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Sample records for adsorption powder x-ray

  1. 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.

  2. Parts per Million Powder X-ray Diffraction

    DOE PAGES

    Newman, Justin A.; Schmitt, Paul D.; Toth, Scott J.; ...

    2015-10-14

    Here in this paper we demonstrate the use of second harmonic generation (SHG) microscopy-guided synchrotron powder X-ray diffraction (PXRD) for the detection of trace crystalline active pharmaceutical ingredients in a common polymer blend. The combined instrument is capable of detecting 100 ppm crystalline ritonavir in an amorphous hydroxypropyl methylcellulose matrix with a high signal-to-noise ratio (>5000). The high spatial resolution afforded by SHG microscopy allows for the use of a minibeam collimator to reduce the total volume of material probed by synchrotron PXRD. The reduction in probed volume results in reduced background from amorphous material. The ability to detect lowmore » crystalline loading has the potential to improve measurements in the formulation pipeline for pharmaceutical solid dispersions, for which even trace quantities of crystalline active ingredients can negatively impact the stability and bioavailability of the final drug product.« less

  3. Parts per Million Powder X-ray Diffraction

    SciTech Connect

    Newman, Justin A.; Schmitt, Paul D.; Toth, Scott J.; Deng, Fengyuan; Zhang, Shijie; Simpson, Garth J.

    2015-10-14

    Here in this paper we demonstrate the use of second harmonic generation (SHG) microscopy-guided synchrotron powder X-ray diffraction (PXRD) for the detection of trace crystalline active pharmaceutical ingredients in a common polymer blend. The combined instrument is capable of detecting 100 ppm crystalline ritonavir in an amorphous hydroxypropyl methylcellulose matrix with a high signal-to-noise ratio (>5000). The high spatial resolution afforded by SHG microscopy allows for the use of a minibeam collimator to reduce the total volume of material probed by synchrotron PXRD. The reduction in probed volume results in reduced background from amorphous material. The ability to detect low crystalline loading has the potential to improve measurements in the formulation pipeline for pharmaceutical solid dispersions, for which even trace quantities of crystalline active ingredients can negatively impact the stability and bioavailability of the final drug product.

  4. 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.

  5. Fractal analysis of powder X-ray diffraction patterns

    NASA Astrophysics Data System (ADS)

    Ortiz-Cruz, A.; Santolalla, C.; Moreno, E.; de los Reyes-Heredia, J. A.; Alvarez-Ramirez, J.

    2012-02-01

    X-ray diffraction (XRD) patterns with broad background are commonly found in the characterization of materials with a certain degree of amorphicity, so the sharp intensity peaks associated with material phases are not well defined. This work used rescaled range (denoted by R/S) analysis, a method intended for fractal analysis of noisy signals, to characterize XRD patterns with broad background. It is found that XRD patterns with broad background are not random at all, but contain information on regularities expressed as autocorrelations of the intensity signal. Sol-gel alumina fired at different temperatures was used as an example to illustrate the applicability of the method. It is shown that fractal R/S analysis is able to locate angular regions that can be associated to ideal International Centre for Diffraction Data Powder Diffraction File (ICDD PDF) lines of diverse alumina phases.

  6. 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

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

    NASA Astrophysics Data System (ADS)

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

    2006-05-01

    Sepiolite is a hydrous Mg-silicate clay mineral with fibrous morphology that typically occurs as fine-grained, poorly crystalline masses. It occurs in a wide variety of geological environments and has been mined for centuries because of its many uses, e.g. in the pharmaceutical, fertilizer, and pesticide industries. Its versatile functionality derives from the large surface area and microporosity that are characteristic of the material. In recent years, sepiolite has received considerable attention with regard to the adsorption of organics, for use as a support for catalysts, as a molecular sieve, and as an inorganic membrane for ultrafiltration. Because of its fine-grained and poorly crystalline nature, it has not been possible to study sepiolite's crystal structure using single-crystal X-ray diffraction methods, and consequently many details of the structure are still not well known. In this study, Rietveld refinements using synchrotron powder X-ray diffraction data were used to investigate 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 water site. The RT structure under vacuum retained only ~1/8 of the zeolitic water and the volume decreased 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 water is lost by ~390 K, accompanied by a decrease in the a and c unit-cell parameters. Above ~600 K the sepiolite structure folds as one-half of the crystallographically bound water is lost. Rietveld refinements of the "anhydrous" sepiolite structure reveal that, in general, unit-cell parameters a, b, â and volume steadily decrease with increasing temperature; there is an obvious change in slope at ~820 K suggesting a phase

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

    PubMed

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

    2013-06-01

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

    NASA Astrophysics Data System (ADS)

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

    2013-06-01

    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).

  10. 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.

  11. Kinetic products in coordination networks: ab initio X-ray powder diffraction analysis.

    PubMed

    Martí-Rujas, Javier; Kawano, Masaki

    2013-02-19

    Porous coordination networks are materials that maintain their crystal structure as molecular "guests" enter and exit their pores. They are of great research interest with applications in areas such as catalysis, gas adsorption, proton conductivity, and drug release. As with zeolite preparation, the kinetic states in coordination network preparation play a crucial role in determining the final products. Controlling the kinetic state during self-assembly of coordination networks is a fundamental aspect of developing further functionalization of this class of materials. However, unlike for zeolites, there are few structural studies reporting the kinetic products made during self-assembly of coordination networks. Synthetic routes that produce the necessary selectivity are complex. The structural knowledge obtained from X-ray crystallography has been crucial for developing rational strategies for design of organic-inorganic hybrid networks. However, despite the explosive progress in the solid-state study of coordination networks during the last 15 years, researchers still do not understand many chemical reaction processes because of the difficulties in growing single crystals suitable for X-ray diffraction: Fast precipitation can lead to kinetic (metastable) products, but in microcrystalline form, unsuitable for single crystal X-ray analysis. X-ray powder diffraction (XRPD) routinely is used to check phase purity, crystallinity, and to monitor the stability of frameworks upon guest removal/inclusion under various conditions, but rarely is used for structure elucidation. Recent advances in structure determination of microcrystalline solids from ab initio XRPD have allowed three-dimensional structure determination when single crystals are not available. Thus, ab initio XRPD structure determination is becoming a powerful method for structure determination of microcrystalline solids, including porous coordination networks. Because of the great interest across scientific

  12. Synchrotron x-ray powder diffraction studies in pulsed magnetic fields

    NASA Astrophysics Data System (ADS)

    Frings, P.; Vanacken, J.; Detlefs, C.; Duc, F.; Lorenzo, J. E.; Nardone, M.; Billette, J.; Zitouni, A.; Bras, W.; Rikken, G. L. J. A.

    2006-06-01

    X-ray powder diffraction experiments under pulsed magnetic fields were carried out at the DUBBLE beamline (BM26B) at the ESRF. A mobile generator delivered 110kJ to the magnet coil, which was sufficient to generate peak fields of 30T. A liquid He flow cryostat allowed us to vary the sample temperature accurately between 8 and 300K. Powder diffraction patterns of several samples were recorded using 21keV monochromatic x-rays and an on-line image plate detector. Here we present the first results on the suppression of the Jahn-Teller structural distortion in TbVO4 by magnetic field. These data clearly demonstrate the feasibility of x-ray powder diffraction experiments under pulsed magnetic fields with relatively inexpensive instrumentation.

  13. Vibrational spectra, powder X-ray diffractions and physical properties of cyanide complexes with 1-ethylimidazole

    NASA Astrophysics Data System (ADS)

    Kürkçüoğlu, Güneş Süheyla; Kiraz, Fulya Çetinkaya; Sayın, Elvan

    2015-10-01

    The heteronuclear tetracyanonickelate(II) complexes of the type [M(etim)Ni(CN)4]n (hereafter, abbreviated as M-Ni-etim, M = Mn(II), Fe(II) or Co(II); etim = 1-ethylimidazole, C5H8N2) were prepared in powder form and characterized by FT-IR and Raman spectroscopy, powder X-ray diffraction (PXRD), thermal (TG; DTG and DTA), and elemental analysis techniques. The structures of these complexes were elucidated using vibrational spectra and powder X-ray diffraction patterns with the peak assignment to provide a better understanding of the structures. It is shown that the spectra are consistent with a proposed crystal structure for these compounds derived from powder X-ray diffraction measurements. Vibrational spectra of the complexes were presented and discussed with respect to the internal modes of both the etim and the cyanide ligands. The C, H and N analyses were carried out for all the complexes. Thermal behaviors of these complexes were followed using TG, DTG and DTA curves in the temperature range 30-700 °C in the static air atmosphere. The FT-IR, Raman spectra, thermal and powder X-ray analyses revealed no significant differences between the single crystal and powder forms. Additionally, electrical and magnetic properties of the complexes were investigated. The FT-IR and Raman spectroscopy, PXRD, thermal and elemental analyses results propose that these complexes are similar in structure to the Hofmann-type complexes.

  14. Vibrational spectra, powder X-ray diffractions and physical properties of cyanide complexes with 1-ethylimidazole.

    PubMed

    Kürkçüoğlu, Güneş Süheyla; Kiraz, Fulya Çetinkaya; Sayın, Elvan

    2015-10-05

    The heteronuclear tetracyanonickelate(II) complexes of the type [M(etim)Ni(CN)4]n (hereafter, abbreviated as M-Ni-etim, M=Mn(II), Fe(II) or Co(II); etim=1-ethylimidazole, C5H8N2) were prepared in powder form and characterized by FT-IR and Raman spectroscopy, powder X-ray diffraction (PXRD), thermal (TG; DTG and DTA), and elemental analysis techniques. The structures of these complexes were elucidated using vibrational spectra and powder X-ray diffraction patterns with the peak assignment to provide a better understanding of the structures. It is shown that the spectra are consistent with a proposed crystal structure for these compounds derived from powder X-ray diffraction measurements. Vibrational spectra of the complexes were presented and discussed with respect to the internal modes of both the etim and the cyanide ligands. The C, H and N analyses were carried out for all the complexes. Thermal behaviors of these complexes were followed using TG, DTG and DTA curves in the temperature range 30-700 °C in the static air atmosphere. The FT-IR, Raman spectra, thermal and powder X-ray analyses revealed no significant differences between the single crystal and powder forms. Additionally, electrical and magnetic properties of the complexes were investigated. The FT-IR and Raman spectroscopy, PXRD, thermal and elemental analyses results propose that these complexes are similar in structure to the Hofmann-type complexes.

  15. Quantitative determination of hydrate content of theophylline powder by chemometric X-ray powder diffraction analysis.

    PubMed

    Otsuka, Makoto; Kinoshita, Hajime

    2010-03-01

    The purpose of this study was to establish a calibration model to predict the hydrate content in powder materials consisting of anhydrate (theophylline anhydrate (THA)) and theophylline monohydrate (THM) by using various kinds of X-ray powder diffraction (XRPD) analytical methods. XRPD profiles were measured five times each for 11 standard samples containing of THA and THM. THM content in the standard samples was evaluated based on XRPD profiles by the diffraction peak height and area methods, and the Wakelin's and principal component regression (PCR) methods, respectively. Since THA and THM were cube- and rod-shaped particles, the standard samples consisted of THA and THM showed crystal orientation due to THM crystal shape. THA showed reproducible XRPD profiles, but THM showed fluctuating intensities in some specific peaks in the profiles. The linear calibration models were evaluated based on calibration XRPD datasets of the standard materials by various methods. In the result based on validation XRPD datasets, the order of the mean bias and the mean accuracy were peak height > peak area > Wakelin's > PCR, indicating that PCR was the best method to correct sample crystal orientation. The effectiveness of the PCR method in construction of calibration models was discussed by a scientific approach based on regression vectors.

  16. Synchrotron X-ray Powder Diffraction Studies in Pulsed Magnetic Fields

    NASA Astrophysics Data System (ADS)

    Detlefs, C.; Frings, P.; Vanacken, J.; Duc, F.; Lorenzo, J. E.; Nardone, M.; Billette, J.; Zitouni, A.; Bras, W.; Rikken, G. L. J. A.

    2007-01-01

    X-ray powder diffraction experiments under pulsed magnetic fields were carried out at the DUBBLE beamline (BM26B) at the ESRF. A mobile generator delivered 110kJ to the magnet coil, which was sufficient to generate peak fields of 30T. A liquid He flow cryostat allowed us to vary the sample temperature accurately between 8K and 300K.

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

    PubMed

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

    2016-03-01

    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.

  18. 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

  19. Femtosecond powder diffraction with a laser-driven hard X-ray source.

    PubMed

    Zamponi, F; Ansari, Z; Woerner, M; Elsaesser, T

    2010-01-18

    X-ray powder diffraction with a femtosecond time resolution is introduced to map ultrafast structural dynamics of polycrystalline condensed matter. Our pump-probe approach is based on photoexcitation of a powder sample with a femtosecond optical pulse and probing changes of its structure by diffracting a hard X-ray pulse generated in a laser-driven plasma source. We discuss the key aspects of this scheme including an analysis of detection sensitivity and angular resolution. Applying this technique to the prototype molecular material ammonium sulfate, up to 20 powder diffraction rings are recorded simultaneously with a time resolution of 100 fs. We describe how to derive transient charge density maps of the material from the extensive set of diffraction data in a quantitative way.

  20. On the origin of sharp peaks in the X-ray diffraction patterns of xanthan powders.

    PubMed

    Lad, M; Todd, T; Morris, G A; MacNaughtan, W; Sworn, G; Foster, T J

    2013-08-15

    A series of xanthans containing different levels of the charged group pyruvate has been examined. The X-ray diffraction patterns of the powders of these materials had different levels of a sharp pattern superimposed on an amorphous background. As the moisture content increased so the intensity of the sharp pattern increased up to a level between 20% and 40% moisture content where the sharp pattern disappeared. X-ray diffraction pattern identification software and an inorganic X-ray diffraction database showed the origin of the sharp peaks to be due to sodium sulphate polymorphs. The behaviour of the xanthans was thought to be due to the differences in charge on the molecule; however, the increase in the crystalline component observed with increased amounts of water was unexpected. The possibility of the drying of samples was considered but the interplay between ions, the charged polymer and the water present was considered necessary to more closely describe the results.

  1. Synchrotron X-ray Powder Diffraction and Absorption Spectroscopy in Pulsed Magnetic Fields with Milliseconds Duration

    NASA Astrophysics Data System (ADS)

    Vanacken, J.; Detlefs, C.; Mathon, O.; Frings, P.; Duc, F.; Lorenzo, J. E.; Nardone, M.; Billette, J.; Zitouni, A.; Dominguez, M.-C.; Herczeg, J.; Bras, W.; Moshchalkov, V. V.; Rikken, G.

    2007-03-01

    X-ray Powder Diffraction and X-ray Absorption Spectroscopy experiments (WAS) and X-ray magnetic circular dichroism (XMCD) experiments were carried out at the ESRF DUBBLE beam line (BM26) and at the energy dispersive beam line (ID24), respectively. A mobile pulse generator, developed at the LNCMP, delivered 110kJ to the load coil, which was sufficient to generate peak fields of 30T with a rise time of about 5 ms. A liquid He flow cryostat allowed us to vary the sample temperature accurately between 4.2K and 300K. Powder diffraction patterns of TbVO4 were recorded in a broad temperature range using 21 keV monochromatic X-rays and using an on-line image plate detector. We observed the suppression of the Jahn-Teller structural distortion in TbVO4 due to the high magnetic pulsed field. XAS spectra could be measured and finite XMCD signals, directly proportional to the magnetic moment on the Gd absorber atom, were measured in thin Gd foils. Thanks to its element and orbital selectivity, XMCD proofs to be very useful in probing the magnetic properties and due to the strong brilliance of the synchrotron beam, the signals can be measured even in the ms range.

  2. A Mössbauer and X-ray powder diffraction study of some ferrous hematinics.

    PubMed

    Coe, E M; Bowen, L H; Bereman, R D

    1995-06-01

    Iron deficiency anemia is a relatively common illness that can arise from a number of different causes. Three ferrous salts are usually used in its treatment: ferrous fumarate, gluconate, and sulfate. They are administered orally and are relatively well tolerated. These hematinics have been studied by Mössbauer spectroscopy and X-ray powder diffraction, and can easily be distinguished by both techniques. It was found that the two ferrous sulfates studied (Eckerd and SmithKline Beckman Co.) most closely resemble the monohydrate by comparison of the X-ray powder pattern with those of the JCPDS. Both the ferrous fumarate (Femiron) and gluconate (Spring Valley) had approximately 10% ferric iron present. To the authors' knowledge, this is the first reported Mössbauer spectrum for ferrous fumarate.

  3. X-ray powder diffraction patterns for certain beta-lactam, tetracycline and macrolide antibiotic drugs.

    PubMed

    Thangadurai, S; Abraham, J T; Srivastava, A K; Moorthy, M Nataraja; Shukla, S K; Anjaneyulu, Y

    2005-07-01

    X-ray powder diffraction (XRD) data for eight beta-lactam viz., ampicillin sodium, ampicillin trihydrate, penicillin G procaine, benzathine penicillin, benzyl penicillin sodium, cefalexin, cefotaxime sodium and ceftriaxone sodium; three tetracyclines viz., doxycycline hydrochloride, oxytetracycline dihydrate and tetracycline hydrochloride; and two macrolide viz., azithromycin and erythromycin estolate antibiotic drugs were obtained using a powder diffractometer. The drugs were scanned from Bragg angles (2theta) of 10 degrees to 70 degrees. The obtained data were tabulated in terms of the lattice spacing (A) and relative line intensities (I/I(I)). This new information may be useful for identifying these drugs from confiscated materials, which has been frequently encountered in forensic laboratories.

  4. Adsorption of mercury on lignin: combined surface complexation modeling and X-ray absorption spectroscopy studies.

    PubMed

    Lv, Jitao; Luo, Lei; Zhang, Jing; Christie, Peter; Zhang, Shuzhen

    2012-03-01

    Adsorption of mercury (Hg) on lignin was studied at a range of pH values using a combination of batch adsorption experiments, a surface complexation model (SCM) and synchrotron X-ray absorption spectroscopy (XAS). Surface complexation modeling indicates that three types of acid sites on lignin surfaces, namely aliphatic carboxylic-, aromatic carboxylic- and phenolic-type surface groups, contributed to Hg(II) adsorption. The bond distance and coordination number of Hg(II) adsorption samples at pH 3.0, 4.0 and 5.5 were obtained from extended X-ray absorption fine structure (EXAFS) spectroscopy analysis. The results of SCM and XAS combined reveal that the predominant adsorption species of Hg(II) on lignin changes from HgCl(2)(0) to monodentate complex -C-O-HgCl and then bidentate complex -C-O-Hg-O-C- with increasing pH value from 2.0 to 6.0. The good agreement between SCM and XAS results provides new insight into understanding the mechanisms of Hg(II) adsorption on lignin.

  5. 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.

  6. Powder x ray diffraction patterns of energetic materials for use as reference standards

    NASA Astrophysics Data System (ADS)

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

    1993-03-01

    This report lists eighteen quality powder x-ray diffraction patterns produced at Mound for various explosives of recent and current interest. In each case the best possible experimental pattern, obtained from the substance in question via automated diffractometric step-scans, was compared with the corresponding pattern, calculated from the lattice and atomic positional parameters of the crystal structure, if known, and a reconciliation sought between the two was sought. In order to make these patterns more useful to various types of practitioners, previously published patterns for these substances have been included, together with a brief description of their crystallographies, some Chemical Abstracts reference information about them, and an evaluation of their quality via accepted powder diffraction criteria. Most of these patterns have been accepted by the International Center for Diffraction Data for inclusion in their Powder Data File; the others will be submitted in due course.

  7. Powder X-ray diffraction detection on a paper-based platform.

    PubMed

    Ouyang, Liangfei; Liu, Qian; Xu, Chaoping; Liu, Changgui; Liang, Heng

    2017-03-01

    We developed paper-based powder X-ray diffraction (PP-XRD) to implement phase identification and/or crystal structure determination on paper-based platforms. These aims are not possible with other paper-based detectors, such as Raman spectroscopy and mass spectrometry. PP-XRD overcomes these limitations. Here we reported the simple and low-cost in situ PP-XRD protocol for phase identifications of inorganic and organic materials. We demonstrated that sample amounts of lead nitrate on paper substrate can be reduced into 1/30 of conventional ones by using the standard glass substrate at the same signal-to-noise ratio (S/N) of the X-ray diffraction (XRD) pattern. The paper-based method was comparable in sample quantity and intensity with zero background holder method, even though single crystal Si(100) substrate as zero background holder was used for the specimen preparation of CTAB (C19H42BrN). More importantly, paper substrates helped reduce preferred orientation that was generally present in routine powder XRD. Also, combined with paper chromatography, overlap peaks were eliminated in the XRD detection patterns of lead nitrate and cobalt nitrate hexahydrate. This new PP-XRD protocol may accelerate the process to identify phase or determine the molecular structures of new materials using trace sample directly. It also includes a hyphenated technique of powder XRD with a simple paper-based microfluidic separation of chemical solutions.

  8. 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.

  9. Performance calculations of the X-ray powder diffraction beamline at NSLS-II.

    PubMed

    Shi, Xianbo; Ghose, Sanjit; Dooryhee, Eric

    2013-03-01

    The X-ray Powder Diffraction (XPD) beamline at the National Synchrotron Light Source II is a multi-purpose high-energy X-ray diffraction beamline with high throughput and high resolution. The beamline uses a sagittally bent double-Laue crystal monochromator to provide X-rays over a large energy range (30-70 keV). In this paper the optical design and the calculated performance of the XPD beamline are presented. The damping wiggler source is simulated by the SRW code and a filter system is designed to optimize the photon flux as well as to reduce the heat load on the first optics. The final beamline performance under two operation modes is simulated using the SHADOW program. For the first time a multi-lamellar model is introduced and implemented in the ray tracing of the bent Laue crystal monochromator. The optimization and the optical properties of the vertical focusing mirror are also discussed. Finally, the instrumental resolution function of the XPD beamline is described in an analytical method.

  10. 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.

  11. Investigation by laser induced breakdown spectroscopy, X-ray fluorescence and X-ray powder diffraction of the chemical composition of white clay ceramic tiles from Veliki Preslav

    NASA Astrophysics Data System (ADS)

    Blagoev, K.; Grozeva, M.; Malcheva, G.; Neykova, S.

    2013-01-01

    The paper presents the results of the application of laser induced breakdown spectroscopy, X-ray fluorescence spectrometry, and X-ray powder diffraction in assessing the chemical and phase composition of white clay decorative ceramic tiles from the medieval archaeological site of Veliki Preslav, a Bulgarian capital in the period 893-972 AC, well-known for its original ceramic production. Numerous white clay ceramic tiles with highly varied decoration, produced for wall decoration of city's churches and palaces, were found during the archaeological excavations in the old capital. The examination of fourteen ceramic tiles discovered in one of the city's monasteries is aimed at characterization of the chemical profile of the white-clay decorative ceramics produced in Veliki Preslav. Combining different methods and comparing the obtained results provides complementary information regarding the white-clay ceramic production in Veliki Preslav and complete chemical characterization of the examined artefacts.

  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. Chemical analyses and x-ray diffraction patterns of powders and films of chloroaluminum phthalocyanine

    NASA Astrophysics Data System (ADS)

    Cote, Roland; Denes, G.; Gastonguay, Louis; Dodelet, Jean-Pol

    1992-12-01

    Fine powders and sublimed films (15 micrometers thick) of pure chloroaluminum phthalocyanine (ClAlPc) undergo both, chemical reaction and structural modification, when immersed in aqueous solutions containing anions (I3-/I- or Br- at various acid pH values). The x-ray diffraction diagrams of powder and films of untreated ClAlPc exhibit a strong characteristic peak corresponding to a d-spacing of 3.29 angstrom. A 48 h. immersion of ClAlPc (powder or film) resulted in the appearance of a new peak at 3.45 angstrom in the diffraction diagram. The peak intensity at d equals 3.45 angstrom is only 11% (powder) or 47% (film) of the main peak intensity at d equals 3.29 angstrom. It clearly shows that the crystal structure of ClAlPc has only been partially modified in both cases. However, the modification is more complete for the film than for the powder. Chemical analyses by neutron activation were performed on fine powders of ClAlPc before and after immersion. For instance ClAlPc absorbs 7.6% by weight of iodine after 24 h of immersion in I3-/I- (0.005 M/0.4 M) redox electrolyte at pH 1.0. The decrease in the chlorine content of untreated ClAlPc from 6.1% to 3.7% after immersion could be explained in terms of an hydrolysis reaction of some ClAlPc. These results lead us to a model where by the surface of the ClAlPc crystallites would be hydrolyzed to HOAlPc and heavily doped with anions taken up from the aqueous solution. These transformations improve the photoactivity of the material.

  14. 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.

  15. 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.

  16. X-ray powder diffractometry of emissions from the cement industry

    NASA Astrophysics Data System (ADS)

    Parekh, P. P.; Khan, A. R.; Davin, M. T.

    X-ray powder diffractometry has been found capable of identifying and distinguishing limestone and cement particles, the two important emissions of the cement industry. The limestone shows strong reflections principally at 1.87,1.91,2.09,2.28,2.49,3.03 and 3.83 Å from its main constituent, calcite, whereas cement shows reflections at 1.76, 2.18, 2.60, 2.64, a doublet at 2.73-2.77 and 3.02 Å from its main phases, the di-, and tri-calcium silicates. X-ray diffraction analysis of airborne particles collected on glass fibre filters in the vicinity of cement factories in Karachi, Pakistan and Ravena, New York State, revealed limestone but no cement particles. This observation was consistent with our earlier inference drawn from chemical and statistical methods for Karachi's ambient aerosols. The method can complement the selective leaching technique suggested earlier by us for source identification. On the basis of model calculations, a methodology has been worked out that would make the present technique adaptable to plant conditions.

  17. Characteristics of Organobentonite and Study of Iodide Adsorption on Organobentonite using X-ray Absorption Spectroscopy

    NASA Astrophysics Data System (ADS)

    Yoon, J.; Ha, J.; Hwang, B.; Hwang, J.; Brown, G. E.

    2008-12-01

    The adsorption of iodide on untreated bentonite and bentonites modified with organic cation (i.e., hexadecylpyridinium chloride monohydrate (HDP+)) was investigated, and the organobentonites were characterized using uptake measurements, micro X-ray diffraction (micro-XRD), and electrophoretic mobility measurements prior to reaction with KI solutions. Uptake measurements indicate that bentonite has a high affinity for HDP+. Increasing [HDP+](aq) results in an increase in HDP+ uptake on bentonite by up to 280% of the CEC equivalents of bentonite, and causes a concomitant increase in Na released as a result of the replacement of exchangeable inorganic cations in bentonite interlayers. Based micro-XRD, the d001 spacing of untreated bentonite was 1.22 nm whereas organobentonites modified with HDP+ at different equivalent amounts, corresponding to 100%, 200%, and 400% of the cation exchange capacity (CEC) of bentonite, showed d001 spacings of 1.96 nm, 3.77 nm, and 3.77 nm, respectively. Our micro-XRD study indicates that organobentonites significantly expanded in basal spacing and organic cations were substantially intercalated into the interlayer spaces of montmorillonite. The electrophoretic mobility indicates that the untreated bentonite had a negative surface charge over the entire pH range examined (pH 2-12) whereas the organobentonite at an equivalent amount corresponding to 200% of the CEC had a positive surface charge over this pH range. We found significant differences in adsorption capacities of iodide depending on the bentonite properties as follows: iodide adsorption capacities were 439 mmol/kg for the bentonite modified with HDP+ at an equivalent amount corresponding to 200% of the CEC of bentonite whereas no adsorption of iodide was observed for the untreated bentonite. The molecular environments of iodine adsorbed on organobentonites were further studied using I K-edge and LIII-edge x-ray absorption spectroscopy (XAS). The X-ray absorption near

  18. High-performance X-ray detectors for the new powder diffraction beamline I11 at Diamond.

    PubMed

    Tartoni, Nicola; Thompson, Stephen P; Tang, Chiu C; Willis, Brian L; Derbyshire, Gareth E; Wright, Anthony G; Jaye, Stephen C; Homer, J Michael; Pizzey, John D; Bell, Anthony M T

    2008-01-01

    The design and performance characterization of a new light-weight and compact X-ray scintillation detector is presented. The detectors are intended for use on the new I11 powder diffraction beamline at the third-generation Diamond synchrotron facility where X-ray beams of high photon brightness are generated by insertion devices. The performance characteristics of these detection units were measured first using a radioactive source (efficiency of detection and background count rate) and then synchrotron X-rays (peak stability, light yield linearity and response consistency). Here, the results obtained from these tests are reported, and the suitability of the design for the Diamond powder beamline is demonstrated by presenting diffraction data obtained from a silicon powder standard using a prototype multicrystal analyser stage.

  19. 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.

  20. Crystal structure of trirubidium citrate from laboratory X-ray powder diffraction data and DFT comparison

    PubMed Central

    Kaduk, James A.

    2017-01-01

    The crystal structure of trirubidium citrate, 3Rb+·C6H5O7 3−, has been solved and refined using laboratory X-ray powder diffraction data, and optimized using density functional techniques. The two independent Rb+ cations are seven- and eight-coordinate, with bond-valence sums of 0.99 and 0.92 valence units. The coordination polyhedra share edges and corners to form a three-dimensional framework. The only hydrogen bond is an intra­molecular one between the hy­droxy group and the central carboxyl­ate, with graph set S(5). The hydro­phobic methyl­ene groups lie in pockets in the framework. PMID:28217353

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

    PubMed

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

    2017-01-01

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

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

    PubMed

    Rammohan, Alagappa; Kaduk, James A

    2017-02-01

    The crystal structure of trirubidium citrate, 3Rb(+)·C6H5O7(3-), has been solved and refined using laboratory X-ray powder diffraction data, and optimized using density functional techniques. The two independent Rb(+) cations are seven- and eight-coordinate, with bond-valence sums of 0.99 and 0.92 valence units. The coordination polyhedra share edges and corners to form a three-dimensional framework. The only hydrogen bond is an intra-molecular one between the hy-droxy group and the central carboxyl-ate, with graph set S(5). The hydro-phobic methyl-ene groups lie in pockets in the framework.

  3. 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.

  4. Local similarity in organic crystals and the non-uniqueness of X-ray powder patterns.

    PubMed

    Karfunkel; Wilts; Hao; Iqbal; Mizuguchi; Wu

    1999-12-01

    Two new concepts for molecular solids, 'local similarity' and 'boundary-preserving isometry', are defined mathematically and a theorem which relates these concepts is formulated. 'Locally similar' solids possess an identical short-range structure and a 'boundary-preserving isometry' is a new mathematical operation on a finite region of a solid that transforms mathematically a given solid to a locally similar one. It is shown further that the existence of such a 'boundary-preserving isometry' in a given solid has infinitely many 'locally similar' solids as a consequence. Chemical implications, referring to the similarity of X-ray powder patterns and patent registration, are discussed as well. These theoretical concepts, which are first introduced in a schematic manner, are proved to exist in nature by the elucidation of the crystal structure of some diketopyrrolopyrrole (DPP) derivatives with surprisingly similar powder patterns. Although the available powder patterns were not indexable, the underlying crystals could be elucidated by using the new technique of ab initio prediction of possible polymorphs and a subsequent Rietveld refinement. Further ab initio packing calculations on other molecules reveal that 'local crystal similarity' is not restricted to DPP derivatives and should also be exhibited by other molecules such as quinacridones. The 'boundary-preserving isometry' is presented as a predictive tool for crystal engineering purposes and attempts to detect it in crystals of the Cambridge Structural Database (CSD) are reported.

  5. Investigation of recrystallization of amorphous trehalose through hot-humidity stage X-ray powder diffraction.

    PubMed

    Jójárt-Laczkovich, Orsolya; Katona, Gábor; Aigner, Zoltán; Szabó-Révész, Piroska

    2016-12-01

    The aim of this work was an investigation of the physical changes of the amorphous model material spray-dried trehalose through the use of various analytical techniques and to identify a suitable, rapid method able to quantify the changes. The crystallinity changes and recrystallization process of amorphous samples were investigated by hot-humidity stage X-ray powder diffractometry (HH-XRPD) with fresh samples, conventional X-ray powder diffractometry (XRPD) used stored samples and by differential scanning calorimetry (DSC). The data from the three methods were compared and the various forms of trehalose were analysed. HH-XRPD demonstrated that the recrystallization began at 40 and 60°C up to 45% RH and at 70°C up to 30% RH into dihydrate form. At 70°C up to 60% RH the anhydrous form of trehalose appeared too. Conventional XRPD results showed, that in the 28days stored samples the dihydrate form was detected at 40°C, 50% RH. Storage at 60°C, 40% RH resulted in the appearance of the anhydrous form and at 60°C, 50% RH both polymorphic forms were detected. By carrying out the DSC measurements at different temperatures the fraction of recrystallized trehalose dihydrate was detected. The recrystallization investigated by HH-XRPD and DSC followed Avrami kinetics, the calculated rate constants of isothermal crystallization (K) were same. Both HH-XRPD and conventional XRPD was suitable for the detection of the physical changes of the amorphous model material. DSC measurements showed similar results as HH-XRPD. Primarily HH-XRPD could be suggested for prediction, because the method is fast and every changes could be studied on one sample.

