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Sample records for adsorption powder x-ray

  1. Novel characterization of the adsorption sites in large pore metal-organic frameworks: combination of X-ray powder diffraction and thermal desorption spectroscopy.

    PubMed

    Soleimani-Dorcheh, Ali; Dinnebier, Robert E; Kuc, Agnieszka; Magdysyuk, Oxana; Adams, Frank; Denysenko, Dmytro; Heine, Thomas; Volkmer, Dirk; Donner, Wolfgang; Hirscher, Michael

    2012-10-01

    The preferred adsorption sites of xenon in the recently synthesized metal-organic framework MFU-4l(arge) possessing a bimodal pore structure (with pore sizes of 12 Å and 18.6 Å) were studied via the combination of low temperature thermal desorption spectroscopy and in situ X-ray powder diffraction. The diffraction patterns were collected at 110 K and 150 K according to the temperature of the desorption maxima. The maximum entropy method was used to reconstruct the electron density distribution of the structure and to localize the adsorbed xenon using refined data of the Xe-filled and empty sample. First principles calculations revealed that Xe atoms exclusively occupy the Wyckoff 32f position at approximately 2/3 2/3 2/3 along the body diagonal of the cubic crystal structure. At 110 K, Xe atoms occupy all 32 f positions (8 atoms per pore) while at 150 K the occupancy descends to 25% (2 atoms per pore). No Xe occupation of the small pores is observed by neither experimental measurements nor theoretical studies. PMID:22895492

  2. Improved camera for better X-ray powder photographs

    NASA Technical Reports Server (NTRS)

    Parrish, W.; Vajda, I. E.

    1969-01-01

    Camera obtains powder-type photographs of single crystals or polycrystalline powder specimens. X-ray diffraction photographs of a powder specimen are characterized by improved resolution and greater intensity. A reasonably good powder pattern of small samples can be produced for identification purposes.

  3. X-ray characterization by energy-resolved powder diffraction

    NASA Astrophysics Data System (ADS)

    Cheung, G.; Hooker, S. M.

    2016-08-01

    A method for single-shot, nondestructive characterization of broadband x-ray beams, based on energy-resolved powder diffraction, is described. Monte-Carlo simulations are used to simulate data for x-ray beams in the keV range with parameters similar to those generated by betatron oscillations in a laser-driven plasma accelerator. The retrieved x-ray spectra are found to be in excellent agreement with those of the input beams for realistic numbers of incident photons. It is demonstrated that the angular divergence of the x rays can be deduced from the deviation of the detected photons from the Debye-Scherrer rings which would be produced by a parallel beam. It is shown that the angular divergence can be measured as a function of the photon energy, yielding the angularly resolved spectrum of the input x-ray beam.

  4. X-ray diffraction investigation of ultrafine boron nitride powders

    SciTech Connect

    Gurov, S.V.; Chukalin, V.I.; Rezchikova, T.V.; Torbov, V.J.; Troitskii, V.N.

    1986-01-01

    This paper presents an x-ray diffraction analysis of ultrafine boron nitride powders of different mean particle sizes. Diffraction spectra of the ultrafine boron nitride powders were obtained using a DRON-1 apparatus. The experimental facts are indicative of a turbostratic character of deformation of the hexagonal lattice of ultrafinely divided boron nitride.

  5. Scanning CCD Detector for X-ray Powder Diffraction

    NASA Astrophysics Data System (ADS)

    Madden, T.; Baldwin, J.; Von Dreele, R.; Suchomel, M.; Toby, B. H.

    2014-03-01

    We discuss the design, fabrication and use of a custom CCD detector for x-ray powder diffraction measurements. The detector is mounted on a diffractometer arm, where line-by-line readout of the CCD is coupled to continuous motion of the arm. As the arm moves, the data from the CCD detector are accumulated and can be viewed as if it were a "film strip" with partial powder diffraction rings. Because of the unique design of the camera, both high-resolution and rapid measurements can be performed. Powder diffraction patterns are collected with speeds of a few minutes, or less, with many of the advantages of large area position-sensitive detectors, for example amorphous silicon flat panels, such as high sensitivity, direct evidence of grainy samples and freedom from low-angle asymmetry, but with resolution better than linear position-sensitive detectors and nearly as good as the ultimate in resolution, analyser-crystal detection [2,3].

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

    USGS Publications Warehouse

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

    2014-01-01

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

  7. X-ray powder data for uranium and thorium minerals

    USGS Publications Warehouse

    Frondel, Clifford; Riska, Daphne; Frondel, Judith Weiss

    1956-01-01

    The U.S. Geological Survey has in preparation a comprehensive volume on the mineralogy of uranium and thorium. This work has been done as part of a continuing systematic survey of data on uranium and thorium minerals on behalf of the Division of Raw Materials, U.S. Atomic Energy Commission. Pending publication of this volume and in response to a widespread demand among workers in uranium and thorium mineralogy, the X-ray powder diffraction data for the known minerals that contain uranium or thorium as an essential constituent are presented here. The coverage is complete except for a few minerals for which there are no reliable data owing to lack of authentic specimens. With the exception of that for ianthinite, the new data either originated in the Geological Survey or in the Mineralogical Laboratory of Harvard University. Data from the literature or other sources were cross-checked against the files of standard patterns of these laboratories; the sources are indicated in the references. Data not accompanied by a reference were obtained from films in the Harvard Standard File and cross-checked as to the identity of the film with the Geological Survey's file. Minor differences can be expected in the d-spacings reported for the same specimens by different investigators because of the manner of preparation of the mount, the conditions of X-ray irradiation, and the method of photography and measurement of the film or chart. The Harvard and Geological Survey data all were obtained from films taken in 114-mm diameter cameras, using either ethyl cellulose and toluene or collodion spindle mounts and Straumanis-type film mounting. Unless otherwise indicated all patterns were taken with copper radiation (Kα 1.5418 A.) and nickel filter and data are given in Angstrom units. The d-spacings are not corrected for film shrinkage. The correction ordinarily is small and in general is less than either the variation in spacing arising from differences in experimental technique of

  8. Combined synchrotron X-ray tomography and X-ray powder diffraction using a fluorescing metal foil

    SciTech Connect

    Kappen, P.; Arhatari, B. D.; Luu, M. B.; Balaur, E.; Caradoc-Davies, T.

    2013-06-15

    This study realizes the concept of simultaneous micro-X-ray computed tomography and X-ray powder diffraction using a synchrotron beamline. A thin zinc metal foil was placed in the primary, monochromatic synchrotron beam to generate a divergent wave to propagate through the samples of interest onto a CCD detector for tomographic imaging, thus removing the need for large beam illumination and high spatial resolution detection. Both low density materials (kapton tubing and a piece of plant) and higher density materials (Egyptian faience) were investigated, and elemental contrast was explored for the example of Cu and Ni meshes. The viability of parallel powder diffraction using the direct beam transmitted through the foil was demonstrated. The outcomes of this study enable further development of the technique towards in situ tomography/diffraction studies combining micrometer and crystallographic length scales, and towards elemental contrast imaging and reconstruction methods using well defined fluorescence outputs from combinations of known fluorescence targets (elements).

  9. Characterization of ceramic powders by an X-ray measuring method

    NASA Technical Reports Server (NTRS)

    Ziegler, B.

    1983-01-01

    X-ray line broadening analysis gives quantitative data on structural changes of ceramic powders after different processing steps. Various Al2O3 powders were investigated and the following points are discussed on the basis of these results: X-ray line broadening analysis, structural changes during grinding, structural changes during annealing, influence of structural properties on sintering behavior and application of line broadening analysis to quality control of powders.

  10. X-Ray Diffraction Powder Patterns and Thin Section Observations from the Sierra Madera Impact Structure

    NASA Astrophysics Data System (ADS)

    Huson, S. A.; Foit, F. F.; Watkinson, A. J.; Pope, M. C.

    2006-03-01

    X-Ray powder diffraction analysis and thin section observations of carbonate and siliciclastic samples from the Sierra Madera impact structure indicate moderate shock pressures (8 to 30 GPa) were generated during the formation of this crater.

  11. Multiple powder diffraction data for an accurate charge density study using synchrotron radiation x-ray

    NASA Astrophysics Data System (ADS)

    Kasai, Hidetaka; Nishibori, Eiji

    2016-04-01

    In recent years multiple synchrotron radiation (SR) powder x-ray diffraction profiles have been successfully applied to advanced structural studies such as an accurate charge density study and a structure determination from powder diffraction. The results have been presented with several examples. Abilities and future prospects have been discussed using state of the art powder diffraction data.

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

    NASA Astrophysics Data System (ADS)

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

    2014-10-01

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

  13. Quality experimental and calculated powder x-ray diffraction

    SciTech Connect

    Sullenger, D.B.; Cantrell, J.S.; Beiter, T.A.; Tomlin, D.W.

    1996-08-01

    For several years, we have submitted quality powder XRD patterns to the International Centre for Diffraction Data for inclusion as reference standards in their Powder Diffraction File. The procedure followed is described; examples used are {beta}-UH{sub 3}, {alpha}- BaT{sub 2}, alpha-lithium disilicate ({alpha}-Li{sub 2}Si{sub 2}O{sub 5}), and 2,2`,4,4`,6,6`hexanitroazobenzene-III (HNAB-III).

  14. A method for automated determination of the crystal structures from X-ray powder diffraction data

    SciTech Connect

    Hofmann, D. W. M. Kuleshova, L. N.

    2006-05-15

    An algorithm is proposed for determining the crystal structure of compounds. In the framework of this algorithm, X-ray powder diffraction patterns are compared using a new similarity index. Unlike the indices traditionally employed in X-ray powder diffraction analysis, the new similarity index can be applied even in the case of overlapping peaks and large differences in unit cell parameters. The capabilities of the proposed procedure are demonstrated by solving the crystal structures of a number of organic pigments (PY111, PR181, Me-PR170)

  15. Monitoring model drug microencapsulation in PLGA scaffolds using X-ray powder diffraction

    PubMed Central

    Aina, Adeyinka; Gupta, Manish; Boukari, Yamina; Morris, Andrew; Billa, Nashiru; Doughty, Stephen

    2015-01-01

    The microencapsulation of three model drugs; metronidazole, paracetamol and sulphapyridine into Poly (dl-Lactide-Co-Glycolide) (PLGA) scaffolds were probed using X-ray Powder Diffraction (XRPD). Changes in the diffraction patterns of the PLGA scaffolds after encapsulation was suggestive of a chemical interaction between the pure drugs and the scaffolds and not a physical intermixture. PMID:27013917

  16. X-RAY POWDER DIFFRACTION SYSTEM FOR CHEMICAL SPECIATION OF PARTICULATE AEROSOL SAMPLES

    EPA Science Inventory

    An x-ray powder diffraction system has been developed for the automated measurement and analysis of particulate aerosol samples. The system is optimized to process samples with particle loadings of about 100 micrograms/sq cm which are acquired with dichotomous air samplers. A pos...

  17. A compact high-resolution X-ray powder diffractometer.

    PubMed

    Fewster, Paul F; Trout, David R D

    2013-12-01

    A new powder diffractometer operating in transmission mode is described. It can work as a rapid very compact instrument or as a high-resolution instrument, and the sample preparation is simplified. The incident beam optics create pure Cu Kα1 radiation, giving rise to peak widths of ∼0.1° in 2θ in compact form with a sample-to-detector minimum radius of 55 mm, reducing to peak widths of <0.05° in high-resolution mode by increasing the detector radius to 240 mm. The resolution of the diffractometer is shown to be governed by a complex mixture of angular divergence, sample size, diffraction effects and the dimensions of the detector pixels. The data can be collected instantaneously, which combined with trivial sample preparation and no sample alignment, makes it a suitable method for very rapid phase identification. As the detector is moved further from the sample, the angular step from the pixel dimension is reduced and the resolution improves significantly for very detailed studies, including structure determination and analysis of the microstructure. The advantage of this geometry is that the resolution of the diffractometer can be calculated precisely and the instrumental artefacts can be analysed easily without a sample present. The performance is demonstrated with LaB6 and paracetamol, and a critical appraisal of the uncertainties in the measurements is presented. The instantaneous data collection offers possibilities in dynamic experiments. PMID:24282331

  18. Certain features of the preparation of boron powders in x-ray diffraction investigations

    SciTech Connect

    Tsagareishvili, G.V.; Avlokhashvili, D.A.; Bairamashvili, I.A.; Dolidze, T.V.; Gabuniya, D.L.; Nakashidze, T.G.; Oganezov, K.A.; Tabutsidze, M.L.

    1985-05-01

    It is known that elemental boron is characterized by an increased reaction capacity toward oxygen. Boron powders oxidize especially intensely. Under real conditions, boron powders always contain a certain quantity of oxide phase (primarily in the form of B2O3), the quantity of which depends on their degree of dispersion, the method of production, and the storage conditions. In long exposure to air, as the result of its high hygroscopicity, boric anhydride reacts with particles of moisture, as the result of which orthoboric acid is formed. The mass absorption coefficient of x-rays by elemental boron is significantly lower than by its compounds (anhydride and acid). The presence on the surface of particles of boric anhydride and products of its hydration, the total quantity of which in the powder is large, cannot affect the result of x-ray diffraction investigations of the powders. In this work an investigation is made of the possibility of weakening this influence by preliminary treatment of the powders.

  19. Microelemental and mineral compositions of pathogenic biomineral concrements: SRXFA, X-ray powder diffraction and vibrational spectroscopy data

    NASA Astrophysics Data System (ADS)

    Moroz, T. N.; Palchik, N. A.; Dar'in, A. V.

    2009-05-01

    X-ray fluorescence analysis using synchrotron radiation (SRXRF), X-ray powder diffraction, infrared and Raman spectroscopy had been applied for determination of microelemental and mineral composition of the kidney stones, gallstones and salivalities from natives of Novosibirsk and Novosibirsk region, Russia. The relationship between mineral, organic and microelemental composition of pathogenic calcilus was shown.

  20. X-ray Spectromicroscopy Study of Protein Adsorption to a Polystyrene-Polylactide Blend

    SciTech Connect

    Leung, Bonnie; Hitchcock, Adam; Cornelius, Rena; Brash, John; Scholl, Andreas; Doran, Andrew

    2010-06-09

    Synchrotron-based X-ray photoemission electron microscopy (X-PEEM) was used to study the adsorption of human serum albumin (HSA) to polystyrene-polylactide (40:60 PS-PLA, 0.7 wt percent) thin films, annealed under various conditions. The rugosity of the substrate varied from 35 to 90 nm, depending on the annealing conditions. However, the characteristics of the protein adsorption (amounts and phase preference) were not affected by the changes in topography. The adsorption was also not changed by the phase inversion which occured when the PS-PLA substrate was annealed above Tg of the PLA. The amount of protein adsorbed depended on whether adsorption took place from distilled water or phosphate buffered saline solution. These differences are interpreted as a result of ionic strength induced changes in the protein conformation in solution.

  1. Characterization of zeolite structure and fluorocarbon reactivity using solid state NMR and x-ray powder diffraction

    NASA Astrophysics Data System (ADS)

    Ciraolo, Michael Frank

    The research presented in this thesis involves a combination of techniques used to study the structure and interactions zeolites adsorbed with fluorocarbons. This research is specifically aimed at understanding the processes of adsorption, binding, and reactivity of fluorocarbons on cation exchanged faujasite type zeolites. The solid state ion exchange process has also been studied since it is one way to obtain materials with higher exchange levels, which has been shown to effect adsorption and catalytic activity. To improve the understanding of the adsorption and separation processes a time resolved in-situ synchrotron x-ray powder diffraction study has been undertaken. Since faujasite type zeolites have been found to be effective in separating mixtures of HFC-134 (CF2HCF2H) and HFC-134a (CFH2CF3) isomers, the adsorption of these fluorocarbons on NaY have been studied. It has been shown that both the extent of loading and the kinetics of the sorption process in molecular sieves can be followed using this technique. A model for the binding of hydrochlorofluorocarbon (HCFC) 124a (CF 2HCF2Cl) adsorbed on NaX at 100K has been determined using a combination x-ray and neutron powder diffraction and solid state NMR. Using Rietveld refinement of the diffraction data, the HCFC molecule was found localized in the zeolite cavities bound on either end by sodium cations in the SII and SIII' positions. The model is consistent with hydrogen bonding between the proton of the HCFC and the framework oxygen. The NMR results further confirm the model and are consistent with Na-F binding and HCFC-framework interactions. Solid-state MAS NMR, synchrotron X-ray powder diffraction and a mass spectrometer and gas chromatograph catalysis system have been used to study the reactivity of HCFC-124a (CF2HCF2Cl) on NaX, Zn 2+-exchanged NaX (ZnX) and Rb+-exchanged NaX (RbX). We have chosen to study HCFC-124a (CF2HCF2Cl) since HCFC-124a can undergo both dehydrofluorination and dehydrochlorination

  2. Lead adsorption at the calcite-water interface: Synchrotron x-ray standing wave and x-ray reflectivity studies

    SciTech Connect

    Sturchio, N.C.; Chiarello, R.P.; You, Hoydoo

    1997-01-01

    By combining synchrotron X-ray standing wave (XSW) measurements with synchrotron X-ray reflectivity measurements, we have determined: (1) the precise three-dimensional location within the calcite unit cell of submonolayer Pb ions adsorbed at the calcite (104) surface from dilute aqueous solutions, and (2) the precise one-dimensional location of these unit cells relative to the calcite surface. Our XSW measurements, using three separate calcite Bragg reflections for triangulation, show that most adsorbed Pb ions occupy Ca sites in the calcite lattice with an ordered coverage of 0.05 equivalent monolayers, while the remaining Pb ions are disordered with a coverage of 0.03 equivalent monolayers. Our X-ray reflectivity measurements show that the ordered Ph ions occur primarily (>70%) in the surface atomic layer of calcite. Atomic force microscopy (AFM) was used to characterize the topography of the calcite (104) surface under conditions similar to the X-ray experiments. The quantitative morphological information obtained by AFM was used to develop realistic models of the calcite surface. The calculated X-ray reflectivities for these model surfaces were compared with the measured X-ray reflectivities. The new combined X-ray method that we have developed can be used to determine the atomic-scale structure of other metals adsorbed at mineral-water interfaces. Such high-resolution structural determinations are essential before detailed conceptual and theoretical models can be further developed to understand and predict the behavior of dissolved metals in mineral-water systems. 60 refs., 8 figs., 3 tabs.

  3. Synchrotron hard X-ray imaging of shock-compressed metal powders

    NASA Astrophysics Data System (ADS)

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

    2015-06-01

    This poster will present the application of a new, high-energy (50 to 250 keV) synchrotron X-ray radiography technique to the study of shock-compressed granular materials. Following plate-impact loading, transmission radiography was used to quantitatively observe the compaction and release processes in a range of high-Z metal powders (e.g. Fe, Ni, Cu). By comparing the predictions of 3D numerical models initialized from X-ray tomograms-captured prior to loading-with experimental results, this research represents a new approach to refining mesoscopic compaction models. The authors gratefully acknowledge the ongoing support of Imperial College London, EPSRC, STFC and the Diamond Light Source, and AWE Plc.

  4. Transient electron density maps of ionic materials from femtosecond x-ray powder diffraction

    NASA Astrophysics Data System (ADS)

    Elsaesser, Thomas

    2014-05-01

    X-ray diffraction represents a key method for spatially resolving electron distributions in crystalline materials. So far, electron density maps have been derived from stationary diffraction patterns, providing detailed insight into the equilibrium charge distribution and crystal geometry. Functional processes in condensed matter are frequently connected with nonequilibrium excitations resulting in atomic motions and charge relocations on ultrashort time scales. Transient structures are resolved in space and time by novel x-ray diffraction methods with a femtosecond time resolution, giving access to the driving mechanisms and underlying interactions. In this talk, new results are presented on transient electron distributions of ionic materials mapped with the help of femtosecond x-ray powder diffraction. Experiments are based on a pump-probe approach in which an optical pulse initiates structural dynamics and a hard x-ray pulse from a synchronized laser-driven plasma source is diffracted from the excited powder sample. Such measurements reveal the interplay of lattice and charge motions in the photoexcited prototype material KDP (KH2PO4) which occur on distinctly different length scales. As a second topic, electron relocations induced by strong external optical fields will be discussed. This interaction mechanism allows for generating coherent superpositions of valence and conduction band quantum states and inducing fully reversible charge dynamics. While the materials LiBH4 and NaBH4 display electron relocations from the (BH4)- ions to the neighboring Li+ and Na+ ions, LiH exhibits an electron transfer from Li to H. The latter is a manifestation of electron correlations and in agreement with theoretical calculations.

  5. X-ray standing wave investigations of Group III and V metal adsorption on Si(001)

    SciTech Connect

    Qian, Y.; Bedzyk, M.J. |; Lyman, P.F.

    1997-05-01

    Investigations of atomic bonding, surface reconstruction, surface dynamics, and growth kinetics of group III and V metals on Si(001) are important for understanding the initial growth stage of III-V semiconductors on Si(001). Such studies can also provide valuable information for other important issues such as surfactant-mediated epitaxy, surface passivation and delta-doping layers. X-ray standing waves generated by dynamical Bragg diffraction were used as an element-specific structural probe for investigating Ga and Sb adsorption on Si(001). These high-resolution measurements reveal important quantitative structural information regarding the dimerized surface structures, and provide a stringent test for structural models proposed by various theoretical calculations. An overview of the X-ray standing wave technique and its application to surface structure and dynamics is presented.

  6. Comparative determination of polymorphs of indomethacin in powders and tablets by chemometrical near-infrared spectroscopy and x-ray powder diffractometry.

    PubMed

    Otsuka, Makoto; Kato, Fumie; Matsuda, Yoshihisa; Ozaki, Yukihiro

    2003-01-01

    The purpose of this research was to develop a rapid chemometrical method based on near-infrared (NIR) spectroscopy to determine indomethacin (IMC) polymorphic content in mixed pharmaceutical powder and tablets. Mixed powder samples with known polymorphic contents of forms alpha and gamma were obtained from physical mixing of 50% of IMC standard polymorphic sample and 50% of excipient mixed powder sample consisting of lactose, corn starch, and hydroxypropylcellulose. The tablets were obtained by compressing the mixed powder at 245 MPa. X-ray powder diffraction profiles and NIR spectra were recorded for 6 kinds of standard materials with various polymorphic contents. The principal component regression analysis was performed based on normalized NIR spectra sets of mixed powder standard samples and tablets. The relationships between the actual and predicted polymorphic contents of form g in the mixed powder measured using x-ray powder diffraction and NIR spectroscopy show a straight line with a slope of 0.960 and 0.995, and correlation coefficient constants of 0.970 and 0.993, respectively. The predicted content values of unknown samples by x-ray powder diffraction and NIR spectroscopy were reproducible and in close agreement, but those by NIR spectroscopy had smaller SDs than those by x-ray powder diffraction. The results suggest that NIR spectroscopy provides a more accurate quantitative analysis of polymorphic content in pharmaceutical mixed powder and tablets than does conventional x-ray powder diffractometry. PMID:12916901

  7. Structure and intermolecular interactions of glipizide from laboratory X-ray powder diffraction.

    PubMed

    Burley, Jonathan C

    2005-12-01

    The crystal structure of glipizide, used as a major treatment of type-2 diabetes, has been determined ab initio using variable-temperature laboratory X-ray powder diffraction combined with a direct-space Monte Carlo/simulated annealing methodology. The strengths of the intermolecular interactions (van der Waals, pi-pi stacking, hydrogen bonding and steric interlock) were quantitatively estimated using the thermal expansion data, which were collected in the same set of experiments as those used to determine the structure. PMID:16306678

  8. RbCa2Nb3O10 from X-ray powder data

    PubMed Central

    Liang, Zhen-Hua; Tang, Kai-Bin; Chen, Qian-Wang; Zheng, Hua-Gui

    2009-01-01

    Rubidium dicalcium triniobate(V), RbCa2Nb3O10, has been synthesized by solid-state reaction and its crystal structure refined from X-ray powder diffraction data using Rietveld analysis. The compound is a three-layer perovskite Dion–Jacobson phase with the perovskite-like slabs derived by termination of the three-dimensional CaNbO3 perovskite structure along the ab plane. The rubidium ions (4/mmm symmetry) are located in the inter­stitial space. PMID:21582979

  9. An electrochemical cell for in operando studies of lithium/sodium batteries using a conventional x-ray powder diffractometer

    NASA Astrophysics Data System (ADS)

    Shen, Yanbin; Pedersen, Erik E.; Christensen, Mogens; Iversen, Bo B.

    2014-10-01

    An electrochemical cell has been designed for powder X-ray diffraction studies of lithium ion batteries (LIB) and sodium ion batteries (SIB) in operando with high time resolution using a conventional powder X-ray diffractometer. The cell allows for studies of both anode and cathode electrode materials in reflection mode. The cell design closely mimics that of standard battery testing coin cells and allows obtaining powder X-ray diffraction patterns under representative electrochemical conditions. In addition, the cell uses graphite as the X-ray window instead of beryllium, and it is easy to operate and maintain. Test examples on lithium insertion/extraction in two spinel-type LIB electrode materials (Li4Ti5O12 anode and LiMn2O4 cathode) are presented as well as first results on sodium extraction from a layered SIB cathode material (Na0.84Fe0.56Mn0.44O2).

  10. An electrochemical cell for in operando studies of lithium/sodium batteries using a conventional x-ray powder diffractometer.

    PubMed

    Shen, Yanbin; Pedersen, Erik E; Christensen, Mogens; Iversen, Bo B

    2014-10-01

    An electrochemical cell has been designed for powder X-ray diffraction studies of lithium ion batteries (LIB) and sodium ion batteries (SIB) in operando with high time resolution using a conventional powder X-ray diffractometer. The cell allows for studies of both anode and cathode electrode materials in reflection mode. The cell design closely mimics that of standard battery testing coin cells and allows obtaining powder X-ray diffraction patterns under representative electrochemical conditions. In addition, the cell uses graphite as the X-ray window instead of beryllium, and it is easy to operate and maintain. Test examples on lithium insertion/extraction in two spinel-type LIB electrode materials (Li4Ti5O12 anode and LiMn2O4 cathode) are presented as well as first results on sodium extraction from a layered SIB cathode material (Na0.84Fe0.56Mn0.44O2). PMID:25362421

  11. Quantification of Pharmaceutical Compounds Based on Powder X-Ray Diffraction with Chemometrics.

    PubMed

    Otsuka, Yuta; Ito, Akira; Matsumura, Saki; Takeuchi, Masaki; Pal, Suvra; Tanaka, Hideji

    2016-01-01

    We propose an approach for the simultaneous determination of multiple components in pharmaceutical mixed powder based on powder X-ray diffraction (PXRD) method coupled with chemometrics. Caffeine anhydrate, acetaminophen and lactose monohydrate were mixed at various ratios. The samples were analyzed by PXRD method in the ranges of 2θ=5.00-30.0 and 35.0-45.0 degrees. Obtained diffractograms were analyzed by conventional peak intensity method, multi curve resolution (MCR)-alternating least squares (ALS) method and partial least squares (PLS) method. Constructed PLS models can most accurately predict the concentrations among different methods used. Each regression vector of PLS correlates not only to the compound of interest but also to the coexisting compounds. The combination of PXRD and PLS methods is concluded to be powerful approach for analyzing multi components in pharmaceutical formulations. PMID:27477651

  12. X-ray studies of ion adsorption at charged titania-electrolyte interfaces

    NASA Astrophysics Data System (ADS)

    Kohli, Vaibhav

    Interaction of counter ions with charged solid-electrolyte interfaces plays an important role in wide ranging chemical and environmental processes including ion adsorption, colloidal stability, and electrokinetic transport. A complete molecular-level characterization of the counter-ion profile near the interface is critical to understanding the interfacial reactivity. Resonant anomalous X-ray reflectivity (RAXR), and crystal truncation rod (CTR) techniques were used to directly measure the vertical density profiles of Rb+ and Sr2+ at the rutile TiO2(110)-electrolyte interface. These results are the first experimental confirmation of a recent molecular dynamics prediction that the adsorbed ion structure is distributed between multiple inner-sphere sites (i.e., tetra-dentate and bi-dentate) rather than a single site (i.e., tetra-dentate) as thought from previous investigations. Rb+ and Sr2+ are found to be specifically-adsorbed with coverages of 0.080+/-0.003 and 0.40+/-0.07 monolayers respectively, and average heights of 3.72+/-0.03 A and 3.05+/-0.16 A above the interface respectively. A new generalized model-independent approach was developed for the analysis of long-period x-ray standing waves (XSW) data. The approach is applicable to various reflection geometries, including simple x-ray mirrors, and multi-layers, and is valid for XSW in an attenuating medium. The formalism allows direct extraction of the amplitudes and phases of the elemental structure factor from the measured long-period XSW data, leading to a fully model-independent recovery of the elemental distribution. The method is demonstrated by extracting the 1D profile of Ti normal to the surface for a TiO2/Si/Mo tri-layer sample on a Si substrate, using Ti-Kalpha fluorescence yield measured in ex situ and in situ environments. Using long period XSW, X-ray fluorescence (XRF) and X-ray reflectivity (XR), it is shown that titania nanofilms grown by atomic layer deposition (ALD) exhibit significantly

  13. Characterization by X-ray tomography of granulated alumina powder during in situ die compaction

    SciTech Connect

    Cottrino, Sandrine; Jorand, Yves Maire, Eric; Adrien, Jérôme

    2013-07-15

    Compaction process, the aim of which being to obtain green bodies with low porosity and small size, is often used before sintering treatment. Prior to die filling, the ceramic powder is generally granulated to improve flowability. However during compaction, density heterogeneity and critical size defects may appear due to intergranule and granule-die wall frictions. In this work, the influence of granule formulation on the compact morphology has been studied. To do so, a compaction setup was installed inside an X-ray tomography equipment so that the evolution of the compact morphology could be analysed during the whole compaction process. We have demonstrated that high humidity rate and the addition of binder in the granule formulation increase density heterogeneity and generate larger defects. - Highlights: • An original compaction set up was installed inside an X-Ray tomography equipment. • The compaction process of granulated ceramic powder is imaged. • The compact green microstructure is quantified and related to the compaction stages. • The most detrimental defects of dry-pressed parts are caused by hollow granules. • Formulations without binder allow a reduction of the number of large defects.

  14. Synchrotron Powder X-ray Diffraction Study of the Structure and Dehydration Behavior of Sepiolite

    SciTech Connect

    Post,J.; Bish, D.; Heaney, P.

    2007-01-01

    Rietveld refinements using synchrotron powder X-ray diffraction data were used to study the crystal structure and dehydration behavior of sepiolite from Durango, Mexico. The room-temperature (RT) sepiolite structure in air compares well with previous models but reveals an additional zeolitic H{sub 2}O site. The RT structure under vacuum retained only {approx}1/8 of the zeolitic H{sub 2}O and the volume decreased by 1.3%. Real-time, temperature-resolved synchrotron powder X-ray diffraction data and Rietveld refinements were used to investigate the behavior of the sepiolite structure from 300 to 925 K. Rietveld refinements revealed that most of the zeolitic H{sub 2}O is lost by {approx}390 K, accompanied by a decrease in the a and c unit-cell parameters. Above {approx}600 K the sepiolite structure folds as one-half of the crystallographically bound H{sub 2}O is lost. Rietveld refinements of the 'anhydrous' sepiolite structure reveal that, in general, unit-cell parameters a and b and volume steadily decrease with increasing temperature; there is an obvious change in slope at {approx}820 K suggesting a phase transformation coinciding with the loss of the remaining bound H{sub 2}O molecule.

  15. An X-ray diffraction analysis of crystallised whey and whey-permeate powders.

    PubMed

    Nijdam, Justin; Ibach, Alexander; Eichhorn, Klaus; Kind, Matthias

    2007-11-26

    Amorphous whey, whey-permeate and lactose powders have been crystallised at various air temperatures and humidities, and these crystallised powders have been examined using X-ray diffraction. The most stable lactose crystal under normal storage conditions, alpha-lactose monohydrate, forms preferentially in whey and whey-permeate powders at 50 degrees C, provided sufficient moisture is available, whereas anhydrous beta-lactose and mixed anhydrous lactose crystals, which are unstable under normal storage conditions, form preferentially at 90 degrees C. Thus, faster crystallisation at higher temperatures is offset by the formation of lactose-crystal forms that are less stable under normal storage conditions. Very little alpha-lactose monohydrate crystallised in the pure lactose powders over the range of temperatures and humidities tested, because the crystallisation of alpha- and beta-lactose is considerably more rapid than the mutarotation of beta- to alpha-lactose in the amorphous phase and the hydration of alpha-lactose during crystallisation. Protein and salts hinder the crystallisation process, which provides more time for mutarotation and crystal hydration in the whey and whey-permeate powders. PMID:17719020

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

    NASA Astrophysics Data System (ADS)

    Richter, Andrew

    2007-03-01

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

  17. X-ray photoelectron spectroscopy (XPS) investigation of the surface film on magnesium powders.

    PubMed

    Burke, Paul J; Bayindir, Zeynel; Kipouros, Georges J

    2012-05-01

    Magnesium (Mg) and its alloys are attractive for use in automotive and aerospace applications because of their low density and good mechanical properties. However, difficulty in forming magnesium and the limited number of available commercial alloys limit their use. Powder metallurgy may be a suitable solution for forming near-net-shape parts. However, sintering pure magnesium presents difficulties due to surface film that forms on the magnesium powder particles. The present work investigates the composition of the surface film that forms on the surface of pure magnesium powders exposed to atmospheric conditions and on pure magnesium powders after compaction under uniaxial pressing at a pressure of 500 MPa and sintering under argon at 600 °C for 40 minutes. Initially, focused ion beam microscopy was utilized to determine the thickness of the surface layer of the magnesium powder and found it to be ~10 nm. The X-ray photoelectron analysis of the green magnesium sample prior to sintering confirmed the presence of MgO, MgCO(3)·3H(2)O, and Mg(OH)(2) in the surface layer of the powder with a core of pure magnesium. The outer portion of the surface layer was found to contain MgCO(3)·3H(2)O and Mg(OH)(2), while the inner portion of the layer is primarily MgO. After sintering, the MgCO(3)·3H(2)O was found to be almost completely absent, and the amount of Mg(OH)(2) was also decreased significantly. This is postulated to occur by decomposition of the compounds to MgO and gases during the high temperature of sintering. An increase in the MgO content after sintering supports this theory. PMID:22524956

  18. High-pressure powder x-ray diffraction study of EuVO{sub 4}

    SciTech Connect

    Garg, Alka B.; Errandonea, D.

    2015-03-15

    The high-pressure structural behavior of europium orthovanadate has been studied using in-situ, synchrotron based, high-pressure x-ray powder diffraction technique. Angle-dispersive x-ray diffraction measurements were carried out at room temperature up to 34.7 GPa using a diamond-anvil cell, extending the pressure range reported in previous experiments. We confirmed the occurrence of zircon–scheelite phase transition at 6.8 GPa and the coexistence of low- and high-pressure phases up to 10.1 GPa. In addition, clear evidence of a scheelite–fregusonite transition is found at 23.4 GPa. The fergusonite structure remains stable up to 34.7 GPa, the highest pressure reached in the present measurements. A partial decomposition of EuVO{sub 4} was also observed from 8.1 to 12.8 GPa; however, this fact did not preclude the identification of the different crystal structures of EuVO{sub 4}. The crystal structures of the different phases have been Rietveld refined and their equations of state (EOS) have been determined. The results are compared with the previous experimental data and theoretical calculations. - Graphical abstract: The high-pressure structural sequence of EuVO{sub 4}. - Highlights: • EuVO{sub 4} is studied under pressure up to 35 GPa using synchrotron XRD. • The zircón–scheelite–fergusonite structural sequence is observed. • Crystal structures are refined and equations of state determined.

  19. High-pressure powder x-ray diffraction study of EuVO4

    NASA Astrophysics Data System (ADS)

    Garg, Alka B.; Errandonea, D.

    2015-03-01

    The high-pressure structural behavior of europium orthovanadate has been studied using in-situ, synchrotron based, high-pressure x-ray powder diffraction technique. Angle-dispersive x-ray diffraction measurements were carried out at room temperature up to 34.7 GPa using a diamond-anvil cell, extending the pressure range reported in previous experiments. We confirmed the occurrence of zircon-scheelite phase transition at 6.8 GPa and the coexistence of low- and high-pressure phases up to 10.1 GPa. In addition, clear evidence of a scheelite-fregusonite transition is found at 23.4 GPa. The fergusonite structure remains stable up to 34.7 GPa, the highest pressure reached in the present measurements. A partial decomposition of EuVO4 was also observed from 8.1 to 12.8 GPa; however, this fact did not preclude the identification of the different crystal structures of EuVO4. The crystal structures of the different phases have been Rietveld refined and their equations of state (EOS) have been determined. The results are compared with the previous experimental data and theoretical calculations.

  20. X-ray powder diffraction investigations of the composition of uranium-containing precipitates

    SciTech Connect

    Ionov, R.A.; Molchanova, T.V.; Rodionov, V.V.; Vodolazov, L.I.; Matyunina, E.N.; Zharova, E.V.

    1988-03-01

    Uranium-containing precipitates which were formed from solutions of uranyl sulfate containing various amounts of ammonium bicarbonate in the pH 2-7 range and which imitate the composition of the uranyl complexes formed in the phase of an ion exchanger at corresponding values of the sorption pH have been investigated by the methods of x-ray powder diffraction analysis, thermal analysis, and chemical analysis. It has been established that uranyl sulfates, basic sulfates, and carbonates of varying composition form as the pH is increased in accordance with the form in which uranium exists in the liquid phase. The formation of polynuclear uranyl complexes in the pH 2-4 range has been postulated.

  1. 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.

  2. Fast X-ray powder diffraction on I11 at Diamond.

    PubMed

    Thompson, Stephen P; Parker, Julia E; Marchal, Julien; Potter, Jonathan; Birt, Adrian; Yuan, Fajin; Fearn, Richard D; Lennie, Alistair R; Street, Steven R; Tang, Chiu C

    2011-07-01

    The commissioning and performance characterization of a position-sensitive detector designed for fast X-ray powder diffraction experiments on beamline I11 at Diamond Light Source are described. The detecting elements comprise 18 detector-readout modules of MYTHEN-II silicon strip technology tiled to provide 90° coverage in 2θ. The modules are located in a rigid housing custom designed at Diamond with control of the device fully integrated into the beamline data acquisition environment. The detector is mounted on the I11 three-circle powder diffractometer to provide an intrinsic resolution of Δ2θ approximately equal to 0.004°. The results of commissioning and performance measurements using reference samples (Si and AgI) are presented, along with new results from scientific experiments selected to demonstrate the suitability of this facility for powder diffraction experiments where conventional angle scanning is too slow to capture rapid structural changes. The real-time dehydrogenation of MgH(2), a potential hydrogen storage compound, is investigated along with ultrafast high-throughput measurements to determine the crystallite quality of different samples of the metastable carbonate phase vaterite (CaCO(3)) precipitated and stabilized in the presence of amino acid molecules in a biomimetic synthesis process. PMID:21685682

  3. Model-independent structure factors from powder X-ray diffraction: a novel approach.

    PubMed

    Straasø, Tine; Dippel, Ann-Christin; Becker, Jacob; Als-Nielsen, Jens

    2014-01-01

    Under the experimental condition that all Bragg peaks in a powder X-ray diffraction (PXRD) pattern have the same shape, one can readily obtain the Bragg intensities without fitting any parameters. This condition is fulfilled at the P02.1 beamline at PETRA III using the seventh harmonic from a 23 mm-period undulator (60 keV) at a distance of 65 m. For grain sizes of the order of 1 µm, the Bragg peak shape in the PXRD is entirely determined by the diameter of the capillary containing the powder sample and the pixel size of the image plate detector, and consequently it is independent of the scattering angle. As an example, a diamond powder has been chosen and structure factors derived which are in accordance with those calculated from density functional theory methods of the WIEN2k package to within an accuracy that allows a detailed electron density analysis. PMID:24365925

  4. Crystal structure determination of thymoquinone by high-resolution X-ray powder diffraction.

    PubMed

    Pagola, S; Benavente, A; Raschi, A; Romano, E; Molina, M A A; Stephens, P W

    2004-01-01

    The crystal structure of 2-isopropyl-5-methyl-1,4-benzoquinone (thymoquinone) and its thermal behavior--as necessary physical and chemical properties--were determined in order to enhance the current understanding of thymoquinone chemical action by using high resolution x-ray powder diffraction, Fourier transform infrared spectroscopy (FTIR), and 3 thermo-analytical techniques thermogravimetric analysis (TGA), differential thermal analysis (DTA), and differential scanning calorimetry (DSC). The findings obtained with high-resolution x-ray powder diffraction and molecular location methods based on a simulated annealing algorithm after Rietveld refinement showed that the triclinic unit cell was a = 6.73728(8) A, b = 6.91560(8) A, c = 10.4988(2) A, alpha = 88.864(2) degrees, beta = 82.449(1) degrees, gamma = 77.0299(9) degrees; cell volume = 472.52(1) A3, Z = 2, and space group P1. In addition, FTIR spectrum revealed absorption bands corresponding to the carbonyl and C-H stretching of aliphatic and vinylic groups characteristically observed in such p-benzoquinones. Also, a chemical decomposition process starting at 65 degrees C and ending at 213 degrees C was noted when TGA was used. DSC allowed for the determination of onset at 43.55 degrees C and a melting enthalpy value of DeltaH(m) = 110.6 J/g. The low value obtained for the fusion point displayed a van der Waals pattern for molecular binding, and the thermograms performed evidence that thymoquinone can only be found in crystalline triclinic form, as determined by DRX methods. PMID:15760086

  5. Powder X-Ray Diffraction of the Grain Components of Carbonaceous Chondrite Meteorites.

    NASA Astrophysics Data System (ADS)

    Furton, D. G.; Hurt, Kendra; Bos, Abram

    Carbonaceous chondrite meteorites are thought to bring to Earth samples of primordial interstellar material. Detailed chemical analysis of meteorites representative of this class (i.e., Allende, Murchison, and Orgueil) establish the primordial character of the material they include and, among other things, reveal that nanometer-sized diamond grains are present in the carbonaceous component of these meteorites at about the 1,000 ppm level (Lewis et al. 1987, Nature, 326, 160). The high abundance of nanodiamonds in these meteoritic samples contributes to the hypothesis that nanodiamonds are present in the interstellar medium at relatively high abundance, but direct observational support of this hypothesis is not so conclusive. (It may also be, according to Dai et al. (2002, Nature, 418, 157), that the nanodiamond grains were formed in situ). On the other hand, there is a growing body of observational evidence that indicates nanometer-sized silicon grains are present in the interstellar medium at relatively high abundance (e.g., Smith & Witt 2001, ApJ, 565, 304). But, silicon nanoparticles have yet to be discovered in a sample of carbonaceous chondrite meteorite. It is relevant in this context that the chemical process that has been used to extract nanodiamond grains from meteoritic samples involves dissolving in strong acid the silicate component of the meteorite. The process is ultimately destructive to any silicon grains that may be present and possibly even alters the nanodiamonds it is used to extract (Mutschke et al. 1995, ApJL, 454, L160). There does not appear to be a similar chemical process that could be used to extract silicon nanoparticles from meteoritic samples. We are in the process of establishing to what extent powder X-ray diffraction can be use as a non-destructive analytical tool to examine nanometer-sized grain components of carbonaceous chondrite meteorites. We present powder X-ray diffraction patterns obtained from samples of the Murchison and

  6. Neutron and X-ray powder diffraction study of skutterudite thermoelectrics

    DOE PAGESBeta

    Wang, H.; Kirkham, M. J.; Watkins, T. R.; Payzant, E. A.; Salvador, J. R.; Thompson, A. J.; Sharp, J.; Brown, D.; Miller, D.

    2016-02-17

    N- and p-type filled-skutterudite materials prepared for thermoelectric power generation modules were analyzed by neutron diffraction at the POWGEN beam line of the Spallation Neutron Source (SNS) and X-ray diffraction (XRD). The skutterudite powders were processed by melt spinning, followed by ball milling and annealing. The n-type material consists of Ba–Yb–Co–Sb and the p-type material consists of Di–Fe–Ni–Sb or Di–Fe–Co–Sb (Di = didymium, an alloy of Pr and Nd). Powders for prototype module fabrication from General Motors and Marlow Industries were analyzed in this study. XRD and neutron diffraction studies confirm that both the n- and p-type materials have cubicmore » symmetry. Structural Rietveld refinements determined the lattice parameters and atomic parameters of the framework and filler atoms. The cage filling fraction was found to depend linearly on the lattice parameter, which in turn depends on the average framework atom size. Ultimately, this knowledge may allow the filling fraction of these skutterudite materials to be purposefully adjusted, thereby tuning the thermoelectric properties.« less

  7. Studies of clays and clay minerals using x-ray powder diffraction and the Rietveld method

    SciTech Connect

    Bish, D.L.

    1993-09-01

    The Rietveld method was originally developed (Rietveld, 1967, 1969) to refine crystal structures using neutron powder diffraction data. Since then, the method has been increasingly used with X-ray powder diffraction data, and today it is safe to say that this is the most common application of the method. The method has been applied to numerous natural and synthetic materials, most of which do not usually form crystals large enough for study with single-crystal techniques. It is the ability to study the structures of materials for which sufficiently large single crystals do not exist that makes the method so powerful and popular. It would thus appear that the method is ideal for studying clays and clay minerals. In many cases this is true, but the assumptions implicit in the method and the disordered nature of many clay minerals can limit titsapplicability. This chapter will describe the Rietveld method, emphasizing the assumptions important for the study of disordered materials, and it will outline the potential applications of the method to these minerals. These applications include, in addition to the refinement of crystal structures, quantitative analysis of multicomponent mixtures, analysis of peak broadening, partial structure solution, and refinement of unit-cell parameters.

  8. Structure Determination and Refinement of Acid Strontium Oxalate from X-Ray and Neutron Powder Diffraction

    NASA Astrophysics Data System (ADS)

    Vanhoyland, G.; Bourée, F.; Van Bael, M. K.; Mullens, J.; Van Poucke, L. C.

    2001-03-01

    The structure of acid strontium oxalate Sr(HC2O4)·{1}/{2}(C2O4)·H2O has been determined by conventional X-ray powder diffractometry. The diffraction pattern was indexed from a monoclinic unit cell with cell parameters a=6.341(1) Å, b=16.880(2) Å, c=5.7798(8) Å, and β=97.60(1)°; space group, P21/n (No. 14) with Z=4. Final (isotropic) Rietveld refinement of the neutron powder data yielded RB=4.57%, RF=2.87%, and Rwp=7.87% as conventional Rietveld parameters. Strontium is eight-fold coordinated and can be described as a distorted bicapped trigonal prism. The SrO8 polyhedra form one-dimensional chains along the c-axis by sharing edges. In contrast to all other known strontium oxalates, in this compound H2O acts as bridging ligand between two Sr atoms. SDPD-D classification (1): Sr(HC2O4)-{1}/{2}(C2O4)-H2O, P21/n, C1=14, Nc=42, C2=11, XC1+N/TREOR-97 & DICVOL-91, EXTRA, EQUI, SIRPOW-92 (DM), GFOURIER, FULLPROF.

  9. Concerted electron and proton transfer in ionic crystals mapped by femtosecond x-ray powder diffraction

    SciTech Connect

    Woerner, Michael; Zamponi, Flavio; Ansari, Zunaira; Dreyer, Jens; Freyer, Benjamin; Premont-Schwarz, Mirabelle; Elsaesser, Thomas

    2010-08-14

    X-ray powder diffraction, a fundamental technique of structure research in physics, chemistry, and biology, is extended into the femtosecond time domain of atomic motions. This allows for mapping (macro)molecular structure generated by basic chemical and biological processes and for deriving transient electronic charge density maps. In the experiments, the transient intensity and angular positions of up to 20 Debye Scherrer reflections from a polycrystalline powder are measured and atomic positions and charge density maps are determined with a combined spatial and temporal resolutions of 30 pm and 100 fs. We present evidence for the so far unknown concerted transfer of electrons and protons in a prototype material, the hydrogen-bonded ionic ammonium sulfate [(NH{sub 4}){sub 2}SO{sub 4}]. Photoexcitation of ammonium sulfate induces a sub-100 fs electron transfer from the sulfate groups into a highly confined electron channel along the c-axis of the unit cell. The latter geometry is stabilized by transferring protons from the adjacent ammonium groups into the channel. Time-dependent charge density maps derived from the diffraction data display a periodic modulation of the channel's charge density by low-frequency lattice motions with a concerted electron and proton motion between the channel and the initial proton binding site. Our results set the stage for femtosecond structure studies in a wide class of (bio)molecular materials.

  10. X-ray powder pattern analysis of cytoplasmic polyhedrosis virus inclusion bodies

    SciTech Connect

    Di, X.; Sun, Y.K.; McCrae, M.A.; Rossmann, M.G. )

    1991-01-01

    Cytoplasmic polyhedrosis virus is an insect reovirus which is occluded in crystalline inclusion bodies that form in the mid-gut of certain insects. Inclusion bodies of cytoplasmic polyhedrosis virus from Bombyx mori were isolated and purified. These crystalline bodies, about 1-3 microns in linear size, were compacted in a capillary tube while immersed in buffer. X-ray diffraction photographs showed powder rings, extending to 8.2 A resolution, which could be indexed with a cell measuring a = b = 49.9 +/- 0.4 A, c = 41.5 +/- 0.4 A, alpha = beta = gamma = 90 degrees. The polyhedrin protein, which is the major component of the inclusion body, has a molecular weight of about 30,000 daltons and, hence, there are probably two molecules in the unit cell. Thus, the unit cell is monoclinic or possibly triclinic. A Patterson derived from the measured powder pattern intensities, assuming monoclinic symmetry, could be interpreted in terms of a molecule with two larger globes. Such a structure is roughly consistent with the breakdown of the polyhedrin into two larger fragments of molecular weight 17,000 and 14,000 when raising the pH to near 10. Under these conditions the inclusion bodies disintegrate, releasing virus and catalyzing the proteolysis of the polyhedrin.

  11. Study of polymorphism of Atenolol and Captopril antihypertensives using x-ray powder diffraction and Rietveld refinement

    NASA Astrophysics Data System (ADS)

    Sato, Juliana; Ferreira, Fabio

    2013-03-01

    Characterization of bulk drugs has become increasingly important in the pharmaceutical industry. X-ray powder diffractometry is an effective technique for the identification of crystalline solid-phase drugs. The technique is unique, since it combines specificity with a high degree of accuracy for the characterization of pharmaceuticals in solid state and is an especially useful method to describe the possible polymorphic behavior of drugs substances. In this work X-ray diffraction data have been obtained for two well-known antihypertensive drugs currently being administered in tablet form. They include atenolol and captopril. Atenolol and captopril were purchased from drugstore. The characterizations of the atenolol and captopril samples were carried out by FTIR spectroscopy and X-ray powder diffraction (XRPD). We would like to thank the Brazilian agencies CNPq and FAPESP for their financial support.

  12. Synchrotron X-ray powder diffraction data of LASSBio-1515: A new N-acylhydrazone derivative compound

    NASA Astrophysics Data System (ADS)

    Costa, F. N.; Braz, D.; Ferreira, F. F.; da Silva, T. F.; Barreiro, E. J.; Lima, L. M.; Colaço, M. V.; Kuplich, L.; Barroso, R. C.

    2014-02-01

    In this work, synchrotron X-ray powder diffraction data allowed for a successful indexing of LASSBio-1515 compound, candidate to analgesic and anti-inflammatory activity. X-ray powder diffraction data collected in transmission and high-throughput geometries were used to analyze this compound. The X-ray wavelength of the synchrotron radiation used in this study was determined to be λ=1.55054 Å. LASSBio-1515 was found to be monoclinic with space group P21/c and unit cell parameters a=11.26255(16) Å, b=12.59785(16) Å, c=8.8540(1) Å, β=90.5972(7)° and V=1256.17(3) Å3.

  13. An Inquiry-Based Project Focused on the X-Ray Powder Diffraction Analysis of Common Household Solids

    ERIC Educational Resources Information Center

    Hulien, Molly L.; Lekse, Jonathan W.; Rosmus, Kimberly A.; Devlin, Kasey P.; Glenn, Jennifer R.; Wisneski, Stephen D.; Wildfong, Peter; Lake, Charles H.; MacNeil, Joseph H.; Aitken, Jennifer A.

    2015-01-01

    While X-ray powder diffraction (XRPD) is a fundamental analytical technique used by solid-state laboratories across a breadth of disciplines, it is still underrepresented in most undergraduate curricula. In this work, we incorporate XRPD analysis into an inquiry-based project that requires students to identify the crystalline component(s) of…

  14. Using Variable Temperature Powder X-Ray Diffraction to Determine the Thermal Expansion Coefficient of Solid MgO

    ERIC Educational Resources Information Center

    Corsepius, Nicholas C.; DeVore, Thomas C.; Reisner, Barbara A.; Warnaar, Deborah L.

    2007-01-01

    A laboratory exercise was developed by using variable temperature powder X-ray diffraction (XRD) to determine [alpha] for MgO (periclase)and was tested in the Applied Physical Chemistry and Materials Characterization Laboratories at James Madison University. The experiment which was originally designed to provide undergraduate students with a…

  15. Adsorption of 2-propanol on ice probed by ambient pressure X-ray photoelectron spectroscopy

    SciTech Connect

    Newberg, John T.; Bluhm, Hendrik

    2015-08-18

    The interaction of 2-propanol with ice was examined via ambient pressure X-ray photoelectron spectroscopy (APXPS), a surface sensitive technique that probes the adsorbed 2-propanol directly with submonolayer resolution. Isothermal uptake experiments were performed on vapor deposited ice at 227 K in the presence of the equilibrium water vapor pressure of 0.05 Torr and 2-propanol partial pressures ranging from 5 × 10-5 to 2 × 10-3 Torr. The C 1s APXPS spectra of adsorbed 2-propanol showed two characteristic peaks associated with the COH alcohol group and CMe methyl groups in a 1 : 2 ratio, respectively. Coverage increased with 2-propanol partial pressure and followed first order Langmuir kinetics with a Langmuir constant of K = 6.3 × 103 Torr-1. The 1 : 2 ratio of COH : CMe remained constant with increasing coverage, indicating there is no chemical reaction upon adsorption. The observed Langmuir kinetics using APXPS is consistent with previous observations of other small chain alcohols via indirect adsorption methods using, e.g., Knudsen cell and coated wall flow tube reactors.

  16. Adsorption of 2-propanol on ice probed by ambient pressure X-ray photoelectron spectroscopy

    DOE PAGESBeta

    Newberg, John T.; Bluhm, Hendrik

    2015-08-18

    The interaction of 2-propanol with ice was examined via ambient pressure X-ray photoelectron spectroscopy (APXPS), a surface sensitive technique that probes the adsorbed 2-propanol directly with submonolayer resolution. Isothermal uptake experiments were performed on vapor deposited ice at 227 K in the presence of the equilibrium water vapor pressure of 0.05 Torr and 2-propanol partial pressures ranging from 5 × 10-5 to 2 × 10-3 Torr. The C 1s APXPS spectra of adsorbed 2-propanol showed two characteristic peaks associated with the COH alcohol group and CMe methyl groups in a 1 : 2 ratio, respectively. Coverage increased with 2-propanol partialmore » pressure and followed first order Langmuir kinetics with a Langmuir constant of K = 6.3 × 103 Torr-1. The 1 : 2 ratio of COH : CMe remained constant with increasing coverage, indicating there is no chemical reaction upon adsorption. The observed Langmuir kinetics using APXPS is consistent with previous observations of other small chain alcohols via indirect adsorption methods using, e.g., Knudsen cell and coated wall flow tube reactors.« less

  17. X-Ray Powder Diffraction as a Tool for the Identification of Impact Deformed Rocks

    NASA Astrophysics Data System (ADS)

    Huson, S.; Pope, M.; Foit, F.; Watkinson, A.

    2007-12-01

    Previous X-ray powder diffraction (XRD) studies indicated shock deformed minerals have broader XRD peaks when compared to those of unshocked samples. Entire XRD patterns, single peak profiles and Rietveld refined parameters of carbonate samples from the Sierra Madera impact crater, west Texas and the Mission Canyon Formation of southwest Montana and western Wyoming were used to evaluate the use of X-ray powder diffraction as a tool for distinguishing impact deformed rocks from tectonically deformed rocks. Both sample locations contain rocks subjected to varying degrees of deformation. At Sierra Madera dolostone and limestone samples were collected from the crater rim (lower shock intensity) and the central uplift (higher shock intensity). Carbonate rocks of the Mission Canyon Formation were sampled along a transect across the tectonic front of the Sevier and Laramide orogenies. Peaks in the XRD patterns of shocked calcite in samples from Sierra Madera are generally broader than those of calcite samples from the Mission Canyon Formation whereas peak broadening of shocked dolomite in samples from the outer central uplift of Sierra Madera is similar to those of Mission Canyon Formation samples. Single peak profile patterns of calcite and dolomite samples from both locations are complex and their full width half maxima (FWHM) show no relationship to shock intensity, especially above ~80 ° 2θ. Rietveld refinement of peak shape parameters yields a more precise measure of the 2θ angular dependence of peak FWHM and, therefore, the degree of shock deformation. FWHM values obtained from Rietveld crystal structure refinements increase with shock intensity for all Sierra Madera samples. Additionally, FWHM values of some tectonically deformed Mission Canyon Formation calcites overlap with those of weakly shocked calcite from the crater rim of Sierra Madera. FWHM values of shocked dolomite from the central uplift of Sierra Madera are distinctly higher than tectonically

  18. Characterization by X-Ray Absorption, X-Ray Powder Diffraction, and Magnetic Susceptibility of Cu Zn Co Al Containing Hydroxycarbonates, Oxycarbonates, Oxides, and Their Products of Reduction

    NASA Astrophysics Data System (ADS)

    Porta, Piero; Morpurgo, Simone; Pettiti, Ida

    1996-02-01

    Copper-zinc-cobalt-aluminium-containing crystalline hydroxycarbonates having hydrotalcite structure have been prepared by coprecipitation. X-ray powder diffraction (XRPD), magnetic susceptibility, and extended X-ray absorption fine structure (EXAFS) indicate that Cu2+, Zn2+, and Co2+are present in an octahedral environment. Calcination of the hydroxycarbonates at 723 K produces quasi-amorphous oxycarbonates where Cu2+and Co2+still retain octahedral coordination and cobalt is almost completely oxidized to Co3+. The coordination of Zn2+, at this stage, is intermediate between the octahedral one of the precursors and the tetrahedral one of ZnO and Zn-based spinels. Further calcination at 973 K produces a mixture of crystalline oxides such as CuO, ZnO, CuAl2O4, ZnAl2O4, and ZnCo2O4. EXAFS analysis of these samples indicates that copper is mainly in a fourfold coordination (although two longer Cu-O distances are also detected), zinc is tetrahedral, and cobalt (as Co3+) is essentially octahedral. EXAFS and XANES investigations performed afterin situreduction (10% H2/N2, at 523 and 623 K) on the oxycarbonates and oxides reveal that the total Cu2+→ Cu0reduction occurs only at 623 K in both series of samples, Co3+is reduced to Co2+only at 623 K in the oxycarbonates, and Zn2+is never reduced.

  19. An electrochemical cell for in operando studies of lithium/sodium batteries using a conventional x-ray powder diffractometer

    SciTech Connect

    Shen, Yanbin; Pedersen, Erik E.; Christensen, Mogens; Iversen, Bo B.

    2014-10-15

    An electrochemical cell has been designed for powder X-ray diffraction studies of lithium ion batteries (LIB) and sodium ion batteries (SIB) in operando with high time resolution using a conventional powder X-ray diffractometer. The cell allows for studies of both anode and cathode electrode materials in reflection mode. The cell design closely mimics that of standard battery testing coin cells and allows obtaining powder X-ray diffraction patterns under representative electrochemical conditions. In addition, the cell uses graphite as the X-ray window instead of beryllium, and it is easy to operate and maintain. Test examples on lithium insertion/extraction in two spinel-type LIB electrode materials (Li{sub 4}Ti{sub 5}O{sub 12} anode and LiMn{sub 2}O{sub 4} cathode) are presented as well as first results on sodium extraction from a layered SIB cathode material (Na{sub 0.84}Fe{sub 0.56}Mn{sub 0.44}O{sub 2})

  20. A wavelet transform algorithm for peak detection and application to powder x-ray diffraction data

    NASA Astrophysics Data System (ADS)

    Gregoire, John M.; Dale, Darren; van Dover, R. Bruce

    2011-01-01

    Peak detection is ubiquitous in the analysis of spectral data. While many noise-filtering algorithms and peak identification algorithms have been developed, recent work [P. Du, W. Kibbe, and S. Lin, Bioinformatics 22, 2059 (2006); A. Wee, D. Grayden, Y. Zhu, K. Petkovic-Duran, and D. Smith, Electrophoresis 29, 4215 (2008)] has demonstrated that both of these tasks are efficiently performed through analysis of the wavelet transform of the data. In this paper, we present a wavelet-based peak detection algorithm with user-defined parameters that can be readily applied to the application of any spectral data. Particular attention is given to the algorithm's resolution of overlapping peaks. The algorithm is implemented for the analysis of powder diffraction data, and successful detection of Bragg peaks is demonstrated for both low signal-to-noise data from theta-theta diffraction of nanoparticles and combinatorial x-ray diffraction data from a composition spread thin film. These datasets have different types of background signals which are effectively removed in the wavelet-based method, and the results demonstrate that the algorithm provides a robust method for automated peak detection.

  1. Quantification of febuxostat polymorphs using powder X-ray diffraction technique.

    PubMed

    Qiu, Jing-bo; Li, Gang; Sheng, Yue; Zhu, Mu-rong

    2015-03-25

    Febuxostat is a pharmaceutical compound with more than 20 polymorphs of which form A is most widely used and usually exists in a mixed polymorphic form with form G. In the present study, a quantification method for polymorphic form A and form G of febuxostat (FEB) has been developed using powder X-ray diffraction (PXRD). Prior to development of a quantification method, pure polymorphic form A and form G are characterized. A continuous scan with a scan rate of 3° min(-1) over an angular range of 3-40° 2θ is applied for the construction of the calibration curve using the characteristic peaks of form A at 12.78° 2θ (I/I0100%) and form G at 11.72° 2θ (I/I0100%). The linear regression analysis data for the calibration plots shows good linear relationship with R(2)=0.9985 with respect to peak area in the concentration range 10-60 wt.%. The method is validated for precision, recovery and ruggedness. The limits of detection and quantitation are 1.5% and 4.6%, respectively. The obtained results prove that the method is repeatable, sensitive and accurate. The proposed developed PXRD method can be applied for the quantitative analysis of mixtures of febuxostat polymorphs (forms A and G). PMID:25636167

  2. Versatile in situ powder X-ray diffraction cells for solid–gas investigations

    PubMed Central

    Jensen, Torben R.; Nielsen, Thomas K.; Filinchuk, Yaroslav; Jørgensen, Jens-Erik; Cerenius, Yngve; Gray, Evan MacA.; Webb, Colin J.

    2010-01-01

    This paper describes new sample cells and techniques for in situ powder X-ray diffraction specifically designed for gas absorption studies up to ca 300 bar (1 bar = 100 000 Pa) gas pressure. The cells are for multipurpose use, in particular the study of solid–gas reactions in dosing or flow mode, but can also handle samples involved in solid–liquid–gas studies. The sample can be loaded into a single-crystal sapphire (Al2O3) capillary, or a quartz (SiO2) capillary closed at one end. The advantages of a sapphire single-crystal cell with regard to rapid pressure cycling are discussed, and burst pressures are calculated and measured to be ∼300 bar. An alternative and simpler cell based on a thin-walled silicate or quartz glass capillary, connected to a gas source via a VCR fitting, enables studies up to ∼100 bar. Advantages of the two cell types are compared and their applications are illustrated by case studies. PMID:22477780

  3. 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

    2013-05-01

    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. PMID:23557375

  4. Decomposition of Spinel-Type Nickel Chromium Indium Sulfides—X-Ray Powder Structure Determination

    NASA Astrophysics Data System (ADS)

    Lutz, H. D.; Kringe, Ch.; Mohn, K.; Stingl, Th.

    1998-03-01

    The phase diagram of the quaternary system NiCr 2S 4-NiIn 2S 4-Cr 2S 3-In 2S 3has been studied at 873 and 1223 K by X-ray powder structure determination of quenched samples. At high temperatures, spinel-type Ni y(Cr 2-2 xIn 2 x) 1- yS 3-2 ysolid solutions are formed in a large range of composition ( y: 0-0.5, x: 0.3-1). At temperatures below 1183 K, these solid solutions decompose to Cr-rich and In-rich spinel-type sulfides, whereby nickel is enriched in the Cr-rich compounds. The decomposition of the spinel-type sulfides is greatly retarded, even at temperatures about 900 K, due to both thermodynamic and kinetic reasons. The cation distribution established corresponds to a site preference as Cr 3+>Ni 2+>In 3+at the octahedral 16d site and □ (vacancies)>In 3+>Ni 2+at the tetrahedral 8a site of the spinel structure. The metal-sulfur distances of the solid solutions refined are compared with those calculated from characteristic metal-sulfur distances in close-packed structures, taking into account the site occupation established. For the respective indium-sulfur distances, the following improved values are recommended: In tet-S=247.1 pm; In oct-S=260.6 pm.

  5. Adsorption height determination of nonequivalent C and O species of PTCDA on Ag(110) using x-ray standing waves

    NASA Astrophysics Data System (ADS)

    Mercurio, G.; Bauer, O.; Willenbockel, M.; Fairley, N.; Reckien, W.; Schmitz, C. H.; Fiedler, B.; Soubatch, S.; Bredow, T.; Sokolowski, M.; Tautz, F. S.

