EDS) methods were developed, optimized and validated for the forensic analysis of more complex inks such as toners and inkjets, to determine if their elemental composition can differentiate documents printed from different sources and to associate documents that originated from the same printing source. Comparison of the performance of each of these methods is presented, including the analytical figures of merit, discrimination capability and error rates. Different calibration strategies resulting in semi-quantitative and qualitative analysis, comparison methods (match criteria) and data analysis and interpretation tools were also developed. A total of 27 black laser toners originating from different manufacturing sources and/or batches were examined to evaluate the discrimination capability of each method. The results suggest that SEM-EDS offers relatively poor discrimination capability for this set (~ 70.7% discrimination of all the possible comparison pairs or a 29.3% type II error rate). Nonetheless, SEM-EDS can still be used as a complementary method of analysis since it has

    15. A modular reactor design for in situ synchrotron x-ray investigation of atomic layer deposition processes

      SciTech Connect

      Klug, Jeffrey A. Emery, Jonathan D.; Martinson, Alex B. F.; Proslier, Thomas; Weimer, Matthew S.; Yanguas-Gil, Angel; Elam, Jeffrey W.; Seifert, Sönke; Schlepütz, Christian M.; Hock, Adam S.

      2015-11-15

      Synchrotron characterization techniques provide some of the most powerful tools for the study of film structure and chemistry. The brilliance and tunability of the Advanced Photon Source allow access to scattering and spectroscopic techniques unavailable with in-house laboratory setups and provide the opportunity to probe various atomic layer deposition (ALD) processes in situ starting at the very first deposition cycle. Here, we present the design and implementation of a portable ALD instrument which possesses a modular reactor scheme that enables simple experimental switchover between various beamlines and characterization techniques. As first examples, we present in situ results for (1) X-ray surface scattering and reflectivity measurements of epitaxial ZnO ALD on sapphire, (2) grazing-incidence small angle scattering of MnO nucleation on silicon, and (3) grazing-incidence X-ray absorption spectroscopy of nucleation-regime Er{sub 2}O{sub 3} ALD on amorphous ALD alumina and single crystalline sapphire.

    16. In situ X-ray diffraction monitoring of a mechanochemical reaction reveals a unique topology metal-organic framework

      NASA Astrophysics Data System (ADS)

      Katsenis, Athanassios D.; Puškarić, Andreas; Štrukil, Vjekoslav; Mottillo, Cristina; Julien, Patrick A.; Užarević, Krunoslav; Pham, Minh-Hao; Do, Trong-On; Kimber, Simon A. J.; Lazić, Predrag; Magdysyuk, Oxana; Dinnebier, Robert E.; Halasz, Ivan; Friščić, Tomislav

      2015-03-01

      Chemical and physical transformations by milling are attracting enormous interest for their ability to access new materials and clean reactivity, and are central to a number of core industries, from mineral processing to pharmaceutical manufacturing. While continuous mechanical stress during milling is thought to create an environment supporting nonconventional reactivity and exotic intermediates, such speculations have remained without proof. Here we use in situ, real-time powder X-ray diffraction monitoring to discover and capture a metastable, novel-topology intermediate of a mechanochemical transformation. Monitoring the mechanochemical synthesis of an archetypal metal-organic framework ZIF-8 by in situ powder X-ray diffraction reveals unexpected amorphization, and on further milling recrystallization into a non-porous material via a metastable intermediate based on a previously unreported topology, herein named katsenite (kat). The discovery of this phase and topology provides direct evidence that milling transformations can involve short-lived, structurally unusual phases not yet accessed by conventional chemistry.

    17. A modular reactor design for in situ synchrotron X-ray investigation of atomic layer deposition processes

      SciTech Connect

      Klug, Jeffrey A.; Weimer, Matthew S.; Emery, Jonathan D.; Yanguas-Gil, Angel; Seifert, Sonke; Schleputz, Christian M.; Martinson, Alex B. F.; Elam, Jeffrey W.; Hock, Adam S.; Proslier, Thomas

      2015-11-01

      Synchrotron characterization techniques provide some of the most powerful tools for the study of film structure and chemistry. The brilliance and tunability of the Advanced Photon Source allow access to scattering and spectroscopic techniques unavailable with in-house laboratory setups and provide the opportunity to probe various atomic layer deposition (ALD) processes in situ starting at the very first deposition cycle. Here, we present the design and implementation of a portable ALD instrument which possesses a modular reactor scheme that enables simple experimental switchover between various beamlines and characterization techniques. As first examples, we present \\textit{in situ} results for 1.) X-ray surface scattering and reflectivity measurements of epitaxial ZnO ALD on sapphire, 2.) grazing-incidence small angle scattering of MnO nucleation on silicon, and 3.) grazing-incidence X-ray absorption spectroscopy of nucleation-regime Er2O3 ALD on amorphous ALD alumina and single crystalline sapphire.

    18. Quantifying the Nucleation and Growth Kinetics of Microwave Nanochemistry Enabled by in Situ High-Energy X-ray Scattering.

      PubMed

      Liu, Qi; Gao, Min-Rui; Liu, Yuzi; Okasinski, John S; Ren, Yang; Sun, Yugang

      2016-01-13

      The fast reaction kinetics presented in the microwave synthesis of colloidal silver nanoparticles was quantitatively studied, for the first time, by integrating a microwave reactor with in situ X-ray diffraction at a high-energy synchrotron beamline. Comprehensive data analysis reveals two different types of reaction kinetics corresponding to the nucleation and growth of the Ag nanoparticles. The formation of seeds (nucleation) follows typical first-order reaction kinetics with activation energy of 20.34 kJ/mol, while the growth of seeds (growth) follows typical self-catalytic reaction kinetics. Varying the synthesis conditions indicates that the microwave colloidal chemistry is independent of concentration of surfactant. These discoveries reveal that the microwave synthesis of Ag nanoparticles proceeds with reaction kinetics significantly different from the synthesis present in conventional oil bath heating. The in situ X-ray diffraction technique reported in this work is promising to enable further understanding of crystalline nanomaterials formed through microwave synthesis.

