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Sample records for structural x-ray powder

  1. Acemetacin cocrystal structures by powder X-ray diffraction

    Science.gov (United States)

    Bolla, Geetha

    2017-01-01

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

  2. Acemetacin cocrystal structures by powder X-ray diffraction

    Directory of Open Access Journals (Sweden)

    Geetha Bolla

    2017-05-01

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

  3. Ab initio structure determination via powder X-ray diffraction

    Indian Academy of Sciences (India)

    Unknown

    Although the method of structure completion when once the starting model is provided is ... In this article a survey of the recent development in this area is ..... The Monte Carlo method 4,9 differs from the traditional approaches as it operates in.

  4. The Crystal Structure of the Malaria Pigment Hemozoin as Elucidated by X-ray Powder Diffraction

    DEFF Research Database (Denmark)

    Straasø, Tine

    survival. Successful inhibition of hemozoin crystallization will lead to parasitic death and thus break the cycle. The aim of this thesis is to elucidate the structure of hemozoin by means of X-ray diffraction techniques. Knowledge of the structure will help facilitate intelligent drug design in the future....... As part of the project an all-in-vacuum powder diffractometer was developed, which provides data with a minimum background level and an improved signal-to-noise ratio. Moreover, the diffractometer is designed with the particular purpose of decreasing the number of parameters to be fitted. Installation...

  5. Determination of Ni(II) crystal structure by powder x-ray diffraction ...

    African Journals Online (AJOL)

    X-ray powder diffraction pattern was used to determine the length of the unit cell, “a”, the lattice structure type, and the number of atoms per unit cell of Ni(II) crystal. The “a” value was determined to be 23.66 ± 0.005 Å, particle size of 34.87 nm, volume 13.24 Å and Strain value ε = 9.8 x 10-3. The cell search on PXRD patterns ...

  6. Structure solution from powder neutron and x-ray diffraction data: getting the best of both worlds

    International Nuclear Information System (INIS)

    Hunter, B.A.

    2000-01-01

    Full text: Powder diffraction methods have traditionally been used in three main areas: phase identification and quantification, lattice parameter determination and structure refinement. Until recently structure solution has been the almost exclusive domain of single crystal diffraction methods, predominantly using x-rays. The increasing use of synchrotron and neutron sources, and the unrelenting advances in computing hardware and software means that powder methods are challenging single crystal methods as a practical method for structure solution, especially when single crystal method can not be applied. It is known that structural refinements from a known starting structure using combined X-ray and neutron data sets are capable of providing highly accurate structures. Likewise, using combined x-ray and neutron powder diffraction data in the structure solution process should also be a powerful technique, although to date no one is pursuing this methodology. This paper present examples of solutions to the problem. Namely we are using high resolution powder X-ray and neutron methods to solve the structures of molecular materials and minerals, then refining the structures using both sets of data. In this way we exploit the advantages of both methods while minimising the disadvantages. We present our solution for a small amino acid structure, a metalorganic and a mineral structure

  7. Syntheses and crystal structure determination by X-ray powder diffraction of new compounds of Benzovesamicol

    International Nuclear Information System (INIS)

    Rukiah, M.; Assaad, Th.

    2012-06-01

    The compound 2,2,2-Trifluoro-N-(1a,2,7,7 a-tetra-hydronaphtho[2,3-b]oxiren-3-yl)- acetamide, C 1 2H 1 0F 3 NO 2 , an important precursor in the preparation of benzovesamicol analogues for the diagnosis of Alzheimers disease, was prepared by the epoxidation of 5,8-dihydronaphthalene-1-amine using 3-chloroperoxybenzoic acid. The structure was determined by X-ray powder diffraction, multinuclear NMR spectroscopy and FT-IR spectroscopy. A pair of molecules form intermolecular N- H...O hydrogen bonds, involving the amino and oxirene groups, to produce a dimer.The two racemic compounds (2RS,3RS)-5-amino-3-(4-phenylpiperazin-1-yl)-1,2,3,4 tetrahydronaphthalene-2-ol, C 2 0H 2 5N 3 O, (I) and (2RS,3RS)-5-amino-3-[4-(3- methoxyphenyl)piperazin-1-yl]-1,2,3,4-tetrahydronaphthalene-2-ol, C 2 1H 2 7N 3 O 2 , (II) important benzovesamicol analogues for the diagnosis of Alzheimer's disease, have been synthesized and characterized by FT-IR, and 1 H and 13 C NMR spectroscopic analyses. The crystal structures were analyses using powder diffraction as no suitable single crystal were obtained. The two compounds are racemic mixtures of enantiomers which crystallize in the monoclinic system in a centrosymmetric space group (P21/c). Crystallography, in particular powder X-ray diffraction, was pivotal in revealing that the enantio-resolution did not succeed. In two compounds, the piperazine ring has a chair conformation, while the cyclohexene ring assumes a half-chair conformation. In (I) the crystal packing is mediated by weak contacts, principally by complementary intermolecular N--H...O hydrogen bonds that connect successive molecules into a chain. Further stabilization is provided by weak C--H...N contacts and by a weak intermolecular C--H...π interaction. While in (II), the crystal packing is dominated by intermolecular O--H...N hydrogen bonding which links molecules along the c direction. (authors)

  8. Determination of crystal structures with large known fragments directly from measured X-ray powder diffraction intensities

    International Nuclear Information System (INIS)

    Rius, J.; Miravitlles, C.

    1988-01-01

    A strategy for the determination of crystal structures with large known fragments directly from measured X-ray powder diffraction intensities is presented. It is based on the automated full-symmetry Patterson search method described by Rius and Miravitlles where the Fourier coefficients of the observed Patterson function are modified to allow the use of powder diffraction intensity data. Its application to two structures, one with simulated and one with experimental data, is shown. (orig.)

  9. Powder X-ray diffraction studies of structural and kinetic aspects of polymorphism

    International Nuclear Information System (INIS)

    Chan, F.C.

    1999-01-01

    Polymorphism is a poorly understood phenomenon that is of considerable technological interest to the pharmaceutical industry. The polymorph selected can influence the bioavailability, processing and stability of the pharmaceutical dosage form. In this study structural, kinetic and thermodynamics aspects of polymorphism and polymorphic phase transformations have been examined using powder X-ray diffraction (PXRD). The compound sulphathiazole is a well-studied model in the investigation of polymorphism and crystal growth. There are five known polymorphic forms and the structure of form V was unknown until this study. The difficulty has been that it has not been possibly to prepare crystals of appropriate size and quality for single crystal diffraction. Furthermore, structure solution from powder data for organic molecules is almost impossible. Despite the challenge the structure of sulphathiazole form V have been solved ab initio from powder data using direct methods. With 16 non-hydrogen atoms in the molecule and two molecules in the asymmetric unit, this structure represents a significant advance in terms of the complexity of an organic structure solved from PXRD data. The structural data should be invaluable for rationalizing experimental observations and the development of theoretical ideas regarding polymorphism and crystal growth. The second part of the study, has examined kinetics of polymorphic phase transformations as a function of pressure combined with temperature using real-time synchrotron PXRD. The significance of pressure arises from the fact that phase transitions can be induced in pharmaceuticals during tabletting. The phase transformation behaviour of rubidium iodide (chosen as a simple test model) has been investigated as a function of isobaric pressure at ambient and elevated temperatures. The kinetics have been characterized by using the Johnson-Melil-Avrami equation. The effect of successive cycling across the transition pressure was also

  10. Structure determination of modulated structures by powder X-ray diffraction and electron diffraction

    Czech Academy of Sciences Publication Activity Database

    Zhou, Z.Y.; Palatinus, Lukáš; Sun, J.L.

    2016-01-01

    Roč. 3, č. 11 (2016), s. 1351-1362 ISSN 2052-1553 Institutional support: RVO:68378271 Keywords : electron diffraction * incommensurate structure * powder diffraction Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 4.036, year: 2016

  11. Determination of the structure factors of a LiF powder sample by the energy dispersive x-ray diffraction

    International Nuclear Information System (INIS)

    Uno, R.; Ahtee, A.; Paakkari, T.

    1977-01-01

    The structure factors of a LiF powder sample were determined by energy dispersive x-ray diffraction in the range 9 to 25 keV, with the use of a Si(Li) solid state detector, following the method applied on GaP. Since the absorption coefficient of LiF is small at high energy, a fraction of the incident x-rays penetrates through the sample and does not contribute to the diffraction. This effect was taken into account in the determination of the structure factors. Then the structure factors generally agree, within the limit of 5 % error, with those obtained by the usual angle dispersive method, if the penetrated part of the incident beam is less than 40 %. (author)

  12. Computation of X-ray powder diffractograms of cement components ...

    Indian Academy of Sciences (India)

    Computation of X-ray powder diffractograms of cement components and its application to phase analysis and hydration performance of OPC cement. Rohan Jadhav N C Debnath. Volume 34 Issue 5 August 2011 pp 1137- ... Keywords. Portland cement; X-ray diffraction; crystal structure; characterization; Rietveld method.

  13. Crystal structure and tautomerism of Pigment Yellow 138 determined by X-ray powder diffraction and solid-state NMR

    DEFF Research Database (Denmark)

    Gumbert, Silke D.; Körbitzer, Meike; Alig, Edith

    2016-01-01

    The crystal structure of C.I. Pigment Yellow 138 was determined from X-ray powder diffraction data using real-space methods with subsequent Rietveld refinements. The tautomeric state was investigated by solid-state 1D and 2D multinuclear NMR experiments. In the crystals, the compound exhibits...... the NH-tautomer with a hydrogen atom situated at the nitrogen of the quinoline moiety. Direct evidence of the presence of the NH-tautomer is provided by 1H–14N HMQC solid-state NMR at very fast MAS. Solid-state dispersion-corrected density functional theory calculations with BLYP-D3 confirm...

  14. Structural studies of carbon nanotubes by powder x-ray diffraction at SPring-8 and KEK PF

    CERN Document Server

    Maniwa, Y; Fujiwara, A

    2003-01-01

    Powder X-ray diffraction (XRD) studies on carbon nanotubes (CNTs) using synchrotron radiation are reported. In spite of the observed broad XRD peak profiles of two-dimensional triangular (hexagonal) lattice of single-wall carbon nanotubes (SWNTs), it was shown that useful structural information, such as the tube diameter and its distribution, can be deduced from detailed analysis of the characteristic XRD patterns. In particular, powder-XRD measurements were performed to study the phase transition of encapsulated materials inside SWNTs. In the C sub 7 sub 0 -one dimensional (1D) crystals formed inside SWNTs, importance of one-dimensionality in the C sub 7 sub 0 -molecular dynamics was suggested. It was also shown that water inside SWNTs undergoes a phase transition from liquid to an ice-nanotube structure below -38degC. Conversion process from SWNT to double-wall carbon nanotube (DWNT) was also studied by XRD.

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

    Science.gov (United States)

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

    2018-01-23

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

  16. Spiral chain structure of high pressure selenium-II' and sulfur-II from powder x-ray diffraction

    International Nuclear Information System (INIS)

    Fujihisa, Hiroshi; Yamawaki, Hiroshi; Sakashita, Mami; Yamada, Takahiro; Honda, Kazumasa; Akahama, Yuichi; Kawamura, Haruki; Le Bihan, Tristan

    2004-01-01

    The structure of high pressure phases, selenium-II ' (Se-II ' ) and sulfur-II (S-II), for α-Se 8 (monoclinic Se-I) and α-S 8 (orthorhombic S-I) was studied by powder x-ray diffraction experiments. Se-II ' and S-II were found to be isostructural and to belong to the tetragonal space group I4 1 /acd, which is made up of 16 atoms in the unit cell. The structure consisted of unique spiral chains with both 4 1 and 4 3 screws. The results confirmed that the structure sequence of the pressure-induced phase transitions for the group VIb elements depended on the initial molecular form. The chemical bonds of the phases are also discussed from the interatomic distances that were obtained

  17. Solid-state structural properties of 2,4,6-trimethoxybenzene derivatives, determined directly from powder X-ray diffraction data in conjunction with other techniques

    International Nuclear Information System (INIS)

    Pan Zhigang; Xu Mingcan; Cheung, Eugene Y.; Platts, James A.; Harris, Kenneth D.M.; Constable, Edwin C.; Housecroft, Catherine E.

    2006-01-01

    Structural properties of 2,4,6-trimethoxybenzaldehyde, 2,4,6-trimethoxybenzyl alcohol and 2,4,6-trimethoxyacetophenone have been determined directly from powder X-ray diffraction data, using the direct-space Genetic Algorithm (GA) technique for structure solution followed by Rietveld refinement. Structural similarities and contrasts within this family of materials are elucidated. The work illustrates the value of utilizing information from other sources, including spectroscopic data and computational techniques, as a means of augmenting the structural knowledge established from the powder X-ray diffraction data

  18. Structure of La2Cu2O5 by high-resolution synchrotron X-ray powder diffraction

    International Nuclear Information System (INIS)

    La Placa, S.J.; Bringley, J.F.; Scott, B.A.; Cox, D.E.

    1993-01-01

    Dicopper(II) dilanthanum pentaoxide, La 2 Cu 2 O 5 , M r =484.90, orthorhombic, Pbam. At T=300 K: a=5.5490(1), b=10.4774(2), c=3.8796(1) A, V=225.557(8) A 3 , Z=2, D x =7.139 g cm -3 , λ=1.2000 A. Final R I =6.20, R p =14.6 and R wp =20.61%, 124 independent reflections observed. The structure has been refined from high-resolution synchrotron X-ray powder diffraction data using the Rietveld method. It is of the oxygen-defect perovskite type and is composed entirely of corner-shared CuO 5 square pyramids, which share oxygen vacancies forming vacancy tunnels along the c axis. The La atoms reside at a perovskite-like A-site and are tenfold coordinated by oxygen. (orig.)

  19. Solid state characterization and crystal structure from X-ray powder diffraction of two polymorphic forms of ranitidine base.

    Science.gov (United States)

    de Armas, Héctor Novoa; Peeters, Oswald M; Blaton, Norbert; Van Gyseghem, Elke; Martens, Johan; Van Haele, Gerrit; Van Den Mooter, Guy

    2009-01-01

    Ranitidine hydrochloride (RAN-HCl), a known anti-ulcer drug, is the product of reaction between HCl and ranitidine base (RAN-B). RAN-HCl has been extensively studied; however this is not the case of the RAN-B. The solid state characterization of RAN-B polymorphs has been carried out using different analytical techniques (microscopy, thermal analysis, Fourier transform infrared spectrometry in the attenuated total reflection mode, (13)C-CPMAS-NMR spectroscopy and X-ray powder diffraction). The crystal structures of RAN-B form I and form II have been determined using conventional X-ray powder diffraction in combination with simulated annealing and whole profile pattern matching, and refined using rigid-body Rietveld refinement. RAN-B form I is a monoclinic polymorph with cell parameters: a = 7.317(2), b = 9.021(2), c = 25.098(6) A, beta = 95.690(1) degrees and space group P2(1)/c. The form II is orthorhombic: a = 31.252(4), b = 13.052(2), c = 8.0892(11) A with space group Pbca. In RAN-B polymorphs, the nitro group is involved in a strong intramolecular hydrogen bond responsible for the existence of a Z configuration in the enamine portion of the molecules. A tail to tail packing motif can be denoted via intermolecular hydrogen bonds. The crystal structures of RAN-B forms are compared to those of RAN-HCl polymorphs. RAN-B polymorphs are monotropic polymorphic pairs. (c) 2008 Wiley-Liss, Inc. and the American Pharmacists Association

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

    Science.gov (United States)

    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

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

    Directory of Open Access Journals (Sweden)

    Yifeng Yun

    2015-03-01

    Full Text Available 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

  2. Preparation and Crystal Structures of Some AIVB2IIO4 Compounds: Powder X-Ray Diffraction and Rietveld Analysis

    Directory of Open Access Journals (Sweden)

    K. Jeyadheepan

    2014-01-01

    Full Text Available The AIVB2IIO4 compounds such as cadmium tin oxide (Cd2SnO4 or CTO and zinc tin oxide (Zn2SnO4 or ZTO are synthesized by solid state reaction of the subsequent binary oxides. The synthesized powders were analyzed through the powder X-ray diffraction (PXRD. Cell search done on the PXRD patterns shows that the Cd2SnO4 crystallizes in orthorhombic structure with space group Pbam and the cell parameters as a=5.568(2 Å, b=9.894(3 Å, and c=3.193(1 Å and the Zn2SnO4 crystallizes as cubic with the space group Fd3 -m and with the cell parameter a=8.660(2 Å. Rietveld refinement was done on the PXRD patterns to get the crystal structure of the Cd2SnO4 and Zn2SnO4 and to define the site deficiency of atoms which causes the electrical properties of the materials.

  3. A comparison between the Structural Results obtained by X-ray Single Crystal Data and by Neutron Powder Data for BaVs/sb3/

    International Nuclear Information System (INIS)

    Marezio, M.

    1986-01-01

    The structure of BaVs/sb3/, as refined from X-ray single-crystal data to an R factor of 0.011, is compared to the structure of the same compound obtained from neutron powder data (Rsb(ro) = 6.82, Rsb(psilon) = 4.09). As expected, the X-ray standard deviations of the positional and thermal parameters are smaller than the corresponding neutron standard deviations. However, the dynamical disorder deduced from the anomalously large thermal vibrations of the vanadium atoms obtained from the X-ray data is also evidenced by the neutron refinement. On the other hand, the neutron standard deviations of the lattice parameters are smaller than the X-ray counterparts

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

    International Nuclear Information System (INIS)

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

    1978-08-01

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

  5. A structural investigation into the compaction behavior of pharmaceutical composites using powder X-ray diffraction and total scattering analysis.

    Science.gov (United States)

    Moore, Michael D; Steinbach, Alison M; Buckner, Ira S; Wildfong, Peter L D

    2009-11-01

    To use advanced powder X-ray diffraction (PXRD) to characterize the structure of anhydrous theophylline following compaction, alone, and as part of a binary mixture with either alpha-lactose monohydrate or microcrystalline cellulose. Compacts formed from (1) pure theophylline and (2) each type of binary mixture were analyzed intact using PXRD. A novel mathematical technique was used to accurately separate multi-component diffraction patterns. The pair distribution function (PDF) of isolated theophylline diffraction data was employed to assess structural differences induced by consolidation and evaluated by principal components analysis (PCA). Changes induced in PXRD patterns by increasing compaction pressure were amplified by the PDF. Simulated data suggest PDF dampening is attributable to molecular deviations from average crystalline position. Samples compacted at different pressures were identified and differentiated using PCA. Samples compacted at common pressures exhibited similar inter-atomic correlations, where excipient concentration factored in the analyses involving lactose. Practical real-space structural analysis of PXRD data by PDF was accomplished for intact, compacted crystalline drug with and without excipient. PCA was used to compare multiple PDFs and successfully differentiated pattern changes consistent with compaction-induced disordering of theophylline as a single component and in the presence of another material.

  6. Conformational analysis of an acyclic tetrapeptide: ab-initio structure determination from X-ray powder diffraction, Hirshfeld surface analysis and electronic structure.

    Science.gov (United States)

    Das, Uday; Naskar, Jishu; Mukherjee, Alok Kumar

    2015-12-01

    A terminally protected acyclic tetrapeptide has been synthesized, and the crystal structure of its hydrated form, Boc-Tyr-Aib-Tyr-Ile-OMe·2H2O (1), has been determined directly from powder X-ray diffraction data. The backbone conformation of tetrapeptide (1) exhibiting two consecutive β-turns is stabilized by two 4 → 1 intramolecular N-H · · · O hydrogen bonds. In the crystalline state, the tetrapeptide molecules are assembled through water-mediated O-H · · · O hydrogen bonds to form two-dimensional molecular sheets, which are further linked by intermolecular C-H · · · O hydrogen bonds into a three-dimensional supramolecular framework. The molecular electrostatic potential (MEP) surface of (1) has been used to supplement the crystallographic observations. The nature of intermolecular interactions in (1) has been analyzed quantitatively through the Hirshfeld surface and two-dimensional fingerprint plot. The DFT optimized molecular geometry of (1) agrees closely with that obtained from the X-ray structure analysis. The present structure analysis of Boc-Tyr-Aib-Tyr-Ile-OMe·2H2 O (1) represents a case where ab-initio crystal structure of an acyclic tetrapeptide with considerable molecular flexibility has been accomplished from laboratory X-ray powder diffraction data. Copyright © 2015 European Peptide Society and John Wiley & Sons, Ltd.