    2013-01-01

    The normal incidence x-ray standing wave (NIXSW) technique is used to determine the adsorption geometry of submonolayer 3,4,9,10-perylene tetracarboxylic dianhydride (PTCDA) adsorbed on the Ag(110) surface. An accurate analysis of both C1s and O1s photoemission (PE) spectra allows the respective adsorption heights of carbon and oxygen atoms in different chemical environments within PTCDA to be distinguished. Due to the intricacy of the PE fitting models, a systematic error analysis of NIXSW structural parameters was developed and employed. Based on the adsorption geometry of PTCDA on Ag(110) a bonding mechanism is discussed.

  6. Understanding the Adsorption Mechanism of Xe and Kr in a Metal-Organic Framework from X-ray Structural Analysis and First- Principles Calculations

    SciTech Connect

    Ghose, Sanjit K.; Li, Yan; Yakovenko, Andrey; Dooryhee, Eric; Ehm, Lars; Ecker, Lynne E.; Dippel, Ann-Christin; Halder, Gregory J.; Strachan, Denis M.; Thallapally, Praveen K.

    2015-04-16

    Enhancement of adsorption capacity and separation of radioactive Xe/Kr at room temperature and above is a challenging problem. Here, we report a detailed structural refinement and analysis of the synchrotron X-ray powder diffraction data of Ni-DODBC metal organic framework with in situ Xe and Kr adsorption at room temperature and above. Our results reveal that Xe and Kr adsorb at the open metal sites, with adsorption geometries well reproduced by DFT calculations. The measured temperature-dependent adsorption capacity of Xe is substantially larger than that for Kr, indicating the selectivity of Xe over Kr and is consistent with the more negative adsorption energy (dominated by van der Waals dispersion interactions) predicted from DFT. Our results reveal critical structural and energetic information about host–guest interactions that dictate the selective adsorption mechanism of these two inert gases, providing guidance for the design and synthesis of new MOF materials for the separation of environmentally hazardous gases from nuclear reprocessing applications.

  7. Application of focused-beam flat-sample method to synchrotron powder X-ray diffraction with anomalous scattering effect

    NASA Astrophysics Data System (ADS)

    Tanaka, M.; Katsuya, Y.; Matsushita, Y.

    2013-03-01

    The focused-beam flat-sample method (FFM), which is a method for high-resolution and rapid synchrotron X-ray powder diffraction measurements by combination of beam focusing optics, a flat shape sample and an area detector, was applied for diffraction experiments with anomalous scattering effect. The advantages of FFM for anomalous diffraction were absorption correction without approximation, rapid data collection by an area detector and good signal-to-noise ratio data by focusing optics. In the X-ray diffraction experiments of CoFe2O4 and Fe3O4 (By FFM) using X-rays near the Fe K absorption edge, the anomalous scattering effect between Fe/Co or Fe2+/Fe3+ can be clearly detected, due to the change of diffraction intensity. The change of observed diffraction intensity as the incident X-ray energy was consistent with the calculation. The FFM is expected to be a method for anomalous powder diffraction.

  8. Unmixing 40Ar/39Ar Muscovite Ages Using Powder X-ray Diffraction

    NASA Astrophysics Data System (ADS)

    McAleer, R. J.; Kunk, M. J.; Valley, P. M.; Walsh, G. J.; Bish, D. L.; Wintsch, R. P.

    2014-12-01

    Whole rock powder X-ray diffraction (XRD) experiments from eight samples collected across a retrograde ductile shear zone in the Devonian Littleton Formation near Claremont, NH, exhibit broad and asymmetric to bimodal muscovite 00l reflections. These composite 00l reflections exhibit a systematic change in shape with increasing retrograde strain. Microtextural relationships, electron microprobe quantitative analyses, and element mapping indicate that the change in peak shape reflects progressive dissolution of metastable Na-rich muscovite and the precipitation of stable Na-poor muscovite. 40Ar/39Ar step heating experiments on muscovite concentrates from these samples show a decrease in total gas age from 274 to 258 Ma as the highest strain zone is approached, and steps within individual spectra range in age by ~20 m.y. The correlation between age and 00l peak shape suggests that the argon isotopic system also tracks the dissolution-precipitation process. Furthermore, the variation in age during step heating indicates that these populations exhibit different in-vacuo degassing behavior. Comparison of whole rock and muscovite concentrate XRD patterns from the same samples shows that the mineral separation process can fractionate these muscovite populations. With this knowledge, four muscovite concentrates were prepared from a single hand sample, analyzed by XRD, and dated. Combining modal estimates from XRD experiments with total gas ages, the four splits narrowly define a mixing line that resolves end-member ages of 250 and 300 Ma for the neocrystallized and earlier high grade populations of muscovite, respectively. These ages are consistent with age data from all other samples. The results show that, in some settings, powder XRD provides a powerful and time effective method to both identify the existence of and establish the proportions of multiple compositional populations of muscovite prior to 40Ar/39Ar analysis. This approach will be especially useful in

  9. Quantitative determination of mineral composition by powder X-ray diffraction

    DOEpatents

    Pawloski, Gayle A.

    1986-01-01

    An external standard intensity ratio method is used for quantitatively determining mineralogic compositions of samples by x-ray diffraction. The method uses ratios of x-ray intensity peaks from a single run. Constants are previously determined for each mineral which is to be quantitatively measured. Ratios of the highest intensity peak of each mineral to be quantified in the sample and the highest intensity peak of a reference mineral contained in the sample are used to calculate sample composition.

  10. Quantitative determination of mineral composition by powder x-ray diffraction

    DOEpatents

    Pawloski, G.A.

    1984-08-10

    An external standard intensity ratio method is used for quantitatively determining mineralogic compositions of samples by x-ray diffraction. The method uses ratios of x-ray intensity peaks from a single run. Constants are previously determined for each mineral which is to be quantitatively measured. Ratios of the highest intensity peak of each mineral to be quantified in the sample and the highest intensity peak of a reference mineral contained in the sample are used to calculate sample composition.

  11. Adsorption of lipase on polypropylene powder.

    PubMed

    Gitlesen, T; Bauer, M; Adlercreutz, P

    1997-04-01

    Adsorption of different lipases by EP-100 polypropylene powder from crude and pure lipase preparations was studied. Langmuir isotherms described the adsorption equilibria well both for protein and lipase activity adsorption. Adsorption isotherms for five different proteins all gave a similar saturation level of 220 mg protein per g carrier. Twelve commercial lipase preparations were tested for selectivity in the adsorption of lipase. For all preparations the selectivity factor was larger than one. In a crude lipase preparation from Pseudomonas fluorescence, the specific activity in solution decreased by two orders of magnitude after adsorption. The adsorption was not significantly influenced by pH changes in the adsorption buffer, indicating that hydrophobic and not electrostatic interactions are the dominating adsorption forces. Adsorption of a crude lipase from Candida rugosa (Sigma) was fast and equilibrium was reached in 30 and 100 min for protein and lipase activity adsorption respectively. Desorption in aqueous solution was negligible. Investigations with seven different lipases showed no correlation between the specific lipolytic activity of dissolved enzyme in aqueous solution and the specific activity of adsorbed enzyme in an esterification reaction in organic solvent. PMID:9106498

  12. A flow-through x-ray absorption spectroscopy cell for characterization of powder catalysts in the working state

    NASA Astrophysics Data System (ADS)

    Odzak, J. F.; Argo, A. M.; Lai, F. S.; Gates, B. C.; Pandya, K.; Feraria, L.

    2001-10-01

    We report the design and demonstration of an x-ray absorption spectroscopy (XAS) cell used for the characterization of solid (powder) catalysts in operation with gas-phase reactants. The use of powder samples removes complications arising from mass transfer limitations in pressed wafer samples, the typical form of catalyst used in other in situ XAS cells. The new cell allows collection of XAS data at temperatures ranging from about 230 to 470 K, gas flow rates ranging from about 10 to 500 ml min-1, and pressures ranging from about 1 to 3 atm. The cell is designed to function nearly as a plug flow reactor.

  13. Hydrothermal synthesis of nanocrystalline ZnSe: An in situ synchrotron radiation X-ray powder diffraction study

    SciTech Connect

    Jorgensen, J.-E. Jensen, T.R.; Hanson, J.C.

    2008-08-15

    The hydrothermal synthesis of nanocrystalline ZnSe has been studied by in situ X-ray powder diffraction using synchrotron radiation. The formation of ZnSe was studied using the following starting mixtures: Zn+Se+H{sub 2}O (route A) and ZnCl{sub 2}+Se+H{sub 2}O+Na{sub 2}SO{sub 3} (route B). The route A experiment showed that Zn powder starts reacting with water at 134 deg. C giving ZnO and H{sub 2} followed by the formation of ZnSe which takes place in temperature range from 167 to 195 deg. C. The route B experiment shows a considerably more complex reaction path with several intermediate phases and in this case the formation of ZnSe starts at 141 deg. C and ZnSe and Se were the only crystalline phases observed at the end of the experiment where the temperature was 195 deg. C. The sizes of the nanocrystalline particles were determined to 18 and 9 nm in the route A and B experiments, respectively. Nanocrystalline ZnSe was also synthesized ex situ using the route A and B methods and characterized by conventional X-ray powder diffraction and transmission electron microscopy. An average crystalline domain size of ca. 8 nm was determined by X-ray powder diffraction in fair agreement with TEM images, which showed larger aggregates of nanoparticles having approximate diameters of 10 nm. Furthermore, a method for purification of the ZnSe nanoparticles was developed and the prepared particles showed signs of anisotropic size broadening of the diffraction peaks. - Graphical abstract: Stack of powder diagrams showing the formation of nanocrystalline ZnSe under hydrothermal conditions.

  14. Crystal engineering on industrial diaryl pigments using lattice energy minimizations and X-ray powder diffraction.

    PubMed

    Schmidt, Martin U; Dinnebier, Robert E; Kalkhof, Holger

    2007-08-23

    Diaryl azo pigments play an important role as yellow pigments for printing inks, with an annual pigment production of more than 50,000 t. The crystal structures of Pigment Yellow 12 (PY12), Pigment Yellow 13 (PY13), Pigment Yellow 14 (PY14), and Pigment Yellow 83 (PY83) were determined from X-ray powder data using lattice energy minimizations and subsequent Rietveld refinements. Details of the lattice energy minimization procedure and of the development of a torsion potential for the biphenyl fragment are given. The Rietveld refinements were carried out using rigid bodies, or constraints. It was also possible to refine all atomic positions individually without any constraint or restraint, even for PY12 having 44 independent non-hydrogen atoms per asymmetric unit. For PY14 (23 independent non-hydrogen atoms), additionally all atomic isotropic temperature factors could be refined individually. PY12 crystallized in a herringbone arrangement with twisted biaryl fragments. PY13 and PY14 formed a layer structure of planar molecules. PY83 showed a herringbone structure with planar molecules. According to quantum mechanical calculations, the twisting of the biaryl fragment results in a lower color strength of the pigments, whereas changes in the substitution pattern have almost no influence on the color strength of a single molecule. Hence, the experimentally observed lower color strength of PY12 in comparison with that of PY13 and PY83 can be explained as a pure packing effect. Further lattice energy calculations explained that the four investigated pigments crystallize in three different structures because these structures are the energetically most favorable ones for each compound. For example, for PY13, PY14, or PY83, a PY12-analogous crystal structure would lead to considerably poorer lattice energies and lower densities. In contrast, lattice energy calculations revealed that PY12 could adopt a PY13-type structure with only slightly poorer energy. This structure was

  15. Crystal Engineering on Industrial Diaryl Pigments Using Lattice Energy Minimizations and X-ray Powder Diffraction

    SciTech Connect

    Schmidt,M.; Dinnebier, R.; Kalkhof, H.

    2007-01-01

    Diaryl azo pigments play an important role as yellow pigments for printing inks, with an annual pigment production of more than 50,000 t. The crystal structures of Pigment Yellow 12 (PY12), Pigment Yellow 13 (PY13), Pigment Yellow 14 (PY14), and Pigment Yellow 83 (PY83) were determined from X-ray powder data using lattice energy minimizations and subsequent Rietveld refinements. Details of the lattice energy minimization procedure and of the development of a torsion potential for the biphenyl fragment are given. The Rietveld refinements were carried out using rigid bodies, or constraints. It was also possible to refine all atomic positions individually without any constraint or restraint, even for PY12 having 44 independent non-hydrogen atoms per asymmetric unit. For PY14 (23 independent non-hydrogen atoms), additionally all atomic isotropic temperature factors could be refined individually. PY12 crystallized in a herringbone arrangement with twisted biaryl fragments. PY13 and PY14 formed a layer structure of planar molecules. PY83 showed a herringbone structure with planar molecules. According to quantum mechanical calculations, the twisting of the biaryl fragment results in a lower color strength of the pigments, whereas changes in the substitution pattern have almost no influence on the color strength of a single molecule. Hence, the experimentally observed lower color strength of PY12 in comparison with that of PY13 and PY83 can be explained as a pure packing effect. Further lattice energy calculations explained that the four investigated pigments crystallize in three different structures because these structures are the energetically most favorable ones for each compound. For example, for PY13, PY14, or PY83, a PY12-analogous crystal structure would lead to considerably poorer lattice energies and lower densities. In contrast, lattice energy calculations revealed that PY12 could adopt a PY13-type structure with only slightly poorer energy. This structure was

  16. 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}.

  17. X-ray powder diffraction study of poly/carbon monofluoride/, CF/1.12/

    NASA Technical Reports Server (NTRS)

    Mahajan, V. K.; Badachhape, R. B.; Margrave, J. L.

    1974-01-01

    Data from X-ray diffraction studies of the poly(carbon monofluoride) with empirical formula CF(1.09-1.15) are reported, and possible intercalation arrangements for the substance are discussed. The data do not conform to true hexagonal symmetry, indicating that the carbon atoms are not coplanar. Each bond angle of carbon is 118.8 deg, and the carbon-carbon distance is 1.47 A. The interlayer distance is 5.76 A. A total absence of (hkl) reflections in the X-ray pattern shows that the separate CF layers are not regularly arranged with respect to one another.

  18. Hydrothermal Synthesis of Nanocrystalline ZnSe: An in situ Synchrotron Radiation X-ray Powder Diffraction Study

    SciTech Connect

    Joergensen,J.; Jensen, T.; Hanson, J.

    2008-01-01

    The hydrothermal synthesis of nanocrystalline ZnSe has been studied by in situ X-ray powder diffraction using synchrotron radiation. The formation of ZnSe was studied using the following starting mixtures: Zn+Se+H2O (route A) and ZnCl2+Se+H2O+Na2SO3 (route B). The route A experiment showed that Zn powder starts reacting with water at 134 C giving ZnO and H2 followed by the formation of ZnSe which takes place in temperature range from 167 to 195 C. The route B experiment shows a considerably more complex reaction path with several intermediate phases and in this case the formation of ZnSe starts at 141 C and ZnSe and Se were the only crystalline phases observed at the end of the experiment where the temperature was 195 C. The sizes of the nanocrystalline particles were determined to 18 and 9 nm in the route A and B experiments, respectively. Nanocrystalline ZnSe was also synthesized ex situ using the route A and B methods and characterized by conventional X-ray powder diffraction and transmission electron microscopy. An average crystalline domain size of ca. 8 nm was determined by X-ray powder diffraction in fair agreement with TEM images, which showed larger aggregates of nanoparticles having approximate diameters of 10 nm. Furthermore, a method for purification of the ZnSe nanoparticles was developed and the prepared particles showed signs of anisotropic size broadening of the diffraction peaks.

  19. Adsorption of Uranyl ions on Amine-functionalization of MIL-101(Cr) Nanoparticles by a Facile Coordination-based Post-synthetic strategy and X-ray Absorption Spectroscopy Studies

    PubMed Central

    Zhang, Jian-Yong; Zhang, Na; Zhang, Linjuan; Fang, Yongzheng; Deng, Wei; Yu, Ming; Wang, Ziqiang; Li, Lina; Liu, Xiyan; Li, Jingye

    2015-01-01

    By a facile coordination-based post-synthetic strategy, the high surface area MIL-101(Cr) nanoparticles was functionallized by grafting amine group of ethylenediamine (ED) on coordinatively unsaturated Cr(III) centers, yielding a series of ED-MIL-101(Cr)-based adsorbents and their application for adsorption of U(VI) from aqueous solution were also studied. The obtained ED-functionallized samples with different ED contents were characterized by powder X-ray diffraction (PXRD), scanning electron microscope (SEM), energy dispersive X-ray spectroscopy (EDX), FTIR, elemental analysis (EA) and N2 adsorption and desorption isothermal. Compared with the pristine MIL-101(Cr) sorbents, the ED-functionallized MIL-101(Cr) exhibits significantly higher adsorption capacity for U(VI) ions from water with maximum adsorption capacities as high as 200 mg/g (corresponding to 100% extraction rate) at pH of 4.5 with ED/Cr ratio of 0.68 and the sorbed U(VI) ions can easily be desorbed at lower pH (pH ≤ 2.0). The adsorption mode of U(VI) ions and effects of grafted ED on the MIL-101(Cr) frameworks were also been studied by X-ray absorption spectroscopy (XAS). We believe that this work establishes a simple and energy efficient route to a novel type of functional materials for U(VI) ions extraction from solution via the post-synthetic modification (PSM) strategy. PMID:26354407

  20. Adsorption of Uranyl ions on Amine-functionalization of MIL-101(Cr) Nanoparticles by a Facile Coordination-based Post-synthetic strategy and X-ray Absorption Spectroscopy Studies

    NASA Astrophysics Data System (ADS)

    Zhang, Jian-Yong; Zhang, Na; Zhang, Linjuan; Fang, Yongzheng; Deng, Wei; Yu, Ming; Wang, Ziqiang; Li, Lina; Liu, Xiyan; Li, Jingye

    2015-09-01

    By a facile coordination-based post-synthetic strategy, the high surface area MIL-101(Cr) nanoparticles was functionallized by grafting amine group of ethylenediamine (ED) on coordinatively unsaturated Cr(III) centers, yielding a series of ED-MIL-101(Cr)-based adsorbents and their application for adsorption of U(VI) from aqueous solution were also studied. The obtained ED-functionallized samples with different ED contents were characterized by powder X-ray diffraction (PXRD), scanning electron microscope (SEM), energy dispersive X-ray spectroscopy (EDX), FTIR, elemental analysis (EA) and N2 adsorption and desorption isothermal. Compared with the pristine MIL-101(Cr) sorbents, the ED-functionallized MIL-101(Cr) exhibits significantly higher adsorption capacity for U(VI) ions from water with maximum adsorption capacities as high as 200 mg/g (corresponding to 100% extraction rate) at pH of 4.5 with ED/Cr ratio of 0.68 and the sorbed U(VI) ions can easily be desorbed at lower pH (pH ≤ 2.0). The adsorption mode of U(VI) ions and effects of grafted ED on the MIL-101(Cr) frameworks were also been studied by X-ray absorption spectroscopy (XAS). We believe that this work establishes a simple and energy efficient route to a novel type of functional materials for U(VI) ions extraction from solution via the post-synthetic modification (PSM) strategy.

  1. Crystal structure of anhydrous tripotassium citrate from laboratory X-ray powder diffraction data and DFT comparison

    PubMed Central

    Rammohan, Alagappa; Kaduk, James A.

    2016-01-01

    The crystal structure of anhydrous tripotassium citrate, [K3(C6H5O7)]n, has been solved and refined using laboratory X-ray powder diffraction data, and optimized using density functional techniques. The three unique potassium cations are 6-, 8-, and 6-coordinate (all irregular). The [KOn] coordination polyhedra share edges and corners to form a three-dimensional framework, with channels running parallel to the c axis. The only hydrogen bond is an intra­molecular one involving the hy­droxy group and the central carboxyl­ate group, with graph-set motif S(5). PMID:27536403

  2. Crystal structure of anhydrous tripotassium citrate from laboratory X-ray powder diffraction data and DFT comparison.

    PubMed

    Rammohan, Alagappa; Kaduk, James A

    2016-08-01

    The crystal structure of anhydrous tripotassium citrate, [K3(C6H5O7)] n , has been solved and refined using laboratory X-ray powder diffraction data, and optimized using density functional techniques. The three unique potassium cations are 6-, 8-, and 6-coordinate (all irregular). The [KO n ] coordination polyhedra share edges and corners to form a three-dimensional framework, with channels running parallel to the c axis. The only hydrogen bond is an intra-molecular one involving the hy-droxy group and the central carboxyl-ate group, with graph-set motif S(5). PMID:27536403

  3. Adsorption of uranium(VI) to manganese oxides: X-ray absorption spectroscopy and surface complexation modeling.

    PubMed

    Wang, Zimeng; Lee, Sung-Woo; Catalano, Jeffrey G; Lezama-Pacheco, Juan S; Bargar, John R; Tebo, Bradley M; Giammar, Daniel E

    2013-01-15

    The mobility of hexavalent uranium in soil and groundwater is strongly governed by adsorption to mineral surfaces. As strong naturally occurring adsorbents, manganese oxides may significantly influence the fate and transport of uranium. Models for U(VI) adsorption over a broad range of chemical conditions can improve predictive capabilities for uranium transport in the subsurface. This study integrated batch experiments of U(VI) adsorption to synthetic and biogenic MnO(2), surface complexation modeling, ζ-potential analysis, and molecular-scale characterization of adsorbed U(VI) with extended X-ray absorption fine structure (EXAFS) spectroscopy. The surface complexation model included inner-sphere monodentate and bidentate surface complexes and a ternary uranyl-carbonato surface complex, which was consistent with the EXAFS analysis. The model could successfully simulate adsorption results over a broad range of pH and dissolved inorganic carbon concentrations. U(VI) adsorption to synthetic δ-MnO(2) appears to be stronger than to biogenic MnO(2), and the differences in adsorption affinity and capacity are not associated with any substantial difference in U(VI) coordination. PMID:23227949

  4. Adsorption-site investigation of Rb/Cu(111) using the x-ray standing-wave method

    NASA Astrophysics Data System (ADS)

    Shi, X.; Su, C.; Heskett, D.; Berman, L.; Kao, C. C.; Bedzyk, M. J.

    1994-05-01

    We have carried out a back reflection x-ray standing-wave investigation to study the adsorbate-substrate bond length and bonding site for the system Rb/Cu(111). Our low-energy electron diffraction study showed an ordered (2×2) phase for one monolayer of Rb on Cu(111) (θ=0.25). By measuring both the (111) and (111¯) Bragg reflections at this coverage, we determine the Rb adsorption to be in the top site. We observe a high degree of order in the Rb overlayer perpendicular to the surface, with large disorder parallel to the surface.

  5. An in situ and operando X-ray absorption spectroscopy setup for measuring sub-monolayer model and powder catalysts.

    PubMed

    Weiher, Norbert; Bus, Eveline; Gorzolnik, Blazej; Möller, Martin; Prins, Roel; van Bokhoven, Jeroen Anton

    2005-09-01

    A new spectroscopic cell has been designed for studying model catalysts using in situ or operando X-ray absorption spectroscopy. The setup allows gas treatment and can be used between 100 and 870 K. Pressures from 10(-3) Pa up to 300 kPa can be applied. Measurements on model systems in this particular pressure range are a valuable extension of the commonly used UHV characterization techniques. Using this setup, we were able to analyze the Au L3 EXAFS of a silica wafer covered with sub-monolayer concentrations of gold (0.05 ML). By modifying the sample holder, powder catalysts can also be analyzed under plug-flow conditions. As an example, the reduction of a Au/SiO2 powder catalyst prepared from HAuCl4 was followed. PMID:16120994

  6. Azine bridged silver coordination polymers: Powder X-ray diffraction route to crystal structure determination of silver benzotriazole

    SciTech Connect

    Rajeswaran, Manju . E-mail: manju.rajeswaran@kodak.com; Blanton, Thomas N.; Giesen, David J.; Whitcomb, David R.; Zumbulyadis, Nicholas; Antalek, Brian J.; Neumann, Marcus M.; Misture, Scott T.

    2006-04-15

    In continuation of our interest in solid-state structures of silver complexes of photographic importance, the structure for silver benzotriazole (AgBZT), has now been obtained. The preferred method for solving crystal structures is via single-crystal X-ray diffraction (XRD). However, for some materials, growing single crystals of appropriate size and quality is often difficult or even impossible. AgBZT is an example of such a silver complex with poor solubility. The usual routes to preparing single crystals using recrystallization from a cooperating solvent resulted in polycrystalline powder samples. We propose a crystal structure for AgBZT, solved from synchrotron X-ray powder diffraction data, using a direct-space Monte Carlo simulated annealing approach. AgBZT crystals are monoclinic (P2{sub 1} /c), with unit cell dimensions, a=14.8052(3) A, b=3.7498(4) A, c=12.3495(12) A, and {beta}=114.200(6){sup o}. The AgBZT complex is constructed from all three of the Benzotriazole (BZT) nitrogens bonding to a separate silver atom. As a consequence of this bonding mode, the structure is a highly cross-linked, coordination polymer.

  7. Structural analysis of lead magnesium niobate using synchrotron powder X-ray diffraction and the Rietveld method.

    PubMed

    Bhakar, Ashok; Pandey, Adityanarayan H; Singh, M N; Upadhyay, Anuj; Sinha, A K; Gupta, S M; Ganguli, Tapas

    2016-06-01

    The room-temperature synchrotron powder X-ray diffraction pattern of the single phase perovskite lead magnesium niobate (PMN) has shown significant broadening in the q range ∼ 5-7 Å(-1) compared with standard LaB6 synchrotron powder X-ray diffraction data, taken under similar conditions. This broadening/asymmetry lies mainly towards the lower 2θ side of the Bragg peaks. Attempts to fit this data with the paraelectric cubic phase (Pm\\bar 3m) and the local rhombohedral phase (R3m) corresponding to polar nanoregions (PNRs) are made using the Rietveld method. Rietveld refinements show that neither cubic (Pm\\bar 3m) nor rhombohedral (R3m) symmetry can fit this XRD pattern satisfactorily. The two-phase refinement fits the experimental data satisfactorily and suggests that the weight percentage of the PNRs is approximately 12-16% at room temperature. The unit-cell volume of these rhombohedral PNRs is approximately 0.15% larger than that of the unit cell volume of the paraelectric cubic phase. PMID:27240772

  8. A powder X-ray diffraction method for detection of polyprenylated benzophenones in plant extracts associated with HPLC for quantitative analysis.

    PubMed

    Martins, Felipe T; dos Santos, Marcelo H; Coelho, Carla P; Barbosa, Luiz C A; Dias, Gizelly C; Fracca, Mônica P; Neves, Person P; Stringheta, Paulo C; Doriguetto, Antônio C

    2011-02-20

    A robust, direct, rapid and non-destructive X-ray diffraction crystallography method to detect the polyprenylated benzophenones 7-epi-clusianone (1) and guttiferone A (2) in extracts from Garcinia brasiliensis is presented. Powder samples of benzophenones 1 and 2, dried hexane extracts from G. brasiliensis seeds and fruit's pericarp, and the dried ethanolic extract from G. brasiliensis seeds were unambiguously characterized by powder X-ray diffractometry. The calculated X-ray diffraction peaks from crystal structures of analytes 1 and 2, previously determined by single-crystal X-ray diffraction technique, were overlaid to those of the experimental powder diffractograms, providing a practical identification of these compounds in the analyzed material and confirming the pure contents of the powder samples. Using the X-ray diffraction crystallography method, the studied polyprenylated benzophenones were selectively and simultaneously detected in the extracts which were mounted directly on sample holder. In addition, reference materials of the analytes were not required for analyses since the crystal structures of the compounds are known. High performance liquid chromatography analyses also were comparatively carried out to quantify the analytes in the same plant extracts showing to be in agreement with X-ray diffraction crystallography method. PMID:20943341

  9. Adsorption of halide anions at the Pt(111)-solution interfacestudied by in situ surface x-ray scattering

    NASA Astrophysics Data System (ADS)

    Lucas, C. A.; Marković, N. M.; Ross, P. N.

    1997-03-01

    In this paper we present x-ray scattering results of iodide, bromide, and chloride adsorption onto the Pt(111) surface in solution. Iodide forms two commensurate adlayer structures, a (7×7)R19.1° phase and a hexagonal (3×3) phase, which coexist on the Pt surface. Formation of the (3×3) phase appears to be kinetically limited, whereas the 7 phase shows a hysteretic effect as a function of the electrode potential, associated with an order-disorder transition. Bromide forms a series of high-order commensurate structures on Pt(111) that are poorly ordered unless the size of the unit cell is small. No ordered structures for chloride adsorption are observed and specular x-ray reflectivity results suggest that the chloride coverage at low potential is too small to form a close-packed monolayer on the surface. The differences between the structures formed by the adsorbed anions, and the differences between results for Pt(111) and Au(111), are discussed in terms of the strength of the metal-halide interaction.

  10. Diaplectic Glass Content in Experimentally Shock-loaded Quartz Determined by X-Ray Powder Diffraction

    NASA Technical Reports Server (NTRS)

    Skala, R.; Hoerz, F.; Langenhorst, F.

    2003-01-01

    Quartz is the most common mineral of terrestrial crustal rocks and thus a widespread indicator for impact cratering and associated shock metamorphism. Planar deformation features (PDFs) are among the most prominent and diagnostic shock features in quartz and they represent thin lamellae of glass that formed via solid-state transformations. This socalled 'diaplectic' glass becomes pervasive at higher pressures and results in optically isotropic and X-ray-amorphous phases that resemble texturally the original quartz grains (without evidence of melt flow). In the past, it has been shown that the amount of this amorphous material in experimentally shock-loaded quartz correlates with peak shock pressure. Both reports derive the glass content from density measurements of individual crystals employing the equation X(%) = (rho(sub x) - rho(sub 0))/(rho(sub x) - rho(sub gl)), where x and 0 stands for X-ray and average (optical) density, respectively. The density of glass, rho(sub gl), was adopted as 2.2 g/cu cm. Though the same procedures had been applied, the resulting glass content differs significantly among the above studies. In the present study, we are using a new approach based solely on the integral intensity of a single, carefully selected reflection in the XRD pattern, and we will compare our data to those reported in the literature.

  11. Efficiency of Lu 2SiO 5:Ce (LSO) powder phosphor as X-ray to light converter under mammographic imaging conditions

    NASA Astrophysics Data System (ADS)

    David, S.; Michail, C.; Valais, I.; Nikolopoulos, D.; Liaparinos, P.; Kalivas, N.; Kalatzis, I.; Toutountzis, A.; Efthimiou, N.; Loudos, G.; Sianoudis, I.; Cavouras, D.; Dimitropoulos, N.; Nomicos, C. D.; Kandarakis, I.; Panayiotakis, G. S.

    2007-02-01

    The aim of the present study was to examine the light emission efficiency of Lu 2SiO 5:Ce (LSO) powder scintillator under X-ray mammographic imaging conditions. Powder LSO scintillator has never been used in X-ray imaging. For the purposes of the present study, a 25 mg/cm 2 thick scintillating screen was prepared in our laboratory, by sedimentation of Lu 2SiO 5:Ce powder. Absolute luminescence efficiency measurements were performed within the range of X-ray tube voltages (22-49 kVp) used in mammographic applications. Parameters related to X-ray detection, i.e. the energy absorption efficiency (EAE) and the quantum detection efficiency (QDE) were calculated. A theoretical model, describing radiation and light transfer, was employed to fit experimental data and to estimate values of the intrinsic conversion efficiency and the light attenuation coefficients of the screen. The spectral compatibility of the LSO powder scintillator to mammographic X-ray films and to various electronic optical detectors was determined by performing light emission spectrum measurements and by taking into account the spectral sensitivity of the optical detectors. Results in the voltage range used in mammography showed that Lu 2SiO 5:Ce powder scintillator has approximately 10% higher values of QDE and 4.5% higher values of EAE than Gd 2O 2S:Tb.

  12. Effect of Stacking Faults on the X-Ray Diffraction Profiles of Beta-SiC Powders

    NASA Technical Reports Server (NTRS)

    Pujar, Vijay V.; Cawley, James D.; Levine, Stanley R. (Technical Monitor)

    1995-01-01

    X-ray diffraction patterns or beta-SiC (3C or the cubic polytype or sic) powders often exhibit an additional peak at d = 0.266 nm, high background intensity around the (111) peak, and relative intensities for peaks which differ from those predicted from the crystal structure. Computer simulations were used to show that all these features are due to stacking faults in the powders and not due to the presence of other polytypes in the powders. Such simulations allow diffraction patterns to be generated for different types, frequencies, and spatial distribution or faults. Comparison of the simulation results to the XRD data indicates that the B-SiC particles consist either of heavily faulted clusters distributed irregularly between regions that have only occasional faults or twins, or the powders consist of two types of particles with different populations of faults: those with a high density of faults and those with only twins or occasional faults. Additional information is necessary to determine which description is correct. However, the simulation results can be used to rule out certain fault configurations.

  13. A new analysis of X-ray adsorption branching ratios: Use of Russell Saunders coupling

    NASA Astrophysics Data System (ADS)

    Bagus, Paul S.; Freund, Hajo; Kuhlenbeck, Helmut; Ilton, Eugene S.

    2008-04-01

    The intensities of X-ray absorption peaks at core-level edges are considered in terms of Russell-Saunders multiplets. The contributions of different multiplets to the relativistic wavefunctions of the excited states are determined and the absorption intensity related to the contributions of the dipole allowed multiplets. This is a powerful method because the selection rules for multiplets are stronger than for relativistic J levels. It is also shown that differences in the radial extent of the spin-orbit split core spinors modify the intensity given by these symmetry arguments. Applications are considered for cases involving different degrees of Russell-Saunders or j- j coupling.

  14. An X-ray absorption study of synthesis- and As adsorption-induced microstructural modifications in Fe oxy-hydroxides.

    PubMed

    Pinakidou, F; Katsikini, M; Simeonidis, K; Paloura, E C; Mitrakas, M

    2015-11-15

    Synthetic adsorbents based on Fe oxy-hydroxides (FeOOH) prepared under a wide range of pH-values via intense oxidation conditions of FeSO4 as well as the As(III) and As(V) adsorption mechanism are investigated using X-ray absorption fine structure (XAFS) spectroscopies at the Fe- and As-K-edges. Synthesis in an alkaline environment promotes the face-connectivity of the Fe(O,OH)6 chains at the expense of edge- and corner-sharing linkage, which is consistent with the lower surface charge density and in turn with the lower arsenic adsorption capacity. Microstructural changes are also detected after As(V) adsorption onto FeOOH synthesized at pH 5.5: the ratio of face-/edge-sharing sites increases from approximately 0.4-0.7 as a function of the As(V)-loading. This modification of the polymeric Fe(O,OH)6 structure at higher As/Fe ratios is attributed to strong As(V) bidentate mononuclear ((2)E) and binuclear ((2)C) adsorption. In contrast, no alterations in the FeOOH microstructure were observed, possibly due to the weaker (2)E linkage of As(III). PMID:26057444

  15. Complementing high-throughput X-ray powder diffraction data with quantum-chemical calculations: Application to piroxicam form III.

    PubMed

    Naelapää, Kaisa; van de Streek, Jacco; Rantanen, Jukka; Bond, Andrew D

    2012-11-01

    High-throughput crystallisation and characterisation platforms provide an efficient means to carry out solid-form screening during the pre-formulation phase. To determine the crystal structures of identified new solid phases, however, usually requires independent crystallisation trials to produce single crystals or bulk samples of sufficient quantity to carry out high-quality X-ray diffraction measurements. This process could be made more efficient by a robust procedure for crystal structure determination directly from high-throughput X-ray powder diffraction (XRPD) data. Quantum-chemical calculations based on dispersion-corrected density functional theory (DFT-D) have now become feasible for typical small organic molecules used as active pharmaceutical ingredients. We demonstrate how these calculations can be applied to complement high-throughput XRPD data by determining the crystal structure of piroxicam form III. These combined experimental/quantum-chemical methods can provide access to reliable structural information in the course of an intensive experimentally based solid-form screening activity or in other circumstances wherein single crystals might never be viable, for example, for polymorphs obtained only during high-energy processing such as spray drying or milling. PMID:22886472

  16. A nimesulide derivative with potential anti-inflammatory activity: Synthesis, X-ray powder structure analysis and DFT study

    NASA Astrophysics Data System (ADS)

    Bhattacharya, Abir; Kankanala, Kavitha; Pal, Sarbani; Mukherjee, Alok K.

    2010-06-01

    A nimesulide derivative, N-[4-(2,5-dioxo-2,5-dihydropyrrol-1-yl)-2-phenoxyphenyl]methanesulfonamide ( 2), was synthesized and its crystal structure has been determined from X-ray powder diffraction data following direct-space global optimization technique and refined by the Rietveld method. The molecular geometry and electronic structure of the title compound were calculated at the DFT level using the hybrid exchange-correlation functional, BLYP. The optimized molecular geometry of 2 corresponds closely to that obtained from the X-ray structure analysis. Intermolecular N-H···O and C-H···O hydrogen bonds in 2 form one-dimensional polymeric chains of R22(8) rings propagating along the [1 0 0] direction. Further linking between parallel chains via C-H···π (arene) hydrogen bonds generates a two-dimensional supramolecular assembly in the (1 1 0) plane. The title compound exhibits potential anti-inflammatory activity and can induce 64% edema inhibition in rat paws.

  17. Thermal analysis, X-ray powder diffraction and electron microscopy data related with the production of 1:1 Caffeine:Glutaric Acid cocrystals.

    PubMed

    Duarte, Íris; Andrade, Rita; Pinto, João F; Temtem, Márcio

    2016-09-01

    The data presented in this article are related to the production of 1:1 Caffeine:Glutaric Acid cocrystals as part of the research article entitled "Green production of cocrystals using a new solvent-free approach by spray congealing" (Duarte et al., 2016) [1]. More specifically, here we present the thermal analysis and the X-ray powder diffraction data for pure Glutaric Acid, used as a raw material in [1]. We also include the X-ray powder diffraction and electron microscopy data obtained for the 1:1 Caffeine:Glutaric Acid cocrystal (form II) produced using the cooling crystallization method reported in "Operating Regions in Cooling Cocrystallization of Caffeine and Glutaric Acid in Acetonitrile" (Yu et al., 2010) [2]. Lastly, we show the X-ray powder diffraction data obtained for assessing the purity of the 1:1 Caffeine:Glutaric cocrystals produced in [1]. PMID:27331096

  18. Rb+ adsorption at the quartz(101)-aqueous interface: comparison of resonant anomalous x-ray reflectivity with ab initio calculations

    DOE PAGESBeta

    Bellucci, Francesco; Lee, Sang Soo; Kubicki, James D.; Bandura, Andrei V.; Zhang, Zhan; Wesolowski, David J.; Fenter, Paul

    2015-01-29

    We study adsorption of Rb+ to the quartz(101)–aqueous interface at room temperature with specular X-ray reflectivity, resonant anomalous X-ray reflectivity, and density functional theory. The interfacial water structures observed in deionized water and 10 mM RbCl solution at pH 9.8 were similar, having a first water layer at height of 1.7 ± 0.1 Å above the quartz surface and a second layer at 4.8 ± 0.1 Å and 3.9 ± 0.8 Å for the water and RbCl solutions, respectively. The adsorbed Rb+ distribution is broad and consists of presumed inner-sphere (IS) and outer-sphere (OS) complexes at heights of 1.8 ±more » 0.1 and 6.4 ± 1.0 Å, respectively. Projector-augmented planewave density functional theory (DFT) calculations of potential configurations for neutral and negatively charged quartz(101) surfaces at pH 7 and 12, respectively, reveal a water structure in agreement with experimental results. These DFT calculations also show differences in adsorbed speciation of Rb+ between these two conditions. At pH 7, the lowest energy structure shows that Rb+ adsorbs dominantly as an IS complex, whereas at pH 12 IS and OS complexes have equivalent energies. The DFT results at pH 12 are generally consistent with the two site Rb distribution observed from the X-ray data at pH 9.8, albeit with some differences that are discussed. In conclusion, surface charge estimated on the basis of the measured total Rb+ coverage was -0.11 C/m2, in good agreement with the range of the surface charge magnitudes reported in the literature.« less

  19. Observation of localized heating phenomena during microwave heating of mixed powders using in situ x-ray diffraction technique

    SciTech Connect

    Sabelström, N. Hayashi, M.; Watanabe, T.; Nagata, K.

    2014-10-28

    In materials processing research using microwave heating, there have been several observations of various phenomena occurring known as microwave effects. One significant example of such a phenomenon is increased reaction kinetics. It is believed that there is a possibility that this might be caused by localized heating, were some reactants would attain a higher than apparent temperature. To examine whether such thermal gradients are indeed possible, mixed powders of two microwave non-absorbers, alumina and magnesia, were mixed with graphite, a known absorber, and heated in a microwave furnace. During microwave irradiation, the local temperatures of the respective sample constituents were measured using an in situ x-ray diffraction technique. In the case of the alumina and graphite sample, a temperature difference of around 100 °C could be observed.

  20. Crystal structure and electronic properties of two nimesulide derivatives: A combined X-ray powder diffraction and quantum mechanical study

    NASA Astrophysics Data System (ADS)

    Bhattacharya, Abir; Ghosh, Soumen; Kankanala, Kavitha; Reddy, Vangala Ranga; Mukkanti, Khagga; Pal, Sarbani; Mukherjee, Alok K.

    2010-06-01

    Crystal structures of two nimesulide derivatives, C 13H 14O 3N 2S ( 2) and C 21H 16O 5N 2S ( 3), have been determined from X-ray powder diffraction data and their electronic structures were calculated at the DFT level. The optimized molecular geometries of 2 and 3 correspond closely to that obtained from the crystallographic analysis. Intermolecular hydrogen bonds and π… π stacking interactions form supramolecular assembly in both compounds. The HOMO-LUMO energy gap (>2.2 eV) indicates a high kinetic stability of both compounds. Although the compound 2 does not exhibit any anti-inflammatory activity, 3 can induce 34% edema inhibition in rat paws.

  1. Determining fine-structure parameters for tungsten powder and filings by harmonic analysis of x-ray diffraction lines

    SciTech Connect

    Kravchik, A.E.; Moshkina, T.I.; Osmakov, A.S.

    1986-12-01

    Evidence has been accumulating on determining fine-structure parameters by line shape harmonic analysis (LSHA) although many aspects remain unresolved. In this paper, the authors discuss the interpretations afresh, on-going improvements in x-ray techniques, in recording methods, and in processing the data, as well as in programs for determining the parameters by LSHA. The authors selected tungsten because of its bcc lattice, whose diffraction peaks are widely separated, which almost completely rules out their overlapping even if there is considerable broadening, such as is produced by large plastic strain. The material was produced in two ways: by firing a tungsten single crystal and by grinding VChDK tungsten powder in a laboratory vibration mill for 10, 20, 30, 50, and 100 h.

  2. High-temperature dehydration of talc: a kinetics study using in situ X-ray powder diffraction

    NASA Astrophysics Data System (ADS)

    Wang, Duojun; Yi, Li; Huang, Bojin; Liu, Chuanjiang

    2015-06-01

    High-temperature in situ X-ray powder diffraction patterns were used to study the dehydration kinetics of natural talc with a size of 10-15 µm. The talc was annealed from 1073 to 1223 K, and the variations in the characteristic peaks corresponding to talc with the time were recorded to determine the reaction progress. The decomposition of talc occurred, and peaks corresponding to talc and peaks corresponding to enstatite and quartz were observed. The enstatite and talc exhibited a topotactic relationship. The dehydration kinetics of talc was studied as a function of temperature between 1073 and 1223 K. The kinetics data could be modeled using an Avrami equation that considers nucleation and growth processes ? where n varies from 0.4 to 0.8. The rate constant (k) equation for the natural talc is ? The reaction mechanism for the dehydration of talc is a heterogeneous nucleation and growth mechanism.

  3. An Implementation of the Fundamental Parameters Approach for Analysis of X-ray Powder Diffraction Line Profiles.

    PubMed

    Mendenhall, Marcus H; Mullen, Katharine; Cline, James P

    2015-01-01

    This work presents an open implementation of the Fundamental Parameters Approach (FPA) models for analysis of X-ray powder diffraction line profiles. The original literature describing these models was examined and code was developed to allow for their use within a Python based least squares refinement algorithm. The NIST interest in the FPA method is specific to its ability to account for the optical aberrations of the powder diffraction experiment allowing for an accurate assessment of lattice parameter values. Lattice parameters are one of the primary certified measurands of NIST Standard Reference Materials (SRMs) for powder diffraction. Lattice parameter values obtained from analysis of data from SRMs 640e and 660c using both the NIST FPA Python code and the proprietary, commercial code Topas, that constitutes the only other actively supported, complete implementation of FPA models within a least-squares data analysis environment, agreed to within 2 fm. This level of agreement demonstrates that both the NIST code and Topas constitute an accurate implementation of published FPA models. PMID:26958448

  4. An Implementation of the Fundamental Parameters Approach for Analysis of X-ray Powder Diffraction Line Profiles

    PubMed Central

    Mendenhall, Marcus H.; Mullen, Katharine; Cline, James P.

    2015-01-01

    This work presents an open implementation of the Fundamental Parameters Approach (FPA) models for analysis of X-ray powder diffraction line profiles. The original literature describing these models was examined and code was developed to allow for their use within a Python based least squares refinement algorithm. The NIST interest in the FPA method is specific to its ability to account for the optical aberrations of the powder diffraction experiment allowing for an accurate assessment of lattice parameter values. Lattice parameters are one of the primary certified measurands of NIST Standard Reference Materials (SRMs) for powder diffraction. Lattice parameter values obtained from analysis of data from SRMs 640e and 660c using both the NIST FPA Python code and the proprietary, commercial code Topas, that constitutes the only other actively supported, complete implementation of FPA models within a least-squares data analysis environment, agreed to within 2 fm. This level of agreement demonstrates that both the NIST code and Topas constitute an accurate implementation of published FPA models. PMID:26958448

  5. Three-dimensional electron diffraction as a complementary technique to powder X-ray diffraction for phase identification and structure solution of powders

    PubMed Central

    Yun, Yifeng; Zou, Xiaodong; Hovmöller, Sven; Wan, Wei

    2015-01-01

    Phase identification and structure determination are important and widely used techniques in chemistry, physics and materials science. Recently, two methods for automated three-dimensional electron diffraction (ED) data collection, namely automated diffraction tomography (ADT) and rotation electron diffraction (RED), have been developed. Compared with X-ray diffraction (XRD) and two-dimensional zonal ED, three-dimensional ED methods have many advantages in identifying phases and determining unknown structures. Almost complete three-dimensional ED data can be collected using the ADT and RED methods. Since each ED pattern is usually measured off the zone axes by three-dimensional ED methods, dynamic effects are much reduced compared with zonal ED patterns. Data collection is easy and fast, and can start at any arbitrary orientation of the crystal, which facilitates automation. Three-dimensional ED is a powerful technique for structure identification and structure solution from individual nano- or micron-sized particles, while powder X-ray diffraction (PXRD) provides information from all phases present in a sample. ED suffers from dynamic scattering, while PXRD data are kinematic. Three-dimensional ED methods and PXRD are complementary and their combinations are promising for studying multiphase samples and complicated crystal structures. Here, two three-dimensional ED methods, ADT and RED, are described. Examples are given of combinations of three-dimensional ED methods and PXRD for phase identification and structure determination over a large number of different materials, from Ni–Se–O–Cl crystals, zeolites, germanates, metal–organic frameworks and organic compounds to intermetallics with modulated structures. It is shown that three-dimensional ED is now as feasible as X-ray diffraction for phase identification and structure solution, but still needs further development in order to be as accurate as X-ray diffraction. It is expected that three-dimensional ED

  6. X-ray Absorption Spectroscopic Quantification and Speciation Modeling of Sulfate Adsorption on Ferrihydrite Surfaces.

    PubMed

    Gu, Chunhao; Wang, Zimeng; Kubicki, James D; Wang, Xiaoming; Zhu, Mengqiang

    2016-08-01

    Sulfate adsorption on mineral surfaces is an important environmental chemical process, but the structures and respective contribution of different adsorption complexes under various environmental conditions are unclear. By combining sulfur K-edge XANES and EXAFS spectroscopy, quantum chemical calculations, and surface complexation modeling (SCM), we have shown that sulfate forms both outer-sphere complexes and bidentate-binuclear inner-sphere complexes on ferrihydrite surfaces. The relative fractions of the complexes vary with pH, ionic strength (I), and sample hydration degree (wet versus air-dried), but their structures remained the same. The inner-sphere complex adsorption loading decreases with increasing pH while remaining unchanged with I. At both I = 0.02 and 0.1 M, the outer-sphere complex loading reaches maximum at pH ∼5 and then decreases with pH, whereas it monotonically decreases with pH at I = 0.5 M. These observations result from a combination of the ionic-strength effect, the pH dependence of anion adsorption, and the competition between inner- and outer-sphere complexation. Air-drying drastically converts the outer-sphere complexes to the inner-sphere complexes. The respective contributions to the overall adsorption loading of the two complexes were directly modeled with the extended triple layer SCM by implementing the bidentate-binuclear inner-sphere complexation identified in the present study. These findings improve our understanding of sulfate adsorption and its effects on other environmental chemical processes and have important implications for generalizing the adsorption behavior of anions forming both inner- and outer-sphere complexes on mineral surfaces. PMID:27377619

  7. X-Ray Diffraction.

    ERIC Educational Resources Information Center

    Smith, D. K.; Smith, K. L.

    1980-01-01

    Reviews applications in research and analytical characterization of compounds and materials in the field of X-ray diffraction, emphasizing new developments in applications and instrumentation in both single crystal and powder diffraction. Cites 414 references. (CS)

  8. An in situ sample environment reaction cell for spatially resolved x-ray absorption spectroscopy studies of powders and small structured reactors

    SciTech Connect

    Zhang, Chu; Gustafson, Johan; Merte, Lindsay R.; Evertsson, Jonas; Norén, Katarina; Carlson, Stefan; Svensson, Håkan; Carlsson, Per-Anders

    2015-03-15

    An easy-to-use sample environment reaction cell for X-ray based in situ studies of powders and small structured samples, e.g., powder, pellet, and monolith catalysts, is described. The design of the cell allows for flexible use of appropriate X-ray transparent windows, shielding the sample from ambient conditions, such that incident X-ray energies as low as 3 keV can be used. Thus, in situ X-ray absorption spectroscopy (XAS) measurements in either transmission or fluorescence mode are facilitated. Total gas flows up to about 500 ml{sub n}/min can be fed while the sample temperature is accurately controlled (at least) in the range of 25–500 °C. The gas feed is composed by a versatile gas-mixing system and the effluent gas flow composition is monitored with mass spectrometry (MS). These systems are described briefly. Results from simultaneous XAS/MS measurements during oxidation of carbon monoxide over a 4% Pt/Al{sub 2}O{sub 3} powder catalyst are used to illustrate the system performance in terms of transmission XAS. Also, 2.2% Pd/Al{sub 2}O{sub 3} and 2% Ag − Al{sub 2}O{sub 3} powder catalysts have been used to demonstrate X-ray absorption near-edge structure (XANES) spectroscopy in fluorescence mode. Further, a 2% Pt/Al{sub 2}O{sub 3} monolith catalyst was used ex situ for transmission XANES. The reaction cell opens for facile studies of structure-function relationships for model as well as realistic catalysts both in the form of powders, small pellets, and coated or extruded monoliths at near realistic conditions. The applicability of the cell for X-ray diffraction measurements is discussed.

  9. An in situ sample environment reaction cell for spatially resolved x-ray absorption spectroscopy studies of powders and small structured reactors

    NASA Astrophysics Data System (ADS)

    Zhang, Chu; Gustafson, Johan; Merte, Lindsay R.; Evertsson, Jonas; Norén, Katarina; Carlson, Stefan; Svensson, Hâkan; Carlsson, Per-Anders

    2015-03-01

    An easy-to-use sample environment reaction cell for X-ray based in situ studies of powders and small structured samples, e.g., powder, pellet, and monolith catalysts, is described. The design of the cell allows for flexible use of appropriate X-ray transparent windows, shielding the sample from ambient conditions, such that incident X-ray energies as low as 3 keV can be used. Thus, in situ X-ray absorption spectroscopy (XAS) measurements in either transmission or fluorescence mode are facilitated. Total gas flows up to about 500 mln/min can be fed while the sample temperature is accurately controlled (at least) in the range of 25-500 °C. The gas feed is composed by a versatile gas-mixing system and the effluent gas flow composition is monitored with mass spectrometry (MS). These systems are described briefly. Results from simultaneous XAS/MS measurements during oxidation of carbon monoxide over a 4% Pt/Al2O3 powder catalyst are used to illustrate the system performance in terms of transmission XAS. Also, 2.2% Pd/Al2O3 and 2% Ag - Al2O3 powder catalysts have been used to demonstrate X-ray absorption near-edge structure (XANES) spectroscopy in fluorescence mode. Further, a 2% Pt/Al2O3 monolith catalyst was used ex situ for transmission XANES. The reaction cell opens for facile studies of structure-function relationships for model as well as realistic catalysts both in the form of powders, small pellets, and coated or extruded monoliths at near realistic conditions. The applicability of the cell for X-ray diffraction measurements is discussed.

  10. The MYTHEN detector for X-ray powder diffraction experiments at the Swiss Light Source

    PubMed Central

    Bergamaschi, Anna; Cervellino, Antonio; Dinapoli, Roberto; Gozzo, Fabia; Henrich, Beat; Johnson, Ian; Kraft, Philipp; Mozzanica, Aldo; Schmitt, Bernd; Shi, Xintian

    2010-01-01

    The MYTHEN single-photon-counting silicon microstrip detector has been developed at the Swiss Light Source for time-resolved powder diffraction experiments. An upgraded version of the detector has been installed at the SLS powder diffraction station allowing the acquisition of diffraction patterns over 120° in 2θ in fractions of seconds. Thanks to the outstanding performance of the detector and to the calibration procedures developed, the quality of the data obtained is now comparable with that of traditional high-resolution point detectors in terms of FWHM resolution and peak profile shape, with the additional advantage of fast and simultaneous acquisition of the full diffraction pattern. MYTHEN is therefore optimal for time-resolved or dose-critical measurements. The characteristics of the MYTHEN detector together with the calibration procedures implemented for the optimization of the data are described in detail. The refinements of two known standard powders are discussed together with a remarkable application of MYTHEN to organic compounds in relation to the problem of radiation damage. PMID:20724787

  11. Assessment of the Stoichiometry of Multicomponent Crystals Using Only X-ray Powder Diffraction Data.

    PubMed

    Maguire, Courtney K; Brunskill, Andrew P J

    2015-06-01

    Knowledge of the unit cell volume of a crystalline form and the expected space filling requirements of an API molecule can be used to determine if a crystalline material is likely to be multicomponent, such as a solvate, hydrate, salt, or a co-crystal. The unit cell information can be readily accessed from powder diffraction data alone utilizing powder indexing methodology. If the unit cell has additional space not likely attributable to the API entity, then there is either a void or another component within the crystal lattice. This "leftover" space can be used to determine the likely stoichiometry of the additional component. A simple approach for calculating the expected required volume for a given molecule within a crystal using an atom based additive approach will be discussed. Coupling this estimation with the actual unit cell volumes and space group information obtained from powder indexing allows for the rapid evaluation of the likely stoichiometry of multicomponent crystals using diffraction data alone. This approach is particularly useful for the early assessment of new phases during salt, co-crystal, and polymorph screening, and also for the characterization of stable and unstable solvates. PMID:25872584

  12. Polyaniline fibers, films, and powders: X-ray studies of crystallinity and stress-induced preferred orientation

    SciTech Connect

    Fischer, J.E.; Zhu, Q.; Tang, X.; Scherr, E.M.; MacDiarmid, A.G. . Lab. for Research on the Structure of Matter); Cajipe, V.B. . Inst. des Materiaux des Nantes)

    1994-08-29

    Powder (hk0) and four-circle X-ray diffractometry are used to study the effects of hot-stretching on films and fibers of the emeralidine base form of polyaniline (EB-II). It is shown definitively that hot-stretching induces nucleation of new crystalline material rather than growth and/or orientation of pre-existing crystallites. The diffuse scattering from amorphous EB-II is dominated by short-range interchain correlations and develops preferred orientation in response to stretching but with a broader mosaic than the crystalline phase. For the maximally-stretched samples, the crystal fractions was determined by accounting for the different mosaic distributions of crystalline and amorphous phases, correcting for the mass of N-methylphenazolinium plasticizer and ruling out any significant contribution from NMP diffuse scattering to the amorphous EB-II profiles. Films stretched to L/L[sub 0] = 4.25 contain no more than 4% crystalline material while fibers with L/L[sub 0] = 4.5 are 24--30% crystalline. These fractional crystallinity values are significantly small than found for EB-II powder (60%). More importantly, these results have implications for models of electric properties which invoke interchain interactions.

  13. Electronic structure of cesium butyratouranylate(VI) as derived from DFT-assisted powder X-ray diffraction data.

    PubMed

    Vologzhanina, Anna V; Savchenkov, Anton V; Dmitrienko, Artem O; Korlyukov, Alexander A; Bushmarinov, Ivan S; Pushkin, Denis V; Serezhkina, Larisa B

    2014-10-16

    Investigation of chemical bonding and electronic structure of coordination polymers that do not form high-quality single crystals requires special techniques. Here, we report the molecular and electronic structure of the first cesium butyratouranylate, Cs[UO(2)(n-C(3)H(7)COO)(3)][UO(2)(n-C(3)H(7)COO)(OH)(H2O)], as obtained from DFT-assisted powder X-ray diffraction data because of the low quality of crystalline sample. The topological analysis of the charge distribution within the quantum theory of atoms-in-molecules (QTAIM) space partitioning and the distribution of electron localization function (ELF) is reported. The constancy of atomic domain of the uranium(VI) atom at different coordination numbers (7 and 8) and the presence of three ELF maxima in equatorial plane of an uranyl cation attributed to the 6s and 6p electrons were demonstrated for the first time. Details of methodologies applied for additional verification of the correctness of powder XRD refinement (Voronoi atomic descriptors and the Morse restraints) are discussed. PMID:25289686

  14. Catalyst Chemical State during CO Oxidation Reaction on Cu(111) Studied with Ambient-Pressure X-ray Photoelectron Spectroscopy and Near Edge X-ray Adsorption Fine Structure Spectroscopy.

    PubMed

    Eren, Baran; Heine, Christian; Bluhm, Hendrik; Somorjai, Gabor A; Salmeron, Miquel

    2015-09-01

    The chemical structure of a Cu(111) model catalyst during the CO oxidation reaction in the CO+O2 pressure range of 10-300 mTorr at 298-413 K was studied in situ using surface sensitive X-ray photoelectron and adsorption spectroscopy techniques [X-ray photoelectron spectroscopy (XPS) and near edge X-ray adsorption fine structure spectroscopy (NEXAFS)]. For O2:CO partial pressure ratios below 1:3, the surface is covered by chemisorbed O and by a thin (∼1 nm) Cu2O layer, which covers completely the surface for ratios above 1:3 between 333 and 413 K. The Cu2O film increases in thickness and exceeds the escape depth (∼3-4 nm) of the XPS and NEXAFS photoelectrons used for analysis at 413 K. No CuO formation was detected under the reaction conditions used in this work. The main reaction intermediate was found to be CO2(δ-), with a coverage that correlates with the amount of Cu2O, suggesting that this phase is the most active for CO oxidation. PMID:26275662

  15. Water adsorption on TiO2 surfaces probed by soft X-ray spectroscopies: bulk materials vs. isolated nanoparticles

    NASA Astrophysics Data System (ADS)

    Benkoula, Safia; Sublemontier, Olivier; Patanen, Minna; Nicolas, Christophe; Sirotti, Fausto; Naitabdi, Ahmed; Gaie-Levrel, François; Antonsson, Egill; Aureau, Damien; Ouf, François-Xavier; Wada, Shin-Ichi; Etcheberry, Arnaud; Ueda, Kiyoshi; Miron, Catalin

    2015-10-01

    We describe an experimental method to probe the adsorption of water at the surface of isolated, substrate-free TiO2 nanoparticles (NPs) based on soft X-ray spectroscopy in the gas phase using synchrotron radiation. To understand the interfacial properties between water and TiO2 surface, a water shell was adsorbed at the surface of TiO2 NPs. We used two different ways to control the hydration level of the NPs: in the first scheme, initially solvated NPs were dried and in the second one, dry NPs generated thanks to a commercial aerosol generator were exposed to water vapor. XPS was used to identify the signature of the water layer shell on the surface of the free TiO2 NPs and made it possible to follow the evolution of their hydration state. The results obtained allow the establishment of a qualitative determination of isolated NPs’ surface states, as well as to unravel water adsorption mechanisms. This method appears to be a unique approach to investigate the interface between an isolated nano-object and a solvent over-layer, paving the way towards new investigation methods in heterogeneous catalysis on nanomaterials.

  16. Water adsorption on TiO2 surfaces probed by soft X-ray spectroscopies: bulk materials vs. isolated nanoparticles

    PubMed Central

    Benkoula, Safia; Sublemontier, Olivier; Patanen, Minna; Nicolas, Christophe; Sirotti, Fausto; Naitabdi, Ahmed; Gaie-Levrel, François; Antonsson, Egill; Aureau, Damien; Ouf, François-Xavier; Wada, Shin-Ichi; Etcheberry, Arnaud; Ueda, Kiyoshi; Miron, Catalin

    2015-01-01

    We describe an experimental method to probe the adsorption of water at the surface of isolated, substrate-free TiO2 nanoparticles (NPs) based on soft X-ray spectroscopy in the gas phase using synchrotron radiation. To understand the interfacial properties between water and TiO2 surface, a water shell was adsorbed at the surface of TiO2 NPs. We used two different ways to control the hydration level of the NPs: in the first scheme, initially solvated NPs were dried and in the second one, dry NPs generated thanks to a commercial aerosol generator were exposed to water vapor. XPS was used to identify the signature of the water layer shell on the surface of the free TiO2 NPs and made it possible to follow the evolution of their hydration state. The results obtained allow the establishment of a qualitative determination of isolated NPs’ surface states, as well as to unravel water adsorption mechanisms. This method appears to be a unique approach to investigate the interface between an isolated nano-object and a solvent over-layer, paving the way towards new investigation methods in heterogeneous catalysis on nanomaterials. PMID:26462615

  17. An Investigation of X-ray Luminosity versus Crystalline Powder Granularity

    SciTech Connect

    Borade, Ramesh; Bourret-Courchesne, Edith; ,

    2012-03-07

    At the High-throughput Discovery of Scintillator Materials Facility at Lawrence Berkeley National Laboratory, scintillators are synthesized by solid-state reaction or melt mixing, forming crystalline powders. These powders are formed in various granularity and the crystal grain size affects the apparent luminosity of the scintillator. To accurately predict a "full-size" scintillator's crystal luminosity, the crystal luminosity as a function of crystal granularity size has to be known. In this study, we examine Bi{sub 4}Ge{sub 3}O{sub 12} (BGO), Lu{sub 2}SiO{sub 5}:Ce (LSO), YAlO{sub 3}:Ce (YAP:Ce), and CsBa{sub 2}I{sub 5}:Eu{sup 2+} (CBI) luminosities as a function of crystalline grain size. The highest luminosities were measured for 600- to 1000-{micro}m crystal grain sizes for BGO and LSO, for 310- to 600-{micro}m crystal grain sizes for CBI, and for crystal grains larger than 165{micro}m for YAP:Ce. Crystal grains that were larger than 1 mm had a lower packing fraction, and smaller grains were affected by internal scattering. We measured a 34% decrease in luminosity for BGO when decreasing from the 600- to 1000- {micro}m crystal grain size range down to the 20- to 36-{micro}m range. The corresponding luminosity decrease for LSO was 44% for the same grain size decrease. YAP:Ce exhibited a luminosity decrease of 47% when the grain size decreased from the 165- to 310-{micro}m crystal grains to the 20- to 36-{micro}m range, and CBI exhibited a luminosity decrease of 98% when the grain size decreased from the 310- to 600-{micro}m crystal grain range to the 36- to 50-{micro}m range. We were able to very accurately estimate full-size crystal luminosities from crystalline grains that are larger than 90 {micro}m.

  18. Multivariate calibration of the degree of crystallinity in intact pellets by X-ray powder diffraction.

    PubMed

    Nikowitz, Krisztina; Domján, Attila; Pintye-Hódi, Klára; Regdon, Géza

    2016-04-11

    XRPD is the method of choice to determine crystalline content in an amorphous environment. While several studies describe its use on powders, little information is available on its performance on finished products. The method's use may be limited not only by the need of sample pretreatment and its validation but also by the propensity of some materials to recrystallize when exposed to heat or mechanical stress. In this work the authors describe an attempt at constructing a model based on the XRPD measurement of intact layered pellets using univariate methods based on peak heights and PLS regression. Results indicate that neither the goodness-of-fit (below 0.9 for all tested variables), nor the RMSEC values (above 5 for all tested variables) of any model based on peak height were good enough to consider them for everyday use. PLS regression however provided a model with improved characteristics (R(2)=0.9581, RMSEC=3.04) despite the low API content and individual loading characteristics also reflected the validity of the model. PLS analysis also indicated that a specific sample may be different in some formulation characteristic that did not register on other examinations. This further indicates the method's usefulness in the analysis of intact dosage forms. PMID:26899205

  19. Possibilities and limitations of synchrotron X-ray powder diffraction with double crystal and double multilayer monochromators for microscopic speciation studies

    NASA Astrophysics Data System (ADS)

    De Nolf, Wout; Jaroszewicz, Jakub; Terzano, Roberto; Lind, Ole Christian; Salbu, Brit; Vekemans, Bart; Janssens, Koen; Falkenberg, Gerald

    2009-08-01

    The performance of a combined microbeam X-ray fluorescence/X-ray powder diffraction (XRF/XRPD) measurement station at Hamburger Synchrotronstrahlungslabor (HASYLAB) Beamline L is discussed in comparison to that at European Synchrotron Radiation Facility (ESRF) ID18F/ID22. The angular resolution in the X-ray diffractograms is documented when different combinations of X-ray source, optics and X-ray diffraction detectors are employed. Typical angular resolution values in the range 0.3-0.5° are obtained at the bending magnet source when a 'pink' beam form of excitation is employed. A similar setup at European Synchrotron Radiation Facility beamlines ID18F and ID22 allows to reach angular resolution values of 0.1-0.15°. In order to document the possibilities and limitations for speciation of metals in environmental materials by means of Hamburger Synchrotronstrahlungslabor Beamline L X-ray fluorescence/X-ray powder diffraction setup, two case studies are discussed, one involved in the identification of the crystal phases in which heavy metals such as chromium, iron, barium and lead are present in polluted soils of an industrial site (Val Basento, Italy) and another involved in the speciation of uranium in depleted uranium particles (Ceja Mountains, Kosovo). In the former case, the angular resolution is sufficient to allow identification of most crystalline phases present while in the latter case, it is necessary to dispose of an angular resolution of ca. 0.2° to distinguish between different forms of oxidized uranium.