    19. X-ray photochemical alteration of planetary samples during in situ micro-XRF analysis

      NASA Astrophysics Data System (ADS)

      Flannery, D. T.; Tuite, M. L., Jr.; Hodyss, R. P.; Allwood, A.; Bhartia, R.; Abbey, W. J.; Williford, K. H.

      2015-12-01

      PIXL (Planetary Instrument for X-ray Lithochemistry; selected for the Mars 2020 mission contact science payload) uses a polycapillary to focus X-rays to a ~100 μm spot on sample surfaces, providing higher spatial resolution, higher X-ray flux, and higher fluorescence counts compared to previously flown planetary XRF instruments. Photochemical changes in organic materials occurring during investigations employing x-rays have been reported, particularly for biological samples examined in synchrotrons (e.g. George et al., J. Synchrotron Radiation, 19:875-876). However, little is known about the effect energies and fluxes typical to micro-XRF instruments may have on the organic molecules that are commonly preserved in rocks and sediments. In particular, it is essential to understand the effect of micro-XRF on organics preserved near surfaces that are later subjected to contact science that focuses on organic geochemistry (e.g. UV Raman/fluorescence instruments). We report results of an investigation in which samples containing organic molecules were exposed to X-ray energies and fluxes typical to micro-XRF. Samples containing alkanes and polycyclic aromatic hydrocarbons were characterized by GC-MS and UV Raman/fluorescence before being subjected to various X-ray energies and fluxes typical of PIXL. Following x-ray irradiation, samples were again characterized by GC-MS and UV Raman/fluorescence in order to characterize photochemical effects.

    20. Time-resolved and in-situ X-ray scattering methods beyond photoactivation: Utilizing high-flux X-ray sources for the study of ubiquitous non-photoactive proteins.

      PubMed

      Jain, Rohit; Techert, Simone

      2016-01-01

      X-ray scattering technique, comprising of small-angle/wide-angle X-ray scattering (SAXS/WAXS) techniques is increasingly used to characterize the structure and interactions of biological macromolecules and their complexes in solution. It is a method of choice to characterize the flexible, partially folded and unfolded protein systems. X-ray scattering is the last resort for proteins that cannot be investigated by crystallography or NMR and acts as a complementary technique with different biophysical techniques to answer challenging scientific questions. The marriage of the X-ray scattering technique with the fourth dimension "time" yields structural dynamics and kinetics information for protein motions in hierarchical timescales from picoseconds to days. The arrival of the high-flux X-ray beam at third generation synchrotron sources, exceptional X-ray optics, state-of-the-art detectors, upgradation of X-ray scattering beamlines with microfluidics devices and advanced X-ray scattering data analysis procedures are the important reasons behind the shining years of X-ray scattering technique. The best days of the X-ray scattering technique are on the horizon with the advent of the nanofocus X-ray scattering beamlines and fourth generation X-ray lightsources, i.e., free electron lasers (XFELs). Complementary to the photon-triggered time-resolved X-ray scattering techniques, we will present an overview of the time-resolved and in-situ X-ray scattering techniques for structural dynamics of ubiquitous non-photoactive proteins.

    1. [Energy dispersive x-ray fluorescence spectrometry--a forensic chemistry method for detection of bullet metal residue in gunshot wounds].

      PubMed

      Havel, J; Zelenka, K

      2003-04-01

      The article describes using of energo-dispersive X-ray fluorescence spectrometry (EDXRF) as the forensic method as the tool for detection of metals (gunshot residues--GSR) in connection with gunshot-wounds of persons.

    2. In situ x-ray microscopic observation of the electromigration in passivated Cu interconnects

      NASA Astrophysics Data System (ADS)

      Schneider, G.; Hambach, D.; Niemann, B.; Kaulich, B.; Susini, J.; Hoffmann, N.; Hasse, W.

      2001-03-01

      X-ray imaging of electromigration in a passivated Cu interconnect was performed with 100-nm spatial resolution. A time sequence of 200 images, recorded with the European Synchrotron Radiation Facility x-ray microscope in 2.2 h at 4 keV photon energy, visualizes the mass flow of Cu at current densities up to 2×107 A/cm2. Due to the high penetration power through matter and the element specific image contrast, x-ray microscopy is a unique tool for time-resolved, quantitative mass transport measurements in interconnects. Model calculations predict that failures in operating microprocessors are detectable with 30 nm resolution by nanotomography.

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

      NASA Astrophysics Data System (ADS)

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

      2014-02-01

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

    4. In Situ Grazing Incidence X-Ray Diffraction Study of Electrochemically Deposited Pb Monolayer on Ag(111),

      DTIC Science & Technology

      1987-05-12

      potential for the deposition of Pb2 on a Pb electrode and hence is termed underpotential deposition (UPD). 19 No additional lead is deposited until...K. 0 In Situ Grazing Incidence X-ray Diffraction Study Interim Technical Report of Electrochemically Deposited Pb rMbno layers on...nunoalayer adsorbed at a metal-liquid interface. Diffraction peaks were * ~. observed from a monoalayer of lead electrochemicially deposited onto a

    5. Monitoring potassium metal electrodeposition from an ionic liquid using in situ electrochemical-X-ray photoelectron spectroscopy

      NASA Astrophysics Data System (ADS)

      Wibowo, Rahmat; Aldous, Leigh; Jacobs, Robert M. J.; Manan, Ninie S. A.; Compton, Richard G.