  6. Real-Time Studies of Gallium Adsorption and Desorption Kinetics by Grazing-Incidence Small-Angle X-ray Scattering and X-ray Fluorescence

    SciTech Connect

    Wang, Y.; Ozcan, A; Ludwig, K; Bhattacharyya, A

    2008-01-01

    Gallium adsorption and desorption on c-plane sapphire has been studied by real-time grazing incidence small-angle x-ray scattering and x-ray fluorescence as a function of substrate temperature (680-740 C) and Ga flux. The x-ray techniques monitor the surface morphology evolution and amount of Ga on the surface. During deposition, nanodroplets of liquid Ga are observed to form on the surface and coarsen. The growth of droplet size during continuous deposition follows dynamical scaling, in agreement with expectations from theory and simulations which include deposition-induced droplet coalescence. However, observation of continued droplet distance scale coarsening during desorption points to the necessity of including further physical processes in the modeling. The desorption rate at different substrate temperatures gives the activation energy of Ga desorption as 2.7 eV, comparable to measured activation energies for desorption from Ga droplets on other substrates and to the Ga heat of vaporization.

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

    DOE PAGES

    Wang, H.; Kirkham, M. J.; Watkins, T. R.; ...

    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

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

    SciTech Connect

    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 cubic 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.

  9. 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.

  10. 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.

  11. 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…

  12. 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…

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

    PubMed

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

    2005-12-01

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

  14. 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})

  15. Mineralogical effect correction in wavelength dispersive X-ray florescence analysis of pressed powder pellets

    NASA Astrophysics Data System (ADS)

    Shan, H. Z.; Zhuo, S. J.; Shen, R. X.; Sheng, C.

    2008-05-01

    Two methods are utilized to correct the influence of the mineralogical effect on the calibration of elements in geological samples when the pressed powder pellet method is used in wavelength dispersive X-ray fluorescence analysis. The first method involves checking of the 2θ angle for the analyzed element in each sample to correct peak shift and the second method involves replacing the peak intensity with the peak area of the analytical line, so to correct for any shape distortion of the peak. The results were compared with those obtained from the normal method. Major elements in 27 Chinese Certified Reference Materials (CRMs) of rocks, soils and sediments were calibrated with a linear regression curve without theoretical or empirical coefficients. In view of the K values, the calibrations of all 8 elements were improved by the first method and those of 6 elements were improved by the second method. Sulfur calibrations with 4 iron ore CRMs were improved with the use of both methods. The methods have been successfully applied for the analysis of the major elements in limestone ores from different resources of a cement factory.

  16. X-ray Powder Diffraction for Characterization of Raw Materials in Banknotes.

    PubMed

    Marabello, Domenica; Benzi, Paola; Lombardozzi, Antonietta; Strano, Morela

    2017-01-25

    We report about the X-ray powder diffraction characterization of crystalline materials used to produce genuine and counterfeit banknotes, performed with a single-crystal diffractometer that permits fast and nondestructive measurements in different 0.5-mm sized areas; 20-euro denomination genuine banknotes were analyzed, and results were compared with counterfeit banknotes. The analysis shows that the papers used to print real banknotes are composed, as expected, of cotton-based cellulose and titanium dioxide as crystalline additive, but different polymorphs of TiO2 for different emission countries are evidenced. The counterfeit banknotes are composed of cellulose based on wood pulp; moreover, an unexpected significant quantity of TiO2 was found to be mixed with calcite, indicating that the paper employed by forgers is not simply a common low-cost type. The crystalline index and intensity ratios between the peaks attributable to cellulose and fillers can provide additional information to trace back paper suppliers for forensic purposes.

  17. 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).

  18. Scanning of Adsorption Hysteresis In Situ with Small Angle X-Ray Scattering

    PubMed Central

    Mitropoulos, Athanasios Ch.; Favvas, Evangelos P.; Stefanopoulos, Konstantinos L.; Vansant, Etienne F.

    2016-01-01

    Everett’s theorem-6 of the domain theory was examined by conducting adsorption in situ with small angle x-ray scattering (SAXS) supplemented by the contrast matching technique. The study focuses on the spectrum differences of a point to which the system arrives from different scanning paths. It is noted that according to this theorem at a common point the system has similar macroscopic properties. Furthermore it was examined the memory string of the system. We concluded that opposite to theorem-6: a) at a common point the system can reach in a finite (not an infinite) number of ways, b) a correction for the thickness of the adsorbed film prior to capillary condensation is necessary, and c) the scattering curves although at high-Q values coincide, at low-Q values are different indicating different microscopic states. That is, at a common point the system holds different metastable states sustained by hysteresis effects. These metastable states are the ones which highlight the way of a system back to a return point memory (RPM). Entering the hysteresis loop from different RPMs different histories are implanted to the paths toward the common point. Although in general the memory points refer to relaxation phenomena, they also constitute a characteristic feature of capillary condensation. Analogies of the no-passing rule and the adiabaticity assumption in the frame of adsorption hysteresis are discussed. PMID:27741263

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

    DOE PAGES

    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

  20. 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.

  1. Powder X-ray diffraction can differentiate between enantiomeric variants of calcium lactate pentahydrate crystal in cheese.

    PubMed

    Tansman, G F; Kindstedt, P S; Hughes, J M

    2014-12-01

    Powder X-ray diffraction has been used for decades to identify crystals of calcium lactate pentahydrate in Cheddar cheese. According to this method, diffraction patterns are generated from a powdered sample of the crystals and compared with reference cards within a database that contains the diffraction patterns of known crystals. During a preliminary study of crystals harvested from various Cheddar cheese samples, we observed 2 slightly different but distinct diffraction patterns that suggested that calcium lactate pentahydrate may be present in 2 different crystalline forms. We hypothesized that the 2 diffraction patterns corresponded to 2 enantiomeric forms of calcium lactate pentahydrate (L- and DL-) that are believed to occur in Cheddar cheese, based on previous studies involving enzymatic analyses of the lactate enantiomers in crystals obtained from Cheddar cheeses. However, the powder X-ray diffraction database currently contains only one reference diffraction card under the title “calcium lactate pentahydrate.” To resolve this apparent gap in the powder X-ray diffraction database, we generated diffraction patterns from reagent-grade calcium l-lactate pentahydrate and laboratory-synthesized calcium dl-lactate pentahydrate. From the resulting diffraction patterns we determined that the existing reference diffraction card corresponds to calcium dl-lactate pentahydrate and that the other form of calcium lactate pentahydrate observed in cheese crystals corresponds to calcium l-lactate pentahydrate. Therefore, this report presents detailed data from the 2 diffraction patterns, which may be used to prepare 2 reference diffraction cards that differentiate calcium l-lactate pentahydrate from calcium dl-lactate pentahydrate. Furthermore, we collected crystals from the exteriors and interiors of Cheddar cheeses to demonstrate the ability of powder X-ray diffraction to differentiate between the 2 forms of calcium lactate pentahydrate crystals in Cheddar cheeses

  2. Decomposition of spinel-type nickel chromium indium sulfides -- X-ray powder structure determination

    SciTech Connect

    Lutz, H.D.; Kringe, C.; Mohn, K.; Stingl, T.

    1998-03-01

    The phase diagram of the quaternary system NiCr{sub 2}S{sub 4}-NiIn{sub 2}S{sub 4}-Cr{sub 2}S{sub 3}-In{sub 2}S{sub 3} has been studied at 873 and 1,223 K by X-ray powder structure determination of quenched samples. At high temperatures, spinel-type Ni{sub y}(Cr{sub 2{minus}2x}In{sub 2x}){sub 1{minus}y}S{sub 3{minus}2y} solid solutions are formed in a large range of composition (y:0--0.5, x:03--1). At temperatures below 1,183 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{sup 3+} > Ni{sup 2+} > In{sup 3+} at the octahedral 16d site and {open_square} (vacancies) > In{sup 3+} > Ni{sup 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{sub tet}-S = 247.1 pm; In{sub oct}-S = 260.6 pm.

  3. Pulsed magnetic field synchrotron X-ray powder diffraction of the Jahn-Teller distortion in TbVO4

    NASA Astrophysics Data System (ADS)

    Vanacken, J.; Frings, P.; Detlefs, C.; Duc, F.; Lorenzo, J. E.; Nardone, M.; Billette, J.; Zitouni, A.; Bras, W.; Rikken, G.

    2006-11-01

    X-ray powder diffraction experiments under pulsed magnetic fields were carried out at the DUBBLE beam line at the ESRF. A mobile generator delivered 110 kJ to the load coil, which was sufficient to generate peak fields of 30 T. A liquid He flow cryostat allowed us to vary the sample temperature accurately between 8 K and 300 K. Powder diffraction patterns of TbVO4 were recorded in a broad temperature range using 21 keV monochromatic X-rays and an on-line image plate detector. We present results on the suppression of the Jahn-Teller structural distortion in TbVO4by to the magnetic field.

  4. 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

  5. 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.

  6. 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.

  7. 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.

  8. X-Ray Powder Diffraction Study of Synthetic Palmierite, K{sub 2}Pb(SO{sub 4}){sub 2}

    SciTech Connect

    TISSOT JR.,RALPH G.; RODRIGUEZ,MARK A.; SIPOLA,DIANA L.; VOIGT,JAMES A.

    2000-12-19

    Palmierite (K{sub 2}Pb(SO{sub 4}){sub 2}) has been prepared via a chemical synthesis method. Intensity differences were observed when X-ray powder data from the newly synthesized compound were compared to the published powder diffraction card (PDF) 29-1015 for Palmierite. Investigation of these differences indicated the possibility of preferred orientation and/or chemical inhomogeneity affecting intensities, particularly those of the basal (00{ell}) reflections. Annealing of the Palmierite was found to reduce the effects of preferred orientation. Electron microprobe analysis confirmed K:Pb:S as 2:1:2 for the annealed Palmierite powder. Subsequent least-squares refinement and Rietveld analysis of the annealed powder showed peak intensities very close to that of a calculated Palmierite pattern (based on single crystal data), yet substantially higher than many of the PDF 29-1015 published intensities. Further investigation of peak intensity variation via calculated patterns suggested that the intensity discrepancies between the annealed sample and those found in PDF 29-1015 were potentially due to chemical variation in the K{sub 2}Pb(SO{sub 4}){sub 2} composition. X-ray powder diffraction and crystal data for Palmierite are reported for the annealed sample. Palmierite is Trigonal/Hexagonal with unit cell parameters a = 5.497(1){angstrom}, c = 20.864(2) {angstrom}, space group R-3m (166), and Z = 3.

  9. 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

  10. 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}.

  11. 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.

  12. Using in situ X-ray reflectivity to study protein adsorption on hydrophilic and hydrophobic surfaces: benefits and limitations.

    PubMed

    Richter, Andrew G; Kuzmenko, Ivan

    2013-04-30

    We have employed in situ X-ray reflectivity (IXRR) to study the adsorption of a variety of proteins (lysozyme, cytochrome c, myoglobin, hemoglobin, serum albumin, and immunoglobulin G) on model hydrophilic (silicon oxide) and hydrophobic surfaces (octadecyltrichlorosilane self-assembled monolayers), evaluating this recently developed technique for its applicability in the area of biomolecular studies. We report herein the highest resolution depiction of adsorbed protein films, greatly improving on the precision of previous neutron reflectivity (NR) results and previous IXRR studies. We were able to perform complete scans in 5 min or less with the maximum momentum transfer of at least 0.52 Å(-1), allowing for some time-resolved information about the evolution of the protein film structure. The three smallest proteins (lysozyme, cytochrome c, and myoglobin) were seen to deposit as fully hydrated, nondenatured molecules onto hydrophilic surfaces, with indications of particular preferential orientations. Time evolution was observed for both lysozyme and myoglobin films. The larger proteins were not observed to deposit on the hydrophilic substrates, perhaps because of contrast limitations. On hydrophobic surfaces, all proteins were seen to denature extensively in a qualitatively similar way but with a rough trend that the larger proteins resulted in lower coverage. We have generated high-resolution electron density profiles of these denatured films, including capturing the growth of a lysozyme film. Because the solution interface of these denatured films is diffuse, IXRR cannot unambiguously determine the film extent and coverage, a drawback compared to NR. X-ray radiation damage was systematically evaluated, including the controlled exposure of protein films to high-intensity X-rays and exposure of the hydrophobic surface to X-rays before adsorption. Our analysis showed that standard measuring procedures used for XRR studies may lead to altered protein films

  13. TiC-carbide derived carbon electrolyte adsorption study by ways of X-ray scattering analysis.

    PubMed

    Trognko, Lorie; Lecante, Pierre; Ratel-Ramond, Nicolas; Rozier, Patrick; Daffos, Barbara; Taberna, Pierre-Louis; Simon, Patrice

    Understanding ion adsorption in nanoporous carbon electrodes is of great importance for designing the next-generation of high energy density electrical double-layer capacitors. In this work, X-ray scattering is used for investigating the impregnation of nanoporous carbons with electrolytes in the absence of applied potential. We are able to show that interactions between the carbon surface and electrolytes allow adsorption to take place in sub-nanopores, thus confirming experimentally for the first time the results predicted by molecular dynamic simulations.

  14. Time-resolved in situ powder X-ray diffraction reveals the mechanisms of molten salt synthesis.

    PubMed

    Moorhouse, Saul J; Wu, Yue; Buckley, Hannah C; O'Hare, Dermot

    2016-11-24

    We report the first use of high-energy monochromatic in situ X-ray powder diffraction to gain unprecedented insights into the chemical processes occurring during high temperature, lab-scale metal oxide syntheses. During the flux synthesis of the n = 4 Aurivillius phase, Bi5Ti3Fe0.5Cr0.5O15 at 950 °C in molten Na2SO4 we observe the progression of numerous metastable phases. Using sequential multiphase Rietveld refinement of the time-dependent in situ XRD data, we are able to obtain mechanistic understanding of this reaction under a range of conditions.

  15. 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

  16. Exploiting powder X-ray diffraction for direct structure determination in structural biology: the P2X4 receptor trafficking motif YEQGL.

    PubMed

    Fujii, Kotaro; Young, Mark T; Harris, Kenneth D M

    2011-06-01

    We report the crystal structure of the 5-residue peptide acetyl-YEQGL-amide, determined directly from powder X-ray diffraction data recorded on a conventional laboratory X-ray powder diffractometer. The YEQGL motif has a known biological role, as a trafficking motif in the C-terminus of mammalian P2X4 receptors. Comparison of the crystal structure of acetyl-YEQGL-amide determined here and that of a complex formed with the μ2 subunit of the clathrin adaptor protein complex AP2 reported previously, reveals differences in conformational properties, although there are nevertheless similarities concerning aspects of the hydrogen-bonding arrangement and the hydrophobic environment of the leucine sidechain. Our results demonstrate the potential for exploiting modern powder X-ray diffraction methodology to achieve complete structure determination of materials of biological interest that do not crystallize as single crystals of suitable size and quality for single-crystal X-ray diffraction.

  17. Adsorption, X-ray Diffraction, Photoelectron, and Atomic Emission Spectroscopy Benchmark Studies for the Eighth Industrial Fluid Properties Simulation Challenge.

    PubMed

    Ross, Richard B; Aeschliman, David B; Ahmad, Riaz; Brennan, John K; Brostrom, Myles L; Frankel, Kevin A; Moore, Jonathan D; Moore, Joshua D; Mountain, Raymond D; Poirier, Derrick M; Thommes, Matthias; Shen, Vincent K; Schultz, Nathan E; Siderius, Daniel W; Smith, Kenneth D

    2016-02-01

    The primary goal of the eighth industrial fluid properties simulation challenge was to test the ability of molecular simulation methods to predict the adsorption of organic adsorbates in activated carbon materials. The challenge focused on the adsorption of perfluorohexane in the activated carbon standard BAM-P109 (Panne and Thünemann 2010). Entrants were challenged to predict the adsorption of perfluorohexane in the activated carbon at a temperature of 273 K and at relative pressures of 0.1, 0.3, and 0.6. The relative pressure (P/Po) is defined as that relative to the bulk saturation pressure predicted by the fluid model at a given temperature (273 K in this case). The predictions were judged by comparison to a set of experimentally determined values, which are published here for the first time and were not disclosed to the entrants prior to the challenge. Benchmark experimental studies, described herein, were also carried out and provided to entrants in order to aid in the development of new force fields and simulation methods to be employed in the challenge. These studies included argon, carbon dioxide, and water adsorption in the BAM-P109 activated carbon as well as X-ray diffraction, X-ray microtomography, photoelectron spectroscopy, and atomic emission spectroscopy studies of BAM-P109. Several concurrent studies were carried out for the BAM-P108 activated carbon (Panne and Thünemann 2010). These are included in the current manuscript for comparison.

  18. Adsorption, X-ray Diffraction, Photoelectron, and Atomic Emission Spectroscopy Benchmark Studies for the Eighth Industrial Fluid Properties Simulation Challenge*+

    PubMed Central

    Ross, Richard B.; Aeschliman, David B.; Ahmad, Riaz; Brennan, John K.; Brostrom, Myles L.; Frankel, Kevin A.; Moore, Jonathan D.; Moore, Joshua D.; Mountain, Raymond D.; Poirier, Derrick M.; Thommes, Matthias; Shen, Vincent K.; Schultz, Nathan E.; Siderius, Daniel W.; Smith, Kenneth D.

    2016-01-01

    The primary goal of the eighth industrial fluid properties simulation challenge was to test the ability of molecular simulation methods to predict the adsorption of organic adsorbates in activated carbon materials. The challenge focused on the adsorption of perfluorohexane in the activated carbon standard BAM-P109 (Panne and Thünemann 2010). Entrants were challenged to predict the adsorption of perfluorohexane in the activated carbon at a temperature of 273 K and at relative pressures of 0.1, 0.3, and 0.6. The relative pressure (P/Po) is defined as that relative to the bulk saturation pressure predicted by the fluid model at a given temperature (273 K in this case). The predictions were judged by comparison to a set of experimentally determined values, which are published here for the first time and were not disclosed to the entrants prior to the challenge. Benchmark experimental studies, described herein, were also carried out and provided to entrants in order to aid in the development of new force fields and simulation methods to be employed in the challenge. These studies included argon, carbon dioxide, and water adsorption in the BAM-P109 activated carbon as well as X-ray diffraction, X-ray microtomography, photoelectron spectroscopy, and atomic emission spectroscopy studies of BAM-P109. Several concurrent studies were carried out for the BAM-P108 activated carbon (Panne and Thünemann 2010). These are included in the current manuscript for comparison. PMID:27840543

  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

    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.

  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

    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

  1. Formation mechanism of LiFePO 4/C composite powders investigated by X-ray absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Hsu, Kuei-Feng; Hu, Shao-Kang; Chen, Chinh-Hsiang; Cheng, Ming-Yao; Tsay, Sun-Yuan; Chou, Tse-Chuan; Sheu, Hwo-Shuenn; Lee, Jyh-Fu; Hwang, Bing-Joe

    The local structure and oxidation states for both the precursors and the LiFePO 4/C composite powders were investigated by X-ray absorption spectroscopy (XAS) to provide a deep insight into their formation mechanism. It was found that the local structure and oxidation states of the precursors and the synthesized LiFePO 4/C powders as well as the electrochemical properties of the synthesized powders were strongly influenced by the R ratio (R: molar ratio of citric acid to total metal ions). The oxidation states of iron ions of the precursors for R = 1 and 0.75 consist mainly of Fe(II) and traces of Fe(III). However, the oxidation state of iron ions of the precursor for R = 0.5 comprises mainly of Fe(III). The oxidation state of iron ions of all the synthesized powders is Fe(II). The structure of the precursors and the synthesized powders for R = 1 and 0.75 is more ordering than that for R = 0.5. It is in good agreement with the observation of the cation mixing obtained from the Riteveld analysis of the XRD data. The better the electrochemical performance is, the more ordering the structure or the less the cation mixing. However, the effect of the R values on the carbon content is also essential for the electrochemical properties of the synthesized LiFePO 4/C composite powders. Increasing the carbon content leads to the increase in the electronic conductivity but impedes the Li + ion diffusion of the composite materials. Consequently, the powders synthesized at the optimal R ratio of 0.75 exhibited the highest initial capacity, about 150 mAh g -1 when cycled at 1/40 C rate at room temperature. The structural scheme of the precursors and the synthesized powders and the formation mechanism of the LiFePO 4/C composite powders are also addressed in this work.

  2. Porosity of microporous zeolites A, X and ZSM-5 studied by small angle X-ray scattering and nitrogen adsorption

    NASA Astrophysics Data System (ADS)

    Du, Xiaoming; Wu, Erdong

    2007-09-01

    Small-angle X-ray scattering (SAXS) using synchrotron radiation and nitrogen adsorption have been applied to characterizations of porosities and microporous structures for the zeolites of NaA, KA, CaA, NaX and ZSM-5. Besides the information on the external morphology of the particles of the zeolites, the complementation of the two techniques has revealed rich and consistent structural and surface information on the molecular scale crystalline pores of these zeolites. Analyses of the data suggest that the determined sizes of the micropores imply the pore spaces occupied by the probe molecules of water in the SAXS and nitrogen in adsorption techniques, respectively. The microporous information of NaA and KA are difficult to obtain from nitrogen adsorption, due to the blocking of nitrogen by their narrow channels, but have been satisfactorily measured by SAXS. The factors causing variations of the measured values of the parameters in different analysis methods have been discussed.

  3. Neutron and X-ray reflectivity studies on DNA adsorption on mixed DPPC/DC-Cholesterol monolayers

    NASA Astrophysics Data System (ADS)

    Wu, Jui-Ching; Lin, Tsang-Lang; Jeng, U.-Ser; Lee, Hsin-Yi; Gutberlet, Thomas

    2006-11-01

    We have studied DNA adsorption on mixed DPPC/DC-Chol monolayers. Solid supported mixed monolayers on silicon wafers were prepared using Langmuir-Blodgett (LB) dipping technique. Neutron and X-ray reflectivity measurements were used to characterize these LB monofilms. For LB monofilms with DNA adsorption, the reflectivity data of the DPPC/DNA film are very close to that from the DPPC film, which indicates only minor DNA adsorption on the pure DPPC monolayer. Increasing the percentage of DC-Chol, film thickness increases. The DC-Chol/DNA film is thicker than the pure DC-Chol film (film thickness 18 Å) by about 9 Å due to the presence of adsorbed DNA. A model is presented to explain the structure of the lipid/DNA film.

  4. 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.

  5. 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.

  6. Characterization of photocatalytic TiO2 powder under varied environments using near ambient pressure X-ray photoelectron spectroscopy

    PubMed Central

    Krishnan, Padmaja; Liu, Minghui; Itty, Pierre A.; Liu, Zhi; Rheinheimer, Vanessa; Zhang, Min-Hong; Monteiro, Paulo J. M.; Yu, Liya E.

    2017-01-01

    Consecutive eight study phases under the successive presence and absence of UV irradiation, water vapor, and oxygen were conducted to characterize surface changes in the photocatalytic TiO2 powder using near-ambient-pressure X-ray photoelectron spectroscopy (XPS). Both Ti 2p and O 1s spectra show hysteresis through the experimental course. Under all the study environments, the bridging hydroxyl (OHbr) and terminal hydroxyl (OHt) are identified at 1.1–1.3 eV and 2.1–2.3 eV above lattice oxygen, respectively. This enables novel and complementary approach to characterize reactivity of TiO2 powder. The dynamic behavior of surface-bound water molecules under each study environment is identified, while maintaining a constant distance of 1.3 eV from the position of water vapor. In the dark, the continual supply of both water vapor and oxygen is the key factor retaining the activated state of the TiO2 powder for a time period. Two new surface peaks at 1.7–1.8 and 4.0–4.2 eV above lattice oxygen are designated as peroxides (OOH/H2O2) and H2O2 dissolved in water, respectively. The persistent peroxides on the powder further explain previously observed prolonged oxidation capability of TiO2 powder without light irradiation. PMID:28240300

  7. Characterization of photocatalytic TiO2 powder under varied environments using near ambient pressure X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Krishnan, Padmaja; Liu, Minghui; Itty, Pierre A.; Liu, Zhi; Rheinheimer, Vanessa; Zhang, Min-Hong; Monteiro, Paulo J. M.; Yu, Liya E.

    2017-02-01

    Consecutive eight study phases under the successive presence and absence of UV irradiation, water vapor, and oxygen were conducted to characterize surface changes in the photocatalytic TiO2 powder using near-ambient-pressure X-ray photoelectron spectroscopy (XPS). Both Ti 2p and O 1s spectra show hysteresis through the experimental course. Under all the study environments, the bridging hydroxyl (OHbr) and terminal hydroxyl (OHt) are identified at 1.1–1.3 eV and 2.1–2.3 eV above lattice oxygen, respectively. This enables novel and complementary approach to characterize reactivity of TiO2 powder. The dynamic behavior of surface-bound water molecules under each study environment is identified, while maintaining a constant distance of 1.3 eV from the position of water vapor. In the dark, the continual supply of both water vapor and oxygen is the key factor retaining the activated state of the TiO2 powder for a time period. Two new surface peaks at 1.7–1.8 and 4.0–4.2 eV above lattice oxygen are designated as peroxides (OOH/H2O2) and H2O2 dissolved in water, respectively. The persistent peroxides on the powder further explain previously observed prolonged oxidation capability of TiO2 powder without light irradiation.

  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.

  9. 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.

  10. 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.

  11. The Adsorption of Dodecyltrimethylammonium Bromide on Mica in Aqueous Solution Studied by X-Ray Diffraction and Atomic Force Microscopy.

    PubMed

    Whitby, Catherine P.; Scales, Peter J.; Grieser, Franz; Healy, Thomas W.; Nishimura, Satoshi; Tateyama, Hiroshi

    2001-03-15

    The adsorption of dodecyltrimethylammonium bromide (DTAB) onto natural muscovite mica and a synthetic expandable mica (EM) in aqueous solution has been investigated using both microscopic and macroscopic surface characterization techniques. The electrokinetic properties of the surfaces were monitored as a function of the concentration of DTAB using atomic force microscopy and microelectrophoresis. The adsorption isotherm of DTAB on EM was measured up to a solution concentration just below the critical micelle concentration of the surfactant. The thickness of the adsorbed layer on EM was determined using X-ray diffraction. Results indicate that the adsorbed layer consists of molecules lying quite flat on the mica surface at low concentrations and adsorbed in interleaved aggregate structures at concentrations approaching the critical micelle concentration of the surfactant in solution. Copyright 2001 Academic Press.

  12. 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.

  13. The ab-initio crystal structure determination of UPd 2Sn by synchrotron X-ray powder diffraction

    NASA Astrophysics Data System (ADS)

    Marezio, M.; Cox, D. E.; Rossel, C.; Maple, M. B.

    1988-09-01

    The structure of the heavy-fermion compound UPd 2Sn has been determined by synchrotron x-ray radiation powder diffraction techniques. It is orthorhombic, space group Pnma [lattice parameters a = 9.9787(1), b = 4.58843(5), c = 6.89166(8) Å at room temperature] and Z = 4. All atoms, one U, one Sn, and two Pd are in 4d special positions at (x {1}/{4} z). The refinements were carried out by the Rietveld method with a pseudo-Voigt peak shape function. The final conventional R factors were: R wp = 21.3% and R E = 14.3%. The U positions in the unit cell were unequivocally located, but because of the similarity in x-ray scattering factors it was not possible to determine whether the Pd atoms and the Sn atoms are ordered or disordered on the other three sites. The structural arrangement of UPd 2Sn is of either MnCu 2Al, or ordered NaTl, or disordered Fe 3Al type, all these structures being cubic and b.c.c. related. The orthorhombic distortion is large and is probably due to a size effect of the U atoms which would be in a mixed ( {3+}/{4+}) valence state.

  14. Crystal structure of penta­sodium hydrogen dicitrate from synchrotron X-ray powder diffraction data and DFT comparison

    PubMed Central

    Kaduk, James A.

    2017-01-01

    The crystal structure of penta­sodium hydrogen dicitrate, Na5H(C6H5O7)2, has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Each of the two independent citrate anions is joined into a dimer by very strong centrosymmetric O—H⋯O hydrogen bonds, with O⋯O distances of 2.419 and 2.409 Å. Four octa­hedrally coordinated Na+ ions share edges to form open layers parallel to the ab plane. A fifth Na+ ion in trigonal–bipyramidal coordination shares faces with NaO6 octahedra on both sides of these layers. PMID:28217360

  15. 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.

  16. Crystal structure of caesium di­hydrogen citrate from laboratory X-ray powder diffraction data and DFT comparison

    PubMed Central

    Kaduk, James A.

    2017-01-01

    The crystal structure of caesium di­hydrogen citrate, Cs+·H2C6H5O7 −, has been solved and refined using laboratory X-ray powder diffraction data, and optimized using density functional techniques. The coordination polyhedra of the nine-coordinate Cs+ cations share edges to form chains along the a-axis. These chains are linked by corners along the c-axis. The un-ionized carb­oxy­lic acid groups form two different types of hydrogen bonds; one forms a helical chain along the c-axis, and the other is discrete. The hy­droxy group participates in both intra- and inter­molecular hydrogen bonds. PMID:28217327

  17. Crystal structure of trirubidium citrate monohydrate from laboratory X-ray powder diffraction data and DFT comparison

    PubMed Central

    Kaduk, James A.

    2017-01-01

    The crystal structure of the title compound, 3Rb+·C6H5O7 3−·H2O, has been solved and refined using laboratory X-ray powder diffraction data, and optimized using density functional techniques. The hy­droxy group participates in an intra­molecular hydrogen bond to the deprotonated central carboxyl­ate group with graph-set motif S(5). The water mol­ecule acts as a hydrogen-bond donor to both terminal and central carboxyl­ate O atoms. The three independent rubidium cations are seven-, six- and six-coordinate, with bond-valence sums of 0.84, 1.02, and 0.95, respectively. In the extended structure, their polyhedra share edges and corners to form a three-dimensional network. The hydro­phobic methyl­ene groups occupy channels along the b axis. PMID:28217348

  18. Crystal structure of dirubidium hydrogen citrate from laboratory X-ray powder diffraction data and DFT comparison

    PubMed Central

    Rammohan, Alagappa; Kaduk, James A.

    2017-01-01

    The crystal structure of dirubidium hydrogen citrate, 2Rb+·HC6H5O7 2−, has been solved and refined using laboratory X-ray powder diffraction data, and optimized using density functional techniques. The un-ionized carb­oxy­lic acid group forms helical chains of very strong hydrogen bonds (O⋯O ∼ 2.42 Å) along the b axis. The hy­droxy group participates in a chain of intra- and inter­molecular hydrogen bonds along the c axis. These hydrogen bonds result in corrugated hydrogen-bonded layers in the bc plane. The Rb+ cations are six-coordinate, and share edges and corners to form layers in the ab plane. The inter­layer contacts are composed of the hydro­phobic methyl­ene groups. PMID:28083145

  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 of caesium di-hydrogen citrate from laboratory X-ray powder diffraction data and DFT comparison.

    PubMed

    Rammohan, Alagappa; Kaduk, James A

    2017-02-01

    The crystal structure of caesium di-hydrogen citrate, Cs(+)·H2C6H5O7(-), has been solved and refined using laboratory X-ray powder diffraction data, and optimized using density functional techniques. The coordination polyhedra of the nine-coordinate Cs(+) cations share edges to form chains along the a-axis. These chains are linked by corners along the c-axis. The un-ionized carb-oxy-lic acid groups form two different types of hydrogen bonds; one forms a helical chain along the c-axis, and the other is discrete. The hy-droxy group participates in both intra- and inter-molecular hydrogen bonds.

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

    PubMed

    Rammohan, Alagappa; Kaduk, James A

    2017-01-01

    The crystal structure of dirubidium hydrogen citrate, 2Rb(+)·HC6H5O7(2-), has been solved and refined using laboratory X-ray powder diffraction data, and optimized using density functional techniques. The un-ionized carb-oxy-lic acid group forms helical chains of very strong hydrogen bonds (O⋯O ∼ 2.42 Å) along the b axis. The hy-droxy group participates in a chain of intra- and inter-molecular hydrogen bonds along the c axis. These hydrogen bonds result in corrugated hydrogen-bonded layers in the bc plane. The Rb(+) cations are six-coordinate, and share edges and corners to form layers in the ab plane. The inter-layer contacts are composed of the hydro-phobic methyl-ene groups.

  2. 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

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

    PubMed

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

    2015-03-01

    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 methods

  4. 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

  5. X-ray powder diffraction of high-absorption materials at the XRD1 beamline off the best conditions: Application to (Gd, Nd)5Si4 compounds

    NASA Astrophysics Data System (ADS)

    Carvalho, A. M. G.; Nunes, R. S.; Coelho, A. A.

    2017-03-01

    Representative compounds of the new family of magnetic materials Gd5-xNdxSi4 were analyzed by X-ray diffraction at the XRD1 beamline at LNLS. To reduce X-ray absorption, thin layers of the powder samples were mounted outside the capillaries and measured in Debye-Scherrer geometry as usual. The X-ray diffraction analyses and the magnetometry results indicate that the behavior of the magnetic transition temperature as a function of Nd content may be directly related to the average of the four smallest interatomic distances between different rare earth sites of the majority phase of each compound. The quality and consistency of the results show that the XRD1 beamline is able to perform satisfactory X-ray diffraction experiments on high-absorption materials even off the best conditions.