  20. On the response of Y 3Al 5O 12: Ce (YAG: Ce) powder scintillating screens to medical imaging X-rays

    NASA Astrophysics Data System (ADS)

    Kandarakis, I.; Cavouras, D.; Sianoudis, I.; Nikolopoulos, D.; Episkopakis, A.; Linardatos, D.; Margetis, D.; Nirgianaki, E.; Roussou, M.; Melissaropoulos, P.; Kalivas, N.; Kalatzis, I.; Kourkoutas, K.; Dimitropoulos, N.; Louizi, A.; Nomicos, C.; Panayiotakis, G.

    2005-02-01

    The aim of this study was to examine Y 3Al 5O 12:Ce (also known as YAG:Ce) powder scintillator under X-ray imaging conditions. This material shows a very fast scintillation decay time and it has never been used in X-ray medical imaging. In the present study various scintillator layers (screens) with coating thickness ranging from 13 to 166 mg/cm 2 were prepared in our laboratory by sedimentation of Y 3Al 5O 12: Ce powder. Optical emission spectra and light emission efficiency (spectrum area over X-ray exposure) of the layers were measured under X-ray excitation using X-ray tube voltages (80-120 kVp) often employed in general medical radiography and fluoroscopy. Spectral compatibility with various optical photon detectors (photodiodes, photocathodes, charge coupled devices, films) and intrinsic conversion efficiency values were determined using emission spectrum data. In addition, parameters related to X-ray detection, energy absorption efficiency and K-fluorescence characteristic emission were calculated. A theoretical model describing radiation and light transfer through scattering media was used to fit experimental data. Intrinsic conversion efficiency (η≈0.03-0.05) and light attenuation coefficients (σ≈26.5 cm/g) were derived through this fitting. Y 3Al 5O 12:Ce showed peak emission in the wavelength range 530-550 nm. The light emission efficiency was found to be maximum for the 107 mg/cm 2 layer. Due to its "green" emission spectrum, Y 3Al 5O 12:Ce showed excellent compatibility (of the order of 0.9) with the sensitivity of many currently used photodetectors. Taking into account its very fast response Y 3Al 5O 12:Ce could be considered for application in X-ray imaging especially in various digital detectors.

  1. Locating Organic Guests in Inorganic Host Materials from X-ray Powder Diffraction Data.

    PubMed

    Smeets, Stef; McCusker, Lynne B; Baerlocher, Christian; Elomari, Saleh; Xie, Dan; Zones, Stacey I

    2016-06-01

    Can the location of the organic structure-directing agent (SDA) inside the channel system of a zeolite be determined experimentally in a systematic manner? In an attempt to answer this question, we investigated six borosilicate zeolites of known framework structure (SSZ-53, SSZ-55, SSZ-56, SSZ-58, SSZ-59, and SSZ-60), where the location of the SDA had only been simulated using molecular modeling techniques in previous studies. From synchrotron powder diffraction data, we were able to retrieve reliable experimental positions for the SDA by using a combination of simulated annealing (global optimization) and Rietveld refinement. In this way, problems arising from data quality and only partially compatible framework and SDA symmetries, which can lead to indecipherable electron density maps, can be overcome. Rietveld refinement using geometric restraints were then performed to optimize the positions and conformations of the SDAs. With these improved models, it was possible to go on to determine the location of the B atoms in the framework structure. That is, two pieces of information that are key to the understanding of zeolite synthesis-the location of the organic SDA in the channel system and of the positions adopted by heteroatoms in the silicate framework-can be extracted from experimental data using a systematic strategy. In most cases, the locations of the SDAs determined experimentally compare well with those simulated with molecular modeling, but there are also some clear differences, and the reason for these differences can be understood. The approach is generally applicable, and has also been used to locate organic guests, linkers, and ligands in metal-organic compounds. PMID:27181421

  2. X-ray Powder Diffraction in Conservation Science: Towards Routine Crystal Structure Determination of Corrosion Products on Heritage Art Objects.

    PubMed

    Dinnebier, Robert E; Fischer, Andrea; Eggert, Gerhard; Runčevski, Tomče; Wahlberg, Nanna

    2016-01-01

    The crystal structure determination and refinement process of corrosion products on historic art objects using laboratory high-resolution X-ray powder diffraction (XRPD) is presented in detail via two case studies. The first material under investigation was sodium copper formate hydroxide oxide hydrate, Cu4Na4O(HCOO)8(OH)2∙4H2O (sample 1) which forms on soda glass/copper alloy composite historic objects (e.g., enamels) in museum collections, exposed to formaldehyde and formic acid emitted from wooden storage cabinets, adhesives, etc. This degradation phenomenon has recently been characterized as "glass induced metal corrosion". For the second case study, thecotrichite, Ca3(CH3COO)3Cl(NO3)2∙6H2O (sample 2), was chosen, which is an efflorescent salt forming needlelike crystallites on tiles and limestone objects which are stored in wooden cabinets and display cases. In this case, the wood acts as source for acetic acid which reacts with soluble chloride and nitrate salts from the artifact or its environment. The knowledge of the geometrical structure helps conservation science to better understand production and decay reactions and to allow for full quantitative analysis in the frequent case of mixtures. PMID:27341300

  3. Crystal structure of barium perchlorate anhydrate, Ba(ClO4)2, from laboratory X-ray powder data

    PubMed Central

    Lee, Jeonghoo H.; Kang, Ji Hoon; Lim, Sung-Chul; Hong, Seung-Tae

    2015-01-01

    The previously unknown crystal structure of barium perchlorate anhydrate, determined and refined from laboratory X-ray powder diffraction data, represents a new structure type. The title compound was obtained by heating hydrated barium perchlorate [Ba(ClO4)2·xH2O] at 423 K in vacuo for 6 h. It crystallizes in the ortho­rhom­bic space group Fddd. The asymmetric unit contains one Ba (site symmetry 222 on special position 8a), one Cl (site symmetry 2 on special position 16f) and two O sites (on general positions 32h). The structure can be described as a three-dimensional polyhedral network resulting from the corner- and edge-sharing of BaO12 polyhedra and ClO4 tetra­hedra. Each BaO12 polyhedron shares corners with eight ClO4 tetra­hedra, and edges with two ClO4 tetra­hedra. Each ClO4 tetra­hedron shares corners with four BaO12 polyhedra, and an edge with the other BaO12 polyhedron. PMID:26090128

  4. [X-ray powder diffraction of clay minerals of SZK01 core of Zabuye Lake, Tibetan Plateau].

    PubMed

    Zhang, Xue-Fei; Zheng, Mian-Ping

    2014-11-01

    The present article chooses the core from the borehole SZK01 in Zabuye Lake as the main research object. According to the results of X-ray powder diffraction of clay minerals, the major components are illite, illite and smectite mixed layer mineral (I/S), kaolinite and chlorite. According to the different species and contents of clay, integration of the characteristics of mineral and the results of Δ18O, we reestablished the evolution process of paleoclimate in Zabuye Lake. In compaison with SZK02 core in Zabuye, Greenland GISP2 and GRIP and Guliya ice core, it contains 5 stages since 115 ka in Zabuye: the last interglacial (15-75.5 ka), the earlier last glacial (75.5-60 ka), the interstage of the last glacial (60-30.1 ka), the last glacial maximum (30.1-16.7 ka) and deglacial-holocene (since 16.7 ka). We also recognized 6 Heinrich events (H1-H6) and warm event in 71 ka. In particular, the content of kaolinite is low, with the negative-skewed value of Δ18O in 52-53 ka, while the value of Δ18O in SZK02 and Guliya ice core is negative-skewed too, indicating the cold event in Tibet plateau, named H5-1. All the above demonstrated that the climate in Tibet plateau is global since the earlier last glacial, and it also has regional characteristics. PMID:25752070

  5. Powder X-ray studies of meso-hexamethyl propylene amine oxime (meso-HMPAO) in two different phases.

    PubMed

    Al-Ktaifani, Mahmoud; Rukiah, Mwaffak

    2010-09-01

    Two different forms of meso-3,3'-[2,2-dimethylpropane-1,3-diylbis(azanediyl)]dibutan-2-one dioxime, commonly called meso-hexamethyl propylene amine oxime (HMPAO), C(13)H(28)N(4)O(2), designated alpha and beta, were isolated by fractional crystallization and their crystal structures were determined by powder X-ray diffraction using the direct-space method with the parallel tempering algorithm. The alpha form was first crystallized from acetonitrile solution, while the beta form was obtained by recrystallization of the alpha phase from diethyl ether. The alpha form crystallizes in the triclinic system (space group P-1), with one molecule in the asymmetric unit, while the crystal of the beta form is monoclinic (space group P2(1)/n), with one molecule in the asymmetric unit. In both phases, the molecules have similar conformations and RS/EE geometric isomerism. The crystal packing of the two phases is dominated by intermolecular hydrogen-bonding interactions between the two O-H oxime groups of an individual molecule and the amine N atoms of two different adjacent molecules, which lead to segregation of extended poly(meso-HMPAO) one-dimensional chains along the c direction. The structures of the two phases are primarily different due to the different orientations of the molecules in the chains. PMID:20814112

  6. Crystal structure of barium perchlorate anhydrate, Ba(ClO4)2, from laboratory X-ray powder data.

    PubMed

    Lee, Jeonghoo H; Kang, Ji Hoon; Lim, Sung-Chul; Hong, Seung-Tae

    2015-06-01

    The previously unknown crystal structure of barium perchlorate anhydrate, determined and refined from laboratory X-ray powder diffraction data, represents a new structure type. The title compound was obtained by heating hydrated barium perchlorate [Ba(ClO4)2·xH2O] at 423 K in vacuo for 6 h. It crystallizes in the ortho-rhom-bic space group Fddd. The asymmetric unit contains one Ba (site symmetry 222 on special position 8a), one Cl (site symmetry 2 on special position 16f) and two O sites (on general positions 32h). The structure can be described as a three-dimensional polyhedral network resulting from the corner- and edge-sharing of BaO12 polyhedra and ClO4 tetra-hedra. Each BaO12 polyhedron shares corners with eight ClO4 tetra-hedra, and edges with two ClO4 tetra-hedra. Each ClO4 tetra-hedron shares corners with four BaO12 polyhedra, and an edge with the other BaO12 polyhedron. PMID:26090128

  7. X-ray powder diffractometry and liquid chromatography studies of sibutramine and its analogues content in herbal dietary supplements.

    PubMed

    Stypułkowska, K; Błażewicz, A; Maurin, J; Sarna, K; Fijałek, Z

    2011-12-15

    The contemporary societies of the developed countries are prone to use traditional far-east medicines as remedies for all diseases. Some of them, such as obesity, might be classified as civilization diseases. Combating the problem, people try not only several miraculous diets but also herbal infusions (teas) and variety of "herbal" preparations. All these believing that such treatment is healthy and harmless as far as it is "natural". Leaving out of the way the question if herbal medicines can be taken safely without doctors' control the query arises if the common preparations are strictly natural and herbal. Here we report examples of quality studies of such medicines using both X-ray powder diffraction (XRPD) and liquid chromatography (LC) with various types of detection: ultraviolet (UV), coulometric electrode array (CEAD) and time-of-flight mass spectrometry (TOF-MS). Especially the XRPD assisted with an optical microscopy seems to be useful as a fast screening method of general sample composition of such preparations. First of all it can discriminate between capsules containing pure herbal materials and those with some chemical. PMID:21899974

  8. Hydrostatic Compression Curve for Triamino-Trinitrobenzene Determined to 13.0 GPa with Powder X-Ray Diffraction

    SciTech Connect

    Stevens, Lewis L.; Velisavljevic, Nenad; Hooks, Daniel E.; Dattelbaum, Dana M.

    2008-08-22

    Using powder X-ray diffraction in conjunction with a diamond anvil cell (DAC), the unit cell volume of triamino-trinitrobenzene (TATB) has been measured from ambient pressure to 13 GPa. The resultant isotherm is compared with previous theoretical (Byrd and Rice and Pastine and Bernecker) and experimental (Olinger and Cady) works. While all reports are consistent to approximately 2 GPa, our measurements reveal a slightly stiffer TATB material than reported by Olinger and Cady and an intermediate compressibility compared with the isotherms predicted by the two theoretical works. Analysis of the room temperature isotherm using the semi-empirical, Murnaghan, Birch-Murnaghan, and Vinet equations of state (EOS) provided a determination of the isothermal bulk modulus (K{sub 0}) and its pressure-derivative (K{sub 0}') for TATB. From these fits to our P-V isotherm, from ambient pressure to 8 GPa, the average results for the zero-pressure bulk modulus and its pressure derivative were found to be 14.7 GPa and 10.1, respectively. For comparison to shock experiments on pressed TATB powder and its plastic-bonded formulation PBX 9502 (95% TATB, 5% Kel-F 800), the isotherm was transformed to the pseudo-velocity U{sub s}-u{sub p} plane using the Rankine-Hugoniot jump conditions. This analysis provides an extrapolated bulk sound speed, c{sub 0}=1.70 km s{sup -1}, for TATB and its agreement with a previous determination (c{sub 0}=1.43 km s{sup -1}) is discussed. Furthermore, our P-V and corresponding U{sub s}-u{sub p} curves reveal a subtle cusp at approximately 8 GPa. This cusp is discussed in relation to similar observations made for the aromatic hydrocarbons anthracene, benzene and toluene, graphite, and trinitrotoluene (TNT).

  9. Mass fractal characteristics of silica sonogels as determined by small-angle x-ray scattering and nitrogen adsorption

    SciTech Connect

    Donatti, D.A.; Vollet, D.R.; Ibanez Ruiz, A.; Mesquita, A.; Silva, T.F.P.

    2005-01-01

    A sample series of silica sonogels was prepared using different water-tetraethoxysilane molar ratio (r{sub w}) in the gelation step of the process in order to obtain aerogels with different bulk densities after the supercritical drying. The samples were analyzed by means of small-angle x-ray-scattering (SAXS) and nitrogen-adsorption techniques. Wet sonogels exhibit mass fractal structure with fractal dimension D increasing from {approx}2.1 to {approx}2.4 and mass-fractal correlation length {xi} diminishing from {approx}13 nm to {approx}2 nm, as r{sub w} is changed in the nominal range from 66 to 6. The process of obtaining aerogels from sonogels and heat treatment at 500 deg. C, in general, increases the mass-fractal dimension D, diminishes the characteristic length {xi} of the fractal structure, and shortens the fractal range at the micropore side for the formation of a secondary structured particle, apparently evolved from the original wet structure at a high resolution level. The overall mass-fractal dimension D of aerogels was evaluated as {approx}2.4 and {approx}2.5, as determined from SAXS and from pore-size distribution by nitrogen adsorption, respectively. The fine structure of the 'secondary particle' developed in the obtaining of aerogels could be described as a surface-mass fractal, with the correlated surface and mass-fractal dimensions decreasing from {approx}2.4 to {approx}2.0 and from {approx}2.7 to {approx}2.5, respectively, as the aerogel bulk density increases from 0.25 (r{sub w}=66) up to 0.91 g/cm{sup 3} (r{sub w}=6)

  10. Mechanism of Pb Adsorption to Fatty Acid Langmuir Monolayers Studied by X-ray Absorption Fine Structure Spectroscopy

    SciTech Connect

    Boyanov, M.I.; Kmetko, J.; Shibata, T.; Datta, A.; Dutta, P.; Bunker, B.A.

    2010-09-30

    The local atomic environment of lead (Pb) adsorbed to a CH{sub 3}(CH{sub 2}){sub 19}COOH Langmuir monolayer was investigated in situ using grazing-incidence X-ray absorption fine structure (GI-XAFS) spectroscopy at the Pb L{sub III} edge. Measurements were performed at pH 6.5 of the 10{sup -5} M PbCl{sub 2} solution subphase, a condition under which grazing incidence diffraction (GID) revealed a large-area commensurate superstructure underneath the close-packed organic monolayer. The XAFS results indicate covalent binding of the Pb cations to the carboxyl headgroups, and the observed Pb-Pb coordination suggests that the metal is adsorbed as a hydrolysis polymer, rather than as individual Pb{sup 2+} ions. The data are consistent with a bidentate chelating mechanism and a one Pb atom to one carboxyl headgroup binding stoichiometry. We discuss how this adsorption model can explain the peculiarities observed with Pb in previous metal-Langmuir monolayer studies. A systematic study of lead perchlorate and lead acetate aqueous solutions is presented and used in the analysis. XAFS multiple scattering effects from alignment of the Pb-C-C atoms in the lead acetate solutions are reported.

  11. Acemetacin cocrystals and salts: structure solution from powder X-ray data and form selection of the piperazine salt

    PubMed Central

    Sanphui, Palash; Bolla, Geetha; Nangia, Ashwini; Chernyshev, Vladimir

    2014-01-01

    Acemetacin (ACM) is a non-steroidal anti-inflammatory drug (NSAID), which causes reduced gastric damage compared with indomethacin. However, acemetacin has a tendency to form a less soluble hydrate in the aqueous medium. We noted difficulties in the preparation of cocrystals and salts of acemetacin by mechanochemical methods, because this drug tends to form a hydrate during any kind of solution-based processing. With the objective to discover a solid form of acemetacin that is stable in the aqueous medium, binary adducts were prepared by the melt method to avoid hydration. The coformers/salt formers reported are pyridine carboxamides [nicotinamide (NAM), isonicotinamide (INA), and picolinamide (PAM)], caprolactam (CPR), p-aminobenzoic acid (PABA), and piperazine (PPZ). The structures of an ACM–INA cocrystal and a binary adduct ACM–PABA were solved using single-crystal X-ray diffraction. Other ACM cocrystals, ACM–PAM and ACM–CPR, and the piperazine salt ACM–PPZ were solved from high-resolution powder X-ray diffraction data. The ACM–INA cocrystal is sustained by the acid⋯pyridine heterosynthon and N—H⋯O catemer hydrogen bonds involving the amide group. The acid⋯amide heterosynthon is present in the ACM–PAM cocrystal, while ACM–CPR contains carboxamide dimers of caprolactam along with acid–carbonyl (ACM) hydrogen bonds. The cocrystals ACM–INA, ACM–PAM and ACM–CPR are three-dimensional isostructural. The carboxyl⋯carboxyl synthon in ACM–PABA posed difficulty in assigning the position of the H atom, which may indicate proton disorder. In terms of stability, the salts were found to be relatively stable in pH 7 buffer medium over 24 h, but the cocrystals dissociated to give ACM hydrate during the same time period. The ACM–PPZ salt and ACM–nicotinamide cocrystal dissolve five times faster than the stable hydrate form, whereas the ACM–PABA adduct has 2.5 times faster dissolution rate. The pharmaceutically acceptable piperazine

  12. Neutron and X-Ray Powder Diffraction Study of RBa 2Fe 3O 8+ wPhases

    NASA Astrophysics Data System (ADS)

    Karen, P.; Kjekshus, A.; Huang, Q.; Lynn, J. W.; Rosov, N.; Natali Sora, I.; Karen, V. L.; Mighell, A. D.; Santoro, A.

    1998-02-01

    Compounds of composition RBa 2Fe 3O 8+ w( R=La, Nd, Sm, Gd, Dy, Er, Yb, Lu, and Y) with variable oxygen content have been synthesized using the liquid mixing technique and have been analyzed by powder X-ray and neutron diffraction methods. A triple perovskite-type structure with ordered Ba and Rcations and having the symmetry of space group P4/ mmmwas obtained only for R=Y, Dy, and Er, whereas the larger Ratoms gave the atomic arrangement of disordered, defective perovskites with average symmetry Pmoverline3m. No perovskite-type phases were obtained when Yb and Lu were tried. The oxygen content of the oxygen-saturated phases was found to increase with increasing size of the cation Rfrom w=0.07 for Er to w=0.83 for La. The Néel temperature (˜650 K) and the magnitude of the Fe magnetic moment (˜3.3 μBat room temperature) are highest when trivalent iron is involved ( w=0), but these quantities are rather insensitive to the nature of Rand to slight variations of oxygen content in the triple perovskite-type structure of the Y, Dy, and Er compounds. In the case of the cubic structures, however, both quantities depend strongly on the oxygen stoichiometry. In the magnetically ordered state, nearest-neighbor iron moments are coupled antiferromagnetically along the three crystallographic directions in all samples, resulting in magnetic structures with symmetry Imm' mand magnetic unit cells related to those of the corresponding nuclear structures by the transformation matrix (1 overline10/110/002).

  13. A glass capillary cell for in situ powder X-ray diffraction of condensed volatile compounds. Solid HCFC-123a and HCFC-124.

    PubMed

    Brunelli, Michela; Fitch, Andrew N

    2003-07-01

    A rotating glass capillary cell with a gas handling system has been built to allow in situ studies by powder X-ray diffraction. The cell can be used to condense volatile compounds, or to follow solid-state chemical reactions under vacuum or at gas pressures up to around 7 x 10(5) Pa. Using the cell, cooled by a stream of helium gas, the solid phases of 1,2-dichlorotrifluoroethane (HCFC-123a) and 2-chloro-1,1,1,2-tetrafluoroethane (HCFC-124) have been investigated using powder synchrotron X-ray radiation. These were found to have disordered hexagonal structures, with a = 4.018 (5), c = 6.553 (1) A and a = 4.048 (1), c = 6.625 (1) A, respectively, at 64 K. PMID:12824935

  14. A flow-through reaction cell for in situ X-ray diffraction and absorption studies of heterogeneous powder-liquid reactions and phase transformations.

    PubMed

    Ferrer, Pilar; da Silva, Iván; Rubio-Zuazo, Juan; Alfonso, Belén F; Trobajo, Camino; Khainakov, Sergei; Garcia, Jose R; Garcia-Granda, Santiago; Castro, Germán R

    2012-01-01

    A portable powder-liquid high-corrosion-resistant reaction cell has been designed to follow in situ reactions by X-ray powder diffraction (XRD) and X-ray absorption spectroscopy (XAS) techniques. The cell has been conceived to be mounted on the experimental stations for diffraction and absorption of the Spanish CRG SpLine-BM25 beamline at the European Synchrotron Radiation Facility. Powder reactants and/or products are kept at a fixed position in a vertical geometry in the X-ray pathway by a porous membrane, under forced liquid reflux circulation. Owing to the short pathway of the X-ray beam through the cell, XRD and XAS measurements can be carried out in transmission configuration/mode. In the case of the diffraction technique, data can be collected with either a point detector or a two-dimensional CCD detector, depending on specific experimental requirements in terms of space or time resolution. Crystallization processes, heterogeneous catalytic processes and several varieties of experiments can be followed by these techniques with this cell. Two experiments were carried out to demonstrate the cell feasibility: the phase transformations of layered titanium phosphates in boiling aqueous solutions of phosphoric acid, and the reaction of copper carbonate and L-isoleucine amino acid powders in boiling aqueous solution. In this last case the shrinking of the solid reactants and the formation of Cu(isoleucine)(2) is observed. The crystallization processes and several phase transitions have been observed during the experiments, as well as an unexpected reaction pathway. PMID:22186649

  15. Additional evidence from x-ray powder diffraction patterns that icosahedral quasi-crystals of intermetallic compounds are twinned cubic crystals

    SciTech Connect

    Pauling, L. )

    1988-07-01

    Analysis of the measured values of Q for the weak peaks (small maxima, usually considered to be background fluctuations, noise) on the x-ray powder diffraction curves for 17 rapidly quenched alloys leads directly to the conclusion that they are formed by an 820-atom or 1012-atom primitive cubic structure that by icosahedral twinning produces the so-called icosahedral quasi-crystals.

  16. Comparison of Shock-Deformed Carbonate Samples to Unshocked Carbonate Samples Using X-ray Powder Diffraction

    NASA Astrophysics Data System (ADS)

    Huson, S.; Foit, F.; Pope, M.

    2006-12-01

    Previous studies of carbonate minerals from meteorite impact craters have revealed broader X-ray powder diffraction (XRD) peaks when compared to those of unshocked mineral standards. In this study XRD patterns of shocked minerals from an impact crater are compared to those subjected to terrestrial tectonic processes as well as to undeformed mineral standards from our in-house collection. Shocked dolostone and limestone samples were collected from the central uplift and eroded crater rim of Sierra Madera, a well-exposed, complex impact crater located in west Texas. Unshocked samples of dolostone and limestone were collected from the Mission Canyon Formation of the Madison Limestone Group of southwest Montana and western Wyoming. The Mission Canyon Formation was deposited in a shallow shelf environment during the Mississippian, subsequently buried to varying depths, and deformed during the Laramide and Sevier orogenies in the Cretaceous. These samples are therefore excellent representatives for "normal" terrestrial tectonic processes. Samples were powdered, sieved through a 63 μm mesh sieve to ensure a uniform size, and sifted onto a vaseline coated zero background plate to reduce preferred orientation of grains. Patterns were collected over the range from 15° 120° 2θ with a step width of 0.02° 2θ and count-time of 10s per step. All patterns were analyzed using MDI Jade 7.0 software. Generally, samples collected in the field have XRD patterns that are not as sharp as the mineral standard patterns. With both shocked and unshocked samples, those containing dolomite show more XRD peak broadening than those without dolomite and at least one pattern of an unshocked dolostone sample is indistinguishable from a shocked dolostone pattern. However, dolostone samples in general are problematic. Previous researchers reported that the amount of magnesium in calcite may affect grinding properties and, therefore, influence XRD peak broadening. Currently, it is not always

  17. A portable powder-liquid high corrosion-resistant reaction cell for in situ X-ray diffraction and absorption studies of heterogeneous powder-liquid reactions and phase transformations

    NASA Astrophysics Data System (ADS)

    Ferrer, P.; da Silva, I.; Heyman, C.; Rubio-Zuazo, J.; Castro, G. R.

    2013-03-01

    A portable powder-liquid high corrosion-resistant reaction cell has been designed to follow in situ reactions by X-ray powder diffraction and X-ray absorption spectroscopy techniques in transmission mode. The cell has been conceived to be mounted on the experimental stations for diffraction and absorption of the Spanish CRG SpLine-BM25 beamline at the ESRF. In the case of the diffraction technique, data can be collected with either a point detector or a two-dimensional CCD detector. Using the 2D-CCD camera, the cell can be used for time-resolved in situ studies of phase transitions and reactions. Powder reactants and/or products are kept at a fixed position in a vertical geometry in the X-ray pathway, which is minimized in order to reduce the X-ray absorption by the reaction bath. Sample is fixed by a porous membrane under forced liquid reflux circulation, assuring total powder-liquid contact, with an accurate temperature control in the range from 20 to 220°C.

  18. Precise measurement of the lattice spacing of LaB6 standard powder by the x-ray extended range technique using synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Chantler, C. T.; Tran, C. Q.; Cookson, D. J.

    2004-04-01

    We used the basis of the x-ray extended range technique to measure the lattice spacing of LaB6 standard powder samples relative to silicon 640b standard powder samples with an accuracy of 5× 10-5 Å . Measurements were not constrained to one energy but were carried out over a 5 keV 20 keV energy range. These measurements used powder diffraction to determine the synchrotron beam energy, to diagnose discrepancies in the nominal calibrated beam energies, and to determine beam energy bandwidths as a function of energy. More specifically, this technique is able to yield a result independent of certain energy-dependent systematics and to yield the most accurate determination of the lattice spacing of NIST SRM 660 LaB6 standard powder so far undertaken. This has direct application to beam line energy calibration, structural evaluation, edge energy calibration, and lattice spacing determinations.

  19. Direct observation of solid-phase adsorbate concentration profile in powdered activated carbon particle to elucidate mechanism of high adsorption capacity on super-powdered activated carbon.

    PubMed

    Ando, Naoya; Matsui, Yoshihiko; Matsushita, Taku; Ohno, Koichi

    2011-01-01

    Decreasing the particle size of powdered activated carbon (PAC) by pulverization increases its adsorption capacities for natural organic matter (NOM) and polystyrene sulfonate (PSS, which is used as a model adsorbate). A shell adsorption mechanism in which NOM and PSS molecules do not completely penetrate the adsorbent particle and instead preferentially adsorb near the outer surface of the particle has been proposed as an explanation for this adsorption capacity increase. In this report, we present direct evidence to support the shell adsorption mechanism. PAC particles containing adsorbed PSS were sectioned with a focused ion beam, and the solid-phase PSS concentration profiles of the particle cross-sections were directly observed by means of field emission-scanning electron microscopy/energy-dispersive X-ray spectrometry (FE-SEM/EDXS). X-ray emission from sulfur, an index of PSS concentration, was higher in the shell region than in the inner region of the particles. The X-ray emission profile observed by EDXS did not agree completely with the solid-phase PSS concentration profile predicted by shell adsorption model analysis of the PSS isotherm data, but the observed and predicted profiles were not inconsistent when the analytical errors were considered. These EDXS results provide the first direct evidence that PSS is adsorbed mainly in the vicinity of the external surface of the PAC particles, and thus the results support the proposition that the increase in NOM and PSS adsorption capacity with decreasing particle size is due to the increase in external surface area on which the molecules can be adsorbed. PMID:20851447

  20. Exploring the interfacial structure of protein adsorbates and the kinetics of protein adsorption: an in situ high-energy X-ray reflectivity study.

    PubMed

    Evers, Florian; Shokuie, Kaveh; Paulus, Michael; Sternemann, Christian; Czeslik, Claus; Tolan, Metin

    2008-09-16

    The high energy X-ray reflectivity technique has been applied to study the interfacial structure of protein adsorbates and protein adsorption kinetics in situ. For this purpose, the adsorption of lysozyme at the hydrophilic silica-water interface has been chosen as a model system. The structure of adsorbed lysozyme layers was probed for various aqueous solution conditions. The effect of solution pH and lysozyme concentration on the interfacial structure was measured. Monolayer formation was observed for all cases except for the highest concentration. The adsorbed protein layers consist of adsorbed lysozyme molecules with side-on or end-on orientation. By means of time-dependent X-ray reflectivity scans, the time-evolution of adsorbed proteins was monitored as well. The results of this study demonstrate the capabilities of in situ X-ray reflectivity experiments on protein adsorbates. The great advantages of this method are the broad wave vector range available and the high time resolution. PMID:18715021

  1. Adsorption of dopamine on rutile TiO2 (110): a photoemission and near-edge X-ray absorption fine structure study.

    PubMed

    Jackman, Mark J; Syres, Karen L; Cant, David J H; Hardman, Samantha J O; Thomas, Andrew G

    2014-07-29

    Synchrotron radiation photoelectron spectroscopy and near-edge X-ray absorption fine structure (NEXAFS) techniques have been used to study the adsorption of dopamine on a rutile TiO2 (110) single crystal. Photoemission results suggest that dopamine bonds through the oxygen molecules in a bidentate fashion. From the data, it is ambiguous whether the oxygens bond to the same 5-fold coordinated surface titanium atom or bridges across two, although based on the bonding of pyrocatechol on rutile TiO2 (110), it is likely that the dopamine bridges two titanium atoms. Using the searchlight effect, the carbon K-edge near-edge X-ray absorption fine structure NEXAFS spectra recorded for dopamine on rutile TiO2 (110) show the phenyl ring to be oriented at 78° ± 5° from the surface and twisted 11 ± 10° relative to the (001) direction. PMID:25003716

  2. Evidence from x-ray and neutron powder diffraction patterns that the so-called icosahedral and decagonal quasicrystals of MnAl/sub 6/ and other alloys are twinned cubic crystals

    SciTech Connect

    Pauling, L.

    1987-06-01

    It is shown that the x-ray powder diffraction patterns of rapidly quenched MnAl/sub 6/ and Mg/sub 32/(Al,Zn)/sub 49/ and the neutron powder diffraction pattern of MnAl/sub 5/ are compatible with the proposed 820-atom primitive cubic structure. The values found for the edge of the unit cube are 23.365 A (x-ray) and 23.416 A (neutron) for MnAl/sub 6/ and 24.313 A (x-ray) for Mg/sub 32/(Al,Zn)/sub 49/.

  3. Determination of tungsten in tantalum-tungsten alloy by X-ray fluorescence spectrometry using fusion, thin layer, and pressed powder pellet techniques

    NASA Astrophysics Data System (ADS)

    Tian, Lunfu; Zou, Deshuang; Dai, Yichun; Tang, Guangping

    2015-08-01

    A method is described for the X-ray fluorescence (XRF) determination of tungsten in tantalum-tungsten alloy over the range of 10.5%-13.5%. The sample was prepared by three methods, namely, borate fusion, filter paper disk, and pressed powder pellet, respectively. We compared the feature of the three methods of specimen preparation and found that filter paper disk method was the most suitable technique for specimen preparation. Furthermore, the results were compared with those given by inductively coupled plasma optical emission spectrometry (ICP-OES), and the relative standard deviation was less than 2%, which could meet the requirement of this application.

  4. Effect of chlorine in clay-mineral specimens prepared on silver metal-membrane mounts for X-ray powder diffraction analysis

    USGS Publications Warehouse

    Poppe, L.J.; Commeau, J.A.; Pense, G.M.

    1989-01-01

    Silver metal-membrane filters are commonly used as substrates in the preparation of oriented clay-mineral specimens for X-ray powder diffraction (XRD). The silver metal-membrane filters, however, present some problems after heat treatment if either the filters or the samples contain significant amounts of chlorine. At elevated temperature, the chloride ions react with the silver substrate to form crystalline compounds. These compounds change the mass-absorption coefficient of the sample, reducing peak intensities and areas and, therefore, complicating the semiquantitative estimation of clay minerals. A simple procedure that eliminates most of the chloride from a sample and the silver metal-membrane substrate is presented here.

  5. 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.

  6. Special tablets containing cellulose binder and Sr internal standard for simplifying X-ray fluorescence analysis of powder samples

    NASA Astrophysics Data System (ADS)

    Mzyk, Zofia; Anyszkiewicz, Jacek; Gorewoda, Tadeusz

    2015-12-01

    The addition of a constant amount of SrCO3 was observed to be the proper internal standard for analysis by wavelength-dispersive X-ray fluorescence spectrometry to correct the matrix and grain size effects of many constituents. The weighing of constant amounts of SrCO3, binder and sample allowed for the preparation time for analysis to be extended, and special tablets containing binder and SrCO3 were developed. Several substances were tested as binders, among which microcrystalline cellulose was chosen for further study. The prepared tablets were checked for their weight stability and the repeatability of SrCO3 addition. The tablets were then used to prepare pellets from geological samples for X-ray fluorescence analysis. The exemplary application and calibration curves for several analytes confirmed that the prepared tablets could be useful for the pelletizing of such materials to compensate for matrix effects.

  7. Water adsorption kinetics and contact angles of pharmaceutical powders.

    PubMed

    Muster, Tim H; Prestidge, Clive A

    2005-04-01

    Water sorption kinetics and water contact angles have been characterized for a range of pharmaceutical powders: ambroxol hydrochloride, griseofulvin, N,n-octyl-D-gluconamide, paracetamol, sulfathiazole, and theophylline. The uptake of water by powder samples at saturated vapor pressure was modeled using a pseudo first-order kinetic relationship. Parameters from this model have been correlated with the concentration and reactivity of the active surface sites of the pharmaceutical powders and their contact angles. The study has shown that analysis of water adsorption kinetics can be a powerful technique for characterizing the surface chemistry and wettability of pharmaceutical powders, and is particularly sensitive to their surface modification through excipient adsorption: ethyl(hydroxyethyl)cellulose treatment of griseofulvin and butyryl chloride treatment of sulfathiazole are reported as case studies. PMID:15736196

  8. Chest x-ray

    MedlinePlus

    ... Images Aortic rupture, chest x-ray Lung cancer, frontal chest x-ray Adenocarcinoma - chest x-ray Coal ... cancer - chest x-ray Lung nodule, right middle lobe - chest x-ray Lung mass, right upper lung - ...

  9. Inelastic X-ray scattering studies of the short-time collective vibrational motions in hydrated lysozyme powders and their possible relation to enzymatic function.

    PubMed

    Wang, Zhe; Bertrand, Christopher E; Chiang, Wei-Shan; Fratini, Emiliano; Baglioni, Piero; Alatas, Ahmet; Alp, E Ercan; Chen, Sow-Hsin

    2013-01-31

    High-resolution inelastic X-ray scattering was used to investigate the collective vibrational excitations in hydrated lysozyme powders as a function of hydration level and temperature. It is found that the samples with strong enzymatic function are "soft", in the sense that they exhibit low frequency and large amplitude intraprotein collective vibrational motions on certain length scales. This is not the case for samples with weak or no enzymatic activity. Thus, we identify a possible correlation between the short-time intraprotein collective vibrational motions and the establishment of enzymatic function in hydrated lysozyme powders, and bring new insight to notions of protein "conformational flexibility" and "softness" in terms of these motions. PMID:23301848

  10. Devitrification of Mechanically Alloyed Zr-Ti-Nb-Cu-Ni-Al Glassy Powders Studied by Time-Resolved X-ray Diffraction

    SciTech Connect

    Scudino, S.; Sordelet, D.J.; Eckert, J.

    2009-04-13

    The crystallization of mechanically alloyed Zr{sub 67}Ti{sub 6.14}Nb{sub 1.92}Cu{sub 10.67}Ni{sub 8.52}Al{sub 5.75} glassy powder is investigated by time-resolved X-ray diffraction. The powder displays a multi-step crystallization behavior characterized by the formation of a metastable nanoscale quasicrystalline phase during the first stage of the crystallization process. At higher temperatures, coinciding with the second crystallization event, the amorphous-to-quasicrystalline transformation is followed by the precipitation of the tetragonal Zr{sub 2}Cu phase (space group I4/mmm) and the tetragonal Zr{sub 2}Ni phase (space group I4/mcm). The transformations are gradual and the quasicrystals and the subsequent phases coexist over a temperature interval of about 25K.

  11. Note: An X-ray powder diffractometer with a wide scattering-angle range of 72° using asymmetrically positioned one-dimensional detectors.

    PubMed

    Katsuya, Yoshio; Song, Chulho; Tanaka, Masahiko; Ito, Kimihiko; Kubo, Yoshimi; Sakata, Osami

    2016-01-01

    An X-ray powder diffractometer has been developed for a time-resolved measurement without the requirement of a scattering angle (2θ) scan. Six one-dimensional detector modules are asymmetrically arranged in a vertical line at a designed distance of 286.5 mm. A detector module actually covers a diffraction angle of about 12° with an angular resolution of 0.01°. A diffracted intensity pattern is simultaneously recorded in a 2θ angular range from 1.63° to 74.37° in a "one shot" measurement. We tested the performance of the diffractometer with reference CeO2 powders and demonstrated diffraction measurements from an operating lithium-air battery. PMID:26827367

  12. Note: An X-ray powder diffractometer with a wide scattering-angle range of 72° using asymmetrically positioned one-dimensional detectors

    NASA Astrophysics Data System (ADS)

    Katsuya, Yoshio; Song, Chulho; Tanaka, Masahiko; Ito, Kimihiko; Kubo, Yoshimi; Sakata, Osami

    2016-01-01

    An X-ray powder diffractometer has been developed for a time-resolved measurement without the requirement of a scattering angle (2θ) scan. Six one-dimensional detector modules are asymmetrically arranged in a vertical line at a designed distance of 286.5 mm. A detector module actually covers a diffraction angle of about 12° with an angular resolution of 0.01°. A diffracted intensity pattern is simultaneously recorded in a 2θ angular range from 1.63° to 74.37° in a "one shot" measurement. We tested the performance of the diffractometer with reference CeO2 powders and demonstrated diffraction measurements from an operating lithium-air battery.

  13. Resonant anomalous x-ray reflectivity as a probe of ion adsorption at solid-liquid interfaces.

    SciTech Connect

    Fenter, P.; Park, C.; Nagy, K. L.; Sturchio, N. C.; Chemistry; Univ. of Illinois at Chicago

    2007-05-23

    We discuss new opportunities to understand processes at the solid-liquid interface using resonant anomalous X-ray reflectivity (RAXR). This approach is illustrated by determination of element-specific density profiles at mica surfaces in aqueous electrolyte solutions containing Rb{sup +} and Sr{sup 2+}. The total interfacial electron density profile is determined by specular reflectivity (i.e., reflected intensity vs. momentum transfer, q, at an energy, E, far from any characteristic absorption edge). RAXR spectra (i.e., intensity vs. E at fixed q) reveal element-specific ion distributions. Key differences in the interaction of Rb{sup +} and Sr{sup 2+} with mica are observed using resonant anomalous X-ray reflectivity: Rb{sup +} adsorbs in a partially hydrated state, but Sr{sup 2+} adsorbs in both fully and partially hydrated states.

  14. Kinetics of adsorption with granular, powdered, and fibrous activated carbon

    SciTech Connect

    Shmidt, J.L.; Pimenov, A.V.; Lieberman, A.I.; Cheh, H.Y.

    1997-08-01

    The properties of three different types of activated carbon, fibrous, powdered, and granular, were investigated theoretically and experimentally. The adsorption rate of the activated carbon fiber was found to be two orders of magnitude higher than that of the granular activated carbon, and one order of magnitude higher than that of the powdered activated carbon. Diffusion coefficients of methylene blue in the fibrous, powdered, and granular activated carbons were determined experimentally. A new method for estimating the meso- and macropore surface areas in these carbons was proposed.

  15. Revealing the powdering methods of black makeup in Ancient Egypt by fitting microstructure based Fourier coefficients to the whole x-ray diffraction profiles of galena

    NASA Astrophysics Data System (ADS)

    Ungár, T.; Martinetto, P.; Ribárik, G.; Dooryhée, E.; Walter, Ph.; Anne, M.

    2002-02-01

    Galena (PbS) is a major ingredient in ancient Egyptian eye makeup. The microstructure of PbS in Egyptian cosmetic powders is used as a fingerprint and is matched with the microstructures produced artificially in geological galena minerals. The microstructure of PbS is determined by x-ray diffraction peak profile analysis in terms of dislocation density, crystallite size, and size distribution. High-resolution powder diffractograms were measured at the ESRF Grenoble synchrotron source with high resolution and high peak-to-background ratios. The Fourier coefficients of the first nine measured reflections of galena are fitted using physically based Fourier coefficients of strain and size functions. Strain anisotropy is accounted for by the dislocation model of the mean square strain. The x-ray data are supplemented by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) micrographs, and are compared with archæological documents. It enables us to describe the procedures of eye makeup manufacturing in the Middle and New Kingdoms of Egypt some 2000 years before Christ.

  16. Rietveld analysis of X-ray powder diffraction patterns as a potential tool for the identification of impact-deformed carbonate rocks

    NASA Astrophysics Data System (ADS)

    Huson, S. A.; Foit, F. F.; Watkinson, A. J.; Pope, M. C.

    2009-12-01

    Previous X-ray powder diffraction (XRD) studies revealed that shock deformed carbonates and quartz have broader XRD patterns than those of unshocked samples. Entire XRD patterns, single peak profiles and Rietveld refined parameters of carbonate samples from the Sierra Madera impact crater, west Texas, unshocked equivalent samples from 95 miles north of the crater and the Mission Canyon Formation of southwest Montana and western Wyoming were used to evaluate the use of X-ray powder diffraction as a potential tool for distinguishing impact deformed rocks from unshocked and tectonically deformed rocks. At Sierra Madera dolostone and limestone samples were collected from the crater rim (lower shock intensity) and the central uplift (higher shock intensity). Unshocked equivalent dolostone samples were collected from well cores drilled outside of the impact crater. Carbonate rocks of the Mission Canyon Formation were sampled along a transect across the tectonic front of the Sevier and Laramide orogenic belts. Whereas calcite subjected to significant shock intensities at the Sierra Madera impact crater can be differentiated from tectonically deformed calcite from the Mission Canyon Formation using Rietveld refined peak profiles, weakly shocked calcite from the crater rim appears to be indistinguishable from the tectonically deformed calcite. In contrast, Rietveld analysis readily distinguishes shocked Sierra Madera dolomite from unshocked equivalent dolostone samples from outside the crater and tectonically deformed Mission Canyon Formation dolomite.

  17. Rietveld Analysis of X-ray Powder Diffraction Patterns as a Potential Tool for the Identification of Impact-deformed Carbonate Rocks

    SciTech Connect

    Huson, Sarah A.; Foit, Franklin F.; Watkinson, A. J.; Pope, Michael C.

    2009-11-01

    Previous X-ray powder diffraction (XRD) studies revealed that shock deformed carbonates and quartz have broader XRD patterns than those of unshocked samples. Entire XRD patterns, single peak profiles and Rietveld refined parameters of carbonate samples from the Sierra Madera impact crater, west Texas, unshocked equivalent samples from 95 miles north of the crater and the Mission Canyon Formation of southwest Montana and western Wyoming were used to evaluate the use of X-ray powder diffraction as a potential tool for distinguishing impact deformed rocks from unshocked and tectonically deformed rocks. At Sierra Madera dolostone and limestone samples were collected from the crater rim (lower shock intensity) and the central uplift (higher shock intensity). Unshocked equivalent dolostone samples were collected from well cores drilled outside of the impact crater. Carbonate rocks of the Mission Canyon Formation were sampled along a transect across the tectonic front of the Sevier and Laramide orogenic belts. Whereas calcite subjected to significant shock intensities at the Sierra Madera impact crater can be differentiated from tectonically deformed calcite from the Mission Canyon Formation using Rietveld refined peak profiles, weakly shocked calcite from the crater rim appears to be indistinguishable from the tectonically deformed calcite. In contrast, Rietveld analysis readily distinguishes shocked Sierra Madera dolomite from unshocked equivalent dolostone samples from outside the crater and tectonically deformed Mission Canyon Formation dolomite.

  18. Surface characterization of 7S and 11S globulin powders from soy protein examined by X-ray photoelectron spectroscopy and scanning electron microscopy.

    PubMed

    Zhao, Xiaoyan; Chen, Jun; Zhu, Qingjun; Du, Fangling; Ao, Qiang; Liu, Jie

    2011-09-01

    In this study the surface composition of 7S and 11S globulin powders from soybean proteins by aqueous buffer and reverse micelle extractions had been examined using X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). Analysis by XPS revealed that the O and N atomic percentage of 7S and 11S globulin surfaces from bis(2-ethylhexyl) sodium sulfosuccinate (AOT) reverse micelle was higher than from aqueous buffer, but the C atomic percentage was lower. The O/C ratio of the 7S globulin powder from aqueous buffer and reverse micelle was similar while significant differences were obtained in the O/C ratio of the 11S globulin powder, N/C atom ratios of the 7S and 11S globulin powders and high-resolution XPS C 1s, N 1s, O 1s spectra. Powder microstructure after reverse micelle treatment showed the presence of small pores, indicating the effect of reverse micelle on the 7S and 11S globulin structure. The obtained results indicated that the reverse micelle could affect the C, O and N components on the surface of soybean proteins. PMID:21555209

  19. Integrated X-ray photoelectron spectroscopy and DFT characterization of benzene adsorption on Pt(111), Pt(355) and Pt(322) surfaces.

    PubMed

    Zhang, Renqin; Hensley, Alyssa J; McEwen, Jean-Sabin; Wickert, Sandra; Darlatt, Erik; Fischer, Kristina; Schöppke, Matthias; Denecke, Reinhard; Streber, Regine; Lorenz, Michael; Papp, Christian; Steinrück, Hans-Peter

    2013-12-21

    We systematically investigate the adsorption of benzene on Pt(111), Pt(355) and Pt(322) surfaces by high-resolution X-ray photoelectron spectroscopy (XPS) and first-principle calculations based on density functional theory (DFT), including van der Waals corrections. By comparing the adsorption energies at 1/9, 1/16 and 1/25 ML on Pt(111), we find significant lateral interactions exist between the benzene molecules at 1/9 ML. The adsorption behavior on Pt(355) and Pt(322) is very different. While on Pt(355) a step species is clearly identified in the C 1s spectra at low coverages followed by occupation of a terrace species at high coverages, no evidence for a step species is found on Pt(322). These different adsorption sites are confirmed by extensive DFT calculations, where the most favorable adsorption configurations on Pt(355) and Pt(322) are also found to vary: a highly distorted across the step molecule is found on Pt(355) while a less distorted configuration adjacent to the step molecule is deduced for Pt(322). The theoretically proposed C 1s core level binding energy shifts between these most favorable configurations and the terrace species are found to correlate well with experiment: for Pt(355), two adsorbate states are found, separated by ~0.4 eV in XPS and 0.3 eV in the calculations, in contrast to only one state on Pt(322). PMID:24189500

  20. Microstructure evaluation of nanocrystalline MgO powders using the advanced X-ray line profile analysis

    NASA Astrophysics Data System (ADS)

    Soleimanian, V.; Abedi, M.; Aghdaee, S. R.

    2015-02-01

    In this study the magnesium oxide nanoparticles were synthesized via the sol-gel method and annealed at different temperatures between 400 and 800 °C in air. In order to evaluate the microstructure of samples, the scanning electron microscopy technique as well as the advanced X-ray diffraction analysis (DIFFaX software and eCMWP fitting procedure) was used and the behavior of crystallite size, size distribution function, dislocation density, the fractions of edge/screw dislocation characters and the probability of planar defects were studied as a function of annealing temperature.

  1. Adsorption of adenine, cytosine, thymine, and uracil on sulfide-modified montmorillonite: FT-IR, Mössbauer and EPR spectroscopy and X-ray diffractometry studies.

    PubMed

    Carneiro, Cristine E A; Berndt, Graciele; de Souza Junior, Ivan G; de Souza, Cláudio M D; Paesano, Andrea; da Costa, Antonio C S; di Mauro, Eduardo; de Santana, Henrique; Zaia, Cássia T B V; Zaia, Dimas A M

    2011-10-01

    In the present work the interactions of nucleic acid bases with and adsorption on clays were studied at two pHs (2.00, 7.00) using different techniques. As shown by Mössbauer and EPR spectroscopies and X-ray diffractometry, the most important finding of this work is that nucleic acid bases penetrate into the interlayer of the clays and oxidize Fe(2+) to Fe(3+), thus, this interaction cannot be regarded as a simple physical adsorption. For the two pHs the order of the adsorption of nucleic acid bases on the clays was: adenine ≈ cytosine > thymine > uracil. The adsorption of adenine and cytosine on clays increased with decreasing of the pH. For unaltered montmorillonite this result could be explained by electrostatic forces between adenine/cytosine positively charged and clay negatively charged. However for montmorillonite modified with Na(2)S, probably van der Waals forces also play an important role since both adenine/cytosine and clay were positively charged. FT-IR spectra showed that the interaction between nucleic acid bases and clays was through NH(+) or NH (2) (+) groups. X-ray diffractograms showed that nucleic acid bases adsorbed on clays were distributed into the interlayer surface, edge sites and external surface functional groups (aluminol, silanol) EPR spectra showed that the intensity of the line g ≈ 2 increased probably because the oxidation of Fe(2+) to Fe(3+) by nucleic acid bases and intensity of the line g = 4.1 increased due to the interaction of Fe(3+) with nucleic acid bases. Mössbauer spectra showed a large decreased on the Fe(2+) doublet area of the clays due to the reaction of nucleic acid bases with Fe(2+). PMID:21717172

  2. Low-temperature adsorption of H2S on Ni(001) studied by near-edge- and surface-extended-x-ray-absorption fine structure

    NASA Astrophysics Data System (ADS)

    McGrath, R.; MacDowell, A. A.; Hashizume, T.; Sette, F.; Citrin, P. H.

    1989-11-01

    The adsorption of H2S on Ni(001) has been studied with surface-extended x-ray-absorption fine structure and near-edge x-ray-absorption fine structure (NEXAFS) using the AT&T Bell Laboratories X15B beamline at the National Synchrotron Light Source. At 95 K and full saturation coverage, ~0.45 monolayer (ML) of S atoms in fourfold-hollow sites are produced, characteristic of room-temperature adsorption, accompanied by ~0.05 ML of oriented molecular H2S. Both these atomic and molecular chemisorbed species are buried under ~0.9 ML of disordered physisorbed H2S. No evidence for HS is found. Above 190 K the two molecular H2S phases desorb, leaving only dissociated S. These findings differ from previously reported interpretations of data obtained with high-resolution electron-energy-loss spectroscopy. They also exemplify the utility of NEXAFS for identifying and quantifying atomic and molecular surface species even when their difference involves only H and the two species coexist.

  3. High-pressure powder x-ray diffraction experiments and ab initio calculation of Ti3AlC2

    NASA Astrophysics Data System (ADS)

    Zhang, Haibin; Wu, Xiang; Nickel, Klaus Georg; Chen, Jixin; Presser, Volker

    2009-07-01

    The structural stability of the layered ternary carbide Ti3AlC2 was studied up to 35 GPa using x-ray diffraction with a Merrill-Basset-type diamond anvil cell and ab initio calculations. The structure (P63/mmc) was stable in the present pressure range without any phase transition. The Birch-Murnaghan equation of state was employed to fit the experimental pressure-volume date, from which the isothermal bulk modulus of Ti3AlC2 was determined as 156±5 GPa, which was also supported by theoretical results. In addition, theoretical calculations described anisotropic pressure dependences of the lattice parameters, electronic structure, and bonding properties of Ti3AlC2.

  4. Time-resolved X-ray powder diffraction on a three-way catalyst at the GILDA beamline.

    PubMed

    Martorana, A; Deganello, G; Longo, A; Deganello, F; Liotta, L; Macaluso, A; Pantaleo, G; Balerna, A; Meneghini, C; Mobilio, S

    2003-03-01

    Time-resolved X-ray diffraction experiments carried out at the beamline BM08-GILDA of ESRF allowed a study of the structural modifications taking place in a Pt/ceria-zirconia catalyst while the CO oxidation reaction was in progress. The capillary tube in which the sample is stored acts effectively as a chemical microreactor that ensures homogeneity of the sample treatments and minimization of diffusion effects. During the flowing of the reactant CO/He mixture, the investigated catalyst undergoes a fast Ce(IV)-Ce(III) partial reduction that involves the release of one O atom for every two reduced Ce cations. Because Ce(III) has a larger ionic radius than Ce(IV), the structural modification produces an increase of the lattice constant of the ceria-zirconia mixed oxide, and this increase is monitored by the translating imaging-plate device implemented at GILDA. The CO(2) resulting from the oxidation of the fluxed CO is monitored by a quadrupole mass spectrometer during the recording of the time-resolved X-ray diffraction pattern. The chemical and structural information was combined to show that the CO(2) yield is nearly constant until the catalytic system can provide oxygen for the reaction, while the structural rearrangement of the catalyst is delayed with respect to the switching on of the CO/He flux. After this induction time, during which CO(2) is produced with no structural modification of the catalyst, a fast increase of the lattice constant takes place. PMID:12606797

  5. Combined X-Ray and Neutron Powder Diffraction Studies of Nanoscale Ca5-xFex(PO4)3OH Systems

    NASA Astrophysics Data System (ADS)

    Kyriacou, A.; Leventouri, Th.; Chakoumakos, B. C.; Garlea, V. O.; Cruz, C. D.; Rondinone, A. J.; Sorge, K. D.

    2012-02-01

    Multi-substituted hydroxyapatite (HAp) with crystallite size 4-130 nm is the major mineral phase in physiological apatites. Substitutions at all ionic sites affect their physicochemical properties. Fe is one of the minor substitutions at the Ca sites of HAp. It is important because it reduces the solubility of HAp, functioning as a cavities preventive agent, whereas Fe overload leads to a decreased mechanical strength and osteoporosis. Powder x-ray and neutron diffraction methods as well as energy-filtered transmission electron microscopy were used to study the effect of Fe substitution on the crystal structure properties of the Ca(5-x)Fex(PO4)3OH systems. Single phase HAp is identified in systems with x <= 0.1. Hematite is formed for higher x. Simultaneous Rietveld refinement of the x-ray and neutron diffraction patterns reveals an unexpected increase of the a-lattice constant. It is attributed to the increase of the Ca1-O3 and Ca2-O1 interatomic distances indicating a local lattice relaxation. Fe substitutes in both Ca1 and Ca2 sites with a preference to the Ca2 site and an occupancy up to 0.05 for x=0.3. Magnetic measurements reveal a transition from the diamagnetic state of the HAp to the paramagnetic of the Fe-doped systems.

  6. Structure determination of seven phases and solvates of Pigment Yellow 183 and Pigment Yellow 191 from X-ray powder and single-crystal data.

    PubMed

    Ivashevskaya, Svetlana N; van de Streek, Jacco; Djanhan, Juste E; Brüning, Jürgen; Alig, Edith; Bolte, Michael; Schmidt, Martin U; Blaschka, Peter; Höffken, Hans Wolfgang; Erk, Peter

    2009-04-01

    The crystal structures of two industrially produced laked yellow pigments, Pigment Yellow 183 [P.Y. 183, Ca(C16H10Cl2N4O7S2), alpha phase] and Pigment Yellow 191 [P.Y. 191, Ca(C17H13ClN4O7S2), alpha and beta phases], were determined from laboratory X-ray powder diffraction data. The coordinates of the molecular fragments of the crystal structures were found by means of real-space methods (simulated annealing) with the program DASH. The coordinates of the calcium ions and the water molecules were determined by combining real-space methods (DASH and MRIA) and repeated Rietveld refinements (TOPAS) of the partially finished crystal structures. TOPAS was also used for the final Rietveld refinements. The crystal structure of beta-P.Y. 183 was determined from single-crystal data. The alpha phases of the two pigments are isostructural, whereas the beta phases are not. All four phases exhibit a double-layer structure, built from nonpolar layers containing the C/N backbone and polar layers containing the calcium ions, sulfonate groups and water molecules. Furthermore, the crystal structures of an N,N-dimethylformamide solvate of P.Y. 183, and of P.Y. 191 solvates with N,N-dimethylformamide and N,N-dimethylacetamide were determined by single-crystal X-ray analysis. PMID:19299877

  7. Copper doped TiO2 nanoparticles characterized by X-ray absorption spectroscopy, total scattering, and powder diffraction – a benchmark structure–property study

    SciTech Connect

    Lock, Nina; Jensen, Ellen M. L.; Mi, Jianli; Mamakhel, Aref; Norén, Katarina; Qingbo, Meng; Iversen, Bo B.

    2013-01-01

    Metal functionalized nanoparticles potentially have improved properties e.g. in catalytic applications, but their precise structures are often very challenging to determine. Here we report a structural benchmark study based on tetragonal anatase TiO2 nanoparticles containing 0–2 wt% copper. The particles were synthesized by continuous flow synthesis under supercritical water–isopropanol conditions. Size determination using synchrotron PXRD, TEM, and X-ray total scattering reveals 5–7 nm monodisperse particles. The precise dopant structure and thermal stability of the highly crystalline powders were characterized by X-ray absorption spectroscopy and multi-temperature synchrotron PXRD (300–1000 K). The combined evidence reveals that copper is present as a dopant on the particle surfaces, most likely in an amorphous oxide or hydroxide shell. UV-VIS spectroscopy shows that copper presence at concentrations higher than 0.3 wt% lowers the band gap energy. The particles are unaffected by heating to 600 K, while growth and partial transformation to rutile TiO2 occur at higher temperatures. Anisotropic unit cell behavior of anatase is observed as a consequence of the particle growth (a decreases and c increases).

  8. Rb+ adsorption at the quartz(101)-aqueous interface: comparison of resonant anomalous x-ray reflectivity with ab initio calculations

    SciTech Connect

    Bellucci, Francesco; Lee, Sang Soo; Kubicki, James D.; Bandura, Andrei V.; Zhang, Zhan; Wesolowski, David J.; Fenter, Paul

    2015-01-29

    We study adsorption of Rb+ to the quartz(101)–aqueous interface at room temperature with specular X-ray reflectivity, resonant anomalous X-ray reflectivity, and density functional theory. The interfacial water structures observed in deionized water and 10 mM RbCl solution at pH 9.8 were similar, having a first water layer at height of 1.7 ± 0.1 Å above the quartz surface and a second layer at 4.8 ± 0.1 Å and 3.9 ± 0.8 Å for the water and RbCl solutions, respectively. The adsorbed Rb+ distribution is broad and consists of presumed inner-sphere (IS) and outer-sphere (OS) complexes at heights of 1.8 ± 0.1 and 6.4 ± 1.0 Å, respectively. Projector-augmented planewave density functional theory (DFT) calculations of potential configurations for neutral and negatively charged quartz(101) surfaces at pH 7 and 12, respectively, reveal a water structure in agreement with experimental results. These DFT calculations also show differences in adsorbed speciation of Rb+ between these two conditions. At pH 7, the lowest energy structure shows that Rb+ adsorbs dominantly as an IS complex, whereas at pH 12 IS and OS complexes have equivalent energies. The DFT results at pH 12 are generally consistent with the two site Rb distribution observed from the X-ray data at pH 9.8, albeit with some differences that are discussed. In conclusion, surface charge estimated on the basis of the measured total Rb+ coverage was -0.11 C/m2, in good agreement with the range of the surface charge magnitudes reported in the literature.

  9. Lithium cobalt(II) pyrophosphate, Li[subscript 1.86]CoP[subscript 2]O[subscript 7], from synchrotron X-ray powder data

    SciTech Connect

    Zhou, Hui; Upreti, Shailesh; Chernova, Natasha A.; Whittingham, M.Stanley

    2015-10-15

    Structure refinement of high-resolution X-ray powder diffraction data of the title compound gave the composition Li{sub 1.865}CoP{sub 2}O{sub 7}, which is also verified by the ICP measurement. Two Co sites exist in the structure: one is a CoO{sub 5} square pyramid and the other is a CoO{sub 6} octahedron. They share edges and are further interconnected through P{sub 2}O{sub 7} groups, forming a three-dimensional framework, which exhibits different kinds of intersecting tunnels containing Li cations and could be of great interest in Li ion battery chemistry. The structure also exhibits cation disorder with 13.5% Co residing at the lithium (Li1) site. Co seems to have an average oxidation state of 2.135, as obtained from the strutural stochiometry that closely supports the magnetic susceptibility findings.

  10. Structure and electronic properties of Dy@C 82 studied by UV-VIS absorption, X-ray powder diffraction and XAFS

    NASA Astrophysics Data System (ADS)

    Iida, S.; Kubozono, Y.; Slovokhotov, Y.; Takabayashi, Y.; Kanbara, T.; Fukunaga, T.; Fujiki, S.; Emura, S.; Kashino, S.

    2001-04-01

    Two isomers of Dy@C 82 were separated by high performance liquid chromatography (HPLC), and their UV-VIS absorption spectra were measured to characterize these isomers. The crystalline powder of Dy@C 82 was obtained by removing the solvent (toluene) at 250°C under vacuum. The X-ray diffraction pattern can be indexed with fcc crystal lattice, as that in La@C 82. The lattice constant a at 298 K, 15.86(1) Å, is close to that of La@C 82, 15.78 Å. The distances between Dy and the first and second nearest C atoms are determined to be 2.52(2) and 2.86(2) Å, respectively, on the basis of Dy L III-edge EXAFS. The XANES shows that the valence of the Dy atom in Dy@C 82 is +3.

  11. Crystal Structures of the Trifluoromethyl Sulfonates M(SO3CF3)2 (M = Mg, Ca, Ba, Zn, Cu) from Synchrotron X-ray Powder Diffraction Data

    SciTech Connect

    Dinnebier,R.; Sofina, N.; Hildebrandt, L.; Jansen, M.

    2006-01-01

    The crystal structures of divalent metal salts of trifluoromethyl sulfonic acid ('trifluoromethyl sulfonates') M(SO{sub 3}CF{sub 3}){sub 2} (M = Mg, Ca, Ba, Zn, Cu) were determined from high-resolution X-ray powder diffraction data. Magnesium, calcium and zinc trifluoromethyl sulfonate crystallize in the rhombohedral space group R{bar 3}. Barium trifluoromethyl sulfonate crystallizes in the monoclinic space group I2/a(C2/c) and copper trifluoromethyl sulfonate crystallizes in the triclinic group P{bar 1}. Within the crystal structures the trifluoromethyl sulfonate anions are arranged in double layers with the apolar CF{sub 3} groups pointing towards each other. The cations are located next to the SO{sub 3} groups. The symmetry relations between the different crystal structures have been analyzed.

  12. Vacancy-induced nanoscale phase separation in KxFe2–ySe₂ single crystals evidenced by Raman scattering and powder x-ray diffraction

    DOE PAGESBeta

    Lazarević, N.; Abeykoon, M.; Stephens, P. W.; Lei, Hechang; Bozin, E. S.; Petrovic, C.; Popović, Z. V.

    2012-08-06

    Polarized Raman scattering spectra of KxFe2–ySe₂ were analyzed in terms of peculiarities of both I4/m and I4/mmm space group symmetries. The presence of the Raman active modes from both space group symmetries (16 Raman-active modes of the I4/m phase and two Raman-active modes of the I4/mmm phase) confirmed the existence of two crystallographic domains with different space group symmetry in a KxFe2–ySe₂ sample. High-resolution synchrotron powder x-ray diffraction structural refinement of the same sample confirmed the two-phase description, and determined the atomic positions and occupancies for both domains.