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

    Directory of Open Access Journals (Sweden)

    Palash Sanphui

    2014-03-01

    Full Text Available 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

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

    Science.gov (United States)

    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

  9. 1-(2-furoyl)-3,3-(diphenyl)thiourea: spectroscopic characterization and structural study from X-ray powder diffraction using simulated annealing

    Energy Technology Data Exchange (ETDEWEB)

    Estevez H, O.; Duque, J. [Universidad de La Habana, Instituto de Ciencia y Tecnologia de Materiales, 10400 La Habana (Cuba); Rodriguez H, J. [UNAM, Instituto de Investigaciones en Materiales, 04510 Mexico D. F. (Mexico); Yee M, H., E-mail: oestevezh@yahoo.com [Instituto Politecnico Nacional, Escuela Superior de Fisica y Matematicas, 07738 Mexico D. F. (Mexico)

    2015-07-01

    1-Furoyl-3,3-diphenylthiourea (FDFT) was synthesized, and characterized by Ftir, {sup 1}H and {sup 13}C NMR and ab initio X-ray powder structure analysis. FDFT crystallizes in the monoclinic space group P2{sub 1} with a = 12.691(1), b = 6.026(2), c = 11.861(1) A, β = 117.95(2) and V = 801.5(3) A{sup 3}. The crystal structure has been determined from laboratory X-ray powder diffraction data using direct space global optimization strategy (simulated annealing) followed by the Rietveld refinement. The thiourea group makes a dihedral angle of 73.8(6) with the furoyl group. In the crystal structure, molecules are linked by van der Waals interactions, forming one-dimensional chains along the a axis. (Author)

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

    DEFF Research Database (Denmark)

    Oddershede, Jette; Christiansen, Thomas; Ståhl, Kenny

    2008-01-01

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

  11. Modern trends in x-ray powder diffraction

    International Nuclear Information System (INIS)

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

    1985-01-01

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

  12. Combined Approach for the Structural Characterization of Alkali Fluoroscandates: Solid-State NMR, Powder X-ray Diffraction, and Density Functional Theory Calculations.

    Science.gov (United States)

    Rakhmatullin, Aydar; Polovov, Ilya B; Maltsev, Dmitry; Allix, Mathieu; Volkovich, Vladimir; Chukin, Andrey V; Boča, Miroslav; Bessada, Catherine

    2018-02-05

    The structures of several fluoroscandate compounds are presented here using a characterization approach combining powder X-ray diffraction and solid-state NMR. The structure of K 5 Sc 3 F 14 was fully determined from Rietveld refinement performed on powder X-ray diffraction data. Moreover, the local structures of NaScF 4 , Li 3 ScF 6 , KSc 2 F 7 , and Na 3 ScF 6 compounds were studied in detail from solid-state 19 F and 45 Sc NMR experiments. The 45 Sc chemical shift ranges for six- and seven-coordinated scandium environments were defined. The 19 F chemical shift ranges for bridging and terminal fluorine atoms were also determined. First-principles calculations of the 19 F and 45 Sc NMR parameters were carried out using plane-wave basis sets and periodic boundary conditions (CASTEP), and the results were compared with the experimental data. A good agreement between the calculated shielding constants and experimental chemical shifts was obtained. This demonstrates the good potential of computational methods in spectroscopic assignments of solid-state 45 Sc NMR spectroscopy.

  13. Structural transition induced by charge-transfer in RbMn[Fe(CN) sub 6]. Investigation by synchrotron-radiation X-ray powder analysis

    CERN Document Server

    Moritomo, Y; Sakata, M; Kato, K; Kuriki, A; Tokoro, H; Ohkoshi, S I; Hashimoto, K

    2002-01-01

    Temperature dependence of atomic coordinates is determined for RbMn[Fe(CN) sub 6] by means of synchrotron-radiation (SR) X-ray powder structural analysis. We observed a structural transition from the cubic (F4-bar3m; Z=4) to the tetragonal (I4-barm2; Z=2) phase at approx. =210K in the cooling run and at approx. =300K in the warming run. In the low-temperature tetragonal phase, we found Jahn-Tellar type distortion of the MnN sub 6 octahedra and compression of the averaged Fe-C bond distance. These structural data suggest that the structural transition is triggered by the inter-metallic charge-transfer from the Mn(II) site to the Fe(III) site.

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

    Science.gov (United States)

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

    2013-07-14

    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).

  15. Fundamentals of powder x-ray diffraction practice

    International Nuclear Information System (INIS)

    Raftery, T.

    2002-01-01

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

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

    Science.gov (United States)

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

    2014-01-01

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

  17. Structure determination of β- and γ-BaAlF 5 by X-ray and neutron powder diffraction: A model for the α → β γ transitions

    Science.gov (United States)

    Le Bail, Armel; Ferey, Gérard; Mercier, Anne-Marie; De Kozak, Ariel; Samouél, Maurice

    1990-12-01

    β-BaAlF 5 is monoclinic (space group {P2 1}/{n}): a = 5.1517(1), Å, b = 19.5666(4), Å, c = 7.5567(2), Å, β = 92.426(1)°, Z = 8. γ-BaAlF 5 is monoclinic (space group P2 1): a = 5.2584(1), Å, b = 9.7298(2), Å, c = 7.3701(2), Å, β = 90.875(1)°, Z = 4. Both structures are determined ab initio from X-ray powder data; final results are given from neutron powder data refinements ( RI = 0.038, RP = 0.072, and RWP = 0.087 and RI = 0.048, RP = 0.083, and RWP = 0.101 for the β and γ phases, respectively). Like α-BaAlF 5, the β and γ phases are built up from isolated infinite (AlF 5) 2 n- n chains with AlF 6 octahedra sharing corners in a cis-position. Close structural relationships are shown to exist between the BaAl cationic subnetwork of: α-BaAlF 5 and the CrB-type structure; β-BaAlF 5 and the SrAg-type; γ-BaAlF 5 and the FeB-type. The polymorphic transitions are proposed to be topotactic and a displacive mechanism is suggested.

  18. Fourier transform infrared spectrophotometry and X-ray powder ...

    African Journals Online (AJOL)

    This study aimed at demonstrating complementary roles offered by both Fourier transform infrared (FTIR) spectrophotometry and x-ray powder diffraction (XRPD) techniques in characterizing clay size fraction of kaolins. The clay size fraction of kaolin samples obtained from Kgwakgwe, Makoro, Lobatse and Serule kaolin ...

  19. X-ray powder diffraction in forensic practice

    Czech Academy of Sciences Publication Activity Database

    Kotrlý, M.; Bezdička, Petr

    2006-01-01

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

  20. 5-Arylidene derivatives of Meldrum's acid: Synthesis, structural characterization using single crystal and powder crystal X-ray diffraction, and electronic properties

    Science.gov (United States)

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

    2015-07-01

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

  1. X-ray metrology for ULSI structures

    International Nuclear Information System (INIS)

    Bowen, D. K.; Matney, K. M.; Wormington, M.

    1998-01-01

    Non-destructive X-ray metrological methods are discussed for application to both process development and process control of ULSI structures. X-ray methods can (a) detect the unacceptable levels of internal defects generated by RTA processes in large wafers, (b) accurately measure the thickness and roughness of layers between 1 and 1000 nm thick and (c) can monitor parameters such as crystallographic texture and the roughness of buried interfaces. In this paper we review transmission X-ray topography, thin film texture measurement, grazing-incidence X-ray reflectivity and high-resolution X-ray diffraction. We discuss in particular their suitability as on-line sensors for process control

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

    Energy Technology Data Exchange (ETDEWEB)

    Brown, Allan

    1970-12-15

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

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

    International Nuclear Information System (INIS)

    Brown, Allan

    1970-12-01

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

  4. IL 12: Femtosecond x-ray powder diffraction

    International Nuclear Information System (INIS)

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

    2010-01-01

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

  5. Structural and microstructural changes during anion exchange of CoAl layered double hydroxides: an in situ X-ray powder diffraction study

    DEFF Research Database (Denmark)

    Johnsen, Rune; Krumeich, Frank; Norby, Poul

    2010-01-01

    Anion-exchange processes in cobalt-aluminium layered double hydroxides (LDHs) were studied by in situ synchrotron X-ray powder diffraction (XRPD). The processes investigated were CoAl-CO3 CoAl-Cl CoAl-CO3, CoAl-Cl CoAl-NO3 and CoAl-CO3 CoAl-SO4. The XRPD data show that the CoAl-CO3 CoAl-Cl process...

  6. X-ray powder microdiffraction for routine analysis of paintings

    Czech Academy of Sciences Publication Activity Database

    Šímová, Veronika; Bezdička, Petr; Hradilová, J.; Hradil, David; Grygar, Tomáš

    2005-01-01

    Roč. 20, č. 3 (2005), s. 224-229 ISSN 0885-7156 R&D Projects: GA MŠk(CZ) LN00A028; GA ČR GA203/04/2091; GA AV ČR KJB1032401 Institutional research plan: CEZ:AV0Z40320502 Keywords : powder X-ray microdiffraction * artwork analysis Subject RIV: CA - Inorganic Chemistry Impact factor: 0.483, year: 2005

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

    Science.gov (United States)

    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.

  8. Structural and microstructural changes during anion exchange of CoAl layered double hydroxides. An in situ X-ray powder diffraction study

    International Nuclear Information System (INIS)

    Johnsen, Rune E.; Krumeich, Frank; Norby, Poul

    2010-01-01

    Anion-exchange processes in cobalt-aluminium layered double hydroxides (LDHs) were studied by in situ synchrotron X-ray powder diffraction (XRPD). The processes investigated were CoAl-CO 3 →CoAl-Cl →CoAl-CO 3 , CoAl-Cl→CoAl-NO 3 and CoAl-CO 3 →CoAl-SO 4 . The XRPD data show that the CoAl-CO 3 →CoAl-Cl process is a two-phase transformation, where the amount of the CoAl-CO 3 phase decreases exponentially while that of the CoAl-Cl phase increases exponentially. Energy-dispersive X-ray spectroscopy (EDXS) studies of a partially chloride-exchanged CoAl-CO 3 LDH sample along with in situ XRPD data suggested that the individual particles in the CoAl-CO 3 sample are generally anion-exchanged with chloride one at a time. In contrast with the CoAl-CO 3 →CoAl-Cl transformation, the XRPD data show that the reverse CoAl-Cl→CoAl-CO 3 process is a one-phase transformation. Rietveld refinements indicate that the occupancy factors of the carbon and oxygen sites of the carbonate group increase, while that of the chloride site decreases. In the CoAl-Cl→CoAl-NO 3 anion-exchange reaction, the XRPD patterns reveal the existence of two intermediate phases in addition to the initial CoAl-Cl and final CoAl-NO 3 phases. The in situ data indicate that one of these intermediates is a mixed nitrate- and chloride-based LDH phase, where the disorder decreases as the nitrate content increases. The XRPD data of the partial CoAl-CO 3 →CoAl-SO 4 anion-exchange reaction show that the process is a two-phase transformation involving a sulfate-containing LDH with a 1H polytype structure. (orig.)

  9. Spectroscopic studies, theoretical models and structural characterization. II. Synthesis and X-ray powder diffraction of the elpasolites Cs2NaSmCl6

    International Nuclear Information System (INIS)

    Poblete, V.; Acevedo, R.

    1998-01-01

    In this research work, we report the synthesis and structural characterization of the stoichiometric elpasolite Cs 2 NaSmCl 6 . The synthesis was performed under a solid state reaction in nitrogen atmosphere from the chemicals CsCl, NaCl and SmCl 3 weighted stoichiometrically. The best possible crystallization temperature was obtained using thermal studies of the type DTA/TGA (the thermal treatment was allowed to proceed for 2.5 hours at 755 Centigrade, showing a temperature gradient of 10 Centigrade/minute). The structural characterization by powder X-ray diffraction (XDR) indicates that this elpasolite belongs to the Fm 3m (O h 5 ) space group and the optimized structural parameters are as follows: a 0 = 10.8342 Armstrong, V 1271.72 Armstrong 3 , Z=4, M=651.88, D x =3.406 y D exp=3.41 ± 0.01. The profile refinement, using the Rietveld method, allowed us to fit the experimental and the calculated intensities of a total of 32 lines. The above result indicates that the condition R exp 2+ + 3Cl -1 and the counter ions filling the octahedral holes, in full agreement with anti fluorite type crystal. According to the above description, these elpasolite adopt the form (M 1/3 □ 2/3 ) 4 X 2 , where M labels the central metal, X stand for the chlorine ions and □ represent the vacancies, which may accommodate a significant amount of defects without collapsing. This experimental study provides the necessary input to test theoretical models against experimental data. (Author)

  10. Powder X-ray diffraction study af alkali alanates

    DEFF Research Database (Denmark)

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

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

  11. Functional coordination polymers and MOFs from reactions of the lanthanides and barium with azole ligands. Synthesis and characterization with a focus on structure determination from X-ray powder diffraction data

    International Nuclear Information System (INIS)

    Rybak, Jens-Christoph

    2012-01-01

    This thesis deals with the synthesis and characterization of coordination polymers and MOFs of the lanthanides and barium with different azolic N-heterocycles. A total of 18 new organic-inorganic hybrid materials, as well as a series of co-doped compounds is presented. Besides the structural characterization of these materials from X-ray diffraction powder data, the focus of the investigations is on the thermal and photoluminescence spectroscopic properties. The lanthanides La - Lu, except Eu and Pm, can be reacted with 1H-1,2,3-triazole to give the series of the isotypic dense 3D-MOFs 3 ∞ [Ln(Tz * ) 3 ]. Investigation of the photoluminescence properties of these compounds reveals a broad range of different luminescence phenomena, including the first observation of an intrinsic inner-filter effect of the Ln 3+ -ions. The structure of this isotypic series of compounds was solved and refined from X-ray powder diffraction data. A 2D-polymorph of these compounds 2 ∞ [Ln(Tz * ) 3 ], is observed for Ln = Sm, Tb and was characterized by single crystal data. The reaction of Eu with 1H-benzotriazole yields the 1D-coordination polymer 1 ∞ [Eu(Btz) 2 (BtzH) 2 ], which is the first example of a divalent rare earth benzotriazolate. Analysis of the thermal properties reveals the transformation to the 3D-MOF 3 ∞ [Eu(Btz) 2 ] at higher temperatures. The structure of this material was also solved from X-ray powder diffraction data. Investigation of the photoluminescence properties of the co-doped compounds 3 ∞ [Ba 1-x Eu x (Im) 2 ], which were obtained from reaction of the salt-like hydrides BaH 2 and EuH 2 with imidazole, show that the synthesis of luminescent MOF materials by co-doping of non-luminescent networks with luminescence centers is possible. The structure of these materials was solved from X-ray powder diffraction data of the undoped compound 3 ∞ [BaEu(Im) 2 ]. Structural characterization of materials from X-ray powder diffraction data is an important aspect

  12. Resolution of crystal structures by X-ray and neutrons powder diffraction using global optimisation methods; Resolution des structures cristallines par diffraction des rayons X et neutrons sur poudres en utilisant les methodes d'optimisation globale

    Energy Technology Data Exchange (ETDEWEB)

    Palin, L

    2005-03-15

    We have shown in this work that X-ray diffraction on powder is a powerful tool to analyze crystal structure. The purpose of this thesis is the resolution of crystal structures by X-ray and neutrons diffraction on powder using global optimisation methods. We have studied 3 different topics. The first one is the order-disorder phenomena observed in some globular organic molecular solids. The second is the opiate family of neuropeptides. These neurotransmitters regulate sensory functions including pain and control of respiration in the central nervous system. The aim of our study was to try to determine the crystal structure of Leu-enkephalin and some of its sub-fragments. The determination of the crystal structures has been done performing Monte Carlo simulations. The third one is the location of benzene in a sodium-X zeolite. The zeolite framework was already known and the benzene has been localized by simulated annealing and by the use of maximum entropy maps.

  13. X-ray powder crystallography with vertex instrumentation

    International Nuclear Information System (INIS)

    Chatzisotiriou, V.; Christofis, I.; Dimitriou, N.; Karvelas, S.; Karydas, A.G.; Loukas, D.; Pavlidis, A.; Spirou, S.; Dre, C.; Haralabidis, N.; Misiakos, K.; Tsoi, E.; Perdikatsis, V.; Psycharis, V.; Terzis, A.; Turchetta, R.

    1998-01-01

    An X-ray Diffractometer for Powder Crystallography is described along with experimental results and future plans. This is an intermediate instrument toward a long linear array system. Three channels of a silicon microstrip detector, are the detecting elements in the present instrument. Each detector channel is followed by a VLSI readout chain, which consists of a charge preamplifier with pulse shaping circuitry, a discriminator, and a 16-bit counter. Control and data acquisition is performed with a custom made PC readout card. A motorized goniometer scans the angle range of interest. Calibration of the system is done with reference samples and data which are captured with a one-channel conventional NaI detector. (Copyright (c) 1998 Elsevier Science B.V., Amsterdam. All rights reserved.)

  14. Calculated powder x-ray diffraction data for three tantalum tungstates

    International Nuclear Information System (INIS)

    Holcombe, C.E. Jr.

    1976-11-01

    A study was made of computer-simulated powder x-ray diffraction data for Ta 22 W 4 O 67 , Ta 2 WO 8 , and Ta 16 W 18 O 94 --the three compounds in the Ta 2 O 5 --WO 3 system from 27 to 69 mole percent WO 3 . The crystal structures of Ta 2 WO 8 and one form of Ta 16 W 18 O 94 (Type B) were deduced from reported data. 8 tables

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  16. A sample holder for in-house X-ray powder diffraction studies of protein powders

    DEFF Research Database (Denmark)

    Frankær, Christian Grundahl; Harris, Pernille; Ståhl, Kenny

    2011-01-01

    A sample holder for handling samples of protein for in-house X-ray powder diffraction (XRPD) analysis has been made and tested on lysozyme. The use of an integrated pinhole reduced the background, and good signal-to-noise ratios were obtained from only 7 l of sample, corresponding to approximatel...... 2-3 mg of dry protein. The sample holder is further adaptable to X-ray absorption spectroscopy (XAS) measurements. Both XRPD and XAS at the Zn K-edge were tested with hexameric Zn insulin....

  17. Structure determination by X-ray crystallography

    CERN Document Server

    Ladd, M F C

    1995-01-01

    X-ray crystallography provides us with the most accurate picture we can get of atomic and molecular structures in crystals. It provides a hard bedrock of structural results in chemistry and in mineralogy. In biology, where the structures are not fully crystalline, it can still provide valuable results and, indeed, the impact here has been revolutionary. It is still an immense field for young workers, and no doubt will provide yet more striking develop­ ments of a major character. It does, however, require a wide range of intellectual application, and a considerable ability in many fields. This book will provide much help. It is a very straightforward and thorough guide to every aspect of the subject. The authors are experienced both as research workers themselves and as teachers of standing, and this is shown in their clarity of exposition. There are plenty of iliustrations and worked examples to aid the student to obtain a real grasp of the subject.

  18. Wavelength dispersive X-ray absorption fine structure imaging by parametric X-ray radiation

    International Nuclear Information System (INIS)

    Inagaki, Manabu; Sakai, Takeshi; Sato, Isamu; Hayakawa, Yasushi; Nogami, Kyoko; Tanaka, Toshinari; Hayakawa, Ken; Nakao, Keisuke

    2008-01-01

    The parametric X-ray radiation (PXR) generator system at Laboratory for Electron Beam Research and Application (LEBRA) in Nihon University is a monochromatic and coherent X-ray source with horizontal wavelength dispersion. The energy definition of the X-rays, which depends on the horizontal size of the incident electron beam on the generator target crystal, has been investigated experimentally by measuring the X-ray absorption near edge structure (XANES) spectra on Cu and CuO associated with conventional X-ray absorption imaging technique. The result demonstrated the controllability of the spectrum resolution of XANES by adjusting of the horizontal electron beam size on the target crystal. The XANES spectra were obtained with energy resolution of several eV at the narrowest case, which is in qualitative agreement with the energy definition of the PXR X-rays evaluated from geometrical consideration. The result also suggested that the wavelength dispersive X-ray absorption fine structure measurement associated with imaging technique is one of the promising applications of PXR. (author)

  19. Synchrotron x-ray fluorescence and extended x-ray absorption fine structure analysis

    International Nuclear Information System (INIS)

    Chen, J.R.; Gordon, B.M.; Hanson, A.L.; Jones, K.W.; Kraner, H.W.; Chao, E.C.T.; Minkin, J.A.