      2011-06-01

      The real time electrodeposition of potassium has been monitored for the first time in an ionic liquid using in situ electrodeposition-X-ray photoelectron spectroscopy (XPS). The ionic liquid used was N-butyl- N-methylpyrrolidinium bis(trifluoromethylsulfonyl)imide ([C 4mpyrr][ NTf 2]), and electrodeposition occurred at a nickel mesh electrode. Potassium electrochemistry was monitored at the ionic liquid-vacuum-electrode interface using a novel cell design.

    6. A flow cell for in situ synchrotron x-ray diffraction studies of scale formation under Bayer processing conditions

      NASA Astrophysics Data System (ADS)

      Webster, Nathan A. S.; Madsen, Ian C.; Loan, Melissa J.; Scarlett, Nicola V. Y.; Wallwork, Kia S.

      2009-08-01

      The design, construction, and commissioning of a stainless steel flow cell for in situ synchrotron x-ray diffraction studies of scale formation under Bayer processing conditions is described. The use of the cell is demonstrated by a study of Al(OH)3 scale formation on a mild steel substrate from synthetic Bayer liquor at 70 °C. The cell design allows for interchangeable parts and substrates and would be suitable for the study of scale formation in other industrial processes.

    7. In situ X-ray powder diffraction, synthesis, and magnetic properties of InVO{sub 3}

      SciTech Connect

      Lundgren, Rylan J.; Cranswick, Lachlan M.D.; Bieringer, Mario . E-mail: Mario_Bieringer@umanitoba.ca

      2006-12-15

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

    8. In-situ X-ray CT results of damage evolution in L6 ordinary chondrite meteorites

      SciTech Connect

      Cuadra, Jefferson A.; Hazeli, Kavan; Ramesh, K. T.; Martz, Harry

      2016-06-17

      These are slides about in-situ X-ray CT results of damage evolution in L6 ordinary chondrite meteorites. The following topics are covered: mechanical and thermal damage characterization, list of Grosvenor Mountain (GRO) meteorite samples, in-situ x-ray compression test setup, GRO-chipped reference at 0 N - existing cracks, GRO-chipped loaded at 1580 N, in-situ x-ray thermal fatigue test setup, GRO-B14 room temperature reference, GRO-B14 Cycle 47 at 200°C, GRO-B14 Cycle 47 at room temperature, conclusions from qualitative analysis, future work and next steps. Conclusions are the following: Both GRO-Chipped and GRO-B14 had existing voids and cracks within the volume. These sites with existing damage were selected for CT images from mechanically and thermally loaded scans since they are prone to damage initiation. The GRO-Chipped sample was loaded to 1580 N which resulted in a 14% compressive engineering strain, calculated using LVDT. Based on the CT cross sectional images, the GRO-B14 sample at 200°C has a thermal expansion of approximately 96 μm in height (i.e. ~1.6% engineering strain).

    9. In Situ Ptychography of Heterogeneous Catalysts using Hard X-Rays: High Resolution Imaging at Ambient Pressure and Elevated Temperature.

      PubMed

      Baier, Sina; Damsgaard, Christian D; Scholz, Maria; Benzi, Federico; Rochet, Amélie; Hoppe, Robert; Scherer, Torsten; Shi, Junjie; Wittstock, Arne; Weinhausen, Britta; Wagner, Jakob B; Schroer, Christian G; Grunwaldt, Jan-Dierk

      2016-02-01

      A new closed cell is presented for in situ X-ray ptychography which allows studies under gas flow and at elevated temperature. In order to gain complementary information by transmission and scanning electron microscopy, the cell makes use of a Protochips E-chipTM which contains a small, thin electron transparent window and allows heating. Two gold-based systems, 50 nm gold particles and nanoporous gold as a relevant catalyst sample, were used for studying the feasibility of the cell. Measurements showing a resolution around 40 nm have been achieved under a flow of synthetic air and during heating up to temperatures of 933 K. An elevated temperature exhibited little influence on image quality and resolution. With this study, the potential of in situ hard X-ray ptychography for investigating annealing processes of real catalyst samples is demonstrated. Furthermore, the possibility to use the same sample holder for ex situ electron microscopy before and after the in situ study underlines the unique possibilities available with this combination of electron microscopy and X-ray microscopy on the same sample.

    10. Note: Setup for chemical atmospheric control during in situ grazing incidence X-ray scattering of printed thin films

      NASA Astrophysics Data System (ADS)

      Pröller, Stephan; Moseguí González, Daniel; Zhu, Chenhuii; Schaible, Eric; Wang, Cheng; Müller-Buschbaum, Peter; Hexemer, Alexander; Herzig, Eva M.

      2017-06-01

      In order to tailor the assembling of polymers and organic molecules, a deeper understanding of the kinetics involved in thin film production is necessary. While post-production characterization only provides insight on the final film structure, more sophisticated experimental setups are needed to probe the structure formation processes in situ during deposition. The drying kinetics of a deposited organic thin film strongly influences the assembling process on the nanometer scale. This work presents an experimental setup that enables fine control of the atmosphere composition surrounding the sample during slot die coating, while simultaneously probing the film formation kinetics using in situ grazing incidence X-ray scattering and spectroscopy.

    11. Note: Setup for chemical atmospheric control during in situ grazing incidence X-ray scattering of printed thin films.

      PubMed

      Pröller, Stephan; Moseguí González, Daniel; Zhu, Chenhuii; Schaible, Eric; Wang, Cheng; Müller-Buschbaum, Peter; Hexemer, Alexander; Herzig, Eva M

      2017-06-01

      In order to tailor the assembling of polymers and organic molecules, a deeper understanding of the kinetics involved in thin film production is necessary. While post-production characterization only provides insight on the final film structure, more sophisticated experimental setups are needed to probe the structure formation processes in situ during deposition. The drying kinetics of a deposited organic thin film strongly influences the assembling process on the nanometer scale. This work presents an experimental setup that enables fine control of the atmosphere composition surrounding the sample during slot die coating, while simultaneously probing the film formation kinetics using in situ grazing incidence X-ray scattering and spectroscopy.