  13. Functional biocompatible magnetite-cellulose nanocomposite fibrous networks: Characterization by fourier transformed infrared spectroscopy, X-ray powder diffraction and field emission scanning electron microscopy analysis

    NASA Astrophysics Data System (ADS)

    Habibi, Neda

    2015-02-01

    The preparation and characterization of functional biocompatible magnetite-cellulose nano-composite fibrous material is described. Magnetite-cellulose nano-composite was prepared by a combination of the solution-based formation of magnetic nano-particles and subsequent coating with amino celluloses. Characterization was accomplished using X-ray powder diffraction (XRD), fourier transformed infrared (FTIR) and field emission scanning electron microscopy (FESEM) analysis. The peaks of Fe3O4 in the XRD pattern of nanocomposite confirm existence of the nanoparticles in the amino cellulose matrix. Magnetite-cellulose particles exhibit an average diameter of roughly 33 nm as demonstrated by field emission scanning electron microscopy. Magnetite nanoparticles were irregular spheres dispersed in the cellulose matrix. The vibration corresponding to the Nsbnd CH3 functional group about 2850 cm-1 is assigned in the FTIR spectra. Functionalized magnetite-cellulose nano-composite polymers have a potential range of application as targeted drug delivery system in biomedical field.

  14. Quadrupole lamp furnace for high temperature (up to 2050 K) synchrotron powder x-ray diffraction studies in air in reflection geometry

    SciTech Connect

    Sarin, P.; Yoon, W.; Jurkschat, K.; Zschack, P.; Kriven, W. M.

    2006-09-15

    A four-lamp thermal image furnace has been developed to conduct high temperature x-ray diffraction in reflection geometry on oxide ceramic powder samples in air at temperatures {<=}2050 K using synchrotron radiation. A refractory crucible made of Pt20%Rh alloy was used as a specimen holder. A material with well characterized lattice expansion properties was used as an internal crystallographic thermometer to determine the specimen temperature and displacement. The performance of the apparatus was verified by measurement of the thermal expansion properties of CeO{sub 2}, MgO, and Pt which were found to be within {+-}3% of the acceptable values. The advantages, limitations, and important considerations of the instrument developed are discussed.

  15. Quadrupole lamp furnace for high temperature (up to 2050 K) synchrotron powder x-ray diffraction studies in air in reflection geometry.

    SciTech Connect

    Sarin, P.; Yoon, W.; Jurkschat, K.; Zschack, P.; Kriven, W. M.; Univ. of Illinois; Frederick-Seitz Materials Research Lab.

    2006-09-01

    A four-lamp thermal image furnace has been developed to conduct high temperature x-ray diffraction in reflection geometry on oxide ceramic powder samples in air at temperatures {le} 2050 K using synchrotron radiation. A refractory crucible made of Pt20%Rh alloy was used as a specimen holder. A material with well characterized lattice expansion properties was used as an internal crystallographic thermometer to determine the specimen temperature and displacement. The performance of the apparatus was verified by measurement of the thermal expansion properties of CeO{sub 2}, MgO, and Pt which were found to be within {+-} 3% of the acceptable values. The advantages, limitations, and important considerations of the instrument developed are discussed.

  16. Testing the limits of sensitivity in a solid-state structural investigation by combined X-ray powder diffraction, solid-state NMR, and molecular modelling.

    PubMed

    Filip, Xenia; Borodi, Gheorghe; Filip, Claudiu

    2011-10-28

    A solid state structural investigation of ethoxzolamide is performed on microcrystalline powder by using a multi-technique approach that combines X-ray powder diffraction (XRPD) data analysis based on direct space methods with information from (13)C((15)N) solid-state Nuclear Magnetic Resonance (SS-NMR) and molecular modeling. Quantum chemical computations of the crystal were employed for geometry optimization and chemical shift calculations based on the Gauge Including Projector Augmented-Wave (GIPAW) method, whereas a systematic search in the conformational space was performed on the isolated molecule using a molecular mechanics (MM) approach. The applied methodology proved useful for: (i) removing ambiguities in the XRPD crystal structure determination process and further refining the derived structure solutions, and (ii) getting important insights into the relationship between the complex network of non-covalent interactions and the induced supra-molecular architectures/crystal packing patterns. It was found that ethoxzolamide provides an ideal case study for testing the accuracy with which this methodology allows to distinguish between various structural features emerging from the analysis of the powder diffraction data. PMID:21931906

  17. Calorimetry investigations of milled α-tricalcium phosphate (α-TCP) powders to determine the formation enthalpies of α-TCP and X-ray amorphous tricalcium phosphate.

    PubMed

    Hurle, Katrin; Neubauer, Juergen; Bohner, Marc; Doebelin, Nicola; Goetz-Neunhoeffer, Friedlinde

    2015-09-01

    One α-tricalcium phosphate (α-TCP) powder was either calcined at 500°C to obtain fully crystalline α-TCP or milled for different durations to obtain α-TCP powders containing various amounts of X-ray amorphous tricalcium phosphate (ATCP). These powders containing between 0 and 71wt.% ATCP and up to 2.0±0.1wt.% β-TCP as minor phase were then hydrated in 0.1M Na2HPO4 aqueous solution and the resulting heat flows were measured by isothermal calorimetry. Additionally, the evolution of the phase composition during hydration was determined by in situ XRD combined with the G-factor method, an external standard method which facilitates the indirect quantification of amorphous phases. Maximum ATCP hydration was reached after about 1h, while that of crystalline α-TCP hydration occurred between 4 and 11h, depending on the ATCP content. An enthalpy of formation of -4065±6kJ/mol (T=23°C) was calculated for ATCP (Ca3(PO4)2), while for crystalline α-TCP (α-Ca3(PO4)2) a value of -4113±6kJ/mol (T=23°C) was determined. PMID:26026302

  18. A combined solid-state NMR and synchrotron x-ray diffraction powder study on the structure of the antioxidant(+)-catechin 4.5 hydrate.

    SciTech Connect

    Harper, J. K.; Doebbler, J. A.; Jaccques, E.; Grant, D. M.; Von Dreele, R. B.; Univ. of Utah

    2010-03-10

    Analyses combining X-ray powder diffraction (XRD) and solid-state NMR (SSNMR) data can now provide crystal structures in challenging powders that are inaccessible by traditional methods. The flavonoid catechin is an ideal candidate for these methods, as it has eluded crystallographic characterization despite extensive study. Catechin was first described nearly two centuries ago, and its powders exhibit numerous levels of hydration. Here, synchrotron XRD data provide all heavy-atom positions in (+)-catechin 4.5-hydrate and establish the space group as C2. SSNMR data ({sup 13}C tensor and {sup 1}H/{sup 13}C correlation) complete the conformation by providing catechin's five OH hydrogen orientations. Since 1903, this phase has been erroneously identified as a 4.0 hydrate, but XRD and density data establish that this discrepancy is due to the facile loss of the water molecule located at a Wyckoff special position in the unit cell. A final improvement to heavy-atom positions is provided by a geometry optimization of bond lengths and valence angles with XRD torsion angles held constant. The structural enhancement in this final structure is confirmed by the significantly improved fit of computed {sup 13}C tensors to experimental data.

  19. Single-crystal and humidity-controlled powder diffraction study of the breathing effect in a metal-organic framework upon water adsorption/desorption.

    PubMed

    Aríñez-Soriano, Javier; Albalad, Jorge; Vila-Parrondo, Christian; Pérez-Carvajal, Javier; Rodríguez-Hermida, Sabina; Cabeza, Aurelio; Juanhuix, Jordi; Imaz, Inhar; Maspoch, Daniel

    2016-05-26

    Herein we report a study on water adsorption/desorption-triggered single-crystal to single-crystal transformations in a MOF, by single-crystal and humidity-controlled powder X-ray diffraction and water-sorption measurements. We identified a gate-opening effect at a relative humidity of 85% upon water adsorption, and a gate-closure effect at a relative humidity of 55 to 77% upon water desorption. This reversible breathing effect between the "open" and the "closed" structures of the MOF involves the cleavage and formation of several coordination bonds. PMID:27228426

  20. Characterization of the Adsorption of Nucleic Acid Bases onto Ferrihydrite via Fourier Transform Infrared and Surface-Enhanced Raman Spectroscopy and X-ray Diffractometry.

    PubMed

    Canhisares-Filho, José E; Carneiro, Cristine E A; de Santana, Henrique; Urbano, Alexandre; da Costa, Antonio C S; Zaia, Cássia T B V; Zaia, Dimas A M

    2015-09-01

    Minerals could have played an important role in concentration, protection, and polymerization of biomolecules. Although iron is the fourth most abundant element in Earth's crust, there are few works in the literature that describe the use of iron oxide-hydroxide in prebiotic chemistry experiments. In the present work, the interaction of adenine, thymine, and uracil with ferrihydrite was studied under conditions that resemble those of prebiotic Earth. At acidic pH, anions in artificial seawater decreased the pH at the point of zero charge (pHpzc) of ferrihydrite; and at basic pH, cations increased the pHpzc. The adsorption of nucleic acid bases onto ferrihydrite followed the order adenine > uracil > thymine. Adenine adsorption peaked at neutral pH; however, for thymine and uracil, adsorption increased with increasing pH. Electrostatic interactions did not appear to play an important role on the adsorption of nucleic acid bases onto ferrihydrite. Adenine adsorption onto ferrihydrite was higher in distilled water compared to artificial seawater. After ferrihydrite was mixed with artificial seawaters or nucleic acid bases, X-ray diffractograms and Fourier transform infrared spectra did not show any change. Surface-enhanced Raman spectroscopy showed that the interaction of adenine with ferrihydrite was not pH-dependent. In contrast, the interactions of thymine and uracil with ferrihydrite were pH-dependent such that, at basic pH, thymine and uracil lay flat on the surface of ferrihydrite, and at acidic pH, thymine and uracil were perpendicular to the surface. Ferrihydrite adsorbed much more adenine than thymine; thus adenine would have been better protected against degradation by hydrolysis or UV radiation on prebiotic Earth. PMID:26393397

  1. Precipitation and surface adsorption of metal complexes during electropolishing. Theory and characterization with X-ray nanotomography and surface tension isotherms.

    PubMed

    Nave, Maryana I; Chen-Wiegart, Yu-chen Karen; Wang, Jun; Kornev, Konstantin G

    2015-09-21

    Electropolishing of metals often leads to supersaturation conditions resulting in precipitation of complex compounds. The solubility diagrams and Gibbs adsorption isotherms of the electropolishing products are thus very important to understand the thermodynamic mechanism of precipitation of reaction products. Electropolishing of tungsten wires in aqueous solutions of potassium hydroxide is used as an example illustrating the different thermodynamic scenarios of electropolishing. Electropolishing products are able to form highly viscous films immiscible with the surrounding electrolyte or porous shells adhered to the wire surface. Using X-ray nanotomography, we discovered a gel-like phase formed at the tungsten surface during electropolishing. The results of these studies suggest that the electropolishing products can form a rich library of compounds. The surface tension of the electrolyte depends on the metal oxide ions and alkali-metal complexes. PMID:26279498

  2. X-ray absorption fine structure combined with fluorescence spectrometry for monitoring trace amounts of lead adsorption in the environmental conditions.

    PubMed

    Izumi, Yasuo; Kiyotaki, Fumitaka; Minato, Taketoshi; Seida, Yoshimi

    2002-08-01

    The local structure of trace amounts of lead in an adsorbent matrix that contains a high concentration of iron and magnesium (Mg6Fe2(OH)16(CO3) x 3H2O) was successfully monitored by means of X-ray absorption fine structure spectroscopy combined with fluorescence spectrometry. A eutectic mixture of PbCO3 and Pb(OH)2 coagulated when Pb2+ was adsorbed from a 1.0 ppm aqueous solution, and in contrast, the major species was ion-exchanged Pb2+ in the case of adsorption from a 100 ppb aqueous solution. The difference was ascribed to the balance between the precipitation equilibrium for coagulation and the rate of the ion exchange reaction with surface hydroxyl groups. PMID:12175171

  3. In-situ X-ray diffraction and STM studies of bromide adsorption on Au(111) electrodes

    SciTech Connect

    Magnussen, O.M.; Ocko, B.M; Wang, J.X.; Adzic, R.R.

    1996-03-28

    The structure of bromide adlayers at the Au(111)-aqueous solution interface has been studied by in-situ surface X-ray scattering (SXS) and scanning tunneling microscopy (STM). Both techniques show the existence of a hexagonal close-packed adlayer phase above a critical potential and are in good quantitative agreement on the adlayer structural parameters. The bromide-bromide spacing changes continuously between 4.24 A at the critical potential and 4.03 A at a potential 300 mV more positive. The adlayer is rotated relative to the substrate by an angle dependent on potential and bromide concentration. The potential- dependent adlayer density corresponding to these structural results agrees well with Br surface excess densities from published electrochemical measurements. At very positive potentials a bromide-induced step-flow etching of the Au substrate is observed. The results are used to compare the different techniques and to discuss the adlayer structure, the phase behavior, and the halide-gold chemical interaction. 49 refs., 8 figs.

  4. X-ray photoelectron spectroscopy of fast-frozen hematite colloids in aqueous solutions. 5. Halide ion (F-, Cl-, Br-, I-) adsorption.

    PubMed

    Shimizu, Kenichi; Shchukarev, Andrey; Kozin, Philipp A; Boily, Jean-François

    2013-02-26

    Halide anion (F(-), Cl(-), Br(-), and I(-)) adsorption and its impact on sodium adsorption at the hematite/water interface were studied by cryogenic X-ray photoelectron spectroscopy (XPS). Measurements were carried out on frozen, centrifuged wet hematite pastes that were previously equilibrated in 50 mM electrolytic solutions in the pH 2-11 range. XPS-derived halide ion surface loadings decreased in the order F(-) > I(-) ≈ Cl(-) > Br(-), whereas sodium loadings were in the order Na(F) > Na(I) > Na(Br) > Na(Cl). The greater sodium loadings in NaF and in NaI resulted from larger anion loadings in these systems. Bromide ion had the lowest loading among all halide ions despite having a charge-to-size ratio that is intermediate between those of Cl(-) and I(-). This unexpected result may have arisen from specific properties of the hematite/water interface, such as water structure and electric double layer thickness. Fluoride ion adsorption proceeded via the formation of hydrogen bonds with the surface hydroxo groups (e.g., ≡Fe-OH(2)···F(-) or ≡Fe-OH···F(-)). Surface-bound fluoride ions exert a greater charge-screening effect than the other halide anions, as demonstrated by considerably small zeta potential values. Fe-F bond formation was excluded as a possible interfacial process as the F 1s peak binding energy (684.2 eV) was more comparable to that of NaF (684.6 eV) than FeF(3) (685.4 eV). Overall, these findings motivate further refinements of existing thermodynamic adsorption models for predicting the ionic composition of hematite particle surfaces contacted with sodium halide aqueous solutions. PMID:23347248

  5. X-ray powder diffraction beamline at D10B of LNLS: application to the Ba2FeReO6 double perovskite.

    PubMed

    Ferreira, Fabio Furlan; Granado, Eduardo; Carvalho, Wilson; Kycia, Stefan W; Bruno, Daniele; Droppa, Roosevelt

    2006-01-01

    A new beamline, fully dedicated to X-ray powder diffraction (XPD) measurements, has been installed after the exit port B of the bending magnet D10 at the Brazilian Synchrotron Light Laboratory (LNLS) and commissioned. The technical characteristics of the beamline are described and some performance indicators are listed, such as the incoming photon flux and the angular/energy resolutions obtainable under typical experimental conditions. The results of a Rietveld refinement for a standard sample of Y2O3 using high-resolution data are shown. The refined parameters match those found in the literature, within experimental error. High-resolution XPD measurements on Ba2FeReO6 demonstrate a slight departure from the ideal cubic double-perovskite structure at low temperatures, not detected by previous powder diffraction experiments. The onset of the structural transition coincides with the ferrimagnetic ordering temperature, Tc approximately equal to 315 K. Subtle structural features, such as those reported here for Ba2FeReO6, as well as the determination and/or refinement of complex crystal structures in polycrystalline samples are ideal candidate problems to be investigated on this beamline. PMID:16371707

  6. Formation of {gamma}-Fe{sub 2}O{sub 3} nanoparticles and vacancy ordering: An in situ X-ray powder diffraction study

    SciTech Connect

    Jorgensen, Jens-Erik Mosegaard, Lene; Thomsen, Line E.; Jensen, Torben R.; Hanson, Jonathan C.

    2007-01-15

    The formation of maghemite, {gamma}-Fe{sub 2}O{sub 3} nanoparticles has been studied by in situ X-ray powder diffraction. The maghemite was formed by thermal decomposition of an amorphous precursor compound made by reacting lauric acid, CH{sub 3}(CH{sub 2}){sub 10}COOH with Fe(NO{sub 3}){sub 3}.9H{sub 2}O. It has been shown that cubic {gamma}-Fe{sub 2}O{sub 3} was formed directly from the amorphous precursor and that vacancy ordering starts about 45 min later at 305 deg. C resulting in a tripled unit cell along the c-axis. The kinetics of grain growth was found to obey a power law with growth exponents n equal to 0.136(6) and 0.103(5) at 305 and 340 deg. C, respectively. Particles with average sizes of 12 and 13 nm were obtained in 86 and 76 min at 305 and 340 deg. C, respectively. The structure of cubic and vacancy ordered phases of {gamma}-Fe{sub 2}O{sub 3} was studied at 305 deg. C by Rietveld refinements. - Graphical abstract: Stack of powder diagrams showing the formation of {gamma}-Fe{sub 2}O{sub 3} nanoparticles and subsequent vacancy ordering at 305 deg. C.

  7. 5-Arylidene derivatives of Meldrum's acid: Synthesis, structural characterization using single crystal and powder crystal X-ray diffraction, and electronic properties

    NASA Astrophysics Data System (ADS)

    Dey, Tanusri; Ghosh, Soumen; Ghosh, Somnath; Mukherjee, Alok Kumar

    2015-07-01

    Four 5-arylidene derivatives of Meldrum's acid, 5-(4-chlorobenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (2), 5-(3-hydroxybenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (3), 5-(3,4-dimethoxybenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (4) and 5-(2,4-dimethoxy benzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (5) have been synthesized and their crystal structures have been determined using single crystal X-ray diffractometry for 2, 4 and 5 and X-ray powder diffraction for 3. The nature of intermolecular interactions in 2-5 has been analyzed through Hirshfeld surfaces and 2D fingerprint plots. The DFT optimized molecular geometries in 2-5 agree closely with those obtained from the crystallographic studies. The crystal packing in 2-5 exhibits an interplay of Osbnd H⋯O, Csbnd H⋯O, Csbnd H⋯Cl and Csbnd H⋯π (arene) hydrogen bonds and π⋯π interactions, which assemble molecules into three-dimensional architecture in 2, 3 and 5 and two-dimensional framework in 4. The Hirshfeld surface analyses of 2-5, Meldrum's acid (1) and a few related 5-arylidene derivatives of Meldrum's acid retrieved from the Cambridge Structural Database (CSD) indicate that about 85% of the Hirshfeld surface area (72% in 2 where H⋯Cl contribution is about 13%) in this class of compounds are due to H⋯H, O⋯H and C⋯H contacts. The HOMO-LUMO energy gap (>2.2 eV) in 2-5 indicates a significant degree of internal charge transfer within the molecule.

  8. In situ SERS and X-ray photoelectron spectroscopy studies on the pH-dependant adsorption of anthraquinone-2-carboxylic acid on silver electrode

    NASA Astrophysics Data System (ADS)

    Li, Dan; Jia, Shaojie; Fodjo, Essy Kouadio; Xu, Hu; Wang, Yuhong; Deng, Wei

    2016-03-01

    In this study, in situ surface-enhanced Raman scattering (SERS) spectroelectrochemistry and angle-resolved X-ray photoelectron spectroscopy (AR-XPS) are used to investigate the redox reaction and adsorption behavior of anthraquinone-2-carboxylic acid (AQ-2-COOH) on an Ag electrode at different pH values. The obtained results indicate that AQ-2-COOH is adsorbed tilted on the Ag electrode through O-atom of ring carbonyl in a potential range from -0.3 to -0.5 V vs. SCE, but the orientation turns to more tilted orientation with both O-atom of the ring carbonyl and carboxylate group in positive potential region for pH 6.0 and 7.4. However, at pH 10.0, the orientation adopts tilted conformation constantly on the Ag electrode with both O-atom of the anthraquinone ring and carboxylate group in the potential range from -0.3 to -0.5 V vs. SCE or at positive potentials. Moreover, the adsorption behavior of AQ-2-COOH has been further confirmed by AR-XPS on the Ag surface. Proposed reasons for the observed changes in orientation are presented.

  9. Adsorption of cadmium to Bacillus subtilis bacterial cell walls: a pH-dependent X-ray absorption fine structure spectroscopy study

    NASA Astrophysics Data System (ADS)

    Boyanov, M. I.; Kelly, S. D.; Kemner, K. M.; Bunker, B. A.; Fein, J. B.; Fowle, D. A.

    2003-09-01

    The local atomic environment of Cd bound to the cell wall of the gram-positive bacterium Bacillus subtilis was determined by X-ray absorption fine structure (XAFS) spectroscopy. Samples were prepared at six pH values in the range 3.4 to 7.8, and the bacterial functional groups responsible for the adsorption were identified under each condition. Under the experimental Cd and bacterial concentrations, the spectroscopy results indicate that Cd binds predominantly to phosphoryl ligands below pH 4.4, whereas at higher pH, adsorption to carboxyl groups becomes increasingly important. At pH 7.8, we observe the activation of an additional binding site, which we tentatively ascribe to a phosphoryl site with smaller Cd-P distance than the one that is active at lower pH conditions. XAFS spectra of several cadmium acetate, phosphate, and perchlorate solutions were measured and used as standards for fingerprinting, as well as to assess the ability of FEFF8 and FEFFIT to model carboxyl, phosphoryl, and hydration environments, respectively. The results of this XAFS study in general corroborate existing surface complexation models; however, some binding mechanism details could only be detected with the XAFS technique.

  10. Insights into Surface Interactions between Metal Organic Frameworks and Gases during Transient Adsorption and Diffusion by In-Situ Small Angle X-ray Scattering.

    PubMed

    Dumée, Ludovic F; He, Li; Hodgson, Peter; Kong, Lingxue

    2016-01-01

    The fabrication of molecular gas sieving materials with specific affinities for a single gas species and able to store large quantities of materials at a low or atmospheric pressure is desperately required to reduce the adverse effects of coal and oil usage in carbon capture. Fundamental understanding of the dynamic adsorption of gas, the diffusion mechanisms across thin film membranes, and the impact of interfaces play a vital role in developing these materials. In this work, single gas permeation tests across micro-porous membrane materials, based on metal organic framework crystals grown on the surface of carbon nanotubes (ZiF-8@CNT), were performed for the first time in-situ at the Australian Synchrotron on the small angle X-ray scattering beamline in order to reveal molecular sieving mechanisms and gas adsorption within the material. The results show that specific chemi-sorption of CO₂ across the ZiF-8 crystal lattices affected the morphology and unit cell parameters, while the sieving of other noble or noble like gases across the ZiF-8@CNT membranes was found to largely follow Knudsen diffusion. This work demonstrates for the first time a novel and effective technique to assess molecular diffusion at the nano-scale across sub-nano-porous materials by probing molecular flexibility across crystal lattice and single cell units. PMID:27598211

  11. Abinitio powder x-ray diffraction and PIXEL energy calculations on thiophene derived 1,4 dihydropyridine

    NASA Astrophysics Data System (ADS)

    Karthikeyan, N.; Pachamuthu, M. P.; Sivakumar, K.

    2016-05-01

    We focus on the application of powder diffraction data to get abinitio crystal structure determination of thiophene derived 1,4 DHP prepared by cyclocondensation method using solid catalyst. Crystal structure of the compound has been solved by direct-space approach on Monte Carlo search in parallel tempering mode using FOX program. Initial atomic coordinates were derived using Gaussian 09W quantum chemistry software in semi-empirical approach and Rietveld refinement was carried out using GSAS program. The crystal structure of the compound is stabilized by one N-H…O and three C-H…O hydrogen bonds. PIXEL lattice energy calculation was carried out to understand the physical nature of intermolecular interactions in the crystal packing, on which the total lattice energy is contributed into Columbic, polarization, dispersion, and repulsion energies.

  12. Structural and Thermal Characterization of Zolpidem Hemitartrate Hemihydrate (Form E) and Its Decomposition Products by Laboratory X-Ray Powder Diffraction

    SciTech Connect

    Halasz, I.; Dinnebier, R

    2010-01-01

    The crystal structure of zolpidem hemitartrate hemihydrate (I, Form E) has been solved from high-resolution laboratory powder diffraction data. It crystallizes in the orthorhombic P2{sub 1}2{sub 1}2{sub 1} space group with a = 22.4664(6) {angstrom}, b = 26.0420(7) {angstrom}, and c = 7.4391(1) {angstrom}. Protonation of zolpidem molecules could not be unambiguously determined. Thermal stability of Form E has been investigated by TG-DTA and in situ by temperature resolved X-ray powder diffraction. Water loss occurs between 50 C {le} t {le} 100 C while structure decomposition commences at approximately 120 C yielding zolpidem tartrate (II) and pure zolpidem base (III) in approximately equimolar amounts. Crystal structures of II and III have been solved simultaneously from a single powder pattern of thermally decomposed I. Zolpidem tartrate crystallizes in the orthorhombic P2{sub 1}2{sub 1}2{sub 1} space group with a = 19.9278(8) {angstrom}, b = 15.1345(8) {angstrom}, and c = 7.6246(2) {angstrom} (at 140 C). Zolpidem base crystallizes in the orthorhombic Pcab space group with a = 9.9296(4) {angstrom}, b = 18.4412(9) {angstrom}, and c = 18.6807(9) {angstrom} (at 140 C). In the reported crystal structures zolpidem molecules form stacks through {pi}-{pi} interaction or dipole-dipole interactions while tartrate moieties, if present, form hydrogen bonded chains. Water molecule in I forms a hydrogen bond to the imidazole nitrogen atom of the zolpidem molecule. Free space in the crystal structure of I could allow for the additional water molecules and thus a variable water content.

  13. Effect of calcium on adsorption capacity of powdered activated carbon.

    PubMed

    Li, Gang; Shang, Junteng; Wang, Ying; Li, Yansheng; Gao, Hong

    2013-12-01

    We investigated the effect of calcium ion on the adsorption of humic acid (HA) (as a target pollutant) by powered activated carbon. The HA adsorption isotherms at different pH and kinetics of two different solutions including HA alone and HA doped Ca(2+), were performed. It was showed that the adsorption capacity of powdered activated carbon (PAC) for HA was markedly enhanced when Ca(2+) was doped into HA. Also, HA and Ca(2+) taken as nitrate were tested on the uptake of each other respectively and it was showed that the adsorbed amounts of both of them were significantly promoted when HA and calcium co-existed. Furthermore, the adsorbed amount of HA slightly decreased with the increasing of Ca(2+) concentration, whereas the amount of calcium increased with the increasing of HA concentration, but all above the amounts without addition. Finally, the change of pH before and after adsorption process is studied. In the two different solutions including HA alone and HA doped Ca(2+), pH had a small rise, but the extent of pH of later solution was bigger. PMID:25078809

  14. X-Rays

    MedlinePlus

    X-rays are a type of radiation called electromagnetic waves. X-ray imaging creates pictures of the inside of ... different amounts of radiation. Calcium in bones absorbs x-rays the most, so bones look white. Fat ...

  15. Cosmic x ray physics

    NASA Technical Reports Server (NTRS)

    Mccammon, Dan; Cox, D. P.; Kraushaar, W. L.; Sanders, W. T.

    1990-01-01

    The annual progress report on Cosmic X Ray Physics is presented. Topics studied include: the soft x ray background, proportional counter and filter calibrations, the new sounding rocket payload: X Ray Calorimeter, and theoretical studies.

  16. Cosmic x ray physics

    NASA Technical Reports Server (NTRS)

    Mccammon, Dan; Cox, D. P.; Kraushaar, W. L.; Sanders, W. T.

    1991-01-01

    The annual progress report on Cosmic X Ray Physics for the period 1 Jan. to 31 Dec. 1990 is presented. Topics studied include: soft x ray background, new sounding rocket payload: x ray calorimeter, and theoretical studies.

  17. Joint x-ray

    MedlinePlus

    X-ray - joint; Arthrography; Arthrogram ... x-ray technologist will help you position the joint to be x-rayed on the table. Once in place, pictures are taken. The joint may be moved into other positions for more ...

  18. Adsorption of ammonium dinitramide (ADN) from aqueous solutions. 1. Adsorption on powdered activated charcoal.

    PubMed

    Santhosh, G; Venkatachalam, S; Ninan, K N; Sadhana, R; Alwan, S; Abarna, V; Joseph, M A

    2003-03-17

    Investigations on the adsorption of ammonium dinitramide (NH(4)N(NO(2))(2)) (ADN) from aqueous solutions on powdered activated charcoal (PAC) were carried out in order to find out an effective and easier method of separating ADN from aqueous solutions. The effectiveness of PAC in the selective adsorption of ADN from aqueous solutions of ADN (ADN-F) and ADN in presence of sulfate (SO(4)(2-)) and nitrate (NO(3)(-)) ions (ADN-PS) was examined and compared using batch and column methods. The adsorption process follows both Langmuir and Freundlich adsorption isotherms and the isotherm parameters for the models were determined. The observed data favor the formation of monolayer adsorption. The adsorption capacities were found to be 63.3, 119, 105.3 and 82 mg of ADN per g of PAC for ADN-F (batch), ADN-PS (batch), ADN-F (column) and ADN-PS (column), respectively. Break-through curves for ADN-F and ADN-PS were obtained for the optimization of separation of ADN from aqueous solutions. Elution curves were generated for the desorption of ADN from PAC using hot water as eluent. PMID:12628781

  19. The use of net analyte signal orthogonalization in the separation of multi-component diffraction patterns obtained from X-ray powder diffraction of intact compacts.

    PubMed

    Moore, Michael D; Cogdill, Robert P; Short, Steven M; Hair, Colleen R; Wildfong, Peter L D

    2008-06-01

    X-ray powder diffraction (XRPD) analysis of intact multi-component consolidated mixtures has significant potential owing to the ability to non-destructively quantify and discriminate between solid phases in composite bodies with minimal sample preparation. There are, however, limitations to the quantitative power using traditional univariate methods on diffraction data containing features from all components in the system. The ability to separate multi-component diffraction data into patterns representing single constituents allows both composition as well as physical phenomena associated with the individual components of complex systems to be probed. Intact, four-component compacts, consisting of two crystalline and two amorphous constituents were analyzed using XRPD configured in both traditional Bragg-Brentano reflectance geometry and parallel-beam transmission geometry. Two empirical, model-based methods consisting of a multiple step net analyte signal (NAS) orthogonalization are presented as ways to separate multi-component XRPD patterns into single constituent patterns. Multivariate figures of merit (FOM) were calculated for each of the isolated constituents to compare method-specific parameters such as sensitivity, selectivity, and signal-to-noise, enabling quantitative comparisons between the two modes of XRPD analysis. PMID:18294800

  20. The Optics and Alignment of the Divergent Beam Laboratory X-ray Powder Diffractometer and its Calibration Using NIST Standard Reference Materials.

    PubMed

    Cline, James P; Mendenhall, Marcus H; Black, David; Windover, Donald; Henins, Albert

    2015-01-01

    The laboratory X-ray powder diffractometer is one of the primary analytical tools in materials science. It is applicable to nearly any crystalline material, and with advanced data analysis methods, it can provide a wealth of information concerning sample character. Data from these machines, however, are beset by a complex aberration function that can be addressed through calibration with the use of NIST Standard Reference Materials (SRMs). Laboratory diffractometers can be set up in a range of optical geometries; considered herein are those of Bragg-Brentano divergent beam configuration using both incident and diffracted beam monochromators. We review the origin of the various aberrations affecting instruments of this geometry and the methods developed at NIST to align these machines in a first principles context. Data analysis methods are considered as being in two distinct categories: those that use empirical methods to parameterize the nature of the data for subsequent analysis, and those that use model functions to link the observation directly to a specific aspect of the experiment. We consider a multifaceted approach to instrument calibration using both the empirical and model based data analysis methods. The particular benefits of the fundamental parameters approach are reviewed. PMID:26958446

  1. Rietveld refinement of the semiconducting system Bi{sub 2-x}Fe{sub x}Te{sub 3} from X-ray powder diffraction

    SciTech Connect

    Adam, Alia

    2007-12-04

    The semiconducting system Bi{sub 2-x}Fe{sub x}Te{sub 3} (x = 0.0, 0.02, 0.04 and 0.08) was synthesized at 1000 deg. C for 30 h. The scanning electron microscope (SEM) image reveals the tendency of the Bi{sub 2-x}Fe{sub x}Te{sub 3} system to form a sheet structure with more pronounced alignment and to enhance the formation of some microstructure tubes. The structure of the system under study was refined on the basis of X-ray powder diffraction data using the Rietveld method. The analysis revealed the complete miscibility of Fe in the Bi{sub 2}Te{sub 3} matrix and hence the formation of single phase. The system crystallizes in the space group R-3m [1 6 6]. The lattice parameters and the unit cell size slightly change by the incorporation of Fe. The refinement of instrumental and structural parameters led to reliable values for the R{sub B}, R{sub F} and Chi{sup 2}.

  2. In situ synchrotron X-ray powder diffraction for studying the role of induced structural defects on the thermoluminescence mechanism of nanocrystalline LiF.

    PubMed

    El Ashmawy, Mostafa; Amer, Hany; Abdellatief, Mahmoud

    2016-03-01

    The correlation between the thermoluminescence (TL) response of nanocrystalline LiF and its microstructure was studied. To investigate the detailed TL mechanism, the glow curves of nanocrystalline LiF samples produced by high-energy ball-milling were analyzed. The microstructure of the prepared samples was analyzed by synchrotron X-ray powder diffraction (XRPD) at room temperature. Then, the microstructure of a representative pulverized sample was investigated in detail by performing in situ XRPD in both isothermal and non-isothermal modes. In the present study, the dislocations produced by ball-milling alter the microstructure of the lattice where the relative concentration of the vacancies, responsible for the TL response, changes with milling time. An enhancement in the TL response was recorded for nanocrystalline LiF at high-temperature traps (after dislocations recovery starts >425 K). It is also found that vacancies are playing a major role in the dislocations recovery mechanism. Moreover, the interactions among vacancies-dislocations and/or dislocations-dislocations weaken the TL response. PMID:26917138

  3. The Stoichiometry of Synthetic Alunite as a Function of Hydrothermal Aging Investigated by Solid-State NMR Spectroscopy, Powder X-ray Diffraction and Infrared Spectroscopy

    SciTech Connect

    Grube, Elisabeth; Nielsen, Ulla Gro

    2015-05-01

    The stoichiometry of a series of synthetic alunite [nominally KAl3(SO4)2(OH)6] samples prepared by hydrothermal methods as a function of reaction time (1–31 days) has been investigated by powder X-ray diffraction, Fourier transform infrared spectroscopy as well as solid-state 1H and 27Al magic angle spinning (MAS) nuclear magnetic resonance (NMR) spectroscopy. The 1H MAS NMR spectra recorded at high magnetic field (21.1 T, 900 MHz) allowed for a clear separation of the different proton environments and for quantitative determination of the aluminum vacancy concentration as a function of time. The concentration of structural defects determined from, i.e., aluminum vacancies was reduced from 4 to 1 %, as the reaction time was extended from one to 31 days based on 1H MAS NMR. This was further supported by an increase of the unit cell parameter c, which is indicative of the relative concentration of potassium defects present, from 17.261(1) to 17.324(5) Å. Solid-state 27Al MAS NMR revealed a decrease in the defect concentration as a function of time and showed the presence of 7–10 % impurities in the samples.

  4. The Optics and Alignment of the Divergent Beam Laboratory X-ray Powder Diffractometer and its Calibration Using NIST Standard Reference Materials

    PubMed Central

    Cline, James P.; Mendenhall, Marcus H.; Black, David; Windover, Donald; Henins, Albert

    2015-01-01

    The laboratory X-ray powder diffractometer is one of the primary analytical tools in materials science. It is applicable to nearly any crystalline material, and with advanced data analysis methods, it can provide a wealth of information concerning sample character. Data from these machines, however, are beset by a complex aberration function that can be addressed through calibration with the use of NIST Standard Reference Materials (SRMs). Laboratory diffractometers can be set up in a range of optical geometries; considered herein are those of Bragg-Brentano divergent beam configuration using both incident and diffracted beam monochromators. We review the origin of the various aberrations affecting instruments of this geometry and the methods developed at NIST to align these machines in a first principles context. Data analysis methods are considered as being in two distinct categories: those that use empirical methods to parameterize the nature of the data for subsequent analysis, and those that use model functions to link the observation directly to a specific aspect of the experiment. We consider a multifaceted approach to instrument calibration using both the empirical and model based data analysis methods. The particular benefits of the fundamental parameters approach are reviewed. PMID:26958446

  5. Mitigated phase transition during first cycle of a Li-rich layered cathode studied by in operando synchrotron X-ray powder diffraction.

    PubMed

    Song, Bohang; Day, Sarah J; Sui, Tan; Lu, Li; Tang, Chiu C; Korsunsky, Alexander M

    2016-02-14

    In operando synchrotron X-ray powder diffraction (SXPD) studies were conducted to investigate the phase transition of Li-rich Li(Li0.2Ni0.13Mn0.54Co0.13)O2 and Cr-doped Li(Li0.2Ni0.13Mn0.54Co0.03Cr0.10)O2 cathodes during the first charge/discharge cycle. Crystallographic (lattice parameters) and mechanical (domain size and microstrain) information was collected from SXPD full pattern refinement. It was found that Cr substitution at Co-site benefits in suppressing the activation of Li2MnO3 domains upon 1st charge, and thus mitigates the phase transition. As a consequence, Cr-doped layered cathode holds a better reversibility in terms of a full recovery of both lattice parameters and nano-domain size after a whole charge/discharge cycle. The effects of different cycling rates on the structural change were also discussed. PMID:26799191

  6. Static and Dynamical Structural Investigations of Metal-Oxide Nanocrystals by Powder X-ray Diffraction: Colloidal Tungsten Oxide as a Case Study.

    PubMed

    Caliandro, Rocco; Sibillano, Teresa; Belviso, B Danilo; Scarfiello, Riccardo; Hanson, Jonathan C; Dooryhee, Eric; Manca, Michele; Cozzoli, P Davide; Giannini, Cinzia

    2016-03-01

    We have developed a general X-ray powder diffraction (XPD) methodology for the simultaneous structural and compositional characterization of inorganic nanomaterials. The approach is validated on colloidal tungsten oxide nanocrystals (WO3-x NCs), as a model polymorphic nanoscale material system. Rod-shaped WO3-x NCs with different crystal structure and stoichiometry are comparatively investigated under an inert atmosphere and after prolonged air exposure. An initial structural model for the as-synthesized NCs is preliminarily identified by means of Rietveld analysis against several reference crystal phases, followed by atomic pair distribution function (PDF) refinement of the best-matching candidates (static analysis). Subtle stoichiometry deviations from the corresponding bulk standards are revealed. NCs exposed to air at room temperature are monitored by XPD measurements at scheduled time intervals. The static PDF analysis is complemented with an investigation into the evolution of the WO3-x NC structure, performed by applying the modulation enhanced diffraction technique to the whole time series of XPD profiles (dynamical analysis). Prolonged contact with ambient air is found to cause an appreciable increase in the static disorder of the O atoms in the WO3-x NC lattice, rather than a variation in stoichiometry. The time behavior of such structural change is identified on the basis of multivariate analysis. PMID:26756645

  7. Operando Synchrotron X-ray Powder Diffraction and Modulated-Excitation Infrared Spectroscopy Elucidate the CO2 Promotion on a Commercial Methanol Synthesis Catalyst.

    PubMed

    Martin, Oliver; Mondelli, Cecilia; Cervellino, Antonio; Ferri, Davide; Curulla-Ferré, Daniel; Pérez-Ramírez, Javier

    2016-09-01

    Optimal amounts of CO2 are added to syngas to boost the methanol synthesis rate on Cu-ZnO-Al2 O3 in the industrial process. The reason for CO2 promotion is not sufficiently understood at the particle level due to the catalyst complexity and the high demands of characterization under true reaction conditions. Herein, we applied operando synchrotron X-ray powder diffraction and modulated-excitation infrared spectroscopy on a commercial catalyst to gain insights into its morphology and surface chemistry. These studies unveiled that Cu and ZnO agglomerate and ZnO particles flatten under CO/H2 and/or CO2 /H2 . Under the optimal CO/CO2 /H2 mixture, sintering is prevented and ZnO crystals adopt an elongated shape due to the minimal presence of the H2 O byproduct, enhancing the water-gas shift activity and thus the methanol production. Our results provide a rationale to the CO2 promotion emphasizing the importance of advanced analytical methods to establish structure-performance relations in heterogeneous catalysis. PMID:27383374

  8. Crystal structure refinement of the semiconducting compound Cu{sub 2}SnSe{sub 3} from X-ray powder diffraction data

    SciTech Connect

    Delgado, G.E.; Mora, A.J.; Marcano, G.; Rincon, C

    2003-12-10

    The semiconducting compound Cu{sub 2}SnSe{sub 3} has been investigated by means of X-ray powder diffraction and its structure has been refined by the Rietveld method. The compound crystallizes in the monoclinic space group Cc (C{sub s}{sup 4}, No. 9), Z=4, with unit cell parameters a=6.9670(3) A, b=12.0493(7) A, c=6.9453(3) A, {beta}=109.19(1) deg. , and V=550.6(5) A{sup 3}. The refinement of 36 instrumental and structural parameters converged to R{sub p}=6.1%, R{sub wp}=8.6%, R{sub exp}=5.7%, R{sub B}=6.4%, S=1.5, for 4501 step intensities and 280 independent reflections. The structure of Cu{sub 2}SnSe{sub 3} can be described as an adamantane compound derivative of the sphalerite structure.

  9. Plumbonacrite identified by X-ray powder diffraction tomography as a missing link during degradation of red lead in a Van Gogh painting.

    PubMed

    Vanmeert, Frederik; Van der Snickt, Geert; Janssens, Koen

    2015-03-16

    Red lead, a semiconductor pigment used by artists since antiquity, is known to undergo several discoloration phenomena. These transformations are either described as darkening of the pigment caused by the formation of either plattnerite (β-PbO2) or galena (PbS) or as whitening by which red lead is converted into anglesite (PbSO4) or (hydro)cerussite (2 PbCO3⋅Pb(OH)2; PbCO3). X-ray powder diffraction tomography, a powerful analytical method that allows visualization of the internal distribution of different crystalline compounds in complex samples, was used to investigate a microscopic paint sample from a Van Gogh painting. A very rare lead mineral, plumbonacrite (3 PbCO3⋅Pb(OH)2⋅PbO), was revealed to be present. This is the first reported occurrence of this compound in a painting dating from before the mid 20th century. It constitutes the missing link between on the one hand the photoinduced reduction of red lead and on the other hand (hydro)cerussite, and thus sheds new light on the whitening of red lead. PMID:25703204

  10. Temperature Dependence of the Structural Parameters in the Transformation of Aragonite to Calcite, as Determined from In Situ Synchrotron Powder X-ray-Diffratction Data

    SciTech Connect

    Antao, Sytle M.; Hassan, Ishmael

    2011-09-06

    The temperature dependency of the crystal structure and the polymorphic transition of CaCO{sub 3} from aragonite to calcite were studied using Rietveld structure refinement and high-temperature in situ synchrotron powder X-ray-diffraction data at ambient pressure, P. The orthorhombic metastable aragonite at room P, space group Pmcn, transforms to trigonal calcite, space group R{bar 3}c, at about T{sub c} = 468 C. This transformation occurs rapidly; it starts at about 420 C and is completed by 500 C, an 80 C interval that took about 10 minutes using a heating rate of 8 C/min. Structurally, from aragonite to calcite, the distribution of the Ca atom changes from approximately hexagonal to cubic close-packing. A 5.76% discontinuous increase in volume accompanies the reconstructive first-order transition. Besides the change in coordination of the Ca atom from nine to six from aragonite to calcite, the CO{sub 3} groups change by a 30{sup o} rotation across the transition.

  11. Early age hydration and pozzolanic reaction in natural zeolite blended cements: Reaction kinetics and products by in situ synchrotron X-ray powder diffraction

    SciTech Connect

    Snellings, R.; Mertens, G.; Cizer, O.; Elsen, J.

    2010-12-15

    The in situ early-age hydration and pozzolanic reaction in cements blended with natural zeolites were investigated by time-resolved synchrotron X-ray powder diffraction with Rietveld quantitative phase analysis. Chabazite and Na-, K-, and Ca-exchanged clinoptilolite materials were mixed with Portland cement in a 3:7 weight ratio and hydrated in situ at 40 {sup o}C. The evolution of phase contents showed that the addition of natural zeolites accelerates the onset of C{sub 3}S hydration and precipitation of CH and AFt. Kinetic analysis of the consumption of C{sub 3}S indicates that the enveloping C-S-H layer is thinner and/or less dense in the presence of alkali-exchanged clinoptilolite pozzolans. The zeolite pozzolanic activity is interpreted to depend on the zeolite exchangeable cation content and on the crystallinity. The addition of natural zeolites alters the structural evolution of the C-S-H product. Longer silicate chains and a lower C/S ratio are deduced from the evolution of the C-S-H b-cell parameter.

  12. Obtaining aluminas from the thermal decomposition of their different precursors: An {sup 27}Al MAS NMR and X-ray powder diffraction studies

    SciTech Connect

    Chagas, L.H.; De Carvalho, G.S.G.; San Gil, R.A.S.; Chiaro, S.S.X.; Leitão, A.A.; Diniz, R.

    2014-01-01

    Graphical abstract: - Highlights: • We synthesized three precursors of alumina from different methods. • The calcination of the precursors generated several alumina polymorphs. • XRD and NMR were used for structural investigation of the polymorphs. • The synthesis route determines the structural and textural properties of the solids. - Abstract: A commercial sample of Boehmite was used as precursor of alumina polymorphs. For comparison, three other precursors were synthesized from different methods. Particularly, the use of excess of urea promoted a very crystalline form of basic aluminum carbonate. The characteristics of the four precursors were investigated by thermal, vibrational and X-ray powder diffraction (XRD) analysis. Additionally, the nuclear magnetic resonance, with magic angle spinning ({sup 27}Al MAS NMR), was used to verify the coordination of aluminum cations. Each precursor was calcined at various temperatures generating alumina polymorphs, which were structurally analyzed by XRD and {sup 27}Al MAS NMR. Due to interest in catalysis supports, special attention was given to the γ-Al{sub 2}O{sub 3} phase, which in addition to structural investigation was subjected to textural analysis. The results showed that, from different synthesis procedures and common route of calcination, one can obtain materials with the same composition but with different structural and textural properties, which in turn can significantly influence the performance of a supported catalyst.

  13. Powder X-Ray Reference Patterns of Sr2RGaCu2Oy (R = Pr, Nd, Sm, Eu, Gd, Dy, Ho, Er, Tm, and Y)

    PubMed Central

    Wong-Ng, W.; Kaduk, J. A.; Levin, I.; Greenwood, W.; Dillingham, J.

    2001-01-01

    X-Ray Rietveld refinements were conducted on a series of eleven lanthanide phases, Sr2RGaCu2Oy (2112 phase, R = Pr, Nd, Sm, Eu, Gd, Dy, Ho, Y, Er, Tm, and Yb) that are structurally related to the high Tc superconductor Ba2YCu3O7 (213). In the 2112 structure, instead of square planar Cu-O chains, tetrahedral GaO4 chains were found to run in a zig-zag fashion along the diagonal of the basal 213 ab-direction. Reference powder patterns for these compounds were prepared by using the Rietveld decomposition technique. The unit cell volume of these compounds follows the expected trend of the lanthanide contraction. The lattice parameters range from a = 22.9694(3) Å, b = 5.5587(2) Å, and c = 5.44743(7) Å for R = Pr, to a = 22.8059(2) Å, b = 5.46031(5) Å, and c = 5.37773(5) Å for R = Yb. An electon diffraction study of the Sm- and Er-analogs showed characteristic diffuse streaks along the b-axis, suggesting some disorder within the GaO4 chains.

  14. Formation of γ-Fe 2O 3 nanoparticles and vacancy ordering: An in situ X-ray powder diffraction study

    NASA Astrophysics Data System (ADS)

    Jørgensen, Jens-Erik; Mosegaard, Lene; Thomsen, Line E.; Jensen, Torben R.; Hanson, Jonathan C.

    2007-01-01

    The formation of maghemite, γ-Fe 2O 3 nanoparticles has been studied by in situ X-ray powder diffraction. The maghemite was formed by thermal decomposition of an amorphous precursor compound made by reacting lauric acid, CH 3(CH 2) 10COOH with Fe(NO 3) 3·9H 2O. It has been shown that cubic γ-Fe 2O 3 was formed directly from the amorphous precursor and that vacancy ordering starts about 45 min later at 305 °C resulting in a tripled unit cell along the c-axis. The kinetics of grain growth was found to obey a power law with growth exponents n equal to 0.136(6) and 0.103(5) at 305 and 340 °C, respectively. Particles with average sizes of 12 and 13 nm were obtained in 86 and 76 min at 305 and 340 °C, respectively. The structure of cubic and vacancy ordered phases of γ-Fe 2O 3 was studied at 305 °C by Rietveld refinements.

  15. Synchrotron X-ray powder diffraction and convergent beam electron diffraction studies on the cubic phase of MgV{sub 2}O{sub 4} spinel

    SciTech Connect

    Niitaka, Seiji; Lee, Soyeon; Oshima, Yoshifumi; Kato, Kenichi; Hashizume, Daisuke; Takata, Masaki; Takagi, Hidenori

    2014-07-01

    The A V{sub 2}O{sub 4} (A=Mg{sup 2+}, Zn{sup 2+}, Cd{sup 2+}) spinels are three-dimensional spin-1 frustrated systems with orbital degree of freedom, which have been known to possess intriguing orbital states causing releases of spin frustration at low temperatures. We have performed synchrotron X-ray and convergent beam electron diffraction measurements for one of these vanadates, MgV{sub 2}O{sub 4} in order to clarify its crystal structure in the high temperature cubic phase, which is regarded as an important starting point for understanding the details of the low temperature phase. We have successfully observed that the [001] zone axis convergent beam electron diffraction pattern exhibits 4mm symmetry, suggesting the space group of Fd3{sup ¯}m in the cubic MgV{sub 2}O{sub 4}. It has also been demonstrated that the crystal structure of the cubic MgV{sub 2}O{sub 4} contains VO{sub 6} octahedra elongated along the threefold rotation axis. Based on our results, we discuss the orbital states of MgV{sub 2}O{sub 4} as well as the other spinel vanadates. - Graphical abstract: Precise geometry of the VO{sub 6} octahedra in the cubic phase of MgV{sub 2}O{sub 4} spinel determined with the synchrotron powder XRD data. - Highlights: • We examined the crystal structure of the cubic phase of MgV{sub 2}O{sub 4} spinel. • We prepared the single crystal and powdered sample of MgV{sub 2}O{sub 4} with high quality. • The result of the CBED measurement agrees with the space group of Fd3{sup ¯}m in the phase. • The cubic phase has VO{sub 6} octahedra elongated along the threefold rotation axis.

  16. Maximum Entropy Method and Charge Flipping, a Powerful Combination to Visualize the True Nature of Structural Disorder from in situ X-ray Powder Diffraction Data

    SciTech Connect

    Samy, A.; Dinnebier, R; van Smaalen, S; Jansen, M

    2010-01-01

    In a systematic approach, the ability of the Maximum Entropy Method (MEM) to reconstruct the most probable electron density of highly disordered crystal structures from X-ray powder diffraction data was evaluated. As a case study, the ambient temperature crystal structures of disordered {alpha}-Rb{sub 2}[C{sub 2}O{sub 4}] and {alpha}-Rb{sub 2}[CO{sub 3}] and ordered {delta}-K{sub 2}[C{sub 2}O{sub 4}] were investigated in detail with the aim of revealing the 'true' nature of the apparent disorder. Different combinations of F (based on phased structure factors) and G constraints (based on structure-factor amplitudes) from different sources were applied in MEM calculations. In particular, a new combination of the MEM with the recently developed charge-flipping algorithm with histogram matching for powder diffraction data (pCF) was successfully introduced to avoid the inevitable bias of the phases of the structure-factor amplitudes by the Rietveld model. Completely ab initio electron-density distributions have been obtained with the MEM applied to a combination of structure-factor amplitudes from Le Bail fits with phases derived from pCF. All features of the crystal structures, in particular the disorder of the oxalate and carbonate anions, and the displacements of the cations, are clearly obtained. This approach bears the potential of a fast method of electron-density determination, even for highly disordered materials. All the MEM maps obtained in this work were compared with the MEM map derived from the best Rietveld refined model. In general, the phased observed structure factors obtained from Rietveld refinement (applying F and G constraints) were found to give the closest description of the experimental data and thus lead to the most accurate image of the actual disorder.

  17. [Study on high pressure sample preparation method for pressed powder pellet and its application in X-ray fluorescence spectrum analysis].

    PubMed

    Zhang, Qin; Yu, Zhao-Shui; Li, Xiao-Li; Li, Guo-hui

    2013-12-01

    Using the independently designed high pressure sample preparation mold and high pressure sample preparation technology (patent number: 201310125772. 5), studies on the high pressure pressed various geological samples such as rocks, soils and stream sediments were first described in the present paper. It is the first experiment conducted in this field with significant achievements obtained. Without any binder, various types of geological powder samples can be pelleted well using 1600KN high pressure method. Such pellet has the characteristics of dense, flat, smooth and shiny surface, no cracks, no delamination, and no powder dropping. The study provides a new and contamination-free approach to sample preparation of X-ray fluorescence spectrum analysis. The comparison study conducted between the same samples pelleted under the low pressure (400 kN) and high pressure (1 600 kN) showed that using the high pressure the element peak to background ratios, and sensitivities are significantly improved, the detection limits are lowed, and the accuracies, the precisions and sample preparation repeatability are greatly improved. The Si FWHM became wider for the high pressure (1 600 kN) pellet than the same sample pelleted under the lower pressure (400 kN). The further SEM observation revealed that variation of Si spectrum shape may be caused by that the silica crystal lattices are destroyed and the particle size becomes smaller by using the high pressure pelleting techniques. So the particle size and mineral effects are also effectively reduced and the precisions and accuracies of the analytical method are improved. PMID:24611411

  18. Water adsorption, solvation and deliquescence of alkali halide thin films on SiO2 studied by ambient pressure X-ray photoelectron spectroscopy

    SciTech Connect

    Arima, Kenta; Jiang, Peng; Deng, Xingyi; Bluhm, Henrik; Salmeron, Miquel

    2010-03-31

    The adsorption of water on KBr thin films evaporated onto SiO2 was investigated as a function of relative humidity (RH) by ambient pressure X-ray photoelectron spectroscopy. At 30percent RH adsorbed water reaches a coverage of approximately one monolayer. As the humidity continues to increase, the coverage of water remains constant or increases very slowly until 60percent RH, followed by a rapid increase up to 100percent RH. At low RH a significant number of the Br atoms are lost due to irradiation damage. With increasing humidity solvation increases ion mobility and gives rise to a partial recovery of the Br/K ratio. Above 60percent RH the increase of the Br/K ratio accelerates. Above the deliquescence point (85percent RH), the thickness of the water layer continues to increase and reaches more than three layers near saturation. The enhancement of the Br/K ratio at this stage is roughly a factor 2.3 on a 0.5 nm KBr film, indicating a strong preferential segregation of Br ions to the surface of the thin saline solution on SiO2.

  19. Chest x-ray

    MedlinePlus

    Chest radiography; Serial chest x-ray; X-ray - chest ... You stand in front of the x-ray machine. You will be told to hold your breath when the x-ray is taken. Two images are usually taken. You will ...

  20. Powder-based adsorbents having high adsorption capacities for recovering dissolved metals and methods thereof

    DOEpatents

    Janke, Christopher J.; Dai, Sheng; Oyola, Yatsandra

    2016-05-03

    A powder-based adsorbent and a related method of manufacture are provided. The powder-based adsorbent includes polymer powder with grafted side chains and an increased surface area per unit weight to increase the adsorption of dissolved metals, for example uranium, from aqueous solutions. A method for forming the powder-based adsorbent includes irradiating polymer powder, grafting with polymerizable reactive monomers, reacting with hydroxylamine, and conditioning with an alkaline solution. Powder-based adsorbents formed according to the present method demonstrated a significantly improved uranium adsorption capacity per unit weight over existing adsorbents.

  1. CTAB-assisted synthesis of mesoporous F-N-codoped TiO{sub 2} powders with high visible-light-driven catalytic activity and adsorption capacity

    SciTech Connect

    Xie Yi Zhao Xiujian Li Yuanzhi; Zhao Qingnan; Zhou Xuedong; Yuan Qihua

    2008-08-15

    This article describes the preparation of mesoporous rod-like F-N-codoped TiO{sub 2} powder photocatalysts with anatase phase via a sol-gel route at the temperature of 373 K, using cetyltrimethyl ammonium bromide (CTAB) as surfactant. The as-prepared photocatalysts were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and UV-visible diffuse reflectance spectra (UV-vis DRS). The results showed that the photocatalysts possessed a homogeneous pore diameter and a high surface area of 106.3-160.7 m{sup 3} g{sup -1}. The increasing CTAB reactive concentration extended the visible-light absorption up to 600 nm. The F-N-codoped TiO{sub 2} powders exhibited significant higher adsorption capacity for methyl orange (MO) than that of Degussa P25 and showed more than 6 times higher visible-light-induced catalytic degradation for MO than that of P25. - Graphical abstract: The introduction of surfactant CTAB not only extended the visible light absorption of mesoporous F-N-codoped TiO{sub 2} up to 600 nm but also significantly enhanced the adsorption capacity and visible-light-induced degradation for methyl orange. Mesoporous rod-like F-N-codoped TiO{sub 2} powder photocatalysts were synthesized via a sol-gel route at low temperature of 373 K.

  2. Pulsed supercritical synthesis of anatase TiO2 nanoparticles in a water-isopropanol mixture studied by in situ powder X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Eltzholtz, Jakob Rostgaard; Tyrsted, Christoffer; Jensen, Kirsten Marie Ørnsbjerg; Bremholm, Martin; Christensen, Mogens; Becker-Christensen, Jacob; Iversen, Bo Brummerstedt

    2013-02-01

    A new step in supercritical nanoparticle synthesis, the pulsed supercritical synthesis reactor, is investigated in situ using synchrotron powder X-ray diffraction (PXRD) to understand the formation of nanoparticles in real time. This eliminates the common problem of transferring information gained during in situ studies to subsequent laboratory reactor conditions. As a proof of principle, anatase titania nanoparticles were synthesized in a 50/50 mixture of water and isopropanol near and above the critical point of water (P = 250 bar, T = 300, 350, 400, 450, 500 and 550 °C). The evolution of the reaction product was followed by sequentially recording PXRD patterns with a time resolution of less than two seconds. The crystallite size of titania is found to depend on both temperature and residence time, and increasing either parameter leads to larger crystallites. A simple adjustment of either temperature or residence time provides a direct method for gram scale production of anatase nanoparticles of average crystallite sizes between 7 and 35 nm, thus giving the option of synthesizing tailor-made nanoparticles. Modeling of the in situ growth curves using an Avrami growth model gave an activation energy of 66(19) kJ mol-1 for the initial crystallization. The in situ PXRD data also provide direct information about the size dependent macrostrain in the nanoparticles and with decreasing crystallite size the unit cell contracts, especially along the c-direction. This agrees well with previous ex situ results obtained for hydrothermal synthesis of titania nanoparticles.A new step in supercritical nanoparticle synthesis, the pulsed supercritical synthesis reactor, is investigated in situ using synchrotron powder X-ray diffraction (PXRD) to understand the formation of nanoparticles in real time. This eliminates the common problem of transferring information gained during in situ studies to subsequent laboratory reactor conditions. As a proof of principle, anatase titania

  3. In situ high-pressure synchrotron X-ray powder diffraction study of tunnel manganese oxide minerals: hollandite, romanechite, and todorokite

    NASA Astrophysics Data System (ADS)

    Hwang, Gil Chan; Post, Jeffrey E.; Lee, Yongjae

    2015-05-01

    In situ high-pressure synchrotron X-ray powder diffraction study of three tunnel manganese oxide minerals (hollandite with 2 × 2 MnO6 octahedra tunnels, romanechite with 2 × 3 tunnels, and todorokite with 3 × 3 tunnels) was performed using a diamond anvil cell and nominally penetrating alcohol and water mixture as a pressure-transmitting medium up to ~8 GPa. Bulk moduli ( B 0) calculated using Murnaghan's equation of state are inversely proportional to the size of the tunnel, i.e., 134(4) GPa for hollandite ( I2/m), 108(2) GPa for romanechite ( C2/m), and 67(5) GPa for todorokite ( P2/m). On the other hand, axial compressibilities show different elastic anisotropies depending on the size of the tunnel, i.e., ( a/ a 0) = -0.00066(3) GPa-1, ( b/ b 0) = 0.00179(8) GPa-1, ( c/ c 0) = 0.00637(4) GPa-1 [ c > b > a] for hollandite; ( a/ a 0) = 0.00485(4) GPa-1, ( b/ b 0) = 0.0016(1) GPa-1, ( c/ c 0) = 0.00199(8) GPa-1 [ a > c > b] for romanechite; and ( a/ a 0) = 0.00826(9) GPa-1, ( b/ b 0) = 0.0054(1) GPa-1, ( c/ c 0) = 0.00081(8) GPa-1 [ a > b > c] for todorokite. Overall, the degree of tunnel distortion increases with increasing pressure and correlates with the size of the tunnel, which is evidenced by the gradual increases in the monoclinic β angles up to 3 GPa of 0.62°, 0.8°, and 1.15° in hollandite, romanechite, and todorokite, respectively. The compression of tunnel manganese oxides is related to the tunnel distortion and the size of the tunnel.

  4. Crystal-structure analysis of four mineral samples of anhydrite, CaSO[subscript 4], using synchrotron high-resolution powder X-ray diffraction data

    SciTech Connect

    Antao, Sytle M.

    2014-05-28

    The crystal structures of four samples of anhydrite, CaSO{sub 4}, were obtained by Rietveld refinements using synchrotron high-resolution powder X-ray diffraction (HRPXRD) data and space group Amma. As an example, for one sample of anhydrite from Hants County, Nova Scotia, the unit-cell parameters are a = 7.00032(2), b = 6.99234(1), c = 6.24097(1) {angstrom}, and V = 305.487(1) {angstrom}{sup 3} with a > b. The eight-coordinated Ca atom has an average distance of 2.4667(4) {angstrom}. The tetrahedral SO{sub 4} group has two independent S-O distances of 1.484(1) to O1 and 1.478(1) {angstrom} to O2 and an average distance of 1.4810(5) {angstrom}. The three independent O-S-O angles [108.99(8) x 1, 110.38(3) x 4, 106.34(9){sup o} x 1; average [6] = 109.47(2){sup o}] and S-O distances indicate that the geometry of the SO{sub 4} group is quite distorted in anhydrite. The four anhydrite samples have structural trends where the a, b, and c unit-cell parameters increase linearly with increasing unit-cell volume, V, and their average and distances are nearly constant. The grand mean = 2.4660(2) {angstrom}, and grand mean = 1.4848(3) {angstrom}, the latter is longer than 1.480(1) {angstrom} in celestite, SrSO{sub 4}, as expected.

  5. Hidden Superlattice in Tl2(SC6H4S) and Tl2(SeC6H4Se) Solved from Powder X-ray Diffraction

    SciTech Connect

    K Stone; D Turner; M Singh; T Vaid; P Stephens

    2011-12-31

    The crystal structures of the isostructural title compounds poly[({mu}-benzene-1,4-dithiolato)dithallium], Tl{sub 2}(SC{sub 6}H{sub 4}S), and poly[({mu}-benzene-1,4-diselenolato)dithallium], Tl{sub 2}(SeC{sub 6}H{sub 4}Se), were solved by simulated annealing from high-resolution synchrotron X-ray powder diffraction. Rietveld refinements of an initial structure with one formula unit per triclinic cell gave satisfactory agreement with the data, but led to a structure with impossibly close non-bonded contacts. A disordered model was proposed to alleviate this problem, but an alternative supercell structure leads to slightly improved agreement with the data. The isostructural superlattice structures were confirmed for both compounds through additional data collection, with substantially better counting statistics, which revealed the presence of very weak superlattice peaks not previously seen. Overall, each structure contains Tl-S or Tl-Se two-dimensional networks, connected by phenylene bridges. The sulfur (or selenium) coordination sphere around each thallium is a highly distorted square pyramid or a 'see-saw' shape, depending upon how many Tl-S or Tl-Se interactions are considered to be bonds. In addition, the two compounds contain pairs of Tl{sup I} ions that interact through a closed-shell 'thallophilic' interaction: in the sulfur compound there are two inequivalent pairs of Tl atoms with Tl-Tl distances of 3.49 and 3.58 {angstrom}, while in the selenium compound those Tl-Tl interactions are at 3.54 and 3.63 {angstrom}.

  6. Neutron and X-ray powder diffraction study of RBa{sub 2}Fe{sub 3}O{sub 8+w} phases

    SciTech Connect

    Karen, P.; Kjekshus, A.; Huang, Q.; Lynn, J.W.; Rosov, N.; Sora, I.N.; Karen, V.L.; Mighell, A.D.; Santoro, A.