    1984-01-01

    The advent of dedicated synchrotron radiation sources has led to a significant increase in activity in many areas of science dealing with the interaction of x-rays with matter. Synchrotron radiation provides intense, linearly polarized, naturally collimated, continuously tunable photon beams, which are used to determine not only the elemental composition of a complex, polyatomic, dilute material but also the chemical form of the elements with improved accuracy. Examples of the application of synchrotron radiation include experiments in synchrotron x-ray fluorescence (SXRF) analysis and extended x-ray absorption fine structure (EXAFS) analysis. New synchrotron radiation x-ray microprobes for elemental analysis in the parts per billion range are under construction at several laboratories. 76 references, 24 figures

  20. Solving Crystal Structures from Powder Diffraction Data

    DEFF Research Database (Denmark)

    Christensen, A. Nørlund; Lehmann, M. S.; Nielsen, Mogens

    1985-01-01

    High resolution powder data from both neutron and X-ray (synchrotron) sources have been used to estimate the possibility of direct structure determination from powder data. Two known structures were resolved by direct methods with neutron and X-ray data. With synchrotron X-ray data, the measured ...

  1. A standardless method of quantitative ceramic analysis using X-ray powder diffraction

    International Nuclear Information System (INIS)

    Mazumdar, S.

    1999-01-01

    A new procedure using X-ray powder diffraction data for quantitative estimation of the crystalline as well as the amorphous phase in ceramics is described. Classification of the crystalline and amorphous X-ray scattering was achieved by comparison of the slopes at two successive points of the powder pattern at scattering angles at which the crystalline and amorphous phases superimpose. If the second slope exceeds the first by a stipulated value, the intensity is taken as crystalline; otherwise the scattering is considered as amorphous. Crystalline phase analysis is obtained by linear programming techniques using the concept that each observed X-ray diffraction peak has contributions from n component phases, the proportionate analysis of which is required. The method does not require the measurement of calibration data for use as an internal standard, but knowledge of the approximate crystal structure of each phase of interest in the mixture is necessary. The technique is also helpful in qualitative analysis because each suspected phase is characterized by the probability that it will be present when a reflection zone is considered in which the suspected crystalline phase could contribute. The amorphous phases are determined prior to the crystalline ones. The method is applied to ceramic materials and some results are presented. (orig.)

  2. In situ X-ray powder diffraction, synthesis, and magnetic properties of InVO 3

    Science.gov (United States)

    Lundgren, Rylan J.; Cranswick, Lachlan M. D.; Bieringer, Mario

    2006-12-01

    We report the first synthesis and high-temperature in situ X-ray diffraction study of InVO 3. Polycrystalline InVO 3 has been prepared via reduction of InVO 4 using a carbon monoxide/carbon dioxide buffer gas. InVO 3 crystallizes in the bixbyite structure in space group Ia-3 (206) with a=9.80636(31) Å with In 3+/V 3+ disorder on the (8 b) and (24 d) cation sites. In situ powder X-ray diffraction experiments and thermal gravimetric analysis in a CO/CO 2 buffer gas revealed the existence of the metastable phase InVO 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) Å. Magnetic susceptibility and neutron diffraction experiments suggest a spin-glass ground state for InVO 3.

  3. Multiscale structural study using scanning X-ray microscope

    International Nuclear Information System (INIS)

    Ohsumi, Hiroyuki; Arima, Taka-hisa

    2016-01-01

    Correspondence between structures at the atomic- and meso-scales can be given by scanning X-ray microscopy integrated with polarized X-ray diffractometry. Symmetry is the common structural feature available across multiple hierarchies. This article introduces a symmetry evaluation technique based on polarized X-ray diffractometry and describes two embodiments: chirality domain observation and antiferromagnetic domain observation. Multiscale structural studies would play an important role in uncovering universality of hierarchical structure. (author)

  4. A readout system for X-ray powder crystallography

    CERN Document Server

    Loukas, D; Pavlidis, A; Karvelas, E; Psycharis, K; Misiakos, V; Mousa, J; Dre, C

    2000-01-01

    A system for capturing and processing data, from radiation detectors, in the field of X-ray crystallography has been developed. The system includes a custom-made mixed analog-digital 16-channel VLSI circuit in 50 mu m pitch. Each channel comprises a charge amplifier, a shaper, a comparator and a 21-bit counter. The circuit can be scaled in a daisy chain configuration. Data acquisition is performed with a custom made PCI card while the control software is developed with Visual C++ under the MS Windows NT environment. Performance of a fully operational system, in terms of electronic noise, statistical variations and data capture speed is presented. The noise level permits counting of X-rays down to 8 keV while the counting capability is in excess of 200 kHz. The system is intended for X-ray crystallography with silicon detectors.

  5. Validation of missed space-group symmetry in X-ray powder diffraction structures with dispersion-corrected density functional theory.

    Science.gov (United States)

    Hempler, Daniela; Schmidt, Martin U; van de Streek, Jacco

    2017-08-01

    More than 600 molecular crystal structures with correct, incorrect and uncertain space-group symmetry were energy-minimized with dispersion-corrected density functional theory (DFT-D, PBE-D3). For the purpose of determining the correct space-group symmetry the required tolerance on the atomic coordinates of all non-H atoms is established to be 0.2 Å. For 98.5% of 200 molecular crystal structures published with missed symmetry, the correct space group is identified; there are no false positives. Very small, very symmetrical molecules can end up in artificially high space groups upon energy minimization, although this is easily detected through visual inspection. If the space group of a crystal structure determined from powder diffraction data is ambiguous, energy minimization with DFT-D provides a fast and reliable method to select the correct space group.

  6. Structure determination by X-ray crystallography

    CERN Document Server

    Ladd, M F C

    1977-01-01

    Crystallography may be described as the science of the structure of materi­ als, using this word in its widest sense, and its ramifications are apparent over a broad front of current scientific endeavor. It is not surprising, therefore, to find that most universities offer some aspects of crystallography in their undergraduate courses in the physical sciences. It is the principal aim of this book to present an introduction to structure determination by X-ray crystal­ lography that is appropriate mainly to both final-year undergraduate studies in crystallography, chemistry, and chemical physics, and introductory post­ graduate work in this area of crystallography. We believe that the book will be of interest in other disciplines, such as physics, metallurgy, biochemistry, and geology, where crystallography has an important part to play. In the space of one book, it is not possible either to cover all aspects of crystallography or to treat all the subject matter completely rigorously. In particular, certain ...

  7. Stabilization of high-temperature antimony oxide with molybdenum incorporation. Structure of Mo-doped Sb2O4 by powder neutron diffraction and extended X-ray absorption fine structure spectroscopy

    International Nuclear Information System (INIS)

    Teller, R.G.; Antonio, M.R.; Brazdil, J.F.; Mehicic, M.; Grasselli, R.K.

    1985-01-01

    It has been discovered that the presence of MoO 3 lowers the α-β transition in Sb 2 O 4 from 935 to 850 0 C with concurrent dissolution of Mo in the high-temperature (β) form. The structure of Mo-doped β-Sb 2 O 4 has been investigated by powder neutron diffraction, extended X-ray absorption fine structure (EXAFS) and Raman spectroscopies, and scanning-electron microscopy (SEM). Cell parameters: a = 12.0571 (12) A, b = 4.8335 (1) A, c = 5.3838 (6) A, β = 105.579 (5) 0 , monoclinic, space group C2/c, Z = 4. Combining the results of these techniques leads to the hypothesis that Mo is located interstitially within channels of electron density in the Sb 2 O 4 structure with concurrent vacancy of two Sb/sup III/ atoms. There is no apparent oxygen deficiency in the resulting structure. 25 references, 6 figures, 3 tables

  8. X-Ray powder diffractometry, crystallographic phase analysis and ...

    African Journals Online (AJOL)

    Computerized X-Ray diffraction system has been used to determine the composition and lattice parameters of raw and activated kaolinite. The universal diffractometry URD 63 was interfaced with computer via an APX 63 software package for rapid capturing of data on reflected intensity and other crystallographic ...

  9. X-ray mapping in heterocyclic design: IV. Crystal structure determination of 3-(p-nitrobenzoyl)-2-oxooxazolo[3,2-a]pyridine from powder diffraction data

    International Nuclear Information System (INIS)

    Rybakov, V.B.; Zhukov, S.G.; Babaev, E.V.; Sonneveld, E.J.

    2001-01-01

    The structure of 3-(p-nitrobenzoy)-2-oxooxazolo[3,2-a]pyridine is determined by the powder diffraction technique. The crystals are monoclinic, a = 13.642(2) A, b = 22.278(3) A, c = 3.917(1) A, β = 90.63(2) deg., Z 4, and space group P2 1 /n. The structure is solved by a modified Monte Carlo method and refined by the Reitveld method. The six-membered heterocycle is characterized by the alternation of partially single and partially double bonds. The system of two conjugated heterocycles is planar and forms a dihedral angle of 46.1(1) deg. with the plane of the phenyl ring. The nitro group is virtually coplanar with the phenyl fragment. An extensive system of intramolecular and intermolecular contacts involving hydrogen, oxygen, and nitrogen atoms is observed in the crystal

  10. In Situ High Resolution Synchrotron X-Ray Powder Diffraction Studies of Lithium Batteries

    DEFF Research Database (Denmark)

    Amri, Mahrez; Fitch, Andy; Norby, Poul

    2015-01-01

    allowing diffraction information to be obtained from only the active material during battery operation [2]. High resolution synchrotron x-ray powder diffraction technique has been undertaken to obtain detailed structural and compositional information during lithiation/delithiation of commercial LiFePO4...... materials [3]. We report results from the first in situ time resolved high resolution powder diffraction experiments at beamline ID22/31 at the European Synchrotron Radiation Facility, ESRF. We follow the structural changes during charge of commercial LiFePO4 based battery materials using the Rietveld...... method. Conscientious Rietveld analysis shows slight but continuous deviation of lattice parameters from those of the fully stoichiometric end members LiFePO4 and FePO4 indicating a subsequent variation of stoichiometry during cathode delithiation. The application of an intermittent current pulses during...

  11. Qualitative analysis of powder x-ray diffraction data

    International Nuclear Information System (INIS)

    Raftery, T.

    1999-01-01

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

  12. ENDIX. A computer program to simulate energy dispersive X-ray and synchrotron powder diffraction diagrams

    International Nuclear Information System (INIS)

    Hovestreydt, E.; Karlsruhe Univ.; Parthe, E.; Benedict, U.

    1987-01-01

    A Fortran 77 computer program is described which allows the simulation of energy dispersive X-ray and synchrotron powder diffraction diagrams. The input consists of structural data (space group, unit cell dimensions, atomic positional and displacement parameters) and information on the experimental conditions (chosen Bragg angle, type of X-ray tube and applied voltage or operating power of synchrotron radiation source). The output consists of the normalized intensities of the diffraction lines, listed by increasing energy (in keV), and of an optional intensity-energy plot. The intensities are calculated with due consideration of the wave-length dependence of both the anomalous dispersion and the absorption coefficients. For a better agreement between observed and calculated spectra provision is made to optionally superimpose, on the calculated diffraction line spectrum, all additional lines such as fluorescence and emission lines and escape peaks. The different effects which have been considered in the simulation are discussed in some detail. A sample calculation of the energy dispersive powder diffraction pattern of UPt 3 (Ni 3 Sn structure type) is given. Warning: the user of ENDIX should be aware that for a successful application it is necessary to adapt the program to correspond to the actual experimental conditions. Even then, due to the only approximately known values of certain functions, the agreement between observed and calculated intensities will not be as good as for angle dispersive diffraction methods

  13. Hard X-ray irradiation of cosmic silicate analogs: structural evolution and astrophysical implications

    Science.gov (United States)

    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

  14. Elemental investigation of talcum baby powder by X-Ray florescence and fast neutron activation Techniques

    International Nuclear Information System (INIS)

    Hassan, M. F.; Abd El Wahab, M.; Nada, A.

    2008-01-01

    Different samples of Egyptian and Hungarian talcum powders were studied, using X-ray florescence (XRF) and Fast Neutron Activation Analysis (FNAA) techniques to ensure the safety of its use. The K (X-rays) and the gamma-rays were measured, using Si(Li) and high-purity germanium (HPGe) spectrometers to detect and determine qualitatively and quantitatively the constituents of the studied samples. The concentrations of the elements (Mg, Si, Al, Fe, Zn, and Ba) were measured and their presence was confirmed by X-ray, lifetime and/or XRF measurements. One of these samples was also studied, using the Environmental Scanning Electron Microscope (ESEM)

  15. Soft x-ray resonant magnetic powder diffraction on PrNiO{sub 3}

    Energy Technology Data Exchange (ETDEWEB)

    Staub, U [Swiss Light Source, Paul Scherrer Institut, CH-5232 Villigen PSI (Switzerland); GarcIa-Fernandez, M [Swiss Light Source, Paul Scherrer Institut, CH-5232 Villigen PSI (Switzerland); Mulders, A M [Department of Applied Physics, Curtin University of Technology, GPO Box U1987, Perth WA 6845 (Australia); Bodenthin, Y [Swiss Light Source, Paul Scherrer Institut, CH-5232 Villigen PSI (Switzerland); MartInez-Lope, M J [Instituto de Ciencia de Materiales de Madrid, CSIC, Cantoblanco, E-28049 Madrid (Spain); Alonso, J A [Instituto de Ciencia de Materiales de Madrid, CSIC, Cantoblanco, E-28049 Madrid (Spain)

    2007-03-07

    We report on the first soft x-ray resonant powder diffraction experiments performed at the Ni L{sub 2,3} edges of PrNiO{sub 3}. The temperature, polarization and energy dependence of the (1/2 0 1/2) reflection indicates a magnetic origin for the signal. This experiment demonstrates that x-ray resonant magnetic powder diffraction can be relatively easily performed in the soft x-ray regime due to the very large enhancement factors at the absorption edges. Such experiments allow us to extract important information on the electronic states of the d shell. Similar results can be anticipated from orbital reflections measured in a powder. (fast track communication)

  16. X-ray structure analysis of soil compositions

    International Nuclear Information System (INIS)

    Tillaev, T.; Kalonov, M.; Kuziev, Sh.; Khatamov, Sh.; Suvanov, M.

    1998-01-01

    The analytic characteristics of techniques developed to analyse soil structure by means of X-ray diffraction method are presented. Presence of 8 minerals in Fergana valley soils have been established. It is shown that X-ray structure analysis of soils gives rise to new original possibilities to determine not only their structure but also quantative content and type of chemical compound of element in soil. (author)

  17. 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.

    Science.gov (United States)

    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. Copyright 2010 Elsevier B.V. All rights reserved.

  18. Combined experimental powder X-ray diffraction and DFT data to obtain the lowest energy molecular conformation of friedelin

    International Nuclear Information System (INIS)

    Oliveira, Djalma Menezes de; Mussel, Wagner da Nova; Duarte, Lucienir Pains; Silva, Gracia Divina de Fatima; Duarte, Helio Anderson; Gomes, Elionai Cassiana de Lima; Guimaraes, Luciana; Vieira Filho, Sidney A.

    2012-01-01

    Friedelin molecular conformers were obtained by Density Functional Theory (DFT) and by ab initio structure determination from powder X-ray diffraction. Their conformers with the five rings in chair-chair-chair-boat-boat, and with all rings in chair, are energy degenerated in gas-phase according to DFT results. The powder diffraction data reveals that rings A, B and C of friedelin are in chair, and rings D and E in boat-boat, conformation. The high correlation values among powder diffraction data, DFT and reported single crystal data indicate that the use of conventional X-ray diffractometer can be applied in routine laboratory analysis in the absence of a single-crystal diffractometer. (author)

  19. Combined experimental powder X-ray diffraction and DFT data to obtain the lowest energy molecular conformation of friedelin

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Djalma Menezes de; Mussel, Wagner da Nova; Duarte, Lucienir Pains; Silva, Gracia Divina de Fatima; Duarte, Helio Anderson; Gomes, Elionai Cassiana de Lima [Universidade Federal de Minas Gerais (UFMG), Belo Horizonte, MG (Brazil). Dept. de Quimica; Guimaraes, Luciana [Universidade Federal de Sao Joao Del-Rei (UFSJ), MG (Brazil). Dept. de Ciencias Naturais; Vieira Filho, Sidney A., E-mail: bibo@ef.ufop.br [Universidade Federal de Ouro Preto (UFOP), MG (Brazil). Dept. de Farmacia

    2012-07-01

    Friedelin molecular conformers were obtained by Density Functional Theory (DFT) and by ab initio structure determination from powder X-ray diffraction. Their conformers with the five rings in chair-chair-chair-boat-boat, and with all rings in chair, are energy degenerated in gas-phase according to DFT results. The powder diffraction data reveals that rings A, B and C of friedelin are in chair, and rings D and E in boat-boat, conformation. The high correlation values among powder diffraction data, DFT and reported single crystal data indicate that the use of conventional X-ray diffractometer can be applied in routine laboratory analysis in the absence of a single-crystal diffractometer. (author)

  20. Structure of polysaccharide and structural analysis by x-ray

    International Nuclear Information System (INIS)

    Yuguchi, Yoshiaki

    2010-01-01

    Polysaccharides occur in plants and the living body in the solid, gel, or liquid. They have a highly structural diversity and possess the potential to be used for development of new materials and energy sources. So it is very important to understand their molecular structure under various conditions. This review introduces the structural characteristics of polysaccharides and the examples of their analysis by the X-ray scattering method. (author)

  1. Combining selective sequential extractions, X-Ray Absorption Spectroscopy, and X-Ray Powder Diffraction for Cu (II speciation in soil and mineral phases

    Directory of Open Access Journals (Sweden)

    Tatiana Minkina

    2017-04-01

    Full Text Available Interaction of Cu (II ions with the matrix of soil and mineral phases of layered silicates was assessed by the Miller method of selective sequential fractionation and a set of synchrotron X-ray methods, including X-ray powder diffraction (XRD and X-ray absorption spectroscopy (XANES. It was shown that the input of Cu into Calcic Chernozem in the form of monoxide (CuO and salt (Cu(NO32 affected the transformation of Cu compounds and their affinity for metal-bearing phases. It was found that the contamination of soil with a soluble Cu(II salt increased the bioavailability of the metal and the role of organic matter and Fe oxides in the fixation and retention of Cu. During the incubation of soil with Cu monoxide, the content of the metal in the residual fractions increased, which was related to the possible entry of Cu in the form of isomorphic impurities into silicates, as well as to the incomplete dissolution of exogenic compounds at the high level of their input into the soil. A mechanism for the structural transformation of minerals was revealed, which showed that ion exchange processes result in the sorption of Cu (II ions from the saturated solution by active sites on the internal surface of the lattice of dioctahedral aluminosilicates. Surface hydroxyls at the octahedral aluminum atom play the main role. X-ray diagnostics revealed that excess Cu(II ions are removed from the system due to the formation and precipitation of coarsely crystalline Cu(NO3(OH3.

  2. Structure in galactic soft X-ray features

    International Nuclear Information System (INIS)

    Davelaar, J.

    1979-01-01

    Observations are described of the soft X-ray background in a part of the northern hemisphere in the energy range 0.06 - 3.0 keV. The X-ray instruments, placed onboard a sounding rocket, are a one-dimensional focusing collector with multi-cell proportional counters in the focal plane and eight large area counters on deployable panels. A description of the instruments and their preflight calibration is given. Precautions were taken to prevent UV sensitivity of the X-ray instruments. The observation program, which consisted of a number of pre-programmed slow scans, is outlined. The spectral date on the soft X-ray background in these and previous observations showed that at least two components of different temperature are present. A low temperature component of approximately (3-10)x10 5 is found all over the sky. Components of higher temperature approximately 3x10 6 K are found in regions of soft X-ray enhancement; The North Polar Spur has been observed in two scans at the galactic latitude b=25 0 and b=75 0 . The X-ray ridge structure is found to be strongly energy dependent. The low energy data ( 0 reveals two separate emission features on the ridge, both probably of finite extensions (approximately equal to 0 0 .5). A wider X-ray ridge (approximately equal to 10 0 ) is observed above 0.4 keV. (Auth.)