    12. Time-resolved in situ powder X-ray diffraction reveals the mechanisms of molten salt synthesis.

      PubMed

      Moorhouse, Saul J; Wu, Yue; Buckley, Hannah C; O'Hare, Dermot

      2016-11-24

      We report the first use of high-energy monochromatic in situ X-ray powder diffraction to gain unprecedented insights into the chemical processes occurring during high temperature, lab-scale metal oxide syntheses. During the flux synthesis of the n = 4 Aurivillius phase, Bi5Ti3Fe0.5Cr0.5O15 at 950 °C in molten Na2SO4 we observe the progression of numerous metastable phases. Using sequential multiphase Rietveld refinement of the time-dependent in situ XRD data, we are able to obtain mechanistic understanding of this reaction under a range of conditions.

    13. In-situ X-ray nano-CT System for Polymer Electrolyte Fuel Cells under Operating Conditions

      NASA Astrophysics Data System (ADS)

      Sekizawa, O.; Uruga, T.; Ishiguro, N.; Matsui, H.; Higashi, K.; Sakata, T.; Iwasawa, Y.; Tada, M.

      2017-06-01

      We developed two types of in-situ three-dimensional imaging systems on the basis of full-field transmission X-ray computed tomography (XCT) methods for polymer electrolyte fuel cells (PEFCs) under operating conditions at beamline BL36XU at SPring-8. One was for a wide field of view (more than 500 μm) to obtain the whole membrane electrode assembly (MEA) images, and the other was for nano spatial resolution (less than 100 nm) using a Fresnel zone plate as objective optics. We succeeded in in-situ three-dimensional visualization of an MEA in PEFC using both XCT measurement systems and show preliminary results.

    14. In-plate protein crystallization, in situ ligand soaking and X-ray diffraction.

      PubMed

      le Maire, Albane; Gelin, Muriel; Pochet, Sylvie; Hoh, François; Pirocchi, Michel; Guichou, Jean François; Ferrer, Jean Luc; Labesse, Gilles

      2011-09-01

      X-ray crystallography is now a recognized technique for ligand screening, especially for fragment-based drug design. However, protein crystal handling is still tedious and limits further automation. An alternative method for the solution of crystal structures of proteins in complex with small ligands is proposed. Crystallization drops are directly exposed to an X-ray beam after cocrystallization or soaking with the desired ligands. The use of dedicated plates in connection with an optimal parametrization of the G-rob robot allows efficient data collection. Three proteins currently under study in our laboratory for ligand screening by X-ray crystallography were used as validation test cases. The protein crystals belonged to different space groups, including a challenging monoclinic case. The resulting diffraction data can lead to clear ligand recognition, including indication of alternating conformations. These results demonstrate a possible method for automation of ligand screening by X-ray crystallography.

    15. In situ X-ray Microscopy Studies of Electromigration in Copper Interconnects

      NASA Astrophysics Data System (ADS)

      Schneider, G.; Meyer, M.-A.; Zschech, E.; Denbeaux, G.; Neuhäusler, U.; Guttmann, P.

      2003-09-01

      Real-time X-ray microscopy is applied for degradation studies to understand electromigration-induced transport processes in on-chip copper interconnects. The material transport in inlaid Cu line/via structures is observed with about 40 nm lateral resolution. The image sequences show void formation, migration and nucleation processes. Correlation of the real-time X-ray images with post-mortem SEM micrographs is used to discuss degradation mechanisms in inlaid copper interconnects. Due to the high penetration power of X-rays through matter and its high spatial resolution, X-ray microscopy (XRM) overcomes several limitations of conventional microscopic techniques. It utilizes the natural absorption contrast between the structures of interest, i.e. for on-chip copper interconnects embedded in dielectrics. Due to their different X-ray absorption characteristics at 0.52 keV, even different silicon compounds like Si, SiO2, and Si3N4 can be distinguished in X-ray images of thinned layers as demonstrated. For failure analysis of thicker layers, phase contrast microscopy in the multi-keV photon energy range is proposed.

    16. In-situ GISAXS monitoring of ultrashort period W/B4C multilayer x-ray mirror growth

      NASA Astrophysics Data System (ADS)

      Hodas, Martin; Siffalovic, Peter; Halahovets, Yuriy; Pelletta, Marco; Vegso, Karol; Jergel, Matej; Majkova, Eva

      2015-08-01

      Ultrashort period multilayer X-ray mirrors with the layer thickness down to 1 nm or less represent a technological challenge. Here, the layer thickness becomes comparable to the interface roughness and discontinuous layers producing strong diffuse scattering may appear. The grazing-incidence small-angle X-ray scattering (GISAXS) is a unique nondestructive technique to probe the mirror quality in terms of the statistical interface roughness and its correlation properties. We present the first in-situ laboratory GISAXS experiments of monitoring the multilayer mirror growth in order to better understand and optimize the deposition process. A microfocus X-ray source IμS with focusing Montel optics (Incoatec) and 2D X-ray detector Pilatus 200K (Dectris) were mounted on a custom-designed dual-ion beam sputtering apparatus (Bestec). Two W/B4C mirrors with 15 periods of 1.8 nm and 2.1 nm were prepared as determined from the post-deposition specular X-ray reflectivity measurements. The in-situ GISAXS tracking was done by a fast repeated collection of the GISAXS frames with the integration time of 8 s at the incidence angle of 0.25 degree. Two distinct features along qz at qy = 0, namely Yoneda and Bragg-like (BL) multilayer peaks evolved in the GISAXS pattern. Oscillatory behavior of the latter in terms of intensity and FWHM was observed after the initial stage. Lateral cuts of the diffuse scattering concentration stripes surrounding BL peaks in particular GISAXS frames provided temporal evolution of the correlation and fractal interface parameters. Their potential for tailoring the multilayer properties is discussed.