    1998-02-15

    Compounds of composition RBa{sub 2}Fe{sub 3}O{sub 8+w} (R = La, Nd, Sm, Gd, Dy, Er, Yb, Lu, and Y) with variable oxygen content have been synthesized using the liquid mixing technique and have been analyzed by powder X-ray and neutron diffraction methods. A triple perovskite-type structure with ordered Ba and R cations and having the symmetry of space group P4/mmm was obtained only for R = Y, Dy, and Er, whereas the larger R atoms gave the atomic arrangement of disordered, defective perovskites with average symmetry Pm{bar 3}m. No perovskite-type phases were obtained when Yb and Lu were tried. The oxygen content of the oxygen-saturated phases was found to increase with increasing size of the cation R from w = 0.07 for Er to w = 0.83 for La. The Neel temperature ({approximately}650 K) and the magnitude of the Fe magnetic moment ({approximately}3.3 {mu}{sub B} at room temperature) are highest when trivalent iron is involved (w = 0), but these quantities are rather insensitive to the nature of R and to slight variations of oxygen content in the triple perovskite-type structure of the Y, Dy, and Er compounds. In the case of the cubic structures, however, both quantities depend strongly on the oxygen stoichiometry. In the magnetically ordered state, nearest-neighbor iron moments are coupled antiferromagnetically along the three crystallographic directions in all samples, resulting in magnetic structures with symmetry Imm{prime}m and magnetic unit cells related to those of the corresponding nuclear structures by the transformation matrix (1{bar 1}0/110/002).

  7. Optical absorption characteristics in the assessment of powder phosphor-based x-ray detectors: from nano- to micro-scale.

    PubMed

    Liaparinos, P F

    2015-11-21

    X-ray phosphor-based detectors have enormously improved the quality of medical imaging examinations through the optimization of optical diffusion. In recent years, with the development of science and technology in the field of materials, improved powder phosphors require structural and optical properties that contribute to better optical signal propagation. The purpose of this paper was to provide a quantitative and qualitative understanding of the optical absorption characteristics in the assessment of powder phosphor-based detectors (from nano- scale up to micro-scale). Variations on the optical absorption parameters (i.e. the light extinction coefficient [Formula: see text] and the percentage probability of light absorption p%) were evaluated based on Mie calculations examining a wide range of light wavelengths, particle refractive indices and sizes. To model and assess the effects of the aforementioned parameters on optical diffusion, Monte Carlo simulation techniques were employed considering: (i) phosphors of different layer thickness, 100 μm (thin layer) and 300 μm (thick layer), respectively, (ii) light extinction coefficient values, 1, 3 and 6 μm(-1), and (iii) percentage probability of light absorption p% in the range 10(-4)-10(-2). Results showed that the [Formula: see text] coefficient is high for phosphor grains in the submicron scale and for low light wavelengths. At higher wavelengths (above 650 nm), optical quanta follow approximately similar depths until interaction for grain diameter 500 nm and 1 μm. Regarding the variability of the refractive index, high variations of the [Formula: see text] coefficient occurred above 1.6. Furthermore, results derived from Monte Carlo modeling showed that high spatial resolution phosphors can be accomplished by increasing the [Formula: see text] parameter. More specifically, the FWHM was found to decrease (i.e. higher resolution): (i) 4.8% at 100 μm and (ii) 9.5%, at 300 μm layer thickness. This study

  8. Optical absorption characteristics in the assessment of powder phosphor-based x-ray detectors: from nano- to micro-scale

    NASA Astrophysics Data System (ADS)

    Liaparinos, P. F.

    2015-11-01

    X-ray phosphor-based detectors have enormously improved the quality of medical imaging examinations through the optimization of optical diffusion. In recent years, with the development of science and technology in the field of materials, improved powder phosphors require structural and optical properties that contribute to better optical signal propagation. The purpose of this paper was to provide a quantitative and qualitative understanding of the optical absorption characteristics in the assessment of powder phosphor-based detectors (from nano- scale up to micro-scale). Variations on the optical absorption parameters (i.e. the light extinction coefficient {{m}\\text{ext}} and the percentage probability of light absorption p%) were evaluated based on Mie calculations examining a wide range of light wavelengths, particle refractive indices and sizes. To model and assess the effects of the aforementioned parameters on optical diffusion, Monte Carlo simulation techniques were employed considering: (i) phosphors of different layer thickness, 100 μm (thin layer) and 300 μm (thick layer), respectively, (ii) light extinction coefficient values, 1, 3 and 6 μm-1, and (iii) percentage probability of light absorption p% in the range 10-4-10-2. Results showed that the {{m}\\text{ext}} coefficient is high for phosphor grains in the submicron scale and for low light wavelengths. At higher wavelengths (above 650 nm), optical quanta follow approximately similar depths until interaction for grain diameter 500 nm and 1 μm. Regarding the variability of the refractive index, high variations of the {{m}\\text{ext}} coefficient occurred above 1.6. Furthermore, results derived from Monte Carlo modeling showed that high spatial resolution phosphors can be accomplished by increasing the {{m}\\text{ext}} parameter. More specifically, the FWHM was found to decrease (i.e. higher resolution): (i) 4.8% at 100 μm and (ii) 9.5%, at 300 μm layer thickness. This study attempted to

  9. NH{sub 3} adsorption and decomposition on Ir(110): A combined temperature programmed desorption and high resolution fast x-ray photoelectron spectroscopy study

    SciTech Connect

    Weststrate, C.J.; Bakker, J.W.; Rienks, E.D.L.; Lizzit, S.; Petaccia, L.; Baraldi, A.; Vinod, C.P.; Nieuwenhuys, B.E.

    2005-05-08

    The adsorption and decomposition of NH{sub 3} on Ir(110) has been studied in the temperature range from 80 K to 700 K. By using high-energy resolution x-ray photoelectron spectroscopy it is possible to distinguish chemically different surface species. At low temperature a NH{sub 3} multilayer, which desorbs at {approx}110 K, was observed. The second layer of NH{sub 3} molecules desorbs around 140 K, in a separate desorption peak. Chemisorbed NH{sub 3} desorbs in steps from the surface and several desorption peaks are observed between 200 and 400 K. A part of the NH{sub 3ad} decomposes into NH{sub ad} between 225 and 300 K. NH{sub ad} decomposes into N{sub ad} between 400 K and 500 K and the hydrogen released in this process immediately desorbs. N{sub 2} desorption takes place between 500 and 700 K via N{sub ad} combination. The steady state decomposition reaction of NH{sub 3} starts at 500 K. The maximum reaction rate is observed between 540 K and 610 K. A model is presented to explain the occurrence of a maximum in the reaction rate. Hydrogenation of N{sub ad} below 400 K results in NH{sub ad}. No NH{sub 2ad} or NH{sub 3ad}/NH{sub 3} were observed. The hydrogenation of NH{sub ad} only takes place above 400 K. On the basis of the experimental findings an energy scheme is presented to account for the observations.

  10. The Long-Term Fate of Cu2+, Zn2+, and Pb2+ Adsorption Complexes at the Calcite Surface: An X-ray Absorption Spectroscopy Study

    SciTech Connect

    Elzinga,E.; Rouff, A.; Reeder, R.

    2006-01-01

    In this study, the speciation of Zn{sup 2+}, Pb{sup 2+}, and Cu{sup 2+} ions sorbed at the calcite surface was monitored during a 2.5-year reaction period, using extended X-ray absorption spectroscopy to characterize metal speciation on the molecular scale. Experiments were performed using pre-equilibrated calcite-water suspensions of pH 8.3, at metal concentrations below the solubility of metal hydroxide and carbonate precipitates, and at constant metal surface loadings. The EXAFS results indicate that all three metals remained coordinated at the calcite surface as inner-sphere adsorption complexes during the 2.5-year ageing period, with no evidence to suggest slow formation of dilute metal-calcite solid solutions under the reaction conditions employed. All three divalent metals were found to form non-octahedral complexes upon coordination to the calcite surface, with Zn{sup 2+} adsorbing as a tetrahedral complex, Cu{sup 2+} as a Jahn-Teller distorted octahedral complex, and Pb{sup 2+} coordinating as a trigonal- or square-pyramidal surface complex. The non-octahedral configurations of these surface complexes may have hindered metal transfer from the calcite surface into the bulk, where Ca{sup 2+} is in octahedral coordination with respect to first-shell O. The use of pre-equilibrated calcite suspensions, with no net calcite dissolution or precipitation, likely prevented metal incorporation into the lattice as a result of surface recrystallization. The results from this study imply that ageing alone does not increase the stability of Zn{sup 2+}, Pb{sup 2+}, and Cu{sup 2+} partitioning to calcite if equilibrium with the solution is maintained during reaction; under these conditions, these metals are likely to remain available for exchange even after extended sorption times.

  11. Effect of the preparation conditions of Al-3%Y powder on its structural and adsorption properties

    NASA Astrophysics Data System (ADS)

    Ryabina, A. V.; Shevchenko, V. G.

    2016-01-01

    In view of the great practical utility of aluminum-rare earth metal (REM) powders as adsorbents and catalyst supports, the dispersion composition and morphology of Al-3%Y alloy powder particles obtained by various methods (gas plasma recondensation, nitrogen sputtering) were studied by low-temperature nitrogen adsorption, scanning electron microscopy, XRD, etc. The phase composition of the powders was determined, and the amount of active aluminum was calculated. The nitrogen adsorption on the powder surface was studied experimentally at-196°C at relative pressures of P/Ps = 10-3-0.999. The specific surface areas of the powders were determined.

  12. Dental x-rays

    MedlinePlus

    X-ray - teeth; Radiograph - dental; Bitewings; Periapical film; Panoramic film ... dentist's office. There are many types of dental x-rays. Some are: Bitewing Periapical Palatal (also called occlusal) ...

  13. X-ray (image)

    MedlinePlus

    X-rays are a form of ionizing radiation that can penetrate the body to form an image on ... will be shades of gray depending on density. X-rays can provide information about obstructions, tumors, and other ...

  14. X-Ray Lasers

    ERIC Educational Resources Information Center

    Chapline, George; Wood, Lowell

    1975-01-01

    Outlines the prospects of generating coherent x rays using high-power lasers and indentifies problem areas in their development. Indicates possible applications for coherent x rays in the fields of chemistry, biology, and crystallography. (GS)

  15. X Ray Topography

    ERIC Educational Resources Information Center

    Balchin, A. A.

    1974-01-01

    Discusses some aspects in X-ray topography, including formation of dislocations, characteristics of stacking faults, x-ray contrast in defect inspection, Berg-Barrett technique, and Lang traversing crystal and Borrmann's methods. (CC)

  16. Extremity x-ray

    MedlinePlus

    ... degenerative) Bone tumor Broken bone (fracture) Dislocated bone Osteomyelitis (infection) Other conditions for which the test may ... Bone tumor Bone x-ray Broken bone Clubfoot Osteomyelitis X-ray Update Date 10/22/2014 Updated ...

  17. X-Ray Imaging

    MedlinePlus

    ... Brain Surgery Imaging Clinical Trials Basics Patient Information X-Ray Imaging Print This Page X-ray imaging is perhaps the most familiar type of imaging. Images produced by X-rays are due to the different absorption rates of ...

  18. X-Rays

    MedlinePlus

    X-rays are a type of radiation called electromagnetic waves. X-ray imaging creates pictures of the inside of your ... different amounts of radiation. Calcium in bones absorbs x-rays the most, so bones look white. Fat and ...

  19. Hand x-ray

    MedlinePlus

    X-ray - hand ... A hand x-ray is taken in a hospital radiology department or your health care provider's office by an ... technician. You will be asked to place your hand on the x-ray table, and keep it ...

  20. Sinus x-ray

    MedlinePlus

    Paranasal sinus radiography; X-ray - sinuses ... sinus x-ray is taken in a hospital radiology department. Or the x-ray may be taken ... Brown J, Rout J. ENT, neck, and dental radiology. In: Adam A, Dixon AK, Gillard JH Schaefer- ...

  1. Nepheline: Structure of Three Samples from the Bancroft Area, Ontario, Obtained using Synchrotron High-Resolution Powder X-Ray Diffraction

    SciTech Connect

    Antao, Sytle M.; Hassan, Ishmael

    2010-05-25

    The crystal structure of three samples of nepheline (ideally, K{sub 2}Na{sub 6}[Al{sub 8}Si{sub 8}O{sub 32}]) from the Bancroft area of Ontario (1a, b: Egan Chute, 2: Nephton, and 3: Davis Hill), each with different types of superstructure reflections, has been studied using synchrotron high-resolution powder X-ray diffraction (HRPXRD) data and Rietveld structure refinement. The samples have different origins. The structure was refined in space group P6{sub 3}. The R{sub F}{sup 2} index, number of unique observed reflections, pseudohexagonal subcell parameters, and site-occupancy factor (sof) for the K site are as follows: Sample 1b: R{sub F}{sup 2} = 0.0433, N{sub obs} = 1399, a = 9.99567(1), c = 8.37777(1) {angstrom}, V = 724.907(2) {angstrom}{sub 3}, and K (sof) = 0.716(1). Sample 2: R{sub F}{sup 2} = 0.0669, N{sub obs} = 1589, a = 10.00215(1), c = 8.38742(1) {angstrom}, V = 726.684(1) {angstrom}{sub 3}, and K (sof) = 0.920(1). Sample 3: R{sub F}{sup 2} = 0.0804, N{sub obs} = 1615, a = 9.99567(1), c = 8.37873(1) {angstrom}, V = 724.991(1) {angstrom}{sub 3}, and K (sof) = 0.778(2). Sample 2 has the largest sof for K and the largest volume. The satellite reflections in the three nepheline samples were observed in the HRPXRD traces and give rise to different incommensurate superstructures. The Al and Si atoms in the T{sub 3} and T{sub 4} sites are ordered differently in the three samples, which may indicate the presence of a domain structure based on Al-Si order. The positions for the Al and Si atoms were interchanged in two samples because of the resulting distances. The slight excess of Si over Al atoms, characteristically encountered in well-analyzed samples of nepheline, is reflected in the distances.

  2. Adsorption of myoglobin to Cu(II)-IDA and Ni(II)-IDA functionalized langmuir monolayers : study of the protein layer structure during the adsorption process by neutron and X-ray reflectivity.

    SciTech Connect

    Seo, Young-Soo; Satija, Sushil K.; Majewski, Jaroslaw; Sasaki, Darryl Yoshio; Kent, Michael Stuart; Yim, Hyun

    2005-05-01

    The structure and orientation of adsorbed myoglobin as directed by metal-histidine complexation at the liquid-film interface was studied as a function of time using neutron and X-ray reflectivity (NR and XR, respectively). In this system, adsorption is due to the interaction between iminodiacetate (IDA)-chelated divalent metal ions Ni(II) and Cu(II) and histidine moieties at the outer surface of the protein. Adsorption was examined under conditions of constant area per lipid molecule at an initial pressure of 40 mN/m. Adsorption occurred over a time period of about 15 h, allowing detailed characterization of the layer structure throughout the process. The layer thickness and the in-plane averaged segment volume fraction were obtained at roughly 40 min intervals by NR. The binding constant of histidine with Cu(II)-IDA is known to be about four times greater than that of histidine with Ni(II)-IDA. The difference in interaction energy led to significant differences in the structure of the adsorbed layer. For Cu(II)-IDA, the thickness of the adsorbed layer at low protein coverage was {le} 20 {angstrom} and the thickness increased almost linearly with increasing coverage to 42 {angstrom}. For Ni(II)-IDA, the thickness at low coverage was - 38 {angstrom} and increased gradually with coverage to 47 {angstrom}. The in-plane averaged segment volume fraction of the adsorbed layer independently confirmed a thinner layer at low coverage for Cu(II)-IDA. These structural differences at the early stages are discussed in terms of either different preferred orientations for isolated chains in the two cases or more extensive conformational changes upon adsorption in the case of Cu(II)-IDA. Subphase dilution experiments provided additional insight, indicating that the adsorbed layer was not in equilibrium with the bulk solution even at low coverages for both IDA-chelated metal ions. We conclude that the weight of the evidence favors the interpretation based on more extensive

  3. Adsorption of Myoglobin to Cu(II)-IDA and Ni(II)-IDA Functionalized Langmuir Monolayers: Study of the Protein Layer Structure during the Adsorption Process by Neutron and X-Ray Reflectivity

    SciTech Connect

    Kent, M.S.; Yim, H.; Sasaki, D.Y.; Satija, Sushil; Seo, Young-Soo; Majewski, J.

    2010-07-19

    The structure and orientation of adsorbed myoglobin as directed by metal-histidine complexation at the liquid-film interface was studied as a function of time using neutron and X-ray reflectivity (NR and XR, respectively). In this system, adsorption is due to the interaction between iminodiacetate (IDA)-chelated divalent metal ions Ni(II) and Cu(II) and histidine moieties at the outer surface of the protein. Adsorption was examined under conditions of constant area per lipid molecule at an initial pressure of 40 mN/m. Adsorption occurred over a time period of about 15 h, allowing detailed characterization of the layer structure throughout the process. The layer thickness and the in-plane averaged segment volume fraction were obtained at roughly 40 min intervals by NR. The binding constant of histidine with Cu(II)-IDA is known to be about four times greater than that of histidine with Ni(II)-IDA. The difference in interaction energy led to significant differences in the structure of the adsorbed layer. For Cu(II)-IDA, the thickness of the adsorbed layer at low protein coverage was {le} 20 {angstrom} and the thickness increased almost linearly with increasing coverage to 42 {angstrom}. For Ni(II)-IDA, the thickness at low coverage was 38 {angstrom} and increased gradually with coverage to 47 {angstrom}. The in-plane averaged segment volume fraction of the adsorbed layer independently confirmed a thinner layer at low coverage for Cu(II)-IDA. These structural differences at the early stages are discussed in terms of either different preferred orientations for isolated chains in the two cases or more extensive conformational changes upon adsorption in the case of Cu(II)-IDA. Subphase dilution experiments provided additional insight, indicating that the adsorbed layer was not in equilibrium with the bulk solution even at low coverages for both IDA-chelated metal ions. We conclude that the weight of the evidence favors the interpretation based on more extensive

  4. The first protein crystal structure determined from high-resolution X-ray powder diffraction data: a variant of T3R3 human insulin-zinc complex produced by grinding.

    PubMed

    Von Dreele, R B; Stephens, P W; Smith, G D; Blessing, R H

    2000-12-01

    X-ray diffraction analysis of protein structure is often limited by the availability of suitable crystals. However, the absence of single crystals need not present an insurmountable obstacle in protein crystallography any more than it does in materials science, where powder diffraction techniques have developed to the point where complex oxide, zeolite and small organic molecular structures can often be solved from powder data alone. Here, that fact is demonstrated with the structure solution and refinement of a new variant of the T(3)R(3) Zn-human insulin complex produced by mechanical grinding of a polycrystalline sample. High-resolution synchrotron X-ray powder diffraction data were used to solve this crystal structure by molecular replacement adapted for Rietveld refinement. A complete Rietveld refinement of the 1630-atom protein was achieved by combining 7981 stereochemical restraints with a 4800-step (d(min) = 3.24 A) powder diffraction pattern and yielded the residuals R(wp) = 3.73%, R(p) = 2.84%, R(F)(2) = 8.25%. It was determined that the grinding-induced phase change is accompanied by 9.5 and 17.2 degrees rotations of the two T(3)R(3) complexes that comprise the crystal structure. The material reverts over 2-3 d to recover the original T(3)R(3) crystal structure. A Rietveld refinement of this 815-atom protein by combining 3886 stereochemical restraints with a 6000-step (d(min) = 3.06 A) powder diffraction pattern yielded the residuals R(wp) = 3.46%, R(p) = 2.64%, R(F)(2) = 7.10%. The demonstrated ability to solve and refine a protein crystal structure from powder diffraction data suggests that this approach can be employed, for example, to examine structural changes in a series of protein derivatives in which the structure of one member is known from a single-crystal study. PMID:11092920

  5. Panoramic Dental X-Ray

    MedlinePlus

    ... X-ray? What is Panoramic X-ray? Panoramic radiography , also called panoramic x-ray , is a two- ... Exams Dental Cone Beam CT X-ray, Interventional Radiology and Nuclear Medicine Radiation Safety About this Site ...

  6. X-ray binaries

    NASA Technical Reports Server (NTRS)

    1976-01-01

    Satellite X-ray experiments and ground-based programs aimed at observation of X-ray binaries are discussed. Experiments aboard OAO-3, OSO-8, Ariel 5, Uhuru, and Skylab are included along with rocket and ground-based observations. Major topics covered are: Her X-1, Cyg X-3, Cen X-3, Cyg X-1, the transient source A0620-00, other possible X-ray binaries, and plans and prospects for future observational programs.

  7. Confirmation of the monoclinic Cc space group for the ground state phase of Pb(Zr0.525Ti0.475)O3: A combined synchrotron X-ray and neutron powder diffraction study

    NASA Astrophysics Data System (ADS)

    Singh Solanki, Ravindra; Kumar Mishra, Sunil; Senyshyn, Anatoliy; Yoon, Songhak; Baik, Sunggi; Shin, Namsoo; Pandey, Dhananjai

    2013-02-01

    The low temperature antiferrodistortive phase transition in a pseudo-tetragonal composition of Pb(ZrxTi1-x)O3 (PZT) with x = 0.525 is investigated through a combined synchrotron x-ray and neutron powder diffraction study. It is shown that the superlattice peaks cannot be correctly accounted for in the Rietveld refinement using R3c or R3c + Cm structural models, whereas the Cc space group gives excellent fits to the superlattice peaks as well as to the perovskite peaks. This settles at rest the existing controversies about the structure of the ground state phase of PZT in the morphotropic phase boundary region.

  8. Development of x-ray laminography under an x-ray microscopic condition.

    PubMed

    Hoshino, Masato; Uesugi, Kentaro; Takeuchi, Akihisa; Suzuki, Yoshio; Yagi, Naoto

    2011-07-01

    An x-ray laminography system under an x-ray microscopic condition was developed to obtain a three-dimensional structure of laterally-extended planar objects which were difficult to observe by x-ray tomography. An x-ray laminography technique was introduced to an x-ray transmission microscope with zone plate optics. Three prototype sample holders were evaluated for x-ray imaging laminography. Layered copper grid sheets were imaged as a laminated sample. Diatomite powder on a silicon nitride membrane was measured to confirm the applicability of this method to non-planar micro-specimens placed on the membrane. The three-dimensional information of diatom shells on the membrane was obtained at a spatial resolution of sub-micron. Images of biological cells on the membrane were also obtained by using a Zernike phase contrast technique. PMID:21806188

  9. Development of x-ray laminography under an x-ray microscopic condition

    SciTech Connect

    Hoshino, Masato; Uesugi, Kentaro; Takeuchi, Akihisa; Suzuki, Yoshio; Yagi, Naoto

    2011-07-15

    An x-ray laminography system under an x-ray microscopic condition was developed to obtain a three-dimensional structure of laterally-extended planar objects which were difficult to observe by x-ray tomography. An x-ray laminography technique was introduced to an x-ray transmission microscope with zone plate optics. Three prototype sample holders were evaluated for x-ray imaging laminography. Layered copper grid sheets were imaged as a laminated sample. Diatomite powder on a silicon nitride membrane was measured to confirm the applicability of this method to non-planar micro-specimens placed on the membrane. The three-dimensional information of diatom shells on the membrane was obtained at a spatial resolution of sub-micron. Images of biological cells on the membrane were also obtained by using a Zernike phase contrast technique.

  10. Development of x-ray laminography under an x-ray microscopic condition

    NASA Astrophysics Data System (ADS)

    Hoshino, Masato; Uesugi, Kentaro; Takeuchi, Akihisa; Suzuki, Yoshio; Yagi, Naoto

    2011-07-01

    An x-ray laminography system under an x-ray microscopic condition was developed to obtain a three-dimensional structure of laterally-extended planar objects which were difficult to observe by x-ray tomography. An x-ray laminography technique was introduced to an x-ray transmission microscope with zone plate optics. Three prototype sample holders were evaluated for x-ray imaging laminography. Layered copper grid sheets were imaged as a laminated sample. Diatomite powder on a silicon nitride membrane was measured to confirm the applicability of this method to non-planar micro-specimens placed on the membrane. The three-dimensional information of diatom shells on the membrane was obtained at a spatial resolution of sub-micron. Images of biological cells on the membrane were also obtained by using a Zernike phase contrast technique.

  11. Correlation between Charge State of Insulating NaCl Surfaces and Ionic Mobility Induced by Water Adsorption: A Combined Ambient Pressure X-ray Photoelectron Spectroscopy and Scanning Force Microscopy Study

    SciTech Connect

    Verdaguer, Albert; Jose Segura, Juan; Fraxedas, Jordi; Bluhm, Hendrik; Salmeron, Miquel

    2008-09-03

    In situ ambient pressure X-ray photoelectron spectroscopy (APPES) and scanning force microscopy were used to characterize the surface discharge induced by water layers grown on (001) surfaces of sodium chloride single crystals. The APPES studies show that both kinetic energy (KE) and full width at half-maximum (FWHM) of the Na 2s and Cl 2p core level peaks, monitored as a function of relative humidity (RH), mimic surface conductivity curves measured using scanning force microscopy. The KE position and FWHM of the core level peaks therefore are directly related to the solvation and diffusion of ions at the NaCl(100) surface upon adsorption of water.

  12. Clay sized fraction and powdered whole-rock X-ray analyses from alluvial basin deposits in central and southern New Mexico

    USGS Publications Warehouse

    Anderholm, S.K.

    1985-01-01

    As part of the study of the water quality and geochemistry of Southwest Alluvial Basins (SWAB) in parts of Colorado, New Mexico, and Texas, which is a Regional Aquifer-System Analysis (RASA) program, whole rock x-ray analysis and clay-size fraction mineralogy (x-ray) analysis of selected samples from alluvial basin deposits were done to investigate the types of minerals and clay types present in the aquifers. This was done to determine the plausible minerals and clay types in the aquifers that may be reacting with groundwater and affecting the water quality. The purpose of this report is only to present the whole rock x-ray and clay-fraction mineralogy data. Nineteen surface samples or samples from outcrop of Tertiary and Quaternary alluvial basin deposits in the central and southern Rio Grande rift were collected and analyzed. The analysis of the samples consisted of grain size analysis, and clay-size fraction mineralogy and semiquantitative analysis of the relative abundance of different clay mineral groups present. (USGS)

  13. X-ray beamsplitter

    DOEpatents

    Ceglio, Natale M.; Stearns, Daniel S.; Hawryluk, Andrew M.; Barbee, Jr., Troy W.

    1989-01-01

    An x-ray beamsplitter which splits an x-ray beam into two coherent parts by reflecting and transmitting some fraction of an incident beam has applications for x-ray interferometry, x-ray holography, x-ray beam manipulation, and x-ray laser cavity output couplers. The beamsplitter is formed of a wavelength selective multilayer thin film supported by a very thin x-ray transparent membrane. The beamsplitter resonantly transmits and reflects x-rays through thin film interference effects. A thin film is formed of 5-50 pairs of alternate Mo/Si layers with a period of 20-250 A. The support membrane is 10-200 nm of silicon nitride or boron nitride. The multilayer/support membrane structure is formed across a window in a substrate by first forming the structure on a solid substrate and then forming a window in the substrate to leave a free-standing structure over the window.

  14. X-ray beamsplitter

    DOEpatents

    Ceglio, N.M.; Stearns, D.G.; Hawryluk, A.M.; Barbee, T.W. Jr.

    1987-08-07

    An x-ray beamsplitter which splits an x-ray beam into two coherent parts by reflecting and transmitting some fraction of an incident beam has applications for x-ray interferometry, x-ray holography, x-ray beam manipulation, and x-ray laser cavity output couplers. The beamsplitter is formed of a wavelength selective multilayer thin film supported by a very thin x-ray transparent membrane. The beamsplitter resonantly transmits and reflects x-rays through thin film interference effects. A thin film is formed of 5--50 pairs of alternate Mo/Si layers with a period of 20--250 A. The support membrane is 10--200 nm of silicon nitride or boron nitride. The multilayer/support membrane structure is formed across a window in a substrate by first forming the structure on a solid substrate and then forming a window in the substrate to leave a free-standing structure over the window. 6 figs.

  15. X-ray - skeleton

    MedlinePlus

    A skeletal x-ray is an imaging test used to look at the bones. It is used to detect fractures , tumors, or ... in the health care provider's office by an x-ray technologist. You will lie on a table or ...

  16. Extremity x-ray

    MedlinePlus

    An extremity x-ray is an image of the hands, wrist, feet, ankle, leg, thigh, forearm humerus or upper arm, hip, shoulder ... term "extremity" often refers to a human limb. X-rays are a form of radiation that passes through ...

  17. X-ray Spectrometry.

    ERIC Educational Resources Information Center

    Markowicz, Andrzej A.; Van Grieken, Rene E.

    1984-01-01

    Provided is a selective literature survey of X-ray spectrometry from late 1981 to late 1983. Literature examined focuses on: excitation (photon and electron excitation and particle-induced X-ray emission; detection (wavelength-dispersive and energy-dispersive spectrometry); instrumentation and techniques; and on such quantitative analytical…

  18. X-ray monochromator

    NASA Technical Reports Server (NTRS)

    Hoover, Richard B. (Inventor)

    1992-01-01

    An x-ray monochromator is described, wherin a housing supports a plurality of mirrors forming a plurality of opposed mirror faces in parallel with each other and having thereon multilayer coatings, with each of said pairs of mirror faces being provided with identical coatings which are different from the coatings on the other pairs of mirror faces such that each pair of mirror faces has a peak x-ray reflection at a different wavelength regime. The housing is moveable to bring into a polychromatic x-ray beam that pair of mirror faces having the best x-ray reflection for the desired wavelength, with the mirrors being pivotable to move the mirror faces to that angle of incidence at which the peak reflectivity of the desired wavelength x-rays occurs.

  19. X-ray generator

    DOEpatents

    Dawson, John M.

    1976-01-01

    Apparatus and method for producing coherent secondary x-rays that are controlled as to direction by illuminating a mixture of high z and low z gases with an intense burst of primary x-rays. The primary x-rays are produced with a laser activated plasma, and these x-rays strip off the electrons of the high z atoms in the lasing medium, while the low z atoms retain their electrons. The neutral atoms transfer electrons to highly excited states of the highly striped high z ions giving an inverted population which produces the desired coherent x-rays. In one embodiment, a laser, light beam provides a laser spark that produces the intense burst of coherent x-rays that illuminates the mixture of high z and low z gases, whereby the high z atoms are stripped while the low z ones are not, giving the desired mixture of highly ionized and neutral atoms. To this end, the laser spark is produced by injecting a laser light beam, or a plurality of beams, into a first gas in a cylindrical container having an adjacent second gas layer co-axial therewith, the laser producing a plasma and the intense primary x-rays in the first gas, and the second gas containing the high and low atomic number elements for receiving the primary x-rays, whereupon the secondary x-rays are produced therein by stripping desired ions in a neutral gas and transfer of electrons to highly excited states of the stripped ions from the unionized atoms. Means for magnetically confining and stabilizing the plasma are disclosed for controlling the direction of the x-rays.

  20. Structural properties of a family of hydrogen-bonded co-crystals formed between gemfibrozil and hydroxy derivatives of t-butylamine, determined directly from powder X-ray diffraction data

    NASA Astrophysics Data System (ADS)

    Cheung, Eugene Y.; David, Sarah E.; Harris, Kenneth D. M.; Conway, Barbara R.; Timmins, Peter

    2007-03-01

    We report the formation and structural properties of co-crystals containing gemfibrozil and hydroxy derivatives of t-butylamine H 2NC(CH 3) 3-n(CH 2OH) n, with n=0, 1, 2 and 3. In each case, a 1:1 co-crystal is formed, with transfer of a proton from the carboxylic acid group of gemfibrozil to the amino group of the t-butylamine derivative. All of the co-crystal materials prepared are polycrystalline powders, and do not contain single crystals of suitable size and/or quality for single crystal X-ray diffraction studies. Structure determination of these materials has been carried out directly from powder X-ray diffraction data, using the direct-space Genetic Algorithm technique for structure solution followed by Rietveld refinement. The structural chemistry of this series of co-crystal materials reveals well-defined structural trends within the first three members of the family ( n=0, 1, 2), but significantly contrasting structural properties for the member with n=3.

  1. Cation substitution in synthetic meridianiite (MgSO4·11H2O) I: X-ray powder diffraction analysis of quenched polycrystalline aggregates

    NASA Astrophysics Data System (ADS)

    Fortes, A. Dominic; Browning, Frank; Wood, Ian G.

    2012-05-01

    Meridianiite, MgSO4·11H2O, is the most highly hydrated phase in the binary MgSO4-H2O system. Lower hydrates in the MgSO4-H2O system have end-member analogues containing alternative divalent metal cations (Ni2+, Zn2+, Mn2+, Cu2+, Fe2+, and Co2+) and exhibit extensive solid solution with MgSO4 and with one another, but no other undecahydrate is known. We have prepared aqueous MgSO4 solutions doped with these other cations in proportions up to and including the pure end-members. These liquids have been solidified into fine-grained polycrystalline blocks of metal sulfate hydrate + ice by rapid quenching in liquid nitrogen. The solid products have been characterised by X-ray powder diffraction, and the onset of partial melting has been quantified using a thermal probe. We have established that of the seven end-member metal sulfates studied, only MgSO4 forms an undecahydrate; ZnSO4 forms an orthorhombic heptahydrate (synthetic goslarite), MnSO4, FeSO4, and CoSO4 form monoclinic heptahydrates (syn. mallardite, melanterite, bieberite, respectively), and CuSO4 crystallises as the well-known triclinic pentahydrate (syn. chalcanthite). NiSO4 forms a new hydrate which has been indexed with a triclinic unit cell of dimensions a = 6.1275(1) Å, b = 6.8628(1) Å, c = 12.6318(2) Å, α = 92.904(2)°, β = 97.678(2)°, and γ = 96.618(2)°. The unit-cell volume of this crystal, V = 521.74(1) Å3, is consistent with it being an octahydrate, NiSO4·8H2O. Further analysis of doped specimens has shown that synthetic meridianiite is able to accommodate significant quantities of foreign cations in its structure; of the order 50 mol. % Co2+ or Mn2+, 20-30 mol. % Ni2+ or Zn2+, but less than 10 mol. % of Cu2+ or Fe2+. In three of the systems we examined, an `intermediate' phase occurred that differed in hydration state both from the Mg-bearing meridianiite end-member and the pure dopant end-member hydrate. In the case of CuSO4, we observed a melanterite-structured heptahydrate at Cu

  2. X-ray crystallography

    NASA Technical Reports Server (NTRS)

    2001-01-01

    X-rays diffracted from a well-ordered protein crystal create sharp patterns of scattered light on film. A computer can use these patterns to generate a model of a protein molecule. To analyze the selected crystal, an X-ray crystallographer shines X-rays through the crystal. Unlike a single dental X-ray, which produces a shadow image of a tooth, these X-rays have to be taken many times from different angles to produce a pattern from the scattered light, a map of the intensity of the X-rays after they diffract through the crystal. The X-rays bounce off the electron clouds that form the outer structure of each atom. A flawed crystal will yield a blurry pattern; a well-ordered protein crystal yields a series of sharp diffraction patterns. From these patterns, researchers build an electron density map. With powerful computers and a lot of calculations, scientists can use the electron density patterns to determine the structure of the protein and make a computer-generated model of the structure. The models let researchers improve their understanding of how the protein functions. They also allow scientists to look for receptor sites and active areas that control a protein's function and role in the progress of diseases. From there, pharmaceutical researchers can design molecules that fit the active site, much like a key and lock, so that the protein is locked without affecting the rest of the body. This is called structure-based drug design.

  3. Modeling high adsorption capacity and kinetics of organic macromolecules on super-powdered activated carbon.

    PubMed

    Matsui, Yoshihiko; Ando, Naoya; Yoshida, Tomoaki; Kurotobi, Ryuji; Matsushita, Taku; Ohno, Koichi

    2011-02-01

    The capacity to adsorb natural organic matter (NOM) and polystyrene sulfonates (PSSs) on small particle-size activated carbon (super-powdered activated carbon, SPAC) is higher than that on larger particle-size activated carbon (powdered-activated carbon, PAC). Increased adsorption capacity is likely attributable to the larger external surface area because the NOM and PSS molecules do not completely penetrate the adsorbent particle; they preferentially adsorb near the outer surface of the particle. In this study, we propose a new isotherm equation, the Shell Adsorption Model (SAM), to explain the higher adsorption capacity on smaller adsorbent particles and to describe quantitatively adsorption isotherms of activated carbons of different particle sizes: PAC and SPAC. The SAM was verified with the experimental data of PSS adsorption kinetics as well as equilibrium. SAM successfully characterized PSS adsorption isotherm data for SPACs and PAC simultaneously with the same model parameters. When SAM was incorporated into an adsorption kinetic model, kinetic decay curves for PSSs adsorbing onto activated carbons of different particle sizes could be simultaneously described with a single kinetics parameter value. On the other hand, when SAM was not incorporated into such an adsorption kinetic model and instead isotherms were described by the Freundlich model, the kinetic decay curves were not well described. The success of the SAM further supports the adsorption mechanism of PSSs preferentially adsorbing near the outer surface of activated carbon particles. PMID:21172719

  4. Lumbosacral spine x-ray

    MedlinePlus

    X-ray - lumbosacral spine; X-ray - lower spine ... The test is done in a hospital x-ray department or your health care provider's office by an x-ray technician. You will be asked to lie on the x-ray table ...

  5. Thoracic spine x-ray

    MedlinePlus

    Vertebral radiography; X-ray - spine; Thoracic x-ray; Spine x-ray; Thoracic spine films; Back films ... The test is done in a hospital radiology department or in the health care provider's office. You will lie on the x-ray table in different positions. If the x-ray ...

  6. X-ray laser

    DOEpatents

    Nilsen, Joseph

    1991-01-01

    An X-ray laser (10) that lases between the K edges of carbon and oxygen, i.e. between 44 and 23 Angstroms, is provided. The laser comprises a silicon (12) and dysprosium (14) foil combination (16) that is driven by two beams (18, 20) of intense line focused (22, 24) optical laser radiation. Ground state nickel-like dysprosium ions (34) are resonantly photo-pumped to their upper X-ray laser state by line emission from hydrogen-like silicon ions (32). The novel X-ray laser should prove especially useful for the microscopy of biological specimens.

  7. Adsorption of clofibric acid and ketoprofen onto powdered activated carbon: effect of natural organic matter.

    PubMed

    Gao, Yaohuan; Deshusses, Marc A

    2011-12-01

    The adsorption of two acidic pharmaceutically active compounds (PhACs), clofibric acid and ketoprofen, onto powdered activated carbon (PAC) was investigated with a particular focus on the influence of natural organic matter (NOM) on the adsorption of the PhACs. Suwannee River humic acids (SRHAs) were used as a substitute for NOM. Batch adsorption experiments were conducted to obtain adsorption kinetics and adsorption isotherms with and without SRHAs in the system. The adsorption isotherms and adsorption kinetics showed that the adsorption ofclofibric acid was not significantly affected by the presence of SRHAs at a concentration of 5 mg (as carbon) L(-1). An adsorption capacity of 70 to 140 mg g(-1) was observed and equilibrium was reached within 48 h. In contrast, the adsorption of ketoprofen was markedly decreased (from about 120 mg g(-1) to 70-100 mg g(-1)) in the presence of SRHAs. Higher initial concentrations of clofibric acid than ketoprofen during testing may explain the different behaviours that were observed. Also, the more hydrophobic ketoprofen molecules may have less affinity for PAC when humic acids (which are hydrophilic) are present. The possible intermolecular forces that could account for the different behaviour of clofibric acid and ketoprofen adsorption onto PAC are discussed. In particular, the relevance of electrostatic forces, electron donor-acceptor interaction, hydrogen bonding and London dispersion forces are discussed PMID:22439557

  8. Medical X-Rays

    MedlinePlus

    ... Diagnostic X-Ray Equipment Compliance Program Guidance Manual CP 7386.003 Field Compliance Testing of Diagnostic (Medical) ... and Exporting Electronic Products Compliance Program Guidance Manual CP 7386.003 Field Compliance Testing of Diagnostic (Medical) ...

  9. Dental x-rays

    MedlinePlus

    ... or impacted teeth The presence and extent of dental caries (cavities) Bone damage (such as from periodontitis ) Abscessed ... Dental x-rays can reveal dental cavities (tooth decay) before they ... take yearly bitewings for the early development of cavities.

  10. X-ray - skeleton

    MedlinePlus

    ... is used to look for: Fractures or broken bone Cancer that has spread to other areas of the ... 2014:chap 8. Read More Bone tumor Broken bone Cancer Metastasis Osteomyelitis X-ray Update Date 5/9/ ...

  11. Abdominal x-ray

    MedlinePlus

    An abdominal x-ray is an imaging test to look at organs and structures in the abdomen. Organs include the spleen, stomach, and intestines. When the test is done to look at the bladder and kidney structures, ...

  12. X-Ray Spectrometry.

    ERIC Educational Resources Information Center

    Macdonald, G. L.

    1980-01-01

    Reviews instrumental developments and technique improvements in X-ray spectrometry, grouped into major topic areas of excitation, dispersion and detection, instrumentation and techniques, and quantitative analyses. Cites 162 references. (CS)

  13. Bone x-ray

    MedlinePlus

    ... or broken bone Bone tumors Degenerative bone conditions Osteomyelitis (inflammation of the bone caused by an infection) ... Multiple myeloma Osgood-Schlatter disease Osteogenesis imperfecta Osteomalacia Osteomyelitis Paget disease of the bone Rickets X-ray ...

  14. Cosmic x ray physics

    NASA Technical Reports Server (NTRS)

    Mccammon, Dan; Cox, D. P.; Kraushaar, W. L.; Sanders, W. T.

    1992-01-01

    This final report covers the period 1 January 1985 - 31 March 1992. It is divided into the following sections: the soft x-ray background; proportional counter and filter calibrations; sounding rocket flight preparations; new sounding rocket payload: x-ray calorimeter; and theoretical studies. Staff, publications, conference proceedings, invited talks, contributed talks, colloquia and seminars, public service lectures, and Ph. D. theses are listed.

  15. Thoracic spine x-ray

    MedlinePlus

    Vertebral radiography; X-ray - spine; Thoracic x-ray; Spine x-ray; Thoracic spine films; Back films ... Gillard JH, Schaefer-Prokop CM, eds. Grainger & Allison's Diagnostic Radiology: A Textbook of Medical Imaging . 6th ed. New ...

  16. Transmission and fluorescence X-ray absorption spectroscopy cell/flow reactor for powder samples under vacuum or in reactive atmospheres

    NASA Astrophysics Data System (ADS)

    Hoffman, A. S.; Debefve, L. M.; Bendjeriou-Sedjerari, A.; Ouldchikh, S.; Bare, Simon R.; Basset, J.-M.; Gates, B. C.

    2016-07-01

    X-ray absorption spectroscopy is an element-specific technique for probing the local atomic-scale environment around an absorber atom. It is widely used to investigate the structures of liquids and solids, being especially valuable for characterization of solid-supported catalysts. Reported cell designs are limited in capabilities—to fluorescence or transmission and to static or flowing atmospheres, or to vacuum. Our goal was to design a robust and widely applicable cell for catalyst characterizations under all these conditions—to allow tracking of changes during genesis and during operation, both under vacuum and in reactive atmospheres. Herein, we report the design of such a cell and a demonstration of its operation both with a sample under dynamic vacuum and in the presence of gases flowing at temperatures up to 300 °C, showing data obtained with both fluorescence and transmission detection. The cell allows more flexibility in catalyst characterization than any reported.

  17. Transmission and fluorescence X-ray absorption spectroscopy cell/flow reactor for powder samples under vacuum or in reactive atmospheres.

    PubMed

    Hoffman, A S; Debefve, L M; Bendjeriou-Sedjerari, A; Ouldchikh, S; Bare, Simon R; Basset, J-M; Gates, B C

    2016-07-01

    X-ray absorption spectroscopy is an element-specific technique for probing the local atomic-scale environment around an absorber atom. It is widely used to investigate the structures of liquids and solids, being especially valuable for characterization of solid-supported catalysts. Reported cell designs are limited in capabilities-to fluorescence or transmission and to static or flowing atmospheres, or to vacuum. Our goal was to design a robust and widely applicable cell for catalyst characterizations under all these conditions-to allow tracking of changes during genesis and during operation, both under vacuum and in reactive atmospheres. Herein, we report the design of such a cell and a demonstration of its operation both with a sample under dynamic vacuum and in the presence of gases flowing at temperatures up to 300 °C, showing data obtained with both fluorescence and transmission detection. The cell allows more flexibility in catalyst characterization than any reported. PMID:27475549

  18. Adsorption of Halogenated Fire-Extinguishing Agents on Powders

    NASA Technical Reports Server (NTRS)

    Barduhn, Allen J.; Patel, Bhailal S.; Meyer, Walter; Smura, Bronislaw B.

    1960-01-01

    The amounts of four different Freons adsorbed by carbon, silica gel, alumina, and molecular sieves were determined at pressures up to 225 lb/sq in. The carbon adsorbed 50 to 100 percent and the silica gels, 30 to 50 percent of their own weight of Freon. Several adsorbed systems were tested in a standard dry-powder extinguisher on a 5-sq-ft gasoline fire for their effectiveness in putting out a fire. One of the Freons (bromotrifluoromethane) and carbon extinguished fires about as well as bicarbonate powder and nitrogen.

  19. Ammonia plasma treated polyethylene films for adsorption or covalent immobilization of trypsin: quantitative correlation between X-ray photoelectron spectroscopy data and enzyme activity.

    PubMed

    Ghasemi, Mahsa; Minier, Michel J G; Tatoulian, Michaël; Chehimi, Mohamed M; Arefi-Khonsari, Farzaneh

    2011-09-01

    The ammonia plasma process was used for generating reactive groups, particularly primary amine functions on the surface of polyethylene (PE) films, to immobilize the enzyme trypsin. The attachment of the enzyme was achieved by directly applying an aqueous solution of trypsin to the plasma-activated surface or by using glutaraldehyde as a chemical linker. In both cases, the utilization of sodium cyanoborohydride efficiently stabilized the immobilization. The surfaces were analyzed by X-ray photoelectron spectroscopy (XPS) and enzymatic activity measurements. Active trypsin was successfully immobilized on the surface with a mean activity of 0.09 ± 0.02 U/cm(2). The study of the stability of the immobilized enzyme during repetitive assays showed that some activity could be maintained during several months. An original quantitative correlation between the immobilized enzyme activity and the XPS signal intensity of the S 2p electrons present in the sulfur-containing amino acid residues was evidenced. PMID:21770448

  20. Vacancy-induced nanoscale phase separation in KxFe2–ySe₂ single crystals evidenced by Raman scattering and powder x-ray diffraction

    SciTech Connect

    Lazarević, N.; Abeykoon, M.; Stephens, P. W.; Lei, Hechang; Bozin, E. S.; Petrovic, C.; Popović, Z. V.

    2012-08-06

    Polarized Raman scattering spectra of KxFe2–ySe₂ were analyzed in terms of peculiarities of both I4/m and I4/mmm space group symmetries. The presence of the Raman active modes from both space group symmetries (16 Raman-active modes of the I4/m phase and two Raman-active modes of the I4/mmm phase) confirmed the existence of two crystallographic domains with different space group symmetry in a KxFe2–ySe₂ sample. High-resolution synchrotron powder x-ray diffraction structural refinement of the same sample confirmed the two-phase description, and determined the atomic positions and occupancies for both domains.

  1. Crystal structure of LiLnW{sub 2}O{sub 8} (Ln=lanthanides and Y): An X-ray powder diffraction study

    SciTech Connect

    Postema, J.M.; Fu, W.T.; IJdo, D.J.W.

    2011-08-15

    Crystal structures that occur in LiLnW{sub 2}O{sub 8} (Ln=lanthanides and Y) have been studied using Rietveld profile analysis of X-ray diffraction data. Two types of structures were observed. The scheelite structure of the space group I4{sub 1}/a is adopted for compounds containing large lanthanides Ln=La-Gd. For smaller lanthanides (Ln=Dy-Lu and Y) the wolframite structure with the space group P2/n is observed. In LiTbW{sub 2}O{sub 8}, both structures occur. The phase transition between the two is a slow process making the obtainment of pure low temperature phase (wolframite) difficult. The space groups P1-bar and P2, recently reported for LiEuW{sub 2}O{sub 8} and LiYW{sub 2}O{sub 8}, have not been observed in this series of compounds. - Graphical abstract: Part of the X-ray diffraction patterns of LiSmW{sub 2}O{sub 8} and LiDyW{sub 2}O{sub 8} representing two structure types in LiLnW{sub 2}O{sub 8}: the scheelite with Ln=La-Gd and wolframite with Ln=Dy-Lu and Y. In LiTbW{sub 2}O{sub 8} both the scheelite and the wolframite structures occur at high and low temperatures, respectively. Highlights: > Double tungstates of the formula LiLnW{sub 2}O{sub 8} (Ln=lanthanides and Y) were systematically synthesised and their crystal structures were determined. > LiLnW{sub 2}O{sub 8} adopt either the scheelite structure (I4{sub 1}/a) (Ln=La-Gd) or wolframite structure (P2/n) (Ln=Dy-Lu and Y). > Both structures occur in LiTbW{sub 2}O{sub 8} and the I4{sub 1}/a{yields}P2/n phase transition is a slow process. > The space groups P1-bar and P2 recently reported for LiEuW{sub 2}O{sub 8} and LiYW{sub 2}O{sub 8} were not observed.

  2. X-ray nanotomography

    NASA Astrophysics Data System (ADS)

    Sasov, Alexander

    2004-10-01

    A compact laboratory x-ray "nano-CT" scanner has been created for 3D non-invasive imaging with 150-200 nanometers 3D spatial resolution, using advanced x-ray technologies and specific physical phenomena for signal detection. This spatial resolution in volume terms is 3 orders better than can be achieved in synchrotron tomography, 5 orders better then in existing laboratory micro-CT instruments and 10-12 orders better in comparison to clinical CT. The instrument employs an x-ray source with a 300-400nm x-ray spot size and uses small-angle scattering to attain a detail detectability of 150-200nm. An object manipulator allows positioning and rotation with an accuracy of 150nm. The x-ray detector is based on an intensified CCD with single-photon sensitivity. A typical acquisition cycle for 3D reconstruction of the full object volume takes from 10 to 60 minutes, with the collection of several hundred angular views. Subsequent volumetric reconstruction produces results as a set of cross sections with isotropic voxel size down to 140 x 140 x 140nm, or as a 3D-model, which can be virtually manipulated and measured. This unique spatial resolution in non-invasive investigations gives previously unattainable 3D images in several application areas, such as composite materials, paper and wood microstructure, biomedical applications and others.

  3. Adsorption and reaction of acetylene on clean and oxygen-precovered Pd(100) studied with high-resolution X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Höfert, O.; Lorenz, M. P. A.; Streber, R.; Zhao, W.; Bayer, A.; Steinrück, H.-P.; Papp, C.

    2013-10-01

    We investigated the adsorption and thermal evolution of acetylene on clean Pd(100) and Pd(100) precovered with 0.25 ML oxygen. The measurements were performed in situ by fast XPS at the synchrotron radiation facility BESSY II. On Pd(100) acetylene molecularly adsorbs at 130 K. Upon heating transformation to a CCH species occurs around 390 K along with the formation of a completely dehydrogenated carbon species. On the oxygen-precovered surface partial CCH formation already occurs upon adsorption at 130 K, and the dehydrogenation temperature and the stability range of CCH are shifted to lower temperatures by ˜200 K.

  4. Adsorption and reaction of acetylene on clean and oxygen-precovered Pd(100) studied with high-resolution X-ray photoelectron spectroscopy.

    PubMed

    Höfert, O; Lorenz, M P A; Streber, R; Zhao, W; Bayer, A; Steinrück, H-P; Papp, C

    2013-10-28

    We investigated the adsorption and thermal evolution of acetylene on clean Pd(100) and Pd(100) precovered with 0.25 ML oxygen. The measurements were performed in situ by fast XPS at the synchrotron radiation facility BESSY II. On Pd(100) acetylene molecularly adsorbs at 130 K. Upon heating transformation to a CCH species occurs around 390 K along with the formation of a completely dehydrogenated carbon species. On the oxygen-precovered surface partial CCH formation already occurs upon adsorption at 130 K, and the dehydrogenation temperature and the stability range of CCH are shifted to lower temperatures by ∼200 K. PMID:24182063

  5. Lumbosacral spine x-ray

    MedlinePlus

    X-ray - lumbosacral spine; X-ray - lower spine ... be placed over the lower part of your spine. You will be asked to hold your breath ... x-ray. The most common reason for lumbosacral spine x-ray is to look for the cause ...

  6. Metal incorporation in sputter-deposited MoS{sub 2} films studied by extended x-ray adsorption fine structure

    SciTech Connect

    Lince, J.R.; Hilton, M.R.; Bommannavar, A.S.

    1995-08-01

    Solid lubricant films produced by cosputtering metals with MoS{sub 2} and by forming metal/MoS{sub 2} multilayers are being planned for use in the next generation of solid lubricated devices on spacecraft, including gimbal and sensor bearings, actuators, and sliding electrical contacts. The films exhibit increased densities and wear lives compared to films without additives, but the mechanism of density enhancement is not well understood. The extended x-ray absorption fine structure (EXAFS) technique is ideal for elucidating the structure of these poorly crystalline films. We analyzed MoS{sub 2} films cosputtered with 0, 2, and 10% Ni, as well as Ni/MoS{sub 2} and Au(Pd)/MoS{sub 2} multilayer films. The results obtained at the Mo-K absorption edge showed that the metal-containing films comprised predominantly the same nanocrystalline phases present in similar films without added metals: pure MoS{sub 2} and a MoS{sub 2{minus}{ital x}}O{sub {ital x}} phase. MoS{sub 2{minus}{ital x}}O{sub {ital x}} is isostructural with MoS{sub 2}, with O atoms substituting for S atoms in the MoS{sub 2} crystal lattice. For all Ni-containing films, EXAFS data obtained at the Ni--K absorption edge showed that the Ni had not chemically reacted with the MoS{sub 2{minus}{ital x}}O{sub {ital x}} and MoS{sub 2}, but formed a disordered NiO{sub {ital x}} phase. However, Ni-cosputtered films showed decreasing Mo--Mo bond lengths in the MoS{sub 2{minus}{ital x}}O{sub {ital x}} phase with increasing Ni content, probably due to preferential oxidation of Ni compared to MoS{sub 2}. EXAFS of these Ni-cosputtered films showed only a small decrease in short-range order with Ni content, while x-ray diffraction showed a concurrent large decrease in long-range order. The results indicate that film densification in Ni-cosputtered films is caused by NiO{sub {ital x}} formation at the edges of nucleating MoS{sub 2{minus}{ital x}}O{sub {ital x}} /MoS{sub 2} crystallites.

  7. X-ray beam finder

    DOEpatents

    Gilbert, H.W.

    1983-06-16

    An X-ray beam finder for locating a focal spot of an X-ray tube includes a mass of X-ray opaque material having first and second axially-aligned, parallel-opposed faces connected by a plurality of substantially identical parallel holes perpendicular to the faces and a film holder for holding X-ray sensitive film tightly against one face while the other face is placed in contact with the window of an X-ray head.

  8. X-ray astronomical spectroscopy

    NASA Technical Reports Server (NTRS)

    Holt, Stephen S.

    1987-01-01

    The contributions of the Goddard group to the history of X-ray astronomy are numerous and varied. One role that the group has continued to play involves the pursuit of techniques for the measurement and interpretation of the X-ray spectra of cosmic sources. The latest development is the selection of the X-ray microcalorimeter for the Advanced X-ray Astrophysics Facility (AXAF) study payload. This technology is likely to revolutionize the study of cosmic X-ray spectra.

  9. X-ray

    MedlinePlus

    ... Most experts feel that the benefits of appropriate x-ray imaging greatly outweigh any risks. Young children and babies ... be pregnant. Alternative Names ... CM, eds. Grainger & Allison's Diagnostic Radiology: A Textbook of Medical Imaging . 6th ed. Philadelphia, PA: Elsevier Churchill Livingstone; 2014: ...

  10. Adsorption of counter ions to a stearate monolayer spread at the water-air interface: A synchrotron x-ray study

    SciTech Connect

    Bloch, J.M.; Yun, W.B.; Yang, X. ); Montano, P.A. . Dept. of Physics); Ramanathan, M. ); Capasso, C. )

    1988-06-01

    The Near Total External Fluorescence (NTEF) technique was used to measure in-situ the adsorption of a metal ion from a subphase solution to the liquid-air interface, induced by a surfactant monolayer on the interface. For a monolayer formed by spreading stearic acid (a surfactant material) on a 10{sup {minus}3} mole/l solution of MnCl{sub 2}, the ratio of Mn ions segregated to the interface to the number of stearate molecules on the surface was determined to be approximately 0.6 {plus minus} 0.2. SEXAFS experiments revealed local order of the Mn ions at the surface at the condensed phase but no order showed up in the expanded phase. We explain these findings using a self consistent Poisson-Boltzman calculation of a partially ionized monolayer. Our model also explains earlier reports of adsorption of metal ions to the liquid/monolayer interface. 19 refs., 3 figs.

  11. High temperature phase stability in Li{sub 0.12}Na{sub 0.88}NbO{sub 3}: A combined powder X-ray and neutron diffraction study

    SciTech Connect

    Mishra, S. K.; Krishna, P. S. R.; Shinde, A. B.; Jayakrishnan, V. B.; Mittal, R.; Sastry, P. U.; Chaplot, S. L.

    2015-09-07

    The phase stabilities of ecofriendly piezoelectric material of lithium doped sodium niobate for composition Li{sub 0.12}Na{sub 0.88}NbO{sub 3} (LNN12) have been investigated by a combination of powder X-ray and neutron diffraction techniques in the temperature range of 300–1100 K. We observed interesting changes with appearance or disappearance of the super-lattice reflections in the powder diffraction patterns. Unambiguous experimental evidence is shown for coexistence of paraelectric and ferroelectric orthorhombic phases in the temperature range of 525 K to 675 K. We identified the correct crystal structure of LNN12 with temperature and correlated it with observed anomaly in the physical properties. Identification of crystal structure also helps in the mode assignments in Raman and infrared spectroscopies. We argued that application of chemical pressure as a result of Li substitution in NaNbO{sub 3} matrix favors the freezing of zone centre phonons in contrast to the freezing of zone boundary phonons in pure NaNbO{sub 3} with the variation of temperature.

  12. The adsorption of small hydrocarbons on Cu(111): A combined He-atom scattering and x-ray absorption study for ethane, ethylene, and acetylene

    NASA Astrophysics Data System (ADS)

    Fuhrmann, D.; Wacker, D.; Weiss, K.; Hermann, K.; Witko, M.; Wöll, Ch.

    1998-02-01

    Ethane (C2H6), ethylene (C2H4), and acetylene (C2H2) adsorbed on Cu (111) are investigated using high-resolution helium atom scattering and x-ray absorption spectroscopy (NEXAFS). For C2H6/Cu(111) and C2H4/Cu(111) the excitation energies of the frustrated molecular translation normal to the surface (FTz) amount to 6.7 meV, suggesting the presence of a physisorbed species which is consistent with the NEXAFS data for ethylene. In contrast, for C2H2/Cu(111) the NEXAFS data indicate strong intramolecular distortions of the acetylene adsorbate compatible with a tilt of both CH ends away from the molecular axis. While the latter finding is in agreement with recent theoretical studies the theoretically predicted chemisorbed ethylene species could not be observed by the experiment. However, more detailed theoretical studies of the ethylene-Cu(111) interaction potential reveal two minima separated by an activation barrier. The minimum closer to the surface refers to strongly distorted chemisorbed C2H4 whereas the outer minimum is characterized by a free molecule-like physisorbed species. Thus the results from the present measurements are explained by the theoretically confirmed physisorbed species while chemisorbed C2H4 has to be excluded. Complementary results for ethylene and acetylene adsorbed on Pb(111) reveal a FTz-mode energy of 6.5 and 6.7 meV, respectively, thus revealing a much weaker acetylene-substrate binding than seen for Cu(111). Also in case of Pb(111) the FTz-mode showed an Einstein-like behavior with a flat dispersion curve, as for corresponding modes on the Cu(111)-substrate, see above.

  13. Synthetic, spectral, thermal and powder X-ray diffraction studies of bis(O-alkyldithiocarbonato-S,S‧) antimony(III) dialkyldithiocarbamates

    NASA Astrophysics Data System (ADS)

    Chauhan, H. P. S.; Joshi, Sapana; Carpenter, Jaswant

    2015-02-01

    Compounds of antimony(III) with mixed sulfur donor ligands of the type [(ROCS2)2SbS2CNR‧2] (where, R = C2H5, and iC3H7; R‧ = CH3, C2H5, and CH2CH2) have been synthesized using anhydrous acetone as a solvent by the one pot reaction of antimony(III) tris(O-alkyldithiocarbonato-S,S‧), antimony(III) chloride and sodium/ammonium salt of dialkyldithiocarbamate in 2:1:3 molar ratios. These compounds have been characterized by physicochemical [melting points, molecular weight determinations, elemental analyses (C, H, N, S, and Sb)], spectral [UV, IR, Far-IR and NMR (1H and 13C)] studies. In IR spectra strong band was observed at 1028-1051 cm-1 which indicates anisobidentate mode of bonding of both the ligands with antimony metal. NMR spectral data of these compounds show expected proton resonance due to corresponding moieties. The powder XRD, ESI-Mass and thermal (TG and DTA) studies have also been performed to get the information about geometrical parameters, fragmentation pattern and last thermal decomposition product, respectively. The powder XRD studies lead to the structural properties of the synthesized compounds and show the nanorange crystallite size and monoclinic crystal system. Thermal data of these compounds indicate the formation of antimony sulfide (Sb2S3) as a final thermal degradation product which is used in a number of ways like switching devices television cameras and microwave devices.

  14. Physicochemical properties and adsorption of cholesterol by okra (Abelmoschus esculentus) powder.

    PubMed

    Chen, Yi; Zhang, Bing-Cheng; Sun, Yu-Han; Zhang, Jian-Guo; Sun, Han-Ju; Wei, Zhao-Jun

    2015-12-01

    Okra (Abelmoschus esculentus) is a widely used medicine and functional food. In order to clarify the effects of the particle size on its functional properties, okra pods were subjected to superfine grinding, and its properties were determined using different methods. Four particle size levels of okra powders were prepared: 380 to 250, 250 to 75, 75 to 40 and less than 40 μm. The results showed that superfine grinding technology could efficiently pulverize the particles into the submicron scale, whose distribution was close to a Gaussian distribution. With decreasing okra powder size, the specific surface area, water holding capacity (WHC), water-retention capacity (WRC), oil-binding capacity (OBC), tapped density and total flavonoids extraction were increased significantly (p < 0.05). Moreover, the adsorption of cholesterol by okra powder was improved after superfine grinding. These results suggest that okra powder can be used in food manufacturing as a functional food ingredient. PMID:26359588

  15. CH 3Cl adsorption on a Si(100)2 × 1 surface modified by alkali metal overlayer studied by soft X-ray photoemission using synchrotron radiation

    NASA Astrophysics Data System (ADS)

    Gentle, T. M.; Soukiassian, P.; Schuette, K. P.; Bakshi, M. H.; Hurych, Z.

    1988-08-01

    We present the first study of the effect of an alkali metal overlayer on the adsorption of an organic molecule, methylchloride, on a Si(100)2 × 1 surface. In strong contrast to the behavior of molecular oxygen or nitrogen which were found to react with the silicon substrate, there was no significant interaction between methylchloride and silicon, rather, the formation of alkali-chlorine bonds was observed. Core level and valence band spectroscopies using synchrotron radiation were used to study these systems. Sodium was found to exhibit the strongest interaction with mehtylchloride which was dissociated, while the effects produced by K and Cs were weaker.

  16. Pressure-induced phase transitions in organic molecular crystals: a combination of x-ray single-crystal and powder diffraction, raman and IR-spectroscopy

    NASA Astrophysics Data System (ADS)

    Boldyreva, E. V.; Sowa, H.; Ahsbahs, H.; Goryainov, S. V.; Chernyshev, V. V.; Dmitriev, V. P.; Seryotkin, Y. V.; Kolesnik, E. N.; Shakhtshneider, T. P.; Ivashevskaya, S. N.; Drebushchak, T. N.

    2008-07-01

    The contribution summarizes the results of recent studies of phase transitions induced by high pressure in a number of molecular organic crystals, such as polymorphs of paracetamol, chlorpropamide, polymorphs of glycine, L- and DL-serine, β-alanine. The main attention is paid to the following topics: (1) Reversible / irreversible transformations; (2) Different behavior of single crystals / powders; (3) The role of pressure-transmitting liquid; (4) The role of the kinetic factors: phase transitions on decompression, or after a long storage at a selected pressure; (5) Isosymmetric phase transitions; (6) The role of the changes in the hydrogen bond networks / intramolecular conformational changes in the phase transitions; (7) Superstructures / nanostructures formed as a result of pressure-induced phase transitions.

  17. X-Ray Astronomy

    NASA Technical Reports Server (NTRS)

    Wu, S. T.

    2000-01-01

    Dr. S. N. Zhang has lead a seven member group (Dr. Yuxin Feng, Mr. XuejunSun, Mr. Yongzhong Chen, Mr. Jun Lin, Mr. Yangsen Yao, and Ms. Xiaoling Zhang). This group has carried out the following activities: continued data analysis from space astrophysical missions CGRO, RXTE, ASCA and Chandra. Significant scientific results have been produced as results of their work. They discovered the three-layered accretion disk structure around black holes in X-ray binaries; their paper on this discovery is to appear in the prestigious Science magazine. They have also developed a new method for energy spectral analysis of black hole X-ray binaries; four papers on this topics were presented at the most recent Atlanta AAS meeting. They have also carried Monte-Carlo simulations of X-ray detectors, in support to the hardware development efforts at Marshall Space Flight Center (MSFC). These computation-intensive simulations have been carried out entirely on the computers at UAH. They have also carried out extensive simulations for astrophysical applications, taking advantage of the Monte-Carlo simulation codes developed previously at MSFC and further improved at UAH for detector simulations. One refereed paper and one contribution to conference proceedings have been resulted from this effort.