  3. X-ray structural analysis of plasma sprayed europium oxide

    Energy Technology Data Exchange (ETDEWEB)

    Gorshkov, B.N.; Loskutov, V.S.; Gavrish, A.A.; Shakh, G.E.

    1981-12-01

    An X-ray structure microanalysis is made for europium oxide powder produced by sintering and plasmic spheroidization for plasma spraying. The technique of concern is shown not to alter chemical composition of the powder. It is stated that a rise in the plasma jet enthalpy while spraying does not result in dissociation of europium oxide and its interaction with the plasma flux. The coating (to 15.2 kWxs/g) is found to have only a high-temperature (monoclinic) europium oxide phase and there appears a low-temperature (cubic) phase with a subsequent increase in the enthalpy. The plasma jet enthalpy increasing the grain size and the crystal lattice c parameter of the sprayed europium oxide are shown to decrease; the a parameter reduces with an enthalpy growth to 16.2 kW s/g and then smoothly increases with the enthalpy further growth. It is noticed that the europium oxide coating does not interact with an aluminium D16 alloy substrate.

  4. A laboratory-based hard x-ray monochromator for high-resolution x-ray emission spectroscopy and x-ray absorption near edge structure measurements

    Energy Technology Data Exchange (ETDEWEB)

    Seidler, G. T., E-mail: seidler@uw.edu; Mortensen, D. R.; Remesnik, A. J.; Pacold, J. I.; Ball, N. A.; Barry, N.; Styczinski, M.; Hoidn, O. R. [Physics Department, University of Washington, Seattle, Washington 98195-1560 (United States)

    2014-11-15

    We report the development of a laboratory-based Rowland-circle monochromator that incorporates a low power x-ray (bremsstrahlung) tube source, a spherically bent crystal analyzer, and an energy-resolving solid-state detector. This relatively inexpensive, introductory level instrument achieves 1-eV energy resolution for photon energies of ∼5 keV to ∼10 keV while also demonstrating a net efficiency previously seen only in laboratory monochromators having much coarser energy resolution. Despite the use of only a compact, air-cooled 10 W x-ray tube, we find count rates for nonresonant x-ray emission spectroscopy comparable to those achieved at monochromatized spectroscopy beamlines at synchrotron light sources. For x-ray absorption near edge structure, the monochromatized flux is small (due to the use of a low-powered x-ray generator) but still useful for routine transmission-mode studies of concentrated samples. These results indicate that upgrading to a standard commercial high-power line-focused x-ray tube or rotating anode x-ray generator would result in monochromatized fluxes of order 10{sup 6}–10{sup 7} photons/s with no loss in energy resolution. This work establishes core technical capabilities for a rejuvenation of laboratory-based hard x-ray spectroscopies that could have special relevance for contemporary research on catalytic or electrical energy storage systems using transition-metal, lanthanide, or noble-metal active species.

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

    Science.gov (United States)

    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.

  6. Synthesis and X-ray Powder Structure of a New Pillared Layered Cadmium Phosphonate, Giving Evidence that the Intercalation of Alkylamines into Cd(O(3)PR).H(2)O Is Topotactic.

    Science.gov (United States)

    Fredoueil, Florence; Massiot, Dominique; Janvier, Pascal; Gingl, Franz; Bujoli-Doeuff, Martine; Evain, Michel; Clearfield, Abraham; Bujoli, Bruno

    1999-04-19

    A new pillared layered phosphonate, cadmium 2-aminoethylphosphonate, Cd(O(3)PC(2)H(4)NH(2)) (1), has been synthesized, and its structure was solved ab initio from X-ray powder diffraction data and refined by Rietveld methods. Compound 1 is orthorhombic: space group Pna2(1), a = 15.4643(2) Å, b = 5.16512(7) Å, c = 6.27650(8) Å, and Z = 4. Its layer arrangement is similar to that in Cd(O(3)PR).H(2)O, except that the water molecule coordinated to cadmium in Cd(O(3)PR).H(2)O is replaced by the nitrogen atom from the amino ends of the ethyl chains borne by phosphorus of the upper and lower layers. The strong similarity of the IR, (31)P, and (113)Cd NMR data for Cd(O(3)PC(2)H(4)NH(2)) and Cd(O(3)PCH(3)).n-NH(2)C(4)H(9) clearly shows the topotactic character of the intercalation of n-alkylamines in the dehydrated form of Cd(O(3)PR).H(2)O to yield Cd(O(3)PR).n-NH(2)R'.

  7. Qualitative analysis of a powdered diamond sample by particle induced X-ray emission (PIXE)

    International Nuclear Information System (INIS)

    Mabida, C.; Annegarn, H.J.; Renan, M.J.; Sellschop, J.P.F.

    The main purpose of this analysis was to determine whether nickel is present in diamond powder as a trace element. Particle induced X-ray emission (PIXE) showed unambiguously that nickel was present. Due to the convenience of PIXE in multielemental analysis, the investigations also include a number of other trace elements in the sample

  8. X-ray powder microdiffraction in the analysis of art works

    Czech Academy of Sciences Publication Activity Database

    Šímová, Veronika; Bezdička, Petr; Hradilová, J.; Bayerová, T.; Hradil, David

    2004-01-01

    Roč. 11, 1a (2004), s. 43 ISSN 1211-5894. [European Powder Diffraction Conference /9./. Prague, 02.09.2004-05.09.2004] R&D Projects: GA MŠk LN00A028; GA ČR GA203/04/2091; GA AV ČR KJB1032401 Institutional research plan: CEZ:AV0Z4032918 Keywords : X-ray powder microdiffraction * pigments * colour layers of artworks Subject RIV: CA - Inorganic Chemistry

  9. Thermal expansion and phase transformation studies on some materials by high temperature x-ray powder diffractometry

    International Nuclear Information System (INIS)

    Rajagopalan, S.; Kutty, K.V.G.; Jajoo, H.K.; Ananthakrishnan, S.K.; Asurvatharaman, R.

    1988-01-01

    A high temperature chamber based on electrical resistance heating has been integrated to an existing x-ray powder diffractometer. The system is capable of going upto 2500degC at programmed rates of heating. Temperature measurement is carried out by means by Pt/Rh or W/Re thermocouples or by optical pyrometry depending upon the temperature range. Provision exists for performing high temperature x-ray diffractometry in vacuum or in a gaseous atmosphere of low x-ray absorption. The x-ray optical alignment has been ensured by accurately measuring the unit cell lengths of x-ray diffraction standards like silicon and tungsten. The thermocouples have been calibrated within the system by monitoring the melting points of gold and silver. The well characterized transformation of zirconia from the monoclinic to tetragonal structure occuring around 1100degC has been satisfactorily reproduced . The high temperature phase transitions in some rare earth oxides have been studi ed. lattice parameter measurements on a variety of materials as a function of temperature upto 1500degC have been carried out and the data found to be in agreement with the literature values. From the measured lattice parameter values, percentage thermal expansion and coefficients of thermal expansion have been calculated for many substances from room temperature to 15000degC. (author). 20 refs., 9 figs

  10. Application of powder X-ray diffraction in studying the compaction behavior of bulk pharmaceutical powders.

    Science.gov (United States)

    Bandyopadhyay, Rebanta; Selbo, Jon; Amidon, Gregory E; Hawley, Michael

    2005-11-01

    This study investigates the effects of crystal lattice deformation on the powder X-ray diffraction (PXRD) patterns of compressed polycrystalline specimen (compacts/tablets) made from molecular, crystalline powders. The displacement of molecules and the corresponding adjustment of interplanar distances (d-spacings) between diffracting planes of PNU-288034 and PNU-177553, which have crystal habits with a high aspect ratio favoring preferred orientation during tableting, are demonstrated by shifts in the diffracted peak positions. The direction of shift in diffracted peak positions suggests a reduction of interplanar d-spacing in the crystals of PNU-288034 and PNU-177553 following compaction. There is also a general reduction of peak intensities following compression at the different compressive loads. The lattice strain representing the reduction in d-spacing is proportional to the original d-spacing of the uncompressed sample suggesting that, as with systems that obey a simple Hooke's law relationship, the further apart the planes of atoms/molecules within the lattice are, the easier it is for them to approach each other under compressive stresses. For a third model compound comprising more equant-shaped crystals of PNU-141659, the shift in diffracted peak positions are consistent with an expansion of lattice spacing after compression. This apparent anomaly is supported by the PXRD studies of the bulk powder consisting of fractured crystals where also, the shift in peak position suggests expansion of the lattice planes. Thus the crystals of PNU-141659 may be fracturing under the compressive loads used to produce the compacts. Additional studies are underway to relate the PXRD observations with the bulk tableting properties of these model compounds.

  11. Validation of missed space-group symmetry in X-ray powder diffraction structures with dispersion-corrected density functional theory

    DEFF Research Database (Denmark)

    Hempler, Daniela; Schmidt, Martin U.; Van De Streek, Jacco

    2017-01-01

    More than 600 molecular crystal structures with correct, incorrect and uncertain space-group symmetry were energy-minimized with dispersion-corrected density functional theory (DFT-D, PBE-D3). For the purpose of determining the correct space-group symmetry the required tolerance on the atomic...... with missed symmetry were investigated by dispersion-corrected density functional theory. In 98.5% of the cases the correct space group is found....

  12. Reflection-mode x-ray powder diffraction cell for in situ studies of electrochemical reactions

    International Nuclear Information System (INIS)

    Roberts, G.A.; Stewart, K.D.

    2004-01-01

    The design and operation of an electrochemical cell for reflection-mode powder x-ray diffraction experiments are discussed. The cell is designed for the study of electrodes that are used in rechargeable lithium batteries. It is designed for assembly in a glove box so that air-sensitive materials, such as lithium foil electrodes and carbonate-based electrolytes with lithium salts, can be used. The cell uses a beryllium window for x-ray transmission and electrical contact. A simple mechanism for compressing the electrodes is included in the design. Sample results for the cell are shown with a Cu Kα source and a position-sensitive detector

  13. X-ray diffraction microstructural analysis of bimodal size distribution MgO nano powder

    International Nuclear Information System (INIS)

    Suminar Pratapa; Budi Hartono

    2009-01-01

    Investigation on the characteristics of x-ray diffraction data for MgO powdered mixture of nano and sub-nano particles has been carried out to reveal the crystallite-size-related microstructural information. The MgO powders were prepared by co-precipitation method followed by heat treatment at 500 degree Celsius and 1200 degree Celsius for 1 hour, being the difference in the temperature was to obtain two powders with distinct crystallite size and size-distribution. The powders were then blended in air to give the presumably bimodal-size- distribution MgO nano powder. High-quality laboratory X-ray diffraction data for the powders were collected and then analysed using Rietveld-based MAUD software using the lognormal size distribution. Results show that the single-mode powders exhibit spherical crystallite size (R) of 20(1) nm and 160(1) nm for the 500 degree Celsius and 1200 degree Celsius data respectively with the nano metric powder displays narrower crystallite size distribution character, indicated by lognormal dispersion parameter of 0.21 as compared to 0.01 for the sub-nano metric powder. The mixture exhibits relatively more asymmetric peak broadening. Analysing the x-ray diffraction data for the latter specimen using single phase approach give unrealistic results. Introducing two phase models for the double-phase mixture to accommodate the bimodal-size-distribution characteristics give R = 100(6) and σ = 0.62 for the nano metric phase and R = 170(5) and σ= 0.12 for the σ sub-nano metric phase. (author)

  14. Clarithromycin monohydrate: a synchrotron X-ray powder study

    Directory of Open Access Journals (Sweden)

    Shigeru Itai

    2012-03-01

    Full Text Available In the crystal structure of the title compound, clarithromycin (CAM monohydrate, C38H69NO13·H2O, the water molecule behaves as a proton donor and is hydrogen bonded to the hydroxy O atom of the CAM cladinose ring. The hydroxy O atom also behaves as a proton donor, forming an intermolecular hydrogen bond with one of the hydroxy groups of the 14-membered aglycone ring. The CAM molecules are linked through these hydrogen bonds into chains running parallel to the c axis.

  15. Characterisation of microfocused beam for synchrotron powder diffraction using a new X-ray camera

    International Nuclear Information System (INIS)

    Thomas, C; Potter, J; Tang, C C; Lennie, A R

    2012-01-01

    The powder diffraction beamline I11, Diamond Light Source, is being continually upgraded as requirements of the user community evolve. Intensities of X-rays from the I11 in-vacuum electron undulator in the 3 GeV synchrotron fall off at higher energies. By focusing higher energy X-rays, we can overcome flux limitations, and open up new diffraction experiments. Here, we describe characterisation of microfocusing using compound refractive lenses (CRL). For a relatively modest outlay, we have developed an experimental setup and a novel X-ray camera with good sensitivity and a resolution specification suitable for characterising these focusing optics. We show that vertical oscillations in the focused beam compromise resolution of the source imaged by the CRL. Nevertheless, we have measured CRL focusing properties, and demonstrate the use of energy scanning to determine lens alignment. Real benefits of the intensity gain are illustrated.

  16. About some practical aspects of X-ray diffraction : From powder to thin film

    Energy Technology Data Exchange (ETDEWEB)

    Valvoda, V [Charles Univ. Prague (Czech Republic). Faculty of Mathematics and Physics

    1996-09-01

    Structure of thin films can be amorphous, polycrystalline or epitaxial, and the films can be prepared as a single layer films, multilayers or as graded films. A complete structure analysis of thin films by means of X-ray diffraction (XRD) usually needs more than one diffraction geometry to be used. Their principles, advantages and disadvantages will be shortly described, especially with respect to their different sampling depth and different response to orientation of diffracting crystallographic planes. Main differences in structure of thin films with respect to powder samples are given by a singular direction of their growth, by their adhesion to a substrate and often also by a simultaneous bombardment by atomic species during the growth. It means that a thermodynamically unstable atomic structures can be found too. These special features of growth of thin polycrystalline films are reflected in often found strong preferred orientation of grains and in residual stresses conserved in the films. The methods of structure analysis of thin films by XRD will be compared with other techniques which can supply structure images on different scales.

  17. High-pressure powder X-ray diffraction at the turn of the century

    International Nuclear Information System (INIS)

    Paszkowicz, W.

    2002-01-01

    Studies at extreme pressures and temperatures are helpful for understanding the physical properties of the solid state, including such classes of materials as semiconductors, superconductors or minerals. This is connected with the opportunity of tuning the pressure by many orders of magnitude. Diamond-anvil and large-anvil pressure cells installed at dedicated synchrotron beamlines are efficient tools for examination of crystal structure, equation of state, compressibility and phase transitions. One of basic methods in such studies is powder diffraction. This review is devoted to methods of powder X-ray diffraction at high-pressures generated by devices installed at synchrotron radiation sources, in particular to the principles of operation of high-pressure-high-temperature cells. General information on high-pressure diffraction facilities installed at 11 synchrotron storage rings in the world is provided. Measurement aspects are considered, including (i) pressure generation and calibration, (ii) strain in the sample, the pressure marker and the pressure-transmitting medium and (iii) pressure and temperature distributions within the cells. Sources of interest in high-pressure diffraction studies (design of new materials, observation of new phenomena, confrontation of theory with experiment) are briefly discussed. Recent developments of high-pressure methods make that pressure becomes a variable playing a key role in investigation of condensed matter. The paper ends with some remarks on the possible future developments of the technique

  18. Evaluation of high packing density powder X-ray screens by Monte Carlo methods

    International Nuclear Information System (INIS)

    Liaparinos, P.; Kandarakis, I.; Cavouras, D.; Kalivas, N.; Delis, H.; Panayiotakis, G.

    2007-01-01

    Phosphor materials are employed in intensifying screens of both digital and conventional X-ray imaging detectors. High packing density powder screens have been developed (e.g. screens in ceramic form) exhibiting high-resolution and light emission properties, and thus contributing to improved image transfer characteristics and higher radiation to light conversion efficiency. For the present study, a custom Monte Carlo simulation program was used in order to examine the performance of ceramic powder screens, under various radiographic conditions. The model was developed using Mie scattering theory for the description of light interactions, based on the physical characteristics (e.g. complex refractive index, light wavelength) of the phosphor material. Monte Carlo simulations were carried out assuming: (a) X-ray photon energy ranging from 18 up to 49 keV, (b) Gd 2 O 2 S:Tb phosphor material with packing density of 70% and grain size of 7 μm and (c) phosphor thickness ranging between 30 and 70 mg/cm 2 . The variation of the Modulation Transfer Function (MTF) and the Luminescence Efficiency (LE) with respect to the X-ray energy and the phosphor thickness was evaluated. Both aforementioned imaging characteristics were shown to take high values at 49 keV X-ray energy and 70 mg/cm 2 phosphor thickness. It was found that high packing density screens may be appropriate for use in medical radiographic systems

  19. X-ray structure based evaluation of analogs of citalopram

    DEFF Research Database (Denmark)

    Topiol, Sid; Bang-Andersen, Benny; Sanchez, Connie

    2017-01-01

    The recent publication of X-ray structures of SERT includes structures with the potent antidepressant S-Citalopram (S-Cit). Earlier predictions of ligand binding at both a primary (S1) and an allosteric modulator site (S2), were confirmed. We provide herein examples of a series of Citalopram anal...

  20. Mixed-linker UiO-66: structure-property relationships revealed by a combination of high-resolution powder X-ray diffraction and density functional theory calculations.

    Science.gov (United States)

    Taddei, Marco; Tiana, Davide; Casati, Nicola; van Bokhoven, Jeroen A; Smit, Berend; Ranocchiari, Marco

    2017-01-04

    The use of mixed-linker metal-organic frameworks (MIXMOFs) is one of the most effective strategies to modulate the physical-chemical properties of MOFs without affecting the overall crystal structure. In many instances, MIXMOFs have been recognized as solid solutions, with random distribution of ligands, in agreement with the empirical rule known as Vegard's law. In this work, we have undertaken a study combining high-resolution powder X-ray diffraction (HR-PXRD) and density functional theory (DFT) calculations with the aim of understanding the reasons why UiO-66-based amino- and bromo-functionalized MIXMOFs (MIXUiO-66) undergo cell expansion obeying Vegard's law and how this behaviour is related to their physical-chemical properties. DFT calculations predict that the unit cell in amino-functionalized UiO-66 experiences only minor expansion as a result of steric effects, whereas major modification to the electronic features of the framework leads to weaker metal-linker interaction and consequently to the loss of stability at higher degrees of functionalization. For bromo-functionalized UiO-66, steric repulsion due to the size of bromine yields a large cell expansion, but the electronic features remain very similar to pristine UiO-66, preserving the stability of the framework upon functionalization. MIXUiO-66 obtained by either direct synthesis or by post-synthetic exchange shows Vegard-like behaviour, suggesting that both preparation methods yield solid solutions, but the thermal stability and the textural properties of the post-synthetic exchanged materials do not display a clear dependence on the chemical composition, as observed for the MOFs obtained by direct synthesis.

  1. One-dimensional curved wire chamber for powder x-ray crystallography

    International Nuclear Information System (INIS)

    Ortendahl, D.; Perez-Mendez, V.; Stoker, J.; Beyermann, W.

    1978-01-01

    A xenon filled single anode wire chamber with delay line readout has been constructed for use in powder x-ray crystallography using 8 to 20 keV x-rays. The entire chamber including the anode wire and the delay line which forms part of the cathode plane is a section of a circular arc whose center is the powder specimen. The anode wire--38 μm gold-plated tungsten--is suspended in a circular arc by the interaction of a current flowing through it and magnetic field provided by two permanent magnets, above and below the wire, extending along the active length of the chamber. When filled with xenon to 3 atmospheres the chamber has uniform sensitivity in excess of 80% at 8 keV and a spatial resolution better than 0.3 mm

  2. Astrophysical extended X-ray absorption fine-structure analysis

    International Nuclear Information System (INIS)

    Woo, J.W.; Forrey, R.C.; Cho, K.; Department of Physics and Division of Applied Sciences, Harvard University)

    1997-01-01

    We present an astrophysical extended X-ray absorption fine-structure (EXAFS) analysis (AEA) tool. The AEA tool is designed to generate a numerical model of the modification to the X-ray absorption coefficient due to the EXAFS phenomenon. We have constructed a complete database (elements up to the atomic number 92) of EXAFS parameters: central atom phase shift (2δ 1 ), backscattering phase shift (φ b ), and backscattering amplitude (F). Using the EXAFS parameter data base, the AEA tool can generate a numerical model of any compound when the atomic numbers of neighboring atoms and their distances to the central X-ray-absorbing atom are given. copyright 1997 The American Astronomical Society

  3. High-pressure powder x-ray diffraction experiments on Zn at low temperature

    CERN Document Server

    Takemura, K; Fujihisa, H; Kikegawa, T

    2002-01-01

    High-pressure powder x-ray diffraction experiments have been performed on Zn with a He-pressure medium at low temperature. When the sample was compressed in the He medium at low temperature, large nonhydrostaticity developed, yielding erroneous lattice parameters. On the other hand, when the pressure was changed at high temperatures, good hydrostaticity was maintained. No anomaly in the volume dependence of the c/a axial ratio has been found.