    17. Application of energy-dispersive X-ray elemental mapping to probe the homogeneity of sol-gel derived YBa{sub 2}Cu{sub 3}O{sub 7-{delta}} and related phases

      SciTech Connect

      Houk, C.S.; Burgoine, G.A.; Page, C.J.

      1995-04-01

      The authors describe results obtained using energy dispersive X-ray (EDX) elemental mapping to probe the homogeneity of YBa{sub 2}Cu{sub 3}O{sub 7{minus}{delta}}. Sol-gel synthesis and conventional solid-state synthesis of the ceramic with firing to 950{degrees}C and sol-gel synthesis with firing at 700{degrees}C are the synthetic routes considered. It was found that the low temperature sol-gel method yields high-quality YBa{sub 2}Cu{sub 3}O{sub 7{minus}{delta}} provided the firing stage is of sufficient duration.

    18. X-ray irradiation of soda-lime glasses studied in situ with surface plasmon resonance spectroscopy

      SciTech Connect

      Serrano, A.; Galvez, F.; Rodriguez de la Fuente, O.; Garcia, M. A.

      2013-03-21

      We present here a study of hard X-ray irradiation of soda-lime glasses performed in situ and in real time. For this purpose, we have used a Au thin film grown on glass and studied the excitation of its surface plasmon resonance (SPR) while irradiating the sample with X-rays, using a recently developed experimental setup at a synchrotron beamline [Serrano et al., Rev. Sci. Instrum. 83, 083101 (2012)]. The extreme sensitivity of the SPR to the features of the glass substrate allows probing the modifications caused by the X-rays. Irradiation induces color centers in the soda-lime glass, modifying its refractive index. Comparison of the experimental results with simulated data shows that both, the real and the imaginary parts of the refractive index of soda-lime glasses, change upon irradiation in time intervals of a few minutes. After X-ray irradiation, the effects are partially reversible. The defects responsible for these modifications are identified as non-bridging oxygen hole centers, which fade by recombination with electrons after irradiation. The kinetics of the defect formation and fading process are also studied in real time.

    19. In-Situ X-Ray Microscopy of Phase and Composition Distributions in Metal Alloys During Solidification

      NASA Technical Reports Server (NTRS)

      Kaukler, William F.; Curreri, Peter A.

      1999-01-01

      This research applies a state of the art X-ray Transmission Microscope, to image the solidification of metallic or semiconductor alloys in real-time. By employing a hard x-ray source with sub-micron dimensions, resolutions of up to 3 gm can be obtained with magnifications of over 800 X. Specimen growth conditions were optimized and the best imaging technologies applied to maintain x-ray image resolution, contrast and sensitivity. In addition, a special furnace design is required to permit controlled growth conditions and still offer maximum resolution and image contrast. We have successfully imaged in real-time: interfacial morphologies, phase growth, coalescence, incorporation of phases into the growing interface, and the solute boundary layer in the liquid at the solid-liquid inter-face. We have also measured true local growth rates and can evaluate segregation structures in the solid; a form of in-situ metallography. Composition gradients within the specimen cause vafiations in absorption of the flux such that the final image represents a spatial integral of composition (or thickness). During this study, the growth of secondary phase fibers and lameilae from eutectic and monotectic alloys have been imaged during solidification, in real-time, for the first time in bulk metal alloys. Keywords: x-ray, microscope, solidification, microfocus, real-time, microstructure

    20. Development of high-performance X-ray transparent crystallization plates for in situ protein crystal screening and analysis

      SciTech Connect

      Soliman, Ahmed S. M.; Warkentin, Matthew; Apker, Benjamin; Thorne, Robert E.

      2011-07-01

      An optically, UV and X-ray transparent crystallization plate suitable for in situ analysis has been developed. The plate uses contact line pinning rather than wells to confine the liquids. X-ray transparent crystallization plates based upon a novel drop-pinning technology provide a flexible, simple and inexpensive approach to protein crystallization and screening. The plates consist of open cells sealed top and bottom by thin optically, UV and X-ray transparent films. The plates do not need wells or depressions to contain liquids. Instead, protein drops and reservoir solution are held in place by rings with micrometre dimensions that are patterned onto the bottom film. These rings strongly pin the liquid contact lines, thereby improving drop shape and position uniformity, and thus crystallization reproducibility, and simplifying automated image analysis of drop contents. The same rings effectively pin solutions containing salts, proteins, cryoprotectants, oils, alcohols and detergents. Strong pinning by rings allows the plates to be rotated without liquid mixing to 90° for X-ray data collection or to be inverted for hanging-drop crystallization. The plates have the standard SBS format and are compatible with standard liquid-handling robots.

    1. In-Situ X-Ray Microscopy of Phase and Composition Distributions in Metal Alloys During Solidification

      NASA Technical Reports Server (NTRS)

      Kaukler, William F.; Curreri, Peter A.

      1999-01-01

      This research applies a state of the art X-ray Transmission Microscope, to image the solidification of metallic or semiconductor alloys in real-time. By employing a hard x-ray source with sub-micron dimensions, resolutions of up to 3 gm can be obtained with magnifications of over 800 X. Specimen growth conditions were optimized and the best imaging technologies applied to maintain x-ray image resolution, contrast and sensitivity. In addition, a special furnace design is required to permit controlled growth conditions and still offer maximum resolution and image contrast. We have successfully imaged in real-time: interfacial morphologies, phase growth, coalescence, incorporation of phases into the growing interface, and the solute boundary layer in the liquid at the solid-liquid inter-face. We have also measured true local growth rates and can evaluate segregation structures in the solid; a form of in-situ metallography. Composition gradients within the specimen cause vafiations in absorption of the flux such that the final image represents a spatial integral of composition (or thickness). During this study, the growth of secondary phase fibers and lameilae from eutectic and monotectic alloys have been imaged during solidification, in real-time, for the first time in bulk metal alloys. Keywords: x-ray, microscope, solidification, microfocus, real-time, microstructure

    2. Determination of the solubility of tin indium oxide using in situ and ex x-ray diffraction

      SciTech Connect

      Gonzalez, G. B.; Mason, T. O.; Okasinski, J. S.; Buslaps, T.; Honkimaki, V.