  18. X-ray Spectrometer

    NASA Technical Reports Server (NTRS)

    Porter, F. Scott

    2004-01-01

    The X-ray Spectrometer (XRS) instrument is a revolutionary non-dispersive spectrometer that will form the basis for the Astro-E2 observatory to be launched in 2005. We have recently installed a flight spare X R S microcalorimeter spectrometer at the EBIT-I facility at LLNL replacing the XRS from the earlier Astro-E mission and providing twice the resolution. The X R S microcalorimeter is an x-ray detector that senses the heat deposited by the incident photon. It achieves a high energy resolution by operating at 0.06K and by carefully controlling the heat capacity and thermal conductance. The XRS/EBIT instrument has 32 pixels in a square geometry and achieves an energy resolution of 6 eV at 6 keV, with a bandpass from 0.1 to 12 keV (or more at higher operating temperature). The instrument allows detailed studies of the x-ray line emission of laboratory plasmas. The XRS/EBIT also provides an extensive calibration "library" for the Astro-E2 observatory.

  19. Monitoring X-Ray Emission from X-Ray Bursters

    NASA Technical Reports Server (NTRS)

    Kaaret, Philip

    1998-01-01

    The goal of this investigation was to use the All-Sky Monitor on the Rossi X-Ray Timing Explorer (RXTE) in combination with the Burst and Transient Source Experiment on the Compton Gamma-Ray Observatory to simultaneously measure the x-ray (2-12 keV) and hard x-ray (20-100 keV) emission from x-ray bursters. The investigation was successful. We made the first simultaneous measurement of hard and soft x-ray emission and found a strong anticorrelation of hard and soft x-ray emission from the X-Ray Burster 4U 0614+091. The monitoring performed under this investigation was also important in triggering target of opportunity observations of x-ray bursters made under the investigation hard x-ray emission of x-ray bursters approved for RXTE cycles 1 and 2. These observations lead to a number of papers on high-frequency quasi-periodic oscillations and on hard x-ray emission from the x-ray bursters 4U 0614+091 and 4U 1705-44.

  20. Adsorption of Cd(II) Ions from Aqueous Solutions by Lalang (Imperata cylindrica)Leaf Powder: Effect of Physicochemical Environment

    NASA Astrophysics Data System (ADS)

    Megat Hanafiah, M. A. K.; Yahya, M. Z. A.; Zakaria, H.; Ibrahim, S. C.

    The adsorption of cadmium from aqueous solution with a plant waste particularly Lalang or Imperata cylindrica (IC) leaf powder was investigated. The effect of various operating variables mainly adsorbate concentration, adsorbent dose, adsorbent size, temperature and pH was studied. The adsorption of Cd2+ ions increased with increase in pH, temperature, adsorbent dose and decrease in adsorbent size. Adsorption was rapid and occurred within 15 min for cadmium concentration of 1 mg L-1 and 30 min for cadmium concentrations of 2 and 5 mg L-1. The kinetic process of Cd2+ adsorption onto IC leaf powder was found to fit the pseudo-second-order rate equation.

  1. Experimental study of germanium adsorption on goethite and germanium coprecipitation with iron hydroxide: X-ray absorption fine structure and macroscopic characterization

    NASA Astrophysics Data System (ADS)

    Pokrovsky, O. S.; Pokrovski, G. S.; Schott, J.; Galy, A.

    2006-07-01

    Adsorption of germanium on goethite was studied at 25 °C in batch reactors as a function of pH (1-12), germanium concentration in solution (10 -7 to 0.002 M) and solid/solution ratio (1.8-17 g/L). The maximal surface site density determined via Ge adsorption experiments at pH from 6 to 10 is equal to 2.5 ± 0.1 μmol/m 2. The percentage of adsorbed Ge increases with pH at pH < 9, reaches a maximum at pH ˜ 9 and slightly decreases when pH is further increased to 11. These results allowed generation of a 2-p K Surface Complexation Model (SCM) which implies a constant capacitance of the electric double layer and postulates the presence of two Ge complexes, >FeO-Ge(OH)30 and >FeO-GeO(OH)2-, at the goethite-solution interface. Coprecipitation of Ge with iron oxy(hydr)oxides formed during Fe(II) oxidation by atmospheric oxygen or by Fe(III) hydrolysis in neutral solutions led to high Ge incorporations in solid with maximal Ge/Fe molar ratio close to 0.5. The molar Ge/Fe ratio in precipitated solid is proportional to that in the initial solution according to the equation (Ge/Fe) solid = k × (Ge/Fe) solution with 0.7 ⩽ k ⩽ 1.0. The structure of adsorbed and coprecipitated Ge complexes was further characterized using XAFS spectroscopy. In agreement with previous data on oxyanions adsorption on goethite, bi-dentate bi-nuclear surface complexes composed of tetrahedrally coordinated Ge attached to the corners of two adjacent Fe octahedra represent the dominant contribution to the EXAFS signal. Coprecipitated samples with Ge/Fe molar ratios >0.1, and samples not aged in solution (<1 day) having intermediate Ge/Fe ratios (0.01-0.1) show 4 ± 0.3 oxygen atoms at 1.76 ± 0.01 Å around Ge. Samples less concentrated in Ge (0.001 < Ge/Fe < 0.10) and aged longer times in solution (up to 280 days) exhibit a splitting of the first atomic shell with Ge in both tetrahedral ( R = 1.77 ± 0.02 Å) and octahedral ( R = 1.92 ± 0.03 Å) coordination with oxygen. In these samples

  2. Fluctuation X-Ray Scattering

    SciTech Connect

    Saldin, PI: D. K.; Co-I's: J. C. H. Spence and P. Fromme

    2013-01-25

    The work supported by the grant was aimed at developing novel methods of finding the structures of biomolecules using x-rays from novel sources such as the x-ray free electron laser and modern synchrotrons

  3. Adsorption of heavy metal from aqueous solution by dehydrated root powder of long-root Eichhornia crassipes.

    PubMed

    Li, Qiang; Chen, Bo; Lin, Peng; Zhou, Jiali; Zhan, Juhong; Shen, Qiuying; Pan, Xuejun

    2016-01-01

    The root powder of long-root Eichhornia crassipes, as a new kind of biodegradable adsorbent, has been tested for aqueous adsorption of Pb, Zn, Cu, and Cd. From FT-IR, we found that the absorption peaks of phosphorous compounds, carbonyl, and nitrogenous compounds displayed obvious changes before and after adsorption which illustrated that plant characteristics may play a role in binding with metals. Surface properties and morphology of the root powders have been characterized by means of SEM and BET. Energy spectrum analysis showed that the metals were adsorbed on root powders after adsorption. Then, optimum quantity of powder, pH values, and metal ion concentrations in single-system and multi-system were detected to discuss the characteristics and mechanisms of metal adsorption. Freundlich model and the second-order kinetics equation could well describe the adsorption of heavy metals in single-metal system. The adsorption of Pb, Zn, and Cd in the multi-metal system decreased with the concentration increased. At last, competitive adsorption of every two metals on root powder proved that Cu and Pb had suppressed the adsorption performance of Cd and Zn. PMID:26605425

  4. Accelerated adsorption by activated carbon powders in the presence of an acoustic field

    NASA Astrophysics Data System (ADS)

    Hawkins, Timothy W.; Meegan, G. Douglas; Peterson, Chris E.

    2003-10-01

    Vaporous contaminants can be removed from a gas stream by adsorption into powdered activated carbon (PAC). For example, the injection of PAC upstream of particle collectors is the leading approach for the removal of mercury vapor from the exhaust streams of incinerators and coal fired power plants. The removal of dilute vapors, though, can require significant time and significant quantities of PAC. A numerical model will be described that suggests that the adsorption process can be accelerated by applying an intense sound field to the gas after the PAC is injected. It is theorized that a sound field improves diffusion limited adsorption reactions by creating an oscillatory motion of the gas relative to the activated carbon particles. The translation effectively mixes the particles and gas on a microscopic scale and improves the concentration gradient at the surface of the PAC. Results from the numerical model suggest that adsorption rates can be increased by over 50% with the application of an appropriate sound field. Simple laboratory experiments have been performed studying the adsorption of dilute vaporous ethanol in air, and the results support the model. Data has also been collected at a coal fired power plant that demonstrates the improved adsorption of mercury vapor.

  5. X-ray Crystallography Facility

    NASA Technical Reports Server (NTRS)

    2000-01-01

    Edward Snell, a National Research Council research fellow at NASA's Marshall Space Flight Center (MSFC), prepares a protein crystal for analysis by x-ray crystallography as part of NASA's structural biology program. The small, individual crystals are bombarded with x-rays to produce diffraction patterns, a map of the intensity of the x-rays as they reflect through the crystal.

  6. Tunable X-ray source

    DOEpatents

    Boyce, James R.

    2011-02-08

    A method for the production of X-ray bunches tunable in both time and energy level by generating multiple photon, X-ray, beams through the use of Thomson scattering. The method of the present invention simultaneously produces two X-ray pulses that are tunable in energy and/or time.

  7. Unraveling the Hydrogenation of TiO 2 and Graphene Oxide/TiO 2 Composites in Real Time by in Situ Synchrotron X-ray Powder Diffraction and Pair Distribution Function Analysis

    DOE PAGESBeta

    Nguyen-Phan, Thuy-Duong; Liu, Zongyuan; Luo, Si; Gamalski, Andrew D.; Vovchok, Dimitry; Xu, Wenqian; Stach, Eric A.; Polyansky, Dmitry E.; Fujita, Etsuko; Rodriguez, José A.; et al

    2016-02-18

    The functionalization of graphene oxide (GO) and graphene by TiO2 and other metal oxides has attracted considerable attention due to numerous promising applications in catalysis, energy conversion, and storage. We propose hydrogenation of this class of materials as a promising way to tune catalytic properties by altering the structural and chemical transformations that occur upon H incorporation. We also investigate the structural changes that occur during the hydrogenation process using in situ powder X-ray diffraction and pair distribution function analysis of GO–TiO2 and TiO2 under H2 reduction. Sequential Rietveld refinement was employed to gain insight into the evolution of crystalmore » growth of TiO2 nanoparticles in the presence of two-dimensional (2D) GO nanosheets. GO sheets not only significantly retarded the nucleation and growth of rutile impurities, stabilizing the anatase structure, but was also partially reduced to hydrogenated graphene by the introduction of atomic hydrogen into the honeycomb lattice. We discuss the hydrogenation processes and the resulting composite structure that occurs during the incorporation of atomic H and the dynamic structural transformations that leads to a highly active photocatalyst.« less

  8. High-energy X-ray powder diffraction and atomic-pair distribution-function studies of charged/discharged structures in carbon-hybridized Li2MnSiO4 nanoparticles as a cathode material for lithiumion batteries

    SciTech Connect

    Moriya, Maki; Miyahara, Masahiko; Hokazono, Mana; Sasaki, Hirokazu; Nemoto, Atsushi; Katayama, Shingo; Akimoto, Yuji; Hirano, Shin-ichi; Ren, Yang

    2014-10-01

    The stable cycling performance with a high discharge capacity of similar to 190 mAh g(-1) in a carbon-hybridized Li2MnSiO4 nanostructured powder has prompted an experimental investigation of the charged/discharged structures using synchrotron-based and laboratory-based X-rays and atomic-pair distributionfunction (PDF) analyses. A novel method of in-situ spray pyrolysis of a precursor solution with glucose as a carbon source enabled the successful synthesis of the carbon-hybridized Li2(M)nSiO(4) nanoparticles. The XRD patters of the discharged (lithiated) samples exhibit a long-range ordered structure characteristic of the (beta) Li2MnSiO4 crystalline phase (space group Pmn2(1)) which dissipates in the charged (delithiated) samples. However, upon discharging the long-range ordered structure recovers in each cycle. The disordered structure, according to the PDF analysis, is mainly due to local distortions of the MnO4 tetrahedra which show a mean Mn-O nearest neighbor distance shorter than that of the long-range ordered phase. These results corroborate the notion of the smaller Mn3+/Mn4+ ionic radii in the Li extracted phase versus the larger Mn2+ ionic radius in Li inserted phase. Thus Li extraction/insertion drives the fluctuation between the disordered and the long-range ordered structures. (C) 2014 Elsevier B.V. All rights reserved.

  9. Syntheses, Vibrational Spectroscopy, and Crystal Structure Determination from X-Ray Powder Diffraction Data of Alkaline Earth Dicyanamides M[N(CN) 2] 2 with M=Mg, Ca, Sr, and Ba

    NASA Astrophysics Data System (ADS)

    Jürgens, Barbara; Irran, Elisabeth; Schnick, Wolfgang

    2001-03-01

    The alkaline earth dicyanamides Mg[N(CN)2]2, Ca[N(CN)2]2, Sr[N(CN)2]2, and Ba[N(CN)2]2 were synthesized by ion exchange using Na[N(CN)2] and the respective nitrates or bromides as starting materials. The crystal structures were determined from X-ray powder diffractometry: Mg[N(CN)2]2, Pnnm, Z=2, a=617.14(3), b=716.97(3), and c=740.35(5) pm; Ca[N(CN)2]2 and Sr[N(CN)2]2, C2/c, Z=4; Ca[N(CN)2]2, a=1244.55(3), b=607.97(1), and c=789.81(1) pm, β=98.864(2)°; Sr[N(CN)2]2, a=1279.63(2), b=624.756(8), and c=817.56(1) pm, β=99.787(1)°; Ba[N(CN)2]2, Pnma, Z=4, a=1368.68(7), b=429.07(7), and c=1226.26(2) pm. The dicyanamides consist of the respective alkaline earth cations and bent planar [N(CN)2]- ions. The structural features were correlated with vibrational spectroscopic data. The thermal behavior was studied by thermoanalytical experiments.

  10. Polymorphism of ceramide 3. Part 2: a vibrational spectroscopic and X-ray powder diffraction investigation of N-octadecanoyl phytosphingosine and the analogous specifically deuterated d(35) derivative.

    PubMed

    Raudenkolb, Steve; Wartewig, Siegfried; Neubert, Reinhard H H

    2003-07-01

    In order to characterize the arrangements of the hydrocarbon chains of ceramide 3, the thermotropic phase behaviour of the ceramides N-octadecanoylphytosphingosine (CER3) and its chain deuterated derivative N-(d(35)-octadecanoyl)phytosphingosine (d(35)CER3) was studied by means of X-ray powder diffraction, FT-IR and Raman spectroscopy. CER3 and d(35)CER3 exhibit an identical thermotropic polymorphism involving three different crystalline phases. The selective deuteration of the fatty acid chain enables to distinguish the sphingoid part from the fatty acid part by means of FT-IR and Raman spectroscopy. It could be shown that both hydrocarbon chains are arranged in different subcells. Temperature dependent Raman measurements elucidate simultaneously the changes in the trans/gauche ratios and the packing of both the hydrocarbon chains of the fatty acid and of the sphingoid part. The phase behaviour of CER3 and d(35)CER3, both dry and hydrated, was investigated. PMID:12818735

  11. Assessment of the optimum degree of Sr{sub 3}Fe{sub 2}MoO{sub 9} electron-doping through oxygen removal: An X-ray powder diffraction and {sup 57}Fe Moessbauer spectroscopy study

    SciTech Connect

    Lopez, Carlos A.; Viola, Maria del C.; Pedregosa, Jose C.; Mercader, Roberto C.

    2010-10-15

    We describe the preparation and structural characterization by X-ray powder diffraction (XRPD) and Moessbauer spectroscopy of three electron-doped perovskites Sr{sub 3}Fe{sub 2}MoO{sub 9-{delta}} with Fe/Mo = 2 obtained from Sr{sub 3}Fe{sub 2}MoO{sub 9}. The compounds were synthesized by topotactic reduction with H{sub 2}/N{sub 2} (5/95) at 600, 700 and 800 {sup o}C. Above 800 {sup o}C the Fe/Mo ratio changes from Fe/Mo = 2-1 < Fe/Mo < 2. The structural refinements of the XRPD data for the reduced perovskites were carried out by the Rietveld profile analysis method. The crystal structure of these phases is cubic, space group Fm3-bar m, with cationic disorder at the two different B sites that can be populated in variable proportions by the Fe atoms. The Moessbauer spectra allowed determining the evolution of the different species formed after the treatments at different temperatures and confirm that Fe ions in the samples reduced at 600, 700 and 800 {sup o}C are only in the high-spin Fe{sup 3+} electronic state.

  12. Refinement of the crystal structure of the high-temperature phase G0 in (NH4)2WO2F4 (powder, x-ray, and neutron scattering)

    SciTech Connect

    Novak, D. M.; Smirnov, Lev S; Kolesnikov, Alexander I; Voronin, Vladimir; Berger, I. F.; Laptash, N. M.; Vasil'ev, N. M.; Flerov, I. N.

    2013-01-01

    The (NH4)2WO2F4 compound undergoes a series of phase transitions: G0 -> 201 K -> G1 -> 160 K -> G2, with a significant change in entropy ( S1 ~ Rln10 at the G0 -> G1 transition), which indicates significant orientational disordering in the G0 phase and the order disorder type of the phase transition. X-ray diffraction is used to identify the crystal structure of the G0 phase as rhombohedral (sp. gr. Cmcm, Z = 4), determine the lattice parameters and the positions of all atoms (except hydrogen), and show that [WO2F4]2 ions can form a superposition of dynamic and static orientational disorders in the anionic sublattice. A determination of the orientational position of [NH4]+ ions calls for the combined method of elastic and inelastic neutron scattering. Inelastic neutron scattering is used to determine the state of hindered rotation for ammonium ions in the G0 phase. Powder neutron diffraction shows that the orientational disorder of NH4 ions can adequately be described within the free rotation approximation.

  13. Hydrogen in polar intermetallics: Syntheses and structures of the ternary Ca5Bi3D0.93, Yb5Bi3Hx, and Sm5Bi3H~1 by powder neutron or single crystal X-ray diffraction

    SciTech Connect

    Leon-Escamilla, E. Alejandro; Dervenagas, Panagiotis; Stasis, Constantine; Corbett, John D.

    2010-01-01

    The syntheses of the title compounds are described in detail. Structural characterizations from refinements of single crystal X-ray diffraction data for Yb{sub 5}Bi{sub 3}H{sub x} and Sm{sub 5}Bi{sub 3}H{sub 1} and of powder neutron diffraction data for Ca{sub 5}Bi{sub 3}D{sub 0.93(3)} are reported. These confirm that all three crystallize with the heavy atom structure type of {beta}-Yb{sub 5}Sb{sub 3}, and the third gives the first proof that the deuterium lies in the center of nominal calcium tetrahedra, isostructural with the Ca{sub 5}Sb{sub 3}F-type structure. These Ca and Yb phases are particularly stable with respect to dissociation to Mn{sub 5}Si{sub 3}-type product plus H{sub 2}. Some contradictions in the literature regarding Yb{sub 5}Sb{sub 3} and Yb{sub 5}Sb{sub 3}H{sub x} phases are considered in terms of adventitious hydrogen impurities that are generated during reactions in fused silica containers at elevated temperatures.

  14. The thermal behaviour and structural stability of nesquehonite, MgCO3.3H2O, evaluated by in situ laboratory parallel-beam X-ray powder diffraction: New constraints on CO2 sequestration within minerals.

    PubMed

    Ballirano, Paolo; De Vito, Caterina; Ferrini, Vincenzo; Mignardi, Silvano

    2010-06-15

    In order to gauge the appropriateness of CO(2) reaction with Mg chloride solutions as a process for storing carbon dioxide, the thermal behaviour and structural stability of its solid product, nesquehonite (MgCO(3).3H(2)O), were investigated in situ using real-time laboratory parallel-beam X-ray powder diffraction. The results suggest that the nesquehonite structure remains substantially unaffected up to 373 K, with the exception of a markedly anisotropic thermal expansion acting mainly along the c axis. In the 371-390 K range, the loss of one water molecule results in the nucleation of a phase of probable composition MgCO(3).2H(2)O, which is characterized by significant structural disorder. At higher temperatures (423-483 K), both magnesite and MgO.2MgCO(3) coexist. Finally, at 603 K, periclase nucleation starts and the disappearance of carbonate phases is completed at 683 K. Consequently, the structural stability of nesquehonite at high temperatures suggests that it will remain stable under the temperature conditions that prevail at the Earth's surface. These results will help (a) to set constraints on the temperature conditions under which nesquehonite may be safely stored and (b) to develop CO(2) sequestration via the synthesis of nesquehonite for industrial application. PMID:20167421

  15. Refinement of the crystal structure of the high-temperature phase G{sub 0} in (NH{sub 4}){sub 2}WO{sub 2}F{sub 4} (powder, X-ray, and neutron scattering)

    SciTech Connect

    Novak, D. M. Smirnov, L. S.; Kolesnikov, A. I.; Voronin, V. I.; Berger, I. F.; Laptash, N. M.; Vasil'ev, A. D.; Flerov, I. N.

    2013-01-15

    The (NH{sub 4}){sub 2}WO{sub 2}F{sub 4} compound undergoes a series of phase transitions: G{sub 0} {yields} 201, K {yields} G{sub 1} {yields} 160, and K {yields} G{sub 2}, with a significant change in entropy ({Delta}S{sub 1} {approx} Rln10 at the G{sub 0} {yields} G{sub 1} transition), which indicates significant orientational disordering in the G{sub 0} phase and the order-disorder type of the phase transition. X-ray diffraction is used to identify the crystal structure of the G{sub 0} phase as rhombohedral (sp. gr. Cmcm, Z = 4), determine the lattice parameters and the positions of all atoms (except hydrogen), and show that [WO{sub 2}F{sub 4}]{sup 2-} ions can form a superposition of dynamic and static orientational disorders in the anionic sublattice. A determination of the orientational position of [NH{sub 4}]{sup +} ions calls for the combined method of elastic and inelastic neutron scattering. Inelastic neutron scattering is used to determine the state of hindered rotation for ammonium ions in the G{sub 0} phase. Powder neutron diffraction shows that the orientational disorder of NH{sub 4} ions can adequately be described within the free-rotation approximation.

  16. Phase transition and NH3 dynamics in [Ni(NH3)4](ReO4)2 studied by infrared absorption, X-ray powder diffraction and neutron scattering methods

    NASA Astrophysics Data System (ADS)

    Hetmańczyk, Łukasz; Hetmańczyk, Joanna

    2016-05-01

    The phase transition in [Ni(NH3)4](ReO4)2 detected previously by differential scanning calorimetry (DSC) at Tch = 188 K was now investigated by infrared absorption (FT-IR), incoherent inelastic and elastic neutron scattering (IINS, ND), and X-ray powder diffraction (XRPD) methods. The reorientational dynamics of NH3 groups was investigated by infrared band shape analysis (IRBS) and quasielastic neutron scattering (QENS) methods. The infrared data show that some of the bands split in the vicinity of the phase transition temperature, which suggests a change in the crystal structure. The systematic narrowing of particular bands at cooling is also observed, but reorientational dynamics of NH3 is not stopped at the phase transition temperature, which is fully confirmed by the QENS analysis. The broadening of the quasielastic neutron scattering peak is clearly visible below the phase transition temperature. Both NPD and XRPD measurements indicate that a small change of crystal structure is associated with the phase transition.

  17. Stepwise effects of the BCR sequential chemical extraction procedure on dissolution and metal release from common ferromagnesian clay minerals: a combined solution chemistry and X-ray powder diffraction study.

    PubMed

    Ryan, P C; Hillier, S; Wall, A J

    2008-12-15

    Sequential extraction procedures (SEPs) are commonly used to determine speciation of trace metals in soils and sediments. However, the non-selectivity of reagents for targeted phases has remained a lingering concern. Furthermore, potentially reactive phases such as phyllosilicate clay minerals often contain trace metals in structural sites, and their reactivity has not been quantified. Accordingly, the objective of this study is to analyze the behavior of trace metal-bearing clay minerals exposed to the revised BCR 3-step plus aqua regia SEP. Mineral quantification based on stoichiometric analysis and quantitative powder X-ray diffraction (XRD) documents progressive dissolution of chlorite (CCa-2 ripidolite) and two varieties of smectite (SapCa-2 saponite and SWa-1 nontronite) during steps 1-3 of the BCR procedure. In total, 8 (+/-1) % of ripidolite, 19 (+/-1) % of saponite, and 19 (+/-3) % of nontronite (% mineral mass) dissolved during extractions assumed by many researchers to release trace metals from exchange sites, carbonates, hydroxides, sulfides and organic matter. For all three reference clays, release of Ni into solution is correlated with clay dissolution. Hydrolysis of relatively weak Mg-O bonds (362 kJ/mol) during all stages, reduction of Fe(III) during hydroxylamine hydrochloride extraction and oxidation of Fe(II) during hydrogen peroxide extraction are the main reasons for clay mineral dissolution. These findings underscore the need for precise mineral quantification when using SEPs to understand the origin/partitioning of trace metals with solid phases. PMID:18951614

  18. X-ray satellite

    NASA Technical Reports Server (NTRS)

    1985-01-01

    An overview of the second quarter 1985 development of the X-ray satellite project is presented. It is shown that the project is proceeding according to plan and that the projected launch date of September 9, 1987 is on schedule. An overview of the work completed and underway on the systems, subsystems, payload, assembly, ground equipment and interfaces is presented. Problem areas shown include cost increases in the area of focal instrumentation, the star sensor light scattering requirements, and postponements in the data transmission subsystems.

  19. SMM x ray polychromator

    NASA Technical Reports Server (NTRS)

    Saba, J. L. R.

    1993-01-01

    The objective of the X-ray Polychromator (XRP) experiment was to study the physical properties of solar flare plasma and its relation to the parent active region to understand better the flare mechanism and related solar activity. Observations were made to determine the temperature, density, and dynamic structure of the pre-flare and flare plasma as a function of wavelength, space and time, the extent to which the flare plasma departs from thermal equilibrium, and the variation of this departure with time. The experiment also determines the temperature and density structure of active regions and flare-induced changes in the regions.

  20. Soft x-ray lasers

    SciTech Connect

    Matthews, D.L.; Rosen, M.D.

    1988-12-01

    One of the elusive dreams of laser physicists has been the development of an x-ray laser. After 25 years of waiting, the x-ray laser has at last entered the scientific scene, although those now in operation are still laboratory prototypes. They produce soft x rays down to about five nanometers. X-ray lasers retain the usual characteristics of their optical counterparts: a very tight beam, spatial and temporal coherence, and extreme brightness. Present x-ray lasers are nearly 100 times brighter that the next most powerful x-ray source in the world: the electron synchrotron. Although Lawrence Livermore National Laboratory (LLNL) is widely known for its hard-x-ray laser program which has potential applications in the Strategic Defense Initiative, the soft x-ray lasers have no direct military applications. These lasers, and the scientific tools that result from their development, may one day have a place in the design and diagnosis of both laser fusion and hard x-ray lasers. The soft x-ray lasers now in operation at the LLNL have shown great promise but are still in the primitive state. Once x-ray lasers become reliable, efficient, and economical, they will have several important applications. Chief among them might be the creation of holograms of microscopic biological structures too small to be investigated with visible light. 5 figs.

  1. X-ray lithography source

    DOEpatents

    Piestrup, Melvin A.; Boyers, David G.; Pincus, Cary

    1991-01-01

    A high-intensity, inexpensive X-ray source for X-ray lithography for the production of integrated circuits. Foil stacks are bombarded with a high-energy electron beam of 25 to 250 MeV to produce a flux of soft X-rays of 500 eV to 3 keV. Methods of increasing the total X-ray power and making the cross section of the X-ray beam uniform are described. Methods of obtaining the desired X-ray-beam field size, optimum frequency spectrum and elminating the neutron flux are all described. A method of obtaining a plurality of station operation is also described which makes the process more efficient and economical. The satisfying of these issues makes transition radiation an exellent moderate-priced X-ray source for lithography.

  2. X-ray lithography source

    DOEpatents

    Piestrup, M.A.; Boyers, D.G.; Pincus, C.

    1991-12-31

    A high-intensity, inexpensive X-ray source for X-ray lithography for the production of integrated circuits is disclosed. Foil stacks are bombarded with a high-energy electron beam of 25 to 250 MeV to produce a flux of soft X-rays of 500 eV to 3 keV. Methods of increasing the total X-ray power and making the cross section of the X-ray beam uniform are described. Methods of obtaining the desired X-ray-beam field size, optimum frequency spectrum and eliminating the neutron flux are all described. A method of obtaining a plurality of station operation is also described which makes the process more efficient and economical. The satisfying of these issues makes transition radiation an excellent moderate-priced X-ray source for lithography. 26 figures.

  3. Monitoring X-Ray Emission from X-Ray Bursters

    NASA Technical Reports Server (NTRS)

    Halpern, Jules P.; Kaaret, Philip

    1999-01-01

    The scientific goal of this project was to monitor a selected sample of x-ray bursters using data from the All-Sky Monitor (ASM) on the Rossi X-Ray Timing Explorer together with data from the Burst and Transient Source Experiment (BATSE) on the Compton Gamma-Ray Observatory to study the long-term temporal evolution of these sources in the x-ray and hard x-ray bands. The project was closely related to "Long-Term Hard X-Ray Monitoring of X-Ray Bursters", NASA project NAG5-3891, and and "Hard x-ray emission of x-ray bursters", NASA project NAG5-4633, and shares publications in common with both of these. The project involved preparation of software for use in monitoring and then the actual monitoring itself. These efforts have lead to results directly from the ASM data and also from Target of Opportunity Observations (TOO) made with the Rossi X-Ray Timing Explorer based on detection of transient hard x-ray outbursts with the ASM and BATSE.

  4. Isotope microscopy visualization of the adsorption profile of 2-methylisoborneol and geosmin in powdered activated carbon.

    PubMed

    Matsui, Yoshihiko; Sakamoto, Asuka; Nakao, Soichi; Taniguchi, Takuma; Matsushita, Taku; Shirasaki, Nobutaka; Sakamoto, Naoya; Yurimoto, Hisayoshi

    2014-09-16

    Decreasing the particle size of powdered activated carbon may enhance its equilibrium adsorption capacity for small molecules and micropollutants, such as 2-methylisoborneol (MIB) and geosmin, as well as for macromolecules and natural organic matter. Shell adsorption, in which adsorbates do not completely penetrate the adsorbent but instead preferentially adsorb near the outer surface of the adsorbent, may explain this enhancement in equilibrium adsorption capacity. Here, we used isotope microscopy and deuterium-doped MIB and geosmin to directly visualize the solid-phase adsorbate concentration profiles of MIB and geosmin in carbon particles. The deuterium/hydrogen ratio, which we used as an index of the solid-phase concentration of MIB and geosmin, was higher in the shell region than in the inner region of carbon particles. Solid-phase concentrations of MIB and geosmin obtained from the deuterium/hydrogen ratio roughly agreed with those predicted by shell adsorption model analyses of isotherm data. The direct visualization of the localization of micropollutant adsorbates in activated carbon particles provided direct evidence of shell adsorption. PMID:25162630

  5. Quantitative determination of two polymorphic forms of imatinib mesylate in a drug substance and tablet formulation by X-ray powder diffraction, differential scanning calorimetry and attenuated total reflectance Fourier transform infrared spectroscopy.

    PubMed

    Bellur Atici, Esen; Karlığa, Bekir

    2015-10-10

    Imatinib has been identified as a tyrosine kinase inhibitor that selectively inhibits the Abl tyrosine kinases, including Bcr-Abl. The active substance used in drug product is the mesylate salt form of imatinib, a phenylaminopyrimidine derivative and chemically named as N-(3-(4-(pyridin-3-yl) pyrimidin-2-ylamino)-4-methylphenyl)-4-((4-methylpiperazin-1-yl) methyl)-benzamide methanesulfonic acid salt. It exhibits many polymorphic forms and most stable and commercialized polymorphs are known as α and β forms. Molecules in α and β polymorphic forms exhibit significant conformational differences due to their different intra- and intermolecular interactions, which stabilize their molecular conformations and affect their physicochemical properties such as bulk density, melting point, solubility, stability, and processability. The manufacturing process of a drug tablet included granulation, compression, coating, and drying may cause polymorphic conversions. Therefore, polymorphic content of the drug substance should be controlled during quality control and stability testing. Attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy, differential scanning calorimetry (DSC), and powder X-ray diffraction (PXRD) methods were evaluated for determination of the polymorphic content of the drug substance and drug product; and PXRD was the most accurate technique and selected as preferred method and validated. Prior to development of a quantification method, pure α and β polymorphs were characterized and used throughout the method development and validation studies. Mixtures with different ratios of α and β forms were scanned using X-ray diffractometer with a scan rate of 0.250°/min over an angular range of 19.5-21.0° 2θ and the peak heights for characteristic peak of β form at 20.5 ± 0.2° 2θ diffraction angle were used to generate a calibration curve. The detection limit of β polymorph in α form imatinib mesylate tablets was found as 4% and

  6. X-ray and neutron powder diffraction analyses of Gly·MgSO4·5H2O and Gly·MgSO4·3H2O, and their deuterated counterparts.

    PubMed

    Howard, Christopher; Wood, Ian G; Knight, Kevin S; Fortes, A Dominic

    2016-03-01

    We have identified a new compound in the glycine-MgSO4-water ternary system, namely glycine magnesium sulfate trihydrate (or Gly·MgSO4·3H2O) {systematic name: catena-poly[[tetraaquamagnesium(II)]-μ-glycine-κ(2)O:O'-[diaquabis(sulfato-κO)magnesium(II)]-μ-glycine-κ(2)O:O']; [Mg(SO4)(C2D5NO2)(D2O)3]n}, which can be grown from a supersaturated solution at ∼350 K and which may also be formed by heating the previously known glycine magnesium sulfate pentahydrate (or Gly·MgSO4·5H2O) {systematic name: hexaaquamagnesium(II) tetraaquadiglycinemagnesium(II) disulfate; [Mg(D2O)6][Mg(C2D5NO2)2(D2O)4](SO4)2} above ∼330 K in air. X-ray powder diffraction analysis reveals that the trihydrate phase is monoclinic (space group P21/n), with a unit-cell metric very similar to that of recently identified Gly·CoSO4·3H2O [Tepavitcharova et al. (2012). J. Mol. Struct. 1018, 113-121]. In order to obtain an accurate determination of all structural parameters, including the locations of H atoms, and to better understand the relationship between the pentahydrate and the trihydrate, neutron powder diffraction measurements of both (fully deuterated) phases were carried out at 10 K at the ISIS neutron spallation source, these being complemented with X-ray powder diffraction measurements and Raman spectroscopy. At 10 K, glycine magnesium sulfate pentahydrate, structurally described by the `double' formula [Gly(d5)·MgSO4·5D2O]2, is triclinic (space group P-1, Z = 1), and glycine magnesium sulfate trihydrate, which may be described by the formula Gly(d5)·MgSO4·3D2O, is monoclinic (space group P21/n, Z = 4). In the pentahydrate, there are two symmetry-inequivalent MgO6 octahedra on sites of -1 symmetry and two SO4 tetrahedra with site symmetry 1. The octahedra comprise one [tetraaquadiglcyinemagnesium](2+) ion (centred on Mg1) and one [hexaaquamagnesium](2+) ion (centred on Mg2), and the glycine zwitterion, NH3(+)CH2COO(-), adopts a monodentate coordination to Mg2. In the

  7. Probing the Orientation of Electrostatically Immobilized Protein G B1 by Time of Flight Secondary Ion Spectrometry, Sum Frequency Generation and Near-edge X-Ray Adsorption Fine Structure Spectroscopy

    PubMed Central

    Baio, Joe E.; Weidner, Tobias; Baugh, Loren; Gamble, Lara J.; Stayton, Patrick S.; Castner, David G.

    2011-01-01

    To fully develop techniques that provide an accurate description of protein structure at a surface, we must start with a relatively simple model system before moving on to increasingly complex systems. In this study, x-ray photoelectron spectroscopy (XPS), sum frequency generation spectroscopy (SFG), near-edge x-ray adsorption fine structure (NEXAFS) spectroscopy, and time-of-flight secondary ion mass spectrometry (ToF-SIMS) were used to probe the orientation of Protein G B1 (6 kDa) immobilized onto both amine (NH3+) and carboxyl (COO−) functionalized gold. Previously, we have shown that we could successful control orientation of a similar Protein G fragment via a cysteine-maleimide bond. In this investigation, to induce opposite end-on orientations, a charge distribution was created within the Protein G B1 fragment by first substituting specific negatively charged amino acids with neutral amino acids and then immobilizing the protein onto two oppositely charged self-assembled monolayer (SAM) surfaces (NH3+ and COO−). Protein coverage, on both surfaces, was monitored by the change in the atomic % N, as determined by XPS. Spectral features within the SFG spectra, acquired for the protein adsorbed onto a NH3+-SAM surface, indicates that this electrostatic interaction does induce the protein to form an oriented monolayer on the SAM substrate. This corresponded to the polarization dependence of the spectral feature related to the NEXAFS N1s to π* transition of the β-sheet peptide bonds within the protein layer. ToF-SIMS data demonstrated a clear separation between the two samples based on the intensity differences of secondary ions stemming from amino acids located asymmetrically within Protein G B1 (Methionine: 62 and 105 m/z; Tyrosine: 107 and 137 m/z; Leucine: 86 m/z). For a more quantitative examination of orientation, we developed a ratio comparing the sum of the intensities of secondary-ions stemming from the amino acid residues at either end of the protein

  8. Hard X-Ray Emission of X-Ray Bursters

    NASA Technical Reports Server (NTRS)

    Kaaret, P.

    1999-01-01

    The primary goal of this proposal was to perform an accurate measurement of the broadband x-ray spectrum of a neutron-star low-mass x-ray binary found in a hard x-ray state. This goal was accomplished using data obtained under another proposal, which has provided exciting new information on the hard x-ray emission of neutron-star low-mass x-ray binaries. In "BeppoSAX Observations of the Atoll X-Ray Binary 4U0614+091", we present our analysis of the spectrum of 4U0614+091 over the energy band from 0.3-150 keV. Our data confirm the presence of a hard x-ray tail that can be modeled as thermal Comptonization of low-energy photons on electrons having a very high temperature, greater than 220 keV, or as a non-thermal powerlaw. Such a very hard x-ray spectrum has not been previously seen from neutron-star low-mass x-ray binaries. We also detected a spectral feature that can be interpreted as reprocessing, via Compton reflection, of the direct emission by an optically-thick disk and found a correlation between the photon index of the power-law tail and the fraction of radiation reflected which is similar to the correlation found for black hole candidate x-ray binaries and Seyfert galaxies. A secondary goal was to measure the timing properties of the x-ray emission from neutronstar low-mass x-ray binaries in their low/hard states.

  9. Hard X-ray emission from X-ray bursters.

    NASA Astrophysics Data System (ADS)

    Tavani, M.; Liang, E.

    1996-11-01

    Hard X-ray emission from compact objects has been considered a spectral signature of black hole candidates. However, SIGMA and BATSE recently detected transient emission in the energy range 30-200keV from several X-ray bursters (XRBs) believed to contain weakly magnetized neutron stars. At least seven XRBs (including Aquila X-1 and 4U 1608-52) are currently known to produce erratic hard X-ray outbursts with typical durations of several weeks. These results lead us to reconsider theoretical models of high-energy emission from compact objects, and in particular thermal Comptonization models vs. non-thermal models of particle energization and X-ray emission from weakly magnetized neutron stars. We summarize here recent results for magnetic field reconnection models of non-thermal particle acceleration and high-energy emission of accretion disks. For intermediate soft X-ray luminosities below the Eddington limit, non-thermal hard X-ray emission is predicted to have a (broken) power-law spectrum with intensity anticorrelated with the soft X-ray luminosity. Recent GINGA/BATSE data for the XRB 4U 1608-52 are in agreement with the mechanism of emission proposed here: transient hard X-ray emission consistent with a broken power-law spectrum was detected for a sub-Eddington soft X-ray luminosity.

  10. Miniature x-ray source

    DOEpatents

    Trebes, James E.; Stone, Gary F.; Bell, Perry M.; Robinson, Ronald B.; Chornenky, Victor I.

    2002-01-01

    A miniature x-ray source capable of producing broad spectrum x-ray emission over a wide range of x-ray energies. The miniature x-ray source comprises a compact vacuum tube assembly containing a cathode, an anode, a high voltage feedthru for delivering high voltage to the anode, a getter for maintaining high vacuum, a connection for an initial vacuum pump down and crimp-off, and a high voltage connection for attaching a compact high voltage cable to the high voltage feedthru. At least a portion of the vacuum tube wall is highly x-ray transparent and made, for example, from boron nitride. The compact size and potential for remote operation allows the x-ray source, for example, to be placed adjacent to a material sample undergoing analysis or in proximity to the region to be treated for medical applications.

  11. Solar X-ray physics

    SciTech Connect

    Bornmann, P.L. )

    1991-01-01

    Research on solar X-ray phenomena performed by American scientists during 1987-1990 is reviewed. Major topics discussed include solar images observed during quiescent times, the processes observed during solar flares, and the coronal, interplanetary, and terrestrial phenomena associated with solar X-ray flares. Particular attention is given to the hard X-ray emission observed at the start of the flare, the energy transfer to the soft X-ray emitting plasma, the late resolution of the flare as observed in soft X-ray, and the rate of occurrence of solar flares as a function of time and latitude. Pertinent aspects of nonflaring, coronal X-ray emission and stellar flares are also discussed. 175 refs.

  12. Topological X-Rays Revisited

    ERIC Educational Resources Information Center

    Lynch, Mark

    2012-01-01

    We continue our study of topological X-rays begun in Lynch ["Topological X-rays and MRI's," iJMEST 33(3) (2002), pp. 389-392]. We modify our definition of a topological magnetic resonance imaging and give an affirmative answer to the question posed there: Can we identify a closed set in a box by defining X-rays to probe the interior and without…

  13. Adsorption of malachite green on groundnut shell waste based powdered activated carbon

    SciTech Connect

    Malik, R.; Ramteke, D.S. Wate, S.R.

    2007-07-01

    In the present technologically fast changing situation related to waste management practices, it is desirable that disposal of plant waste should be done in a scientific manner by keeping in view economic and pollution considerations. This is only possible when the plant waste has the potential to be used as raw material for some useful product. In the present study, groundnut shell, an agricultural waste, was used for the preparation of an adsorbent by chemical activation using ZnCl{sub 2} under optimized conditions and its comparative characterisation was conducted with commercially available powdered activated carbon (CPAC) for its physical, chemical and adsorption properties. The groundnut shell based powdered activated carbon (GSPAC) has a higher surface area, iodine and methylene blue number compared to CPAC. Both of the carbons were used for the removal of malachite green dye from aqueous solution and the effect of various operating variables, viz. adsorbent dose (0.1-1 g l{sup -1}), contact time (5-120 min) and adsorbate concentrations (100-200 mg l{sup -1}) on the removal of dye, has been studied. The experimental results indicate that at a dose of 0.5 g l{sup -1} and initial concentration of 100 mg l{sup -1}, GSPAC showed 94.5% removal of the dye in 30 min equilibrium time, while CPAC removed 96% of the dye in 15 min. The experimental isotherm data were analyzed using the linearized forms of Freundlich, Langmuir and BET equations to determine maximum adsorptive capacities. The equilibrium data fit well to the Freundlich isotherm, although the BET isotherm also showed higher correlation for both of the carbons. The results of comparative adsorption capacity of both carbons indicate that groundnut shell can be used as a low-cost alternative to commercial powdered activated carbon in aqueous solution for dye removal.

  14. Self-flocculated powdered activated carbon with different oxidation methods and their influence on adsorption behavior.

    PubMed

    Gong, Zailin; Li, Shujin; Ma, Jun; Zhang, Xiangdong

    2016-03-01

    The commercial powdered activated carbon (PAC) has been selectively oxidized by two methods. The two oxidized methods are wet oxidation with ammonium persulfate and thermal treatment after acidification with hydrochloride acid, respectively. The two oxidized PAC were then functionalized with thermoresponsive poly (N-isopropylacrylamide) (PNIPAM) in aqueous solution at ambient temperature. Comparing the two oxidized PAC products and their grafted derivatives, the oxidized PAC modified with thermal treatment after acidification shows larger surface area of 1184 m(2)/g and better adsorption of bisphenol A. Its derivative also exhibits relatively large surface area and adsorption capacity after grafted with PNIPAM. The maximum surface adsorption capacity simulated under Langmuir Models reached 156 mg/g. In addition, the grafted PAC products show self-flocculation behaviors with rapid response to temperature because of the thermal phase transition and entanglement behaviors of PNIPAM. The present study provides a new way to obtain carboxyl-rich activated carbon with large surface area and better adsorption capacity. The retrievable grafted PAC with good self-flocculation effect responsive to temperature will have high potential application in water remediation which requires pre-heating and emergency water treatment in the wild. PMID:26551226

  15. On the crystal structures of Ln{sub 3}MO{sub 7} (Ln=Nd, Sm, Y and M=Sb, Ta)-Rietveld refinement using X-ray powder diffraction data

    SciTech Connect

    Fu, W.T.; IJdo, D.J.W.

    2009-09-15

    We have investigated, using X-ray powder diffraction data, the crystal structures of some fluorite derivatives with the formula Ln{sub 3}MO{sub 7} (Ln=lanthanide or Y and M=Sb and Ta). In these compounds ordering of Ln and M occurs, leading to a parent structure in Cmmm. Tilting of the MO{sub 6} octahedra causes doubling of one of the cubic axes, leading to a number of non-isomorphic subgroups, e.g. Cmcm, Ccmm and Cccm. We have identified an alternative space group Ccmm instead of C222{sub 1} for those compounds containing a medium sized lanthanide or Y and M being Sb or Ta. Interestingly this is an alternative setting for the space group of the structure obtained when Ln is large (Cmcm). However, there tilting of the octahedra is around the a-axis of the parent structure, rather than around the b-axis as it is found in the compounds which we are reporting on here. In one compound, Nd{sub 3}TaO{sub 7}, both tilts occur. The phase transition between the two possible structures is a slow and difficult process above 80 K, allowing both phases to coexist. - Graphical abstract: (a) A projected view of Ln{sub 3}MO{sub 7} along the a-axis showing the ordering of Ln and M cations in the fluoride lattice. Note that the unit cells of the fluorite (dashed line), the parent Cmmm (dashed line) and the Cmcm/Ccmm structures (continuous line) are indicated. (b) Schematic representations of the crystal structures of Y{sub 3}SbO{sub 7} showing SbO{sub 6} octahedra and Y. Oxygens that do not bond to M cations are also shown.

  16. High-resolution synchrotron x-ray powder diffraction study of the incommensurate modulation in the martensite phase of Ni2MnGa: Evidence for nearly 7M modulation and phason broadening

    NASA Astrophysics Data System (ADS)

    Singh, Sanjay; Petricek, V.; Rajput, Parasmani; Hill, Adrian H.; Suard, E.; Barman, S. R.; Pandey, Dhananjai

    2014-07-01

    The modulated structure of the martensite phase of Ni2MnGa is revisited using high-resolution synchrotron x-ray powder diffraction measurements, which reveal higher-order satellite reflections up to the third order and phason broadening of the satellite peaks. The structure refinement, using the (3+1) dimensional superspace group approach, shows that the modulated structure of Ni2MnGa can be described by orthorhombic superspace group Immm(00γ)s00 with lattice parameters a=4.218 61(2)Å,b=5.546 96(3)Å, and c=4.187 63(2) Å, and an incommensurate modulation wave vector q =0.43160(3)c*=(3/7+δ)c*, where δ =0.00303(3) is the degree of incommensuration of the modulated structure. Additional satellite peak broadening, which could not be accounted for in terms of the anisotropic strain broadening based on a lattice parameter distribution, has been modeled in terms of phasons using fourth-rank covariant strain-tensor representation for incommensurate structures. The simulation of single-crystal diffraction patterns from the refined structural parameters unambiguously reveals a rational approximant structure with 7M modulation. The inhomogeneous displacement of different atomic sites on account of incommensurate modulation and the presence of phason broadening clearly rule out the adaptive phase model proposed recently by Kaufmann et al. [S. Kaufmann, U. K. Rößler, O. Heczko, M. Wuttig, J. Buschbeck, L. Schultz, and S. Fähler, Phys. Rev. Lett. 104, 145702 (2010), 10.1103/PhysRevLett.104.145702] and suggest that the modulation in Ni2MnGa originates from soft-mode phonons.

  17. Crystal structure analysis of tetragonal bronzes {beta}-SrTa{sub 2}O{sub 6} and {beta}'-SrTa{sub 2}O{sub 6} by synchrotron x-ray and neutron powder diffraction.

    SciTech Connect

    Lee, E.; Park, C-H.; Shoemaker, D. P.; Avdeev, M.; Kim, Y-I.

    2012-07-01

    Strontium ditantalum oxide SrTa{sub 2}O{sub 6} exists in {alpha}-, {beta}-, and {beta}{prime}-polymorphs. Herein the crystal structures of the latter two were studied using synchrotron X-ray and constant-wavelength neutron powder diffraction. While {beta}{prime}-SrTa{sub 2}O{sub 6} [space group P4/mbm, a = 12.47099(1) {angstrom}, c = 3.898210(5) {angstrom}, V = 606.271(2) {angstrom}{sup 3}, Z = 5] belongs to the regular tetragonal tungsten bronze (TTB) family, it contains locally disordered strontium atoms within the pentagonal channel. {beta}-SrTa{sub 2}O{sub 6} [space group Pnam, a = 12.36603(2) {angstrom}, b = 12.43467(2) {angstrom}, c = 7.72403(1) {angstrom}, V = 1187.705(4) {angstrom}{sup 3}, Z = 10] can be described as an orthorhombic modification of the TTB, where the octahedral tilting distortion effectively alleviates the bonding strains around TaO{sub 6} and SrO{sub 13} polyhedra. For comparison, rynersonite type {alpha}-SrTa{sub 2}O{sub 6} [space group Pnma, a = 11.00610(6) {angstrom}, b = 7.63397(3) {angstrom}, c = 5.62634(3) {angstrom}, V = 472.727(5) {angstrom}{sup 3}, and Z = 4] is built from edge-shared dimer units of TaO{sub 6} octahedra. As measured by diffuse-reflection absorption spectroscopy, {alpha}-, {beta}-, and {beta}{prime}-SrTa{sub 2}O{sub 6} have indirect band gap energies of 4.4, 4.0, and 3.8 eV, respectively.

  18. X-ray Absorption Spectroscopy

    SciTech Connect

    Yano, Junko; Yachandra, Vittal K.

    2009-07-09

    This review gives a brief description of the theory and application of X-ray absorption spectroscopy, both X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS), especially, pertaining to photosynthesis. The advantages and limitations of the methods are discussed. Recent advances in extended EXAFS and polarized EXAFS using oriented membranes and single crystals are explained. Developments in theory in understanding the XANES spectra are described. The application of X-ray absorption spectroscopy to the study of the Mn4Ca cluster in Photosystem II is presented.

  19. 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.

  20. Determination of the adsorptive capacity and adsorption isotherm of vapor-phase mercury chloride on powdered activated carbon using thermogravimetric analysis

    SciTech Connect

    Hsun-Yu Lin; Chung-Shin Yuan; Wei-Ching Chen; Chung-Hsuang Hung

    2006-11-15

    This study investigated the use of thermogravimetric analysis (TGA) to determine the adsorptive capacity and adsorption isotherm of vapor-phase mercury chloride on powdered activated carbon (PAC). The technique is commonly applied to remove mercury-containing air pollutants from gas streams emitted from municipal solid waste incinerators. An alternative form of powdered activated carbon derived from a pyrolyzed tire char was prepared for use herein. The capacity of waste tire-derived PAC to adsorb vapor-phase HgCl{sub 2} was successfully measured using a self-designed TGA adsorption system. Experimental results showed that the maximum adsorptive capacities of HgCl{sub 2} were 1.75, 0.688, and 0.230 mg of HgCl{sub 2} per gram of powdered activated carbon derived from carbon black at 30, 70, and 150{sup o} for 500 {mu}g/m{sup 3} of HgCl{sub 2}, respectively. Four adsorption isotherms obtained using the Langmuir, Freundlich, Redlich-Peterson, and Brunauer-Emmett-eller (BET) models were used to simulate the adsorption of HgCl{sub 2}. The comparison of experimental data associated with the four adsorption isotherms indicated that BET fit the experimental results better than did the other isotherms at 30{sup o}, whereas the Freundlich isotherm fit the experimental results better at 70 and 150{sup o}. Furthermore, the calculations of the parameters associated with Langmuir and Freundlich isotherms revealed that the adsorption of HgCl{sub 2} by PAC-derived carbon black favored adsorption at various HgCl{sub 2} concentrations and temperatures. 35 refs., 7 figs., 3 tabs.

  1. X-ray beam pointer

    NASA Technical Reports Server (NTRS)

    Nelson, C. W.

    1980-01-01

    Inexpensive, readily assembled pointer aims X-ray machine for welded assembly radiographs. Plumb bob used for vertical alinement and yardstick used to visualize X-ray paths were inconvenient and inaccurate. Pointer cuts alinement time by one-half and eliminates necessity of retakes. For 3,000 weld radiographs, pointer will save 300 worker-hours and significant materials costs.

  2. Plug Would Collimate X Rays

    NASA Technical Reports Server (NTRS)

    Anders, Jeffrey E.; Adams, James F.

    1989-01-01

    Device creates narrow, well-defined beam for radiographic measurements of thickness. Cylindrical plug collimates and aligns X rays with respect to through holes in parts. Helps in determination of wall thickness by radiography. Lead absorbs X rays that do not pass axially through central hole. Lead/vinyl seals prevent off-axis rays from passing along periphery of plug.

  3. X-ray based extensometry

    NASA Technical Reports Server (NTRS)

    Jordan, E. H.; Pease, D. M.

    1988-01-01

    A totally new method of extensometry using an X-ray beam was proposed. The intent of the method is to provide a non-contacting technique that is immune to problems associated with density variations in gaseous environments that plague optical methods. X-rays are virtually unrefractable even by solids. The new method utilizes X-ray induced X-ray fluorescence or X-ray induced optical fluorescence of targets that have melting temperatures of over 3000 F. Many different variations of the basic approaches are possible. In the year completed, preliminary experiments were completed which strongly suggest that the method is feasible. The X-ray induced optical fluorescence method appears to be limited to temperatures below roughly 1600 F because of the overwhelming thermal optical radiation. The X-ray induced X-ray fluorescence scheme appears feasible up to very high temperatures. In this system there will be an unknown tradeoff between frequency response, cost, and accuracy. The exact tradeoff can only be estimated. It appears that for thermomechanical tests with cycle times on the order of minutes a very reasonable system may be feasible. The intended applications involve very high temperatures in both materials testing and monitoring component testing. Gas turbine engines, rocket engines, and hypersonic vehicles (NASP) all involve measurement needs that could partially be met by the proposed technology.

  4. X-ray shearing interferometer

    DOEpatents

    Koch, Jeffrey A.

    2003-07-08

    An x-ray interferometer for analyzing high density plasmas and optically opaque materials includes a point-like x-ray source for providing a broadband x-ray source. The x-rays are directed through a target material and then are reflected by a high-quality ellipsoidally-bent imaging crystal to a diffraction grating disposed at 1.times. magnification. A spherically-bent imaging crystal is employed when the x-rays that are incident on the crystal surface are normal to that surface. The diffraction grating produces multiple beams which interfere with one another to produce an interference pattern which contains information about the target. A detector is disposed at the position of the image of the target produced by the interfering beams.

  5. X-Ray Diffraction Apparatus

    NASA Technical Reports Server (NTRS)

    Blake, David F. (Inventor); Bryson, Charles (Inventor); Freund, Friedmann (Inventor)

    1996-01-01

    An x-ray diffraction apparatus for use in analyzing the x-ray diffraction pattern of a sample is introduced. The apparatus includes a beam source for generating a collimated x-ray beam having one or more discrete x-ray energies, a holder for holding the sample to be analyzed in the path of the beam, and a charge-coupled device having an array of pixels for detecting, in one or more selected photon energy ranges, x-ray diffraction photons produced by irradiating such a sample with said beam. The CCD is coupled to an output unit which receives input information relating to the energies of photons striking each pixel in the CCD, and constructs the diffraction pattern of photons within a selected energy range striking the CCD.

  6. X-Ray Tomographic Reconstruction

    SciTech Connect

    Bonnie Schmittberger

    2010-08-25

    Tomographic scans have revolutionized imaging techniques used in medical and biological research by resolving individual sample slices instead of several superimposed images that are obtained from regular x-ray scans. X-Ray fluorescence computed tomography, a more specific tomography technique, bombards the sample with synchrotron x-rays and detects the fluorescent photons emitted from the sample. However, since x-rays are attenuated as they pass through the sample, tomographic scans often produce images with erroneous low densities in areas where the x-rays have already passed through most of the sample. To correct for this and correctly reconstruct the data in order to obtain the most accurate images, a program employing iterative methods based on the inverse Radon transform was written. Applying this reconstruction method to a tomographic image recovered some of the lost densities, providing a more accurate image from which element concentrations and internal structure can be determined.

  7. Focusing X-Ray Telescopes

    NASA Technical Reports Server (NTRS)

    O'Dell, Stephen; Brissenden, Roger; Davis, William; Elsner, Ronald; Elvis, Martin; Freeman, Mark; Gaetz, Terrance; Gorenstein, Paul; Gubarev, Mikhall; Jerlus, Diab; Juda, Michael; Kolodziejczak, Jeffrey; Murray, Stephen; Petre, Robert; Podgorski, William; Ramsey, Brian; Reid, Paul; Saha, Timo; Wolk, Scott; Troller-McKinstry, Susan; Weisskopf, Martin; Wilke, Rudeger; Zhang, William

    2010-01-01

    During the half-century history of x-ray astronomy, focusing x-ray telescopes, through increased effective area and finer angular resolution, have improved sensitivity by 8 orders of magnitude. Here, we review previous and current x-ray-telescope missions. Next, we describe the planned next-generation x-ray-astronomy facility, the International X-ray Observatory (IXO). We conclude with an overview of a concept for the next next-generation facility, Generation X. Its scientific objectives will require very large areas (about 10,000 sq m) of highly-nested, lightweight grazing-incidence mirrors, with exceptional (about 0.1-arcsec) resolution. Achieving this angular resolution with lightweight mirrors will likely require on-orbit adjustment of alignment and figure.

  8. Equilibrium and kinetics study on the adsorption of perfluorooctanoic acid from aqueous solution onto powdered activated carbon.

    PubMed

    Qu, Yan; Zhang, Chaojie; Li, Fei; Bo, Xiaowen; Liu, Guangfu; Zhou, Qi

    2009-09-30

    Powdered activated carbon (PAC) was applied to remove perfluorooctanoic acid (PFOA) from the aqueous PFOA solution in this study. Contact time, adsorbent dose and temperature were analyzed as the effect factors in the adsorption reaction. The contact time of maximum PFOA uptake was around 1h while the sorption removal efficiency increased with the PAC concentrations. And the process of adsorption increased from 303 K to 313 K and then decreased from 313 K to 323 K. Among four applied models, the experimental isotherm data were discovered to follow Langmuir isotherm model more closely. Thermodynamically, adsorption was endothermic because enthalpy, entropy and Gibbs constants were 198.5 kJ/mol, 0.709 kJ/mol/K and negative, respectively, which also indicated that the adsorption process was spontaneous and feasible. From kinetic analysis, the adsorption was suggested to be pseudo-second-order model. The adsorption of PFOA on the PAC was mainly controlled by particle diffusion. PMID:19395160

  9. Use of heat of adsorption to quantify amorphous content in milled pharmaceutical powders.

    PubMed

    Alam, Shamsul; Omar, Mahmoud; Gaisford, Simon

    2014-01-01

    Isothermal calorimetry operated in gas perfusion mode (IGPC) is often used to quantify the amorphous content of pharmaceutical powders. Typically, the calibration line is constructed using the heat of crystallisation as the sample is exposed to high levels of a plasticising vapour. However, since the physical form to which the amorphous fraction crystallises may be dependent on the presence of any crystalline seed, the calibration line is often seen to be non-linear, especially as the amorphous content of the sample approaches 100% w/w. Redesigning the experiment so that the calibration line is constructed with the heat of adsorption is an alternative approach that, because it is not dependent upon crystallisation to a physical form should ameliorate this problem. The two methods are compared for a model compound, salbutamol sulphate, which forms either a hydrate or an anhydrate depending on the amorphous content. The heat of adsorption method was linear between amorphous contents of 0 and 100% w/w and resulted in a detection limit of 0.3% w/w and a quantification limit of 0.92% w/w. The heat of crystallisation method was linear only between amorphous contents of 0 and 80% w/w and resulted in a detection limit of 1.7% w/w and a quantification limit of 5.28% w/w. Thus, the use of heat of adsorption is shown to be a better method for quantifying amorphous contents to better than 1% w/w. PMID:24315924

  10. Crystal structure analysis of tungsten bronzes {beta}-SrTa{sub 2}O{sub 6} and {beta} Prime -SrTa{sub 2}O{sub 6} by synchrotron X-ray and neutron powder diffraction

    SciTech Connect

    Lee, Eunhye; Park, Cheol-Hee; Shoemaker, Daniel P.; Avdeev, Maxim; Kim, Young-Il

    2012-07-15

    Strontium ditantalum oxide SrTa{sub 2}O{sub 6} exists in {alpha}-, {beta}-, and {beta} Prime -polymorphs. Herein the crystal structures of the latter two were studied using synchrotron X-ray and constant-wavelength neutron powder diffraction. While {beta} Prime -SrTa{sub 2}O{sub 6} [space group P4/mbm, a=12.47099(1) A, c=3.898210(5) A, V=606.271(2) Angstrom-Sign {sup 3}, Z=5] belongs to the regular tetragonal tungsten bronze (TTB) family, it contains locally disordered strontium atoms within the pentagonal channel. {beta}-SrTa{sub 2}O{sub 6} [space group Pnam, a=12.36603(2) Angstrom-Sign , b=12.43467(2) A, c=7.72403(1) A, V=1187.705(4) Angstrom-Sign {sup 3}, Z=10] can be described as an orthorhombic modification of the TTB, where the octahedral tilting distortion effectively alleviates the bonding strains around TaO{sub 6} and SrO{sub 13} polyhedra. For comparison, rynersonite type {alpha}-SrTa{sub 2}O{sub 6} [space group Pnma, a=11.00610(6) Angstrom-Sign , b=7.63397(3) Angstrom-Sign , c=5.62634(3) Angstrom-Sign , V=472.727(5) Angstrom-Sign {sup 3}, and Z=4] is built from edge-shared dimer units of TaO{sub 6} octahedra. As measured by diffuse-reflection absorption spectroscopy, {alpha}-, {beta}-, and {beta} Prime -SrTa{sub 2}O{sub 6} have indirect band gap energies of 4.4, 4.0, and 3.8 eV, respectively. - Graphical Abstract: Difference Fourier map for {beta} Prime -SrTa{sub 2}O{sub 6} at z=0. Highlights: Black-Right-Pointing-Pointer Structure refinements of {beta}-SrTa{sub 2}O{sub 6} and {beta} Prime -SrTa{sub 2}O{sub 6}. Black-Right-Pointing-Pointer Strontium disorder in tetragonal tungsten bronze {beta} Prime -SrTa{sub 2}O{sub 6}. Black-Right-Pointing-Pointer Orthorhombic distortion and cell doubling in {beta}-SrTa{sub 2}O{sub 6}.

  11. Solid state 13C-NMR, infrared, X-ray powder diffraction and differential thermal studies of the homologous series of some mono-valent metal (Li, Na, K, Ag) n-alkanoates: A comparative study

    NASA Astrophysics Data System (ADS)

    Nelson, Peter N.; Ellis, Henry A.; White, Nicole A. S.

    2015-06-01

    A comparative study of the molecular packing, lattice structures and phase behaviors of the homologous series of some mono-valent metal carboxylates (Li, Na, K and Ag) is carried out via solid state FT-infrared and 13C-NMR spectroscopes, X-rays powder diffraction, density measurements, differential scanning calorimetry, polarizing light microscopy and variable temperature infrared spectroscopy. It is proposed that, for lithium, sodium and potassium carboxylates, metal-carboxyl coordination is via asymmetric chelating bidentate bonding with extensive intermolecular interactions to form tetrahedral metal centers, irrespective of chain length. However, for silver n-alkanoates, carboxyl moieties are bound to silver ions via syn-syn type bridging bidentate coordination to form dimeric units held together by extensive head group inter-molecular interactions. Furthermore, the fully extended hydrocarbon chains which are crystallized in the all-trans conformation are tilted at ca. 30°, 27°, 15° and 31° with respect to a normal to the metal plane, for lithium, sodium, silver and potassium carboxylates, respectively. All compounds are packed as lamellar bilayer structures, however, lithium compounds are crystallized in a triclinic crystal system whilst silver, sodium and potassium n-alkanoates are all monoclinic with possible P1 bravais lattice. Odd-even alternation observed in various physical features is associated with different inter-planar spacing between closely packed layers in the bilayer which are not in the same plane; a phenomenon controlled by lattice packing symmetry requirements. All compounds, except silver carboxylates, show partially reversibly first order pre-melting transitions; the number of which increases with increasing chain length. These transitions are associated, for the most part, with lamellar collapse followed by increased gauche-trans isomerism in the methylene group assembly, irrespective of chain length. It is proposed that the absence of

  12. Structural characterization of Bi{sub 2}Te{sub 3} and Sb{sub 2}Te{sub 3} as a function of temperature using neutron powder diffraction and extended X-ray absorption fine structure techniques

    SciTech Connect

    Mansour, A. N.; Wong-Ng, W.; Huang, Q.; Tang, W.; Thompson, A.; Sharp, J.