  6. 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.

  7. 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

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

    DOE PAGES

    Bellucci, Francesco; Lee, Sang Soo; Kubicki, James D.; ...

    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

  10. 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.

  11. Equilibrium, FTIR, scanning electron microscopy and small wide angle X-ray scattering studies of chromates adsorption on modified bentonite

    NASA Astrophysics Data System (ADS)

    Majdan, Marek; Maryuk, Oksana; Pikus, Stanisław; Olszewska, Elzbieta; Kwiatkowski, Ryszard; Skrzypek, Henryk

    2005-04-01

    The study presents a discussion about the adsorption mechanism of chromate anions on bentonite modified by hexadecyltrimethylammonium bromide (HDTMA-Br). The formation of alkylammonium chromates: HDTMAHCrO 4, (HDTMA) 2Cr 2O 7 and to the lesser extent (HDTMA) 2CrO 4 at the water-bentonite interface is examined based on the Scanning Electron Microscopy and surface tension measurements. The histograms of HDTMA/Cr(VI) molar ratio on the bentonite surface, found from Scanning Electron Microscopy (SEM) measurements, show that for the majority of points of bentonite surface the value of this ratio is in 1-2 range. FTIR spectra of modified bentonite samples show the change from gauche to trans conformation in the surfactant arrangement in the clay interlayer accompanying its concentration increase. In turn Small Wide Angle X-Ray Scattering (SWAXS) patterns evidently suggest incorporation of chromate anions into the interlamellar space of bentonite structure.

  12. Analytical capabilities of total reflection X-ray fluorescence spectrometry for silver nanoparticles determination in soil adsorption studies

    NASA Astrophysics Data System (ADS)

    Torrent, Laura; Iglesias, Mònica; Hidalgo, Manuela; Marguí, Eva

    2016-12-01

    In recent years, the production of silver nanoparticles (AgNPs) has grown due to their antibacterial properties. This fact enhances the release of these particles into the environment, especially in soils that are the major sink. To better understand adsorption processes in soils, usually batch kinetic studies are carried out. In this context, we tested the possibilities of using total reflection X-ray fluorescence spectrometry (TXRF) to monitor the silver content in soil adsorption kinetic studies. It was found that the lower limit of detection for Ag (through Ag-Kα detection) in aqueous solutions was around 37 μg·L- 1, which was suitable to carry out this kind of studies. Moreover, the direct analysis of Ag adsorbed onto soil after the kinetic studies was investigated. In this case, the limit of detection for Ag was around 1.7 mg·kg- 1. All TXRF results were compared with those obtained by inductively coupled plasma optic emission spectrometry and good agreement was found. The batch adsorption tests performed showed that 98% of polyvinylpyrrolidone coated AgNPs were retained on the tested soils in < 6 h.

  13. X-Ray diffraction on large single crystals using a powder diffractometer

    DOE PAGES

    Jesche, A.; Fix, M.; Kreyssig, A.; ...

    2016-06-16

    Information on the lattice parameter of single crystals with known crystallographic structure allows for estimations of sample quality and composition. In many cases it is sufficient to determine one lattice parameter or the lattice spacing along a certain, high- symmetry direction, e.g. in order to determine the composition in a substitution series by taking advantage of Vegard’s rule. Here we present a guide to accurate measurements of single crystals with dimensions ranging from 200 μm up to several millimeter using a standard powder diffractometer in Bragg-Brentano geometry. The correction of the error introduced by the sample height and the optimizationmore » of the alignment are discussed in detail. Finally, in particular for single crystals with a plate-like habit, the described procedure allows for measurement of the lattice spacings normal to the plates with high accuracy on a timescale of minutes.« less

  14. X-Ray diffraction on large single crystals using a powder diffractometer

    SciTech Connect

    Jesche, A.; Fix, M.; Kreyssig, A.; Meier, W. R.; Canfield, P. C.

    2016-06-16

    Information on the lattice parameter of single crystals with known crystallographic structure allows for estimations of sample quality and composition. In many cases it is sufficient to determine one lattice parameter or the lattice spacing along a certain, high- symmetry direction, e.g. in order to determine the composition in a substitution series by taking advantage of Vegard’s rule. Here we present a guide to accurate measurements of single crystals with dimensions ranging from 200 μm up to several millimeter using a standard powder diffractometer in Bragg-Brentano geometry. The correction of the error introduced by the sample height and the optimization of the alignment are discussed in detail. Finally, in particular for single crystals with a plate-like habit, the described procedure allows for measurement of the lattice spacings normal to the plates with high accuracy on a timescale of minutes.

  15. 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.

  16. 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.

  17. 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.

  18. X-Ray Fluorescence Analysis of Yttrium-Iron-Gadolinium Solutions Used to Prepare Spray Dried Powders.

    DTIC Science & Technology

    IRON, * GADOLINIUM , *X RAY SPECTROSCOPY, *YTTRIUM, COMPUTER PROGRAMS, SOLUTIONS(MIXTURES), QUALITY CONTROL, NITRIC ACID, RARE EARTH ELEMENTS, CHEMICAL ANALYSIS, FERRITES , PHASE SHIFT CIRCUITS, YTTRIUM IRON GARNET.

  19. Fluid adsorption in ordered mesoporous solids determined by in situ small-angle X-ray scattering.

    PubMed

    Findenegg, Gerhard H; Jähnert, Susanne; Müter, Dirk; Prass, Johannes; Paris, Oskar

    2010-07-14

    The adsorption of two organic fluids (n-pentane and perfluoropentane) in a periodic mesoporous silica material (SBA-15) is investigated by in situ small-angle X-ray scattering (SAXS) using synchrotron radiation. Structural changes are monitored as the ordered and disordered pores in the silica matrix are gradually filled with the fluids. The experiments yield integrated peak intensities from up to ten Bragg reflections from the 2D hexagonal pore lattice, and additionally diffuse scattering contributions arising from disordered (mostly intrawall) porosity. The analysis of the scattering data is based on a separation of these two contributions. Bragg scattering is described by adopting a form factor model for ordered pores of cylindrical symmetry which accounts for the filling of the microporous corona, the formation of a fluid film at the pore walls, and condensation of the fluid in the core. The filling fraction of the disordered intrawall pores is extracted from the diffuse scattering intensity and its dependence on the fluid pressure is analyzed on the basis of a three-phase model. The data analysis introduced here provides an important generalisation of a formalism presented recently (J. Phys. Chem. C, 2009, 13, 15201), which was applicable to contrast-matching fluids only. In this way, the adsorption behaviour of fluids into ordered and disordered pores in periodic mesoporous materials can be analyzed quantitatively irrespective of the fluid density.

  20. 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

  1. 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

    2016-06-08

    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.

  2. Coherent 3D nanostructure of γ-Al2O3: Simulation of whole X-ray powder diffraction pattern

    NASA Astrophysics Data System (ADS)

    Pakharukova, V. P.; Yatsenko, D. A.; Gerasimov, E. Yu.; Shalygin, A. S.; Martyanov, O. N.; Tsybulya, S. V.

    2017-02-01

    The structure and nanostructure features of nanocrystalline γ-Al2O3 obtained by dehydration of boehmite with anisotropic platelet-shaped particles were investigated. The original models of 3D coherent nanostructure of γ-Al2O3 were constructed. The models of nanostructured γ-Al2O3 particles were first confirmed by a direct simulation of powder X-Ray diffraction (XRD) patterns using the Debye Scattering Equation (DSE) with assistance of high-resolution transmission electron microscopy (HRTEM) study. The average crystal structure of γ-Al2O3 was shown to be tetragonally distorted. The experimental results revealed that thin γ-Al2O3 platelets were heterogeneous on a nanometer scale and nanometer-sized building blocks were separated by partially coherent interfaces. The XRD simulation results showed that a specific packing of the primary crystalline blocks in the nanostructured γ-Al2O3 particles with formation of planar defects on {001}, {100}, and {101} planes nicely accounted for pronounced diffuse scattering, anisotropic peak broadening and peak shifts in the experimental XRD pattern. The identified planar defects in cation sublattice seem to be described as filling cation non-spinel sites in existing crystallographic models of γ-Al2O3 structure. The overall findings provided an insight into the complex nanostructure, which is intrinsic to the metastable γ-Al2O3 oxide.

  3. A new approach for structure analysis of two-dimensional membrane protein crystals using X-ray powder diffraction data

    PubMed Central

    Dilanian, R A; Darmanin, C; Varghese, J N; Wilkins, S W; Oka, T; Yagi, N; Quiney, H M; Nugent, K A

    2011-01-01

    The application of powder diffraction methods to problems in structural biology is generally regarded as intractable because of the large number of unresolved, overlapping X-ray reflections. Here, we use information about unit cell lattice parameters, space group transformations, and chemical composition as a priori information in a bootstrap process that resolves the ambiguities associated with overlapping reflections. The measured ratios of reflections that can be resolved experimentally are used to refine the position, the shape, and the orientation of low-resolution molecular structures within the unit cell, in leading to the resolution of the overlapping reflections. The molecular model is then made progressively more sophisticated as additional diffraction information is included in the analysis. We apply our method to the recovery of the structure of the bacteriorhodopsin molecule (bR) to a resolution of 7 Å using experimental data obtained from two-dimensional purple membrane crystals. The approach can be used to determine the structure factors directly or to provide reliable low-resolution phase information that can be refined further by the conventional methods of protein crystallography. PMID:21154412

  4. Limits of visual detection for finasteride polymorphs in prepared binary mixtures: analysis by X-ray powder diffraction.

    PubMed

    Bezzon, Vinícius D N; Antonio, Selma G; Paiva-Santos, Carlos O

    2014-11-01

    Finasteride (FNT) is a drug that inhibits human enzyme type II 5α-reductase that metabolizes testosterone into dihydrotestosterone. There are two enantiotropic polymorphs with known crystal structure: designated as forms I and II. Identification and control of these polymorphic forms in mixtures can be performed using X-ray powder diffraction (XRPD) data and Rietveld method (RM). As experimental conditions may limit the detection of minority phases in mixtures, it is interesting to show what are these limits for some usual and one high-resolution equipment. So, in this work, we discuss the parameters to find the limit of the detection in binary mixtures of forms I and II of FNT according to each experimental condition. The samples analyzed were binary mixtures prepared with anhydrous polymorphs of the drug FNT. These samples were measured in four diffractometers with different experimental condition. These equipments represent the main resolutions generally used for drug analysis by XRPD. For the development of this work, a batch of form I was obtained pure, and another batch with forms I and II was used to obtain pure form II by heat treatment. Depending on the experimental condition, the polymorphs could be detected in a proportion as low as 0.5 wt%. © 2014 Wiley Periodicals, Inc. and the American Pharmacists Association J Pharm Sci 103:3567-3575, 2014.

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

    PubMed

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

    2014-03-01

    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 salt of acemetacin exhibits superior

  6. 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

  7. Adsorption of arsenate on untreated dolomite powder.

    PubMed

    Ayoub, G M; Mehawej, M

    2007-09-05

    Raw dolomite powder was evaluated for its efficiency in adsorbing As(V) from water. An experimental setup comprised of a fluidized dolomite powder bed was used to assess the impact of various test variables on the efficiency of removal of As(V). Test influents including distilled water (DW), synthetic groundwater (SGW) and filtered sewage effluent (FSE) were employed to assess the effect of influent parameters on the adsorption process and the quality of the effluent generated. Dolomite exhibited good As(V) removal levels for distilled water (>92%) and synthetic ground water (>84%) influents at all initial As(V) concentrations tested (0.055-0.600 ppm). Breakthrough of dolomite bed occurred after 45 bed volumes for DW and 20 bed volumes for SGW influents with complete breakthrough taking place at more than 300 bed volumes. As(V) removal from FSE influents was relatively unsuccessful as compared to the DW and SGW influents. Partial removal in the order of 32% from filtered sewage effluent at initial concentration of 0.6 mg/L started at 75 bed volumes and gradually stopped at 165 bed volumes. Varying degrees of As(V) adsorption capacities were observed by the different test influents employed, which indicate that the adsorption of As(V) is adversely affected by competing species, mainly sulfates and phosphates present in the influent. The adsorptive behavior of dolomite was described by fitting data generated from the study into the Langmuir and Freundlich isotherm models. Both models described well the adsorption of dolomite. The average isotherm adsorptive capacity was determined at 5.02 mug/g. Regeneration of the dolomite bed can be achieved with the use of caustic soda solution at a pH of 10.5.

  8. 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.

  9. Structure of Calcium Aluminate Decahydrate (CaAl2O4.10D2O) from Neutron and X-ray Powder Diffraction Data

    SciTech Connect

    Christensen,A.; Lebech, B.; Sheptyakov, D.; Hanson, J.

    2007-01-01

    Calcium aluminate decahydrate is hexagonal with the space group P63/m and Z = 6. The compound has been named CaAl2O4{center_dot}10H2O (CAH10) for decades and is known as the product obtained by hydration of CaAl2O4 (CA) in the temperature region 273-288 K - one of the main components in high-alumina cements. The lattice constants depend on the water content. Several sample preparations were used in this investigation: one CAH10, three CAD10 and one CA(D/H)10, where the latter is a zero-matrix sample showing no coherent scattering contribution from the D/H atoms in a neutron diffraction powder pattern. The crystal structure including the positions of the H/D atoms was determined from analyses of four neutron diffraction powder patterns by means of the ab initio crystal structure determination program FOX and the FULLPROF crystal structure refinement program. Additionally, eight X-ray powder diffraction patterns (Cu K[alpha]1 and synchrotron X-rays) were used to establish phase purity. The analyses of these combined neutron and X-ray diffraction data clearly show that the previously published positions of the O atoms in the water molecules are in error. Thermogravimetric analysis of the CAD10 sample preparation used for the neutron diffraction studies gave the composition CaAl2(OD)8(D2O)2{center_dot}2.42D2O. Neutron and X-ray powder diffraction data gave the structural formula CaAl2(OX)8(X2O)2{center_dot}[gamma]X2O (X = D, H and D/H), where the [gamma] values are sample dependent and lie between 2.3 and 3.3.

  10. 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.

  11. Synthesis, X-ray powder structure, and magnetic properties of the new, weak ferromagnet iron(II) phenylphosphonate.

    PubMed

    Bellitto, C; Federici, F; Altomare, A; Rizzi, R; Ibrahim, S A

    2000-04-17

    A new molecule-based weak ferromagnet of formula Fe[C6H5PO3].H2O was synthesized. It was characterized by thermogravimetric analysis and UV-visible and infrared spectroscopy, and the magnetic properties were studied using a superconducting quantum interference device magnetometer. The crystal structure of the compound was determined "ab initio" from X-ray powder diffraction data and refined by the Rietveld method. The crystals of Fe[C6H5PO3].H2O are orthorhombic, space group Pmn2(1), with a = 5.668(8) A, b = 14.453(2) A, c = 4.893(7) A, and Z = 2. The title compound is isostructural with the previously reported lamellar M[C6H5PO3].H2O, M = Mn(II), Zn(II), and Cd(II). The inorganic layers are made of Fe(II) ions octahedrally coordinated by five phosphonate oxygen atoms and one from oxygen of the water molecule. These layers are then separated by bilayers of the phenyl groups, and van der Waals contacts are established between them. The refinement has shown that the phenyl rings are disordered in the lattice. The oxidation state of the metal ion is +2, and the electronic configuration is d6 (S = 2) high-spin, as determined from dc magnetic susceptibility measurements from 150 K to room temperature. Below 100 K, the magnetic moment of Fe[C6H5PO3].H2O rises rapidly to a maximum at TN = 21.5 K, and then it decreases again. The peak at TN is associated with the 3D antiferromagnetic long-range ordering. Below the critical temperature, the title compound behaves as a "weak" ferromagnet, which represents the third type of magnetic materials characterized by having a finite zero-field magnetization, ferromagnets and ferrimagnets being the other two types. The large coercive field (i.e., 6400 G) observed in the hysteresis loop at T = 10 K is rare in molecule-based materials; it can be ascribed to a pronounced spin-orbit coupling for the 5T2g ground state of the Fe(II) ion in the octahedral environment.

  12. A combined approach for characterisation of fresh and brined vine leaves by X-ray powder diffraction, NMR spectroscopy and direct infusion high resolution mass spectrometry.

    PubMed

    Rizzuti, Antonino; Caliandro, Rocco; Gallo, Vito; Mastrorilli, Piero; Chita, Giuseppe; Latronico, Mario

    2013-12-01

    X-ray powder diffraction was combined, for the first time, with Nuclear Magnetic Resonance spectroscopy and direct infusion mass spectrometry to characterise fresh and brined grape leaves. Covariance analysis of data generated by the three techniques was performed with the aim to correlate information deriving from the solid part with those obtained for soluble metabolites. The results obtained indicate that crystalline components can be correlated to the metabolites contained in the grape leaves, paving the way to the use of X-ray diffraction analysis for food fingerprinting purposes. Moreover it was ascertained that, differently from most of the metabolites present in the fresh vine leaves, linolenic acid (an omega-3-fatty acid) and quercetin-3-O-glucuronide (a polyphenol metabolite) do not undergo sensible degradation during the brining process, which is used as preservative method for the grape leaves.

  13. 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/.

  14. 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.

  15. Adsorption of adenine and thymine on zeolites: FT-IR and EPR spectroscopy and X-ray diffractometry and SEM studies.

    PubMed

    Baú, João Paulo T; Carneiro, Cristine E A; de Souza Junior, Ivan G; de Souza, Cláudio M D; da Costa, Antonio C S; di Mauro, Eduardo; Zaia, Cássia T B V; Coronas, Joaquin; Casado, Clara; de Santana, Henrique; Zaia, Dimas A M

    2012-02-01

    The interactions of adenine and thymine with and adsorption on zeolites were studied using different techniques. There were two main findings. First, as shown by X-ray diffractometry, thymine increased the decomposition of the zeolites (Y, ZSM-5) while adenine prevented it. Second, zeolite Y adsorbed almost the same amount of adenine and thymine, thus both nucleic acid bases could be protected from hydrolysis and UV radiation and could be available for molecular evolution. The X-ray diffractometry and SEM showed that artificial seawater almost dissolved zeolite A. The adsorption of adenine on ZSM-5 zeolite was higher than that of thymine (Student-Newman-Keuls test-SNK p<0.05). Adenine was also more greatly adsorbed on ZSM-5 zeolite, when compared to other zeolites (SNK p<0.05). However the adsorption of thymine on different zeolites was not statistically different (SNK p>0.05). The adsorption of adenine and thymine on zeolites did not depend on pore size or Si/Al ratio and it was not explained only by electrostatic forces; rather van der Waals interactions should also be considered.

  16. Strategies for reducing preferred orientation and strain in powder samples for high-pressure synchrotron X-ray diffraction in diamond-anvil cells

    SciTech Connect

    Tschauner, Oliver; McClure, Jason; Nicol, Malcolm

    2010-07-20

    Among the many problems associated with high-pressure X-ray diffraction from polycrystalline samples in the diamond-anvil cell are strain and preferred orientation. A method is presented for efficiently reducing preferred orientation of powder samples compressed in diamond-anvil cells to pressures in excess of 20 GPa. This method may be successfully applied to samples of yield strength higher than alkalihalides. In addition, the problem of strain is discussed using ice-VII as an example and as an illustration of the importance of laser heating as a method of minimizing strain.

  17. 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.

  18. Disorder in the composite crystal structure of the manganese `disilicide' MnSi1.73 from powder X-ray diffraction data.

    PubMed

    Akselrud, L; Cardoso Gil, R; Wagner-Reetz, M; Grin, Yu

    2015-12-01

    The crystal structure of the higher manganese silicide MnSi1.7 (known in the literature as HMS) is investigated in samples with different compositions obtained by different techniques at temperatures not higher than 1273 K. Powder X-ray diffraction was applied. The crystal structure is described as incommensurate composite. In addition to the ordered model already known in the literature, the partial disorder in the silicon substructure was detected and described introducing an additional atomic site with a different modulation function.

  19. 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.

  20. 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.

  1. Driving force behind adsorption-induced protein unfolding: a time-resolved X-ray reflectivity study on lysozyme adsorbed at an air/water interface.

    PubMed

    Yano, Yohko F; Uruga, Tomoya; Tanida, Hajime; Toyokawa, Hidenori; Terada, Yasuko; Takagaki, Masafumi; Yamada, Hironari

    2009-01-06

    Time-resolved X-ray reflectivity measurements for lysozyme (LSZ) adsorbed at an air/water interface were performed to study the mechanism of adsorption-induced protein unfolding. The time dependence of the density profile at the air/water interface revealed that the molecular conformation changed significantly during adsorption. Taking into account previous work using Fourier transform infrared (FTIR) spectroscopy, we propose that the LSZ molecules initially adsorbed on the air/water interface have a flat unfolded structure, forming antiparallel beta-sheets as a result of hydrophobic interactions with the gas phase. In contrast, as adsorption continues, a second layer forms in which the molecules have a very loose structure having random coils as a result of hydrophilic interactions with the hydrophilic groups that protrude from the first layer.

  2. A comparative study of the use of powder X-ray diffraction, Raman and near infrared spectroscopy for quantification of binary polymorphic mixtures of piracetam.

    PubMed

    Croker, Denise M; Hennigan, Michelle C; Maher, Anthony; Hu, Yun; Ryder, Alan G; Hodnett, Benjamin K

    2012-04-07

    Diffraction and spectroscopic methods were evaluated for quantitative analysis of binary powder mixtures of FII(6.403) and FIII(6.525) piracetam. The two polymorphs of piracetam could be distinguished using powder X-ray diffraction (PXRD), Raman and near-infrared (NIR) spectroscopy. The results demonstrated that Raman and NIR spectroscopy are most suitable for quantitative analysis of this polymorphic mixture. When the spectra are treated with the combination of multiplicative scatter correction (MSC) and second derivative data pretreatments, the partial least squared (PLS) regression model gave a root mean square error of calibration (RMSEC) of 0.94 and 0.99%, respectively. FIII(6.525) demonstrated some preferred orientation in PXRD analysis, making PXRD the least preferred method of quantification.

  3. 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.

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

    SciTech Connect

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

    2016-01-15

    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 CeO{sub 2} powders and demonstrated diffraction measurements from an operating lithium-air battery.

  5. 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.

  6. Adsorption and stability of malonic acid on rutile TiO2 (110), studied by near edge X-ray absorption fine structure and photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Syres, Karen L.; Thomas, Andrew G.; Graham, Darren M.; Spencer, Ben F.; Flavell, Wendy R.; Jackman, Mark J.; Dhanak, Vinod R.

    2014-08-01

    The adsorption of malonic acid on rutile TiO2 (110) has been studied using photoelectron spectroscopy and C K-edge, near edge X-ray fine structure spectroscopy (NEXAFS). Analysis of the O 1s and Ti 2p spectra suggest that the molecule adsorbs dissociatively in a doubly-bidentate adsorption geometry as malonate. The data are unable to distinguish between a chelating bonding mode with the backbone of the molecule lying along the [001] azimuth or a bridging geometry along the direction. Work carried out on a wiggler beamline suggests that the molecule is unstable under irradiation by high-flux synchrotron radiation from this type of insertion device.

  7. Combined MAS NMR and X-ray powder diffraction structural characterization of hydrofluorocarbon-134 adsorbed on zeolite NaY: Observation of cation migration and strong sorbate-cation interactions

    SciTech Connect

    Grey, C.P.; Poshni, F.I.; Gualtieri, A.F.; Norby, P. |; Hanson, J.C.; Corbin, D.R.

    1997-02-26

    {sup 23}Na MAS NMR and synchrotron X-ray powder diffraction methods have been used to study the binding of hydrofluorocarbon-134 (HFC-134, CF{sub 2}HCF{sub 2}H) in zeolite NaY. A contraction of the volume of the unit cell is observed on gas adsorption, and the interaction of HFC-134 with the extraframework sodium cations is so strong that extraframework sodium cations in the sodalite cages (site I`) migrate into the supercages. These sodium cations are found on positions close to the site III` positions of zeolite NaX. Both ends of the HFC molecules are bound sodium cations, the HFC molecule bridging the site II and III` cations in the supercages. The strong cation-HFC interaction results in a considerable displacement of the sodium site II cation along the [111] direction into the supercage and an increase in the T-O-T bond angle for the three oxygen atoms coordinated to this cation. A decrease in the {sup 23}Na quadrupole coupling constant on HFC adsorption from 4.4 to less than 2.8 MHz, for the sodium cations originally located in the sodalite cages (site I`), is consistent with the sodium cation migrations. 26 refs., 7 figs., 5 tabs.

  8. 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.

  9. Pyrite surface environment drives molecular adsorption: cystine on pyrite(100) investigated by X-ray photoemission spectroscopy and low energy electron diffraction.

    PubMed

    Sanchez-Arenillas, M; Mateo-Marti, E

    2016-10-05

    We have demonstrated that the annealing process for cleaning pyrite surfaces is a critical parameter in promoting ordering on the surface and driving surface reactivity. Furthermore, we describe a spectroscopic surface characterization of the presence or absence of the surface ordering, as indicated by the Low Energy Electron Diffraction (LEED) pattern, as a function of the surface annealing process. Complementary X-ray photoemission spectroscopy (XPS) results provide evidence that longer annealing processes of over 3 hours repair the sulfur vacancies in the pyrite, making FeS species partially disappear in favor of FeS2 species. These features play an important role in molecular adsorption. We show that in the case of the cystine amino acid on the (100) pyrite surface, the substrate structure is responsible for the chemical adsorption form. The presence of an ordered structure on the surface, as indicated by the LEED pattern, favors the cystine NH3(+) chemical form, whereas the absence of the surface ordering promotes cystine NH2 adsorption due to the sulfur-deficient surface. The cystine molecule could then act by changing its chemical functionalities to compensate for the iron surface coordination. The chemical molecular adsorption form can be selected by the surface annealing conditions, implying that environmental conditions could drive molecular adsorption on mineral surfaces. These findings are relevant in several surface processes, and they could play a possible role in prebiotic chemistry surface reactions and iron-sulfur scenarios.

  10. Adsorption of basic dyes from aqueous solution onto pumice powder.

    PubMed

    Akbal, Feryal

    2005-06-15

    The adsorption of methylene blue and crystal violet on pumice powder samples of varying compositions was investigated using a batch adsorption technique. The effects of various experimental parameters, such as adsorbent dosage, initial dye concentration, and contact time, were also investigated. The extent of dye removal increased with decreased initial concentration of the dye and also increased with increased contact time and amount of adsorbent used. Adsorption data were modeled using the Freundlich adsorption isotherm. The adsorption kinetic of methylene blue and crystal violet could be described by the pseudo-second-order reaction model.

  11. 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).

  12. Crystal structure of dicesium hydrogen citrate from laboratory single-crystal and powder X-ray diffraction data and DFT comparison.

    PubMed

    Rammohan, Alagappa; Sarjeant, Amy A; Kaduk, James A

    2017-02-01

    The crystal structure of dicesium hydrogen citrate, 2Cs(+)·C6H6O7(2-), has been solved using laboratory X-ray single-crystal diffraction data, refined using laboratory powder X-ray data, and optimized using density functional techniques. The Cs(+) cation is nine-coordinate, with a bond-valence sum of 0.92 valence units. The CsO9 coordination polyhedra share edges and corners to form a three-dimensional framework. The citrate anion is located on a mirror plane. Its central hy-droxy/carboxyl-ate O-H⋯O hydrogen bond is short, and (unusually) inter-molecular. The centrosymmetric end-end carboxyl-ate hydrogen bond is exceptionally short (O⋯O = 2.416 Å) and strong. These hydrogen bonds contribute 16.5 and 21.7 kcal mol(-1), respectively, to the crystal energy. The hydro-phobic methyl-ene groups occupy pockets in the framework.

  13. Germanate with three-dimensional 12 × 12 × 11-ring channels solved by X-ray powder diffraction with charge-flipping algorithm.

    PubMed

    Xu, Yan; Liu, Leifeng; Chevrier, Daniel M; Sun, Junliang; Zhang, Peng; Yu, Jihong

    2013-09-16

    A new open-framework germanate, denoted as GeO-JU90, was prepared by the hydrothermal synthesis method using 1,5-bis(methylpyrrolidinium)pentane dihydroxide as the organic structure-directing agent (SDA). The structure of GeO-JU90 was determined from synchrotron X-ray powder diffraction (XRPD) data using the charge-flipping algorithm. It revealed a complicated framework structure containing 11 Ge atoms in the asymmetric unit. The framework is built of 7-connected Ge7 clusters and additional tetrahedral GeO3(OH) units forming a new three-dimensional interrupted framework with interesting 12 × 12 × 11-ring intersecting channels. The Ge K-edge extended X-ray absorption fine structure (EXAFS) analysis was performed to provide the local structural information around Ge atoms, giving rise to a first-shell contribution from about 4.2(2) O atoms at the average distance of 1.750(8) Å. The guest species in the channels were subsequently determined by the simulated annealing method from XRPD data combining with other characterization techniques, e.g., (13)C NMR spectroscopy, infrared spectroscopy (FTIR), compositional analyses, and thermogravimetric analysis (TGA). Crystallographic data |(C15N2H32)(NH4)|[Ge11O21.5(OH)4], orthorhombic Ama2 (No. 40), a = 37.82959 Å, b = 15.24373 Å, c = 12.83659 Å, and Z = 8.

  14. Crystal structure of dicesium hydrogen citrate from laboratory single-crystal and powder X-ray diffraction data and DFT comparison

    PubMed Central

    Rammohan, Alagappa; Sarjeant, Amy A.; Kaduk, James A.

    2017-01-01

    The crystal structure of dicesium hydrogen citrate, 2Cs+·C6H6O7 2−, has been solved using laboratory X-ray single-crystal diffraction data, refined using laboratory powder X-ray data, and optimized using density functional techniques. The Cs+ cation is nine-coordinate, with a bond-valence sum of 0.92 valence units. The CsO9 coordination polyhedra share edges and corners to form a three-dimensional framework. The citrate anion is located on a mirror plane. Its central hy­droxy/carboxyl­ate O—H⋯O hydrogen bond is short, and (unusually) inter­molecular. The centrosymmetric end-end carboxyl­ate hydrogen bond is exceptionally short (O⋯O = 2.416 Å) and strong. These hydrogen bonds contribute 16.5 and 21.7 kcal mol−1, respectively, to the crystal energy. The hydro­phobic methyl­ene groups occupy pockets in the framework. PMID:28217349

  15. Analysis of the average poly-cyclic aromatic unit in a meta-anthracite coal using conventional x-ray powder diffraction and intensity separation methods

    SciTech Connect

    Wertz, D.L.; Bissell, M.

    1994-12-31

    X-ray characterizations of coals and coal products have occurred for many years. Hirsch and Cartz measured the diffraction from several coals over the reciprocal space region from s = 0.12 {angstrom}{sup -1} to 7.5 {angstrom}{sup -1} where s = (4{pi}/{lambda}) sin{Theta}. In these studies, a 9 cm powder camera was used to study the high angle region, and a transmission type focusing camera equipped with a LiF monochromator was used for the low angle measurements. They reported that the height of the graphene peak measured for each coal is proportional to the % carbon in the coals. Hirsch also suggested that the ontyberem anthracite has a lamellar diameter of ca. 16 {angstrom} corresponding to an aromatic lamellae of ca. C{sub 87}. For coals with lower carbon content, Hirsch proposed much smaller lamellae; C{sub 19} for a coal with 80% carbon, and C{sub 24} for a coal with 89% carbon. The subject coal for this study is a meta-anthracite which was derived from the Portsmouth, RI mine. The Narragansett Basin contains anthracite and meta-anthracite coals of Pennsylvanian Age. The Basin was a techtonically active non-marine coal-forming basin which has been impacted by several tectonic events. Because of the importance placed by coal scientists no correctly characterizing the nature of the micro-level structural cluster(s) in coals and because of improvements in both x-ray experimentation capabilities and computing power, we have measured the x-ray diffraction and scattering produced from irradiation of this meta-anthracite coal which contains about 94% aromatic carbon. The goal of our study is to determine the intra-planar, and where possible, inter-planar structural details of coals. To accomplish this goal we have utilized the methods normally used for the molecular analysis of non-crystalline condensed phases such as liquids, solutions, and amorphous solids. Reported herein are the results obtained from the high angle x-ray analysis of this coal.

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

    DOE PAGES

    Lazarević, N.; Abeykoon, M.; Stephens, P. W.; ...

    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.

  17. Crystal structure of silica-ZSM-12 by the combined use of high-resolution solid-state MAS NMR spectroscopy and synchrotron x-ray powder diffraction

    SciTech Connect

    Fyfe, C.A.; Kokotailo, G.T. ); Gies, H.; Marler, B. ); Cox, D.E. )

    1990-05-03

    The crystal structure of the synthetic zeolite silica-ZSM-12, 56 SiO{sub 2}, has been solved by the combined use of high-resolution solid-state MAS NMR spectroscopy and high-resolution synchrotron X-ray powder diffraction ZSM-12 crystallizes in the monoclinic space group C2/c with a{sub 0} = 24.863 {angstrom}, b{sub 0} = 5.012 {angstrom}, c{sub 0} = 24.328 {angstrom}, and {beta} = 107.7{degree}. The zeolite host structure is built from corner-linked SiO{sub 4} tetrahedra to give a three-dimensional 4-connected net. The pores of the structure are one-dimensional channels that do not intersect, with 12-membered ring pore openings of approximately 5.6 {times} 7.7 {angstrom}. The structure of ZSM-12 is frequently twinned with (100) as the twin plane, which indicates a new zeolite structure type.