      2012-02-01

      A novel approach to determine the thermodynamic solubility of tin in indium oxide via the exsolution from tin overdoped nano-ITO powders is presented. High-energy, in situ and ex situ synchrotron X-ray diffraction was utilized to study the solubility limit at temperatures ranging from 900 C to 1375 C. The tin exsolution from overdoped nanopowders and the formation of In{sub 4}Sn{sub 3}O{sub 12} were observed in situ during the first 4-48 h of high-temperature treatment. Samples annealed between 900 C and 1175 C were also studied ex situ with heat treatments for up to 2060 h. Structural results obtained from Rietveld analysis include compositional phase analysis, atomic positions, and lattice parameters. The tin solubility in In{sub 2}O{sub 3} was determined using the phase analysis compositions from X-ray diffraction and the elemental compositions obtained from X-ray fluorescence. Experimental complications that can lead to incorrect tin solubility values in the literature are discussed.

    3. In Situ X-ray Microtomography of Stress Corrosion Cracking and Corrosion Fatigue in Aluminum Alloys

      NASA Astrophysics Data System (ADS)

      Singh, Sudhanshu S.; Stannard, Tyler J.; Xiao, Xianghui; Chawla, Nikhilesh

      2017-08-01

      Structural materials are subjected to combinations of stress and corrosive environments that work synergistically to cause premature failure. Therefore, studies on the combined effect of stress and corrosive environments on material behavior are required. Existing studies have been performed in two dimensions that are inadequate for full comprehension of the three-dimensional (3D) processes related to stress corrosion cracking (SCC) and corrosion-fatigue (CF) behavior. Recently, x-ray synchrotron tomography has evolved as an excellent technique to obtain the microstructure in 3D. Moreover, being nondestructive in nature, x-ray synchrotron tomography is well suited to study the evolution of microstructure with time (4D, or fourth dimension in time). This article presents our recent 4D studies on SCC and CF of Al 7075 alloys using x-ray synchrotron tomography.

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

      NASA Astrophysics Data System (ADS)

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

      2014-01-01

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

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

      SciTech Connect

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

      2013-08-20

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

    6. Note: A novel method for in situ loading of gases via x-ray induced chemistry

      SciTech Connect

      Pravica, Michael; Bai, Ligang; Park, Changyong; Liu, Yu; Galley, Martin; Robinson, John; Bhattacharya, Neelanjan

      2011-12-14

      We have developed and demonstrated a novel method to load oxygen in a sealed diamond anvil cell via the x-ray induced decomposition of potassium chlorate. By irradiating a pressurized sample of an oxidizer (KClO{sub 3}) with either monochromatic or white beam x-rays from the Advanced Photon Source at ambient temperature and variable pressure, we succeeded in creating a localized region of molecular oxygen surrounded by unreacted sample which was confirmed via Raman spectroscopy. We anticipate that this technique will be useful in loading even more challenging, difficult-to-load gases such as hydrogen and also to load multiple gases.

    7. Note: A novel method for in situ loading of gases via x-ray induced chemistry

      NASA Astrophysics Data System (ADS)

      Pravica, Michael; Bai, Ligang; Park, Changyong; Liu, Yu; Galley, Martin; Robinson, John; Bhattacharya, Neelanjan

      2011-10-01

      We have developed and demonstrated a novel method to load oxygen in a sealed diamond anvil cell via the x-ray induced decomposition of potassium chlorate. By irradiating a pressurized sample of an oxidizer (KClO3) with either monochromatic or white beam x-rays from the Advanced Photon Source at ambient temperature and variable pressure, we succeeded in creating a localized region of molecular oxygen surrounded by unreacted sample which was confirmed via Raman spectroscopy. We anticipate that this technique will be useful in loading even more challenging, difficult-to-load gases such as hydrogen and also to load multiple gases.

    8. In situ X-ray photoelectron and Auger electron spectroscopic characterization of reaction mechanisms during Li-ion cycling.

      PubMed

      Tang, Ching-Yen; Haasch, Richard T; Dillon, Shen J

      2016-11-03

      The complex nature of Li-ion battery reactions along with their sensitivity to environmental exposure necessitates in situ characterization, particularly for surface sensitive methods. In this work, we demonstrate in situ X-ray photoelectron spectroscopy and in situ Auger electron spectroscopy applied to characterize the evolution of bonding and chemistry during cycling of nanoparticle electrodes. We apply the method to study the conversion reaction associated with Li insertion and extraction from CuO nanoparticle electrodes. This approach circumvents the need for ion sputtering and mechanical erosion, previously required to remove solid electrolyte interphase during ex situ measurements. This allows the elucidation of the changes in Cu oxidation state, during initial Li insertion, without the introduction of artifacts that have caused prior disagreement in the published literature.

    9. Novel cell design for combined in situ acoustic emission and x-ray diffraction study during electrochemical cycling of batteries

      SciTech Connect

      Rhodes, Kevin; Meisner, Roberta; Daniel, Claus; Kirkham, Melanie; Parish, Chad M.; Dudney, Nancy

      2011-07-15

      An in situ acoustic emission (AE) and x-ray diffraction cell for use in the study of battery electrode materials has been designed and tested. This cell uses commercially available coin cell hardware retrofitted with a metalized polyethylene terephthalate (PET) disk, which acts as both an x-ray window and a current collector. In this manner, the use of beryllium and its associated cost and hazards is avoided. An AE sensor may be affixed to the cell face opposite the PET window in order to monitor degradation effects, such as particle fracture, during cell cycling. Silicon particles, which were previously studied by the AE technique, were tested in this cell as a model material. The performance of these cells compared well with unmodified coin cells, while providing information about structural changes in the active material as the cell is repeatedly charged and discharged.