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

    International Nuclear Information System (INIS)

    Gulden, Johannes

    2013-03-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Gulden, Johannes

    2013-03-15

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

  6. Theoretical approaches to x-ray absorption fine structure

    International Nuclear Information System (INIS)

    Rehr, J. J.; Albers, R. C.

    2000-01-01

    Dramatic advances in the understanding of x-ray absorption fine structure (XAFS) have been made over the past few decades, which have led ultimately to a highly quantitative theory. This review covers these developments from a unified multiple-scattering viewpoint. The authors focus on extended x-ray absorption fine structure (EXAFS) well above an x-ray edge, and, to a lesser extent, on x-ray absorption near-edge structure (XANES) closer to an edge. The discussion includes both formal considerations, derived from a many-electron formulation, and practical computational methods based on independent-electron models, with many-body effects lumped into various inelastic losses and energy shifts. The main conceptual issues in XAFS theory are identified and their relative importance is assessed; these include the convergence of the multiple-scattering expansion, curved-wave effects, the scattering potential, inelastic losses, self-energy shifts, and vibrations and structural disorder. The advantages and limitations of current computational approaches are addressed, with particular regard to quantitative experimental comparisons. (c) 2000 The American Physical Society

  7. Structured scintillators for X-ray imaging with micrometre resolution

    DEFF Research Database (Denmark)

    Olsen, Ulrik Lund; Schmidt, Søren; Poulsen, Henning Friis

    2009-01-01

    A 3D X-ray detector for imaging of 30–200 keV photons is described. It comprises a stack of semitransparent structured scintillators, where each scintillator is a regular array of waveguides in silicon, and with pores filled with CsI. The performance of the detector is described theoretically...

  8. Structural Investigations of Nanowires Using X-Ray Diffraction

    DEFF Research Database (Denmark)

    Stankevic, Tomas

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

  9. The structure of denisovite, a fibrous nanocrystalline polytypic disordered `very complex' silicate, studied by a synergistic multi-disciplinary approach employing methods of electron crystallography and X-ray powder diffraction

    Directory of Open Access Journals (Sweden)

    Ira V. Rozhdestvenskaya

    2017-05-01

    Full Text Available Denisovite is a rare mineral occurring as aggregates of fibres typically 200–500 nm diameter. It was confirmed as a new mineral in 1984, but important facts about its chemical formula, lattice parameters, symmetry and structure have remained incompletely known since then. Recently obtained results from studies using microprobe analysis, X-ray powder diffraction (XRPD, electron crystallography, modelling and Rietveld refinement will be reported. The electron crystallography methods include transmission electron microscopy (TEM, selected-area electron diffraction (SAED, high-angle annular dark-field imaging (HAADF, high-resolution transmission electron microscopy (HRTEM, precession electron diffraction (PED and electron diffraction tomography (EDT. A structural model of denisovite was developed from HAADF images and later completed on the basis of quasi-kinematic EDT data by ab initio structure solution using direct methods and least-squares refinement. The model was confirmed by Rietveld refinement. The lattice parameters are a = 31.024 (1, b = 19.554 (1 and c = 7.1441 (5 Å, β = 95.99 (3°, V = 4310.1 (5 Å3 and space group P12/a1. The structure consists of three topologically distinct dreier silicate chains, viz. two xonotlite-like dreier double chains, [Si6O17]10−, and a tubular loop-branched dreier triple chain, [Si12O30]12−. The silicate chains occur between three walls of edge-sharing (Ca,Na octahedra. The chains of silicate tetrahedra and the octahedra walls extend parallel to the z axis and form a layer parallel to (100. Water molecules and K+ cations are located at the centre of the tubular silicate chain. The latter also occupy positions close to the centres of eight-membered rings in the silicate chains. The silicate chains are geometrically constrained by neighbouring octahedra walls and present an ambiguity with respect to their z position along these walls, with displacements between neighbouring layers being

  10. Polymorphous transformation in the crystal structure of [Mg(H.sub.2./sub.O).sub.6./sub. Br.sub.2./sub.][(C.sub.7./sub.H.sub.14./sub.N.sub.4./sub.).sub.2./sub.] . 4 (H.sub.2./sub.O) studied by powder and single crystal X-ray diffraction

    Czech Academy of Sciences Publication Activity Database

    Rivera, A.; Rohlíček, Jan; Sadat-Bernal, J.; Ríos-Motta, J.; Dušek, Michal

    2014-01-01

    Roč. 229, č. 4 (2014), s. 319-327 ISSN 0044-2968 Grant - others:AV ČR(CZ) Praemium Academiae Institutional support: RVO:68378271 Keywords : polymorphism * powder X-ray * single crystal diffraction * 1,3,6,8-tetraazatricyclo[4.3.1.13,ˑ 8]undecane * phase transformation * crystal structure analysis Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.310, year: 2014

  11. Single crystal X-ray structure of the artists’ pigment zinc yellow

    DEFF Research Database (Denmark)

    Simonsen, Kim Pilkjær; Christiansen, Marie Bitsch; Vinum, Morten Gotthold

    2017-01-01

    electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS), attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR), and powder X-ray diffraction (PXRD), showed that the synthesised products and the industrial pigment were identical. Single-crystal X-ray crystallography......The artists’ pigment zinc yellow is in general described as a complex potassium zinc chromate with the empirical formula 4ZnCrO4·K2O·3H2O. Even though the pigment has been in use since the second half of the 19th century also in large-scale industrial applications, the exact structure had hitherto...... been unknown. In this work, zinc yellow was synthesised by precipitation from an aqueous solution of zinc nitrate and potassium chromate under both neutral and basic conditions, and the products were compared with the pigment used in industrial paints. Analyses by Raman microscopy (MRS), scanning...

  12. Capillary based Li-air batteries for in situ synchrotron X-ray powder diffraction studies

    DEFF Research Database (Denmark)

    Storm, Mie Møller; Johnsen, Rune E.; Younesi, Reza

    2015-01-01

    For Li-air batteries to reach their full potential as energy storage system, a complete understanding of the conditions and reactions in the battery during operation is needed. To follow the reactions in situ a capillary-based Li-O2 battery has been developed for synchrotron-based in situ X......-ray powder diffraction (XRPD). In this article, we present the results for the analysis of 1st and 2nd deep discharge and charge for a cathode being cycled between 2 and 4.6 V. The crystalline precipitation of Li2O2 only is observed in the capillary battery. However, there are indications of side reactions...... of constant exposure of X-ray radiation to the electrolyte and cathode during charge of the battery was also investigated. X-ray exposure during charge leads to changes in the development of the intensity and the FWHM of the Li2O2 diffraction peaks. The X-ray diffraction results are supported by ex situ X...

  13. X-ray lasers for structural and dynamic biology

    International Nuclear Information System (INIS)

    Spence, J C H; Weierstall, U; Chapman, H N

    2012-01-01

    Research opportunities and techniques are reviewed for the application of hard x-ray pulsed free-electron lasers (XFEL) to structural biology. These include the imaging of protein nanocrystals, single particles such as viruses, pump–probe experiments for time-resolved nanocrystallography, and snapshot wide-angle x-ray scattering (WAXS) from molecules in solution. The use of femtosecond exposure times, rather than freezing of samples, as a means of minimizing radiation damage is shown to open up new opportunities for the molecular imaging of biochemical reactions at room temperature in solution. This is possible using a ‘diffract-and-destroy’ mode in which the incident pulse terminates before radiation damage begins. Methods for delivering hundreds of hydrated bioparticles per second (in random orientations) to a pulsed x-ray beam are described. New data analysis approaches are outlined for the correlated fluctuations in fast WAXS, for protein nanocrystals just a few molecules on a side, and for the continuous x-ray scattering from a single virus. Methods for determining the orientation of a molecule from its diffraction pattern are reviewed. Methods for the preparation of protein nanocrystals are also reviewed. New opportunities for solving the phase problem for XFEL data are outlined. A summary of the latest results is given, which now extend to atomic resolution for nanocrystals. Possibilities for time-resolved chemistry using fast WAXS (solution scattering) from mixtures is reviewed, toward the general goal of making molecular movies of biochemical processes. (key issues reviews)

  14. The development of structural x-ray crystallography

    Science.gov (United States)

    Woolfson, M. M.

    2018-03-01

    From its birth in 1912, when only the simplest structures could be solved, x-ray structural crystallography is now able to solve macromolecular structures containing many thousands of independent non-hydrogen atoms. This progress has depended on, and been driven by, great technical advances in the development of powerful synchrotron x-ray sources, advanced automated equipment for the collection and storage of large data sets and powerful computers to deal with everything from data processing to running programmes employing complex algorithms for the automatic solution of structures. The sheer number of developments in the subject over the past century makes it impossible for this review to be exhaustive, but it will describe some major developments that will enable the reader to understand how the subject has grown from its humble beginnings to what it is today.

  15. Digital Image Correlation of 2D X-ray Powder Diffraction Data for Lattice Strain Evaluation

    Directory of Open Access Journals (Sweden)

    Hongjia Zhang

    2018-03-01

    Full Text Available High energy 2D X-ray powder diffraction experiments are widely used for lattice strain measurement. The 2D to 1D conversion of diffraction patterns is a necessary step used to prepare the data for full pattern refinement, but is inefficient when only peak centre position information is required for lattice strain evaluation. The multi-step conversion process is likely to lead to increased errors associated with the ‘caking’ (radial binning or fitting procedures. A new method is proposed here that relies on direct Digital Image Correlation analysis of 2D X-ray powder diffraction patterns (XRD-DIC, for short. As an example of using XRD-DIC, residual strain values along the central line in a Mg AZ31B alloy bar after 3-point bending are calculated by using both XRD-DIC and the conventional ‘caking’ with fitting procedures. Comparison of the results for strain values in different azimuthal angles demonstrates excellent agreement between the two methods. The principal strains and directions are calculated using multiple direction strain data, leading to full in-plane strain evaluation. It is therefore concluded that XRD-DIC provides a reliable and robust method for strain evaluation from 2D powder diffraction data. The XRD-DIC approach simplifies the analysis process by skipping 2D to 1D conversion, and opens new possibilities for robust 2D powder diffraction data analysis for full in-plane strain evaluation.

  16. Digital Image Correlation of 2D X-ray Powder Diffraction Data for Lattice Strain Evaluation

    Science.gov (United States)

    Zhang, Hongjia; Sui, Tan; Daisenberger, Dominik; Fong, Kai Soon

    2018-01-01

    High energy 2D X-ray powder diffraction experiments are widely used for lattice strain measurement. The 2D to 1D conversion of diffraction patterns is a necessary step used to prepare the data for full pattern refinement, but is inefficient when only peak centre position information is required for lattice strain evaluation. The multi-step conversion process is likely to lead to increased errors associated with the ‘caking’ (radial binning) or fitting procedures. A new method is proposed here that relies on direct Digital Image Correlation analysis of 2D X-ray powder diffraction patterns (XRD-DIC, for short). As an example of using XRD-DIC, residual strain values along the central line in a Mg AZ31B alloy bar after 3-point bending are calculated by using both XRD-DIC and the conventional ‘caking’ with fitting procedures. Comparison of the results for strain values in different azimuthal angles demonstrates excellent agreement between the two methods. The principal strains and directions are calculated using multiple direction strain data, leading to full in-plane strain evaluation. It is therefore concluded that XRD-DIC provides a reliable and robust method for strain evaluation from 2D powder diffraction data. The XRD-DIC approach simplifies the analysis process by skipping 2D to 1D conversion, and opens new possibilities for robust 2D powder diffraction data analysis for full in-plane strain evaluation. PMID:29543728

  17. Study of properties of chemically modified samples of halloysite mineral with X-ray fluorescence and X-ray powder diffraction methods

    International Nuclear Information System (INIS)

    Banaś, D.; Kubala-Kukuś, A.; Braziewicz, J.; Majewska, U.; Pajek, M.; Wudarczyk-Moćko, J.; Czech, K.; Garnuszek, M.; Słomkiewicz, P.; Szczepanik, B.

    2013-01-01

    Elemental and chemical composition of raw and activated samples of halloysite mineral using wavelength dispersive X-ray fluorescence (WDXRF), total reflection X-ray fluorescence (TXRF) and X-ray powder diffraction (XRPD) methods were determined. As the result, it has been shown that application of the complementary X-ray spectrometry techniques allows very precise observation of changes in composition of halloysite mineral samples caused by its chemical modifications. Sample preparation procedure and usability of the research methods applied are described in details. Procedure of activation of raw halloysite mineral samples by etching them in sulfuric acid of various concentrations has been described and discussed. The ability of the samples to adsorb lead from intentionally contaminated water was tested and confirmed. - Author-Highlights: • We measured elemental and chemical composition of raw and activated halloysite mineral samples. • We showed that X-ray techniques allow precise study of changes in the sample composition. • We describe procedure of activation of the samples by etching them in sulfuric acid. • We tested ability of halloysite mineral to absorb lead from contaminated water

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

    Science.gov (United States)

    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.

  19. Functional coordination polymers and MOFs from reactions of the lanthanides and barium with azole ligands. Synthesis and characterization with a focus on structure determination from X-ray powder diffraction data; Funktionale Koordinationspolymere und MOFs aus Reaktionen der Lanthanide und des Bariums mit Azol-Liganden. Synthese und Charakterisierung mit dem Fokus der Strukturbestimmung anhand von Roentgenpulverbeugungsdaten

    Energy Technology Data Exchange (ETDEWEB)

    Rybak, Jens-Christoph

    2012-07-01

    This thesis deals with the synthesis and characterization of coordination polymers and MOFs of the lanthanides and barium with different azolic N-heterocycles. A total of 18 new organic-inorganic hybrid materials, as well as a series of co-doped compounds is presented. Besides the structural characterization of these materials from X-ray diffraction powder data, the focus of the investigations is on the thermal and photoluminescence spectroscopic properties. The lanthanides La - Lu, except Eu and Pm, can be reacted with 1H-1,2,3-triazole to give the series of the isotypic dense 3D-MOFs {sup 3}{sub ∞}[Ln(Tz{sup *}){sub 3}]. Investigation of the photoluminescence properties of these compounds reveals a broad range of different luminescence phenomena, including the first observation of an intrinsic inner-filter effect of the Ln{sup 3+}-ions. The structure of this isotypic series of compounds was solved and refined from X-ray powder diffraction data. A 2D-polymorph of these compounds {sup 2}{sub ∞}[Ln(Tz{sup *}){sub 3}], is observed for Ln = Sm, Tb and was characterized by single crystal data. The reaction of Eu with 1H-benzotriazole yields the 1D-coordination polymer {sup 1}{sub ∞}[Eu(Btz){sub 2}(BtzH){sub 2}], which is the first example of a divalent rare earth benzotriazolate. Analysis of the thermal properties reveals the transformation to the 3D-MOF {sup 3}{sub ∞}[Eu(Btz){sub 2}] at higher temperatures. The structure of this material was also solved from X-ray powder diffraction data. Investigation of the photoluminescence properties of the co-doped compounds {sup 3}{sub ∞}[Ba{sub 1-x}Eu{sub x}(Im){sub 2}], which were obtained from reaction of the salt-like hydrides BaH{sub 2} and EuH{sub 2} with imidazole, show that the synthesis of luminescent MOF materials by co-doping of non-luminescent networks with luminescence centers is possible. The structure of these materials was solved from X-ray powder diffraction data of the undoped compound {sup 3}{sub

  20. Diffraction anomalous fine structure using X-ray anomalous dispersion

    International Nuclear Information System (INIS)

    Soejima, Yuji; Kuwajima, Shuichiro

    1998-01-01

    A use of X-ray anomalous dispersion effects for structure investigation has recently been developed by using synchrotron radiation. One of the interesting method is the observation of anomalous fine structure which arise on diffraction intensity in energy region of incident X-ray at and higher than absorption edge. The phenomenon is so called Diffraction Anomalous Fine Structure (DAFS). DAFS originates in the same physical process an that of EXAFS: namely photoelectric effect at the corresponding atom and the interaction of photoelectron waves between the atom and neighboring atoms. In contrast with EXAFS, the method is available for only the crystalline materials, but shows effective advantages of the structure investigations by a use of diffraction: one is the site selectivity and the other is space selectivity. In the present study, demonstrations of a use of X-ray anomalous dispersion effect for the superstructure determination will be given for the case of PbZrO 3 , then recent trial investigations of DAFS in particular on the superlattice reflections will be introduced. In addition, we discuss about Forbidden Reflection near Edge Diffraction (FRED) which is more recently investigated as a new method of the structure analysis. (author)

  1. Parallelization for X-ray crystal structural analysis program

    Energy Technology Data Exchange (ETDEWEB)

    Watanabe, Hiroshi [Japan Atomic Energy Research Inst., Tokyo (Japan); Minami, Masayuki; Yamamoto, Akiji

    1997-10-01

    In this report we study vectorization and parallelization for X-ray crystal structural analysis program. The target machine is NEC SX-4 which is a distributed/shared memory type vector parallel supercomputer. X-ray crystal structural analysis is surveyed, and a new multi-dimensional discrete Fourier transform method is proposed. The new method is designed to have a very long vector length, so that it enables to obtain the 12.0 times higher performance result that the original code. Besides the above-mentioned vectorization, the parallelization by micro-task functions on SX-4 reaches 13.7 times acceleration in the part of multi-dimensional discrete Fourier transform with 14 CPUs, and 3.0 times acceleration in the whole program. Totally 35.9 times acceleration to the original 1CPU scalar version is achieved with vectorization and parallelization on SX-4. (author)

  2. Dynamical X-ray scattering from the relaxed structures

    International Nuclear Information System (INIS)

    Benediktovitch, A.; Feranchuk, I.; Ulyanenkov, A.

    2009-01-01

    High-resolution X-ray diffraction is now widely used analytical tool for investigation of nano scale multilayered structures in semiconductor and optical technologies. The HRXRD method delivers unique information on the crystallographic lattice of the samples, concentration of solid solutions, lattice mismatches, layer thicknesses, defect distribution, and relaxation degree of the epitaxial layers. The evaluation of the experimental results, however, requires a robust and precise theory due to complex dynamical scattering of X-rays from near perfect crystallographic structure of the samples. Usually, the Takagi-Taupin approach [1] or the recurrent matrix methods [2] are used for the simulation of the X-ray diffraction profiles from the epitaxial multilayered structures. The use of these theories, however, becomes essentially difficult, when the lateral lattice mismatches are present in multilayers, for example, in the case of partially or fully relaxed epitaxially grown samples. In the present work, the general solution of this problem is found analytically. The angular divergence of the incident beam is also considered and the algorithm for the diffracted profile mapping in the reciprocal space is developed. The experimental reciprocal space mapping of typical AlGaN/GaN/AlN samples with partially relaxed layers is compared to the simulated maps, which describe well the location and character of the diffraction spots caused by different layers. (author)

  3. The X-ray powder diffraction pattern and lattice parameters of perovskite

    International Nuclear Information System (INIS)

    Ball, C.J.; Napier, J.G.

    1988-02-01

    The interplanar spacings and intensities of all lines appearing in the X-ray powder diffraction pattern of perovskite have been calculated. Many of the lines occur in groups with a large amount of overlap. As an aid to identifying the lines which are observed, the intensity profiles of the major groups have been plotted. Those lines which are relatively free of overlap and can be identified unambiguously have been used to calculate the lattice parameters, with the results a=5.4424 ± 0.0001 A, b=7.6417 ± 0.0002 A, c=5.3807 ± 0.0001 A

  4. Quantitative X-ray determination of CFRP micro structures

    International Nuclear Information System (INIS)

    Hentschel, Manfred P.; Mueller, Bernd R.; Lange, Axel; Wald, Oliver

    2008-01-01

    Beyond imaging the mass distribution of materials by X-ray absorption techniques recent synchrotron and laboratory X-ray refraction techniques provide interface contrast imaging of micro structures. This is of specific relevance to carbon fibre composites (CFRP) which constitute advanced aerospace components. Apart from merely finding isolated flaws like cracks or pores within the natural high interface density only the quantitative measurement of the differences after defined mechanical treatment provides a reliable understanding of the related macroscopic properties. The contribution of the fibre matrix interface of CFRP laminates to the mechanical properties is investigated by relating the mechanical damage to the additional fibre debonding after impact and fatigue. Composites of industrially sized carbon fibres for aerospace applications and of unsized fibres are compared. (orig.)