  18. Description of a flexible cell for in situ X-ray and far-IR characterization of the surface of powdered materials

    NASA Astrophysics Data System (ADS)

    Lamberti, C.; Prestipino, C.; Bordiga, S.; Berlier, G.; Spoto, G.; Zecchina, A.; Laloni, A.; La Manna, F.; D'Anca, F.; Felici, R.; D'Acapito, F.; Roy, P.

    2003-01-01

    We have designed and realized a cell where a powdered sample, in form of self-supported pellet, can be (i) in situ heated up to 900 K, either under dynamical vacuum or in reducing/oxidizing atmosphere; (ii) contacted with the desired amount of adsorbed gas; (iii) cooled down to 77 K for measurements. The cell (transmission geometry) has been employed in X-ray absorption experiments at LURE DCI (EXAFS13) and ESRF (GILDA BM8 and ID24), in far-IR experiments at LURE Super-ACO (SIRLOIN) and in conventional mid-IR experiments in our laboratory, only by changing the windows (mylar, silicon and KBr, respectively). A brief overview on the results obtained with this cell is reported to illustrate the potentialities of the instrument. Literature is quoted to allow possible in-depth study.

  19. Comparison of high sensitivity micro differential scanning calorimetry with X-ray powder diffractometry and FTIR spectroscopy for the characterization of pharmaceutically relevant non-crystalline materials.

    PubMed

    Song, M; Liebenberg, W; De Villiers, M M

    2006-04-01

    In this study, high sensitivity micro differential scanning calorimetry (MDSC) in the scanning of dynamic mode was compared to X-ray powder diffractometry (XRPD) for quantifying amorphous nifedipine in mixtures crystalline nifedipine. This technique was also compared with FTIR for quantifying polymorph A of chloramphenicol palmitate (CAP) and poly DL-lactide-co-glycolide) (PLGA) in pharmaceutical formulations. The limit of determination (LOD) achieved by MDSC were 0.06% compared to 5% for XRPD quantification of amorphous nifedipine and 0.02% compared to 7% for IR quanitfication of polymorph A of CAP. As little as 0.165 mg PLGA could be measured in excipients mixtures. Desirable linearity and repeatability were established in all cases.

  20. Polymorphism of ceramide 6: a vibrational spectroscopic and X-ray powder diffraction investigation of the diastereomers of N-(alpha-hydroxyoctadecanoyl)-phytosphingosine.

    PubMed

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

    2005-01-01

    A preparative chromatographic method was developed for the quantitative isolation of the diastereomers of synthetic N-(alpha-hydroxyoctadecanoyl)-phytosphingosine (DL-CER6). The L- and the D-compound were studied each by means X-ray powder diffraction, FT-Raman and FT-IR spectroscopy. The diastereomers exhibit different thermotropic polymorphism. Three lamellar crystalline and a lamellar liquid crystalline phase were found for L-CER6. The natural occurring D-CER6 forms an Lalpha phase with a larger repeating distance than the L-CER6. The two lamellar crystalline phases of the D-compound have a significant larger dimension than those of the L-compound. The addition of water lowers the phase transition temperatures but does not induce structural changes such as incorporation into the lamellar sheets.

  1. Lithium cobalt(II) pyrophosphate, Li1.86CoP2O7, from synchrotron X-ray powder data

    PubMed Central

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

    2011-01-01

    Structure refinement of high-resolution X-ray powder diffraction data of the title compound gave the composition Li1.865CoP2O7, which is also verified by the ICP measurement. Two Co sites exist in the structure: one is a CoO5 square pyramid and the other is a CoO6 octa­hedron. They share edges and are further inter­connected through P2O7 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. PMID:22065824

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. Molecular and crystalline structures of three (S)-4-alkoxycarbonyl-2-azetidinones containing long alkyl side chains from synchrotron X-ray powder diffraction data.

    PubMed

    Seijas, Luis E; Mora, Asiloé J; Delgado, Gerzon E; López-Carrasquero, Francisco; Báez, María E; Brunelli, Michela; Fitch, Andrew N

    2009-12-01

    The (S)-4-alkoxo-2-azetidinecarboxylic acids are optically active beta-lactam derivatives of aspartic acid, which are used as precursors of carbapenem-type antibiotics and poly-beta-aspartates. The crystal structures of three (S)-4-alkoxo-2-azetidinecarboxylic acids with alkyl chains with 10, 12 and 16 C atoms were solved using parallel tempering and refined against the X-ray powder diffraction data using the Rietveld method. The azetidinone rings in the three compounds display a pattern of asymmetrical bond distances and an almost planar conformation; these characteristics are compared with periodic solid-state, gas-phase density-functional theory (DFT) calculations and MOGUL average bond distances and angles from the CSD. The compounds pack along [001] as corrugated sheets separated by approximately 4.40 A and connected by hydrogen bonds of the type N-H...O.

  7. 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.

  8. 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.

  9. 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.

  10. In situ powder X-ray diffraction, synthesis, and magnetic properties of the defect zircon structure ScVO(4-x).

    PubMed

    Shafi, Shahid P; Kotyk, Matthew W; Cranswick, Lachlan M D; Michaelis, Vladimir K; Kroeker, Scott; Bieringer, Mario

    2009-11-16

    We report the formation pathway of ScVO(4) zircon from ScVO(3) bixbyite with emphasis on the synthesis and stability of the novel intermediate defect zircon phase ScVO(4-x) (0.0 < x powder X-ray diffraction. The oxidation of ScVO(3) to ScVO(4) involves two intermediates of composition ScVO(3.5+y) (0.00 powder X-ray diffraction, neutron diffraction, and bulk magnetic susceptibility data as well as (45)Sc and (51)V solid state NMR spectroscopy. ScVO(4-x) can only be obtained by oxidation of ScVO(3) or ScVO(3.5+y) while the reduction of ScVO(4) does not yield the novel defect structure. Mechanistic insights into the oxidative formation of ScVO(4) via the defect structure are presented.

  11. Single-crystal X-ray and powder neutron diffraction of ThB 2C (ThB 2C-type)

    NASA Astrophysics Data System (ADS)

    Rogl, Peter; Fischer, Peter

    1989-02-01

    The crystal structure of ThB 2C was determined using single-crystal X-ray and powder neutron diffraction data. ThB 2C crystallizes in the rhombohedral space group R overline3m with a = 0.66761(23), c = 1.13760(31) nm, {c}/{a} = 1.704, V = 0.4391 nm 3, Z = 9 . X-ray intensity data were obtained from a four-circle diffractometer; the structure was solved by Patterson methods and refined by full-matrix least-squares calculation. R = {∑|ΔF|}/{∑|F o| } = 0.034 for an asymmetric set of 219 independent reflections (| Fo| > 2 σ( Fo)). Precise nonmetal atom parameters and bond distances have been derived from room-temperature neutron powder diffraction data employing the Rietveld-Young profile analysis method. The reliability value of the neutron refinement was RI = 0.067. The crystal structure of ThB 2C is a new structure type with slightly puckered 6 3-Th-metal layers alternating with nonmetal layers each composed of hexagons of boron atoms, the hexagons being linked by carbon atoms. Boron atoms are in a triangular prismatic metal surrounding of a tetrakaidekahedral coordination |Th 6B 2C 1|B, whereas carbon atoms occupy the center points of quadratic bipyramids |Th 4B 2|C. The crystal structure of ThB 2C derives from the AlB 2-type structure with carbon atoms entering the boron nets to form a 2∞ - (6B) · (6B(3C)) 2 layer.

  12. 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.

  13. 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.

  14. 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.

  15. Chest X-Ray

    MedlinePlus

    ... by Image/Video Gallery Your radiologist explains chest x-ray. Transcript Welcome to Radiology Info dot org! Hello, ... you about chest radiography also known as chest x-rays. Chest x-rays are the most commonly performed ...

  16. 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 ...

  17. Assessment of in vitro binding of isolated pectic domains to cellulose by adsorption isotherms, electron microscopy, and X-ray diffraction methods.

    PubMed

    Zykwinska, Agata; Gaillard, Cédric; Buléon, Alain; Pontoire, Bruno; Garnier, Catherine; Thibault, Jean-François; Ralet, Marie-Christine

    2007-01-01

    Isolated pectic domains representative of the pectic backbone and the neutral sugar side chains were tested for their ability to interact with cellulose in comparison to the well-known binding of xyloglucan. Pectic side chains displayed a significant in vitro binding capacity to cellulose, whereas pectic backbone domains exhibited only slight adsorption to cellulose microfibrils. To support the binding results, electron microscopy and X-ray diffraction were applied. Celluloses from bacteria and sugar beet cell walls were used as substrates for the precipitation of isolated pectic domains or xyloglucan by acetone vapor diffusion. Pectic side chains grew attached to the cellulose surfaces, whereas pectic backbone domains were observed separately from cellulose microfibrils. Xyloglucan seeded with cellulose provoked a decrease of microfibrils entanglement, but no clear cross-links between neighboring microfibrils were observed. These results led to the elucidation of the pectic domains responsible for binding with cellulose microfibrils.

  18. 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.

  19. Biosorption of chromium by alginate extraction products from Sargassum filipendula: investigation of adsorption mechanisms using X-ray photoelectron spectroscopy analysis.

    PubMed

    Bertagnolli, Caroline; Uhart, Arnaud; Dupin, Jean-Charles; da Silva, Meuris Gurgel Carlos; Guibal, Eric; Desbrieres, Jacques

    2014-07-01

    The alginate extraction products from Brazilian brown seaweed Sargassum filipendula were studied for chromium biosorption. Batch experiments were conducted at pH 2 and 3 and 20°C to determine the sorption capacity of this biosorbents for chromium (VI) and (III). The biomass was characterized before and after metal binding by X-ray photoelectron spectroscopy (XPS) in order to determine the mechanisms of chromium biosorption. The residue has a high adsorption capacity, close the value obtained with seaweed and higher than that of alginate for both Cr(III) and Cr(VI). XPS analysis of the biosorbents revealed that carboxyl, amino and sulfonate groups are responsible for the binding of the metal ions. The analysis also indicated that the Cr(VI) bound to the biomass was reduced to Cr(III).

  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.

  1. 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.

  2. CHARACTERIZATION OF THE LOCAL TITANIUM ENVIRONMENT IN DOPED SODIUM ALUMINUM HYDRIDE USING X-RAY ADSORPTION SPECTROSCOPY.

    SciTech Connect

    GRAETZ, J.; IGNATOV, A. YU; TYSON, T.A.; REILLY, J.J.; JOHNSON, J.

    2004-11-30

    Ti K-edge x-ray absorption spectroscopy was used to explore the local titanium environment and valence in 2-4 mol% Ti-doped sodium alanate. An estimate of the oxidation state of the dopant, based upon known standards, revealed a zero-valent titanium atom. An analysis of the near-edge and extended fine structures indicates that the Ti does not enter substitutional or interstitial sites in the NaAlH{sub 4} lattice. Rather, the Ti is located on/near the surface and is coordinated by 10.2 {+-} 1 aluminum atoms with an interatomic distance of 2.82 {+-} 0.01 {angstrom}, similar to that of TiAl{sub 3}. The Fourier transformed EXAFS spectra reveals a lack of long-range order around the Ti dopant indicating that the Ti forms nano-clusters of TiAl{sub 3}. The similarity of the spectra in the hydrided and dehydrided samples suggests that the local Ti environment is nearly invariant during hydrogen cycling.

  3. 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.

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

    PubMed

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

    2013-06-14

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

  5. [Study on X-ray powder diffraction of various structured zinc titanate prepared by the method of direct precipitation].

    PubMed

    Guo, Jian; Wang, Zhi-hua; Tao, Dong-liang; Guo, Guang-sheng

    2007-05-01

    Zinc titanate powders were prepared from Ti(SO4)2, Zn(NO3)2 x (6)H2O and (NH4)2CO3 by the method of direct precipitation. The effects of reaction conditions on the structure of zinc titanate were studied. The sample was analyzed by means of XRD and TG-DTA. The structure of zinc titanate was affected by the reaction subsequence of the formation of titanic acid and zinc carbonate. In the reaction system where titanic acid was generated earlier, collision reaction occurred between the generated zinc carbonate molecule and the surrounding titanic acid molecule. When titanic acid was generated earlier and precipitant (NH4)2CO3 was sufficient, Zn2Ti3O8 was obtained because of the sufficient collision reaction and superfluous titanic acid. In the reaction system where zinc carbonate was generated earlier, collision reaction occurred between the generated titanic acid molecule and the surrounding zinc carbonate molecule. When zinc carbonate was generated earlier and precipitant (NH4)2CO3 was sufficient, Zn2TiO4 was obtained because of the sufficient collision reaction and superfluous zinc carbonate. In addition, the kinds and structure of the production were affected by the dosage of precipitant and the reaction temperature. Zn2Ti3O8 or Zn2TiO4 could be obtained easier when using more precipitant or higher reaction temperature which could cause more sufficient collision reaction. ZnTiO3 could be obtained under the conditions of less precipitant and lower reaction temperature.

  6. 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.

  7. Insights from arsenate adsorption on rutile (110): grazing-incidence X-ray absorption fine structure spectroscopy and DFT+U study.

    PubMed

    Yan, Li; Hu, Shan; Duan, Jinming; Jing, Chuanyong

    2014-07-03

    Insights into the bonding of As(V) at the metal oxide/aqueous interface can further our understanding of its fate and transport in the environment. The motivation of this work is to explore the interfacial configuration of As(V) on single crystal rutile (110) using grazing-incidence X-ray absorption fine structure spectroscopy (GI-XAFS) and planewave density functional calculations with on-site repulsion (DFT+U). In contrast to the commonly considered corner-sharing bidentate binuclear structure, tetrahedral As(V) binds as an edge/corner-sharing tridentate binuclear complex on rutile (110), as evidenced by observation of three As-Ti distances at 2.83, 3.36, and 4.05 Å. In agreement with the GI-XAFS analysis, our DFT+U calculations for this configuration resulted in the lowest adsorption energy among five possible alternatives. In addition, the electron density difference further demonstrated the transfer of charge between surface Ti atoms and O atoms in AsO4. This charge transfer consequently induced the formation of a chemical bond, which is also confirmed by the partial density of states analysis. Our results may shed new light on coupling the GI-XAFS and DFT approaches to explore molecular-scale adsorption mechanisms on single crystal surfaces.

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

    PubMed Central

    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

  9. Thermal expansion of anatase and rutile between 300 and 575 K using synchrotron powder X-ray diffraction

    SciTech Connect

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

    2007-01-01

    High-precision unit-cell parameters for the TiO2 polymorphs anatase and rutile at temperatures between 300 and 575 K have been determined using Rietveld analysis of synchrotron powder XRD data. Polynomial models were used to express the tetragonal unit-cell parameters as a function of absolute temperature, with a (anatase)=1.759 37x10-8xT2+6.418 16x10-6xT+3.779 84, c (anatase)=6.6545x10-8xT2+4.0464x10-5xT+9.4910, V (anatase)=2.237 58x10-6xT2+1.027 77x10-3xT+135.602, a (rutile)=-6.636 42x10-11xT3+1.005 01x10-7xT2-1.009 9310-5xT+4.586 34, c (rutile)=-4.115 50x10-11xT3+6.405 94x10-8xT2+4.675 61x10-7T+2.951 81, and V (rutile)=-2.7790x10-9xT3+4.2386x10-6xT2-3.3551x10-4xT+62.100. The polynomial expressions were used to calculate linear (alpha) and volume (beta) thermal expansion coefficients of anatase and rutile between 300 and 575 K. At 298.15 K, these values were alphaa=4.46943x10-6 K-1, alphac=8.4283x10-6 K-1, and beta=17.3542x10-6 K-1 for anatase, and alphaa=6.99953x10-6 K-1, alphac=9.36625x10-6 K-1, and beta=28.680x10-6 K-1 for rutile.

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

    SciTech Connect

    Caliandro, Rocco; Sibillano, Teresa; Belviso, B. Danilo; Scarfiello, Riccardo; Dooryhee, Eric; Manca, Michele; Cozzoli, P. Davide

    2016-02-02

    In this study, 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. Finally, the time behavior of such structural change is identified on the basis of multivariate analysis.

  11. 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

  12. 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

    2016-03-03

    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.

  13. Determination of tacrolimus crystalline fraction in the commercial immediate release amorphous solid dispersion products by a standardized X-ray powder diffraction method with chemometrics.

    PubMed

    Rahman, Ziyaur; Siddiqui, Akhtar; Bykadi, Srikant; Khan, Mansoor A

    2014-11-20

    Clinical performance of an amorphous solid dispersion (ASD) drug product is related to the amorphous drug content because of the greater bioavailability of this form of the drug than its crystalline form. Therefore, it is paramount to monitor the amorphous and the crystalline fractions in the ASD products. The objective of the present investigation was to study the feasibility of using a standardized X-ray powder diffraction (XRPD) in conjunction with chemometric methods to quantitate the amorphous and crystalline fraction of the drug in several tacrolimus ASD products. Three ASD products were prepared in which drug to excipients ratios ranged from 1:19 to 1:49. The amorphous and crystalline drug products were mixed in various proportions so that amorphous/crystalline tacrolimus in the samples vary from 0 to 100%. XRPD of the samples of the drug products were collected, and PLSR and PCR chemometric methods were applied to the data. The R(2) was greater than '0.987' for all the models and bias in the models were statistically insignificant (p>0.05). RMSEP and SEP values were smaller for PLSR models than PCR models. The models prediction capabilities were good and can predict as low as 10% when drug to excipient ratio is as high as 1:49. In summary, XRPD and chemometric provide powerful analytical tools to monitor the crystalline fractions of the drug in the ASD products.

  14. X-Ray Powder Diffraction Data for Na8(AlSiO4)6(ReO4)2

    SciTech Connect

    McCready, David E.; Mattigod, Shas V.; Young, James S.; McGrail, B. Peter

    2004-01-31

    X-ray powder diffraction data for a new zeolite, Na8(AlSiO4)6(ReO4)2, are reported. Rietveld refinement shows this compound adopts the primitive cubic structure of sodalite (Space Group , #218) with a = 9.1528 (1) Å. The calculated value of the reference intensity ratio (RIR, or I/Ic) is 7.54. The experimental density (Dm) is 2.98 ± 0.10 g/cm3, in agreement with the calculated density (Dx) of 3.029 g/cm3. Chemical analysis of Na8(AlSiO4)6(ReO4)2 gives its composition as 11.7 ± 1.6 wt % Na; 10.7 ± 0.2 wt % Al; 11.6 ± 0.9 wt % Si; 30.6 ± 1.2 wt % Re, which compares favorably with the theoretical composition of 13.2 wt % Na, 11.6 wt% Al, 12.1 wt% Si; 26.6 wt % Re. In addition, scanning electron microscopy reveals a doubly terminated trapezohedral crystal morphology for Na8(AlSiO4)6(ReO4)2, which is typical of sodalite.

  15. 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.

  16. 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.

  17. X-ray powder diffraction, spectroscopic study, dielectric properties and thermal analysis of new doped compound TiGa0.67Te2.33O8

    NASA Astrophysics Data System (ADS)

    Smaoui, S.; Ben Aribia, W.; Kabadou, A.; Abdelmouleh, M.

    2017-04-01

    A novel mixed valence tellurium oxide, TiGa0.67Te2.33O8, was synthesized and its crystal structure determined using the X-ray powder diffraction technique. The obtained oxide was found to crystallize in a cubic unit-cell, Ia 3 bar space group, with the lattice parameter a = 10.9557(1) Å. Rietveld refinement of the structure led to ultimate confidence factors Rp = 7.63 and Rwp = 6.71. This structure was based on slabs containing groups of (Te/Ga)O4 joined by the metal cations Ti4+. The structure analysis showed a cation ordering of Te4+ and Te6+ yielding a TiGa2/3Te7/3O8 formula. The IR and RAMAN spectra confirmed the presence of the TiO6 and (Te/Ga)O4 groups. The dielectric anomalies observed at 500 K were attributed to the mixed valence structure, arising from the mixed-valence Te6+/Te4+. We detected only one peak in thermal behavior by the DTA/TG analysis; which implied a melting reaction.

  18. Structural studies of Ni{sub 2+x}Mn{sub 1-x}Ga by powder x-ray diffraction and total energy calculations

    SciTech Connect

    Banik, S.; Bhardwaj, S.; Lalla, N. P.; Awasthi, A. M.; Sathe, V.; Phase, D. M.; Barman, S. R.; Ranjan, R.; Pandey, D.; Chakrabarti, A.; Mukhopadhyay, P. K.

    2007-03-01

    The crystal structure of Ni{sub 2+x}Mn{sub 1-x}Ga has been studied as a function of composition (x) by powder x-ray diffraction. For Ni{sub 2.24}Mn{sub 0.75}Ga, where one-fourth of the Mn atoms are replaced by Ni, the experimentally determined lattice constants are in good agreement with theoretical equilibrium lattice constants calculated by minimization of total energy using full potential linearized augmented plane-wave method. For 0.15{<=}x{<=}0.35, a nonmodulated tetragonal martensitic phase is obtained at room temperature, whose lattice constant c increases and a decreases linearly with increasing x following Vegard's law. A 7M modulated monoclinic phase is obtained for x=0.2 due to annealing. The small width of the hysteresis of the martensitic transition shows its thermoelastic nature that is the characteristic of a shape memory alloy. Phase coexistence is observed for 0.1{<=}x{<=}0.15 at room temperature, confirming the first-order nature of the martensitic transition.

  19. 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.

  20. 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}.

  1. Synthesis, solid-state NMR, and X-ray powder diffraction characterization of group 12 coordination polymers, including the first example of a C-mercuriated pyrazole.

    PubMed

    Masciocchi, Norberto; Galli, Simona; Alberti, Enrica; Sironi, Angelo; Di Nicola, Corrado; Pettinari, Claudio; Pandolfo, Luciano

    2006-10-30

    Cadmium and mercury acetates have been reacted with pyrazole (Hpz) and 3,5-dimethylpyrazole (Hdmpz), affording distinct mixed-ligand species, selectively prepared upon slightly modifying the reaction conditions. Two polymorphs of [{Cd(mu-ac)2(Hpz)2}n], as well as the [{Cd(mu-ac)2(Hdmpz)2}n] species (Hac = acetic acid), were obtained by solution chemistry, while the two-dimensional [{Cd3(mu3-ac)4(mu-pz)2(Hpz)2}n] and [{Cd(mu-ac)(mu-pz)}n] polymers were prepared upon controlled thermal treatment of one of the [{Cd(mu-ac)2(Hpz)2}n] forms. Two mercury derivatives, [{Hg3(mu-ac)3(mu-pz)3}n] and [{Hg(ac)(mu-dmpz)}n], were also prepared, the latter containing one-dimensional chains of Hg(II) ions bridged by C-mercuriated Hdmpz ligands. All their crystal structures (but one) were determined by powder diffraction methods using conventional X-ray laboratory equipment, supported by 13C CPMAS NMR measurements. The latter method helped in assigning a C-metalated nature to an amorphous material of [Hg(ac)(pz)] formula, obtained by employing EtOH as a solvent. A few other Hdmpz-containing cadmium acetates were also prepared, but their polyphasic nature, evidenced by diffraction methods, hampered their complete structural characterization.

  2. Characterisation of Incommensurate Bi2+xSr2-xCuOz by X-Ray Powder Diffraction and Oxygen Content Determinations

    NASA Astrophysics Data System (ADS)

    Sinclair, D. C.; Irvine, J. T. S.; West, A. R.

    1990-11-01

    The composition-temperature stability region of the solid solution Bi2+xSr2-xCuOz, phase R, has been determined. At 800°C, 0.15X-ray powder diffraction pattern can be indexed using a pseudo-tetragonal subcell, a{=}b{=}5.390(1), c{=}24.59 Å, with a supercell vector q* given by q*{=}nδ b*-n\\varepsilon c*, where δ{=}0.21, \\varepsilon{=}0.55, for x{=}0.30 and n{=}1, 2\\cdots. Both a and \\varepsilon increased with x, c decreased with x and δ was independent of x. The excess oxygen content, α, was determined to be (0.18± 0.02) by citrate iodometry and was independent of x. The total oxygen content z, given by z{=}6+x/2+α, was confirmed to be 6.33± 0.04, for x{=}0.30, by hydrogen reduction thermogravimetry.

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

    PubMed

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

    2013-03-21

    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.

  4. Structure determination of the crystalline phase of n-butanol by powder X-ray diffraction and study of intermolecular associations by Raman spectroscopy.

    PubMed

    Derollez, Patrick; Hédoux, Alain; Guinet, Yannick; Danède, Florence; Paccou, Laurent

    2013-04-01

    X-ray powder diffraction patterns of n-butanol at 110 K and the isothermal transformation above the glass transition temperature of the supercooled liquid into the glacial state were recorded with a laboratory diffractometer. The starting structural model of the crystalline stable phase was found by a Monte-Carlo simulated annealing method. The final structure was obtained through Rietveld refinements with soft restraints on the interatomic bond lengths and angles. The cell is triclinic with space group P1 and contains two molecules. The width of the Bragg peaks is interpreted by a phenomenological microstructural approach in terms of anisotropic strain effects. The study of the hydrogen bonds by Raman spectroscopy shows the existence of two main kinds of hydrogen bonds in the crystal, in agreement with the structure obtained by diffraction. The glacial state resulting from an abortive crystallization is composed of microcrystallites of the stable phase coexisting with non-transformed supercooled liquid. Crystalline features of the glacial state were determined as closely connected to the microstructural description of the crystal, leading to information about the origin of the glacial state.

  5. 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.

  6. 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.

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

    DOE PAGES

    Caliandro, Rocco; Sibillano, Teresa; Belviso, B. Danilo; ...

    2016-02-02

    In this study, 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 deviationsmore » 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. Finally, the time behavior of such structural change is identified on the basis of multivariate analysis.« less

  8. Crystal structure of carnidazole form II from synchrotron X-ray powder diffraction: structural comparison with form I, the hydrated form and the low energy conformations in vacuo.

    PubMed

    de Armas, Héctor Novoa; Peeters, Oswald M; Blaton, Norbert; Van den Mooter, Guy; De Ridder, Dirk J A; Schenk, Henk

    2006-10-01

    The crystal structure of carnidazole form II, O-methyl [2-(2-methyl-5-nitro-1H-imidazole-1-yl)ethyl]thiocarbamate, has been determined using synchrotron X-ray powder diffraction in combination with simulated annealing and whole profile pattern matching, and refined by the Rietveld method. For structure solution, 12 degrees of freedom were defined: one motion group and six torsions. Form II crystallizes in space group P2(1)/n, Z=4, with unit cell parameters after Rietveld refinement: a=13.915(4), b=8.095(2), c=10.649(3) A, beta=110.83(1) degrees, and V=1121.1(5) A3. The two polymorphic forms, as well as the hydrate, crystallize in the monoclinic space group P2(1)/n having four molecules in the cell. In form II, the molecules are held together by forming two infinite zig-zag chains via hydrogen bonds of the type N--H...N, the same pattern as in form I. A conformational study of carnidazole, at semiempirical PM3 level, was performed using stochastic approaches based on modification of the flexible torsion angles. The values of the torsion angles for the molecules of the two polymorphic forms and the hydrate of carnidazole are compared to those obtained from the conformational search. Form I and form II are enantiotropic polymorphic pairs this agrees with the fact that the two forms are conformational polymorphs.

  9. Synthesis, spectroscopic characterization, X-ray powder structure analysis, DFT study and in vitro anticancer activity of N-(2-methoxyphenyl)-3-methoxysalicylaldimine

    NASA Astrophysics Data System (ADS)

    Chattopadhyay, Basab; Basu, Soumya; Chakraborty, Paramita; Choudhuri, Soumitra Kumar; Mukherjee, Alok K.; Mukherjee, Monika

    2009-08-01

    Schiff base, N-(2-methoxyphenyl)-3-methoxysalicylaldimine (MPMS), was synthesized and characterized by spectroscopic methods. Crystal structure of the title compound crystallizing in the orthorhombic space group P ca2 1, a = 23.695(2), b = 7.7011(8), c = 7.3570(9) Å, V = 1342.5(2) Å 3, Z = 4 has been solved from X-ray powder diffraction data following direct-space approach and refined by the Rietveld method. In solid state, the salicylaldimine compound exists as a phenol-imine tautomer with a strong intramolecular O-H…N hydrogen bond. The molecular geometry and electronic structure of MPMS were calculated at the DFT level using the hybrid exchange-correlation functional, BLYP. The optimized molecular geometry corresponds to the non-planar conformation of the molecule as established by the crystallographic analysis. The anticancer activity of the title Schiff base was evaluated against three different cell lines, SF-268, MCF-7 and NCI-H460.

  10. The use of in situ powder X-ray diffraction in the investigation of dolomite as a potential reversible high-temperature CO2 sorbent.

    PubMed

    Readman, Jennifer E; Blom, Richard

    2005-03-21

    We report the use of gas sorption experiments and in situ powder X-ray diffraction to study the use of dolomite (MgCa(CO3)2) as a potential reversible high-temperature CO2 sorbent. When dolomite is treated in inert atmosphere at 900 degrees C it decomposes into separate CaO and MgO rich phases and dolomite is never reformed pon CO2 sorption. Gas sorption studies show that the calcined dolomite can go through several cycles of CO2 sorption/desorption in a reversible manner, however, the sorption capacity diminishes with each cycle. Only calcium seems to be involved in the CO2 sorption, while MgO acts as a carrier for the calcium phase. Some evidence of magnesium contamination of the calcium phase was found. BET and SEM measurements were carried out to find differences in the surface area/particle morphology that may explain similarities in the sorption capacities of dolomite and calcite (CaCO3).

  11. 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.

  12. Adsorption onto fluidized powdered activated carbon flocs-pACF.

    PubMed

    Serpa, Ana Lídia; Schneider, Ivo André H; Rubio, Jorge

    2005-02-01

    This work presents a new adsorption technique where the adsorbent (powdered activated carbon-PAC) is in the form of suspended flocs formed with water-soluble polymer flocculants. Thus, the adsorption of a typical dye, methylene blue (MB), was studied onto polyacrylamide flocs of PAC (PACF) in a fluidized bed reactor. The technique is based on the fact that the adsorption capacity of PAC does not decrease after flocculation because the adsorbed polymer occupies only a few surface sites, in the form of trains, loops, and tails. Moreover, the adsorption was found to proceed through a rapid mass transfer of MB to the adsorbing PAC flocs, in the same extent as onto PAC. Because of the rapid settling characteristics of the aggregates formed, the two phase separations, loaded PAC and solution, become easier. Thus, the technique offers the advantages of conducting simultaneously both adsorption and solid/liquid separation all in one single stage. Results obtained showed that high MB removal values can be attained in a fluidized bed reactor (>90%) and that PACF presents a much higher adsorption capacity (breakthrough points) than granulated activated carbon (GAC) in the same adsorbing bed. It is believed that this technique highly broadens the potential of the use of powdered activated carbon or other similar ultrafine adsorbents.

  13. 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.

  14. Low-temperature high magnetic field powder x-ray diffraction setup for field-induced structural phase transition studies from 2 to 300 K and at 0 to 8-T field.

    PubMed

    Shahee, Aga; Sharma, Shivani; Kumar, Dhirendra; Yadav, Poonam; Bhardwaj, Preeti; Ghodke, Nandkishor; Singh, Kiran; Lalla, N P; Chaddah, P

    2016-10-01

    A low-temperature and high magnetic field powder x-ray diffractometer (XRD) has been developed at UGC-DAE CSR (UGC: University Grant Commission, DAE: Department of Atomic Energy, and CSR: Consortium for scientific research), Indore, India. The setup has been developed around an 18 kW rotating anode x-ray source delivering Cu-Kα x-rays coming from a vertical line source. It works in a symmetric θ-2θ parallel beam geometry. It consists of a liquid helium cryostat with an 8 T split-pair Nb-Ti superconducting magnet comprising two x-ray windows each covering an angular range of 65°. This is mounted on a non-magnetic type heavy duty goniometer equipped with all necessary motions along with data collection accessories. The incident x-ray beam has been made parallel using a parabolic multilayer mirror. The scattered x-ray is detected using a NaI detector through a 0.1° acceptance solar collimator. To control the motions of the goniometer, a computer programme has been developed. The wide-angle scattering data can be collected in a range of 2°-115° of 2θ with a resolution of ∼0.1°. The whole setup is tightly shielded for the scattered x-rays using a lead hutch. The functioning of the goniometer and the artifacts arising possibly due to the effect of stray magnetic field on the goniometer motions, on the x-ray source, and on the detector have been characterized by collecting powder XRD data of a National Institute of Standards and Technology certified standard reference material LaB6 (SRM-660b) and Si powder in zero-field and in-field conditions. Occurrence of field induced structural-phase transitions has been demonstrated on various samples like Pr0.5Sr0.5MnO3, Nd0.49Sr0.51MnO3-δ and La0.175Pr0.45Ca0.375MnO3 by collecting data in zero field cool and field cool conditions.