    10. Novel cell design for combined in situ acoustic emission and x-ray diffraction study during electrochemical cycling of batteries

      NASA Astrophysics Data System (ADS)

      Rhodes, Kevin; Kirkham, Melanie; Meisner, Roberta; Parish, Chad M.; Dudney, Nancy; Daniel, Claus

      2011-07-01

      An in situ acoustic emission (AE) and x-ray diffraction cell for use in the study of battery electrode materials has been designed and tested. This cell uses commercially available coin cell hardware retrofitted with a metalized polyethylene terephthalate (PET) disk, which acts as both an x-ray window and a current collector. In this manner, the use of beryllium and its associated cost and hazards is avoided. An AE sensor may be affixed to the cell face opposite the PET window in order to monitor degradation effects, such as particle fracture, during cell cycling. Silicon particles, which were previously studied by the AE technique, were tested in this cell as a model material. The performance of these cells compared well with unmodified coin cells, while providing information about structural changes in the active material as the cell is repeatedly charged and discharged.

    11. An ultra-high vacuum electrochemical flow cell for in situ/operando soft X-ray spectroscopy study

      SciTech Connect

      Bora, Debajeet K. E-mail: jguo@lbl.gov; Glans, Per-Anders; Pepper, John; Liu, Yi-Sheng; Guo, J.-H. E-mail: jguo@lbl.gov; Du, Chun; Wang, Dunwei

      2014-04-15

      An in situ flow electrochemical cell has been designed and fabricated to allow better seal under UHV chamber thus to achieve a good signal to noise ratio in fluorescence yield detection of X-ray absorption spectra for spectroelectrochemical study. The cell also stabilizes the thin silicon nitride membrane window in an effective manner so that the liquid cell remains intact during X-ray absorption experiments. With the improved design of the liquid cell, electrochemical experiments such as cyclic voltammetry have been performed for 10 cycles with a good stability of sample window. Also an operando electrochemical experiment during photoelectrochemistry has been performed on n-type hematite electrode deposited on silicon nitride window. The experiment allows us to observe the formation of two extra electronic transitions before pre edge of O K-edge spectra.

    12. In situ X-ray powder diffraction studies of the synthesis of graphene oxide and formation of reduced graphene oxide

      NASA Astrophysics Data System (ADS)

      Storm, Mie Møller; Johnsen, Rune E.; Norby, Poul

      2016-08-01

      Graphene oxide (GO) and reduced graphene oxide (rGO) are important materials in a wide range of fields. The modified Hummers methods, for synthesizing GO, and subsequent thermal reduction to rGO, are often employed for production of rGO. However, the mechanism behinds these syntheses methods are still unclear. We present an in situ X-ray diffraction study of the synthesis of GO and thermal reduction of GO. The X-ray diffraction revealed that the Hummers method includes an intercalation state and finally formation of additional crystalline material. The formation of GO is observed during both the intercalation and the crystallization stage. During thermal reduction of GO three stages were observed: GO, a disordered stage, and the rGO stage. The appearance of these stages depends on the heating ramp. The aim of this study is to provide deeper insight into the chemical and physical processes during the syntheses.

    13. Design of a continuous-flow reactor for in situ x-ray absorption spectroscopy of solids in supercritical fluids.

      PubMed

      Dreher, M; De Boni, E; Nachtegaal, M; Wambach, J; Vogel, F

      2012-05-01

      This paper presents the design and performance of a novel high-temperature and high-pressure continuous-flow reactor, which allows for x-ray absorption spectroscopy or diffraction in supercritical water and other fluids under high pressure and temperature. The in situ cell consists of a tube of sintered, polycrystalline aluminum nitride, which is tolerant to corrosive chemical media, and was designed to be stable at temperatures up to 500 °C and pressures up to 30 MPa. The performance of the reactor is demonstrated by the measurement of extended x-ray absorption fine structure spectra of a carbon-supported ruthenium catalyst during the continuous hydrothermal gasification of ethanol in supercritical water at 400 °C and 24 MPa.

    14. In Situ Heater Design for Nanoscale Synchrotron-Based Full-Field Transmission X-Ray Microscopy

      SciTech Connect

      Kiss, Andrew M.; Harris, William M.; Nakajo, Arata; Wang, Steve; Vila-Comamala, Joan; Deriy, Alex; Chiu, Wilson K. S.

      2015-03-05

      Abstract

      The oxidation of nickel powder under a controlled gas and temperature environment was studied using synchrotron-based full-field transmission X-ray microscopy. The use of this technique allowed for the reaction to be imagedin situat 55 nm resolution. The setup was designed to fit in the limited working distance of the microscope and to provide the gas and temperature environments analogous to solid oxide fuel cell operating conditions. Chemical conversion from nickel to nickel oxide was confirmed using X-ray absorption near-edge structure. Using an unreacted core model, the reaction rate as a function of temperature and activation energy were calculated. This method can be applied to study many other chemical reactions requiring similar environmental conditions.

    15. In-situ x-ray scattering investigation of strain in thin-film morphological evolution of homoepitaxial Ag(001)

      NASA Astrophysics Data System (ADS)

      Hayden, S. T.; Kim, C.; Conrad, E. H.; Gramlich, M. W.; Miceli, P. F.