  5. Colliding Stellar Winds Structure and X-ray Emission

    Science.gov (United States)

    Pittard, J. M.; Dawson, B.

    2018-04-01

    We investigate the structure and X-ray emission from the colliding stellar winds in massive star binaries. We find that the opening angle of the contact discontinuity (CD) is overestimated by several formulae in the literature at very small values of the wind momentum ratio, η. We find also that the shocks in the primary (dominant) and secondary winds flare by ≈20° compared to the CD, and that the entire secondary wind is shocked when η ≲ 0.02. Analytical expressions for the opening angles of the shocks, and the fraction of each wind that is shocked, are provided. We find that the X-ray luminosity Lx∝η, and that the spectrum softens slightly as η decreases.

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

    International Nuclear Information System (INIS)

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

    1999-01-01

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

  7. Structural enzymology using X-ray free electron lasers

    Directory of Open Access Journals (Sweden)

    Christopher Kupitz

    2017-07-01

    Full Text Available Mix-and-inject serial crystallography (MISC is a technique designed to image enzyme catalyzed reactions in which small protein crystals are mixed with a substrate just prior to being probed by an X-ray pulse. This approach offers several advantages over flow cell studies. It provides (i room temperature structures at near atomic resolution, (ii time resolution ranging from microseconds to seconds, and (iii convenient reaction initiation. It outruns radiation damage by using femtosecond X-ray pulses allowing damage and chemistry to be separated. Here, we demonstrate that MISC is feasible at an X-ray free electron laser by studying the reaction of M. tuberculosis ß-lactamase microcrystals with ceftriaxone antibiotic solution. Electron density maps of the apo-ß-lactamase and of the ceftriaxone bound form were obtained at 2.8 Å and 2.4 Å resolution, respectively. These results pave the way to study cyclic and non-cyclic reactions and represent a new field of time-resolved structural dynamics for numerous substrate-triggered biological reactions.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-05-15

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

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

    International Nuclear Information System (INIS)

    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. X-ray powder diffraction analysis of liquid-phase-sintered silicon carbide ceramics

    Energy Technology Data Exchange (ETDEWEB)

    Ortiz, A.L.; Sanchez-Bajo, F. [Universidad de Extremadura, Badajoz (Spain). Dept. de Electronica e Ingenieria Electromecanica; Cumbrera, F.L. [Universidad de Extremadura, Badajoz (Spain). Dept. de Fisica

    2002-07-01

    In an attempt to gain a comprehensive understanding of the microstructural evolution in liquid-phase-sintered silicon carbide ceramics, the effect of the starting {beta}-SiC powder has been studied. Pellets of two different {beta}-SiC starting powders were sintered with simultaneous additions of Al{sub 2}O{sub 3} and Y{sub 2}O{sub 3} at 1950 C for 1 hour in flowing argon atmosphere. Here we have used X-ray diffraction to obtain the relative abundance of the resulting SiC polytypes after sintering. The significant influence of the defects concentration on the {beta} to {alpha} transformation rate has been determined using the Rietveld method. (orig.)

  11. X-ray crystal structure and small-angle X-ray scattering of sheep liver sorbitol dehydrogenase

    DEFF Research Database (Denmark)

    Yennawar, Hemant; Møller, Magda; Gillilan, Richard

    2011-01-01

    The X-ray crystal structure of sheep liver sorbitol dehydrogenase (slSDH) has been determined using the crystal structure of human sorbitol dehydrogenase (hSDH) as a molecular-replacement model. slSDH crystallized in space group I222 with one monomer in the asymmetric unit. A conserved tetramer...

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

    Energy Technology Data Exchange (ETDEWEB)

    Cottrino, Sandrine; Jorand, Yves, E-mail: yves.jorand@insa-lyon.fr; Maire, Eric; Adrien, Jérôme

    2013-07-15

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

  13. Characterization of cubic ceria?zirconia powders by X-ray diffraction and vibrational and electronic spectroscopy

    Science.gov (United States)

    Sánchez Escribano, Vicente; Fernández López, Enrique; Panizza, Marta; Resini, Carlo; Gallardo Amores, José Manuel; Busca, Guido

    2003-10-01

    The X-ray diffraction (XRD) patterns and the Infrared, Raman and UV-visible spectra of CeO 2ZrO 2 powders prepared by co-precipitation are presented. Raman spectra provide evidence for the largely predominant cubic structure of the powders with CeO 2 molar composition higher than 25%. Also skeletal IR spectra allow to distinguish cubic from tetragonal phases which are instead not easily distinguished on the basis of the XRD patterns. All mixed oxides including pure ceria are strong UV absorbers although also absorb in the violet visible region. By carefully selecting their composition and treatment temperature, the onset of the radiation that they cut off can be chosen in the 425-475 nm interval. Although they are likely metastable, the cubic phases are still pure even after heating at 1173 K for 4 h.

  14. Testing ion structure models with x-ray Thomson scattering

    Directory of Open Access Journals (Sweden)

    Wünsch K.

    2013-11-01

    Full Text Available We investigate the influence of various ionic structure models on the interpretation of the X-ray Thomson scattering signal. For the calculation of the ion structure, classical hypernetted chain equations are used applying different effective inter-particle potentials. It is shown that the different models lead to significant discrepancies in the theoretically predicted weight of the Rayleigh peak, in particular for small k-values where correlation effects are important. Here, we propose conditions which might allow for an experimental verification of the theories under consideration of experimental constraints of k-vector blurring.

  15. Automatic protein structure solution from weak X-ray data

    Science.gov (United States)

    Skubák, Pavol; Pannu, Navraj S.

    2013-11-01

    Determining new protein structures from X-ray diffraction data at low resolution or with a weak anomalous signal is a difficult and often an impossible task. Here we propose a multivariate algorithm that simultaneously combines the structure determination steps. In tests on over 140 real data sets from the protein data bank, we show that this combined approach can automatically build models where current algorithms fail, including an anisotropically diffracting 3.88 Å RNA polymerase II data set. The method seamlessly automates the process, is ideal for non-specialists and provides a mathematical framework for successfully combining various sources of information in image processing.

  16. X-ray crystal structure and small-angle X-ray scattering of sheep liver sorbitol dehydrogenase

    Energy Technology Data Exchange (ETDEWEB)

    Yennawar, Hemant [Pennsylvania State University, 8 Althouse Laboratory, University Park, PA 16802 (United States); Møller, Magda [Cornell High Energy Synchrotron Source, Ithaca, NY 14853 (United States); University of Copenhagen, DK-2100 Copenhagen (Denmark); Gillilan, Richard [Cornell High Energy Synchrotron Source, Ithaca, NY 14853 (United States); Yennawar, Neela, E-mail: nhy1@psu.edu [Pennsylvania State University, 8 Althouse Laboratory, University Park, PA 16802 (United States)

    2011-05-01

    The X-ray crystal structure and a small-angle X-ray scattering solution structure of sheep liver sorbitol dehydrogenase have been determined. The details of the interactions that enable the tetramer scaffold to be the functional biological unit have been analyzed. The X-ray crystal structure of sheep liver sorbitol dehydrogenase (slSDH) has been determined using the crystal structure of human sorbitol dehydrogenase (hSDH) as a molecular-replacement model. slSDH crystallized in space group I222 with one monomer in the asymmetric unit. A conserved tetramer that superposes well with that seen in hSDH (despite belonging to a different space group) and obeying the 222 crystal symmetry is seen in slSDH. An acetate molecule is bound in the active site, coordinating to the active-site zinc through a water molecule. Glycerol, a substrate of slSDH, also occupies the substrate-binding pocket together with the acetate designed by nature to fit large polyol substrates. The substrate-binding pocket is seen to be in close proximity to the tetramer interface, which explains the need for the structural integrity of the tetramer for enzyme activity. Small-angle X-ray scattering was also used to identify the quaternary structure of the tetramer of slSDH in solution.

  17. Neutron and X-ray diffraction from modulated structures

    International Nuclear Information System (INIS)

    Harris, P.

    1994-07-01

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

  18. Structural and microstructural characterization of U3Si2 nuclear fuel using X-ray diffraction

    International Nuclear Information System (INIS)

    Ichikawa, Rodrigo U.; Garcia, Rafael H.L.; Silva, Andre S.B. da; Saliba-Silva, Adonis M.; Lima, Nelson B.; Martinez, Luis G.; Turrillas, Xavier

    2017-01-01

    In this work, two uranium silicide powdered samples, containing 67% and 42 mol% of Si, were analyzed using X-ray diffraction (named as 67 Si and 42 Si). For structural characterization, Rietveld refinement was used to estimate cell parameters, volume fraction (weight percent) of crystalline phases and atomic positions. For the main phases, X-ray line profile analysis (XLPA) was used to estimate mean crystallite sizes and micro strains. The 67 Si sample presents higher content of USi 2( tetragonal) and the 42 Si sample presents higher content of U 3 Si 2 (tetragonal) as identified and calculated from the XRD profiles. Overall there are no appreciable structural changes and the parameters refined are in good accordance with the ones reported in the literature. Mean crystallite sizes determined by XLPA revealed small crystallites of the order of 10 1 nm and low micro strain for all samples. (author)

  19. Structure determination of spider silk from X-ray images

    Energy Technology Data Exchange (ETDEWEB)

    Ulrich, Stephan; Zippelius, Annette [Universitaet Goettingen, Institut fuer Theoretische Physik (Germany); Meling, Martin [Max-Planck-Institut fuer biophysikalische Chemie, Goettingen (Germany); Glisovic, Anja; Salditt, Tim [Universitaet Goettingen, Institut fuer Roentgenphysik (Germany)

    2008-07-01

    Spider silk consists of interconnected crystallites, which are typically aligned along the fiber axis. We present a method to systematically determine the structure of these crystallites. Hereby we introduce a model that calculates the scattering function G(q) which is fitted to the measured X-ray image (silk from nephila clavipes). With it, the crystallites' size, the constitution and dimensions of their unit cell, as well as their tilt with respect to the fiber axis is identified, and furthermore the effect of coherent scattering from different crystallites is investigated. The shown methods and the presented model can easily be generalized to a wide class of composite materials.

  20. Status and limitations of multilayer X-ray interference structures

    International Nuclear Information System (INIS)

    Kortright, J.B.

    1996-01-01

    Trends in the performance of x-ray multilayer interference structures with periods ranging from 9 to 130 (angstrom) are reviewed. Analysis of near-normal incidence reflectance data vs photon energy reveals that the effective interface with σ in a static Debye-Waller model, describing interdiffusion and roughness, decreases as the multilayer period decreases, and reaches a lower limit of roughly 2 (angstrom). Specular reflectance and diffuse scattering from uncoated and multilayer-coated substrates having different roughness suggest that this lower limit results largely from substrate roughness. The increase in interface width with period thus results from increasing roughness of interdiffusion as the layer thickness increases

  1. X-ray structure determination and deuteration of nattokinase

    International Nuclear Information System (INIS)

    Yanagisawa, Yasuhide; Chatake, Toshiyuki; Naito, Sawa; Ohsugi, Tadanori; Yatagai, Chieko; Sumi, Hiroyuki; Kawaguchi, Akio; Chiba-Kamosida, Kaori; Ogawa, Megumi; Adachi, Tatsumi; Morimoto, Yukio

    2013-01-01

    X-ray structure determination and deuteration of nattokinase were performed to facilitate neutron crystallographic analysis. Nattokinase (NK) is a strong fibrinolytic enzyme, which is produced in abundance by Bacillus subtilis natto. Although NK is a member of the subtilisin family, it displays different substrate specificity when compared with other subtilisins. The results of molecular simulations predict that hydrogen arrangements around Ser221 at the active site probably account for the substrate specificity of NK. Therefore, neutron crystallographic analysis should provide valuable information that reveals the enzymatic mechanism of NK. In this report, the X-ray structure of the non-hydrogen form of undeuterated NK was determined, and the preparation of deuterated NK was successfully achieved. The non-hydrogen NK structure was determined at 1.74 Å resolution. The three-dimensional structures of NK and subtilisin E from Bacillus subtilis DB104 are near identical. Deuteration of NK was carried out by cultivating Bacillus subtilis natto in deuterated medium. The D 2 O resistant strain of Bacillus subtilis natto was obtained by successive cultivation rounds, in which the concentration of D 2 O in the medium was gradually increased. NK was purified from the culture medium and its activity was confirmed by the fibrin plate method. The results lay the framework for neutron protein crystallography analysis

  2. X-ray structure determination and deuteration of nattokinase

    Energy Technology Data Exchange (ETDEWEB)

    Yanagisawa, Yasuhide [Chiba Institute of Science, 15-8 Shiomi-cho, Cho-shi, Chiba 288-025 (Japan); Chatake, Toshiyuki [Kyoto University, Asashironishi 2, Kumatori, Osaka 590-0494 (Japan); Naito, Sawa; Ohsugi, Tadanori; Yatagai, Chieko; Sumi, Hiroyuki [Kurashiki University of Science and the Arts, 2640 Nishinoura, Tsurajima-cho, Kurashiki, Okayama 712-8505 (Japan); Kawaguchi, Akio [Kyoto University, Asashironishi 2, Kumatori, Osaka 590-0494 (Japan); Chiba-Kamosida, Kaori [Nippon Advanced Technology Co. Ltd, J-PARC, 2-4 Shirane Shirakata, Tokai, Ibaraki 319-1195 (Japan); Ogawa, Megumi; Adachi, Tatsumi [Chiba Institute of Science, 15-8 Shiomi-cho, Cho-shi, Chiba 288-025 (Japan); Morimoto, Yukio [Kyoto University, Asashironishi 2, Kumatori, Osaka 590-0494 (Japan)

    2013-11-01

    X-ray structure determination and deuteration of nattokinase were performed to facilitate neutron crystallographic analysis. Nattokinase (NK) is a strong fibrinolytic enzyme, which is produced in abundance by Bacillus subtilis natto. Although NK is a member of the subtilisin family, it displays different substrate specificity when compared with other subtilisins. The results of molecular simulations predict that hydrogen arrangements around Ser221 at the active site probably account for the substrate specificity of NK. Therefore, neutron crystallographic analysis should provide valuable information that reveals the enzymatic mechanism of NK. In this report, the X-ray structure of the non-hydrogen form of undeuterated NK was determined, and the preparation of deuterated NK was successfully achieved. The non-hydrogen NK structure was determined at 1.74 Å resolution. The three-dimensional structures of NK and subtilisin E from Bacillus subtilis DB104 are near identical. Deuteration of NK was carried out by cultivating Bacillus subtilis natto in deuterated medium. The D{sub 2}O resistant strain of Bacillus subtilis natto was obtained by successive cultivation rounds, in which the concentration of D{sub 2}O in the medium was gradually increased. NK was purified from the culture medium and its activity was confirmed by the fibrin plate method. The results lay the framework for neutron protein crystallography analysis.

  3. Quantitative x-ray structure determination of superlattices and interfaces

    International Nuclear Information System (INIS)

    Schuller, I.K.; Fullerton, E.E.

    1990-01-01

    This paper presents a general procedure for quantitative structural refinement of superlattice structures. To analyze a wide range of superlattices, the authors have derived a general kinematical diffraction formula that includes random, continuous and discrete fluctuations from the average structure. By implementing a non-linear fitting algorithm to fit the entire x-ray diffraction profile, refined parameters that describe the average superlattice structure, and deviations from this average are obtained. The structural refinement procedure is applied to a crystalline/crystalline Mo/Ni superlattices and crystalline/amorphous Pb/Ge superlattices. Roughness introduced artificially during growth in Mo/Ni superlattices is shown to be accurately reproduced by the refinement

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

    Science.gov (United States)

    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.

  5. FTIR spectroscopy and X-ray powder diffraction characterization of microcrystalline cellulose obtained from alfa fibers

    Directory of Open Access Journals (Sweden)

    Trache D.

    2013-07-01

    Full Text Available Many cereal straws have been used as raw materials for the preparation of microcrystalline cellulose (MCC. These raw materials were gradually replaced with wood products; nevertheless about 10% of the world overall pulp production is obtained from non-wood raw material. The main interest in pulp made from straw is that it provides excellent fibres for different industries with special properties, and that it is the major available source of fibrous raw material in some geographical areas. The aim of the present work was to characterize microcrystalline cellulose prepared from alfa fibers using the hydrolysis process. The products obtained are characterized with FTIR spectroscopy and X-ray powder diffraction. As a result, FTIR spectroscopy is an appropriate technique for studying changes occurred by any chemical treatment. The spectrum of alfa grass stems shows the presence of lignin and hemicelluloses. However, the cellulose spectrum indicates that the extraction of lignin and hemicellulose was effective. The X-ray analysis indicates that the microcrystalline cellulose is more crystalline than the source material.

  6. Characterization of polymorphic solid-state changes using variable temperature X-ray powder diffraction

    DEFF Research Database (Denmark)

    Karjalainen, Milja; Airaksinen, Sari; Rantanen, Jukka

    2005-01-01

    The aim of this study was to use variable temperature X-ray powder diffraction (VT-XRPD) to understand the solid-state changes in the pharmaceutical materials during heating. The model compounds studied were sulfathiazole, theophylline and nitrofurantoin. This study showed that the polymorph form...... of sulfathiazole SUTHAZ01 was very stable and SUTHAZ02 changed as a function of temperature to SUTHAZ01. Theophylline monohydrate changed via its metastable form to its anhydrous form during heating and nitrofurantoin monohydrate changed via amorphous form to its anhydrous form during heating. The crystallinity...... to the anhydrous form. The average crystallite size of sulfathiazole samples varied only a little during heating. The average crystallite size of both theophylline and nitrofurantoin monohydrate decreased during heating. However, the average crystallite size of nitrofurantoin monohydrate returned back to starting...

  7. Effect of Pressure on Valence and Structural Properties of YbFe2Ge2 Heavy Fermion Compound A Combined Inelastic X-ray Spectroscopy, X-ray Diffraction, and Theoretical Investigation

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, Ravhi S.; Svane, Axel; Vaitheeswaran; #8741; , Ganapathy; Kanchana, Venkatakrishnan; Antonio, Daniel; Cornelius, Andrew L.; Bauer, Eric D.; Xiao, Yuming; Chow, Paul (Aarhus); (CIW); (Hyderabad - India); (IIT-India); (LANL); (UNLV)

    2016-06-03

    The crystal structure and the Yb valence of the YbFe2Ge2 heavy fermion compound was measured at room temperature and under high pressures using high-pressure powder X-ray diffraction and X-ray absorption spectroscopy via both partial fluorescence yield and resonant inelastic X-ray emission techniques. Furthermore, the measurements are complemented by first-principles density functional theoretical calculations using the self-interaction corrected local spin density approximation investigating in particular the magnetic structure and the Yb valence. While the ThCr2Si2-type tetragonal (I4/mmm) structure is stable up to 53 GPa, the X-ray emission results show an increase of the Yb valence from v = 2.72(2) at ambient pressure to v = 2.93(3) at ~9 GPa, where at low temperature a pressure-induced quantum critical state was reported.

  8. Single crystal X-ray structure of the artists' pigment zinc yellow

    Science.gov (United States)

    Simonsen, Kim Pilkjær; Christiansen, Marie Bitsch; Vinum, Morten Gotthold; Sanyova, Jana; Bendix, Jesper

    2017-08-01

    The artists' pigment zinc yellow is in general described as a complex potassium zinc chromate with the empirical formula 4ZnCrO4·K2O·3H2O. Even though the pigment has been in use since the second half of the 19th century also in large-scale industrial applications, the exact structure had hitherto been unknown. In this work, zinc yellow was synthesised by precipitation from an aqueous solution of zinc nitrate and potassium chromate under both neutral and basic conditions, and the products were compared with the pigment used in industrial paints. Analyses by Raman microscopy (MRS), scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS), attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR), and powder X-ray diffraction (PXRD), showed that the synthesised products and the industrial pigment were identical. Single-crystal X-ray crystallography determined the structure of zinc yellow as KZn2(CrO4)2(H2O)(OH) or as KZn2(CrO4)2(H3O2) emphasizing the μ-H3O2- moiety. Notably, the zinc yellow is isostructural to the recently structurally characterized cadmium analog and both belong to the natrochalcite structure type.