  15. Low-temperature high magnetic field powder x-ray diffraction setup for field-induced structural phase transition studies from 2 to 300 K and at 0 to 8-T field

    NASA Astrophysics Data System (ADS)

    Shahee, Aga; Sharma, Shivani; Kumar, Dhirendra; Yadav, Poonam; Bhardwaj, Preeti; Ghodke, Nandkishor; Singh, Kiran; Lalla, N. P.; Chaddah, P.

    2016-10-01

    A low-temperature and high magnetic field powder x-ray diffractometer (XRD) has been developed at UGC-DAE CSR (UGC: University Grant Commission, DAE: Department of Atomic Energy, and CSR: Consortium for scientific research), Indore, India. The setup has been developed around an 18 kW rotating anode x-ray source delivering Cu-Kα x-rays coming from a vertical line source. It works in a symmetric θ-2θ parallel beam geometry. It consists of a liquid helium cryostat with an 8 T split-pair Nb-Ti superconducting magnet comprising two x-ray windows each covering an angular range of 65°. This is mounted on a non-magnetic type heavy duty goniometer equipped with all necessary motions along with data collection accessories. The incident x-ray beam has been made parallel using a parabolic multilayer mirror. The scattered x-ray is detected using a NaI detector through a 0.1° acceptance solar collimator. To control the motions of the goniometer, a computer programme has been developed. The wide-angle scattering data can be collected in a range of 2°-115° of 2θ with a resolution of ˜0.1°. The whole setup is tightly shielded for the scattered x-rays using a lead hutch. The functioning of the goniometer and the artifacts arising possibly due to the effect of stray magnetic field on the goniometer motions, on the x-ray source, and on the detector have been characterized by collecting powder XRD data of a National Institute of Standards and Technology certified standard reference material LaB6 (SRM-660b) and Si powder in zero-field and in-field conditions. Occurrence of field induced structural-phase transitions has been demonstrated on various samples like Pr0.5Sr0.5MnO3, Nd0.49Sr0.51MnO3-δ and La0.175Pr0.45Ca0.375MnO3 by collecting data in zero field cool and field cool conditions.

  16. 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.

  17. 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

  18. An X-ray photoelectron spectroscopy study of BF3 adsorption on positively and negatively poled LiNbO3 (0001)

    NASA Astrophysics Data System (ADS)

    Herdiech, M. W.; Mönig, H.; Altman, E. I.

    2014-08-01

    Adsorption of the strong Lewis acid BF3 was investigated to probe the sensitivity of the Lewis basicity of surface oxygens on LiNbO3 (0001) to the ferroelectric polarization direction. Adsorption and desorption were characterized by using X-ray photoelectron spectroscopy (XPS) to monitor the intensity and binding energy of the F 1s core level as a function of BF3 exposure and temperature. The results indicate that both BF3 uptake and desorption are very similar on the positively and negatively poled surfaces. In particular, BF3 only weakly adsorbs with the majority of the adsorbed BF3 desorbing below 200 K. Despite the similarities in the uptake and desorption behavior, the binding energy of the F 1s peak relative to the substrate Nb 3d5/2 peak was sensitive to the polarization direction, with the F 1s peak occurring at a binding energy up to 0.3 eV lower on positively poled than negatively poled LiNbO3 for equivalent BF3 exposures. Rather than reflecting a difference in bonding to the surface, however, this shift could be associated with oppositely oriented dipoles at the positively and negatively poled surfaces creating opposite band offsets between the adsorbate and the substrate. A similar effect was observed with lead zirconate titanate thin films where the Pb 4f XPS peak position changes as a function of temperature as a result of the pyroelectric effect which changes the magnitude of the surface and interface dipoles.

  19. 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)

  20. 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 ...

  1. Bone x-ray

    MedlinePlus

    ... not being scanned. Alternative Names X-ray - bone Images Skeleton Skeletal spine Osteogenic sarcoma - x-ray References ... urac.org). URAC's accreditation program is an independent audit to verify that A.D.A.M. follows ...

  2. X-ray

    MedlinePlus

    ... think you might be pregnant. Alternative Names Radiography Images X-ray X-ray References Geleijns J, Tack ... urac.org). URAC's accreditation program is an independent audit to verify that A.D.A.M. follows ...

  3. Extremity x-ray

    MedlinePlus

    ... sensitive to the risks of an x-ray. Images X-ray References Kelly DM. Congenital anomalies of ... urac.org). URAC's accreditation program is an independent audit to verify that A.D.A.M. follows ...

  4. X-Ray Toolkit

    SciTech Connect

    2015-10-20

    Radiographic Image Acquisition & Processing Software for Security Markets. Used in operation of commercial x-ray scanners and manipulation of x-ray images for emergency responders including State, Local, Federal, and US Military bomb technicians and analysts.

  5. KYHP 3O 10: Rietveld refinement using X-ray powder diffraction data and Raman study of the conductivity phase transition

    NASA Astrophysics Data System (ADS)

    Zouari, N.; Hadrich, A.; Mhiri, T.; Daoud, A.; Gravereau, P.

    2002-02-01

    Potassium yttrium hydrogen triphosphate (KYHP 3O 10) crystallises in the triclinic system P1¯ at room temperature with the following parameters: a=6.8522(2), b=7.6254(2), c=8.5351(2) Å, α=106.658(1), β=106.435(2) and γ=82.344(2)°; Z=2. This structure has been refined from X-ray powder diffraction data using the Rietveld method, with the isostructural compounds KSmHP 3O 10 and NH 4BiHP 3O 10 as the starting model. Refinement of 70 parameters by the Rietveld method, using 2447 reflections, led to cRwp=0.138, cRp=0.104 and RB=0.041. This compound is a chain-based structure. The K + and Y 3+ cations are intercalated between chains, formed of (HP 3O 104-) groups linked by OH⋯O hydrogen bonding along the c-axis. The yttrium atoms are in an eight-fold coordination and also build infinite chains of edge-sharing YO 8 polyhedra running parallel to the a-axis. The potassium cations are coordinated by 10 oxygen atoms and build chains of KO 10 polyhedra running parallel to the b-axis. A calorimetric study of the title compound shows one endothermal peak, which is detected at 519 K. Samples were examined by impedance and Raman spectroscopy techniques. The Raman spectra of KYHP 3O 10, recorded at different temperatures in the frequency range 50-1250 cm -1 show the presence of a transition, which is characterised by an unusual high conductivity caused by breaking of the hydrogen bridges and suggests a great dynamic disorder of protons. This permits H + ions at high temperature to contribute with the potassium cations to the ionic conductivity of the product.

  6. 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}.

  7. Crystal fingerprinting: elucidating the crystals of Cheddar, Parmigiano-Reggiano, Gouda, and soft washed-rind cheeses using powder x-ray diffractometry.

    PubMed

    Tansman, G F; Kindstedt, P S; Hughes, J M

    Crystals in cheese may be considered defects or positive features, depending on the variety and mode of production (industrial, artisanal). Powder x-ray diffractometry (PXRD) offers a simple means to identify and resolve complex combinations of crystals that contribute to cheese characteristics. The objective of the present research was to demonstrate the application of PXRD to study crystals from a range of different cheese types, specifically Cheddar, Parmigiano-Reggiano, Gouda, and soft washed-rind (smear ripened) cheeses. In studies of Parmigiano-Reggiano and long-aged Gouda, PXRD has confirmed that hard (crunchy) crystals that form abundantly within these cheeses consist of tyrosine. Furthermore, PXRD has tentatively identified the presence of an unusual form of crystalline leucine in large (up to 6 mm in diameter) spherical entities, or "pearls", that occur abundantly in 2-year-old Parmigiano Reggiano and long-aged Gouda cheeses, and on the surface of rindless hard Italian-type cheese. Ongoing investigations into the nature of these "pearls" are providing new insight into the roles that crystals play in the visual appearance and texture of long-aged cheeses. Crystals also sometimes develop profusely in the eyes of long-aged Gouda, which have been shown by PXRD to consist of tyrosine and the aforementioned presumptive form of crystalline leucine. Finally, crystals have been shown by PXRD to form in the smears of soft washed-rind cheeses. These crystals may be associated in some cheeses with gritty mouth feel and with zonal body softening that occurs during ripening. Heightened interest in artisanal cheeses highlights the need to better understand crystals and their contributions to cheese characteristics.

  8. 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- ...

  9. 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 ...

  10. 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

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. X-Ray

    MedlinePlus

    ... of gray. For some types of X-ray tests, a contrast medium — such as iodine or barium — is introduced into your body to provide greater detail on the images. X-ray technology is used to examine many parts of the ...

  17. Chest X-Ray

    MedlinePlus Videos and Cool Tools

    ... Site Index A-Z Spotlight Recently posted: Anal Cancer Facet Joint Block Video: Lung Cancer Screening Video: Upper GI Tract X-ray Video: ... of lung conditions such as pneumonia, emphysema and cancer. A chest x-ray requires no special preparation. ...

  18. 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…

  19. 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.

  20. Dental x-rays

    MedlinePlus

    ... X-rays are a form of high energy electromagnetic radiation. The x-rays penetrate the body to form ... for detecting cavities, unless the decay is very advanced and deep. Many ... The amount of radiation given off during the procedure is less than ...

  1. 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.

  2. 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.

  3. Molecular and crystalline structure of cycloheptanespiro-3'(4'H)-6',7',8',9'-tetrahydrocyclohexa[b][1,4]thiazole-2'(5'H)-thione from powder synchrotron X-ray diffraction data.

    PubMed

    Avila, Edward E; Mora, Asiloé J; Delgado, Gerzon E; Contreras, Ricardo R; Fitch, Andrew N; Brunelli, Michela

    2008-04-01

    A series of bidentate nitrogen-sulfur pro-ligands has been designed and synthesized with the purpose of introducing a structural modification that favours the tetrahedral site distortions of metalloprotein systems with metallic centers surrounded by ligands containing two N atoms and two S atoms as donor groups. Some of these new pro-ligands were obtained only as powders. Here we present the molecular and crystalline structure of cycloheptanespiro-3'(4'H)-6',7',8',9'-tetrahydrocyclohexa[b][1,4]thiazole-2'(5'H)-thione (I) solved and refined from powder synchrotron X-ray diffraction data. Two independent molecules comprising a total of 36 non-H atoms were obtained from the direct-methods solution and refined against the powder X-ray diffraction data using the Rietveld method. The molecular conformations of the heterocyclic benzothiazine ring, the fused heptenyl ring and the heptanyl spiro ring are thoroughly discussed and compared with VASP theoretical calculations and other related structures. The packing of molecules in (I) is based on hydrogen bonds of the type N-H...S and hydrophobic C-H interactions.

  4. 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.

  5. 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)

  6. 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.

  7. 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

  8. 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.

  9. 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.

  10. X-ray superbubbles

    NASA Technical Reports Server (NTRS)

    Cash, W.

    1983-01-01

    Four regions of the galaxy, the Cygnus Superbubble, the Eta Carina complex, the Orion/Eridanus complex, and the Gum Nebula, are discussed as examples of collective effects in the interstellar medium. All four regions share certain features, indicating a common structure. The selection effects which determine the observable X-ray properties of the superbubbles are discussed, and it is demonstrated that only a very few more in our Galaxy can be detected in X rays. X-ray observation of extragalactic superbubbles is shown to be possible but requires the capabilities of a large, high quality, AXAF class observatory.

  11. 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 ...

  12. 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 ...

  13. X-ray - skeleton

    MedlinePlus

    ... medlineplus.gov/ency/article/003381.htm X-ray - skeleton To use the sharing features on this page, ... ray views may be uncomfortable. If the whole skeleton is being imaged, the test usually takes 1 ...

  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. X-ray Binaries

    NASA Astrophysics Data System (ADS)

    Lewin, Walter H. G.; van Paradijs, Jan; van den Heuvel, Edward Peter Jacobus

    1997-01-01

    Preface; 1. The properties of X-ray binaries, N. E. White, F. Nagase and A. N. Parmar; 2. Optical and ultraviolet observations of X-ray binaries J. van Paradijs and J. E. McClintock; 3. Black-hole binaries Y. Tanaka and W. H. G. Lewin; 4. X-ray bursts Walter H. G. Lewin, Jan Van Paradijs and Ronald E. Taam; 5. Millisecond pulsars D. Bhattacharya; 6. Rapid aperiodic variability in binaries M. van der Klis; 7. Radio properties of X-ray binaries R. M. Hjellming and X. Han; 8. Cataclysmic variable stars France Anne-Dominic Córdova; 9. Normal galaxies and their X-ray binary populations G. Fabbiano; 10. Accretion in close binaries Andrew King; 11. Formation and evolution of neutron stars and black holes in binaries F. Verbunt and E. P. J. van den Heuvel; 12. The magnetic fields of neutron stars and their evolution D. Bhattacharya and G. Srinivasan; 13. Cosmic gamma-ray bursts K. Hurley; 14. A catalogue of X-ray binaries Jan van Paradijs; 15. A compilation of cataclysmic binaries with known or suspected orbital periods Hans Ritter and Ulrich Kolb; References; Index.

  16. Application of maximum entropy method for the study of electron density distribution in SrS, BaS and PuS using powder X-ray data

    NASA Astrophysics Data System (ADS)

    Saravanan, R.

    2006-06-01

    A study of the electronic structure of the three sulphides, SrS, BaS and PuS has been carried out in this work, using the powder X-ray intensity data from JCPDS powder diffraction data base. The statistical approach, MEM (maximum entropy method) is used for the analysis of the data for the electron density distribution in these materials and an attempt has been made to understand the bonding between the metal atom and the sulphur atom. The mid-bond electron density is found to be maximum for PuS among these three sulphides, being 0.584 e/Å^3 at 2.397 Å. SrS is found to have the lowest electron density at the mid-bond (0.003 e/Å^3) at 2.118 Å from the origin leaving it more ionic than the other two sulphides studied in this work. The two-dimensional electron density maps on (1 0 0) and (1 1 0) planes and the one-dimensional profiles along the bonding direction [1 1 1] are used for these analyses. The overall and individual Debye-Waller factors of atoms in these systems have also been studied and analyzed. The refinements of the observed X-ray data were carried out using standard softwares and also a routine written by the author.

  17. 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.

  18. 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.

  19. 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.; Ould-Chikh, 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.

  20. Structural studies of a non-stoichiometric channel hydrate using high resolution X-ray powder diffraction, solid-state nuclear magnetic resonance, and moisture sorption methods.

    PubMed

    Kiang, Y-H; Cheung, Eugene; Stephens, Peter W; Nagapudi, Karthik

    2014-09-01

    Structural investigations of a nonstoichiometric hydrate, AMG 222 tosylate, a DPP-IV inhibitor in clinical development for type II diabetes, were performed using a multitechnique approach. The moisture sorption isotherm is in good agreement with a simple Langmuir model, suggesting that the hydrate water is located in well-defined crystallographic sites, which become vacant during dehydration. Crystal structures of AMG 222 tosylate at ambient and dry conditions were determined from high-resolution X-ray diffraction using the direct space method. On the basis of these crystal structures, hydrated water is located in channels formed by the drug framework. Upon dehydration, an isostructural dehydrate is formed with the channels remaining void and accessible to water for rehydration. Kitaigorodskii packing coefficients of the solid between relative humidity of 0% and 90% indicate that the equilibrium form of AMG 222 tosylate is the fully hydrated monohydrate.

  1. Clocking femtosecond X rays.

    PubMed

    Cavalieri, A L; Fritz, D M; Lee, S H; Bucksbaum, P H; Reis, D A; Rudati, J; Mills, D M; Fuoss, P H; Stephenson, G B; Kao, C C; Siddons, D P; Lowney, D P; Macphee, A G; Weinstein, D; Falcone, R W; Pahl, R; Als-Nielsen, J; Blome, C; Düsterer, S; Ischebeck, R; Schlarb, H; Schulte-Schrepping, H; Tschentscher, Th; Schneider, J; Hignette, O; Sette, F; Sokolowski-Tinten, K; Chapman, H N; Lee, R W; Hansen, T N; Synnergren, O; Larsson, J; Techert, S; Sheppard, J; Wark, J S; Bergh, M; Caleman, C; Huldt, G; van der Spoel, D; Timneanu, N; Hajdu, J; Akre, R A; Bong, E; Emma, P; Krejcik, P; Arthur, J; Brennan, S; Gaffney, K J; Lindenberg, A M; Luening, K; Hastings, J B

    2005-03-25

    Linear-accelerator-based sources will revolutionize ultrafast x-ray science due to their unprecedented brightness and short pulse duration. However, time-resolved studies at the resolution of the x-ray pulse duration are hampered by the inability to precisely synchronize an external laser to the accelerator. At the Sub-Picosecond Pulse Source at the Stanford Linear-Accelerator Center we solved this problem by measuring the arrival time of each high energy electron bunch with electro-optic sampling. This measurement indirectly determined the arrival time of each x-ray pulse relative to an external pump laser pulse with a time resolution of better than 60 fs rms.

  2. X-ray fluorescence experiment

    NASA Technical Reports Server (NTRS)

    Adler, I.; Trombka, J. I.; Gerard, J.; Schmadebeck, R.; Lowman, P.; Blodgett, H.; Yin, L.; Eller, E.; Lamothe, R.; Gorenstein, P.

    1972-01-01

    The preliminary results from the Sco X-1 and Cyg X-1 obtained from the Apollo 15 X-ray detector data are presented along with preliminary results of the X-ray fluorescence spectrometric data of the lunar surface composition. The production of the characteristic X-rays following the interaction of solar X-rays with the lunar surface is described along with the X-ray spectrometer. Preliminary analyses of the astronomical X-ray observation and the X-ray fluorescence data are presented.

  3. Development of heavy mineral and heavy element database of soil sediments in Japan using synchrotron radiation X-ray powder diffraction and high-energy (116 keV) X-ray fluorescence analysis: 1. Case study of Kofu and Chiba region.

    PubMed

    Bong, Willy Shun Kai; Nakai, Izumi; Furuya, Shunsuke; Suzuki, Hiroko; Abe, Yoshinari; Osaka, Keiichi; Matsumoto, Takuya; Itou, Masayoshi; Imai, Noboru; Ninomiya, Toshio

    2012-07-10

    We have started the construction of a nationwide forensic soil sediment database for Japan based on the heavy mineral and trace heavy element compositions of stream sediments collected at 3024 points all over Japan obtained by high-resolution synchrotron X-ray powder diffraction (SR-XRD) and high-energy synchrotron X-ray fluorescence analysis (HE-SR-XRF). In this study, the performance of both techniques was demonstrated by analyzing soil sediments from two different geological regions, the Kofu and Chiba regions in Kanto province, to construct database that can be applied in the future to provenance analysis of soil evidence from a crime scene. The sediments from the quaternary volcanic lithology of the Chiba region were found to be dominated by heavy minerals of volcanic origin - orthopyroxene, clinopyroxene, and amphibole, and the REEs (rare earth elements) within the region showed similar geochemical behavior. On the other hand, four distinct heavy mineral groups were identified in the sediments of the Kofu region, where there is a great variety of underlying bedrock, and the geochemical behavior of the REEs in the sediments also varied accordingly to their geological origins. As such, our study shows that high-resolution SR-XRD data can provide information on the spatial distribution patterns of heavy minerals in stream sediments, playing an important role in determining their likely geographical origin. Meanwhile, the highly sensitive HE-SR-XRF data allow us to study the geochemical behavior of trace heavy elements, especially the REEs in the sediments, providing additional support to further constrain the likely geographical origin of the sediments determined by heavy minerals.

  4. 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.

  5. Neck x-ray

    MedlinePlus

    ... look at cervical vertebrae. These are the 7 bones of the spine in the neck. ... A neck x-ray can detect: Bone joint that is out of position (dislocation) Breathing in a foreign object Broken bone (fracture) Disk problems (disks ...

  6. Abdominal x-ray

    MedlinePlus

    ... a kidney stone Identify blockage in the intestine Locate an object that has been swallowed Help diagnose diseases, such as tumors or other conditions Normal Results The x-ray will show normal structures for a person your age. What Abnormal Results Mean Abnormal findings ...

  7. 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.

  8. High-pressure Powder X-ray Diffraction Study of Cu5Si and Pressure-driven Isostructural Phase Transition

    SciTech Connect

    Li, C.; Yu, Z.; Liu, H.; Lu, T.

    2012-12-03

    The structural behaviour of Cu5Si under high-pressure (HP) has been studied by angular dispersive X-ray diffraction up to 49.9 GPa. The experimental results suggest that a pressure-induced isostructural phase transition occurs around 13.5 GPa as revealed by a discontinuity in volume as a function of pressure. The lattice parameter decreases with the pressure increasing for both low-pressure (LP) and HP phases of Cu5Si. However, a plot of the lattice parameter vs. pressure shows the existence of a plateau between 11.7 and 15.3 GPa. The bulk moduli, derived from the fitting of Birch–Murnaghan equation of state, are 150(2) GPa and 210(3) GPa for the LP phase and the HP phase of Cu5Si, respectively. A change in the electronic state of the copper is assumed to govern the observed structural phase transition.

  9. 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.

  10. X-Ray Vision

    NASA Technical Reports Server (NTRS)

    Ramsey, B. D.; Elsner, R. F.; Engelhaupt, D.; Kolodziejczak, J. J.; ODell, S. L.; Speegle, C. O.; Weisskopf, M. C.

    2004-01-01

    We are fabricating optics for the hard-x-ray region using electroless nickel replication. The attraction of this process, which has been widely used elsewhere, is that the resulting full shell optics are inherently stable and thus can have very good angular resolution. The challenge with this process is to develop lightweight optics (nickel has a relatively high density of 8.9 g/cu cm), and to keep down the costs of mandrel fabrication. We accomplished the former through the development of high-strength nickel alloys that permit very thin shells without fabrication- and handling-induced deformations. For the latter, we have utilized inexpensive grinding and diamond turning to figure the mandrels and then purpose-built polishing machines to finish the surface. In-house plating tanks and a simple water-bath separation system complete the process. To date we have built shells ranging in size from 5 cm diameter to 50 cm, and with thickness down to 100 micron. For our HERO balloon program, we are fabricating over 200 iridium-coated shells, 250 microns thick, for hard-x-ray imaging up to 75 keV. Early test results on these have indicated half-power-diameters of 15 arcsec. The status of these and other hard-x-ray optics will be reviewed.

  11. 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.

  12. X-ray lithography masking

    NASA Technical Reports Server (NTRS)

    Smith, Henry I. (Inventor); Lim, Michael (Inventor); Carter, James (Inventor); Schattenburg, Mark (Inventor)

    1998-01-01

    X-ray masking apparatus includes a frame having a supporting rim surrounding an x-ray transparent region, a thin membrane of hard inorganic x-ray transparent material attached at its periphery to the supporting rim covering the x-ray transparent region and a layer of x-ray opaque material on the thin membrane inside the x-ray transparent region arranged in a pattern to selectively transmit x-ray energy entering the x-ray transparent region through the membrane to a predetermined image plane separated from the layer by the thin membrane. A method of making the masking apparatus includes depositing back and front layers of hard inorganic x-ray transparent material on front and back surfaces of a substrate, depositing back and front layers of reinforcing material on the back and front layers, respectively, of the hard inorganic x-ray transparent material, removing the material including at least a portion of the substrate and the back layers of an inside region adjacent to the front layer of hard inorganic x-ray transparent material, removing a portion of the front layer of reinforcing material opposite the inside region to expose the surface of the front layer of hard inorganic x-ray transparent material separated from the inside region by the latter front layer, and depositing a layer of x-ray opaque material on the surface of the latter front layer adjacent to the inside region.

  13. Panoramic Dental X-Ray

    MedlinePlus

    ... Physician Resources Professions Site Index A-Z Panoramic Dental X-ray Panoramic dental x-ray uses a ... Your e-mail address: Personal message (optional): Bees: Wax: Notice: RadiologyInfo respects your privacy. Information entered here ...

  14. 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

  15. Abdomen X-Ray (Radiography)

    MedlinePlus

    ... examined, an x-ray machine produces a small burst of radiation that passes through the body, recording ... tissue shows up in shades of gray and air appears black. Until recently, x-ray images were ...

  16. Dual X-ray absorptiometry

    NASA Astrophysics Data System (ADS)

    Altman, Albert; Aaron, Ronald

    2012-07-01

    Dual X-ray absorptiometry is widely used in analyzing body composition and imaging. Both the method and its limitations are related to the Compton and photoelectric contributions to the X-ray attenuation coefficients of materials.

  17. Encapsulating X-Ray Detectors

    NASA Technical Reports Server (NTRS)

    Conley, Joseph M.; Bradley, James G.

    1987-01-01

    Vapor-deposited polymer shields crystals from environment while allowing X rays to pass. Polymer coating transparental to X rays applied to mercuric iodide detector in partial vacuum. Coating protects crystal from sublimation, chemical attack, and electrical degradation.

  18. 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.

  19. Neutron and X-Ray Reflectivity Studies of the Adsorption of Aerosol-OT at the Air-Water Interface: The Structure of the Calcium Salt

    PubMed

    Li; Lee; Thomas; Penfold

    1997-03-15

    We have used neutron and X-ray reflection to determine the structure of a layer of calcium bis-(2-ethyl 1-hexyl) sulphosuccinate (Aerosol-OT or AOT) adsorbed at the air/solution interface. The widths of the distributions of the chains and head groups of the molecule, and their positions in relation to the underlying water, have been measured at four concentrations varying from the solubility limit (CMC) at 4 x 10(-4) M to 1 x 10(-6) M. Over this concentration range the coverage changes from 68 ± 3 to 142 ± 8 Å2 per AOT unit. The structure of the layer both is quite different from that of NaAOT and varies quite differently with surface concentration. The Ca(AOT)2 layer is slightly (1 Å) further out from the water, but the chain region is thinner for the calcium surfactant. This is reflected most in the greatly reduced chain to head separation, which drops from about 6 Å in NaAOT to about 4 Å in Ca(AOT)2.

  20. X-Ray Exam: Hip

    MedlinePlus

    ... Old Feeding Your 1- to 2-Year-Old X-Ray Exam: Hip KidsHealth > For Parents > X-Ray Exam: Hip A A A What's in this ... español Radiografía: cadera What It Is A hip X-ray is a safe and painless test that uses ...

  1. X-Ray Exam: Wrist

    MedlinePlus

    ... Old Feeding Your 1- to 2-Year-Old X-Ray Exam: Wrist KidsHealth > For Parents > X-Ray Exam: Wrist A A A What's in this ... español Radiografía: muñeca What It Is A wrist X-ray is a safe and painless test that uses ...

  2. X-Ray Exam: Ankle

    MedlinePlus

    ... Old Feeding Your 1- to 2-Year-Old X-Ray Exam: Ankle KidsHealth > For Parents > X-Ray Exam: Ankle A A A What's in this ... español Radiografía: tobillo What It Is An ankle X-ray is a safe and painless test that uses ...

  3. X-Ray Exam: Foot

    MedlinePlus

    ... Old Feeding Your 1- to 2-Year-Old X-Ray Exam: Foot KidsHealth > For Parents > X-Ray Exam: Foot A A A What's in this ... español Radiografía: pie What It Is A foot X-ray is a safe and painless test that uses ...

  4. X-Ray Exam: Finger

    MedlinePlus

    ... Old Feeding Your 1- to 2-Year-Old X-Ray Exam: Finger KidsHealth > For Parents > X-Ray Exam: Finger Print A A A What's in ... español Radiografía: dedo What It Is A finger X-ray is a safe and painless test that uses ...

  5. X-Ray Exam: Foot

    MedlinePlus

    ... Old Feeding Your 1- to 2-Year-Old X-Ray Exam: Foot KidsHealth > For Parents > X-Ray Exam: Foot Print A A A What's in ... español Radiografía: pie What It Is A foot X-ray is a safe and painless test that uses ...

  6. X-Ray Exam: Ankle

    MedlinePlus

    ... Old Feeding Your 1- to 2-Year-Old X-Ray Exam: Ankle KidsHealth > For Parents > X-Ray Exam: Ankle Print A A A What's in ... español Radiografía: tobillo What It Is An ankle X-ray is a safe and painless test that uses ...

  7. X-Ray Exam: Pelvis

    MedlinePlus

    ... Old Feeding Your 1- to 2-Year-Old X-Ray Exam: Pelvis KidsHealth > For Parents > X-Ray Exam: Pelvis Print A A A What's in ... español Radiografía: pelvis What It Is A pelvis X-ray is a safe and painless test that uses ...

  8. Tunable X-ray source

    DOEpatents

    Boyce, James R [Williamsburg, VA

    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.

  9. Investigation of structural and dynamic properties of NH 4[N(CN) 2] by means of X-ray and neutron powder diffraction as well as vibrational and solid-state NMR spectroscopy

    NASA Astrophysics Data System (ADS)

    Lotsch, Bettina V.; Senker, Jürgen; Kockelmann, Winfried; Schnick, Wolfgang

    2003-11-01

    The crystal structure, spectroscopic and thermal properties of ammonium dicyanamide NH 4[N(CN) 2] have been thoroughly investigated by means of temperature-dependent single-crystal X-ray and neutron powder diffraction, vibrational and MAS-NMR spectroscopy as well as thermoanalytical measurements. The comprehensive elucidation of structural details is of special interest with respect to the unique solid-state transformation of ammonium dicyanamide into dicyandiamide. This reaction occurs at temperatures >80°C and it represents the isolobal analogue of Wöhler's historic transformation of ammonium cyanate into urea. NH 4[N(CN) 2] crystallizes in the monoclinic space group P2 1/ c with lattice constants a=3.7913(8), b=12.412(2), c=9.113(2) Å, β=91.49(2)° and Z=4 (single-crystal X-ray data, T=200 K). The temperature dependence of the lattice constants shows anisotropic behavior, however, no evidence for phase transitions in the investigated temperature range was observed. The hydrogen positions could be localized by neutron diffraction (10-370 K), and the temperature-dependent behavior of the ammonium group has been analyzed by Rietveld refinements using anisotropic thermal displacement parameters. They were interpreted by utilizing a rigid body model and extracting the libration and translation matrices of the ammonium ion by applying the TLS formalism. The results obtained by the diffraction methods were confirmed and supplemented by vibrational spectroscopy and solid-state 15N and 13C MAS-NMR investigations.

  10. 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.

  11. Single-crystal and synchrotron x-ray powder diffraction study of the one-dimensial orthorhombic polymer phase of C[sub 60}.

    SciTech Connect

    Papoular, R. J.; Toby, B. H.; Davydov, V. A.; Rakhmanina, A. V.; Dzyabchenko,, A.; Allouchi,, H.; Agafonov, V.; X-Ray Science Division; Leon Brillouin Lab.; Vereshchagin Inst. of High-Presure Physics; Karpov Inst. of Physical Chemistry; Labo. de Synthese Physco-Chimique et Therapeutique; Lab. d'Electrodynamique des Materiaux Avances

    2008-07-20

    The 1D-orthorhombic polymer phase of C{sub 60} was originally mentioned in 1995. The present work provides the first direct experimental quantitative evidences of the 1D-polymer chains, clearly seen by single-crystal diffraction. Geometrical details of the [2+2]-cycloaddition rings are compared with those of C{sub 60} dimers and 2D-polymers. Another key structural parameter is the angle of rotation {Psi} of the 1D chains about the polymerization axis. Single-crystal diffraction yields {Psi} {approx} 78{sup o}, whereas accurate synchrotron powder diffraction independently produces a similar {Psi} {approx} 73{sup o}. These values are in qualitative agreement with a former theoretical prediction ({Psi} {approx} 61{sup o}).

  12. Powder X-ray investigation of 4,4′-diisocyano-3,3′-dimethyl­biphen­yl

    PubMed Central

    Rukiah, Mwaffak; Al-Ktaifani, Mahmoud

    2013-01-01

    The title compound, C16H12N2, was investigated in a powder diffraction study and its structure refined utilizing the Rietveld Method. The mol­ecule has approximate C2 symmetry. The dihedral angle between the rings is 25.6 (7)°. The crystal packing is consolidated by weak C—H⋯C N hydrogen-bond-like contacts, which lead to the formation of a three-dimensional network. Further stabilization of the crystal structure is achived by weak non-covalent π–π inter­actions between aromatic rings, with a centroid–centroid distance of 3.839 (8) Å. PMID:23476590

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. On the estimation of statistical uncertainties on powder diffraction and small-angle scattering data from two-dimensional X-ray detectors

    SciTech Connect

    Yang, X.; Juhás, P.; Billinge, S. J. L.