      2010-03-01

      Because it escapes detection in most experimental probes of surfaces, the role of strain during film growth has not been widely investigated. However, large strain fields arise from vacancy nano-clusters [C. Kim et al., APL 91, 093131 (2007)] that can be incorporated during film growth at lower temperatures. It has also been suggested that extreme surface morphologies, resulting from a deposition flux at grazing angles, might lead to significant strain [Y. Shim et. al., PRL 101, 11601 (2008)]. Because of its simultaneous sensitivity to both the surface and the subsurface, x-ray scattering is a particularly valuable technique for exploring the role of strain in epitaxial crystal growth. This talk will discuss our recent in-situ x-ray diffuse scattering and reflectivity measurements, performed at the Advanced Photon Source, which investigate the low temperature homoepitaxial growth of Ag(001).

    16. In situ study of the Porticello Bronzes by portable X-ray fluorescence and laser-induced breakdown spectroscopy

      NASA Astrophysics Data System (ADS)

      Ferretti, M.; Cristoforetti, G.; Legnaioli, S.; Palleschi, V.; Salvetti, A.; Tognoni, E.; Console, E.; Palaia, P.

      2007-12-01

      This paper reports the results of a measurement campaign performed at the National Museum of Magna Grecia in Reggio Calabria (Italy). Portable X-Ray Fluorescence (XRF) and Laser-Induced Breakdown Spectroscopy (LIBS) instrumentation allowed in situ analysis of several bronze pieces belonging to the group of the so-called Porticello Bronzes. The find occurred at sea, off the village of Porticello (Reggio Calabria) in 1969 and consists of a number of fragments, including a bearded head, pertaining to at least two statues. The use of X-Ray Fluorescence and Laser-Induced Breakdown Spectroscopy techniques allowed for a classification of the fragments according to their elemental composition. The fragments appear to belong to at least two different statues; although, in general, the compositional classification agrees well with the stylistic analysis of the fragments, significant improvements with respect to previous achievements emerge from the joint results of the two techniques used.

    17. Using in situ X-ray reflectivity to study protein adsorption on hydrophilic and hydrophobic surfaces: benefits and limitations.

      PubMed

      Richter, Andrew G; Kuzmenko, Ivan

      2013-04-30

      We have employed in situ X-ray reflectivity (IXRR) to study the adsorption of a variety of proteins (lysozyme, cytochrome c, myoglobin, hemoglobin, serum albumin, and immunoglobulin G) on model hydrophilic (silicon oxide) and hydrophobic surfaces (octadecyltrichlorosilane self-assembled monolayers), evaluating this recently developed technique for its applicability in the area of biomolecular studies. We report herein the highest resolution depiction of adsorbed protein films, greatly improving on the precision of previous neutron reflectivity (NR) results and previous IXRR studies. We were able to perform complete scans in 5 min or less with the maximum momentum transfer of at least 0.52 Å(-1), allowing for some time-resolved information about the evolution of the protein film structure. The three smallest proteins (lysozyme, cytochrome c, and myoglobin) were seen to deposit as fully hydrated, nondenatured molecules onto hydrophilic surfaces, with indications of particular preferential orientations. Time evolution was observed for both lysozyme and myoglobin films. The larger proteins were not observed to deposit on the hydrophilic substrates, perhaps because of contrast limitations. On hydrophobic surfaces, all proteins were seen to denature extensively in a qualitatively similar way but with a rough trend that the larger proteins resulted in lower coverage. We have generated high-resolution electron density profiles of these denatured films, including capturing the growth of a lysozyme film. Because the solution interface of these denatured films is diffuse, IXRR cannot unambiguously determine the film extent and coverage, a drawback compared to NR. X-ray radiation damage was systematically evaluated, including the controlled exposure of protein films to high-intensity X-rays and exposure of the hydrophobic surface to X-rays before adsorption. Our analysis showed that standard measuring procedures used for XRR studies may lead to altered protein films

    18. An X-Ray Microprobe for In-Situ Stone and Wood Characterization

      NASA Astrophysics Data System (ADS)

      Lovoi, P.; Asmus, J. F.

      NonDestructive Testing (NDT) has become an essential ingredient in the conservation of artworks and in the preservation of historic buildings. In many instances it is necessary to characterize the underlying strata of an artistic or historic object in order to plan technical conservation measures, to understand its history, to authenticate it, or to search for hidden features. X-ray and gamma-ray radiography as well as infrared imaging have been ubiquitous in conservation practice for generations. Recent decades have also seen the introduction of ultrasonic imaging, thermovision, x-ray fluorescence, neutron activation analyses, holographic interferometry, isotopic and trace element analyses, the electron microprobe, the laser microprobe, microwave impulse radar, eddy current imaging, and fiber-optic imaging. Unfortunately, for mainstream conservation and preservation some of these technologies are too costly or difficult to be implemented in any general way. In other instances penetration is too superficial or signals from the depth of interest are masked by interferences. Nevertheless, sufficiently important problems have arisen to warrant the utilization of each of the above NDT technologies as well as still others. A new diagnostic device has been introduced into the conservation field. Stone characterization analyses are reported using miniature x-ray devices that can be inserted into cracks and holes in specimens of interest. The family of x-ray tubes employed in these studies range in diameter from 1 to 6 mm. Operating voltages up to 50 kV are available. Electrical power and cooling are delivered through a flexible cable that has a bend diameter of less than 3 cm. Thus, it was possible to insert the x-ray tube into small holes and cracks in marble stones. In this manner radiographs of the outer strata of stones (and embedded metal pins) have been produced without having to transmit through the entire thickness of large blocks. It should also be possible to

    19. In-situ x-ray monitoring of damage accumulation in SiC/RBSN tensile specimens

      NASA Technical Reports Server (NTRS)

      Baaklini, George Y.; Bhatt, Ramakrishna 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 (0)1, (0)3, (0)5, and (0)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.

    20. X-ray chemical analyzer for field applications

      DOEpatents

      Gamba, Otto O. M.

      1977-01-01

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