  9. X-ray structural analysis of some Indian coals

    International Nuclear Information System (INIS)

    Binoy K Saikia, B.K.

    2009-01-01

    Coal is one of the most abundant energy resources and has the capability to meet future energy needs with high reliability. The use of coal as an energy source and as a source of organic chemicals feedstock may become more important in the future. It is physically and chemically a heterogeneous and carbonaceous rock which consists of organic and inorganic materials. Assam coal has been, and continuous to be, a valuable energy source, especially for the various industry in India and for liquefactions of coal. The basic chemical structure of coal that has been widely accepted today was built up from the synthesis of results obtained from X-ray diffraction data. The present paper reports a comparative investigation of coals from different collieries/areas of Makum coal field, Assam viz. Ledo, Tikak, Baragolai, Tipong and Tirap collieries Makum coal field, Assam with the help of X-ray diffraction (XRD). The X-ray diffraction patterns indicate that the coals are amorphous in nature. The present XRD method includes the evaluation of Function of Radial Distribution of Atoms (FRDA) and structural interpretations of the coals from their Radial Distribution Function (RDF) plots after proper corrections for air scatter, absorption by sample and polarization. The curve intensity profiles in FRDA clearly show quite regular molecular packets for these coals. The first maxima in the FRDA curves was obtained at r= 0.4 Amstrong for Ledo, Baragolai and Tipong coals whereas for Tikak coal it was observed at r= 0.5 Amstrong. The first maximum in the pair distribution function plots, G (r) of Ledo, Tikak, and Tipong coals was obtained at r=0.15 nm whereas for Baragolai and Tirap coals it was observed at r=0.14 nm and r=0.12 nm respectively, which relates to the C=C (aliphatic/aromatic) bonds in coal matrix. The Assam coal samples from Ledo, Tikak, Baragolai, Tipong and Tirap collieries of Makum coalfield have almost the same RDF inter-atomic distances except slight differences. This

  10. X-ray diffraction studies of the structure and orientations of thiophene and fluorenone based molecule

    International Nuclear Information System (INIS)

    Porzio, William; Pasini, Mariacecilia; Destri, Silvia; Giovanella, Umberto; Fontaine, Philippe

    2006-01-01

    The crystal structure of a conjugated molecule containing thiophene and fluorenone residues has been determined from powder X-ray diffraction (XRD). Thin films ( -5 Pa) onto oxidized silicon substrates, are oriented along with different crystallographic directions. A comparison of XRD in both Grazing Incidence and Bragg-Brentano geometries allowed to perform a quantitative analysis of the various orientations. This approach is generally applicable in the case of multi-oriented films. The results fully account for the poor performance of this molecule in p-type field effect transistor devices

  11. Structural studies using X-ray absorption and scattering techniques

    International Nuclear Information System (INIS)

    Ericson, Agneta.

    1989-01-01

    The thesis presents extended X-ray absorption fine structure, EXAFS, and large angle X-ray scattering, LAXS, techniques; instrumentation, data collection and reduction, and applications. These techniques have been used to determine the structures of magnesium halides and organomagnesium halides in diethyl ether and tetrahydrofuran solution. The iodides were used for the LAXS measurements and Br K edge EXAFS data were collected for the corresponding bromides. Two different complexes are present in the diethyl ether solution of magnesium iodide; a polymeric chain-type structure where magnesium is tetrahedrally coordinated, as well as dimeric complex with octahedrally coordinated magnesium. Solvated MgI + is the dominating species in tetrahydrofuran solution. The organomagnesium halides are present in diethyl ether solution as both solvated monomeric and dimeric complexes. Magnesium coordinates a halide ion, an alkyl or aryl group and four solvent molecules octahedrally in the monomeric complex. In the dimeric complex magnesium is octahedrally coordinated by two bridging halide ions, an alkyl or aryl group and three solvent molecules. The distribution of monomeric and dimeric complexes in various solutions are given by a dimerisation constant, K dl . The results indicate that the Schlenk equilibrium is present in these solutions, however, in an extended form. In diethyl ether solution, where MgX 2 does not dissociate, no MgX 2 complex and thereby no Schlenk equilibrium has been observed. In tetrahydrofuran solution MgI 2 has dissociated into mainly MgI + and I - . This indicates that the concentration of MgI 2 is low and that the Schlenk equilibrium should be expanded even further to include the dissociation equilibrium of the magnesium halide. In the thesis Fe K edge EXAFS data collected for the semireduced form of protein A of methane monooxygenase from Methylococcus capsulatus, are also presented. (139 refs.)

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2006-11-15

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

  14. Homogeneity characterisation of (U,Gd)O2 sintered pellets by X-ray diffraction powder analysis applying Rietveld method

    International Nuclear Information System (INIS)

    Leyva, Ana G.; Vega, Daniel R.; Trimarco, Veronica G.; Marchi, Daniel E.

    1999-01-01

    The (U,Gd)O 2 sintered pellets are fabricated by different methods. The homogeneity characterisation of Gd content seems to be necessary as a production control to qualify the process and the final product. The micrographic technique is the most common method used to analyse the homogeneity of these samples, this method requires time and expertise to obtain good results. In this paper, we propose an analysis of the X-ray diffraction powder patterns through the Rietveld method, in which the differences between the experimental data and the calculated from a crystalline structure model proposed are evaluated. This result allows to determine the cell parameters, that can be correlated with the Gd concentration, and the existence of other phases with different Gd ratio. (author)

  15. Establishment of X-ray Measurement System for On-line Monitoring of Water Content in Powder

    Energy Technology Data Exchange (ETDEWEB)

    Hwang, J. S. [Korea Institute of Industrial Technology, Cheonan (Korea, Republic of); Choi, Y. S. [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of); Choi, B. J. [Idealsystem Co., Daegu (Korea, Republic of)

    2012-05-15

    On-line process monitoring is of critical importance in many industries, and therefore a variety of the state-of-the-art physical and chemical measurement techniques have been proposed. But, these techniques have their own pros and cons under the field process environments. Because the field process environments are very different from the well-organized chemical laboratories, many factors should be considered in order to optimize the process monitoring system. However, there have been few studies on the on-line measurement of water content in powder materials. For that reason, the X-ray measurement system based on the X-ray scattering technique, which was first proposed in 2011 as a new method for the determination of water content in powder, has been improved. in the present study, our original X-ray measurement system has been modified for more rapid, simple, and adequate for maximizing the field applicability of the on-line monitoring system

  16. Mechanical design of a high-resolution x-ray powder diffractometer at the Advanced Photon Source.

    Energy Technology Data Exchange (ETDEWEB)

    Shu, D.; Lee, P.; Preissner, C.; Ramanathan, M.; Beno, M.; VonDreele, R.; Ranay, R.; Ribaud, L.; Kurtz, C.; Jiao, X.; Kline, D.; Jemian, P.; Toby, B.

    2007-01-01

    A novel high-resolution x-ray powder diffractometer has been designed and commissioned at the bending magnet beamline 11-BM at the Advanced Photon Source (APS), Argonne National Laboratory (ANL). This state-of-the-art instrument is designed to meet challenging mechanical and optical specifications for producing high-quality powder diffraction data with high throughput. The 2600 mm (H) X 2100 mm (L) X 1700 mm (W) diffractometer consists of five subassemblies: a customized two-circle goniometer with a 3-D adjustable supporting base; a twelve-channel high-resolution crystal analyzer system with an array of precision x-ray slits; a manipulator system for a twelve scintillator x-ray detectors; a 4-D sample manipulator with cryo-cooling capability; and a robot-based sample exchange automation system. The mechanical design of the diffractometer as well as the test results of its positioning performance are presented in this paper.

  17. Mechanical design of a high-resolution x-ray powder diffractometer at the Advanced Photon Source

    International Nuclear Information System (INIS)

    Shu, D.; Lee, P.; Preissner, C.; Ramanathan, M.; Beno, M.; VonDreele, R.; Ranay, R.; Ribaud, L.; Kurtz, C.; Jiao, X.; Kline, D.; Jemian, P.; Toby, B.

    2007-01-01

    A novel high-resolution x-ray powder diffractometer has been designed and commissioned at the bending magnet beamline 11-BM at the Advanced Photon Source (APS), Argonne National Laboratory (ANL). This state-of-the-art instrument is designed to meet challenging mechanical and optical specifications for producing high-quality powder diffraction data with high throughput. The 2600 mm (H) X 2100 mm (L) X 1700 mm (W) diffractometer consists of five subassemblies: a customized two-circle goniometer with a 3-D adjustable supporting base; a twelve-channel high-resolution crystal analyzer system with an array of precision x-ray slits; a manipulator system for a twelve scintillator x-ray detectors; a 4-D sample manipulator with cryo-cooling capability; and a robot-based sample exchange automation system. The mechanical design of the diffractometer as well as the test results of its positioning performance are presented in this paper.

  18. Discovery of Spatial and Spectral Structure in the X-Ray Emission from the Crab Nebula

    Science.gov (United States)

    Weisskopf, Martin C.; Hester, J. Jeff; Tennant, Allyn F.; Elsner, Ronald F.; Schulz, Norbert S.; Marshall, Herman L.; Karovska, Margarita; Nichols, Joy S.; Swartz, Douglas A.; Kolodziejczak, Jeffery J.

    2000-01-01

    The Chandra X-Ray Observatory observed the Crab Nebula and pulsar during orbital calibration. Zeroth-order images with the High-Energy Transmission Grating (HETG) readout by the Advanced Charge Coupled Devices (CCD) Imaging Spectrometer spectroscopy array (ACIS-S) show a striking richness of X-ray structure at a resolution comparable to that of the best ground-based visible-light observations. The HETG-ACIS-S images reveal, for the first time, an X-ray inner ring within the X-ray torus, the suggestion of a hollow-tube structure for the torus, and X-ray knots along the inner ring and (perhaps) along the inward extension of the X-ray jet. Although complicated by instrumental effects and the brightness of the Crab Nebula, the spectrometric analysis shows systematic variations of the X-ray spectrum throughout the nebula.

  19. Discovery of Spatial and Spectral Structure in the X-Ray Emission from the Crab Nebula.

    Science.gov (United States)

    Weisskopf; Hester; Tennant; Elsner; Schulz; Marshall; Karovska; Nichols; Swartz; Kolodziejczak; O'Dell

    2000-06-20

    The Chandra X-Ray Observatory observed the Crab Nebula and pulsar during orbital calibration. Zeroth-order images with the High-Energy Transmission Grating (HETG) readout by the Advanced CCD Imaging Spectrometer spectroscopy array (ACIS-S) show a striking richness of X-ray structure at a resolution comparable to that of the best ground-based visible-light observations. The HETG-ACIS-S images reveal, for the first time, an X-ray inner ring within the X-ray torus, the suggestion of a hollow-tube structure for the torus, and X-ray knots along the inner ring and (perhaps) along the inward extension of the X-ray jet. Although complicated by instrumental effects and the brightness of the Crab Nebula, the spectrometric analysis shows systematic variations of the X-ray spectrum throughout the nebula.

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

    Science.gov (United States)

    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…

  1. X-ray Tomography Characterisation of Lattice Structures Processed by Selective Electron Beam Melting

    Directory of Open Access Journals (Sweden)

    Everth Hernández-Nava

    2017-08-01

    Full Text Available Metallic lattice structures intentionally contain open porosity; however, they can also contain unwanted closed porosity within the structural members. The entrained porosity and defects within three different geometries of Ti-6Al-4V lattices, fabricated by Selective Electron Beam Melting (SEBM, is assessed from X-ray computed tomography (CT scans. The results suggest that horizontal struts that are built upon loose powder show particularly high (~20 × 10−3 vol % levels of pores, as do nodes at which many (in our case 24 struts meet. On the other hand, for struts more closely aligned (0° to 54° to the build direction, the fraction of porosity appears to be much lower (~0.17 × 10−3% arising mainly from pores contained within the original atomised powder particles.

  2. Advances in X-ray powder diffraction profile analysis and its application in ceramic material studies

    International Nuclear Information System (INIS)

    Zhang, Y.

    1988-01-01

    This dissertation is concerned with the following major aspects: (1) the development of necessary computer codes to carry out X-ray powder diffraction profile analysis (XPDPA) calculations; (2) the establishment of a general reference material (GRM) which greatly extends the application of XPDPA and the study of the application of the GRM in profile analysis; (3) the determination of the coherent diffracting domain size and the lattice residual microstrain for some shock-modified and jet-milled materials. A computer code for diffraction profile refinement, XRAYL, fits a diffraction profile with any one of five mathematical functions, either as symmetric or asymmetric (split mode) forms. The resulting patterns meet the requirements for successful profile analysis of microstrain and crystallite size. Powder diffraction profile analysis requires an instrument calibration standard to correct data for instrumental profiles due to the system optics. A general reference material, LaB 6 , has been established. The pattern of this LaB 6 powder can be used to generate a reference pattern for any other substance. Through three applications, it has been shown that this LaB 6 sample can be used to remove the instrumental broadenings and gives reasonable size and strain estimates in the profile analysis of other materials. Many previous studies have shown that the solid state reactivity and physical properties of some ceramic materials can be substantially enhanced. XPDPA techniques have been used to study the plastic deformation and the reduction of crystallite size for eight shock-modified ceramic materials. The size and strain values of these materials are correlated with shock parameters

  3. Directional fine structure in absorption of white x rays: A tomographic interpretation

    International Nuclear Information System (INIS)

    Korecki, P.; Szymonski, M.; Tolkiehn, M.; Novikov, D. V.; Materlik, G.

    2006-01-01

    We discuss directional fine structure in absorption of white x rays for tomographic imaging of crystal structure at the atomic level. The interference between a direct x-ray beam and the secondary waves coherently scattered inside a specimen modifies the total wave field at the position of the absorbing atoms. For a white x-ray beam, the wave field variations cancel out by energy integration for all directions, except for the near forward scattering components, coinciding with the incident beam. Therefore, two-dimensional patterns of the angular-dependent fine structure in absorption of white x rays can be interpreted as real-space projections of atomic structure. In this work, we present a theory describing the directional fine structure in white x-ray absorption and a tomographic approach for crystal structure retrieval developed on its basis. The tomographic algorithm is applied to the experimental x-ray absorption data recorded for GaP crystals

  4. X-ray Structure of the Mature Ectodomain of Phogrin

    Energy Technology Data Exchange (ETDEWEB)

    Noguera, M. E. [National Univ. of Quilmes, Buenos Aires (Argentina); Primo, M. [Univ. of Buenos Aires (Argentina); Jakoncic, J. [Brookhaven National Lab. (BNL), Upton, NY (United States); Poskus, E. [Univ. of Buenos Aires (Argentina); Solimena, M. [Dresden Univ. of Technology and Max Planck Inst. of Molecular Cell Biology and Genetics (Germany); Ermacora, M. R. [National Univ. of Quilmes and Multidisciplinary Inst. of Cellular Biology, Buenos Aires (Argentina)

    2014-11-26

    Phogrin/IA-2β and ICA512/IA-2 are two paralogs receptor-type protein-tyrosine phosphatases (RPTP) that localize in secretory granules of various neuroendocrine cells. In pancreatic islet β-cells, they participate in the regulation of insulin secretion, ensuring proper granulogenesis, and β-cell proliferation. The role of their cytoplasmic tail has been partially unveiled, while that of their luminal region remains unclear. To advance the understanding of its structure–function relationship, the X-ray structure of the mature ectodomain of phogrin (ME phogrin) at pH 7.4 and 4.6 has been solved at 1.95- and 2.01-Å resolution, respectively. Likewise to the ME of ICA512, ME phogrin adopts a ferredoxin-like fold: a sheet of four antiparallel β-strands packed against two α-helices. Furthermore, sequence conservation among vertebrates, plants and insects suggests that the structural similarity extends to all the receptor family. Crystallized ME phogrin is monomeric, in agreement with solution studies but in striking contrast with the behavior of homodimeric ME ICA512. The structural details that may cause the quaternary structure differences are analyzed. The results provide a basis for building models of the overall orientation and oligomerization state of the receptor in biological membranes.

  5. 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

    International Nuclear Information System (INIS)

    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. - Highlights: ► LIBS, XRF and XRD analyses of medieval white-clay ceramic tiles fragments are done. ► Different elements and phases, presented in the ceramics fragments were determined. ► Differences in the tiles' raw material mineral composition are found. ► Information of the tiles' production process and the raw clay deposits is obtained

  6. 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

    Energy Technology Data Exchange (ETDEWEB)

    Blagoev, K., E-mail: kblagoev@issp.bas.bg [Institute of Solid State Physics, Bulgarian Academy of Sciences, 72 Tzarigradsko Chaussee, 1784 Sofia (Bulgaria); Grozeva, M., E-mail: margo@issp.bas.bg [Institute of Solid State Physics, Bulgarian Academy of Sciences, 72 Tzarigradsko Chaussee, 1784 Sofia (Bulgaria); Malcheva, G., E-mail: bobcheva@issp.bas.bg [Institute of Solid State Physics, Bulgarian Academy of Sciences, 72 Tzarigradsko Chaussee, 1784 Sofia (Bulgaria); Neykova, S., E-mail: sevdalinaneikova@abv.bg [National Institute of Archaeology with Museum, Bulgarian Academy of Sciences, 2 Saborna, 1000 Sofia (Bulgaria)

    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. - Highlights: ► LIBS, XRF and XRD analyses of medieval white-clay ceramic tiles fragments are done. ► Different elements and phases, presented in the ceramics fragments were determined. ► Differences in the tiles' raw material mineral composition are found. ► Information of the tiles' production process and the raw clay deposits is obtained.

  7. X-ray structure determination and deuteration of nattokinase.

    Science.gov (United States)

    Yanagisawa, Yasuhide; Chatake, Toshiyuki; Naito, Sawa; Ohsugi, Tadanori; Yatagai, Chieko; Sumi, Hiroyuki; Kawaguchi, Akio; Chiba-Kamosida, Kaori; Ogawa, Megumi; Adachi, Tatsumi; Morimoto, Yukio

    2013-11-01

    Nattokinase (NK) is a strong fibrinolytic enzyme, which is produced in abundance by Bacillus subtilis natto. Although NK is a member of the subtilisin family, it displays different substrate specificity when compared with other subtilisins. The results of molecular simulations predict that hydrogen arrangements around Ser221 at the active site probably account for the substrate specificity of NK. Therefore, neutron crystallographic analysis should provide valuable information that reveals the enzymatic mechanism of NK. In this report, the X-ray structure of the non-hydrogen form of undeuterated NK was determined, and the preparation of deuterated NK was successfully achieved. The non-hydrogen NK structure was determined at 1.74 Å resolution. The three-dimensional structures of NK and subtilisin E from Bacillus subtilis DB104 are near identical. Deuteration of NK was carried out by cultivating Bacillus subtilis natto in deuterated medium. The D2O resistant strain of Bacillus subtilis natto was obtained by successive cultivation rounds, in which the concentration of D2O in the medium was gradually increased. NK was purified from the culture medium and its activity was confirmed by the fibrin plate method. The results lay the framework for neutron protein crystallography analysis.

  8. Computer x-ray powder diffraction patterns and densities for corundum, aluminium, zirconium, delta-UZr2 and the zirconium hydrides

    International Nuclear Information System (INIS)

    Ferguson, I.F.

    1976-11-01

    The computer-calculated X-ray powder diffraction patterns and theoretical densities of α-Al 2 O 3 ; Al; α-Zr; β-Zr; delta-UZr 2 ; γ, delta - and epsilon-zirconium hydrides are presented. Brief comments are given on some of the published X-ray powder diffraction data on these phases. (author)

  9. Fast synchrotron X-ray tomography study of the rod packing structures

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Xiaodan; Xia Chengjie; Sun Haohua; Wang Yujie [Department of Physics, Shanghai Jiao Tong University, 800 Dong Chuan Road, Shanghai 200240 (China)

    2013-06-18

    We present a fast synchrotron X-ray tomography study of the packing structures of rods under tapping. Utilizing the high flux of the X-rays generated from the third-generation synchrotron source, we can complete a tomography scan within several seconds, after which the three-dimensional (3D) packing structure can be obtained for the subsequent structural analysis. Due to the high-energy nature of the X-ray beam, special image processing steps including image phase-retrieval has been implemented. Overall, this study suggests the possibility of acquiring statistically significant static packing structures within a reasonable time scale using high-intensity X-ray sources.