    2014-08-28

    The structure of Bi{sub 2}Te{sub 3} (Seebeck coefficient Standard Reference Material (SRM™ 3451)) and the related phase Sb{sub 2}Te{sub 3} have been characterized as a function of temperature using the neutron powder diffraction (NPD) and the extended X-ray absorption fine structure (EXAFS) techniques. The neutron structural studies were carried out from 20 K to 300 K for Bi{sub 2}Te{sub 3} and from 10 K to 298 K for Sb{sub 2}Te{sub 3}. The EXAFS technique for studying the local structure of the two compounds was conducted from 19 K to 298 K. Bi{sub 2}Te{sub 3} and Sb{sub 2}Te{sub 3} are isostructural, with a space group of R3{sup ¯}m. The structure consists of repeated quintuple layers of atoms, Te2-M-Te1-M-Te2 (where M = Bi or Sb) stacking along the c-axis of the unit cell. EXAFS was used to examine the bond distances and static and thermal disorders for the first three shells of Bi{sub 2}Te{sub 3} and Sb{sub 2}Te{sub 3} as a function of temperature. The temperature dependencies of thermal disorders were analyzed using the Debye and Einstein models for lattice vibrations. The Debye and Einstein temperatures for the first two shells of Bi{sub 2}Te{sub 3} are similar to those of Sb{sub 2}Te{sub 3} within the uncertainty in the data. However, the Debye and Einstein temperatures for the third shell of Bi-Bi are significantly lower than those of the third shell of Sb-Sb. The Einstein temperature for the third shell is consistent with a soft phonon mode in both Bi{sub 2}Te{sub 3} and Sb{sub 2}Te{sub 3}. The lower Einstein temperature of Bi-Bi relative to Sb-Sb is consistent with the lower value of thermal conductivity of Bi{sub 2}Te{sub 3} relative to Sb{sub 2}Te{sub 3}.

  13. {sup 27}Al and {sup 23}Na MAS NMR and powder x-ray diffraction studies of sodium aluminate speciation and the mechanistics of aluminum hydroxide precipitation upon acid hydrolysis

    SciTech Connect

    Bradley, S.M.; Hanna, J.V.

    1994-08-24

    {sup 27}Al and {sup 23}Na MAS NMR, powder X-ray diffraction, and infrared spectroscopic investigations of freeze-dried sodium aluminates and aluminum hydroxides formed through acid hydrolysis have been undertaken, with OH/Al hydrolysis ratios between 5.3 and 2.8 being analyzed. Numerous {sup 27}AlNMR resonances were observed, the intensities of which vary as a function of OH/Al ratio, and these have been assigned to four-, five-, and six-coordinate aluminum species constituting a variety of structural moieties. The dominant species at an OH/Al ratio above 4.4 appears to be a Q{sup o}Na[Al(OH);{sub 4}] salt, as indicated by a {sup 27}Al resonance at 86.6 ppm. In addition, a second, broader resonance at 71.3 ppm demonstrates the simultaneous existence of further four-coordinate aluminum species linked thorough oxo bonds to other four-coordinate aluminums (e.g., Q{sup 2} [Al(OH);{sub 2}(OAl){sub 2}];{sup x-}). At an OH/Al ratio between 4.4 and 4.1, a water-soluble phase forms that contains both four- and six-coordinate aluminum. At OH/Al ratios fo 4.0 and below, a water-soluble phase forms that contains both four-and six-coordinate aluminum. AT OH/Al ratios of 4.0 and below, a water-insoluble phase exists possessing four-, five-, and six-coordinate aluminum. At OH/Al{le}3.9 range exhibits {sup 27}Al chemical shifts similar to those reported for transitional aluminas such as {gamma}-, {eta}-, and 0-Al{sub 2}O{sub 3} and an infrared spectrum similar to pseudo-spinel gels, suggesting that a pseudo-spinel intermediate is the first phase involved in the crystallization of gibbsite. The resonance assigned to five-coordinate aluminum probably results from species involved in the transformation of the pseudo-spinal phase to pseudo-boehmite. The formation of gibbssite on the acid hydrolysis of alkaline sodium aluminate solutions thus appears to follow the pathway pseudo-spinel {r_arrow} pseudo-boehmite {r_arrow} bayerite {r_arrow} gibbsite. 82 refs., 7 figs., 3 tabs.

  14. Removal of N-nitrosodimethylamine precursors with powdered activated carbon adsorption.

    PubMed

    Beita-Sandí, Wilson; Ersan, Mahmut Selim; Uzun, Habibullah; Karanfil, Tanju

    2016-01-01

    The main objective of this study was to examine the roles of powdered activated carbon (PAC) characteristics (i.e., surface chemistry, pore size distribution, and surface area) in the removal of N-nitrosodimethylamine (NDMA) formation potential (FP) in surface and wastewater-impacted waters. Also, the effects of natural attenuation of NDMA precursors in surface waters, NDMA FP concentration, and carbon dose on the removal of NDMA FP by PAC were evaluated. Finally, the removal of NDMA FP by PAC at two full-scale DWTPs was monitored. Wastewater-impacted and surface water samples were collected to conduct adsorption experiments using different PACs and activated carbon fibers (ACFs) with a wide range of physicochemical characteristics. The removal efficiency of NDMA FP by PAC was significantly higher in wastewater-impacted than surface waters. Adsorbable NDMA precursors showed a size distribution in the waters tested; the adsorbable fraction included precursors accessing the pore size regions of 10-20 Å and <10 Å. Basic carbons showed higher removal of NDMA FP than acidic carbons on a surface area basis. The overall removal of NDMA FP by PAC on a mass basis depended on the surface area, pore size distribution and pHPZC. Thus, PACs with hybrid characteristics (micro and mesoporous), higher surface areas, and basic surface chemistry are more likely to be effective for NDMA precursor control by PAC adsorption. The application of PAC in DWTPs for taste and odor control resulted in an additional 20% removal of NDMA FP for the PAC doses of 7-10 mg/L. The natural attenuation of NDMA precursors through a combination of processes (biodegradation, photolysis and adsorption) decreased their adsorbability and removal by PAC adsorption. PMID:26584342

  15. Removal of Cr(III) from chrome tanning wastewater by adsorption using two natural carbonaceous materials: Eggshell and powdered marble.

    PubMed

    Elabbas, Saliha; Mandi, Laila; Berrekhis, Fatima; Pons, Marie Noelle; Leclerc, Jean Pierre; Ouazzani, Naaila

    2016-01-15

    In the present paper, eggshell and powdered marble, two carbonaceous materials, were used to remove Cr(III) ions from a real chrome tanning wastewater. The effects of initial effluent pH, adsorbent dose, contact time and temperature were studied. The maximum uptake of chromium ions was obtained at pH 5.0 with the dose 20 g L(-1) and 12 g L(-1) for eggshell and powdered marble respectively. Adsorption equilibrium was reached after 14 h contact time for eggshell and only after 30 min for powdered marble. Under these conditions, almost 99% Cr(III) was removed from chrome tanning wastewater having an initial concentration of chromium of 3.21 g L(-1). Kinetic data were satisfactorily described by a pseudo-second order chemical sorption model. The equilibrium rate constant was notably greater for powdered marble than for eggshell with 1.142·10(-3) (g mg(-1) min(-1)) and 0.041·10(-3) (g mg(-1) min(-1)) respectively. The adsorption isotherm were well described by a Langmuir model and showed that the interaction of chromium with the two adsorbents surface is a localized monolayer adsorption with a smaller energy constant for the powdered marble than for eggshell (0.020 (L mg(-1)) and 0.083 (L mg(-1)) respectively). The powdered marble was able to adsorb faster a large amount of Cr (III) in comparison to eggshell. The use of a standardized lettuce seed bioassay allowed evaluating a better effectiveness of the Cr adsorption on the powdered marble, removing up to 40% of the treated effluent toxicity than by eggshell 25%. The powdered marble could be considered as an effective, low cost carbonaceous material to be used for chromium removal from tanning wastewater. PMID:26598282

  16. X-Ray Imaging System

    NASA Astrophysics Data System (ADS)

    1986-01-01

    The FluoroScan Imaging System is a high resolution, low radiation device for viewing stationary or moving objects. It resulted from NASA technology developed for x-ray astronomy and Goddard application to a low intensity x-ray imaging scope. FlouroScan Imaging Systems, Inc, (formerly HealthMate, Inc.), a NASA licensee, further refined the FluoroScan System. It is used for examining fractures, placement of catheters, and in veterinary medicine. Its major components include an x-ray generator, scintillator, visible light image intensifier and video display. It is small, light and maneuverable.

  17. X-ray burst sources

    NASA Technical Reports Server (NTRS)

    Lewin, W. H. G.

    1986-01-01

    There are about 100 bright X-ray sources in the Galaxy that are accretion-driven systems composed of a neutron star and a low mass companion that fills its critical Roche lobe. Many of these systems generate recurring X-ray bursts that are the result of thermonuclear flashes in the neutron star's surface layers, and are accompanied by a somewhat delayed optical burst due to X-ray heating of accretion disk. The Rapid Burster discovered in 1976 exhibits an interval between bursts that is strongly correlated with the energy in the preceding burst. There is no optical identification for this object.

  18. Miniature x-ray source

    DOEpatents

    Trebes, James E.; Bell, Perry M.; Robinson, Ronald B.

    2000-01-01

    A miniature x-ray source utilizing a hot filament cathode. The source has a millimeter scale size and is capable of producing broad spectrum x-ray emission over a wide range of x-ray energies. The miniature source consists of a compact vacuum tube assembly containing the hot filament cathode, an anode, a high voltage feedthru for delivering high voltage to the cathode, a getter for maintaining high vacuum, a connector for initial vacuum pump down and crimp-off, and a high voltage connection for attaching a compact high voltage cable to the high voltage feedthru. At least a portion of the vacuum tube wall is fabricated from highly x-ray transparent materials, such as sapphire, diamond, or boron nitride.

  19. Imaging X-ray spectrometer

    NASA Astrophysics Data System (ADS)

    Grant, P. A.; Jackson, J. W., Jr.; Alcorn, G. E.; Marshall, F. E.

    1984-09-01

    An X-ray spectrometer for providing imaging and energy resolution of an X-ray source is described. This spectrometer is comprised of a thick silicon wafer having an embedded matrix or grid of aluminum completely through the wafer fabricated, for example, by thermal migration. The aluminum matrix defines the walls of a rectangular array of silicon X-ray detector cells or pixels. A thermally diffused aluminum electrode is also formed centrally through each of the silicon cells with biasing means being connected to the aluminum cell walls and causes lateral charge carrier depletion between the cell walls so that incident X-ray energy causes a photoelectric reaction within the silicon producing collectible charge carriers in the form of electrons which are collected and used for imaging.

  20. Abdomen X-Ray (Radiography)

    MedlinePlus

    ... have very controlled x-ray beams and dose control methods to minimize stray (scatter) radiation. This ensures that those parts of a patient's body not being imaged receive minimal radiation exposure. top ...

  1. Picosecond x-ray science.

    SciTech Connect

    Landahl, E.; Reis, D.; Wang, J.; Young, L.

    2006-01-01

    The report discusses the exciting times for short pulse X-rays and the current users of the technology in the United States. Tracking nuclear motions with X-rays transcends scientific disciplines and includes Biology, Materials Science, Condensed Matter and Chemistry. 1 picosecond accesses many phenomena previously hidden at 100ps. Synchrotron advantage over laser plasma and LCLS is that it's easily tunable. There is a large and diverse user community of this technology that is growing rapidly. A working group is being formed to implement 'fast track' Phases 1 and 2 which includes tunable, polarized, monochromatic, focused X-rays; variable pulse length (1 to 100ps) and 1 kHz, 10{sup 9} X-rays/s with 1% bandwidth. ERL would be a major advance for ultrafast time-resolved studies.

  2. X-ray microtomographic scanners

    SciTech Connect

    Syryamkin, V. I. Klestov, S. A.

    2015-11-17

    The article studies the operating procedures of an X-ray microtomographic scanner and the module of reconstruction and analysis 3D-image of a test sample in particular. An algorithm for 3D-image reconstruction based on image shadow projections and mathematical methods of the processing are described. Chapter 1 describes the basic principles of X-ray tomography and general procedures of the device developed. Chapters 2 and 3 are devoted to the problem of resources saving by the system during the X-ray tomography procedure, which is achieved by preprocessing of the initial shadow projections. Preprocessing includes background noise removing from the images, which reduces the amount of shadow projections in general and increases the efficiency of the group shadow projections compression. In conclusion, the main applications of X-ray tomography are presented.

  3. X-Ray Exam: Finger

    MedlinePlus

    ... KidsHealth in the Classroom What Other Parents Are Reading Upsetting News Reports? What to Say Vaccines: Which ... Results A radiologist, a doctor specially trained in reading and interpreting X-ray images, will look at ...

  4. X-Ray Exam: Hip

    MedlinePlus

    ... KidsHealth in the Classroom What Other Parents Are Reading Upsetting News Reports? What to Say Vaccines: Which ... For older kids, be sure to explain the importance of keeping still while the X-ray is ...

  5. X-Ray Exam: Foot

    MedlinePlus

    ... KidsHealth in the Classroom What Other Parents Are Reading Upsetting News Reports? What to Say Vaccines: Which ... For older kids, be sure to explain the importance of staying still while the X-ray is ...

  6. X-Ray Exam: Ankle

    MedlinePlus

    ... KidsHealth in the Classroom What Other Parents Are Reading Upsetting News Reports? What to Say Vaccines: Which ... For older kids, be sure to explain the importance of staying still while the X-ray is ...

  7. X-Ray Exam: Pelvis

    MedlinePlus

    ... KidsHealth in the Classroom What Other Parents Are Reading Upsetting News Reports? What to Say Vaccines: Which ... For older kids, be sure to explain the importance of keeping still while the X-ray is ...

  8. X-Ray Exam: Forearm

    MedlinePlus

    ... KidsHealth in the Classroom What Other Parents Are Reading Upsetting News Reports? What to Say Vaccines: Which ... For older kids, be sure to explain the importance of staying still while the X-ray is ...

  9. X-Ray Exam: Wrist

    MedlinePlus

    ... KidsHealth in the Classroom What Other Parents Are Reading Upsetting News Reports? What to Say Vaccines: Which ... For older kids, be sure to explain the importance of staying still while the X-ray is ...

  10. Imaging X-ray spectrometer

    NASA Technical Reports Server (NTRS)

    Grant, P. A.; Jackson, J. W., Jr.; Alcorn, G. E.; Marshall, F. E. (Inventor)

    1984-01-01

    An X-ray spectrometer for providing imaging and energy resolution of an X-ray source is described. This spectrometer is comprised of a thick silicon wafer having an embedded matrix or grid of aluminum completely through the wafer fabricated, for example, by thermal migration. The aluminum matrix defines the walls of a rectangular array of silicon X-ray detector cells or pixels. A thermally diffused aluminum electrode is also formed centrally through each of the silicon cells with biasing means being connected to the aluminum cell walls and causes lateral charge carrier depletion between the cell walls so that incident X-ray energy causes a photoelectric reaction within the silicon producing collectible charge carriers in the form of electrons which are collected and used for imaging.

  11. X-ray astronomical spectroscopy

    NASA Technical Reports Server (NTRS)

    Holt, S. S.

    1980-01-01

    The current status of the X-ray spectroscopy of celestial X-ray sources, ranging from nearby stars to distant quasars, is reviewed. Particular emphasis is placed on the role of such spectroscopy as a useful and unique tool in the elucidation of the physical parameters of the sources. The spectroscopic analysis of degenerate and nondegenerate stellar systems, galactic clusters and active galactic nuclei, and supernova remnants is discussed.

  12. Electromechanical x-ray generator

    DOEpatents

    Watson, Scott A; Platts, David; Sorensen, Eric B

    2016-05-03

    An electro-mechanical x-ray generator configured to obtain high-energy operation with favorable energy-weight scaling. The electro-mechanical x-ray generator may include a pair of capacitor plates. The capacitor plates may be charged to a predefined voltage and may be separated to generate higher voltages on the order of hundreds of kV in the AK gap. The high voltage may be generated in a vacuum tube.

  13. Bisphenol A removal by combination of powdered activated carbon adsorption and ultrafiltration

    NASA Astrophysics Data System (ADS)

    Wang, Rongchang; Tong, Hao; Xia, Siqing; Zhang, Yalei; Zhao, Jianfu

    2010-11-01

    Bisphenol A (BPA) removal from surface water in the presence of natural organic matter (NOM) by combination of powdered activated carbon (PAC) adsorption and ultrafiltration (UF) was investigated in this study. It was especially focused on the effects of various factors on BPA removal, such as PAC dosage, NOM concentration and pH value. BPA removal by UF+PAC process increased sharply from 4% to 92%, when PAC dosage increased from 0 to 120 mg/L. The optimal PAC dosage was determined to be 30 mg/L. The results also showed that BPA retention was slightly favored in the presence of NOM. As pH increased from 7.0 to 10.5, BPA removal substantially decreased from 90% to 59%. PAC+UF process is recommended to be used as an emergence facility in drinking water treatment, especially when an accidental spilling of deleterious substance, e.g., BPA, in the water resources happens.

  14. Operando X-ray absorption and infrared fuel cell spectroscopy

    SciTech Connect

    Lewis, Emily A.; Kendrick, Ian; Jia, Qingying; Grice, Corey; Segre, Carlo U.; Smotkin, Eugene S.

    2011-11-17

    A polymer electrolyte fuel cell enables operando X-ray absorption and infrared spectroscopy of the membrane electrode assembly catalytic layer with flowing fuel and air streams at controlled temperature. Time-dependent X-ray absorption near edge structure spectra of the Pt and Ni edge of Pt based catalysts of an air-breathing cathode show that catalyst restructuring, after a potential step, has time constants from minutes to hours. The infrared Stark tuning plots of CO adsorbed on Pt at 100, 200, 300 and 400 mV vs. hydrogen reference electrode were obtained. The Stark tuning plots of CO adsorbed at 400 mV exhibit a precipitous drop in frequency coincident with the adsorption potential. The turn-down potential decreases relative to the adsorption potential and is approximately constant after 300 mV. These Stark tuning characteristics are attributed to potential dependent adsorption site selection by CO and competitive adsorption processes.

  15. X-Rays, Pregnancy and You

    MedlinePlus

    ... and Procedures Medical Imaging Medical X-ray Imaging X-Rays, Pregnancy and You Share Tweet Linkedin Pin it ... the decision with your doctor. What Kind of X-Rays Can Affect the Unborn Child? During most x- ...

  16. Why Do I Need X-Rays?

    MedlinePlus

    ... to your desktop! more... Why Do I Need X-Rays? Article Chapters Why Do I Need X-Rays? ... of tooth decay. Updated: January 2012 Related Articles: X-Rays The Academy of General Dentistry (AGD) Sets the ...

  17. Understanding the adsorption mechanism of noble gases Kr and Xe in CPO-27-Ni, CPO-27-Mg, and ZIF-8.

    PubMed

    Magdysyuk, O V; Adams, F; Liermann, H-P; Spanopoulos, I; Trikalitis, P N; Hirscher, M; Morris, R E; Duncan, M J; McCormick, L J; Dinnebier, R E

    2014-11-21

    An experimental study of Xe and Kr adsorption in metal-organic frameworks CPO-27-Ni, CPO-27-Mg, and ZIF-8 was carried out. In situ synchrotron X-ray powder diffraction experiments allowed precise determination of the adsorption sites and sequence of their filling with increasing of gas pressure at different temperatures. Structural investigations were used for interpretation of gas adsorption measurements. PMID:25277596

  18. Nanometer x-ray lithography

    NASA Astrophysics Data System (ADS)

    Hartley, Frank T.; Khan Malek, Chantal G.

    1999-10-01

    New developments for x-ray nanomachining include pattern transfer onto non-planar surfaces coated with electrodeposited resists using synchrotron radiation x-rays through extremely high-resolution mask made by chemically assisted focused ion beam lithography. Standard UV photolithographic processes cannot maintain sub-micron definitions over large variation in feature topography. The ability of x-ray printing to pattern thin or thick layers of photoresist with high resolution on non-planar surfaces of large and complex topographies with limited diffraction and scattering effects and no substrate reflection is known and can be exploited for patterning microsystems with non-planar 3D geometries as well as multisided and multilayered substrates. Thin conformal coatings of electro-deposited positive and negative tone photoresist have been shown to be x-ray sensitive and accommodate sub-micro pattern transfer over surface of extreme topographical variations. Chemically assisted focused ion beam selective anisotropic erosion was used to fabricate x-ray masks directly. Masks with feature sizes less than 20 nm through 7 microns of gold were made on bulk silicon substrates and x-ray mask membranes. The technique is also applicable to other high density materials. Such masks enable the primary and secondary patterning and/or 3D machining of Nano-Electro-Mechanical Systems over large depths or complex relief and the patterning of large surface areas with sub-optically dimensioned features.

  19. Universal x-ray unit

    SciTech Connect

    Charrier, P.

    1988-04-26

    An X-ray apparatus capable of X-ray beaming in a multiplicity of directions around and through the body of a horizontally lying stationary patient is described comprising: a horizontal patient's table; a ring in circumscribing position around the table; a X-ray equipment fixedly mounted on the ring for X-ray beaming through the table and through the body of a patient when lying thereon, the X-ray equipment comprising a source of X-rays; support means for holding the ring in the circumscribing position and first drive means on the support means and on the ring for rotating the ring about a first axis perpendicular to the general plane of the ring through the ring center; a suspension member having downwardly extending side legs, second drive means for oscillating the ring support means and the ring together in unison about the second axis; a frame having a top structure above the table, the ring and the suspension member; and a carrier assembly mounted on the top structure and at the center of the suspension member.

  20. Cosmic X-ray physics

    NASA Technical Reports Server (NTRS)

    Mccammon, D.; Cox, D. P.; Kraushaar, W. L.; Sanders, W. T.

    1985-01-01

    A progress report of research activities carried out in the area of cosmic X-ray physics is presented. The Diffuse X-ray Spectrometer DXS which has been flown twice as a rocket payload is described. The observation times proved to be too small for meaningful X-ray data to be obtained. Data collection and reduction activities from the Ultra-Soft X-ray background (UXT) instrument are described. UXT consists of three mechanically-collimated X-ray gas proportional counters with window/filter combinations which allow measurements in three energy bands, Be (80-110 eV), B (90-187 eV), and O (e84-532 eV). The Be band measurements provide an important constraint on local absorption of X-rays from the hot component of the local interstellar medium. Work has also continued on the development of a calorimetric detector for high-resolution spectroscopy in the 0.1 keV - 8keV energy range.

  1. Center for X-Ray Optics, 1992

    SciTech Connect

    Not Available

    1993-08-01

    This report discusses the following topics: Center for X-Ray Optics; Soft X-Ray Imaging wit Zone Plate Lenses; Biological X-Ray microscopy; Extreme Ultraviolet Lithography for Nanoelectronic Pattern Transfer; Multilayer Reflective Optics; EUV/Soft X-ray Reflectometer; Photoemission Microscopy with Reflective Optics; Spectroscopy with Soft X-Rays; Hard X-Ray Microprobe; Coronary Angiography; and Atomic Scattering Factors.

  2. Characteristics of competitive adsorption between 2-methylisoborneol and natural organic matter on superfine and conventionally sized powdered activated carbons.

    PubMed

    Matsui, Yoshihiko; Yoshida, Tomoaki; Nakao, Soichi; Knappe, Detlef R U; Matsushita, Taku

    2012-10-01

    When treating water with activated carbon, natural organic matter (NOM) is not only a target for adsorptive removal but also an inhibitory substance that reduces the removal efficiency of trace compounds, such as 2-methylisoborneol (MIB), through adsorption competition. Recently, superfine (submicron-sized) activated carbon (SPAC) was developed by wet-milling commercially available powdered activated carbon (PAC) to a smaller particle size. It was reported that SPAC has a larger NOM adsorption capacity than PAC because NOM mainly adsorbs close to the external adsorbent particle surface (shell adsorption mechanism). Thus, SPAC with its larger specific external surface area can adsorb more NOM than PAC. The effect of higher NOM uptake on the adsorptive removal of MIB has, however, not been investigated. Results of this study show that adsorption competition between NOM and MIB did not increase when NOM uptake increased due to carbon size reduction; i.e., the increased NOM uptake by SPAC did not result in a decrease in MIB adsorption capacity beyond that obtained as a result of NOM adsorption by PAC. A simple estimation method for determining the adsorbed amount of competing NOM (NOM that reduces MIB adsorption) is presented based on the simplified equivalent background compound (EBC) method. Furthermore, the mechanism of adsorption competition is discussed based on results obtained with the simplified EBC method and the shell adsorption mechanism. Competing NOM, which likely comprises a small portion of NOM, adsorbs in internal pores of activated carbon particles as MIB does, thereby reducing the MIB adsorption capacity to a similar extent regardless of adsorbent particle size. SPAC application can be advantageous because enhanced NOM removal does not translate into less effective removal of MIB. Molecular size distribution data of NOM suggest that the competing NOM has a molecular weight similar to that of the target compound. PMID:22763287

  3. Adsorption of ciprofloxacin, bisphenol and 2-chlorophenol on electrospun carbon nanofibers: in comparison with powder activated carbon.

    PubMed

    Li, Xiaona; Chen, Shuo; Fan, Xinfei; Quan, Xie; Tan, Feng; Zhang, Yaobin; Gao, Jinsuo

    2015-06-01

    Carbon nanofibers (CNFs) were prepared by electrospun polyacrylonitrile (PAN) polymer solutions followed by thermal treatment. For the first time, the influence of stabilization procedure on the structure properties of CNFs was explored to improve the adsorption capacity of CNFs towards the environmental pollutants from aqueous solution. The adsorption of three organic chemicals including ciprofloxacin (CIP), bisphenol (BPA) and 2-chlorophenol (2-CP) on electrospun CNFs with high surface area of 2326m(2)/g and micro/mesoporous structure characteristics were investigated. The adsorption affinities were compared with that of the commercial powder activated carbon (PAC). The adsorption kinetics and isotherms showed that the maximum adsorption capacities (qm) of CNFs towards the three pollutants are sequenced in the order of CIP>BPA>2-CP, which are 2.6-fold (CIP), 1.6-fold (BPA) and 1.1-fold (2-CP) increase respectively in comparison with that of PAC adsorption. It was assumed that the micro/mesoporous structure of CNFs, molecular size of the pollutants and the π electron interaction play important roles on the high adsorption capacity exhibited by CNFs. In addition, electrostatic interaction and hydrophobic interaction also contribute to the adsorption of CNFs. This study demonstrates that the electrospun CNFs are promising adsorbents for the removal of pollutants from aqueous solutions. PMID:25702869

  4. 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.

  5. Structure determination of a complex tubular uranyl phenylphosphonate, (UO{sub 2}){sub 3}(HO{sub 3}PC{sub 6}H{sub 5}){sub 2}(O{sub 3}PC{sub 6}H{sub 5}){sub 2}{center_dot}H{sub 2}O, from conventional x-ray powder diffraction data

    SciTech Connect

    Poojary, D.M.; Cabeza, A.; Aranda, A.G.

    1996-03-13

    The three-dimensional structure of a complex tubular uranyl phosphonate, (UO{sub 2}){sub 3}(HO{sub 3}PC{sub 6}H{sub 5}){sub 2}(O{sub 3}PC{sub 6}H{sub 5}){sub 2}(O{sub 3}PC{sub 6}H{sub 5}){sub 2} {center_dot} H{sub 2}O, was determined ab initio from laboratory X-ray powder diffraction data and refined by the Rietveld method. The crystals belong to the space group P2{sub 1}2{sub 1}2{sub 1}, with {alpha} = 17.1966(2) {Angstrom}, b = 7.2125(2) {Angstrom}, c = 27.8282(4) {Angstrom}, and Z = 4. The structure consists of three independent uranium atoms, among which two are seven-coordinated and the third is eight-coordinated. These metal atoms are connected by four different phosphonate groups to form a one-dimensional channel structure along the b axis. The phenyl groups are arranged on the outer periphery of the channels, and their stacking forces keep the channels intact in the lattice. The determination of this structure which contains 50 non-hydrogen atoms in the asymmetric unit, from conventional X-ray powder data, represents significant progress in the application of powder techniques to structure of complex inorganic compounds, including organometallic compounds.

  6. X-ray Echo Spectroscopy.

    PubMed

    Shvyd'ko, Yuri

    2016-02-26

    X-ray echo spectroscopy, a counterpart of neutron spin echo, is being introduced here to overcome limitations in spectral resolution and weak signals of the traditional inelastic x-ray scattering (IXS) probes. An image of a pointlike x-ray source is defocused by a dispersing system comprised of asymmetrically cut specially arranged Bragg diffracting crystals. The defocused image is refocused into a point (echo) in a time-reversal dispersing system. If the defocused beam is inelastically scattered from a sample, the echo signal acquires a spatial distribution, which is a map of the inelastic scattering spectrum. The spectral resolution of the echo spectroscopy does not rely on the monochromaticity of the x rays, ensuring strong signals along with a very high spectral resolution. Particular schemes of x-ray echo spectrometers for 0.1-0.02 meV ultrahigh-resolution IXS applications (resolving power >10^{8}) with broadband ≃5-13  meV dispersing systems are introduced featuring more than 10^{3} signal enhancement. The technique is general, applicable in different photon frequency domains. PMID:26967404

  7. X-ray Echo Spectroscopy

    NASA Astrophysics Data System (ADS)

    Shvyd'ko, Yuri

    2016-02-01

    X-ray echo spectroscopy, a counterpart of neutron spin echo, is being introduced here to overcome limitations in spectral resolution and weak signals of the traditional inelastic x-ray scattering (IXS) probes. An image of a pointlike x-ray source is defocused by a dispersing system comprised of asymmetrically cut specially arranged Bragg diffracting crystals. The defocused image is refocused into a point (echo) in a time-reversal dispersing system. If the defocused beam is inelastically scattered from a sample, the echo signal acquires a spatial distribution, which is a map of the inelastic scattering spectrum. The spectral resolution of the echo spectroscopy does not rely on the monochromaticity of the x rays, ensuring strong signals along with a very high spectral resolution. Particular schemes of x-ray echo spectrometers for 0.1-0.02 meV ultrahigh-resolution IXS applications (resolving power >108 ) with broadband ≃5 - 13 meV dispersing systems are introduced featuring more than 103 signal enhancement. The technique is general, applicable in different photon frequency domains.

  8. X-ray tensor tomography

    NASA Astrophysics Data System (ADS)

    Malecki, A.; Potdevin, G.; Biernath, T.; Eggl, E.; Willer, K.; Lasser, T.; Maisenbacher, J.; Gibmeier, J.; Wanner, A.; Pfeiffer, F.

    2014-02-01

    Here we introduce a new concept for x-ray computed tomography that yields information about the local micro-morphology and its orientation in each voxel of the reconstructed 3D tomogram. Contrary to conventional x-ray CT, which only reconstructs a single scalar value for each point in the 3D image, our approach provides a full scattering tensor with multiple independent structural parameters in each volume element. In the application example shown in this study, we highlight that our method can visualize sub-pixel fiber orientations in a carbon composite sample, hence demonstrating its value for non-destructive testing applications. Moreover, as the method is based on the use of a conventional x-ray tube, we believe that it will also have a great impact in the wider range of material science investigations and in future medical diagnostics. The authors declare no competing financial interests.

  9. X-ray Timing Measurements

    NASA Technical Reports Server (NTRS)

    Strohmayer, T.

    2008-01-01

    We present new, extended X-ray timing measurements of the ultra-compact binary candidates V407 Vul and RX J0806.3+1527 (J0806), as well as a summary of the first high resolution X-ray spectra of 50806 obtained with the Chandra/LETG. The temporal baseline for both objects is approximately 12 years, and our measurements confirm the secular spin-up in their X-ray periods. The spin-up rate in 50806 is remarkably uniform at 3.55x10(exp -16)Hz/s, with a measurement precision of 0.2%. We place a limit (90% confidence) on 1 d dot nu < 4x10(exp -26)Hz/sq s. Interestingly, for V407 Vul we find the first evidence that the spin-up rate is slowing, with d dot\

  10. X-ray Crystallography Facility

    NASA Technical Reports Server (NTRS)

    1999-01-01

    University of Alabama engineer Stacey Giles briefs NASA astronaut Dr. Bornie Dunbar about the design and capabilities of the X-ray Crystallography Facility under development at the Center for Macromolecular Crystallography of the University of Alabama at Birmingham, AL, April 21, 1999. The X-ray Crystallography Facility is designed to speed the collection of protein structure information from crystals grown aboard the International Space Station. By measuring and mapping the protein crystal structure in space, researchers will avoid exposing the delicate crystals to the rigors of space travel and make important research data available to scientists much faster. The X-ray Crystallography facility is being designed and developed by the Center for Macromolecular Crystallography of the University of Alabama at Birmingham, a NASA Commercial Space Center.

  11. X-ray Crystallography Facility

    NASA Technical Reports Server (NTRS)

    1999-01-01

    University of Alabama engineer Lance Weiss briefs NASA astronaut Dr. Bornie Dunbar about the design and capabilities of the X-ray Crystallography Facility under development at the Center for Macromolecular Crystallography of the University of Alabama at Birmingham, AL, April 21, 1999. The X-ray Crystallography Facility is designed to speed the collection of protein structure information from crystals grown aboard the International Space Station. By measuring and mapping the protein crystal structure in space, researchers will avoid exposing the delicate crystals to the rigors of space travel and make important research data available to scientists much faster. The X-ray Crystallography facility is being designed and developed by the Center for Macromolecular Crystallography of the University of Alabama at Birmingham, a NASA Commercial Space Center.

  12. X-ray fluorescence holography.

    PubMed

    Hayashi, Kouichi; Happo, Naohisa; Hosokawa, Shinya; Hu, Wen; Matsushita, Tomohiro

    2012-03-01

    X-ray fluorescence holography (XFH) is a method of atomic resolution holography which utilizes fluorescing atoms as a wave source or a monitor of the interference field within a crystal sample. It provides three-dimensional atomic images around a specified element and has a range of up to a few nm in real space. Because of this feature, XFH is expected to be used for medium-range local structural analysis, which cannot be performed by x-ray diffraction or x-ray absorption fine structure analysis. In this article, we explain the theory of XFH including solutions to the twin-image problem, an advanced measuring system, and data processing for the reconstruction of atomic images. Then, we briefly introduce our recent applications of this technique to the analysis of local lattice distortions in mixed crystals and nanometer-size clusters appearing in the low-temperature phase of a shape-memory alloy. PMID:22318258

  13. X-ray imaging: Perovskites target X-ray detection

    NASA Astrophysics Data System (ADS)

    Heiss, Wolfgang; Brabec, Christoph

    2016-05-01

    Single crystals of perovskites are currently of interest to help fathom fundamental physical parameters limiting the performance of perovskite-based polycrystalline solar cells. Now, such perovskites offer a technology platform for optoelectronic devices, such as cheap and sensitive X-ray detectors.

  14. Cosmic X-ray physics

    NASA Technical Reports Server (NTRS)

    Mccammon, D.; Cox, D. P.; Kraushaar, W. L.; Sanders, W. T.

    1986-01-01

    The analysis of the beryllium-filtered data from Flight 17.020 was completed. The data base provided by the Wisconsin diffuse X-ray sky survey is being analyzed by correlating the B and C band emission with individual velocity components of neutral hydrogen. Work on a solid state detector to be used in high resolution spectroscopy of diffuse or extend X-ray sources is continuing. A series of 21 cm observations was completed. A paper on the effects of process parameter variation on the reflectivity of sputter-deposited tungsten-carvon multilayers was published.

  15. Portable X-Ray Device

    NASA Technical Reports Server (NTRS)

    1983-01-01

    Portable x-ray instrument developed by NASA now being produced commercially as an industrial tool may soon find further utility as a medical system. The instrument is Lixiscope - Low Intensity X-Ray Imaging Scope -- a self-contained, battery-powered fluoroscope that produces an instant image through use of a small amount of radioactive isotope. Originally developed by Goddard Space Flight Center, Lixiscope is now being produced by Lixi, Inc. which has an exclusive NASA license for one version of the device.

  16. X-Ray Diffraction of Intermetallic Compounds: A Physical Chemistry Laboratory Experiment

    ERIC Educational Resources Information Center

    Varberg, Thomas D.; Skakuj, Kacper

    2015-01-01

    Here we describe an experiment for the undergraduate physical chemistry laboratory in which students synthesize the intermetallic compounds AlNi and AlNi3 and study them by X-ray diffractometry. The compounds are synthesized in a simple one-step reaction occurring in the solid state. Powder X-ray diffractograms are recorded for the two compounds…

  17. Compact x-ray source and panel

    DOEpatents

    Sampayon, Stephen E.

    2008-02-12

    A compact, self-contained x-ray source, and a compact x-ray source panel having a plurality of such x-ray sources arranged in a preferably broad-area pixelized array. Each x-ray source includes an electron source for producing an electron beam, an x-ray conversion target, and a multilayer insulator separating the electron source and the x-ray conversion target from each other. The multi-layer insulator preferably has a cylindrical configuration with a plurality of alternating insulator and conductor layers surrounding an acceleration channel leading from the electron source to the x-ray conversion target. A power source is connected to each x-ray source of the array to produce an accelerating gradient between the electron source and x-ray conversion target in any one or more of the x-ray sources independent of other x-ray sources in the array, so as to accelerate an electron beam towards the x-ray conversion target. The multilayer insulator enables relatively short separation distances between the electron source and the x-ray conversion target so that a thin panel is possible for compactness. This is due to the ability of the plurality of alternating insulator and conductor layers of the multilayer insulators to resist surface flashover when sufficiently high acceleration energies necessary for x-ray generation are supplied by the power source to the x-ray sources.

  18. Focused X-ray source

    DOEpatents

    Piestrup, M.A.; Boyers, D.G.; Pincus, C.I.; Maccagno, P.

    1990-08-21

    Disclosed is an intense, relatively inexpensive X-ray source (as compared to a synchrotron emitter) for technological, scientific, and spectroscopic purposes. A conical radiation pattern produced by a single foil or stack of foils is focused by optics to increase the intensity of the radiation at a distance from the conical radiator. 8 figs.

  19. X-ray backscatter imaging

    NASA Astrophysics Data System (ADS)

    Dinca, Dan-Cristian; Schubert, Jeffrey R.; Callerame, J.

    2008-04-01

    In contrast to transmission X-ray imaging systems where inspected objects must pass between source and detector, Compton backscatter imaging allows both the illuminating source as well as the X-ray detector to be on the same side of the target object, enabling the inspection to occur rapidly and in a wide variety of space-constrained situations. A Compton backscatter image is similar to a photograph of the contents of a closed container, taken through the container walls, and highlights low atomic number materials such as explosives, drugs, and alcohol, which appear as especially bright objects by virtue of their scattering characteristics. Techniques for producing X-ray images based on Compton scattering will be discussed, along with examples of how these systems are used for both novel security applications and for the detection of contraband materials at ports and borders. Differences between transmission and backscatter images will also be highlighted. In addition, tradeoffs between Compton backscatter image quality and scan speed, effective penetration, and X-ray source specifications will be discussed.

  20. X-rays and magnetism.

    PubMed

    Fischer, Peter; Ohldag, Hendrik

    2015-09-01

    Magnetism is among the most active and attractive areas in modern solid state physics because of intriguing phenomena interesting to fundamental research and a manifold of technological applications. State-of-the-art synthesis of advanced magnetic materials, e.g. in hybrid structures paves the way to new functionalities. To characterize modern magnetic materials and the associated magnetic phenomena, polarized x-rays have emerged as unique probes due to their specific interaction with magnetic materials. A large variety of spectroscopic and microscopic techniques have been developed to quantify in an element, valence and site-sensitive way properties of ferro-, ferri-, and antiferromagnetic systems, such as spin and orbital moments, and to image nanoscale spin textures and their dynamics with sub-ns time and almost 10 nm spatial resolution. The enormous intensity of x-rays and their degree of coherence at next generation x-ray facilities will open the fsec time window to magnetic studies addressing fundamental time scales in magnetism with nanometer spatial resolution. This review will give an introduction into contemporary topics of nanoscale magnetic materials and provide an overview of analytical spectroscopy and microscopy tools based on x-ray dichroism effects. Selected examples of current research will demonstrate the potential and future directions of these techniques. PMID:26288956

  1. Alpha proton x ray spectrometer

    NASA Technical Reports Server (NTRS)

    Rieder, Rudi; Waeke, H.; Economou, T.

    1994-01-01

    Mars Pathfinder will carry an alpha-proton x ray spectrometer (APX) for the determination of the elemental chemical composition of Martian rocks and soils. The instrument will measure the concentration of all major and some minor elements, including C, N, and O at levels above typically 1 percent.

  2. Focused X-ray source

    DOEpatents

    Piestrup, Melvin A.; Boyers, David G.; Pincus, Cary I.; Maccagno, Pierre

    1990-01-01

    An intense, relatively inexpensive X-ray source (as compared to a synchrotron emitter) for technological, scientific, and spectroscopic purposes. A conical radiation pattern produced by a single foil or stack of foils is focused by optics to increase the intensity of the radiation at a distance from the conical radiator.

  3. X-Ray Diffractive Optics

    NASA Technical Reports Server (NTRS)

    Dennis, Brian; Li, Mary; Skinner, Gerald

    2013-01-01

    X-ray optics were fabricated with the capability of imaging solar x-ray sources with better than 0.1 arcsecond angular resolution, over an order of magnitude finer than is currently possible. Such images would provide a new window into the little-understood energy release and particle acceleration regions in solar flares. They constitute one of the most promising ways to probe these regions in the solar atmosphere with the sensitivity and angular resolution needed to better understand the physical processes involved. A circular slit structure with widths as fine as 0.85 micron etched in a silicon wafer 8 microns thick forms a phase zone plate version of a Fresnel lens capable of focusing approx. =.6 keV x-rays. The focal length of the 3-cm diameter lenses is 100 microns, and the angular resolution capability is better than 0.1 arcsecond. Such phase zone plates were fabricated in Goddard fs Detector Development Lab. (DDL) and tested at the Goddard 600-microns x-ray test facility. The test data verified that the desired angular resolution and throughput efficiency were achieved.

  4. Soft X-ray spectroscopy studies of adsorption and reaction of CO in the presence of H2 over 6 nm MnO nanoparticles supported on mesoporous Co3O4

    NASA Astrophysics Data System (ADS)

    Ralston, Walter T.; Musselwhite, Nathan; Kennedy, Griffin; An, Kwangjin; Horowitz, Yonatan; Cordones, Amy A.; Rude, Bruce; Ahmed, Musahid; Melaet, Gerome; Alayoglu, Selim

    2016-06-01

    MnO nanoparticles (6 nm) were supported on mesoporous spinel Co3O4 and studied using ambient pressure X-ray photoelectron spectroscopy (APXPS) and in situ X-ray absorption spectroscopy (XAS) during hydrogenation of CO. The nature and evolution of surface adsorbed species as well as the oxidation states of the metal oxide surfaces were evaluated under oxidizing, reducing, and H2 + CO (2:1) reaction atmospheres. From APXPS, MnO nanoparticle surfaces were found to be progressively reduced in H2 atmospheres with increasing temperature. Surface adsorbed CO was found to be formed at the expense of lattice O under H2 + CO reaction conditions. In situ XAS indicated that the dominant oxide species were Co(OH)2, Co (II) oxides, MnO, and Mn3O4 under reaction conditions. In situ XAS also indicated the formation of gas phase CO2, the disappearance of lattice O, and the further reduction of Mn3O4 to MnO upon prolonged reaction in H2 + CO. Mass spectroscopy measurements showed the formation of CO2 and hydrocarbons. The spent catalyst was investigated using scanning transmission X-ray microscopy and (scanning) transmission electron microscopy; the catalyst grains were found to be homogeneous.

  5. X-Ray Diffraction on NIF

    SciTech Connect

    Eggert, J H; Wark, J

    2012-02-15

    The National Ignition Facility (NIF) is currently a 192 beam, 1.6 MJ laser. NIF Ramp-Compression Experiments have already made the relevant exo-planet pressure range from 1 to 50 Mbar accessible. We Proposed to Study Carbon Phases by X-Ray Diffraction on NIF. Just a few years ago, ultra-high pressure phase diagrams for materials were very 'simple'. New experiments and theories point out surprising and decidedly complex behavior at the highest pressures considered. High pressures phases of aluminum are also predicted to be complex. Recent metadynamics survey of carbon proposed a dynamic pathway among multiple phases. We need to develop diagnostics and techniques to explore this new regime of highly compressed matter science. X-Ray Diffraction - Understand the phase diagram/EOS/strength/texture of materials to 10's of Mbar. Strategy and physics goals: (1) Powder diffraction; (2) Begin with diamond; (3) Continue with metals etc.; (4) Explore phase diagrams; (5) Develop liquid diffraction; and (6) Reduce background/improve resolution.

  6. X-ray spectrometry and X-ray microtomography techniques for soil and geological samples analysis

    NASA Astrophysics Data System (ADS)

    Kubala-Kukuś, A.; Banaś, D.; Braziewicz, J.; Dziadowicz, M.; Kopeć, E.; Majewska, U.; Mazurek, M.; Pajek, M.; Sobisz, M.; Stabrawa, I.; Wudarczyk-Moćko, J.; Góźdź, S.

    2015-12-01

    A particular subject of X-ray fluorescence analysis is its application in studies of the multielemental sample of composition in a wide range of concentrations, samples with different matrices, also inhomogeneous ones and those characterized with different grain size. Typical examples of these kinds of samples are soil or geological samples for which XRF elemental analysis may be difficult due to XRF disturbing effects. In this paper the WDXRF technique was applied in elemental analysis concerning different soil and geological samples (therapeutic mud, floral soil, brown soil, sandy soil, calcium aluminum cement). The sample morphology was analyzed using X-ray microtomography technique. The paper discusses the differences between the composition of samples, the influence of procedures with respect to the preparation of samples as regards their morphology and, finally, a quantitative analysis. The results of the studies were statistically tested (one-way ANOVA and correlation coefficients). For lead concentration determination in samples of sandy soil and cement-like matrix, the WDXRF spectrometer calibration was performed. The elemental analysis of the samples was complemented with knowledge of chemical composition obtained by X-ray powder diffraction.

  7. Comparing graphene, carbon nanotubes, and superfine powdered activated carbon as adsorptive coating materials for microfiltration membranes.

    PubMed

    Ellerie, Jaclyn R; Apul, Onur G; Karanfil, Tanju; Ladner, David A

    2013-10-15

    Multi-walled carbon nanotubes (MWCNTs), nano-graphene platelets (NGPs), and superfine powdered activated carbon (S-PAC) were comparatively evaluated for their applicability as adsorptive coatings on microfiltration membranes. The objective was to determine which materials were capable of contaminant removal while causing minimal flux reduction. Methylene blue and atrazine were the model contaminants. When applied as membrane coatings, MWCNTs had minimal retention capabilities for the model contaminants, and S-PAC had the fastest removal. The membrane coating approach was also compared with a stirred vessel configuration, in which the adsorbent was added to a stirred flask preceding the membrane cell. Direct application of the adsorbent to the membrane constituted a greater initial reduction in permeate concentrations of the model contaminants than with the stirred flask setup. All adsorbents except S-PAC showed flux reductions less than 5% after application as thin-layer membrane coatings, and flux recovery after membrane backwashing was greater than 90% for all materials and masses tested. PMID:23911830

  8. Impacts of coagulation on the adsorption of organic micropollutants onto powdered activated carbon in treated domestic wastewater.

    PubMed

    Altmann, Johannes; Zietzschmann, Frederik; Geiling, Eva-Linde; Ruhl, Aki Sebastian; Sperlich, Alexander; Jekel, Martin

    2015-04-01

    The application of powdered activated carbon (PAC) as an advanced wastewater treatment step for the removal of organic micropollutants (OMP) necessitates complete separation of the PAC particles, e.g. by coagulation. In this study, potential positive or negative indirect or direct effects of coagulation on the adsorption of OMPs onto PAC in treated wastewater were investigated. Although the concentration of dissolved organic matter (DOM) was significantly reduced by coagulation, the selective removal of mainly larger DOM components such as biopolymers and humic substances did not improve subsequent OMP adsorption onto PAC, demonstrating that coagulation has minor effects on DOM constituents that are relevant for direct competition or pore blocking. The combination of coagulation and adsorption yielded the sum of the individual removals, as adsorption predominantly affected smaller compounds. While the formation of flocs led to visible incorporation of PAC particles, no significant mass transfer limitations impeded the OMP adsorption. As a result, the dosing sequence of coagulant and PAC is not critical for efficient adsorption of OMPs onto PAC. The relationships between adsorptive OMP removal and corresponding reduction of UV absorption at 254 nm (UVA254) as a promising surrogate correlation for the real-time monitoring and PAC adjustment were affected by coagulation, leading to individual correlations depending on the water composition. Correcting for UVA254 reduction by coagulation produces adsorptive UVA254 removal, which correlates highly with OMP removal for different WWTP effluents and varying coagulant doses and can be applied in combined adsorption/coagulation processes to predict OMP removal and control PAC dosing. PMID:25582393

  9. The adsorptive capacity of vapor-phase mercury chloride onto powdered activated carbon derived from waste tires

    SciTech Connect

    Hsun-Yu Lin; Chung-Shin Yuan; Chun-Hsin Wu; Chung-Hsuang Hung

    2006-11-15

    Injection of powdered activated carbon (PAC) upstream of particulate removal devices (such as electrostatic precipitator and baghouses) has been used effectively to remove hazardous air pollutants, particularly mercury containing pollutants, emitted from combustors and incinerators. Compared with commercial PACs (CPACs), an alternative PAC derived from waste tires (WPAC) was prepared for this study. The equilibrium adsorptive capacity of mercury chloride (HgCl{sub 2}) vapor onto the WPAC was further evaluated with a self-designed bench-scale adsorption column system. The adsorption temperatures investigated in the adsorption column were controlled at 25 and 150{sup o}C. The superficial velocity and residence time of the flow were 0.01 m/sec and 4 sec, respectively. The adsorption column tests were run under nitrogen gas flow. Experimental results showed that WPAC with higher Brunauer Emmett Teller (BET) surface area could adsorb more HgCl{sub 2} at room temperature. The equilibrium adsorptive capacity of HgCl{sub 2} for WPAC measured in this study was 1.49 x 10{sup -1} mg HgCl{sub 2}/g PAC at 25{sup o}C with an initial HgCl{sub 2} concentration of 25 {mu}g/m{sup 3}. With the increase of adsorption temperature {le} 150{sup o}C, the equilibrium adsorptive capacity of HgCl{sub 2} for WPAC was decreased to 1.34 x 10{sup -1} mg HgCl{sub 2}/g PAC. Furthermore, WPAC with higher sulfur contents could adsorb even more HgCl{sub 2}. It was demonstrated that the mechanisms for adsorbing HgCl{sub 2} onto WPAC were physical adsorption and chemisorption at 25 and 150{sup o}C, respectively. 35 refs., 4 figs., 4 tabs.

  10. ZnTe:O phosphor development for x-ray imaging applications

    SciTech Connect

    Kang, Z.T.; Summers, C.J.; Menkara, H.; Wagner, B.K.; Durst, R.; Diawara, Y.; Mednikova, G.; Thorson, T.

    2006-03-13

    An efficient ZnTe:O x-ray powder phosphor was prepared by a dry synthesis process using gaseous doping and etching medias. The x-ray luminescent properties were evaluated and compared to standard commercial phosphors exhibited an x-ray luminescent efficiency equivalent to 76% of Gd{sub 2}O{sub 2}S:Tb and an equal resolution of 2.5 lines/mm. In addition, the fast decay time, low afterglow, and superior spectral match to conventional charge-coupled devices-indicate that ZnTe:O is a very promising phosphor candidate for x-ray imaging applications.

  11. Trinuclear Zinc(II) Complexes and Polymeric Cadmium(II) Complexes with the Ligand 2,5-Bis(2-pyridyl)pyrazine: Synthesis, Spectral Analysis, and Single-Crystal and Powder X-ray Analyses.

    PubMed

    Neels, Antonia; Stoeckli-Evans, Helen

    1999-12-27

    coordination about the metal is best described as a distorted octahedral with four long distances in the basal plane, to two chlorines and to two nitrogen atoms, and two short distances in the axial direction, to two nitrogen atoms. With Cd(II) two polymeric complexes, 4 and 5 were obtained. Compound 4, C(18)H(16)N(4)O(4)Cd.5H(2)O, crystallizes in the triclinic space group P&onemacr;, a = 9.045(1) Å, b = 10.438(1) Å, c = 12.719(1) Å, alpha = 100.48(1) degrees, beta = 95.05(1) degrees, gamma = 95.86(1) degrees, and Z = 2; R1 for 3694 observed reflections [I > 2sigma(I)] was 0.029. The analogous Cd(NO(3))(2) complex with bppz, 5, could only be obtained in microcrystalline form, and its structure was solved by the use of X-ray powder diffraction methods. Compound 5, C(14)H(10)N(6)O(6)Cd, crystallizes in the monoclinic space group C2/c, with a = 11.6601(3) Å, b = 11.9870(3) Å, c = 12.1453(3) Å, beta = 103.348(2) degrees, and Z = 4. In both 4 and 5 the cadmium atoms are bridged by the ligand bppz, so forming uniform one-dimensional coordination polymers. The cadmium ions exhibit the rare coordination number of 8, with two coordinated ligand molecules and two chelating acetate (4) or nitrate (5) groups. PMID:11671328

  12. X-ray reprocessing in binaries

    NASA Astrophysics Data System (ADS)

    Paul, Biswajit

    2016-07-01

    We will discuss several aspects of X-ray reprocessing into X-rays or longer wavelength radiation in different kinds of binary systems. In high mass X-ray binaries, reprocessing of hard X-rays into emission lines or lower temperature black body emission is a useful tool to investigate the reprocessing media like the stellar wind, clumpy structures in the wind, accretion disk or accretion stream. In low mass X-ray binaries, reprocessing from the surface of the companion star, the accretion disk, warps and other structures in the accretion disk produce signatures in longer wavelength radiation. X-ray sources with temporal structures like the X-ray pulsars and thermonuclear burst sources are key in such studies. We will discuss results from several new investigations of X-ray reprocessing phenomena in X-ray binaries.

  13. Impacts of ozonation on the competition between organic micro-pollutants and effluent organic matter in powdered activated carbon adsorption.

    PubMed

    Zietzschmann, F; Mitchell, R-L; Jekel, M

    2015-11-01

    This study investigates if ozonation of wastewater treatment plant (WWTP) effluent can reduce the negative impacts of effluent organic matter (EfOM) on the adsorption of organic micro-pollutants (OMP) onto powdered activated carbon (PAC). Pre-treatment of the water included membrane filtration for the removal of suspended/colloidal organics, ozonation with various specific ozone consumptions, and subsequent OMP spiking to comparable initial concentrations in all of the ozonated waters. This approach allowed for comparative PAC adsorption tests. Adsorption analyses show that the adsorbability of EfOM decreases with increasing specific ozone consumptions. This is also reflected by liquid chromatography with online carbon and UV254 detection (LC-OCD) which shows the ozone-induced disintegration of large EfOM into smaller fragments. Also, small organic neutrals are decreased while the small organic acids peak continuously increases with rising specific ozone consumptions. UV254 demonstrates that the aromaticity of all LC-OCD fractions continuously declines together with increasing specific O3 consumptions. This explains the varying EfOM adsorbabilities that occur due to ozonation. The ozone-induced decrease of EfOM adsorbability directly translates into reduced adsorption competition against the adsorption of OMP. With higher specific ozone consumptions, OMP removal and OMP loadings increase. The reduced adsorption competition is reflected in the outputs from equivalent background compound (EBC) modeling. In each of the ozonated waters, correlations between the OMP removals and the UV254 removal were found. PMID:26231581

  14. X-ray diffraction studies of shocked lunar analogs

    NASA Technical Reports Server (NTRS)

    Hanss, R. E.

    1979-01-01

    The X-ray diffraction experiments on shocked rock and mineral analogs of particular significance to lunar geology are described. Materials naturally shocked by meteorite impact, nuclear-shocked, or artificially shocked in a flat plate accelerator were utilized. Four areas were outlined for investigation: powder diffractometer studies of shocked single crystal silicate minerals (quartz, orthoclase, oligoclase, pyroxene), powder diffractometer studies of shocked polycrystalline monomineralic samples (dunite), Debye-Scherrer studies of single grains of shocked granodiorite, and powder diffractometer studies of shocked whole rock samples. Quantitative interpretation of peak shock pressures experienced by materials found in lunar or terrestrial impact structures is presented.

  15. Effect of the adsorbate (Bromacil) equilibrium concentration in water on its adsorption on powdered activated carbon. Part 1. Equilibrium parameters.

    PubMed

    Al Mardini, Fadi; Legube, Bernard

    2009-10-30

    This study was carried out to investigate the adsorption equilibrium and kinetics of a pesticide of the uracil group on powdered activated carbon (PAC). The experiments were conducted at a wide range of initial pesticide concentrations (approximately 5 microg L(-1) to approximately 500 microg L(-1) at pH 7.8), corresponding to equilibrium concentrations of less than 0.1 microg L(-1) for the weakest, which is compatible with the tolerance limits of drinking water. Such a very broad range of initial solute concentrations resulting powdered activated carbon (PAC) concentrations (0.1-5 mg L(-1)) is the main particularity of our study. The application of several monosolute equilibrium models (two, three or more parameters) has generally shown that Bromacil adsorption is probably effective on two types of sites. High reactivity sites (K(L) approximately 10(3) Lmg(-1)) which are 10-20 less present in a carbon surface than lower reactivity sites (K(L) approximately 10 Lmg(-1)), according to the q(m) values calculated by two- or three-parameter models. The maximum capacity of the studied powdered activated carbon (PAC), corresponding to monolayer adsorption, compared to the Bromacil molecule surface, would be between 170 mg g(-1) and 190 mg g(-1). This theoretical value is very close to the experimental q(m) values obtained when using linearized forms of Langmuir, Tóth and Fritz-Schluender models. PMID:19539425

  16. X-ray microdiffraction of biominerals.

    PubMed

    Tamura, Nobumichi; Gilbert, Pupa U P A

    2013-01-01

    Biominerals have complex and heterogeneous architectures, hence diffraction experiments with spatial resolutions between 500 nm and 10 μm are extremely useful to characterize them. X-ray beams in this size range are now routinely produced at many synchrotrons. This chapter provides a review of the different hard X-ray diffraction and scattering techniques, used in conjunction with efficient, state-of-the-art X-ray focusing optics. These include monochromatic X-ray microdiffraction, polychromatic (Laue) X-ray microdiffraction, and microbeam small-angle X-ray scattering. We present some of the most relevant discoveries made in the field of biomineralization using these approaches. PMID:24188780

  17. Center for X-Ray Optics, 1986

    SciTech Connect

    Not Available

    1987-07-01

    The Center for X-Ray Optics has made substantial progress during the past year on the development of very high resolution x-ray technologies, the generation of coherent radiation at x-ray wavelengths, and, based on these new developments, had embarked on several scientific investigations that would not otherwise have been possible. The investigations covered in this report are topics on x-ray sources, x-ray imaging and applications, soft x-ray spectroscopy, synchrotron radiation, advanced light source and magnet structures for undulators and wigglers. (LSP)

  18. Orbital and magnetic ordering in Pr1-xCaxMnO3 and Nd1-xSrxMnO3 manganites near half doping studied by resonant soft x-ray powder diffraction

    NASA Astrophysics Data System (ADS)

    Staub, U.; García-Fernández, M.; Bodenthin, Y.; Scagnoli, V.; de Souza, R. A.; Garganourakis, M.; Pomjakushina, E.; Conder, K.

    2009-06-01

    Here we present resonant soft x-ray diffraction data in the vicinity of the MnL2,3 edges on R1-xTxMnO3 manganites ( R=Pr , Nd and T=Ca , Sr) close to half doping. For Pr0.6Ca0.4MnO3 (PCMO), the energy dependence of the superimposed orbital and magnetic reflections are studied using various incident x-ray polarizations. For Nd0.5Sr0.5MnO3 (NSMO), the energy dependence of the orbital ordering reflection is found to be very similar to that found in other manganites systems. These two results are compared to those presented in the literature on single-crystal samples. Whereas our results are in good agreement with the spectral shape of a superposition of magnetic and orbital signals in PCMO, the magnetic signals are only moderately larger than the orbital signals. The results on NSMO do not agree with previously presented data on single crystals and cast doubt on the proposed occurrence of a double-stripe orbital order.

  19. Superiority of wet-milled over dry-milled superfine powdered activated carbon for adsorptive 2-methylisoborneol removal.

    PubMed

    Pan, Long; Matsui, Yoshihiko; Matsushita, Taku; Shirasaki, Nobutaka

    2016-10-01

    Superfine powdered activated carbon (SPAC), which is produced from conventionally sized powdered activated carbon (PAC) by wet milling in a bead mill, has attracted attention for its high adsorptive removal ability in both research and practice. In this study, the performance of dry-milled SPAC was investigated. 2-Methylisoborneol (MIB), an earthy-musty compound commonly targeted by water treatment systems, was used as the target adsorbate. Dry-milled SPAC exhibited lower adsorptive removal of MIB than wet-milled SPAC, even when both SPACs were produced from the same PAC and were composed of particles of the same size. One reason for the lower removal of MIB by the dry-milled SPAC was a higher degree of aggregation in the dry-milled SPAC after production; as a result the apparent particle size of dry-milled SPAC was larger than that of wet-milled SPAC. The dry-milled SPAC was also more negatively charged than the wet-milled SPAC, and, owing to its higher repulsion, it was more amenable to dispersion by ultrasonication. However, even after the dry-milled SPAC was ultrasonicated so that its apparent particle size was similar to or less than that of the wet-milled SPAC, the dry-milled SPAC was still inferior in adsorptive removal to the wet-milled SPAC. Therefore, another reason for the lower adsorptive removal of dry-milled SPAC was its lower equilibrium adsorption capacity due to the oxidation during the milling. The adsorption kinetics by SPACs with different degrees of particle aggregation were successfully simulated by a pore diffusion model and a fractal aggregation model. PMID:27403874

  20. Microgap x-ray detector

    SciTech Connect

    Wuest, Craig R.; Bionta, Richard M.; Ables, Elden

    1994-01-01

    An x-ray detector which provides for the conversion of x-ray photons into photoelectrons and subsequent amplification of these photoelectrons through the generation of electron avalanches in a thin gas-filled region subject to a high electric potential. The detector comprises a cathode (photocathode) and an anode separated by the thin, gas-filled region. The cathode may comprise a substrate, such a beryllium, coated with a layer of high atomic number material, such as gold, while the anode can be a single conducting plane of material, such as gold, or a plane of resistive material, such as chromium/silicon monoxide, or multiple areas of conductive or resistive material, mounted on a substrate composed of glass, plastic or ceramic. The charge collected from each electron avalanche by the anode is passed through processing electronics to a point of use, such as an oscilloscope.

  1. Microgap x-ray detector

    DOEpatents

    Wuest, C.R.; Bionta, R.M.; Ables, E.

    1994-05-03

    An x-ray detector is disclosed which provides for the conversion of x-ray photons into photoelectrons and subsequent amplification of these photoelectrons through the generation of electron avalanches in a thin gas-filled region subject to a high electric potential. The detector comprises a cathode (photocathode) and an anode separated by the thin, gas-filled region. The cathode may comprise a substrate, such a beryllium, coated with a layer of high atomic number material, such as gold, while the anode can be a single conducting plane of material, such as gold, or a plane of resistive material, such as chromium/silicon monoxide, or multiple areas of conductive or resistive material, mounted on a substrate composed of glass, plastic or ceramic. The charge collected from each electron avalanche by the anode is passed through processing electronics to a point of use, such as an oscilloscope. 3 figures.

  2. Hard X-ray astrophysics

    NASA Technical Reports Server (NTRS)

    Rothschild, R. E.

    1981-01-01

    Past hard X-ray and lower energy satellite instruments are reviewed and it is shown that observation above 20 keV and up to hundreds of keV can provide much valuable information on the astrophysics of cosmic sources. To calculate possible sensitivities of future arrays, the efficiencies of a one-atmosphere inch gas counter (the HEAO-1 A-2 xenon filled HED3) and a 3 mm phoswich scintillator (the HEAO-1 A-4 Na1 LED1) were compared. Above 15 keV, the scintillator was more efficient. In a similar comparison, the sensitivity of germanium detectors did not differ much from that of the scintillators, except at high energies where the sensitivity would remain flat and not rise with loss of efficiency. Questions to be addressed concerning the physics of active galaxies and the diffuse radiation background, black holes, radio pulsars, X-ray pulsars, and galactic clusters are examined.