    2014-07-19

    Optimal methods are explored for obtaining one-dimensional powder pattern intensities from two-dimensional planar detectors with good estimates of their standard deviations. Methods are described to estimate uncertainties when the same image is measured in multiple frames as well as from a single frame. The importance of considering the correlation of diffraction points during the integration and the resampling process of data analysis is shown. It is found that correlations between adjacent pixels in the image can lead to seriously overestimated uncertainties if such correlations are neglected in the integration process. Off-diagonal entries in the variance–covariance (VC) matrix are problematic as virtually all data processing and modeling programs cannot handle the full VC matrix. It is shown that the off-diagonal terms come mainly from the pixel-splitting algorithm used as the default integration algorithm in many popular two-dimensional integration programs, as well as from rebinning and resampling steps later in the processing. When the full VC matrix can be propagated during the data reduction, it is possible to get accurate refined parameters and their uncertainties at the cost of increasing computational complexity. However, as this is not normally possible, the best approximate methods for data processing in order to estimate uncertainties on refined parameters with the greatest accuracy from just the diagonal variance terms in the VC matrix is explored.

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. Comparison of X-ray powder diffraction and solid-state nuclear magnetic resonance in estimating crystalline fraction of tacrolimus in sustained-release amorphous solid dispersion and development of discriminating dissolution method.

    PubMed

    Rahman, Ziyaur; Bykadi, Srikant; Siddiqui, Akhtar; Khan, Mansoor A

    2015-05-01

    The focus of present investigation was to explore X-ray powder diffraction (XRPD) and solid-state nuclear magnetic resonance (ssNMR) techniques for amorphous and crystalline tacrolimus quantification in the sustained-release amorphous solid dispersion (ASD), and to propose discriminating dissolution method that can detect crystalline drug. The ASD and crystalline physical mixture was mixed in various proportions to make sample matrices containing 0%-100% crystalline-amorphous tacrolimus. Partial-least-square regression and principle component regression were applied to the spectral data. Dissolution of the ASD in the US FDA recommended dissolution medium with and without surfactant was performed. R(2) > 0.99 and slope was close to one for all the models. Root-mean-square of prediction, standard error of prediction, and bias were higher in ssNMR-based models when compared with XRPD data models. Dissolution of the ASD decreased with an increase in the crystalline tacrolimus in the formulations. Furthermore, detection of crystalline tacrolimus in the ASD was progressively masked with an increase in the surfactant level in the dissolution medium. XRPD and ssNMR can be used equally to quantitate the crystalline and amorphous fraction of tacrolimus in the ASD with good accuracy; however, ssNMR data collection time is excessively long, and minimum surfactant level in the dissolution medium maximizes detection of crystalline reversion in the formulation.

  3. Powder X-ray diffraction, infrared and (13)C NMR spectroscopic studies of the homologous series of some solid-state zinc(II) and sodium(I) n-alkanoates.

    PubMed

    Nelson, Peter N; Taylor, Richard A

    2015-03-05

    A comparative study of the room temperature molecular packing and lattice structures for the homologous series of zinc(II) and sodium(I) n-alkanoates adduced from Fourier transform infrared and solid-state (13)C NMR spectroscopic data in conjunction with X-ray powder diffraction measurements is carried out. For zinc carboxylates, metal-carboxyl bonding is via asymmetric bridging bidentate coordination whilst for the sodium adducts, coordination is via asymmetric chelating bidentate bonding. All compounds are packed in a monoclinic crystal system. Furthermore, the fully extended all-trans hydrocarbon chains are arranged as lamellar bilayers. For zinc compounds, there is bilayer overlap, for long chain adducts (nc>8) but not for sodium compounds where methyl groups from opposing layers in the lamellar are only closely packed. Additionally, the hydrocarbon chains are extended along the a-axis of the unit cell for zinc compounds whilst for sodium carboxylates they are extended along the c-axis. These packing differences are responsible for different levels of Van der Waals effects in the lattices of these two series of compounds, hence, observed odd-even alternation is different. The significant difference in lattice packing observed for these two series of compounds is proposed to be due to the difference in metal-carboxyl coordination mode, arising from the different electronic structure of the central metal ions.

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. 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

    SciTech Connect

    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.; Senanayake, Sanjaya D.

    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 crystal 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.

  9. 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 PAGES

    Nguyen-Phan, Thuy-Duong; Liu, Zongyuan; Luo, Si; ...

    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

  10. 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

  11. 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

  12. 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.

  13. British X-ray astronomy

    NASA Astrophysics Data System (ADS)

    Pounds, K. A.

    1986-09-01

    The development of solar and cosmic X-ray studies in the UK, in particular the Skylark and Ariel programs, is discussed. The characteristics and capabilities of the X-ray emulsion detector developed to monitor the solar X-radiation in the Skylark program, and of the proportional counter spectrometer developed for solar X-ray measurements on the Ariel I satellite are described. The designs and functions of the pin-hole camera, the Bragg crystal spectrometer, and the X-ray spectroheliograph are exmained. The Skylark observations of cosmic X-ray sources and high-resolution solar spectra, and the Ariel 5 data on cosmic X-ray sources are presented. Consideration is given to the Ariel 6, the U.S. Einstein Observatory, Exosat, and ASTRO-C.

  14. 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.

  15. 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…

  16. X-Ray Polarization Imaging

    DTIC Science & Technology

    2006-07-01

    anatomic structures. Johns and Yaffe (2), building on the work of Alvarez and Macovski (3) and that of Lehmann et al (4), discuss a method for...sources of contrast related to both the wave and par- ticulate nature of x rays. References 1. Johns PC, Yaffe MJ. X-ray characterization of normal and...application to mammography. Med Phys 1985; 12:289–296. 3. Alvarez RE, Macovski A. Energy-selective reconstructions in x-ray computerized tomography. Phys

  17. 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.

  18. 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

  19. X-ray photonics: Bending X-rays with nanochannels

    NASA Astrophysics Data System (ADS)

    Pelliccia, Daniele

    2016-02-01

    X-ray counterparts of visible light optical elements are notoriously difficult to realize because the refractive index of all materials is close to unity. It has now been demonstrated that curved waveguides fabricated on a silicon chip can channel and deflect X-ray beams by consecutive grazing reflections.

  20. 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

  1. 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.

  2. 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.

  3. X-Ray Exam: Wrist

    MedlinePlus

    ... tissues and the ends of the forearm bones (radius and ulna) and eight small wrist bones (carpal bones). The X-ray image is black and white. Dense structures that block the passage of the X-ray beam through the body, such as the bones, appear white on the image. Softer ...

  4. 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.

  5. Dual x-ray absorptiometry

    NASA Astrophysics Data System (ADS)

    Altman, Albert; Aaron, Ronald

    2011-04-01

    Dual x-ray absorptiometry is widely used in analyzing body composition and imaging. We discuss the physics of the method and exhibit its limitations and show it is related to the Compton and photoelectric contributions to the x-ray absorption coefficients of materials.

  6. Utilization of powdered waste sludge (PWS) for removal of textile dyestuffs from wastewater by adsorption.

    PubMed

    Ozmihci, Serpil; Kargi, Fikret

    2006-11-01

    Acid pre-treated powdered waste sludge (PWS) was used for removal of textile dyestuffs from aqueous medium by adsorption as an alternative to the use of powdered activated carbon (PAC). The rate and extent of dysetuff removals were determined for four different dyestuffs at different PWS concentrations varying between 1 and 6 gl(-1). Biosorbed dyestuff concentrations at equilibrium decreased with increasing PWS concentration for all dyestuffs tested. PWS was more effective for adsorption of Remazol red RR and Chrisofonia direct yellow 12 as compared to the other dyestuffs tested. More than 80% percent dyestuff removal was obtained for all dyestuffs at PWS concentrations above 4 gl(-1) after 6h of incubation. Similar to percent dyestuff removal, the rate of adsorption was maximum at a PWS concentration of 4 gl(-1). Kinetics of adsorption of dyestuffs was investigated by using the first- and second-order kinetic models and the kinetic constants were determined. Second-order kinetics was found to fit the experimental data better than the first-order model for all dyestuffs tested. Adsorption isotherms were established for all dyestuffs used and the isotherm constants were determined by using the experimental data. Langmuir and the generalized adsorption isotherms were found to be more suitable than the Freundlich isotherm for correlation of equilibrium adsorption data. Acid pre-treated PWS was proven to be an effective adsorbent for dyestuff removal as compared to the other adsorbents reported in literature studies.

  7. Phase-targeted X-ray diffraction

    PubMed Central

    Hansford, G. M.

    2016-01-01

    A powder X-ray diffraction (XRD) method to enhance the signal of a specific crystalline phase within a mixture is presented for the first time. Specificity to the targeted phase relies on finding coincidences in the ratios of crystal d spacings and the ratios of elemental characteristic X-ray energies. Such coincidences can be exploited so that the two crystal planes diffract through the same scattering angle at two different X-ray energies. An energy-resolving detector placed at the appropriate scattering angle will detect a significantly enhanced signal at these energies if the target mineral or phase is present in the sample. When implemented using high scattering angles, for example 2θ > 150°, the method is tolerant to sample morphology and distance on the scale of ∼2 mm. The principle of the method is demonstrated experimentally using Pd Lα1 and Pd Lβ1 emission lines to enhance the diffraction signal of quartz. Both a pure quartz powder pellet and an unprepared mudstone rock specimen are used to test and develop the phase-targeted method. The technique is further demonstrated in the sensitive detection of retained austenite in steel samples using a combination of In Lβ1 and Ti Kβ emission lines. For both these examples it is also shown how the use of an attenuating foil, with an absorption edge close to and above the higher-energy characteristic X-ray line, can serve to isolate to some degree the coincidence signals from other fluorescence and diffraction peaks in the detected spectrum. The phase-targeted XRD technique is suitable for implementation using low-cost off-the-shelf components in a handheld or in-line instrument format. PMID:27738415

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. Impact of the long chain omega-acylceramides on the stratum corneum lipid nanostructure. Part 1: Thermotropic phase behaviour of CER[EOS] and CER[EOP] studied using X-ray powder diffraction and FT-Raman spectroscopy.

    PubMed

    Kessner, Doreen; Brezesinski, Gerald; Funari, Sergio S; Dobner, Bodo; Neubert, Reinhard H H

    2010-01-01

    The stratum corneum (SC), the outermost layer of the mammalian skin, is the main skin barrier. Ceramides (CERs) as the major constituent of the SC lipid matrix are of particular interest. At the moment, 11 classes of CERs are identified, but the effect of each single ceramide species is still not known. Therefore in this article, the thermotropic behaviour of the long chain omega-acylceramides CER[EOS] and CER[EOP] was studied using X-ray powder diffraction and FT-Raman spectroscopy. It was found that the omega-acylceramides CER[EOS] and CER[EOP] do not show a pronounced polymorphism which is observed for shorter chain ceramides as a significant feature. The phase behaviour of both ceramides is strongly influenced by the extremely long acyl-chain residue. The latter has a much stronger influence compared with the structure of the polar head group, which is discussed as extremely important for the appearance of a rich polymorphism. Despite the strong influence of the long chain, the additional OH-group of the phyto-sphingosine type CER[EOP] influences the lamellar repeat distance and the chain packing. The less polar sphingosine type CER[EOS] is stronger influenced by the long acyl-chain residue. Hydration is necessary for the formation of an extended hydrogen-bonding network between the polar head groups leading to the appearance of a long-periodicity phase (LPP). In contrast, the more polar CER[EOP] forms the LPP with densely packed alkyl chains already in the dry state.

  13. In-situ powder X-ray diffraction investigation of reaction pathways for the BaCO(3)-CeO(2)-In(2)O(3) and CeO(2)-In(2)O(3) systems.

    PubMed

    Bhella, Surinderjit Singh; Shafi, Shahid P; Trobec, Francesca; Bieringer, Mario; Thangadurai, Venkataraman

    2010-02-15

    We report the first in-situ powder X-ray diffraction (PXRD) study of the BaCO(3)-CeO(2)-In(2)O(3) and CeO(2)-In(2)O(3) systems in air over a wide range of temperature between 25 and 1200 degrees C. Herein, we are investigating the formation pathway and chemical stability of perovskite-type BaCe(1-x)In(x)O(3-delta) (x = 0.1, 0.2, and 0.3) and corresponding fluorite-type Ce(1-x)In(x)O(2-delta) phases. The potential direct solid state reaction between CeO(2) and In(2)O(3) for the formation of indium-doped fluorite-type phase is not observed even up to 1200 degrees C in air. The formation of the BaCe(1-x)In(x)O(3-delta) perovskite structures was investigated and rationalized using in-situ PXRD. Furthermore the decomposition of the indium-doped perovskites in CO(2) is followed using high temperature diffraction and provides insights into the reaction pathway as well as the thermal stability of the Ce(1-x)In(x)O(3-delta) system. In CO(2) flow, BaCe(1-x)In(x)O(3-delta) decomposes above T = 600 degrees C into BaCO(3) and Ce(1-x)In(x)O(2-delta). Furthermore, for the first time, the in-situ PXRD confirmed that Ce(1-x)In(x)O(2-delta) decomposes above 800 degrees C and supported the previously claimed metastability. The maximum In-doping level for CeO(2) has been determined using PXRD. The lattice constant of the fluorite-type structure Ce(1-x)In(x)O(2-delta) follows the Shannon ionic radii trend, and crystalline domain sizes were found to be dependent on indium concentration.

  14. 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.

  15. 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.

  16. X-ray monitoring optical elements

    SciTech Connect

    Stoupin, Stanislav; Shvydko, Yury; Katsoudas, John; Blank, Vladimir D.; Terentyev, Sergey A.

    2016-12-27

    An X-ray article and method for analyzing hard X-rays which have interacted with a test system. The X-ray article is operative to diffract or otherwise process X-rays from an input X-ray beam which have interacted with the test system and at the same time provide an electrical circuit adapted to collect photoelectrons emitted from an X-ray optical element of the X-ray article to analyze features of the test system.

  17. Study of the local distortions of the perovskite system La{sub 1-x}Sr{sub x}CoO{sub 3} (0 {ge} x {ge} 0.35) using the extended x-ray adsorption fine structure technique.

    SciTech Connect

    Jiang, Y.; Bridges, F.; Sundaram, N.; Belanger, D. P.; Anderson, I. E.; Mitchell, J. F.; Zheng, H.; Univ. of California at Santa Cruz

    2009-01-01

    We present a temperature-dependent extended x-ray absorption fine structure (EXAFS)/x-ray absorption near edge structure (XANES) investigation of La{sub 1-x}Sr{sub x}CoO{sub 3} (LSCO) over a wide doping concentration range (0 {le} x {le} 0.35). Five of the samples are nanoparticles (x = 0.15, 0.20, 0.25, 0.30, and 0.35) and four are bulk powders (x = 0, 0.15, 0.20, and 0.30). From the EXAFS analysis, we find that the Co-O bonds are well ordered for both bulk and nanoparticle materials and there is no clear evidence for a Jahn-Teller (JT) distortion in the LSCO system (either static or dynamic). The distortion of the Co-O bond with increasing T, parameterized by the width of the pair distribution function (PDF), {sigma} (T), can easily be modeled using a correlated Debye model with a high correlated Debye temperature {approx} 800 K. There is also no evidence for a step in plots of {sigma}{sup 2} vs T. In addition, the very small nonthermal contribution to {sigma}{sup 2} for the Co-O (PDF), {sigma}{sup 2} static, sets an upper limit on the extent of any Jahn-Teller distortion at low T. These experiments are inconsistent with the existence of a significant fraction of Co sites with an intermediate spin (IS) state, for which there is a JT active e{sub g} electron on the Co atoms. We cannot, however, exclude the possibility of a tiny fraction of sites having a JT distortion or some other (non-JT active) means of producing an IS state. The bulk samples are well ordered out to at least the third neighbors (Co-Co) while the nanoparticles show increased disorder and a reduction in coordination for Co-Co. XANES data are also presented, and, for both bulk and nanoparticle samples, there is essentially no edge shift with increasing Sr concentration. Bond-valence sums also indicate no change in effective Co valence. These results indicate that when holes are introduced via Sr doping, they have little Co(3d) character and the Co configuration remains close to 3d{sup 6}; we argue

  18. The ammonium ion in a silicate under compression: infrared spectroscopy and powder X-ray diffraction of NH4AlSi3O8—buddingtonite to 30 GPa

    NASA Astrophysics Data System (ADS)

    E. Vennari, Cara; O'Bannon, Earl F.; Williams, Quentin

    2017-02-01

    The behavior of the ammoniated feldspar buddingtonite, NH4AlSi3O8, has been studied using infrared (IR) spectroscopy up to 30 GPa and using synchrotron powder X-ray diffraction to 10 GPa at room temperature. We examine the bonding of the ammonium ion under pressure and in particular whether hydrogen bonding is enhanced by compaction, as well as probe how the ammonium ion affects the elasticity and behavior of the aluminosilicate framework at pressure. Powder diffraction data yield a bulk modulus of 49 GPa for a pressure derivative of 4, implying that the ammonium ion substitution may induce a modest softening of the feldspar lattice relative to the potassium ion. Under compression, the N-H vibrations are remarkably insensitive to pressure throughout the pressure range of these experiments. However, the vibrations of the aluminosilicate framework of buddingtonite undergo changes in their slope at 13 GPa, implying that a change in compressional mechanism occurs near this pressure, but the vibrational modes of the ammonium molecule show little response to this change. These results show that (1) there is little, if any, enhancement of hydrogen bonding between the ammonium ion and the oxygen ions of the silica and aluminum tetrahedral framework under pressure, as manifested by the slight (and mostly positive) shifts in the N-H stretching vibrations of the ammonium ion; (2) ordering of the ammonium ion is not observed under compression, as no changes in peak width or in the general appearance of the spectra are observed under compression; and (3) structural changes induced by pressure in the aluminosilicate framework do not produce significant changes in the bonding of the ammonium ion. Hence, it appears that the ammonium ion interacts minimally with its surrounding lattice, even at high pressures: Its behavior is compatible with it being, aside from Coulombic attraction to the oxygen-dominated matrix, a largely non-interactive guest molecule within the silicate

  19. Branched pore kinetic model analysis of geosmin adsorption on super-powdered activated carbon.

    PubMed

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

    2009-07-01

    Super-powdered activated carbon (S-PAC) is activated carbon of much finer particle size than powdered activated carbon (PAC). Geosmin is a naturally occurring taste and odor compound that impairs aesthetic quality in drinking water. Experiments on geosmin adsorption on S-PAC and PAC were conducted, and the results using adsorption kinetic models were analyzed. PAC pulverization, which produced the S-PAC, did not change geosmin adsorption capacity, and geosmin adsorption capacities did not differ between S-PAC and PAC. Geosmin adsorption kinetics, however, were much higher on S-PAC than on PAC. A solution to the branched pore kinetic model (BPKM) was developed, and experimental adsorption kinetic data were analyzed by BPKM and by a homogeneous surface diffusion model (HSDM). The HSDM describing the adsorption behavior of geosmin required different surface diffusivity values for S-PAC and PAC, which indicated a decrease in surface diffusivity apparently associated with activated carbon particle size. The BPKM, consisting of macropore diffusion followed by mass transfer from macropore to micropore, successfully described the batch adsorption kinetics on S-PAC and PAC with the same set of model parameter values, including surface diffusivity. The BPKM simulation clearly showed geosmin removal was improved as activated carbon particle size decreased. The simulation also implied that the rate-determining step in overall mass transfer shifted from intraparticle radial diffusion in macropores to local mass transfer from macropore to micropore. Sensitivity analysis showed that adsorptive removal of geosmin improved with decrease in activated carbon particle size down to 1microm, but further particle size reduction produced little improvement.

  20. Thorough removal of inorganic and organic mercury from aqueous solutions by adsorption on Lemna minor powder.

    PubMed

    Li, Shun-Xing; Zheng, Feng-Ying; Yang, Huang; Ni, Jian-Cong

    2011-02-15

    The adsorption ability of duckweed (Lemna minor) powders for removing inorganic and organic mercury (methyl and ethyl mercury) has been studied using cold vapour atomic absorption spectrometry. The optimal adsorption conditions were: (a) the pH value of the solution 7.0 for inorganic and ethyl mercury, 9.0 for methyl mercury, and (b) equilibrium adsorption time 10, 20, and 40 min for inorganic mercury, methyl mercury, and ethyl mercury, respectively. After adsorption by L. minor powder for 40 min, when the initial concentrations of inorganic and organic mercury were under 12.0 μg L(-1) and 50.0 μg L(-1), respectively, the residual concentrations of mercury could meet the criterion of drinking water (1.0 μg L(-1)) and the permitted discharge limit of wastewater (10.0 μg L(-1)) set by China and USEPA, respectively. Thorough removal of both inorganic and organic mercury from aqueous solutions was reported for the first time. The significant adsorption sites were C-O-P and phosphate groups by the surface electrostatic interactions with aqueous inorganic and organic mercury cations, and then the selective adsorption was resulted from the strong chelating interaction between amine groups and mercury on the surface of L. minor cells.

  1. X-Ray Imaging System

    NASA Technical Reports Server (NTRS)

    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.

  2. Characterizations of strontium(II) and barium(II) adsorption from aqueous solutions using dolomite powder.

    PubMed

    Ghaemi, Ahad; Torab-Mostaedi, Meisam; Ghannadi-Maragheh, Mohammad

    2011-06-15

    In this research, adsorption technique was applied for strontium and barium removal from aqueous solution using dolomite powder. The process has been investigated as a function of pH, contact time, temperature and adsorbate concentration. The experimental data was analyzed using equilibrium isotherm, kinetic and thermodynamic models. The isotherm data was well described by Langmuir isotherm model. The maximum adsorption capacity was found to be 1.172 and 3.958 mg/g for Sr(II) and Ba(II) from the Langmuir isotherm model at 293 K, respectively. The kinetic data was tested using first and pseudo-second order models. The results indicated that adsorption fitted well with the pseudo-second order kinetic model. The thermodynamic parameters (ΔG°, ΔH°, and ΔS°) were also determined using the equilibrium constant value obtained at different temperatures. The results showed that the adsorption for both ions was feasible and exothermic.

  3. 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.

  4. X-Ray Exam: Pelvis

    MedlinePlus

    ... KidsHealth in the Classroom What Other Parents Are Reading Your Child's Development (Birth to 3 Years) Feeding ... radiologist (a doctor who is specially trained in reading and interpreting X-ray images). The radiologist will ...

  5. X-Ray Exam: Forearm

    MedlinePlus

    ... KidsHealth in the Classroom What Other Parents Are Reading Your Child's Development (Birth to 3 Years) Feeding ... a radiologist (a doctor who's specially trained in reading and interpreting X-ray images). The radiologist will ...

  6. X-Ray Exam: Finger

    MedlinePlus

    ... KidsHealth in the Classroom What Other Parents Are Reading Your Child's Development (Birth to 3 Years) Feeding ... Results A radiologist, a doctor specially trained in reading and interpreting X-ray images, will look at ...

  7. X-Ray Exam: Forearm

    MedlinePlus

    ... amount of radiation to take a picture of a person's forearm (including the wrist, radius, ulna, and elbow). During the examination, an X-ray machine sends a beam of radiation through the arm, and an ...

  8. Bone 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 ...

  9. 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 ...

  10. 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.

  11. 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.

  12. CELESTIAL X-RAY SOURCES.

    DTIC Science & Technology

    sources, (4) the physical conditions in the pulsating x-ray source in the Crab Nebula , and (5) miscellaneous related topics. A bibliography of all work performed under the contract is given. (Author)

  13. X-ray computed tomography

    NASA Astrophysics Data System (ADS)

    1993-05-01

    The primary advantage of the X-ray computed tomography (XRCT) NDE method is that features are not superposed in the image, thereby rendering them easier to interpret than radiographic projection images. Industrial XRCT systems, unlike medical diagnostic systems, have no size and dosage constraints; they are accordingly used for systems from the scale of gas turbine blades, with hundreds-of-kV energies, to those of the scale of ICBMs, requiring MV-level X-ray energies.

  14. 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.

  15. 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.

  16. 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- ...

  17. Removal of methylene blue from aqueous solution by adsorption onto pineapple leaf powder.

    PubMed

    Weng, Chih-Huang; Lin, Yao-Tung; Tzeng, Tai-Wei

    2009-10-15

    The ability of an unconventional bio-adsorbent, pineapple leaf powder (PLP) for the adsorption of methylene blue (MB) from aqueous solution was studied. It was observed that intra-particle diffusion was involved in the adsorption process and that the kinetic data fitted well with a pseudo-second-order equation. Fitting parameters revealed that the rate of adsorption increased with decrease in dye concentration and decrease in ionic strength while the mixing speed did not have a significant effect on adsorption. The adsorption was favorable at higher pH and lower temperature, and the equilibrium data were well fitted by the Langmuir isotherm. The maximum adsorption capacity varied from 4.68 x 10(-4) to 9.28 x 10(-4)mol/g when pH increases from 3.5 to 9.5. Thermodynamic parameters suggest that the adsorption is a typical physical process, spontaneous, and exothermic in nature. The results revealed that this agricultural waste has potential to be used as an economical adsorbent for the removal of methylene blue from aqueous solution.

  18. 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.

  19. 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

  20. 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.

    PubMed

    Nelson, Peter N; Ellis, Henry A; White, Nicole A S

    2015-06-15

    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 (13)C-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

  1. 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}.

  2. Structural characterization of iron oxide/hydroxide nanoparticles in nine different parenteral drugs for the treatment of iron deficiency anaemia by electron diffraction (ED) and X-ray powder diffraction (XRPD).

    PubMed

    Fütterer, S; Andrusenko, I; Kolb, U; Hofmeister, W; Langguth, P

    2013-12-01

    Drug products containing iron oxide and hydroxide nanoparticles (INPs) are important for the treatment of iron deficiency anaemia. Pharmaceuticals prepared by the complexation of different kinds of INPs and carbohydrates have different physicochemical and biopharmaceutic characteristics. The increasing number of parenteral non-biological complex drugs (NBCD) containing iron requires physicochemical methods for characterization and enabling of cross comparisons. In this context the structure and the level of crystallinity of the iron phases may be connected to the in vitro and in vivo dissolution rates, which etiologically determine the therapeutic and toxic effects. X-ray powder diffraction (XRPD) and electron diffraction (ED) methods were used in order to investigate the nine different parenteral iron formulations Ferumoxytol (Feraheme(®)), sodium ferric gluconate sucrose (Ferrlecit(®)), iron sucrose (Venofer(®)), low molecular weight iron dextran (CosmoFer(®)), low molecular weight iron dextran (Infed(®)), high molecular weight iron dextran (Ironate(®)), high molecular weight iron dextran (Dexferrum(®)), iron carboxymaltose (Ferinject(®)) and iron isomaltoside 1000 (Monofer(®)). The iron phase in CosmoFer(®), Ferinject(®), Monofer(®), Infed(®), Ironate(®) and Dexferrum(®) was identified as Akaganéite/Akaganéite-like (β-FeOOH), with low amounts of chloride. By combining results of both methods the iron oxide in Feraheme(®) was identified as Magnetite (Fe3O4) with spinel-like structure. Ferrlecit(®) and Venofer(®) were difficult to analyze due to the low degree of crystallinity, but the iron phase seems to fit Lepidocrocite/Lepidocrocite-like (γ-FeOOH) or an amorphous kind of structure. The structural information on the type of iron oxide or hydroxide together with the particle size allows predicting the stability of the different complexes including their labile iron content. The combination of ED and XRPD methods is a very helpful approach

  3. 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}.

  4. 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.

  5. Ultraluminous X-ray Sources.

    NASA Astrophysics Data System (ADS)

    Fabrika, S.; Sholukhova, O.; Abolmasov, P.

    2008-12-01

    We discuss a new type of X-ray sources discovered in galaxies -- ultraluminous X-ray sources (ULXs). They are of two order of magnitude brighter in X-rays than the brightest Galactic black holes. Two mod- els of ULXs are discussed: "intermediate mass" black holes, 100 - 10000 solar masses, with standard accretion disks, and "stellar mass" black holes with su- percritical accretion disks like that in the Galactic object SS 433. A study of gas nebulae surrounding these objects gives us a new important information on the central sources. The observed X-ray radiation of ULXs is not enough to power their nebulae. To understand both spectra and power of the nebulae one needs a powerful UV source. The ULXs must be such bright in UV range as they are in X-rays. Spectroscopy of gas filaments surrounding SS 433 proves that the intrinsic face-on luminosity of the supercritical accretion disk in the far UV region to be "sim; 10^40 erg/s. We expect that observations of ULXs with the WSO-UV Observatory, measurements their UV fluxes and spectral slopes solve the problem of ULXs between the two known models of these sources.

  6. 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.

  7. Clocking Femtosecond X-Rays

    SciTech Connect

    Cavalieri, A L; Fritz, D M; Lee, S H; Bucksbaum, P H; Reis, D A; Mills, D M; Pahl, R; Rudati, J; Fuoss, P H; Stephenson, G B; Lowney, D P; MacPhee, A G; Weinstein, D; Falcone, R W; Als-Nielsen, J; Blome, C; Ischebeck, R; Schlarb, H; Tschentscher, T; Schneider, J; Sokolowski-Tinten, K; Chapman, H N; Lee, R W; Hansen, T N; Synnergren, O; Larsson, J; Techert, S; Sheppard, J; Wark, J S; Bergh, M; Calleman, C; Huldt, G; der Spoel, D v; Timneanu, N; Hajdu, J; Bong, E; Emma, P; Krejcik, P; Arthur, J; Brennan, S; Gaffney, K J; Lindenberg, A M; Hastings, J B

    2004-10-08

    The Sub-Picosecond Pulse Source (SPPS) at the Stanford Linear Accelerator Center (SLAC) produces the brightest ultrafast x-ray pulses in the world, and is the first to employ compressed femtosecond electron bunches for the x-ray source. Both SPPS and future X-ray Free Electron Lasers (XFEL's) will use precise measurements of individual electron bunches to time the arrival of x-ray pulses for time-resolved experiments. At SPPS we use electro-optic sampling (EOS) to perform these measurements. Here we present the first results using this method. An ultrafast laser pulse (135 fs) passes through an electro-optic crystal adjacent to the electron beam. The refractive index of the crystal is distorted by the strong electromagnetic fields of the ultra-relativistic electrons, and this transient birefringence is imprinted on the laser polarization. A polarizer decodes this signal, producing a time-dependent image of the compressed electron bunch. Our measurements yield the relative timing between an ultrafast optical laser and an ultrafast x-ray pulse to within 60 fs, making it possible to use the SPPS to observe atomic-scale ultrafast dynamics initiated by laser-matter interaction.

  8. X-rays surgical revolution.

    PubMed

    Toledo-Pereyra, Luis H

    2009-01-01

    Wilhelm Roentgen (1845-1923) created a surgical revolution with the discovery of the X-rays in late 1895 and the subsequent introduction of this technique for the management of surgical patients. No other physician or scientist had ever imagined such a powerful and worthwhile discovery. Other scientists paved the way for Roentgen to approach the use of these new X-rays for medical purposes. In this way, initially, and prior to Roentgen, Thompson, Hertz, and Lenard applied themselves to the early developments of this technology. They made good advances but never reached the clearly defined understanding brought about by Roentgen. The use of a Crookes tube, a barium platinocyanide screen, with fluorescent light and the generation of energy to propagate the cathode rays were the necessary elements for the conception of an X-ray picture. On November 8, 1895, Roentgen began his experiments on X-ray technology when he found that some kind of rays were being produced by the glass of the tube opposite to the cathode. The development of a photograph successfully completed this early imaging process. After six intense weeks of research, on December 22, he obtained a photograph of the hand of his wife, the first X-ray ever made. This would be a major contribution to the world of medicine and surgery.

  9. Superfine powdered activated carbon incorporated into electrospun polystyrene fibers preserve adsorption capacity.

    PubMed

    Apul, Onur G; Hoogesteijn von Reitzenstein, Natalia; Schoepf, Jared; Ladner, David; Hristovski, Kiril D; Westerhoff, Paul

    2017-03-17

    A composite material consisted of superfine powdered activated carbon (SPAC) and fibrous polystyrene (PS) was fabricated for the first time by electrospinning. SPAC is produced by pulverizing powdered activated carbon. The diameter of SPAC (100-400nm) is more than one hundred times smaller than conventional powdered activated carbon, but it maintains the internal pore structure based on organic micropollutant adsorption isotherms and specific surface area measurements. Co-spinning SPAC into PS fibers increased specific surface area from 6m(2)/g to 43m(2)/g. Unlike metal oxide nanoparticles, which are non-accessible for sorption from solution, electrospinning with SPAC created porous fibers. Composite SPAC-PS electrospun fibers, containing only 10% SPAC, had 30% greater phenanthrene sorption compared against PS fibers alone. SPAC particles embedded within the polymer were either partially or fully incorporated, and the accessibility of terminal adsorption sites were conserved. Conserving the adsorptive functionality of SPAC particles in electrospun non-woven polymeric fiber scaffolding can enable their application in environmental applications such as drinking water treatment.

  10. AN X-RAY STUDY OF THE ETHYLENE GLYCOLMONTMORILLONITE COMPLEX.

    DTIC Science & Technology

    SOILS, * MONTMORILLONITE , *GLYCOLS, *X RAY SPECTROSCOPY, X RAY SPECTRA, X RAY SPECTRA, X RAY SPECTRA, CLAY MINERALS, COMPLEX COMPOUNDS, FOURIER ANALYSIS, CRYSTAL STRUCTURE, THERMAL PROPERTIES, MATHEMATICAL MODELS.

  11. Adsorption from n-heptane/benzene liquid mixture on acid leached bentonite powders

    NASA Astrophysics Data System (ADS)

    Sarıkaya, Yüksel; Baykal, Mehmet; Önal, Müşerref; Yener, Nilgün

    2013-10-01

    In this study, adsorption excess isotherms of n-heptane/benzene liquid mixture on hydrochloric acid leached bentonite powders were determined. Adsorptions were conducted at 25 °C for 48 h. Experimental results were evaluated with both Schay-Nagy (SN) and Everett (E) methods. Specific surface areas (SSN and SE) of the powders were calculated regarding monolayer adsorption capacity of the preferentially adsorbed benzene. Adsorption equilibrium constants (K ≫ 1) were obtained by the E-method. The SE and SSN values are closed to each other. SE-values were found much lower than the corresponding Brunauer, Emmett and Teller (BET)-values. This difference was discussed with respect to the interaction of adsorbed molecules with solid surface, their collision diameter, molar cross sectional surface area and orientation in dense monolayer. Even the maximum for the SE was not associated with the maxima for K and nanopore volume (V), their values changed approximately parallel to each other with respect to the HCl% by the leaching.

  12. Incorporation of AgI clusters into the cages of zeolites LTA and FAU observed by optical spectra and X-ray diffraction patterns

    NASA Astrophysics Data System (ADS)

    Kodaira, Tetsuya; Ikeda, Takuji; Takeo, Harutoshi

    1999-02-01

    The loading of AgI into the cages of zeolites LTA and FAU was performed by vapor-phase adsorption. The successful incorporation of AgI clusters into the cages was confirmed by optical absorption spectra and X-ray powder diffraction patterns. Large blue shifts of the absorption edges were observed in the spectra of adsorbed AgI to both zeolites, compared with the lowest excited state of AgI in the bulk. The present observation of the shift implies that a strong quantum confinement in the photoexcited state of AgI occurs, which leads to the conclusion that AgI clusters have been formed in the cages. In the X-ray powder diffraction pattern of AgI-loaded LTA, superlattice reflection peaks are observed which cannot be assigned either to the reflection of LTA or the AgI in the bulk.

  13. 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.

  14. 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.

  15. Coherent x-ray diffraction

    NASA Astrophysics Data System (ADS)

    Pitney, John Allen

    Conventional x-ray diffraction has historically been done under conditions such that the measured signal consists of an incoherent addition of scattering which is coherent only on a length scale determined by the properties of the beam. The result of the incoherent summation is a statistical averaging over the whole illuminated volume of the sample, which yields certain kinds of information with a high degree of precision and has been key to the success of x-ray diffraction in a variety of applications. Coherent x-ray scattering techniques, such as coherent x-ray diffraction (CXD) and x-ray intensity fluctuation spectroscopy (XIFS), attempt to reduce or eliminate any incoherent averaging so that specific, local structures couple to the measurement without being averaged out. In the case of XIFS, the result is analogous to dynamical light scattering, but with sensitivity to length scales less than 200 nm and time scales from 10-3 s to 103 s. When combined with phase retrieval, CXD represents an imaging technique with the penetration, in situ capabilities, and contrast mechanisms associated with x-rays and with a spatial resolution ultimately limited by the x-ray wavelength. In practice, however, the spatial resolution of CXD imaging is limited by exposure to about 100 A. This thesis describes CXD measurements of the binary alloy Cu3Au and the adaptation of phase retrieval methods for the reconstruction of real-space images of Cu3Au antiphase domains. The theoretical foundations of CXD are described in Chapter 1 as derived from the kinematical formulation for x-ray diffraction and from the temporal and spatial coherence of radiation. The antiphase domain structure of Cu 3Au is described, along with the associated reciprocal-space structure which is measured by CXD. CXD measurements place relatively stringent requirements on the coherence properties of the beam and on the detection mechanism of the experiment; these requirements and the means by which they have been

  16. 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.

  17. X-ray emission spectroscopy.

    PubMed

    Bergmann, Uwe; Glatzel, Pieter

    2009-01-01

    We describe the chemical information that can be obtained by means of hard X-ray emission spectroscopy (XES). XES is presented as a technique that is complementary to X-ray absorption spectroscopy (XAS) and that provides valuable information with respect to the electronic structure (local charge- and spin-density) as well as the ligand environment of a 3d transition metal. We address non-resonant and resonant XES and present results that were recorded on Mn model systems and the Mn(4)Ca-cluster in the oxygen evolving complex of photosystem II. A brief description of the instrumentation is given with an outlook toward future developments.

  18. 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.

  19. Compact Flash X-Ray Units

    DTIC Science & Technology

    1995-07-01

    Flash x-ray units are used to diagnose pulsed power driven experiments on the Pegasus machine at Los Alamos. Several unique designs of Marx powered...employing an x-ray tube configuration which allows closely spaced x-ray emitting anodes. These units all emit a 10 ns FWHM x-ray pulse. Their Marx banks

  20. X-ray exposure sensor and controller

    NASA Technical Reports Server (NTRS)

    Berdahl, C. Martin (Inventor)

    1977-01-01

    An exposure controller for x-ray equipment is provided, which comprises a portable and accurate sensor which can be placed adjacent to and directly beneath the area of interest of an x-ray plate, and which measures the amount of exposure received by that area, and turns off the x-ray equipment when the exposure for the particular area of interest on the x-ray plate reaches the value which provides an optimal x-ray plate.

  1. 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.

  2. Adsorption of Cu2+ and Pb2+ ion on dolomite powder.

    PubMed

    Pehlivan, Erol; Ozkan, Ali Müjdat; Dinç, Salih; Parlayici, Serife

    2009-08-15

    Natural Turkish dolomite was shown to be effective for removing Cu(2+) and Pb(2+) from aqueous solution. Selected information on pH, dose required, initial metal concentration, adsorption capacity of the raw dolomite powder was evaluated for its efficiency in adsorbing metal ions. Dolomite exhibited good Cu(2+) and Pb(2+) removal levels at all initial metal amount tested (0.04-0.32 mmol, 20 mL). It is important to note that the adsorption capacities of the materials in equilibrium vary, depending on the characteristics of the individual adsorbent, the initial concentration of the adsorbate and pH of the solution. One hour was enough for the removal of metal ions from (0.2 mmol in 20 mL) aqueous solution. Effective removal of metal ions was demonstrated at pH values of 5.0. The adsorptive behavior of dolomite was described by fitting data generated from the study of the Langmuir and Freundlich isotherm models. The adsorption capacity of dolomite was found as 8.26 mg for Cu(2+) and 21.74 mg for Pb(2+), respectively, from the calculation of adsorption isotherm equation. More than 85% of studied cations were removed by dolomite from aqueous solution in single step. The mechanism for cations removal by dolomite includes surface complexation and ion exchange.

  3. 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.

  4. Stellar x-ray flares

    NASA Astrophysics Data System (ADS)

    Haisch, B.; Uchida, Y.; Kosugi, T.; Hudson, H. S.

    1995-01-01

    What is the importance of stellar X-ray flares to astrophysics, or even more, to the world at large? In the case of the Sun, changes in solar activity at the two temporal extremes can have quite significant consequences. Longterm changes in solar activity, such as the Maunder Minimum, can apparently lead to non-negligible alterations of the earth's climate. The extreme short term changes are solar flares, the most energetic of which can cause communications disruptions, power outages and ionizing radiation levels amounting to medical X-ray dosages on long commercial flights and even potentially lethal exposures for unshielded astronauts. Why does the Sun exhibit such behaviour? Even if we had a detailed knowledge of the relevant physical processes on the Sun - which we may be on the way to having in hand as evidenced by these Proceedings- our understanding would remain incomplete in regard to fundamental causation so long as we could not say whether the Sun is, in this respect, unique among the stars. This current paper discusses the stellar x-ray flare detections and astronomical models (quasi-static cooling model and two-ribbon model) that are used to observe the x-ray emission.

  5. 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.

  6. 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.

  7. 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.

  8. Rontgen's Discovery of X Rays

    ERIC Educational Resources Information Center

    Thumm, Walter

    1975-01-01

    Relates the story of Wilhelm Conrad Rontgen and presents one view of the extent to which the discovery of the x-ray was an accident. Reconstructs the sequence of events that led to the discovery and includes photographs of the lab where he worked and replicas of apparatus used. (GS)

  9. Compact x-ray source and panel

    SciTech Connect

    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.

  10. [Effects of pH and coexisting cations on ammonia adsorption from aqueous solution by strawberry stem powder].

    PubMed

    Liu, Hai-wei; Liu, Yun; Wang, Hai-yun; Dong, Yuan-hua

    2010-08-01

    Batch equilibrium experiments were carried out to study ammonia adsorptions from aqueous solution by strawberry (Fragaia ananassa Duchesne) stem powder. The effects of pH, coexisting cations, initial ammonia concentration and temperature were investigated as well. The results showed that the equilibrium data fitted well to the Langmuir model and Freundlich model, and the maximum adsorption capacities were 3.05, 4.24 and 4.79 mg x g(-1) at 15, 25 and 35 degrees C respectively. The increase of temperature was favorable to ammonia adsorption. The optimal pH of ammonia adsorption was in the range of 4-8. The NH4+ content decreased at higher pH and the negative charges decreased at lower pH, resulting in the decrease of ammonia adsorption at both higher and lower pH. The pH changes after adsorption buffered both effects. K+, Na+, Ca2+ and Mg2+ had no effect on ammonia adsorption by strawberry stem, but Zn2+ and Al3+ decreased the adsorption for their hydrolyzation. The ammonia adsorption by strawberry stem powder could be applied in a large pH range and could not be affected by usual metal cations in wastewater, therefore the strawberry stem powder not only could be a suitable ammonia adsorbent, but also had advantages comparing with most mineral materials.

  11. 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…

  12. High-temperature, high-pressure hydrothermal synthesis, crystal structure, and solid-state NMR spectroscopy of Cs2(UO2)(Si2O6) and variable-temperature powder X-ray diffraction study of the hydrate phase Cs2(UO2)(Si2O6) x 0.5H2O.

    PubMed

    Chen, Chih-Shan; Chiang, Ray-Kuang; Kao, Hsien-Ming; Lii, Kwang-Hwa

    2005-05-30

    A new uranium(VI) silicate, Cs2(UO2)(Si2O6), has been synthesized by a high-temperature, high-pressure hydrothermal method and characterized by single-crystal X-ray diffraction and solid-state NMR spectroscopy. It crystallizes in the orthorhombic space group Ibca (No. 73) with a = 15.137(1) A, b = 15.295(1) A, c = 16.401(1) A, and Z = 16. Its structure consists of corrugated achter single chains of silicate tetrahedra extending along the c axis linked together via corner-sharing by UO6 tetragonal bipyramids to form a 3-D framework which delimits 8- and 6-ring channels. The Cs+ cations are located in the channels or at sites between channels. The 29Si and 133Cs MAS NMR spectra are consistent with the crystal structure as determined from X-ray diffraction, and the resonances in the spectra are assigned. Variable-temperature in situ powder X-ray diffraction study of the hydrate Cs2(UO2)(Si2O6) x 0.5H2O indicates that the framework structure is stable up to 800 degrees C and transforms to the structure of the title compound at 900 degrees C. A comparison of related uranyl silicate structures is made.

  13. Geosmin and 2-methylisoborneol adsorption on super-powdered activated carbon in the presence of natural organic matter.

    PubMed

    Matsui, Y; Nakano, Y; Hiroshi, H; Ando, N; Matsushita, T; Ohno, K

    2010-01-01

    Geosmin and 2-methylisoborneol (2-MIB) are naturally occurring compounds responsible for musty-earthy-odors in surface water supplies. They are a severe problem confronting utilities worldwide. Adsorption by powdered activated carbon (PAC) is a widely used process to control this problem, but it has low efficiency, which engenders large budget spending for utilities services. Super-powdered activated carbon (S-PAC) is activated carbon with much finer particles than those of PAC. Experiments on geosmin and 2-MIB adsorptions on S-PAC and PAC were conducted. Geosmin and 2-MIB adsorption capacities on S-PAC were not smaller than those on PAC although natural organic matter, which adversely impacted the adsorption capacity of geosmin and 2-MIB, was more adsorbed on S-PAC than on PAC, meaning that the adsorption competition is less severe for S-PAC than for PAC.

  14. 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.

  15. Adsorptive cathodic stripping voltammetric determination of cefoperazone in bulk powder, pharmaceutical dosage forms, and human urine.

    PubMed

    Hoang, Vu Dang; Huyen, Dao Thi; Phuc, Phan Hong

    2013-01-01

    The electroreduction behaviour and determination of cefoperazone using a hanging mercury drop electrode were investigated. Cyclic voltammograms of cefoperazone recorded in universal Britton-Robinson buffers pH 3-6 exhibited a single irreversible cathodic peak. The process was adsorption-controlled. Britton-Robinson buffer 0.04 M pH 4.0 was selected as a supporting electrolyte for quantitative purposes by differential pulse and square wave adsorptive cathodic stripping voltammetry. The experimental voltammetric conditions were optimized using Central Composite Face design. A reduction wave was seen in the range from -0.7 to -0.8 V. These voltammetric techniques were successfully validated as per ICH guidelines and applied for the determination of cefoperazone in its single and sulbactam containing powders for injection and statistically comparable to USP-HPLC. They were further extended to determine cefoperazone in spiked human urine with no matrix effect.

  16. Adsorptive Cathodic Stripping Voltammetric Determination of Cefoperazone in Bulk Powder, Pharmaceutical Dosage Forms, and Human Urine

    PubMed Central

    Hoang, Vu Dang; Huyen, Dao Thi; Phuc, Phan Hong

    2013-01-01

    The electroreduction behaviour and determination of cefoperazone using a hanging mercury drop electrode were investigated. Cyclic voltammograms of cefoperazone recorded in universal Britton-Robinson buffers pH 3–6 exhibited a single irreversible cathodic peak. The process was adsorption-controlled. Britton-Robinson buffer 0.04 M pH 4.0 was selected as a supporting electrolyte for quantitative purposes by differential pulse and square wave adsorptive cathodic stripping voltammetry. The experimental voltammetric conditions were optimized using Central Composite Face design. A reduction wave was seen in the range from −0.7 to −0.8 V. These voltammetric techniques were successfully validated as per ICH guidelines and applied for the determination of cefoperazone in its single and sulbactam containing powders for injection and statistically comparable to USP-HPLC. They were further extended to determine cefoperazone in spiked human urine with no matrix effect. PMID:24109542

  17. Use of cork powder and granules for the adsorption of pollutants: a review.

    PubMed

    Pintor, Ariana M A; Ferreira, Catarina I A; Pereira, Joana C; Correia, Patrícia; Silva, Susana P; Vilar, Vítor J P; Botelho, Cidália M S; Boaventura, Rui A R

    2012-06-15

    Cork powder and granules are the major subproducts of the cork industry, one of the leading economic activities in Portugal and other Mediterranean countries. Many applications have been envisaged for this product, from cork stoppers passing through the incorporation in agglomerates and briquettes to the use as an adsorbent in the treatment of gaseous emissions, waters and wastewaters. This paper aims at reviewing the state of the art on the properties of cork and cork powder and their application in adsorption technologies. Cork biomass has been used on its original form as biosorbent for heavy metals and oils, and is also a precursor of activated carbons for the removal of emerging organic pollutants in water and VOCs in the gas phase. Through this literature review, different potential lines of research not yet explored can be more easily identified.

  18. Effective X-ray beam size measurements of an X-ray tube and polycapillary X-ray lens system using a scanning X-ray fluorescence method

    NASA Astrophysics Data System (ADS)

    Gherase, Mihai R.; Vargas, Andres Felipe

    2017-03-01

    Size measurements of an X-ray beam produced by an integrated polycapillary X-ray lens (PXL) and X-ray tube system were performed by means of a scanning X-ray fluorescence (SXRF) method using three different metallic wires. The beam size was obtained by fitting the SXRF data with the analytical convolution between a Gaussian and a constant functions. For each chemical element in the wire an effective energy was calculated based on the incident X-ray spectrum and its photoelectric cross section. The proposed method can be used to measure the effective X-ray beam size in XRF microscopy studies.

  19. 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)

  20. 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.

  1. Microgap x-ray detector

    DOEpatents

    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.

  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. 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.

  4. 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.

  5. 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.

  6. 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 ...

  7. 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.

  8. Producing X-rays at the APS

    ScienceCinema

    None

    2016-07-12

    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.

  9. Characterization of a pulsed x-ray source for fluorescent lifetime measurements

    NASA Astrophysics Data System (ADS)

    Blankespoor, S. C.; Derenzo, S. E.; Moses, W. W.; Rossington, C. S.; Ito, M.; Oba, K.

    1994-08-01

    To search for new, fast, inorganic scintillators, we have developed a bench-top pulsed x-ray source for determining fluorescent lifetimes and wavelengths of compounds in crystal or powdered form. This source uses a light-excited x-ray tube which produces x-rays when light from a laser diode strikes its photocathode. The x-ray tube has a tungsten anode, a beryllium exit window, a 30 kV maximum tube bias, and a 50 mu A maximum average cathode current. The laser produces 3 x 10(sup 7) photons at 650 nm per approximately 100 ps pulse, with up to 10(sup 7) pulses/sec. The time spread for the laser diode, x-ray tube, and a microchannel plate photomultiplier tube is less than 120 ps fwhm. The mean x-ray energy at tube biases of 20, 25, and 30 kV is 9.4, 10.3, and 11.1 keV, respectively. We measured 140, 230, and 330 x-ray photons per laser diode pulse per steradian, at tube biases of 20, 25, and 30 kV, respectively. Background x-rays due to dark current occur at a rate of 1 x 10(sup 6) and 3 x 10(sup 6) photons/sec/steradian at biases of 25 and 30 kV, respectively. Data characterizing the x-ray output with an aluminum filter in the x-ray beam are also presented.

  10. Phase-sensitive X-ray imager

    SciTech Connect

    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.

  11. 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.

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

    PubMed Central

    Mitsui, Yoshifuru; Koyama, Keiichi; Watanabe, Kazuo

    2009-01-01

    A system was developed measuring x-ray powder diffraction in high magnetic fields up to 5 T and at temperatures from 283 to 473 K. The stability of the temperature is within 1 K over 6 h. In order to examine the ability of the system, the high-field x-ray diffraction measurements were carried out for Si and a Ni-based ferromagnetic shape-memory alloy. The results show that the x-ray powder diffraction measurements in high magnetic fields and at high temperatures are useful for materials research. PMID:27877263

  13. 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.

  14. 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)

  15. 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.

  16. X-Ray Exam: Cervical Spine

    MedlinePlus

    ... to 2-Year-Old X-Ray Exam: Cervical Spine KidsHealth > For Parents > X-Ray Exam: Cervical Spine A A A What's in this article? What ... Radiografía: columna cervical What It Is A cervical spine X-ray is a safe and painless test ...

  17. 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.

  18. X-Ray Exam: Femur (Upper Leg)

    MedlinePlus

    ... Old Feeding Your 1- to 2-Year-Old X-Ray Exam: Femur (Upper Leg) KidsHealth > For Parents > X-Ray Exam: Femur (Upper Leg) Print A A A ... español Radiografía: fémur What It Is A femur X-ray is a safe and painless test that uses ...

  19. X-Ray Exam: Neck (For Parents)

    MedlinePlus

    ... Old Feeding Your 1- to 2-Year-Old X-Ray Exam: Neck KidsHealth > For Parents > X-Ray Exam: Neck Print A A A What's in ... español Radiografía: cuello What It Is A neck X-ray is a safe and painless test that uses ...

  20. X-Ray Exam: Cervical Spine

    MedlinePlus

    ... to 2-Year-Old X-Ray Exam: Cervical Spine KidsHealth > For Parents > X-Ray Exam: Cervical Spine Print A A A What's in this article? ... Radiografía: columna cervical What It Is A cervical spine X-ray is a safe and painless test ...

  1. Chest X-Ray (Chest Radiography)

    MedlinePlus

    ... x-rays. top of page What does the equipment look like? The equipment typically used for chest x-rays consists of ... tube is positioned about six feet away. The equipment may also be arranged with the x-ray ...

  2. 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.

  3. X-ray optics: Diamond brilliance

    NASA Astrophysics Data System (ADS)

    Durbin, Stephen M.; Colella, Roberto

    2010-03-01

    Most materials either absorb or transmit X-rays. This is useful for imaging but makes it notoriously difficult to build mirrors for reflective X-ray optics. A demonstration of the high X-ray reflectivity of diamond could provide a timely solution to make the most of the next generation of free-electron lasers.

  4. 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.

  5. Phenol adsorption onto powdered and granular activated carbon, prepared from Eucalyptus wood.

    PubMed

    Tancredi, Nestor; Medero, Natalia; Möller, Fabiana; Píriz, Javier; Plada, Carina; Cordero, Tomás

    2004-11-15

    Eucalyptus grandis sawdust, a major waste from the growing Uruguayan wood industry, was used in previous work to prepare powdered activated carbon (PAC). In the present work, granular activated carbon (GAC) was prepared by mixing PAC, carboxymethyl cellulose as a binder, and kaolin as reinforcer. Ultimate analysis and surface characterization of GAC and PAC were performed. Phenol adsorption was used as a way to compare the characteristics of different PAC and GAC preparations. Kinetics and isotherms of the different GAC and PAC were performed in a shaking bath at 100 rpm and 298 K. Phenol concentrations were determined by UV spectroscopy. Some kinetics parameters were calculated; from kinetics results, external resistance to mass transfer from the bulk liquid can be neglected as the controlling step. Isotherms were fitted to Langmuir and Freundlich models, and corresponding parameters were determined. Maximum phenol uptakes for all carbons were determined and correlated with carbon characteristics. Thermogravimertic analysis (TGA) determinations were performed in order to study adsorption characteristics and conditions for GAC regeneration after its use. The results showed that phenol is preferentially physisorbed on the carbon of the granules, though some chemisorption was detected. No adsorption was detected in the kaolin-carboxymethyl cellulose mixture.

  6. Mobile X-Ray Unit.

    DTIC Science & Technology

    1996-10-28

    anode 8 surrounded by a coaxial annulus of stainless steel mesh which 9 serves as the cathode, control electronics, and a plurality of 10 spark gap...34Siemens-tube" configuration. More 7 particularly, the X-ray tube 16 has a conical copper/tungsten 8 anode 28, and a stainless steel mesh punched to...160 and 162 each having a typical diameter of 14 2.75 inches. The conflat flanges 160 and 162 are mated to a 15 stainless steel tube 164 having a

  7. 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.

  8. 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.

  9. 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.

  10. X-ray imaging for palaeontology.

    PubMed

    Hohenstein, P

    2004-05-01

    Few may be aware that X-ray imaging is used in palaeontology and has been used since as early as 1896. The X-raying, preparation and exposure of Hunsrück slate fossils are described. Hospital X-ray machines are used by the author in his work. An X-ray is vital to provide evidence that preparation of a slate is worthwhile as well as to facilitate preparation even if there is little external sign of what lies within. The beauty of the X-ray exposure is an added bonus.

  11. 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.

  12. Method for spatially modulating X-ray pulses using MEMS-based X-ray optics

    DOEpatents

    Lopez, Daniel; Shenoy, Gopal; Wang, Jin; Walko, Donald A.; Jung, Il-Woong; Mukhopadhyay, Deepkishore

    2015-03-10

    A method and apparatus are provided for spatially modulating X-rays or X-ray pulses using microelectromechanical systems (MEMS) based X-ray optics. A torsionally-oscillating MEMS micromirror and a method of leveraging the grazing-angle reflection property are provided to modulate X-ray pulses with a high-degree of controllability.

  13. 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.

  14. X-ray omni microscopy.

    PubMed

    Paganin, D; Gureyev, T E; Mayo, S C; Stevenson, A W; Nesterets, Ya I; Wilkins, S W

    2004-06-01

    The science of wave-field phase retrieval and phase measurement is sufficiently mature to permit the routine reconstruction, over a given plane, of the complex wave-function associated with certain coherent forward-propagating scalar wave-fields. This reconstruction gives total knowledge of the information that has been encoded in the complex wave-field by passage through a sample of interest. Such total knowledge is powerful, because it permits the emulation in software of the subsequent action of an infinite variety of coherent imaging systems. Such 'virtual optics', in which software forms a natural extension of the 'hardware optics' in an imaging system, may be useful in contexts such as quantitative atom and X-ray imaging, in which optical elements such as beam-splitters and lenses can be realized in software rather than optical hardware. Here, we develop the requisite theory to describe such hybrid virtual-physical imaging systems, which we term 'omni optics' because of their infinite flexibility. We then give an experimental demonstration of these ideas by showing that a lensless X-ray point projection microscope can, when equipped with the appropriate software, emulate an infinite variety of optical imaging systems including those which yield interferograms, Zernike phase contrast, Schlieren imaging and diffraction-enhanced imaging.

  15. 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.

  16. The Rosat x-ray sky

    NASA Astrophysics Data System (ADS)

    Voges, Wolfgang

    1995-01-01

    The ROSAT (Röntgensatellit) X-ray astronomy satellite has completed the first all-sky x-ray and XUV survey with imaging telescopes. About 60 000 new x-ray and 400 new XUV (1) sources were detected. This contribution will deal with preliminary results from the ROSAT ALL-SKY X-RAY SURVEY. The ROSAT diffuse and point-source x-ray skymaps, the positional accuracy obtained for the x-ray sources, and a few results from correlations performed with available catalogues in various energy bands like the Radio, Infrared, Visible, UV, and hard x-rays as well as identifications from optical follow-up observations will be presented.

  17. Spectral slicing X-ray telescope

    NASA Technical Reports Server (NTRS)

    Hoover, R. B.; Shealy, D.; Chao, S.-H.

    1986-01-01

    Layered synthetic microstructure (LSM) X-ray optics is investigated as a system for coupling a conventional glancing incidence X-ray mirror to a high sensitivity X-ray detector. It is shown that, by the use of figured LSM optics, it is possible to magnify the X-ray image produced by the primary mirrors so as to maintain their high inherent spatial resolution. The results of theoretical and design analyses of several spectral slicing X-ray telescope systems that utilize LSM mirrors of hyperboloidal, spherical, ellipsoidal, and constant optical path aspheric configurations are presented. It is shown that the spherical LSM optics are the preferred configuration, yielding subarcsecond performance over the entire field. The Stanford/Marshall Space Flight Center Rocket X-ray Telescope, which will utilize normal incidence LSM optics to couple a Wolter-Schwarzschild primary mirror to high resolution detectors for solar X-ray/EUV studies, is discussed. Design diagrams are included.

  18. 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.

  19. 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.

  20. A single crystal X-ray and powder neutron diffraction study on NASICON-type Li1+xAlxTi2-x(PO4)3 (0 ≤ x ≤ 0.5) crystals: Implications on ionic conductivity

    NASA Astrophysics Data System (ADS)

    Redhammer, G. J.; Rettenwander, D.; Pristat, S.; Dashjav, E.; Kumar, C. M. N.; Topa, D.; Tietz, F.

    2016-10-01

    Single crystals of NASICON-type material Li1+xTi2-xAlx(PO4)3 (LATP) with 0 ≤ x ≤ 0.5 were successfully grown using long-term sintering techniques. Sample material was studied by chemical analysis, single crystal X-ray and neutron diffraction. The Ti4+ replacement scales very well with the Al3+ and Li+ incorporation. The additional Li+ thereby enters the M3 cavity of the NASICON framework at x, y, z ∼ (0.07, 0.34, 0.09) and is regarded to be responsible for the enhanced Li+ conduction of LATP as compared to Al-free LTP. Variations in structural parameters, associated with the Ti4+ substitution with Al3+ + Li+ will be discussed in detail in this paper.

  1. Adsorption of volatile organic compounds in porous metal-organic frameworks functionalized by polyoxometalates

    NASA Astrophysics Data System (ADS)

    Ma, Feng-Ji; Liu, Shu-Xia; Liang, Da-Dong; Ren, Guo-Jian; Wei, Feng; Chen, Ya-Guang; Su, Zhong-Min

    2011-11-01

    The functionalization of porous metal-organic frameworks (Cu 3( BTC) 2) was achieved by incorporating Keggin-type polyoxometalates (POMs), and further optimized via alkali metal ion-exchange. In addition to thermal gravimetric analysis, IR, single-crystal X-ray diffraction, and powder X-ray diffraction, the adsorption properties were characterized by N 2 and volatile organic compounds (VOCs) adsorption measurements, including short-chain alcohols ( C<4), cyclohexane, benzene, and toluene. The adsorption enthalpies estimated by the modified Clausius-Clapeyron equation provided insight into the impact of POMs and alkali metal cations on the adsorption of VOCs. The introduction of POMs not only improved the stability, but also brought the increase of adsorption capacity by strengthening the interaction with gas molecules. Furthermore, the exchanged alkali metal cations acted as active sites to interact with adsorbates and enhanced the adsorption of VOCs.

  2. 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.

  3. Parametric X-rays from a polycrystalline target

    NASA Astrophysics Data System (ADS)

    Lobach, Ihar; Benediktovitch, Andrei; Feranchuk, Ilya; Lobko, Alexander

    2015-10-01

    A theoretical description of parametric X-ray radiation (PXR) from a nanocrystal powder target is presented in terms of the orientation distribution function (ODF). Two models of ODF resulting in the analytical solution for the PXR intensity distribution are used and the characteristic features of this distribution are considered. A promising estimate of the number of the emitted photons is obtained for the case of a nanodiamond powder target using the parameters of ASTA Facility at Fermilab. The PXR spectra from polycrystal and single crystal targets are compared. The application scenarios of PXR from nanocrystals are discussed.

  4. 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.

  5. 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.

  6. Controlling X-rays with light

    NASA Astrophysics Data System (ADS)

    Glover, T. E.; Hertlein, M. P.; Southworth, S. H.; Allison, T. K.; van Tilborg, J.; Kanter, E. P.; Krässig, B.; Varma, H. R.; Rude, B.; Santra, R.; Belkacem, A.; Young, L.

    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.

  7. Compact Stellar X-ray Sources

    NASA Astrophysics Data System (ADS)

    Lewin, Walter H. G.; van der Klis, Michiel

    2006-04-01

    1. Accreting neutron stars and black holes: a decade of discoveries D. Psaltis; 2. Rapid X-ray variability M. van der Klis; 3. New views of thermonuclear bursts T. Strohmayer and L. Bildsten; 4. Black hole binaries J. McClintock and R. Remillard; 5. Optical, ultraviolet and infrared observations of X-ray binaries P. Charles and M. Coe; 6. Fast X-ray transients and X-ray flashes J. Heise and J. in 't Zand; 7. Isolated neutron stars V. Kaspi, M. Roberts and A. Harding; 8. Globular cluster X-ray sources F. Verbunt and W. Lewin; 9. Jets from X-ray binaries R. Fender; 10. X-Rays from cataclysmic variables E. Kuulkers, A. Norton, A. Schwope and B. Warner; 11. Super soft sources P. Kahabka and E. van den Heuvel; 12. Compact stellar X-ray sources in normal galaxies G. Fabbiano and N. White; 13. Accretion in compact binaries A. King; 14. Soft gamma repeaters and anomalous X-ray pulsars: magnetar candidates P. Woods and C. Thompson; 15. Cosmic gamma-ray bursts, their afterglows, and their host galaxies K. Hurley, R. Sari and S. Djorgovski; 16. Formation and evolution of compact stellar X-ray sources T. Tauris and E. van den Heuvel.

  8. Compact Stellar X-ray Sources

    NASA Astrophysics Data System (ADS)

    Lewin, Walter; van der Klis, Michiel

    2010-11-01

    1. Accreting neutron stars and black holes: a decade of discoveries D. Psaltis; 2. Rapid X-ray variability M. van der Klis; 3. New views of thermonuclear bursts T. Strohmayer and L. Bildsten; 4. Black hole binaries J. McClintock and R. Remillard; 5. Optical, ultraviolet and infrared observations of X-ray binaries P. Charles and M. Coe; 6. Fast X-ray transients and X-ray flashes J. Heise and J. in 't Zand; 7. Isolated neutron stars V. Kaspi, M. Roberts and A. Harding; 8. Globular cluster X-ray sources F. Verbunt and W. Lewin; 9. Jets from X-ray binaries R. Fender; 10. X-Rays from cataclysmic variables E. Kuulkers, A. Norton, A. Schwope and B. Warner; 11. Super soft sources P. Kahabka and E. van den Heuvel; 12. Compact stellar X-ray sources in normal galaxies G. Fabbiano and N. White; 13. Accretion in compact binaries A. King; 14. Soft gamma repeaters and anomalous X-ray pulsars: magnetar candidates P. Woods and C. Thompson; 15. Cosmic gamma-ray bursts, their afterglows, and their host galaxies K. Hurley, R. Sari and S. Djorgovski; 16. Formation and evolution of compact stellar X-ray sources T. Tauris and E. van den Heuvel.