  3. Removal of iodide from water by chlorination and subsequent adsorption on powdered activated carbon.

    PubMed

    Ikari, Mariya; Matsui, Yoshihiko; Suzuki, Yuta; Matsushita, Taku; Shirasaki, Nobutaka

    2015-01-01

    Chlorine oxidation followed by treatment with activated carbon was studied as a possible method for removing radioactive iodine from water. Chlorination time, chlorine dose, the presence of natural organic matter (NOM), the presence of bromide ion (Br⁻), and carbon particle size strongly affected iodine removal. Treatment with superfine powdered activated carbon (SPAC) after 10-min oxidation with chlorine (1 mg-Cl₂/L) removed 90% of the iodine in NOM-containing water (dissolved organic carbon concentration, 1.5 mg-C/L). Iodine removal in NOM-containing water increased with increasing chlorine dose up to 0.1 mg-Cl₂/L but decreased at chlorine doses of >1.0 mg-Cl₂/L. At a low chlorine dose, nonadsorbable iodide ion (I⁻) was oxidized to adsorbable hypoiodous acid (HOI). When the chlorine dose was increased, some of the HOI reacted with NOM to form adsorbable organic iodine (organic-I). Increasing the chlorine dose further did not enhance iodine removal, owing to the formation of nonadsorbable iodate ion (IO₃⁻). Co-existing Br⁻ depressed iodine removal, particularly in NOM-free water, because hypobromous acid (HOBr) formed and catalyzed the oxidation of HOI to IO₃⁻. However, the effect of Br⁻ was small in the NOM-containing water because organic-I formed instead of IO₃⁻. SPAC (median particle diameter, 0.62 μm) had a higher equilibrium adsorption capacity for organic-I than did conventional PAC (median diameter, 18.9 μm), but the capacities of PAC and SPAC for HOI were similar. The reason for the higher equilibrium adsorption capacity for organic-I was that organic-I was adsorbed principally on the exterior of the PAC particles and not inside the PAC particles, as indicated by direct visualization of the solid-phase iodine concentration profiles in PAC particles by field emission electron probe microanalysis. In contrast, HOI was adsorbed evenly throughout the entire PAC particle. PMID:25462731

  4. Soft x-ray tomoholography

    NASA Astrophysics Data System (ADS)

    Guehrs, Erik; Stadler, Andreas M.; Flewett, Sam; Frömmel, Stefanie; Geilhufe, Jan; Pfau, Bastian; Rander, Torbjörn; Schaffert, Stefan; Büldt, Georg; Eisebitt, Stefan

    2012-01-01

    We demonstrate an x-ray imaging method that combines Fourier transform holography with tomography (‘tomoholography’) for three-dimensional (3D) microscopic imaging. A 3D image of a diatom shell with a spatial resolution of 140 nm is presented. The experiment is realized by using a small gold sphere as the reference wave source for holographic imaging. This setup allows us to rotate the sample and to collect a number of 2D projections for tomography.

  5. X-ray Diffraction from Membrane Protein Nanocrystals

    PubMed Central

    Hunter, M.S.; DePonte, D.P.; Shapiro, D.A.; Kirian, R.A.; Wang, X.; Starodub, D.; Marchesini, S.; Weierstall, U.; Doak, R.B.; Spence, J.C.H.; Fromme, P.

    2011-01-01

    Membrane proteins constitute >30% of the proteins in an average cell, and yet the number of currently known structures of unique membrane proteins is <300. To develop new concepts for membrane protein structure determination, we have explored the serial nanocrystallography method, in which fully hydrated protein nanocrystals are delivered to an x-ray beam within a liquid jet at room temperature. As a model system, we have collected x-ray powder diffraction data from the integral membrane protein Photosystem I, which consists of 36 subunits and 381 cofactors. Data were collected from crystals ranging in size from 100 nm to 2 μm. The results demonstrate that there are membrane protein crystals that contain <100 unit cells (200 total molecules) and that 3D crystals of membrane proteins, which contain <200 molecules, may be suitable for structural investigation. Serial nanocrystallography overcomes the problem of x-ray damage, which is currently one of the major limitations for x-ray structure determination of small crystals. By combining serial nanocrystallography with x-ray free-electron laser sources in the future, it may be possible to produce molecular-resolution electron-density maps using membrane protein crystals that contain only a few hundred or thousand unit cells. PMID:21190672

  6. X-ray Diode Preparation

    SciTech Connect

    Henderson, D J; Good, D E; Hogge, K W; Molina, I; Howe, R A; Lutz, S S; Flores, P A; McGillivray, K D; Skarda, W M; Nelson, D S; Ormond, E S; Cordova, S R

    2011-06-16

    A rod pinch x-ray diode assembly culminates in a coaxial anode cathode arrangement where a small anode rod extends through the aperture of a cathode plate. Shotto- shot repeatability in rod placement, and thus x-ray source spot position, has potential to positively affect radiographic image quality. Thus, how to both control and measure, according to a Cartesian coordinate system, anode rod tip displacement (x, y) (off the beam line-of-sight retical) and also anode rod tip extension (z) (along the line-of-sight center line) become salient issues relative to radiographic image set utility. To address these issues both hardware fabrication and x-ray diode assembly methods were reviewed, and additional controls were introduced. A photogrammetric procedure was developed to quantify anode rod tip position in situ. Computer models and mock-up assemblies with precision fiducials were produced to validate this procedure. Therefore, both anode rod tip displacement and anode rod tip extension parameters were successfully controlled. Rod position was measured and met the required specifications: (1) radial displacement <0.25 mm and (2) axial placement of ±0.25 mm. We demonstrated that precision control and measurement of large scale components is achievable in a pulse power system (i.e., hardware and operations). Correlations with diode performance and radiography are presented.

  7. X-Ray Crystallography Reagent

    NASA Technical Reports Server (NTRS)

    Morrison, Dennis R. (Inventor); Mosier, Benjamin (Inventor)

    2003-01-01

    Microcapsules prepared by encapsulating an aqueous solution of a protein, drug or other bioactive substance inside a semi-permeable membrane by are disclosed. The microcapsules are formed by interfacial coacervation under conditions where the shear forces are limited to 0-100 dynes per square centimeter at the interface. By placing the microcapsules in a high osmotic dewatering solution. the protein solution is gradually made saturated and then supersaturated. and the controlled nucleation and crystallization of the protein is achieved. The crystal-filled microcapsules prepared by this method can be conveniently harvested and stored while keeping the encapsulated crystals in essentially pristine condition due to the rugged. protective membrane. Because the membrane components themselves are x-ray transparent, large crystal-containing microcapsules can be individually selected, mounted in x-ray capillary tubes and subjected to high energy x-ray diffraction studies to determine the 3-D smucture of the protein molecules. Certain embodiments of the microcapsules of the invention have composite polymeric outer membranes which are somewhat elastic, water insoluble, permeable only to water, salts, and low molecular weight molecules and are structurally stable in fluid shear forces typically encountered in the human vascular system.

  8. X-Ray-powered Macronovae

    NASA Astrophysics Data System (ADS)

    Kisaka, Shota; Ioka, Kunihito; Nakar, Ehud

    2016-02-01

    A macronova (or kilonova) was observed as an infrared excess several days after the short gamma-ray burst GRB 130603B. Although the r-process radioactivity is widely discussed as an energy source, it requires a huge mass of ejecta from a neutron star (NS) binary merger. We propose a new model in which the X-ray excess gives rise to the simultaneously observed infrared excess via thermal re-emission, and explore what constraints this would place on the mass and velocity of the ejecta. This X-ray-powered model explains both the X-ray and infrared excesses with a single energy source such as the central engine like a black hole, and allows for a broader parameter region than the previous models, in particular a smaller ejecta mass ˜ {10}-3{--}{10}-2{M}⊙ and higher iron abundance mixed as suggested by general relativistic simulations for typical NS-NS mergers. We also discuss the other macronova candidates in GRB 060614 and GRB 080503, and the implications for the search of electromagnetic counterparts to gravitational waves.

  9. Temperature-dependent vibrational spectroscopic and X-ray diffraction investigation of nanosized nickel chromite

    NASA Astrophysics Data System (ADS)

    Matulková, Irena; Holec, Petr; Němec, Ivan; Kitazawa, Hideaki; Furubayashi, Takao; Vejpravová, Jana

    2015-06-01

    The nanocrystalline nickel chromite (NiCr2O4) with particle size of ∼20 nm was prepared by auto-combustion method. The nanocrystals were characterized by powder X-ray diffraction, vibrational spectroscopy and magnetic measurements. The expected structural phase transitions (cubic-tetragonal-orthorhombic) were studied by methods of temperature-dependent X-ray powder diffraction and vibrational spectroscopy. The evolution of the Raman spectra and X-ray diffraction patterns collected from 350 K down to 4 K confirmed the cubic-to-tetragonal distortion at ∼250 K, whereas the tetragonal-to-orthorhombic transition was not confirmed in the nanocrystalline sample.

  10. Aspergillosis - chest x-ray (image)

    MedlinePlus

    ... usually occurs in immunocompromised individuals. Here, a chest x-ray shows that the fungus has invaded the lung ... are usually seen as black areas on an x-ray. The cloudiness on the left side of this ...

  11. Tuberculosis, advanced - chest x-rays (image)

    MedlinePlus

    ... tissue, and can cause tissue death. These chest x-rays show advanced pulmonary tuberculosis. There are multiple light ... location of cavities within these light areas. The x-ray on the left clearly shows that the opacities ...

  12. Advances in transmission x-ray optics

    SciTech Connect

    Ceglio, N.M.

    1983-01-01

    Recent developments in x-ray optics are reviewed. Specific advances in coded aperture imaging, zone plate lens fabrication, time and space resolved spectroscopy, and CCD x-ray detection are discussed.

  13. Producing X-rays at the APS

    ScienceCinema

    None

    2013-04-19

    An introduction and overview of the Advanced Photon Source at Argonne National Laboratory, the technology that produces the brightest X-ray beams in the Western Hemisphere, and the research carried out by scientists using those X-rays.

  14. Producing X-rays at the APS

    SciTech Connect

    2011-01-01

    An introduction and overview of the Advanced Photon Source at Argonne National Laboratory, the technology that produces the brightest X-ray beams in the Western Hemisphere, and the research carried out by scientists using those X-rays.

  15. Phase-sensitive X-ray imager

    DOEpatents

    Baker, Kevin Louis

    2013-01-08

    X-ray phase sensitive wave-front sensor techniques are detailed that are capable of measuring the entire two-dimensional x-ray electric field, both the amplitude and phase, with a single measurement. These Hartmann sensing and 2-D Shear interferometry wave-front sensors do not require a temporally coherent source and are therefore compatible with x-ray tubes and also with laser-produced or x-pinch x-ray sources.

  16. Advanced x-ray imaging spectrometer

    NASA Technical Reports Server (NTRS)

    Callas, John L. (Inventor); Soli, George A. (Inventor)

    1998-01-01

    An x-ray spectrometer that also provides images of an x-ray source. Coded aperture imaging techniques are used to provide high resolution images. Imaging position-sensitive x-ray sensors with good energy resolution are utilized to provide excellent spectroscopic performance. The system produces high resolution spectral images of the x-ray source which can be viewed in any one of a number of specific energy bands.

  17. Center for X-ray Optics, 1988

    SciTech Connect

    Not Available

    1989-04-01

    This report briefly reviews the following topics: soft-x-ray imaging; reflective optics for hard x-rays; coherent XUV sources; spectroscopy with x-rays; detectors for coronary artery imaging; synchrotron-radiation optics; and support for the advanced light source.

  18. Student X-Ray Fluorescence Experiments

    ERIC Educational Resources Information Center

    Fetzer, Homer D.; And Others

    1975-01-01

    Describes the experimental arrangement for x-ray analysis of samples which involves the following: the radioisotopic x-ray disk source; a student-built fluorescence chamber; the energy dispersive x-ray detector, linear amplifier and bias supply; and a multichannel pulse height analyzer. (GS)

  19. Cryotomography x-ray microscopy state

    DOEpatents

    Le Gros, Mark; Larabell, Carolyn A.

    2010-10-26

    An x-ray microscope stage enables alignment of a sample about a rotation axis to enable three dimensional tomographic imaging of the sample using an x-ray microscope. A heat exchanger assembly provides cooled gas to a sample during x-ray microscopic imaging.

  20. Optical observations of X-ray systems

    NASA Astrophysics Data System (ADS)

    Gudets, R.

    The significance of optical observations of X-ray sources is discussed. A short review of X-ray and optical observations of X-ray stars in socialist countries, carried out by the Intercosmos program and by multilateral cooperation of the Academies of Sciences of Socialist Countries is given. Some examples and results of observations are presented.

  1. Electron beam parallel X-ray generator

    NASA Technical Reports Server (NTRS)

    Payne, P.

    1967-01-01

    Broad X ray source produces a highly collimated beam of low energy X rays - a beam with 2 to 5 arc minutes of divergence at energies between 1 and 6 keV in less than 5 feet. The X ray beam is generated by electron bombardment of a target from a large area electron gun.

  2. Zernike x-ray ptychography.

    PubMed

    Vartiainen, Ismo; Mohacsi, Istvan; Stachnik, Karolina; Guizar-Sicairos, Manuel; David, Christian; Meents, Alke

    2016-02-15

    We present an imaging technique combining Zernike phase-contrast imaging and ptychography. The contrast formation is explained by following the theory of Zernike phase-contrast imaging. The method is demonstrated with x-rays at a photon energy of 6.2 keV, showing how ptychographic reconstruction of a phase sample leads to a Zernike phase-contrast image appearing in the amplitude reconstruction. In addition, the results presented in this Letter indicate an improvement of the resolution of the reconstructed object in the case of Zernike ptychography compared with the conventional one. PMID:26872172

  3. X-ray transmissive debris shield

    DOEpatents

    Spielman, Rick B.

    1996-01-01

    An X-ray debris shield for use in X-ray lithography that is comprised of an X-ray window having a layer of low density foam exhibits increased longevity without a substantial increase in exposure time. The low density foam layer serves to absorb the debris emitted from the X-ray source and attenuate the shock to the window so as to reduce the chance of breakage. Because the foam is low density, the X-rays are hardly attenuated by the foam and thus the exposure time is not substantially increased.

  4. X-ray transmissive debris shield

    DOEpatents

    Spielman, R.B.

    1996-05-21

    An X-ray debris shield for use in X-ray lithography that is comprised of an X-ray window having a layer of low density foam exhibits increased longevity without a substantial increase in exposure time. The low density foam layer serves to absorb the debris emitted from the X-ray source and attenuate the shock to the window so as to reduce the chance of breakage. Because the foam is low density, the X-rays are hardly attenuated by the foam and thus the exposure time is not substantially increased.

  5. Three-dimensional x-ray microtomography

    SciTech Connect

    Flannery, B.P.; Deckman, H.W.; Roberge, W.G.; D'Amico, K.L.

    1987-09-18

    The new technique of x-ray microtomography nondestructively generates three-dimensional maps of the x-ray attenuation coefficient inside small samples with approximately 1 percent accuracy and with resolution approaching 1 micrometer. Spatially resolved elemental maps can be produced with synchrotron x-ray sources by scanning samples at energies just above and below characteristic atomic absorption edges. The system consists of a high-resolution imaging x-ray detector and high-speed algorithms for tomographic image reconstruction. The design and operation of the microtomography device are described, and tomographic images that illustrate it performance with both synchrotron and laboratory x-ray sources are presented.

  6. Comets: mechanisms of x-ray activity

    NASA Astrophysics Data System (ADS)

    Ibadov, Subhon

    2016-07-01

    Basic mechanisms of X-ray activity of comets are considered, including D-D mechanism corresponding to generation of X-rays due to production of hot short-living plasma clumps at high-velocity collisions between cometary and interplanetary dust particles as well as M-M one corresponding to production of X-rays due to recombination of multicharge ions of solar wind plasma via charge exchange process at their collisions with molecules/atoms of the cometary atmospheres. Peculiarities of the variation of the comet X-ray spectrum and X-ray luminosity with variation of its heliocentric distance are revealed.

  7. Atmospheric electron x-ray spectrometer

    NASA Technical Reports Server (NTRS)

    Feldman, Jason E. (Inventor); George, Thomas (Inventor); Wilcox, Jaroslava Z. (Inventor)

    2002-01-01

    The present invention comprises an apparatus for performing in-situ elemental analyses of surfaces. The invention comprises an atmospheric electron x-ray spectrometer with an electron column which generates, accelerates, and focuses electrons in a column which is isolated from ambient pressure by a:thin, electron transparent membrane. After passing through the membrane, the electrons impinge on the sample in atmosphere to generate characteristic x-rays. An x-ray detector, shaping amplifier, and multi-channel analyzer are used for x-ray detection and signal analysis. By comparing the resultant data to known x-ray spectral signatures, the elemental composition of the surface can be determined.

  8. X-ray Spectroscopy of Cooling Cluster

    SciTech Connect

    Peterson, J.R.; Fabian, A.C.; /Cambridge U., Inst. of Astron.

    2006-01-17

    We review the X-ray spectra of the cores of clusters of galaxies. Recent high resolution X-ray spectroscopic observations have demonstrated a severe deficit of emission at the lowest X-ray temperatures as compared to that expected from simple radiative cooling models. The same observations have provided compelling evidence that the gas in the cores is cooling below half the maximum temperature. We review these results, discuss physical models of cooling clusters, and describe the X-ray instrumentation and analysis techniques used to make these observations. We discuss several viable mechanisms designed to cancel or distort the expected process of X-ray cluster cooling.

  9. Ionospheric effects of solar x-rays

    NASA Astrophysics Data System (ADS)

    Danskin, Donald

    2016-07-01

    The ionospheric absorption of radio waves caused by solar x-ray bursts is measured directly by Riometers from the Canada Riometer Array. The absorption is found to be proportional to the square root of the flux intensity of the X-ray burst with time delays of 18-20 seconds between the peak X-ray emission and absorption in the ionosphere. A detailed analysis showed that some X-ray flares during 2011-2014 are more effective at producing absorption than others. Solar longitude of X-ray burst for several X-class flares shows no consistent pattern of enhancement in the absorption.

  10. X-ray lithography using holographic images

    DOEpatents

    Howells, Malcolm R.; Jacobsen, Chris

    1995-01-01

    A non-contact X-ray projection lithography method for producing a desired X-ray image on a selected surface of an X-ray-sensitive material, such as photoresist material on a wafer, the desired X-ray image having image minimum linewidths as small as 0.063 .mu.m, or even smaller. A hologram and its position are determined that will produce the desired image on the selected surface when the hologram is irradiated with X-rays from a suitably monochromatic X-ray source of a selected wavelength .lambda.. On-axis X-ray transmission through, or off-axis X-ray reflection from, a hologram may be used here, with very different requirements for monochromaticity, flux and brightness of the X-ray source. For reasonable penetration of photoresist materials by X-rays produced by the X-ray source, the wavelength X, is preferably chosen to be no more than 13.5 nm in one embodiment and more preferably is chosen in the range 1-5 nm in the other embodiment. A lower limit on linewidth is set by the linewidth of available microstructure writing devices, such as an electron beam.

  11. Evolution of X-ray astronomy

    NASA Technical Reports Server (NTRS)

    Rossj, B.

    1981-01-01

    The evolution of X-ray astronomy up to the launching of the Einstein observatory is presented. The evaluation proceeded through the following major steps: (1) discovery of an extrasolar X-ray source, Sco X-1, orders of magnitude stronger than astronomers believed might exist; (2) identification of a strong X-ray source with the Crab Nebula; (3) identification of Sco X-1 with a faint, peculiar optical object; (4) demonstration that X-ray stars are binary systems, each consisting of a collapsed object accreting matter from an ordinary star; (5) discovery of X-ray bursts; (6) discovery of exceedingly strong X-ray emission from active galaxies, quasars and clusters of galaxies; (7) demonstration that the principal X-ray source is a hot gas filling the space between galaxies.

  12. X ray imaging microscope for cancer research

    NASA Technical Reports Server (NTRS)

    Hoover, Richard B.; Shealy, David L.; Brinkley, B. R.; Baker, Phillip C.; Barbee, Troy W., Jr.; Walker, Arthur B. C., Jr.

    1991-01-01

    The NASA technology employed during the Stanford MSFC LLNL Rocket X Ray Spectroheliograph flight established that doubly reflecting, normal incidence multilayer optics can be designed, fabricated, and used for high resolution x ray imaging of the Sun. Technology developed as part of the MSFC X Ray Microscope program, showed that high quality, high resolution multilayer x ray imaging microscopes are feasible. Using technology developed at Stanford University and at the DOE Lawrence Livermore National Laboratory (LLNL), Troy W. Barbee, Jr. has fabricated multilayer coatings with near theoretical reflectivities and perfect bandpass matching for a new rocket borne solar observatory, the Multi-Spectral Solar Telescope Array (MSSTA). Advanced Flow Polishing has provided multilayer mirror substrates with sub-angstrom (rms) smoothnesss for the astronomical x ray telescopes and x ray microscopes. The combination of these important technological advancements has paved the way for the development of a Water Window Imaging X Ray Microscope for cancer research.

  13. Extended range X-ray telescope

    NASA Technical Reports Server (NTRS)

    Hoover, R. B. (Inventor)

    1981-01-01

    An X-ray telescope system is described which is comprised of a tubular mount having a collecting region remote from the one axial end. A soft X-ray/XUV subsystem associated with the collecting region directs only relatively soft, near on-axis X-rays/XUV radiation incident on a first portion of the collecting region into a first detector sensitive to relatively soft X-rays/XUV radiation. A hard X-ray subsystem associated with the collecting region directs only relatively hard near on-axis X-rays incident on a second portion of the collecting region into a second detector sensitive to relatively hard X-rays.

  14. X-ray deconvolution microscopy

    PubMed Central

    Ehn, Sebastian; Epple, Franz Michael; Fehringer, Andreas; Pennicard, David; Graafsma, Heinz; Noël, Peter; Pfeiffer, Franz

    2016-01-01

    Recent advances in single-photon-counting detectors are enabling the development of novel approaches to reach micrometer-scale resolution in x-ray imaging. One example of such a technology are the MEDIPIX3RX-based detectors, such as the LAMBDA which can be operated with a small pixel size in combination with real-time on-chip charge-sharing correction. This characteristic results in a close to ideal, box-like point spread function which we made use of in this study. The proposed method is based on raster-scanning the sample with sub-pixel sized steps in front of the detector. Subsequently, a deconvolution algorithm is employed to compensate for blurring introduced by the overlap of pixels with a well defined point spread function during the raster-scanning. The presented approach utilizes standard laboratory x-ray equipment while we report resolutions close to 10 μm. The achieved resolution is shown to follow the relationship pn with the pixel-size p of the detector and the number of raster-scanning steps n. PMID:27446649

  15. Submicron X-ray diffraction

    SciTech Connect

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

    2000-08-17

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

  16. Parametric X-Ray Radiation

    NASA Astrophysics Data System (ADS)

    Shchagin, Alexander

    1997-10-01

    The main PXR properties [1,2] are considered in the paper: energy, width, smooth tuning of monochromatic PXR spectral line; fine structure and absolute differential yields of PXR in the vicinity of and at angular distances from Brag directions; angular spread of the PXR beam; the influence of incident electron energy and of the density effect on the PXR properties; linear polarization of PXR; background in PXR spectra. Experimental setups for linacs and the results of measurements are discussed. Experimental data are compared to theoretical calculations at PXR energies between 5 and 400 keV for incident electron energies ranging from 15 to 1200 MeV. Possible applications of PXR as a new source of a bright, tunable X-ray beam in science and industry are discussed. [1] A.V. Shchagin and N.A. Khizhnyak, NIM B119, 115-122 (1996). [2] A.V. Shchagin and X.K. Maruyama, "Parametric X-rays", a chapter in the book "Accelerator-based Atomic Physics Techniques and Applications", edited by S.M. Shafroth and J.C. Austin, AIP Press, 1997, pp 279-307.

  17. Transportable X-ray cart

    SciTech Connect

    1995-12-01

    The main body of the report summarizes the project scope, project milestones, highlights any unresolved problems encountered during the project and includes a summary of the financial information. The purpose of this CRADA was to assist Digiray Corporation in the development and evaluation of a Transportable Reverse Geometry X-Ray 0 (RGX-T) cart for aircraft inspection Scope: LLNL was to provide a review of the RGX-T engineering drawing package supplied by Digiray, suggest and incorporate design modifications, fabricate, assemble and provide performance evaluation testing of the RGX-T prototype. Major deliverables were (a) engineering design analysis and evaluation (b) cart prototype hardware, and (c) performance evaluation. Schedule: Procurement and technical delays extended the project twelve months past than the original four month project duration estimate. LLNL reviewed engineering drawings of the RGX-T prototype provided by Digiray, performed a engineering design analysis and evaluation, suggested and incorporated modifications to improve design safety factors, fabricated and assembled the prototype system, and evaluated the motion and positioning capabilities of the assembled system. The RGX-T provides a limited set of positioning orientations for the Digiray x-ray tube head that do not meet the overall Digiray requirements for aircraft inspection. In addition, mechanical stability concerns remain for positioning the tube head with the mechanical arm and for rolling the assembly with arbitrary orientation of the mechanical arm.

  18. X-ray lasing - Theory

    SciTech Connect

    Not Available

    1985-11-01

    The theoretical basis of lasing at very short wavelengths is discussed, and lasing at soft-x-ray (4-50 nm) wavelengths using the electron-collisional excitation scheme is successfully demonstrated. In research at LLNL, thin foils of selenium and yttrium are irradiated with laser light to generate a roughly cylindrical plasma containing neon-like ions. Excitation of ground state 2p electrons to the 3p state in the lasant medium is followed by very fast radioactive decay out of the 3s state, creating a population inversion between the 3s and 3p states. Stimulated x-ray emission is initiated by slower spontaneous decay from a 3p to 3s state. Design goals are to produce a plasma with a flat electron density of approximately 5 x 10 to the 20th/cu cm, a flat temperature profile, a scale length of at least 100 microns, and a population inversion lasting at least the 100 ps necessary to produce a significant gain. Good correlation is seen between experimental data and LANEX and XRASER theoretical modeling predictions over large variations in intensity, pulse length, and probing times. No explanation is found for the weakness of the J = 0 to J = 1 lasing transition line at 18.3 nm. 13 references.

  19. X-ray lasing - Theory

    NASA Astrophysics Data System (ADS)

    1985-11-01

    The theoretical basis of lasing at very short wavelengths is discussed, and lasing at soft-X-ray (4-50 nm) wavelengths using the electron-collisional excitation scheme is successfully demonstrated. In research at LLNL, thin foils of selenium and yttrium are irradiated with laser light to generate a roughly cylindrical plasma containing neon-like ions. Excitation of ground state 2p electrons to the 3p state in the lasant medium is followed by very fast radioactive decay out of the 3s state, creating a population inversion between the 3s and 3p states. Stimulated X-ray emission is initiated by slower spontaneous decay from a 3p to 3s state. Design goals are to produce a plasma with a flat electron density of approximately 5 x 10 to the 20th/cu cm, a flat temperature profile, a scale length of at least 100 microns, and a population inversion lasting at least the 100 ps necessary to produce a significant gain. Good correlation is seen between experimental data and LANEX and XRASER theoretical modeling predictions over large variations in intensity, pulse length, and probing times. No explanation is found for the weakness of the J = 0 to J = 1 lasing transition line at 18.3 nm.

  20. Performance Characteristics of Waste Glass Powder Substituting Portland Cement in Mortar Mixtures

    NASA Astrophysics Data System (ADS)

    Kara, P.; Csetényi, L. J.; Borosnyói, A.

    2016-04-01

    In the present work, soda-lime glass cullet (flint, amber, green) and special glass cullet (soda-alkaline earth-silicate glass coming from low pressure mercury-discharge lamp cullet and incandescent light bulb borosilicate glass waste cullet) were ground into fine powders in a laboratory planetary ball mill for 30 minutes. CEM I 42.5N Portland cement was applied in mortar mixtures, substituted with waste glass powder at levels of 20% and 30%. Characterisation and testing of waste glass powders included fineness by laser diffraction particle size analysis, specific surface area by nitrogen adsorption technique, particle density by pycnometry and chemical analysis by X-ray fluorescence spectrophotometry. Compressive strength, early age shrinkage cracking and drying shrinkage tests, heat of hydration of mortars, temperature of hydration, X-ray diffraction analysis and volume stability tests were performed to observe the influence of waste glass powder substitution for Portland cement on physical and engineering properties of mortar mixtures.

  1. High Mass X-ray Binary Pulsars

    NASA Astrophysics Data System (ADS)

    Naik, Sachindra

    2016-07-01

    High Mass X-ray Binaries (HMXBs) are interesting objects that provide a wide range of observational probes to the nature of the two stellar components, accretion process, stellar wind and orbital parameters of the systems. Most of the transient HMXBs are found to Be/X-ray binaries (~67%), consisting of a compact object (neutron star) in orbit around the companion Be star. The orbit of the compact object around the Be star is wide and highly eccentric. Be/X-ray binaries are generally quiescent in X-ray emission. The transient X-ray outbursts seen in these objects are known to be due to interaction between the compact object and the circumstellar disk surrounding the Be star. In the recent years, another class of transient HMXBs have been found which have supergiant companions and show shorter X-ray outbursts. X-ray, infrared and optical observations of these HMXBs provide vital information regarding these systems. The timing and broad-band X-ray spectral properties of a few HMXB pulsars, mainly Be/X-ray binary pulsars during regular X-ray outbursts will be discussed.

  2. Controlling X-rays With Light

    SciTech Connect

    Glover, Ernie; Hertlein, Marcus; Southworth, Steve; Allison, Tom; van Tilborg, Jeroen; Kanter, Elliot; Krassig, B.; Varma, H.; Rude, Bruce; Santra, Robin; Belkacem, Ali; Young, Linda

    2010-08-02

    Ultrafast x-ray science is an exciting frontier that promises the visualization of electronic, atomic and molecular dynamics on atomic time and length scales. A largelyunexplored area of ultrafast x-ray science is the use of light to control how x-rays interact with matter. In order to extend control concepts established for long wavelengthprobes to the x-ray regime, the optical control field must drive a coherent electronic response on a timescale comparable to femtosecond core-hole lifetimes. An intense field is required to achieve this rapid response. Here an intense optical control pulse isobserved to efficiently modulate photoelectric absorption for x-rays and to create an ultrafast transparency window. We demonstrate an application of x-ray transparencyrelevant to ultrafast x-ray sources: an all-photonic temporal cross-correlation measurement of a femtosecond x-ray pulse. The ability to control x-ray/matterinteractions with light will create new opportunities at current and next-generation x-ray light sources.

  3. Controlling x-rays with light.

    SciTech Connect

    Glover, T. E.; Hertlein, M. P.; Southworth, S. H.; Allison, T. K.; van Tilborg, J.; Kanter, E. P.; Krassig, B.; Varma, H. R.; Rude, B.; Santra, R.; Belkacem, A.; Young, L.; Chemical Sciences and Engineering Division; LBNL; Univ. of California at Berkley; Univ. of Chicago

    2010-01-01

    Ultrafast X-ray science is an exciting frontier that promises the visualization of electronic, atomic and molecular dynamics on atomic time and length scales. A largely unexplored area of ultrafast X-ray science is the use of light to control how X-rays interact with matter. To extend control concepts established for long-wavelength probes to the X-ray regime, the optical control field must drive a coherent electronic response on a timescale comparable to femtosecond core-hole lifetimes. An intense field is required to achieve this rapid response. Here, an intense optical control pulse is observed to efficiently modulate photoelectric absorption for X-rays and to create an ultrafast transparency window. We demonstrate an application of X-ray transparency relevant to ultrafast X-ray sources: an all-photonic temporal cross-correlation measurement of a femtosecond X-ray pulse. The ability to control X-ray-matter interactions with light will create new opportunities for present and next-generation X-ray light sources.

  4. Arsenate adsorption mechanisms at the allophane - Water interface

    USGS Publications Warehouse

    Arai, Y.; Sparks, D.L.; Davis, J.A.

    2005-01-01

    We investigated arsenate (As(V)) reactivity and surface speciation on amorphous aluminosilicate mineral (synthetic allophane) surfaces using batch adsorption experiments, powder X-ray diffraction (XRD), and X-ray absorption spectroscopy (XAS). The adsorption isotherm experiments indicated that As(V) uptake increased with increasing [As(V)]0 from 50 to 1000 ??M (i.e., Langmuir type adsorption isotherm) and that the total As adsorption slightly decreased with increasing NaCl concentrations from 0.01 to 0.1 M. Arsenate adsorption was initially (0-10 h) rapid followed by a slow continuum uptake, and the adsorption processes reached the steady state after 720 h. X-ray absorption spectroscopic analyses suggest that As(V) predominantly forms bidentate binuclear surface species on aluminum octahedral structures, and these species are stable up to 11 months. Solubility calculations and powder XRD analyses indicate no evidence of crystalline AI-As(V) precipitates in the experimental systems. Overall, macroscopic and spectroscopic evidence suggest that the As(V) adsorption mechanisms at the allophane-water interface are attributable to ligand exchange reactions between As(V) and surface-coordinated water molecules and hydroxyl and silicate ions. The research findings imply that dissolved tetrahedral oxyanions (e.g., H2PO42- and H2AsO42-) are readily retained on amorphous aluminosilicate minerals in aquifer and soils at near neutral pH. The innersphere adsorption mechanisms might be important in controlling dissolved arsenate and phosphate in amorphous aluminosilicate-rich low-temperature geochemical environments. ?? 2005 American Chemical Society.

  5. Analysis of tungsten carbides by X-ray fluorescence spectrometry.

    PubMed

    Kinson, K; Knott, A C; Belcher, C B

    Five sample presentation techniques were examined for the X-ray fluorescence spectrometric analysis of tungsten carbide alloys in powder and cemented forms. Powder samples may be oxidized by air at 600 degrees before fusion (I), or preferably by lithium nitrate during fusion (II); the fusion is effected with lithium-lanthanum tetraborate followed by briquetting with graphite. Powder samples may also be blended with wax and briquetted (III). Cemented carbides are surface-prepared with silicon carbide before analysis (V). Briquettes prepared by blending carbide powder, lithium-lanthanum tetraborate and graphite (IV), give poor reproducibility, however, owing to micro-absorption effects the technique is not recommended. The determination of eight common elements in tungsten carbide is discussed and the relative standard deviations are 0.002-0.004 for major and 0.008-0.01 for minor elements. PMID:18961988

  6. Scintillator characterization using the LBL Pulsed X-ray Facility

    SciTech Connect

    Moses, W.W.; Derenzo, S.E.; Weber, M.J.; Blankespoor, S.C.; Ho, M.H.; West, A.C.

    1994-10-01

    The authors have developed a bench-top pulsed x-ray system for measuring scintillation properties of compounds in crystal or powdered form. The source is a light-excited x-ray tube that produces 40 x-ray photons (mean energy 18.5 keV) per steradian in each 100 ps fwhm pulse. The repetition rate is adjustable from 0 to 10{sup 7} pulses per second. The fluorescent emanations from the x-ray excited samples are detected with either a sapphire-windowed microchannel plate photomultiplier tube (spectral range 150--650 nm, transit time jitter 40 ps fwhm) or a quartz windowed GaAs(Cs) photomultiplier tube (spectral range 160--930 nm, transit time jitter 4 ns fwhm). Decay time spectra are acquired using a TDC Havina 40 ps fwhm resolution over a 84 ms dynamic range. A computer controlled monochromator can be inserted into the optical path to measure the emission spectrum or wavelength resolved decay time spectrum. A computer controlled sample changer allows up to 64 samples to be measured without intervention.

  7. Diffractive X-Ray Telescopes

    NASA Technical Reports Server (NTRS)

    Skinner, Gerald K.

    2010-01-01

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

  8. Industrial X-Ray Imaging

    NASA Technical Reports Server (NTRS)

    1997-01-01

    In 1990, Lewis Research Center jointly sponsored a conference with the U.S. Air Force Wright Laboratory focused on high speed imaging. This conference, and early funding by Lewis Research Center, helped to spur work by Silicon Mountain Design, Inc. to break the performance barriers of imaging speed, resolution, and sensitivity through innovative technology. Later, under a Small Business Innovation Research contract with the Jet Propulsion Laboratory, the company designed a real-time image enhancing camera that yields superb, high quality images in 1/30th of a second while limiting distortion. The result is a rapidly available, enhanced image showing significantly greater detail compared to image processing executed on digital computers. Current applications include radiographic and pathology-based medicine, industrial imaging, x-ray inspection devices, and automated semiconductor inspection equipment.

  9. Use of x-ray imaging for evaluation of superconducting ceramics fabricated by PIT method

    SciTech Connect

    Ingerly, D.B.; Ellingson, W.A.; Vasanthamohan, N.; Wu, C.

    1993-08-01

    High-spatial-resolution microfocus-based X-ray imaging technology, both real-time and film, has been used to study the thickness variation that occurs in the oxide core of silver-sheathed BSCCO ribbons produced by the powder-in-tube method. This thickness variation (also called ``sausaging``) occurs during incremental rolling and degrades the critical current densities of the ribbons. Using X-ray image data the authors determined the onset and severity of sausaging. Onset occurred at a ribbon thickness of 203 {micro}m, and the severity increased with subsequent rolling reductions. Scanning electron microscopy was used to confirm the X-ray image data. X-ray imaging provides several advantages over more traditional methods for characterizing the superconductors such as optical or scanning electron microscopy. The X-ray imaging provides nondestructive information about the entire width of the ribbon, with far greater speed, lower cost, and more flexibility than the traditional techniques.

  10. Soft x-ray interferometry

    SciTech Connect

    Not Available

    1993-09-01

    The purpose of the soft x-ray interferometry workshop held at Lawrence Berkeley Laboratory was to discuss with the scientific community the proposed technical design of the soft x-ray Fourier-transform spectrometer being developed at the ALS. Different design strategies for the instrument`s components were discussed, as well as detection methods, signal processing issues, and how to meet the manufacturing tolerances that are necessary for the instrument to achieve the desired levels of performance. Workshop participants were encouraged to report on their experiences in the field of Fourier transform spectroscopy. The ALS is developing a Fourier transform spectrometer that is intended to operate up to 100 eV. The motivation is solely improved resolution and not the throughput (Jaquinot) or multiplex (Fellgett) advantage, neither of which apply for the sources and detectors used in this spectral range. The proposed implementation of this is via a Mach-Zehnder geometry that has been (1) distorted from a square to a rhombus to get grazing incidence of a suitable angle for 100 eV and (2) provided with a mirror-motion system to make the path difference between the interfering beams tunable. The experiment consists of measuring the emergent light intensity (I(x)) as a function of the path difference (x). The resolving power of the system is limited by the amount of path difference obtainable that is 1 cm (one million half-waves at 200{angstrom} wavelength) in the design thus allowing a resolving power of one million. The free spectral range of the system is limited by the closeness with which the function I(x) is sampled. It is proposed to illuminate a helium absorption cell with roughly 1%-band-width light from a monochromator thus allowing one hundred aliases without spectral overlap even for sampling of I(x) at one hundredth of the Nyquist frequency.

  11. Thermodynamic and kinetic behaviors of trinitrotoluene adsorption on powdered activated carbons

    SciTech Connect

    Lee, J.W.; Hwang, K.J.; Shim, W.G.; Moon, I.S.

    2006-07-01

    Regulations on the removal of trinitrotoluene (TNT) from wastewater have become increasingly more stringent, demanding faster, less expensive, and more efficient treatment. This study focuses on the adsorption equilibrium and kinetics of TNT on powered activated carbons (PAC). Three types of PACs (i.e., wood based, coal based, and coconut-shell based) were studied as functions of temperature and pH. Thermodynamic properties including Gibbs free energy, enthalpy, and entropy, were evaluated by applying the Van't Hoff equation. In addition, the adsorption energy distribution functions which describe heterogeneous characteristics of porous solid sorbents were calculated by using the generalized nonlinear regularization method. Adsorption kinetic studies were carried out in batch adsorber under important conditions such as PAC types, temperature, pH, and concentration. We found that fast and efficient removal of TNT dissolved in water can be successfully achieved by PAC adsorption.

  12. Late B Star X-Ray Sources

    NASA Astrophysics Data System (ADS)

    Walter, Frederick M.

    The most basic conclusion to be drawn from the EINSTEIN stellar X-ray observations was that all stars are X-ray sources - except the late-B and early- to mid-A stars. While this is still true in general, observations with the ROSAT X-ray observatory have shown that young late-B/early-A stars, those in and near regions of star formation, are often bright X-ray sources. It is not yet clear why (or, indeed, whether) young B-A stars are often X-ray sources. We request time on the IUE to observe a sample of these stars. We will compare the line profiles against B star models against archival spectra, looking for evidence of mass loss or mass inflows, as well as evidence of transition region gas. Detection of the latter will prove that the B stars are indeed X-ray sources.

  13. Stimulated Electronic X-Ray Raman Scattering

    NASA Astrophysics Data System (ADS)

    Weninger, Clemens; Purvis, Michael; Ryan, Duncan; London, Richard A.; Bozek, John D.; Bostedt, Christoph; Graf, Alexander; Brown, Gregory; Rocca, Jorge J.; Rohringer, Nina

    2013-12-01

    We demonstrate strong stimulated inelastic x-ray scattering by resonantly exciting a dense gas target of neon with femtosecond, high-intensity x-ray pulses from an x-ray free-electron laser (XFEL). A small number of lower energy XFEL seed photons drive an avalanche of stimulated resonant inelastic x-ray scattering processes that amplify the Raman scattering signal by several orders of magnitude until it reaches saturation. Despite the large overall spectral width, the internal spiky structure of the XFEL spectrum determines the energy resolution of the scattering process in a statistical sense. This is demonstrated by observing a stochastic line shift of the inelastically scattered x-ray radiation. In conjunction with statistical methods, XFELs can be used for stimulated resonant inelastic x-ray scattering, with spectral resolution smaller than the natural width of the core-excited, intermediate state.

  14. Deep Extragalactic X-Ray Surveys

    NASA Astrophysics Data System (ADS)

    Brandt, W. N.; Hasinger, G.

    2005-09-01

    Deep surveys of the cosmic X-ray background are reviewed in the context of observational progress enabled by the Chandra X-Ray Observatory and the X-Ray Multi-Mirror Mission-Newton. The sources found by deep surveys are described along with their redshift and luminosity distributions, and the effectiveness of such surveys at selecting active galactic nuclei (AGN) is assessed. Some key results from deep surveys are highlighted, including (a) measurements of AGN evolution and the growth of supermassive black holes, (b) constraints on the demography and physics of high-redshift AGN, (c) the X-ray AGN content of infrared and submillimeter galaxies, and (d) X-ray emission from distant starburst and normal galaxies. We also describe some outstanding problems and future prospects for deep extragalactic X-ray surveys.

  15. Soft x-ray polarimeter laboratory tests

    NASA Astrophysics Data System (ADS)

    Murphy, Kendrah D.; Marshall, Herman L.; Schulz, Norbert S.; Jenks, Kevin; Sommer, Sophie J. B.; Marshall, Eric A.

    2010-07-01

    Multilayer-coated optics can strongly polarize X-rays and are central to a new design of a broad-band, soft X-ray polarimeter. We have begun laboratory work to verify the performance of components that could be used in future soft X-ray polarimetric instrumentation. We have reconfigured a 17 meter beamline facility, originally developed for testing transmission gratings for Chandra, to include a polarized X-ray source, an X-ray-dispersing transmission grating, and a multilayer-coated optic that illuminates a CCD detector. The X-rays produced from a Manson Model 5, multi-anode source are polarized by a multilayer-coated flat mirror. The current configuration allows for a 180 degree rotation of the source in order to rotate the direction of polarization. We will present progress in source characterization and system modulation measurements as well as null and robustness tests.

  16. Time resolved x-ray detection

    NASA Astrophysics Data System (ADS)

    Rentzepis, Peter M.

    1994-04-01

    The goal of the project was to design, develop and construct an x-ray detector with high sensitivity and picosecond time resolution. This was achieved. A Ford Aerospace Charged Coupled Device, CCD, was utilized as the x-ray sensitive material around which the design and construction of the picosecond x-ray detector was built. This device has now become a commercial product sold, among other companies, by Photometrics Inc., and Princeton Research Inc. In addition we designed and built the first picosecond x-ray system. This system was utilized for the first ever picosecond x-ray diffraction experiments. The picosecond x-ray system was utilized in the oxidative fuel cell project to measure the decomposition of methanol and the change of the structure of its platinum catalyst. Another direct product of the work is the publication of 36 papers, in major scientific journals, and two patents.

  17. X-rays for medical use

    NASA Astrophysics Data System (ADS)

    Hessenbruch, A.

    1995-11-01

    1995 is the centenary of the discovery of X-rays by the German physicist Wilhelm C Rontgen. In the past hundred years, the new rays have developed from being unknown to finding application in many walks of life, not least in medicine. This is so much so that in common speech the word `x-ray` refers not to a form of radiation but to an X-ray photograph taken for the purposes of diagnosis (as in: `I had an X-ray done to see if my leg was broken`). X-rays are now used routinely, and they are used both for diagnosis and for therapy. This paper will give an outline of the use of X-rays in medicine throughout our present century.

  18. Hard X-ray imaging from Explorer

    NASA Technical Reports Server (NTRS)

    Grindlay, J. E.; Murray, S. S.

    1981-01-01

    Coded aperture X-ray detectors were applied to obtain large increases in sensitivity as well as angular resolution. A hard X-ray coded aperture detector concept is described which enables very high sensitivity studies persistent hard X-ray sources and gamma ray bursts. Coded aperture imaging is employed so that approx. 2 min source locations can be derived within a 3 deg field of view. Gamma bursts were located initially to within approx. 2 deg and X-ray/hard X-ray spectra and timing, as well as precise locations, derived for possible burst afterglow emission. It is suggested that hard X-ray imaging should be conducted from an Explorer mission where long exposure times are possible.

  19. Effect of carboxylic acid adsorption on the hydrolysis and sintered properties of aluminum nitride powder

    SciTech Connect

    Egashira, Makoto; Shimizu, Yasuhiro; Takao, Yuji; Yamaguchi, Ryoji; Ishikawa, Yasuhiro . Dept. of Materials Science and Engineering)

    1994-07-01

    To suppress the reactivity of AlN powder with water, chemical surface modification with carboxylic acids has been investigated. It was found that the chemical stability of AlN powder increased as the number of carbon atoms in carboxylic acids used for the surface treatment increased. Among the carboxylic acids tested, stearic acid was the most promising from the viewpoint of the chemical stability of the treated powder and the thermal conductivity of the sintered ceramics prepared by cold isostatic pressing and pressureless sintering.

  20. Preparation of titanium peroxide and its selective adsorption property on cationic dyes

    NASA Astrophysics Data System (ADS)

    Zhao, Xiao-guang; Huang, Ji-guo; Wang, Bo; Bi, Qiang; Dong, Li-li; Liu, Xing-juan

    2014-02-01

    Titanium peroxide powder was prepared with the reaction of titanium sulfate and H2O2 and showed good selective adsorption property on cationic dyes. The obtained material was characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS) and thermogravimetric and differential scanning calorimetry (TG-DSC). The selective adsorption property was confirmed and evaluated by adsorption experiments of methyl orange (MO), phenol and three kinds of cationic dyes including methylene blue (MB), malachite green (MG) and neutral red (NR). The adsorption was very fast and adsorption equilibrium was reached in a very short time for all three cationic dyes. The adsorption kinetics of MB, MG and NR were studied then. It was found that the adsorption data fitted perfectly with the pseudo-second-order kinetics and the saturated adsorption capacities for MB, MG and NR were 224.37, 251.38 and 327.61 mg/g at 25 °C, respectively. The characterization and adsorption results indicated the controlling mechanism of adsorption processes could be electrostatic adsorption.

  1. Topological X-Rays and MRIs

    ERIC Educational Resources Information Center

    Lynch, Mark

    2002-01-01

    Let K be a compact subset of the interior of the unit disk D in the plane and suppose one can't see through the boundary of D and identify K. However, assume that one can take "topological X-rays" of D which measure the "density" of K along the lines of the X-rays. By taking these X-rays from all directions, a "topological MRI" is generated for…

  2. X ray microcalorimeters: Principles and performance

    NASA Technical Reports Server (NTRS)

    Moseley, S. H.; Juda, M.; Kelley, R. L.; Mccammon, D.; Stahle, C. K.; Szymkowiak, A. E.; Zhang, J.

    1992-01-01

    Microcalorimeters operating at cryogenic temperatures can be excellent X-ray spectrometers. They simultaneously offer very high spectral resolving power and high efficiency. These attributes are important for X-ray astronomy where most sources have low fluxes and where high spectral resolution is essential for understanding the physics of the emitting regions. The principles of operation of these detectors, limits to their sensitivity, design considerations, techniques of fabrication, and their performance as X-ray spectrometers, are reviewed.

  3. High speed x-ray beam chopper

    DOEpatents

    McPherson, Armon; Mills, Dennis M.

    2002-01-01

    A fast, economical, and compact x-ray beam chopper with a small mass and a small moment of inertia whose rotation can be synchronized and phase locked to an electronic signal from an x-ray source and be monitored by a light beam is disclosed. X-ray bursts shorter than 2.5 microseconds have been produced with a jitter time of less than 3 ns.

  4. X-ray data booklet. Revision

    SciTech Connect

    Vaughan, D.

    1986-04-01

    A compilation of data is presented. Included are properties of the elements, electron binding energies, characteristic x-ray energies, fluorescence yields for K and L shells, Auger energies, energy levels for hydrogen-, helium-, and neonlike ions, scattering factors and mass absorption coefficients, and transmission bands of selected filters. Also included are selected reprints on scattering processes, x-ray sources, optics, x-ray detectors, and synchrotron radiation facilities. (WRF)

  5. Lobster-Eye X-Ray Astronomy

    SciTech Connect

    Hudec, R.; Pina, L.; Marsikova, V.; Inneman, A.

    2010-07-15

    We report on technical and astrophysical aspects of Lobster-Eye wide-field X-ray telescopes expected to monitor the sky with high sensitivity and angular resolution of order of 1 arcmin. They will contribute essentially to study of various astrophysical objects such as AGN, SNe, Gamma-ray bursts (GRBs), X-ray flashes (XRFs), galactic binary sources, stars, CVs, X-ray novae, various transient sources, etc.

  6. X-ray microlaminography with polycapillary optics

    NASA Astrophysics Data System (ADS)

    Dąbrowski, K. M.; Dul, D. T.; Wróbel, A.; Korecki, P.

    2013-06-01

    We demonstrate layer-by-layer x-ray microimaging using polycapillary optics. The depth resolution is achieved without sample or source rotation and in a way similar to classical tomography or laminography. The method takes advantage from large angular apertures of polycapillary optics and from their specific microstructure, which is treated as a coded aperture. The imaging geometry is compatible with polychromatic x-ray sources and with scanning and confocal x-ray fluorescence setups.

  7. Applications of soft x-ray lasers

    SciTech Connect

    Skinner, C.H.

    1993-08-01

    The high brightness and short pulse duration of soft x-ray lasers provide unique advantages for novel applications. Imaging of biological specimens using x-ray lasers has been demonstrated by several groups. Other applications to fields such as chemistry, material science, plasma diagnostics, and lithography are beginning to emerge. We review the current status of soft x-ray lasers from the perspective of applications, and present an overview of the applications currently being developed.

  8. X-ray transmissive debris shield

    DOEpatents

    Spielman, Rick B.

    1994-01-01

    A composite window structure is described for transmitting x-ray radiation and for shielding radiation generated debris. In particular, separate layers of different x-ray transmissive materials are laminated together to form a high strength, x-ray transmissive debris shield which is particularly suited for use in high energy fluences. In one embodiment, the composite window comprises alternating layers of beryllium and a thermoset polymer.

  9. Hard X-ray irradiation of cosmic silicate analogs: structural evolution and astrophysical implications

    NASA Astrophysics Data System (ADS)

    Gavilan, L.; Jäger, C.; Simionovici, A.; Lemaire, J. L.; Sabri, T.; Foy, E.; Yagoubi, S.; Henning, T.; Salomon, D.; Martinez-Criado, G.

    2016-03-01

    Context. Protoplanetary disks, interstellar clouds, and active galactic nuclei contain X-ray-dominated regions. X-rays interact with the dust and gas present in such environments. While a few laboratory X-ray irradiation experiments have been performed on ices, X-ray irradiation experiments on bare cosmic dust analogs have been scarce up to now. Aims: Our goal is to study the effects of hard X-rays on cosmic dust analogs via in situ X-ray diffraction. By using a hard X-ray synchrotron nanobeam, we seek to simulate cumulative X-ray exposure on dust grains during their lifetime in these astrophysical environments and provide an upper limit on the effect of hard X-rays on dust grain structure. Methods: We prepared enstatite (MgSiO3) nanograins, which are analogs to cosmic silicates, via the melting-quenching technique. These amorphous grains were then annealed to obtain polycrystalline grains. These were characterized via scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM) before irradiation. Powder samples were prepared in X-ray transparent substrates and were irradiated with hard X-rays nanobeams (29.4 keV) provided by beamline ID16B of the European Synchrotron Radiation Facility (Grenoble). X-ray diffraction images were recorded in transmission mode, and the ensuing diffractograms were analyzed as a function of the total X-ray exposure time. Results: We detected the amorphization of polycrystalline silicates embedded in an organic matrix after an accumulated X-ray exposure of 6.4 × 1027 eV cm-2. Pure crystalline silicate grains (without resin) do not exhibit amorphization. None of the amorphous silicate samples (pure and embedded in resin) underwent crystallization. We analyze the evolution of the polycrystalline sample embedded in an organic matrix as a function of X-ray exposure. Conclusions: Loss of diffraction peak intensity, peak broadening, and the disappearance of discrete spots and arcs reveal the amorphization

  10. Observation of femtosecond X-ray interactions with matter using an X-ray-X-ray pump-probe scheme.

    PubMed

    Inoue, Ichiro; Inubushi, Yuichi; Sato, Takahiro; Tono, Kensuke; Katayama, Tetsuo; Kameshima, Takashi; Ogawa, Kanade; Togashi, Tadashi; Owada, Shigeki; Amemiya, Yoshiyuki; Tanaka, Takashi; Hara, Toru; Yabashi, Makina

    2016-02-01

    Resolution in the X-ray structure determination of noncrystalline samples has been limited to several tens of nanometers, because deep X-ray irradiation required for enhanced resolution causes radiation damage to samples. However, theoretical studies predict that the femtosecond (fs) durations of X-ray free-electron laser (XFEL) pulses make it possible to record scattering signals before the initiation of X-ray damage processes; thus, an ultraintense X-ray beam can be used beyond the conventional limit of radiation dose. Here, we verify this scenario by directly observing femtosecond X-ray damage processes in diamond irradiated with extraordinarily intense (∼10(19) W/cm(2)) XFEL pulses. An X-ray pump-probe diffraction scheme was developed in this study; tightly focused double-5-fs XFEL pulses with time separations ranging from sub-fs to 80 fs were used to excite (i.e., pump) the diamond and characterize (i.e., probe) the temporal changes of the crystalline structures through Bragg reflection. It was found that the pump and probe diffraction intensities remain almost constant for shorter time separations of the double pulse, whereas the probe diffraction intensities decreased after 20 fs following pump pulse irradiation due to the X-ray-induced atomic displacement. This result indicates that sub-10-fs XFEL pulses enable conductions of damageless structural determinations and supports the validity of the theoretical predictions of ultraintense X-ray-matter interactions. The X-ray pump-probe scheme demonstrated here would be effective for understanding ultraintense X-ray-matter interactions, which will greatly stimulate advanced XFEL applications, such as atomic structure determination of a single molecule and generation of exotic matters with high energy densities. PMID:26811449

  11. A comparative investigation of Lu2SiO5:Ce and Gd2O2S:Eu powder scintillators for use in x-ray mammography detectors

    NASA Astrophysics Data System (ADS)

    Michail, C. M.; Fountos, G. P.; David, S. L.; Valais, I. G.; Toutountzis, A. E.; Kalyvas, N. E.; Kandarakis, I. S.; Panayiotakis, G. S.

    2009-10-01

    The dominant powder scintillator in most medical imaging modalities for decades has been Gd2O2S:Tb due to the very good intrinsic properties and overall efficiency. Apart from Gd2O2S:Tb, there are alternative powder phosphor scintillators such as Lu2SiO5:Ce and Gd2O2S:Eu that have been suggested for use in various medical imaging modalities. Gd2O2S:Eu emits red light and can be combined mainly with digital mammography detectors such as CCDs. Lu2SiO5:Ce emits blue light and can be combined with blue sensitivity films, photocathodes and some photodiodes. For the purposes of the present study, two scintillating screens, one from Lu2SiO5:Ce and the other from Gd2O2S:Eu powders, were prepared using the method of sedimentation. The screen coating thicknesses were 25.0 and 33.1 mg cm-2 respectively. The screens were investigated by evaluating the following parameters: the output signal, the modulation transfer function, the noise equivalent passband, the informational efficiency, the quantum detection efficiency and the zero-frequency detective quantum efficiency. Furthermore, the spectral compatibility of those materials with various optical detectors was determined. Results were compared to published data for the commercially employed 'Kodak Min-R film-screen system', based on a 31.7 mg cm-2 thick Gd2O2S:Tb phosphor. For Gd2O2S:Eu, MTF data were found comparable to those of Gd2O2S:Tb, while the MTF of Lu2SiO5:Ce was even higher resulting in better spatial resolution and image sharpness properties. On the other hand, Gd2O2S:Eu was found to exhibit higher output signal and zero-frequency detective quantum efficiency than Lu2SiO5:Ce.

  12. Compound refractive X-ray lens

    DOEpatents

    Nygren, David R.; Cahn, Robert; Cederstrom, Bjorn; Danielsson, Mats; Vestlund, Jonas

    2000-01-01

    An apparatus and method for focusing X-rays. In one embodiment, his invention is a commercial-grade compound refractive X-ray lens. The commercial-grade compound refractive X-ray lens includes a volume of low-Z material. The volume of low-Z material has a first surface which is adapted to receive X-rays of commercially-applicable power emitted from a commercial-grade X-ray source. The volume of low-Z material also has a second surface from which emerge the X-rays of commercially-applicable power which were received at the first surface. Additionally, the commercial-grade compound refractive X-ray lens includes a plurality of openings which are disposed between the first surface and the second surface. The plurality of openings are oriented such that the X-rays of commercially-applicable power which are received at the first surface, pass through the volume of low-Z material and through the plurality openings. In so doing, the X-rays which emerge from the second surface are refracted to a focal point.

  13. Bent crystal X-ray topography

    NASA Technical Reports Server (NTRS)

    Parker, D. L.

    1978-01-01

    A television X-ray topographic camera system was constructed. The system differs from the previous system in that it incorporates the X-ray TV imaging system and has a semi-automatic wafer loading system. Also the X-ray diffraction is in a vertical plane. This feature makes wafer loading easier and makes the system compatible with any commercial X-ray generating system. Topographs and results obtained from a study of the diffraction contrast variation with impurity concentration for both boron implanted and boron diffused silicon are included.

  14. Symbiotic stars in X-rays

    NASA Astrophysics Data System (ADS)

    Luna, G. J. M.; Sokoloski, J. L.; Mukai, K.; Nelson, T.

    2013-11-01

    Until recently, symbiotic binary systems in which a white dwarf accretes from a red giant were thought to be mainly a soft X-ray population. Here we describe the detection with the X-ray Telescope (XRT) on the Swift satellite of nine white dwarf symbiotics that were not previously known to be X-ray sources and one that had previously been detected as a supersoft X-ray source. The nine new X-ray detections were the result of a survey of 41 symbiotic stars, and they increase the number of symbiotic stars known to be X-ray sources by approximately 30%. The Swift/XRT telescope detected all of the new X-ray sources at energies greater than 2 keV. Their X-ray spectra are consistent with thermal emission and fall naturally into three distinct groups. The first group contains those sources with a single, highly absorbed hard component that we identify as probably coming from an accretion-disk boundary layer. The second group is composed of those sources with a single, soft X-ray spectral component that probably originates in a region where low-velocity shocks produce X-ray emission, i.e., a colliding-wind region. The third group consists of those sources with both hard and soft X-ray spectral components. We also find that unlike in the optical, where rapid, stochastic brightness variations from the accretion disk typically are not seen, detectable UV flickering is a common property of symbiotic stars. Supporting our physical interpretation of the two X-ray spectral components, simultaneous Swift UV photometry shows that symbiotic stars with harder X-ray emission tend to have stronger UV flickering, which is usually associated with accretion through a disk. To place these new observations in the context of previous work on X-ray emission from symbiotic stars, we modified and extended the α/β/γ classification scheme for symbiotic-star X-ray spectra that was introduced by Muerset et al. based upon observations with the ROSAT satellite, to include a new δ classification

  15. Symbiotic Stars in X-rays

    NASA Technical Reports Server (NTRS)

    Luna, G. J. M.; Sokoloski, J. L.; Mukai, K.; Nelson, T.

    2014-01-01

    Until recently, symbiotic binary systems in which a white dwarf accretes from a red giant were thought to be mainly a soft X-ray population. Here we describe the detection with the X-ray Telescope (XRT) on the Swift satellite of 9 white dwarf symbiotics that were not previously known to be X-ray sources and one that was previously detected as a supersoft X-ray source. The 9 new X-ray detections were the result of a survey of 41 symbiotic stars, and they increase the number of symbiotic stars known to be X-ray sources by approximately 30%. Swift/XRT detected all of the new X-ray sources at energies greater than 2 keV. Their X-ray spectra are consistent with thermal emission and fall naturally into three distinct groups. The first group contains those sources with a single, highly absorbed hard component, which we identify as probably coming from an accretion-disk boundary layer. The second group is composed of those sources with a single, soft X-ray spectral component, which likely arises in a region where low-velocity shocks produce X-ray emission, i.e. a colliding-wind region. The third group consists of those sources with both hard and soft X-ray spectral components. We also find that unlike in the optical, where rapid, stochastic brightness variations from the accretion disk typically are not seen, detectable UV flickering is a common property of symbiotic stars. Supporting our physical interpretation of the two X-ray spectral components, simultaneous Swift UV photometry shows that symbiotic stars with harder X-ray emission tend to have stronger UV flickering, which is usually associated with accretion through a disk. To place these new observations in the context of previous work on X-ray emission from symbiotic stars, we modified and extended the alpha/beta/gamma classification scheme for symbiotic-star X-ray spectra that was introduced by Muerset et al. based upon observations with the ROSAT satellite, to include a new sigma classification for sources with

  16. Models for galactic X-ray sources

    NASA Technical Reports Server (NTRS)

    Joss, P. C.

    1980-01-01

    Attention is given to those compact galactic X-ray sources whose X-ray luminosities are considerably in excess of the solar luminosity. It is pointed out that the key breakthrough in the development of an understanding of compact galactic X-ray sources was the discovery of X-ray pulsars with the UHURU satellite. There is now overwhelming evidence that these objects are neutron stars in close binary stellar systems. The X-ray pulsations are thought to be thermal emission from the magnetic polar caps of a neutron star that is accreting matter from a companion star and whose magnetic field is misaligned with its rotation axis. Among the compact galactic X-ray sources that are not X-ray pulsars, some still show direct evidence of binary membership, such as X-ray eclipses. There is evidence that the galactic-bulge sources are, in fact, close binary stellar systems. It is concluded, that the great majority of bright galactic X-ray sources, with only a tiny handful of exceptions (such as the Crab and Vela pulsars), are likely to be binaries.

  17. The Lunar X-ray Observatory (LXO)

    NASA Technical Reports Server (NTRS)

    Porter, F. Scott

    2008-01-01

    X-ray emission from charge exchange recombination between the highly ionized solar wind and neutral material i n Earth's magnetosheath has complicated x-ray observations of celestial objects with x-ray observatories including ROSAT, Chandra, XMM-Newton, and Suzaku. However, the charge-exchange emission can also be used as an important diagnostic of the solar-wind interacting with the magnetosheath. Soft x-ray observations from low-earth orbit or even the highly eccentric orbits of Chandra and XMM-Newton are likely superpositions of the celestial object of interest, the true extra-solar soft x-ray background, geospheric charge exchange, and heliospheric charge exchange. We show that with a small x-ray telescope placed either on the moon, in a similar vein as the Apollo ALSOP instruments, or at a stable orbit near L1, we can begin t o disentangle the complicated emission structure in the soft x-ray band. Here we present initial results of a feasibility study recently funded by NASA t o place a small x-ray telescope on the lunar surface. The telescope operates during lunar night to observe charge exchange interactions between the solar wind and magnetospheric neutrals, between the solar wind and the lunar atmosphere, and an unobstructed view of the soft x-ray background without the geospheric component.

  18. The efficacy of x-ray pelvimetry

    SciTech Connect

    Barton, J.J.; Garbaciak, J.A. Jr.; Ryan, G.M., Jr.

    1982-06-01

    Comparison is made of x-ray pelvimetry use on a public and private service in 1974 with experience in 1979, when the clinic service did no x-ray pelvimetry while the private service continued as before. It is concluded that the use of x-ray pelvimetry is inadequate as a predictor of cesarean section because of cephalopelvic disproportion, does not improve neonatal mortality, and poses potential hazards to the mother and fetus. Its use in the management of breech presentations is not currently established by our data. Guidelines are presented for the management of patients in labor without using x-ray pelvimetry.

  19. Tenma - Japan's X-ray satellite

    NASA Astrophysics Data System (ADS)

    Simpson, C.

    1984-06-01

    Japan's second X-ray satellite, designated 'Tenma', has temporal and spectral sensitivity superior to that of its predecessor, Hakucho. It is a spin-stabilized satellite whose attitude maneuvers are performed through the activation of a magnetic torquing coil, by means of which a typical, 20-deg transfer occupies several orbits. Tenma carries as its instrument set scintillation proportional counters for spectral and temporal studies, an X-ray focusing collector for the study of very soft X-ray sources, a transient source monitor for wide-field sky monitoring, and a radiation belt monitor/gamma-ray burst detector for monitoring the non-X-ray background.

  20. X-rays from the youngest stars

    NASA Technical Reports Server (NTRS)

    Feigelson, Eric D.

    1994-01-01

    The X-ray properties of classical and weak-lined T Tauri stars are briefly reviewed, emphasizing recent results from the ROSAT satellite and prospects for ASCA. The interpretation of the high level of T Tauri X-rays as enhanced solar-type magnetic activity is discussed and criticized. The census of X-ray emitters is significantly increasing estimates of galactic star formation efficiency, and X-ray emission may be important for self-regulation of star formation. ASCA images will detect star formation regions out to several kiloparsecs and will study the magnetically heated plasma around T Tauri stars. However, images will often suffer from crowding effects.