  9. Comparative study of GeO2/Ge and SiO2/Si structures on anomalous charging of oxide films upon water adsorption revealed by ambient-pressure X-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Mori, Daichi; Oka, Hiroshi; Hosoi, Takuji; Kawai, Kentaro; Morita, Mizuho; Crumlin, Ethan J.; Liu, Zhi; Watanabe, Heiji; Arima, Kenta

    2016-09-01

    The energy difference between the oxide and bulk peaks in X-ray photoelectron spectroscopy (XPS) spectra was investigated for both GeO2/Ge and SiO2/Si structures with thickness-controlled water films. This was achieved by obtaining XPS spectra at various values of relative humidity (RH) of up to ˜15%. The increase in the energy shift is more significant for thermal GeO2 on Ge than for thermal SiO2 on Si above ˜10-4% RH, which is due to the larger amount of water molecules that infiltrate into the GeO2 film to form hydroxyls. Analyzing the origins of this energy shift, we propose that the positive charging of a partially hydroxylated GeO2 film, which is unrelated to X-ray irradiation, causes the larger energy shift for GeO2/Ge than for SiO2/Si. A possible microscopic mechanism of this intrinsic positive charging is the emission of electrons from adsorbed water species in the suboxide layer of the GeO2 film to the Ge bulk, leaving immobile cations or positively charged states in the oxide. This may be related to the reported negative shift of flat band voltages in metal-oxide-semiconductor diodes with an air-exposed GeO2 layer.

  10. Formation of ettringite, Ca 6Al 2(SO 4) 3(OH) 12·26H 2O, AFt, and monosulfate, Ca 4Al 2O 6(SO 4)·14H 2O, AFm-14, in hydrothermal hydration of Portland cement and of calcium aluminum oxide—calcium sulfate dihydrate mixtures studied by in situ synchrotron X-ray powder diffraction

    NASA Astrophysics Data System (ADS)

    Christensen, Axel Nørlund; Jensen, Torben R.; Hanson, Jonathan C.

    2004-06-01

    In the hydration of calcium aluminum oxide-gypsum mixtures, i.e., Ca 3Al 2O 6, Ca 12Al 14O 33 and CaSO 4·2H 2O, the reaction products can be ettringite, Ca 6Al 2(SO 4) 3(OH) 12·26H 2O, monosulfate, Ca 4Al 2O 6(SO 4)·14H 2O, or the calcium aluminum oxide hydrate, Ca 4Al 2O 7·19H 2O. Ettringite is formed if sufficient CaSO 4·2H 2O is present in the mixture. Ettringite is converted to monosulfate when all CaSO 4·2H 2O is consumed in the synthesis of ettringite. The reactions were investigated in the temperature range 25-170°C using in situ synchrotron X-ray powder diffraction. This technique allows the study of very fast chemical reactions that are observed here under hydrothermal conditions. A new experimental approach was developed to perform in situ mixing of the reactants during X-ray data collection.

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. The anomalous X-ray pulsars

    NASA Astrophysics Data System (ADS)

    Chen, Rui; Li, Xiangdong

    2002-03-01

    In the last few years it has been recognized that a group of X-ray pulsars have peculiar properties which set them apart from the majority of accreting pulars in X-ray binaries. They are called the Anomalous X-ray Pulsars (AXP). These objects are characterized by very soft X-ray spectra with low and steady X-ray fluxes, narrow-distributed spin periods, steady spin-down, no optical/infrared counterparts. Some of them may associate with supernova remnants. The nature of AXP remains mysterious. It has been suggested that AXP are accreting neutron stars, or solitary "magnetars", neutron stars with super strong magnetic fields (≍1010-1011T). In this paper we review the recent progress in the studies of AXP, and discuss the possible implications from comparison of AXP with other neutron stars, such as radio pulsars, radio quiet X-ray pulsar candidates and soft γ-ray repeaters.

  17. 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)

  18. 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.

  19. 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.

  20. UV observations of x ray binaries

    NASA Technical Reports Server (NTRS)

    Raymond, John C.

    1990-01-01

    IUE (International Ultraviolet Explorer) has observed both high and low mass x ray binaries throughout its life. The UV spectra of high mass systems reveal the nature of the massive companion star and the effects of the x ray illumination of the stellar wind. In loss mass systems, the x ray illuminated disk or companion star dominates the UV light. System parameters and the characteristics of the accretion disk can be inferred.

  1. 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.

  2. 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…

  3. 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.

  4. Negative affinity X-ray photocathodes

    NASA Technical Reports Server (NTRS)

    Vanspeybroeck, L.; Kellogg, E.; Murray, S.; Duckett, S.

    1974-01-01

    A new X-ray image intensifier is described. The device should eventually have a quantum efficiency which is an order of magnitude greater than that of presently available high spatial resolution X-ray detectors, such as microchannel plates. The new intesifier is based upon a GaAs crystal photocathode which is activated to achieve negative electron affinity. Details concerning the detector concept are discussed together with the theoretical relations involved, X-ray data, and optical data.

  5. The Overutilization of X-rays

    PubMed Central

    Lyon, W. K.

    1981-01-01

    Within 20 years of Roentgen's discovery of X-rays in 1895, it became apparent that large doses of radiation damaged human tissue.1 Yet the medical profession continues to contribute to the overutilization of X-rays, occasionally spending health care dollars to subject our patients to a health risk. This paper discusses the evidence to support the claim that X-rays are overutilized, and offers recommendations to rectify the situation. PMID:21289771

  6. 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

    2016-02-09

    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.

  7. 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.

  8. Ultrashort X-ray pulse science

    SciTech Connect

    Chin, Alan Hap

    1998-05-01

    A variety of phenomena involves atomic motion on the femtosecond time-scale. These phenomena have been studied using ultrashort optical pulses, which indirectly probe atomic positions through changes in optical properties. Because x-rays can more directly probe atomic positions, ultrashort x-ray pulses are better suited for the study of ultrafast structural dynamics. One approach towards generating ultrashort x-ray pulses is by 90° Thomson scattering between terawatt laser pulses and relativistic electrons. Using this technique, the author generated ~ 300 fs, 30 keV (0.4 Å) x-ray pulses. These x-ray pulses are absolutely synchronized with ultrashort laser pulses, allowing femtosecond optical pump/x-ray probe experiments to be performed. Using the right-angle Thomson scattering x-ray source, the author performed time-resolved x-ray diffraction studies of laser-perturbated InSb. These experiments revealed a delayed onset of lattice expansion. This delay is due to the energy relaxation from a dense electron-hole plasma to the lattice. The dense electron-hole plasma first undergoes Auger recombination, which reduces the carrier concentration while maintaining energy content. Longitudinal-optic (LO) phonon emission then couples energy to the lattice. LO phonon decay into acoustic phonons, and acoustic phonon propagation then causes the growth of a thermally expanded layer. Source characterization is instrumental in utilizing ultrashort x-ray pulses in time-resolved x-ray spectroscopies. By measurement of the electron beam diameter at the generation point, the pulse duration of the Thomson scattered x-rays is determined. Analysis of the Thomson scattered x-ray beam properties also provides a novel means of electron bunch characterization. Although the pulse duration is inferred for the Thomson scattering x-ray source, direct measurement is required for other x-ray pulse sources. A method based on the laser-assisted photoelectric effect (LAPE) has been demonstrated as a

  9. 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.

  10. Separating Peaks in X-Ray Spectra

    NASA Technical Reports Server (NTRS)

    Nicolas, David; Taylor, Clayborne; Wade, Thomas

    1987-01-01

    Deconvolution algorithm assists in analysis of x-ray spectra from scanning electron microscopes, electron microprobe analyzers, x-ray fluorescence spectrometers, and like. New algorithm automatically deconvolves x-ray spectrum, identifies locations of spectral peaks, and selects chemical elements most likely producing peaks. Technique based on similarities between zero- and second-order terms of Taylor-series expansions of Gaussian distribution and of damped sinusoid. Principal advantage of algorithm: no requirement to adjust weighting factors or other parameters when analyzing general x-ray spectra.

  11. 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.

  12. 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

  13. X-ray laser microscope apparatus

    DOEpatents

    Suckewer, Szymon; DiCicco, Darrell S.; Hirschberg, Joseph G.; Meixler, Lewis D.; Sathre, Robert; Skinner, Charles H.

    1990-01-01

    A microscope consisting of an x-ray contact microscope and an optical microscope. The optical, phase contrast, microscope is used to align a target with respect to a source of soft x-rays. The source of soft x-rays preferably comprises an x-ray laser but could comprise a synchrotron or other pulse source of x-rays. Transparent resist material is used to support the target. The optical microscope is located on the opposite side of the transparent resist material from the target and is employed to align the target with respect to the anticipated soft x-ray laser beam. After alignment with the use of the optical microscope, the target is exposed to the soft x-ray laser beam. The x-ray sensitive transparent resist material whose chemical bonds are altered by the x-ray beam passing through the target mater GOVERNMENT LICENSE RIGHTS This invention was made with government support under Contract No. De-FG02-86ER13609 awarded by the Department of Energy. The Government has certain rights in this invention.

  14. X-rays from stellar flares

    NASA Technical Reports Server (NTRS)

    Linsky, Jeffrey L.

    1991-01-01

    A summary of X-ray observations of flares on dMe, active spectroscopic binaries and young stars is presented. Consideration is given to the energy associated with the X-ray emission and its relation to other components of the flare energy budget, the time behavior of the flaring plasma as seen by the X-ray emission, and comparisons of stellar flare parameters with solar compact and two ribbon flares. Flares are easily detected when the contrast in the emission from the flaring plasma relative to the stellar photosphere is large as in the X-ray, microwave, and UV regions of the spectrum.

  15. Colloid Coalescence with Focused X Rays

    SciTech Connect

    Weon, B. M.; Kim, J. T.; Je, J. H.; Yi, J. M.; Wang, S.; Lee, W.-K.

    2011-07-01

    We show direct evidence that focused x rays enable us to merge polymer colloidal particles at room temperature. This phenomenon is ascribed to the photochemical scission of colloids with x rays, reducing the molecular weight, glass transition temperature, surface tension, and viscosity of colloids. The observation of the neck bridge growth with time shows that the x-ray-induced colloid coalescence is analogous to viscoelastic coalescence. This finding suggests a feasible protocol of photonic nanofabrication by sintering or welding of polymers, without thermal damage, using x-ray photonics.

  16. 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.

  17. An Imaging X-Ray Polarimetry Mission

    NASA Technical Reports Server (NTRS)

    Weisskopf, Martin C.; Bellazini, Ronaldo; Costa, Enrico; Ramsey, Brian; O'Dell, Steve; Tennant, Allyn; Elsner, Ronald; Pavlov, George; Matt, Girogio; Kaspi, Vicky; Coppi, Paolo; Wu, Kinwah; Siegmund, Oswald

    2008-01-01

    Technical progress both in x-ray optics and in polarization-sensitive x-ray detectors, which our groups have pioneered, enables a scientifically powerful - yet inexpensive - dedicated mission for imaging x-ray polarimetry. Such a mission is sufficiently sensitive to measure x-ray (linear) polarization for a broad range of cosmic sources --- particularly those involving neutron stars, stellar black holes, and supermassive black holes (active galactic nuclei). We describe the technical elements, discuss a mission concept, and synopsiz:e the important physical and astrophysical questions such as mission would address.

  18. An Imaging X-Ray Polarimetry Mission

    NASA Technical Reports Server (NTRS)

    Weisskopf, Martin C.; Bellazini, Ronaldo; Costa, Enrico; Ramsey, Brian; O'Dell, Steve; Elsner, Ronald; Pavlov, George; Matt, Giorgio; Kaspi, Victoria; Tennant, Allyn; Coppi, Paolo; Wu, Kinwah; Siegmund, Oswald

    2008-01-01

    Technical progress both in x-ray optics and in polarization-sensitive x-ray detectors, which our groups have pioneered, enables a scientifically powerful---yet inexpensive---dedicated mission for imaging x-ray polarimetry. Such a mission is sufficiently sensitive to measure x-ray (linear) polarization for a broad range of cosmic sources --particularly those involving neutron stars, stellar black holes, and supermassive black holes (active galactic nuclei). We describe the technical elements, discuss a mission concept, and synopsize the important physical and astrophysical questions such a mission would address.

  19. 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.

  20. Atomic and itinerant effects at the transition-metal x-ray adsorption K pre-edge exemplified in the case of V{sub 2}O{sub 3}.

    SciTech Connect

    Hansmann, P.; Haverkort, M. W.; Toschi, A.; Sangiovanni, G.; Rodolakis, F.; Rueff, J. P.; Marsi, M.; Held, K.

    2012-01-01

    X-ray absorption spectroscopy is a well-established tool for obtaining information about orbital and spin degrees of freedom in transition-metal and rare-earth compounds. For this purpose usually the dipole transitions of the L (2p to 3d) and M (3d to 4f) edges are employed, whereas higher order transitions such as quadrupolar 1s to 3d in the K edge are rarely studied in that respect. This is due to the fact that usually such quadrupolar transitions are overshadowed by dipole-allowed 1s to 4p transitions and, hence, are visible only as minor features in the pre-edge region. Nonetheless, these features carry a lot of valuable information, similar to the dipole L-edge transition, which is not accessible in experiments under pressure due to the absorption of the diamond anvil pressure cell. We recently performed a theoretical and experimental analysis of such a situation for the metal-insulator transition of (V{sub (1-x)}Cr{sub x}){sub 2}O{sub 3}. Since the importance of the orbital degrees of freedom in this transition is widely accepted, a thorough understanding of quadrupole transitions of the vanadium K pre-edge provides crucial information about the underlying physics. Moreover, the lack of inversion symmetry at the vanadium site leads to on-site mixing of vanadium 3d and 4p states and related quantum mechanical interferences between dipole and quadrupole transitions. Here we present a theoretical analysis of experimental high-resolution x-ray absorption spectroscopy at the V K pre-edge measured in partial fluorescence yield mode for single crystals. We carried out density functional as well as configuration interaction calculations in order to capture effects coming from both itinerant and atomic limits.

  1. Planetary X-rays: Relationship with solar X-rays and solar wind

    NASA Astrophysics Data System (ADS)

    Bhardwaj, A.

    Recently X-ray flares are observed from the low-latitude disk of giant planets Jupiter and Saturn in the energy range of 0.2-2 keV. These flares are found to occur in tandem with the occurrence of solar X-ray flare, when light travel time delay is accounted. These studies suggest that disk of outer planets Jupiter and Saturn acts as "diffuse mirror" for solar X-rays and that X-rays from these planets can be used to study flaring on the hemisphere of the Sun that in invisible to near-Earth space weather satellites. Also by proper modeling of the observed planetary X-rays the solar soft X-ray flux can be derived. X-ray flares are also observed on the Mars. On the other hand, X-rays from comets are produced mainly in charge exchange interaction between highly ionized heavy solar wind ions and cometary neutrals. Thus cometary X-rays provide a diagnostics of the solar wind properties. X-rays from Martian exosphere is also dominantly produced via charge exchange interaction between Martian corona and solar wind, providing proxy for solar wind. This paper provides a brief overview on the X-rays from some of the planets and comets and their connection with solar X-rays and solar wind, and how planetary X-rays can be used to study the Sun.

  2. X-Ray Imaging Study

    NASA Technical Reports Server (NTRS)

    OBrien, Susan K.; Workman, Gary L.

    1996-01-01

    The space environment in which the Space Station Freedom and other space platforms will orbit is truly a hostile environment. For example, the currently estimated integral fluence for electrons above 1 Mev at 2000 nautical miles is above 2 x 1O(exp 10) electrons/sq cm/day and the proton integral fluence is above 1 x 10(exp 9) protons/sq cm/day. At the 200 - 400 nautical miles, which is more representative of the altitude which will provide the environment for the Space Station, each of these fluences will be proportionally less; however, the data indicates that the radiation environment will obviously have an effect on structural materials exposed to the environment for long durations. The effects of this combined environment is the issue which needs to be understood for the long term exposure of structures in space. At the same time, there will be substantial potential for collisions between the space platforms and space debris. The current NASA catalogue contains over 4500 objects floating in space which are not considered payloads. This debris can have significant effects on collision with orbiting spacecraft. In order to better understand the effect of these hostile phenomena on spacecraft, several types of studies are being performed to simulate at some level the effect of the environment. In particular the study of debris clouds produced by hypervelocity impact on the various surfaces anticipated on the Space Station is very important at this point in time. The need to assess the threat of such debris clouds on space structures is an on-going activity. The Space Debris Impact facility in Building 4612 provides a test facility to monitor the types of damage produced with hypervelocity impact. These facilities are used to simulate space environmental effects from energetic particles. Flash radiography or x-ray imaging has traditionally provided such information and as such has been an important tool for recording damage in situ with the event. The proper

  3. 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

  4. X-rays from Saturn Pose Puzzles

    NASA Astrophysics Data System (ADS)

    2004-03-01

    The first clear detection of X-rays from the giant, gaseous planet Saturn has been made with NASA's Chandra X-ray Observatory. Chandra's image shows that the X-rays are concentrated near Saturn's equator, a surprising result since Jupiter's X-ray emission is mainly concentrated near the poles. Existing theories cannot easily explain the intensity or distribution of Saturn's X-rays. Chandra observed Saturn for about 20 hours in April of 2003. The spectrum, or distribution with energy of the X-rays, was found to be very similar to that of X-rays from the Sun. "This indicates that Saturn's X-ray emission is due to the scattering of solar X-rays by Saturn's atmosphere," said Jan-Uwe Ness, of the University of Hamburg in Germany and lead author of a paper discussing the Saturn results in an upcoming issue of Astronomy & Astrophysics. "It's a puzzle, since the intensity of Saturn's X-rays requires that Saturn reflects X-rays fifty times more efficiently than the Moon." The observed 90 megawatts of X-ray power from Saturn's equatorial region is roughly consistent with previous observations of the X-radiation from Jupiter's equatorial region. This suggests that both giant, gaseous planets reflect solar X-rays at unexpectedly high rates. Further observations of Jupiter will be needed to test this possibility. The weak X-radiation from Saturn's south-polar region presents another puzzle (the north pole was blocked by Saturn's rings during this observation). Saturn's magnetic field, like that of Jupiter, is strongest near the poles. X-radiation from Jupiter is brightest at the poles because of auroral activity due to the enhanced interaction of high-energy particles from the Sun with its magnetic field. Since spectacular ultraviolet polar auroras have been observed to occur on Saturn, Ness and colleagues expected that Saturn's south pole might be bright in X-rays. It is not clear whether the auroral mechanism does not produce X-rays on Saturn, or for some reason concentrates

  5. Digital X-Ray Imaging

    NASA Astrophysics Data System (ADS)

    Dance, David R.

    The use of X-ray image receptors that produce a digital image is becoming increasingly important. Possible benefits include improved dynamic range and detective quantum efficiency, improved detectability for objects of low intrinsic contrast, and reduced radiation dose. The image can be available quickly. The display is separated from the image capture so that processing and contrast adjustment are possible before the image is viewed. The availability of a digital image means ready input into PACS and opens up the possibility of computer-aided detection and classification of abnormality. Possible drawbacks of digital systems include high cost, limited high contrast resolution and the fact that their clinical value is sometimes not proven in comparison with conventional, analogue techniques. The high contrast resolution attainable with such systems is discussed and the problem of sampling limitations and aliasing considered. The properties and limitations of digital systems using computed radiography, caesium iodide plus CCDs and active matrix arrays with either caesium iodide or selenium detectors are demonstrated. Examples are given of digital systems for mammography and general radiography and their performance is demonstrated in terms of clinical assessment and measurements of the modulation transfer function and detective quantum efficiency.

  6. SMM X-ray polychromator

    NASA Technical Reports Server (NTRS)

    Strong, Keith T.; Haisch, Bernhard M. (Compiler); Lemen, James R. (Compiler); Acton, L. W.; Bawa, H. S.; Claflin, E. S.; Freeland, S. L.; Slater, G. L.; Kemp, D. L.; Linford, G. A.

    1988-01-01

    The range of observing and analysis programs accomplished with the X-Ray Polychromator (XRP) instruments during the decline of solar cycle 21 and the rise of the solar cycle 22 is summarized. Section 2 describes XRP operations and current status. This is meant as a guide on how the instrument is used to obtain data and what its capabilities are for potential users. The science section contains a series of representative abstracts from recently published papers on major XRP science topics. It is not meant to be a complete list but illustrates the type of science that can come from the analysis of the XRP data. There then follows a series of appendixes that summarize the major data bases that are available. Appendix A is a complete bibliography of papers and presentations produced using XRP data. Appendix B lists all the spectroscopic data accumulated by the Flat Crystal Spectrometer (FCS). Appendix C is a compilation of the XRP flare catalogue for events equivalent to a GOES C-level flare or greater. It lists the start, peak and end times as well as the peak Ca XIX flux.

  7. Hard X ray imaging telescope

    NASA Astrophysics Data System (ADS)

    Lubin, P.

    1990-03-01

    This final report covers the work carried out under the LLNL Contract Number B063682, Subcontractor Regents University of California at Santa Barbara. The research carried out under this contract involves the construction of a telemetry, target acquisition and guidance system, and of a light-weight gondola to house an x ray spectrometer. This work is part of the design and construction of the balloon experiment, GRATIS, which will perform the first arcminute imaging of cosmic sources in the 30 to 200 keV energy band. Observations conducted with GRATIS are expected to provide data relevant to several key problems in high energy astrophysics including the physical processes responsible for the high energy tail observed in the soft gamma-ray spectra of clusters of galaxies and the origin of both the diffuse and point source components of the gamma-ray emission from the Galactic Center. This report discusses the scientific motivations for this experiment, presents several aspects of the design and construction of the hardware components, gives an overview of the stabilized platform, and demonstrates the expected performance and sensitivity.

  8. SN X-ray Progenitor?

    NASA Technical Reports Server (NTRS)

    2008-01-01

    Identifying stars that explode, right before they explode, is a tricky proposition since the end of starlife comes swiftly: in thermonuclear deflagrations, in nuclear exhaustion, or maybe in a rapid swirling merger of two dead stellar cores. On the right in the image above is an image of the galaxy NGC 1404 taken by the UV/optical Telescope (UVOT) on the Swift observatory. The circle surrounds SN 2007on, a supernova of Type Ia produced by the explosion of a white dwarf star in a binary system. These types of supernovae are important since they are believed to be 'standard candles', events which have the same intrinsic brightness which can serve as an important yardstick to measure cosmic distances. On the left is an image of the same galaxy taken by the Chandra X-ray observatory four years before the supernova. Conspicuous in the SN source circle is a bright source in the Chandra image, believed to be emission from a compact object+normal star companion: a similar system to the supposed precursor of SN 2007on. If true this would be the first time a Type Ia supernova precursor has ever been seen. But astronomers are still debating whether the Chandra source really is the precursor or not; it seems there's a slight but significant difference in the location of the Chandra source and the supernova. Stay tuned for more developments.

  9. X-ray satellite (Rosat)

    NASA Technical Reports Server (NTRS)

    1986-01-01

    An overview of the current status of the ROSAT X-Ray satellite project is given. Areas discussed include an overview of problem areas, systems and mechanical subsystems, the electrical subsystem, power supply, data processing and transmission, the wide field camera, ground support equipment and the production scheduling. It is shown that the project is proceeding according to schedule, including the hardware production and costs. However, it is stated that estimated additional costs will exceed the plan. The previous schedule for production of the flight model will no longer be met. A modified milestone plan has been worked out with Dornier Systems. The current working schedule calls for a launch data of December 21, 1987; however, this does not take into account a 4-week buffer prior to transporting the flight model to the launch site. As of the date of this report, milestone M5 has been met. Previous problems with the gold vapor deposition on the flight model mirror due to contamination have been eliminated.

  10. Foil X-ray Mirrors

    NASA Astrophysics Data System (ADS)

    Serlemitsos, Peter J.; Soong, Yang

    1996-09-01

    Nested thin foil reflectors have made possible light weight, inexpensive and fast grazing incidence X-ray mirrors for astronomical spectroscopy over a broad band. These mirrors were developed at Goddard for the US Shuttle program and were flown on NASA's shuttleborne Astro-l mission in December 1990. Presently, the Japan/US collaborative spectroscopic mission ASCA, nearing its third year of successful operation in earth orbit, carries, four such mirrors, weighing less than 40 kg and giving total effective areas of ˜ 1200 and 420 cm2 at l and 8 keV respectively. The ˜ 420 kg observatory is the best possible example of how conical foil mirrors opened areas of research that could not have been otherwise addressed with available resources. In this paper, we will briefly review the development and performance of our first generation foil mirrors. We will also describe progress toward improving their imaging capability to prime them for use in future instruments. Such a goal is highly desirable, if not necessary for this mirror technology to remain competitive for future applications.

  11. X ray lithography in Japan

    NASA Astrophysics Data System (ADS)

    Clemens, James T.; Hill, Robert W.; Cerrina, Franco; Fuller, Gene E.; Pease, R. F.

    1991-10-01

    Integrated circuits (semiconductors) are the key components of modern computers, communication systems, consumer electronics, and the new generations of smart machines and instruments. Japan's strong position and growing influence in the manufacture of semiconductors and systems based on them is well known and well documented. Microlithography is one the most critical elements of the semiconductor manufacturing process because it determines the minimum feature size and the functional capabilities of the semiconductor. Because it is used many times in the manufacturing sequence, the quality of the microlithography process (i.e., number of defects, control for feature size, etc.) is critical in determining the yield and cost of semiconductors and hence the competitiveness of the electronics industry. At present all volume semiconductor manufacturing is done with optical UV (ultraviolet) projection lithography, twenty-year-old photographic technology which has been and is still evolving. There are many issues that limit the technical capability and cost-effectiveness of UV lithography, and thus, alternate lithographic techniques are continuously being researched and developed. X-ray lithography, which was invented in the early 1970's, holds the promise of providing higher yields in manufacturing semiconductors by virtue of enhanced process latitude, process robustness, and resolution.

  12. Hard X-ray delays

    NASA Technical Reports Server (NTRS)

    Schwartz, Richard A.

    1986-01-01

    High time resolution hard X-ray rates with good counting statistics over 5 energy intervals were obtained using a large area balloon-borne scintillation detector during the 27 June 1980 solar flare. The impulsive phase of the flare was comprised of a series of major bursts of several to several tens of seconds long. Superimposed on these longer bursts are numerous smaller approximately 0.5 to 1.0 second spikes. The time profiles for different energies were cross-correlated for the major bursts. The rapid burst decay rates and the simultaneous peaks below 120 keV both indicate a rapid electron energy loss process. Thus, the flux profiles reflect the electron acceleration/injection process. The fast rate data was obtained by a burst memory in 8 and 32 msec resolution over the entire main impulsive phase. These rates will be cross-correlated to look for short time delays and to find rapid fluctuations. However, a cursory examination shows that almost all fluctuations, down to the 5% level, were resolved with 256 msec bins.

  13. Wide field x-ray telescopes: Detecting x-ray transients/afterglows related to GRBs

    SciTech Connect

    Hudec, Rene; Pina, Ladislav; Inneman, Adolf; Gorenstein, Paul

    1998-05-16

    The recent discovery of X-ray afterglows of GRBs opens the possibility of analyses of GRBs by their X-ray detections. However, imaging X-ray telescopes in current use mostly have limited fields of view. Alternative X-ray optics geometries achieving very large fields of view have been theoretically suggested in the 70's but not constructed and used so far. We review the geometries and basic properties of the wide-field X-ray optical systems based on one- and two-dimensional lobster-eye geometry and suggest technologies for their development and construction. First results of the development of double replicated X-ray reflecting flats for use in one-dimensional X-ray optics of lobster-eye type are presented and discussed. The optimum strategy for locating GRBs upon their X-ray counterparts is also presented and discussed.

  14. X-ray methods for the chemical characterization of atmospheric aerosols

    SciTech Connect

    Jaklevic, J.M.; Thompson, A.C.

    1981-05-01

    The development and use of several x-ray methods for the chemical characterization of atmospherical aerosol particulate samples are described. These methods are based on the emission, absorption, and scattering of x-ray photons with emphasis on the optimization for the non-destructive analysis of dilute specimens. Techniques discussed include photon induced energy dispersive x-ray fluorescence, extended x-ray absorption fine structure spectroscopy using synchrotron radiation and high-rate x-ray powder diffractometry using a position-sensitive gas proportional counter. These x-ray analysis methods were applied to the measurement of the chemical compositions of size-segregated aerosol particulate samples obtained with dichotomous samplers. The advantages of the various methods for use in such measurements are described and results are presented. In many cases, the complementary nature of the analytical information obtained from the various measurements is an important factor in the characterization of the sample. For example, the multiple elemental analyses obtained from x-ray fluorescence can be used as a cross check on the major compounds observed by powder diffraction.

  15. The rotating-crystal method in femtosecond X-ray diffraction.

    PubMed

    Freyer, B; Stingl, J; Zamponi, F; Woerner, M; Elsaesser, T

    2011-08-01

    We report the first implementation of the rotating-crystal method in femtosecond X-ray diffraction. Applying a pump-probe scheme with 100 fs hard X-ray probe pulses from a laser-driven plasma source, the novel technique is demonstrated by mapping structural dynamics of a photoexcited bismuth crystal via changes of the diffracted intensity on a multitude of Bragg reflections. The method is compared to femtosecond powder diffraction and to Bragg diffraction from a crystal with stationary orientation.

  16. Diffraction leveraged modulation of X-ray pulses using MEMS-based X-ray optics

    DOEpatents

    Lopez, Daniel; Shenoy, Gopal; Wang, Jin; Walko, Donald A.; Jung, Il-Woong; Mukhopadhyay, Deepkishore

    2016-08-09

    A method and apparatus are provided for implementing Bragg-diffraction leveraged modulation of X-ray pulses using MicroElectroMechanical systems (MEMS) based diffractive optics. An oscillating crystalline MEMS device generates a controllable time-window for diffraction of the incident X-ray radiation. The Bragg-diffraction leveraged modulation of X-ray pulses includes isolating a particular pulse, spatially separating individual pulses, and spreading a single pulse from an X-ray pulse-train.

  17. A room-temperature X-ray-induced photochromic material for X-ray detection.

    PubMed

    Wang, Ming-Sheng; Yang, Chen; Wang, Guan-E; Xu, Gang; Lv, Xiang-Ying; Xu, Zhong-Ning; Lin, Rong-Guang; Cai, Li-Zhen; Guo, Guo-Cong

    2012-04-02

    A color change: X-ray-induced photochromic species are rare and can be used for detection of X-rays. A highly robust X-ray-sensitive material with the discrete structure of a metal-organic complex has been found to show both soft and hard X-ray-induced photochromism at room temperature. A new ligand-to-ligand electron-transfer mechanism was proposed to elucidate this photochromic phenomenon.

  18. The future in X-ray surveys

    NASA Astrophysics Data System (ADS)

    Hasinger, Günther

    2015-08-01

    I will chair this "Way Forward" discusson about the future in X-ray Surveys at the Focus Meeting #6Cosmological X-ray Surveys: probing the Hot and Energetic Cosmos. Participants will be R. Gilli,G. Pratt, G. Fabbiano, X. Barcons, T. Ohashi, F. Harrison.

  19. VETA-1 x ray detection system

    NASA Technical Reports Server (NTRS)

    Podgorski, W. A.; Flanagan, Kathy A.; Freeman, Mark D.; Goddard, R. G.; Kellogg, Edwin M.; Norton, T. J.; Ouellette, J. P.; Roy, A. G.; Schwartz, Daniel A.

    1992-01-01

    The alignment and X-ray imaging performance of the Advanced X-ray Astrophysics Facility (AXAF) Verification Engineering Test Article-I (VETA-I) was measured by the VETA-I X-Ray Detection System (VXDS). The VXDS was based on the X-ray detection system utilized in the AXAF Technology Mirror Assembly (TMA) program, upgraded to meet the more stringent requirements of the VETA-I test program. The VXDS includes two types of X-ray detectors: (1) a High Resolution Imager (HRI) which provides X-ray imaging capabilities, and (2) sealed and flow proportional counters which, in conjunction with apertures of various types and precision translation stages, provide the most accurate measurement of VETA-I performance. Herein we give an overview of the VXDS hardware including X-ray detectors, translation stages, apertures, proportional counters and flow counter gas supply system and associated electronics. We also describe the installation of the VXDS into the Marshall Space Flight Center (MSFC) X-Ray Calibration Facility (XRCF). We discuss in detail the design and performance of those elements of the VXDS which have not been discussed elsewhere; translation systems, flow counter gas supply system, apertures and thermal monitoring system.

  20. X-rays from intermediate mass stars

    NASA Astrophysics Data System (ADS)

    Robrade, Jan

    I will review the X-ray properties of intermediate mass stars and discuss possible X-ray generating mechanisms. Main-sequence stars of spectral type mid B to mid A neither drive sufficiently strong winds to produce shock generated X-rays, nor possess an outer convection zone to generate dynamo driven magnetic activity and coronae. Consequently they should be virtually X-ray dark and occasionally detected X-ray emission was usually attributed to undetected low-mass companions. However, in magnetic intermediate mass stars, the Ap/Bp stars, a different X-ray production mechanism may operate. It is termed the magnetically channeled wind-shock model, where the stellar wind from both hemispheres is channelled towards the equatorial plane, collides and forms a rigidly rotating disk around the star. The strong shocks of the nearly head-on wind collision as well as the existence of magnetically confined plasma in a dynamic circumstellar disk can lead to diverse X-ray phenomena. In this sense Ap/Bp stars bridge the 'classical' X-ray regimes of cool and hot stars.