  10. Validation of powder X-ray diffraction following EN ISO/IEC 17025.

    Science.gov (United States)

    Eckardt, Regina; Krupicka, Erik; Hofmeister, Wolfgang

    2012-05-01

    Powder X-ray diffraction (PXRD) is used widely in forensic science laboratories with the main focus of qualitative phase identification. Little is found in literature referring to the topic of validation of PXRD in the field of forensic sciences. According to EN ISO/IEC 17025, the method has to be tested for several parameters. Trueness, specificity, and selectivity of PXRD were tested using certified reference materials or a combination thereof. All three tested parameters showed the secure performance of the method. Sample preparation errors were simulated to evaluate the robustness of the method. These errors were either easily detected by the operator or nonsignificant for phase identification. In case of the detection limit, a statistical evaluation of the signal-to-noise ratio showed that a peak criterion of three sigma is inadequate and recommendations for a more realistic peak criterion are given. Finally, the results of an international proficiency test showed the secure performance of PXRD. © 2012 American Academy of Forensic Sciences.

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

    Science.gov (United States)

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

    2017-07-01

    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 TiO 2 for different emission countries are evidenced. The counterfeit banknotes are composed of cellulose based on wood pulp; moreover, an unexpected significant quantity of TiO 2 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. © 2017 American Academy of Forensic Sciences.

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

    Science.gov (United States)

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

    2011-01-01

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

  13. X-ray photoemission spectroscopy (XPS) and extended x-ray absorption fine structure (EXAFS) studies of silicate based glasses

    International Nuclear Information System (INIS)

    Karim, D.; Lam, D.J.

    1979-01-01

    The application of the x-ray photoemission spectroscopy (XPS) technique to study the electronic structure and bonding of heavy metal oxides in alkali- and alkali-earth-silicate glasses had been demonstrated. The bonding characteristics of the iron oxide and uranium oxide in sodium silicate glasses were deduced from the changes in the oxygen 1s levels and the heavy metal core levels. It is reasonable to expect that the effect of leaching on the heavy metal ions can be monitored using the appropriate core levels of these ions. To study the effect of leaching on the glass forming network, the valence band structure of the bridging and nonbridging oxygens in sodium silicate glasses were investigated. The measurement of extended x-ray absorption fine-structure (EXAFS) is a relatively new analytical technique for obtaining short range (<5 A) structural information around atoms of a selected species in both solid and fluid systems. Experiments have recently begun to establish the feasibility of using EXAFS to study the bonding of actinides in silicate glasses. Because of the ability of EXAFS to yield specific structural data even in complex multicomponent systems, it could prove to be an invaluable tool in understanding glass structure

  14. Microanalysis of iron oxidation state in iron oxides using X Ray Absorption Near Edge Structure (XANES)

    Science.gov (United States)

    Sutton, S. R.; Delaney, J.; Bajt, S.; Rivers, M. L.; Smith, J. V.

    1993-01-01

    An exploratory application of x ray absorption near edge structure (XANES) analysis using the synchrotron x ray microprobe was undertaken to obtain Fe XANES spectra on individual sub-millimeter grains in conventional polished sections. The experiments concentrated on determinations of Fe valence in a suite of iron oxide minerals for which independent estimates of the iron speciation could be made by electron microprobe analysis and x ray diffraction.

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

    International Nuclear Information System (INIS)

    Tanaka, M; Katsuya, Y; Matsushita, Y

    2013-01-01

    The focused-beam flat-sample method (FFM), which is a method for high-resolution and rapid synchrotron X-ray powder diffraction measurements by combination of beam focusing optics, a flat shape sample and an area detector, was applied for diffraction experiments with anomalous scattering effect. The advantages of FFM for anomalous diffraction were absorption correction without approximation, rapid data collection by an area detector and good signal-to-noise ratio data by focusing optics. In the X-ray diffraction experiments of CoFe 2 O 4 and Fe 3 O 4 (By FFM) using X-rays near the Fe K absorption edge, the anomalous scattering effect between Fe/Co or Fe 2+ /Fe 3+ can be clearly detected, due to the change of diffraction intensity. The change of observed diffraction intensity as the incident X-ray energy was consistent with the calculation. The FFM is expected to be a method for anomalous powder diffraction.

  16. X-Ray and Neutron Scattering Study of the Magnetic Structure of Neodymium Metal

    DEFF Research Database (Denmark)

    Lebech, Bente; Als-Nielsen, Jens Aage; McEwen, K. A.

    1979-01-01

    A combined x-ray and neutron diffraction study has shown that the so-called "triple-q⃗" structure is not the correct model of the magnetic structure of neodymium. The x-ray data showed only the Bragg reflections originating from the double-hcp lattice. Hence, all additional reflections observed...

  17. Discovery of novel inhibitors for DHODH via virtual screening and X-ray crystallographic structures

    Energy Technology Data Exchange (ETDEWEB)

    McLean, Larry R.; Zhang, Ying; Degnen, William; Peppard, Jane; Cabel, Dasha; Zou, Chao; Tsay, Joseph T.; Subramaniam, Arun; Vaz, Roy J.; Li, Yi (Sanofi)

    2010-10-28

    Amino-benzoic acid derivatives 1-4 were found to be inhibitors for DHODH by virtual screening, biochemical, and X-ray crystallographic studies. X-ray structures showed that 1 and 2 bind to DHODH as predicted by virtual screening, but 3 and 4 were found to be structurally different from the corresponding compounds initially identified by virtual screening.

  18. Synthesis and X-ray structure of the dysprosium(III) complex derived ...

    African Journals Online (AJOL)

    Synthesis and X-ray structure of the dysprosium(III) complex derived from the ligand 5-chloro-1 ... Bulletin of the Chemical Society of Ethiopia ... synthesized and its crystal structure determined by single X-ray diffraction at room temperature.

  19. Powder X-ray diffraction method for the quantification of cocrystals in the crystallization mixture.

    Science.gov (United States)

    Padrela, Luis; de Azevedo, Edmundo Gomes; Velaga, Sitaram P

    2012-08-01

    The solid state purity of cocrystals critically affects their performance. Thus, it is important to accurately quantify the purity of cocrystals in the final crystallization product. The aim of this study was to develop a powder X-ray diffraction (PXRD) quantification method for investigating the purity of cocrystals. The method developed was employed to study the formation of indomethacin-saccharin (IND-SAC) cocrystals by mechanochemical methods. Pure IND-SAC cocrystals were geometrically mixed with 1:1 w/w mixture of indomethacin/saccharin in various proportions. An accurately measured amount (550 mg) of the mixture was used for the PXRD measurements. The most intense, non-overlapping, characteristic diffraction peak of IND-SAC was used to construct the calibration curve in the range 0-100% (w/w). This calibration model was validated and used to monitor the formation of IND-SAC cocrystals by liquid-assisted grinding (LAG). The IND-SAC cocrystal calibration curve showed excellent linearity (R(2) = 0.9996) over the entire concentration range, displaying limit of detection (LOD) and limit of quantification (LOQ) values of 1.23% (w/w) and 3.74% (w/w), respectively. Validation results showed excellent correlations between actual and predicted concentrations of IND-SAC cocrystals (R(2) = 0.9981). The accuracy and reliability of the PXRD quantification method depend on the methods of sample preparation and handling. The crystallinity of the IND-SAC cocrystals was higher when larger amounts of methanol were used in the LAG method. The PXRD quantification method is suitable and reliable for verifying the purity of cocrystals in the final crystallization product.

  20. Structure and dynamics in liquid water from x-ray absorption spectroscopy

    International Nuclear Information System (INIS)

    Wernet, Philippe

    2009-01-01

    Oxygen K-edge x-ray absorption spectra of water are discussed. The spectra of gas-phase water, liquid water and ice illustrate the sensitivity of oxygen K-edge x-ray absorption spectroscopy to hydrogen bonding in water. Transmission mode spectra of amorphous and crystalline ice are compared to x-ray Raman spectra of ice. The good agreement consolidates the experimental spectrum of crystalline ice and represents an incentive for theoretical calculations of the oxygen K-edge absorption spectrum of crystalline ice. Time-resolved infrared-pump and x-ray absorption probe results are finally discussed in the light of this structural interpretation.

  1. X-ray CT analysis of pore structure in sand

    Science.gov (United States)

    Mukunoki, Toshifumi; Miyata, Yoshihisa; Mikami, Kazuaki; Shiota, Erika

    2016-06-01

    The development of microfocused X-ray computed tomography (CT) devices enables digital imaging analysis at the pore scale. The applications of these devices are diverse in soil mechanics, geotechnical and geoenvironmental engineering, petroleum engineering, and agricultural engineering. In particular, the imaging of the pore space in porous media has contributed to numerical simulations for single-phase and multiphase flows or contaminant transport through the pore structure as three-dimensional image data. These obtained results are affected by the pore diameter; therefore, it is necessary to verify the image preprocessing for the image analysis and to validate the pore diameters obtained from the CT image data. Moreover, it is meaningful to produce the physical parameters in a representative element volume (REV) and significant to define the dimension of the REV. This paper describes the underlying method of image processing and analysis and discusses the physical properties of Toyoura sand for the verification of the image analysis based on the definition of the REV. On the basis of the obtained verification results, a pore-diameter analysis can be conducted and validated by a comparison with the experimental work and image analysis. The pore diameter is deduced from Young-Laplace's law and a water retention test for the drainage process. The results from previous study and perforated-pore diameter originally proposed in this study, called the voxel-percolation method (VPM), are compared in this paper. In addition, the limitations of the REV, the definition of the pore diameter, and the effectiveness of the VPM for an assessment of the pore diameter are discussed.

  2. Application of combined multivariate techniques for the description of time-resolved powder X-ray diffraction data

    Czech Academy of Sciences Publication Activity Database

    Taris, A.; Grosso, M.; Brundu, M.; Guida, V.; Viani, Alberto

    2017-01-01

    Roč. 50, č. 2 (2017), s. 451-461 ISSN 1600-5767 R&D Projects: GA MŠk(CZ) LO1219 Keywords : in situ X-ray powder diffraction * amorphous content * chemically bonded ceramic s * statistical total correlation spectroscopy * multivariate curve resolution Subject RIV: JJ - Other Materials OBOR OECD: Materials engineering Impact factor: 2.495, year: 2016 http://journals.iucr.org/j/issues/2017/02/00/ap5006/index.html

  3. Time-resolved pump-probe X-ray absorption fine structure spectroscopy of Gaq3

    International Nuclear Information System (INIS)

    Dicke, Benjamin

    2013-01-01

    of Gaq 3 was analyzed and presents one of the first time-resolved measurements at PETRA III. In addition to pump-probe XAFS spectroscopy, different phases of Gaq 3 and Alq 3 in form of powder, crystal, film and solution were analyzed by means of UV-VIS and fluorescence spectroscopy. Electronic and optical differences of the molecules related to the particular form could be revealed. Gaq 3 in benzyl alcohol solution and Gaq 3 in crystalline form exhibit very similar optical features, indicating similar structural properties. The various preparation techniques used to obtain the sample forms are presented in this thesis. Analyzing the differences among the diverse sample forms helps to answer the question on how the conclusions extracted from sample systems in liquid form can be transferred to the ones in crystal form or film form, the latter appearing in organic light emitting diodes. The future goal of this research project is the direct measurement of the excited state structure of Alq 3 as well as Gaq 3 , and similar sample systems by time-resolved X-ray crystallography. The sample crystals have to fulfill specific requirements especially for the laser induced photoexcitation process. In this thesis a newly developed preparation method for low roughness singe crystal slices is presented. These crystal slices can be used for future perspective time-resolved X-ray crystallography experiments.

  4. X-ray tomography investigations on pebble bed structures

    International Nuclear Information System (INIS)

    Reimann, J.; Rolli, R.; Pieritz, R.A.; Ferrero, C.; Di Michiel, M.

    2007-01-01

    Granular materials (pebbles) are used in present ceramic breeder blankets both for the ceramic breeder material and beryllium. The thermal-mechanical behaviour of these pebble beds strongly depends on the arrangement of the pebbles in the bed, their contacts and contact surfaces with other pebbles and with walls. The influence of these quantities is most pronounced for beryllium pebble beds because of the large thermal conductivity ratio of beryllium to helium gas atmosphere. At present, the data base for the pebble bed thermal conductivity (k) and heat transfer coefficient (h) is quite limited for compressed beds and significant discrepancies exist in respect to h. The detailed knowledge of the pebble bed topology is, therefore, essential to better understand the heat transfer mechanisms. In the present work, results from detailed X-ray tomography investigations are reported on pebble topology in i) the pebble bed bulk (which is relevant for k), and ii) the region close to walls with thicknesses of several pebble diameters (relevant for h). At Forschungszentrum Karlsruhe, pebble beds consisting of aluminium spheres with diameters of 2.3 and 5 mm, respectively, (simulating the blanket relevant 1 mm beryllium pebbles), were uniaxially compressed at different pressure levels. High resolution three-dimensional microtomography (MT) experiments were subsequently performed at the European Synchrotron Radiation Facility, Grenoble. Radial and axial void fraction distributions were found to be oscillatory next to the walls and non-oscillatory in the bulk. For non-compressed pebble beds, the bulk void fraction is fairly constant; for compressed beds, a gradient exists along the compression axis. In the bulk, the angular distribution of pebble contacts was found to be fairly constant, indicating that no regular packing structure is induced. In the wall region, the pebble layer touching the wall is composed of zones with hexagonal structures as shown clearly by MT images. This

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

    DEFF Research Database (Denmark)

    Frankær, Christian Grundahl

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

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

    Science.gov (United States)

    Crouse, David T.

    2007-01-01

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

  7. Effects of proton irradiation on structure of NdFeB permanent magnets studied by X-ray diffraction and X-ray absorption fine structure

    International Nuclear Information System (INIS)

    Yang, L.; Zhen, L.; Xu, C.Y.; Sun, X.Y.; Shao, W.Z.

    2011-01-01

    The effects of proton irradiation on the structure of NdFeB permanent magnet were investigated by X-ray diffraction and X-ray absorption fine structure (XAFS). The results reveal that proton irradiation has no effect on the long-range structure, but significantly affects the atomic local structure of the NdFeB magnet. The alignment degree of the magnet decreases and the internal stress of the lattice increases after proton irradiation. XAFS results show that the coordination number of Fe-Nd in the first neighboring coordination shell of the Fe atoms decreases and the disorder degree increases.

  8. Effects of proton irradiation on structure of NdFeB permanent magnets studied by X-ray diffraction and X-ray absorption fine structure

    Energy Technology Data Exchange (ETDEWEB)

    Yang, L. [School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001 (China); Zhen, L., E-mail: lzhen@hit.edu.c [School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001 (China); Xu, C.Y.; Sun, X.Y.; Shao, W.Z. [School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001 (China)

    2011-01-15

    The effects of proton irradiation on the structure of NdFeB permanent magnet were investigated by X-ray diffraction and X-ray absorption fine structure (XAFS). The results reveal that proton irradiation has no effect on the long-range structure, but significantly affects the atomic local structure of the NdFeB magnet. The alignment degree of the magnet decreases and the internal stress of the lattice increases after proton irradiation. XAFS results show that the coordination number of Fe-Nd in the first neighboring coordination shell of the Fe atoms decreases and the disorder degree increases.

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

  10. A structural study of ceramic oxides by X-ray absorption spectroscopy

    International Nuclear Information System (INIS)

    Akhtar, M.J.

    1995-01-01

    A detailed structural study of ceramic oxides is presented by employing X-ray Absorption Spectroscopy (XAS). In the present work X-ray Absorption Near Edge Structure (XANES) is used for the investigation of valence state of metal cations; whereas, Extended X-ray Absorption Fine Structure EXAFS) is employed for the determination for bond lengths, coordination numbers and nature of the elements present in the near neighbour shells surrounding the absorbing atom. These results show that local environment of dopant and host cations are different; and this variation in local structure depends on the nature and concentration of the dopant ions. (author)

  11. Hydrogen atoms in protein structures: high-resolution X-ray diffraction structure of the DFPase

    Science.gov (United States)

    2013-01-01

    Background Hydrogen atoms represent about half of the total number of atoms in proteins and are often involved in substrate recognition and catalysis. Unfortunately, X-ray protein crystallography at usual resolution fails to access directly their positioning, mainly because light atoms display weak contributions to diffraction. However, sub-Ångstrom diffraction data, careful modeling and a proper refinement strategy can allow the positioning of a significant part of hydrogen atoms. Results A comprehensive study on the X-ray structure of the diisopropyl-fluorophosphatase (DFPase) was performed, and the hydrogen atoms were modeled, including those of solvent molecules. This model was compared to the available neutron structure of DFPase, and differences in the protein and the active site solvation were noticed. Conclusions A further examination of the DFPase X-ray structure provides substantial evidence about the presence of an activated water molecule that may constitute an interesting piece of information as regard to the enzymatic hydrolysis mechanism. PMID:23915572

  12. Attosecond time-energy structure of X-ray free-electron laser pulses

    Science.gov (United States)

    Hartmann, N.; Hartmann, G.; Heider, R.; Wagner, M. S.; Ilchen, M.; Buck, J.; Lindahl, A. O.; Benko, C.; Grünert, J.; Krzywinski, J.; Liu, J.; Lutman, A. A.; Marinelli, A.; Maxwell, T.; Miahnahri, A. A.; Moeller, S. P.; Planas, M.; Robinson, J.; Kazansky, A. K.; Kabachnik, N. M.; Viefhaus, J.; Feurer, T.; Kienberger, R.; Coffee, R. N.; Helml, W.

    2018-04-01

    The time-energy information of ultrashort X-ray free-electron laser pulses generated by the Linac Coherent Light Source is measured with attosecond resolution via angular streaking of neon 1s photoelectrons. The X-ray pulses promote electrons from the neon core level into an ionization continuum, where they are dressed with the electric field of a circularly polarized infrared laser. This induces characteristic modulations of the resulting photoelectron energy and angular distribution. From these modulations we recover the single-shot attosecond intensity structure and chirp of arbitrary X-ray pulses based on self-amplified spontaneous emission, which have eluded direct measurement so far. We characterize individual attosecond pulses, including their instantaneous frequency, and identify double pulses with well-defined delays and spectral properties, thus paving the way for X-ray pump/X-ray probe attosecond free-electron laser science.

  13. Local structure studies of Fe{sub 2}TeO{sub 6} using x-ray absorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Singh, Harishchandra, E-mail: singh85harish@gmail.com [Homi Bhabha National Institute, Raja Ramanna Centre for Advanced Technology, Indore-452013 (India); Indus Synchrotron Utilization Division, Raja Ramanna Centre for Advanced Technology, Indore-452013 (India); Yadav, A. K. [Atomic & Molecular Physics Division Bhabha Atomic Research Centre, Mumbai – 400 094 (India)

    2016-05-23

    In the present study, we have performed EXAFS measurements on powder samples of Fe{sub 2}TeO{sub 6} (FTO) to probe the local structure surrounding at the Fe site. The structural parameters (atomic coordination and lattice parameters) of FTO used for simulation of theoretical EXAFS spectra of the samples have been obtained from Rietveld refined structure on synchrotron X-ray Diffraction (SXRD) data. Quite similar and satisfactory structural parameters have been obtained from both the study, indicating goodness of synchrotron structural analysis over EXAFS analysis. SXRD and EXAFS results shows absence of any secondary phase proves current synthesis superior over reported techniques.

  14. Structural study of (N{sub 2}H{sub 5},H){sub 2.9}U{sub 1.1}Ce{sub 0.9}(C{sub 2}O{sub 4}){sub 5}·10H{sub 2}O from a conventional X-ray diffraction diagram obtained on a powder synthesized by a fast vortex process

    Energy Technology Data Exchange (ETDEWEB)

    Brackx, E., E-mail: Emmanuelle.brackx@cea.fr [CEA, DEN, DTEC, SGCS, LMAC, Marcoule, 30207 Bagnols sur Cèze (France); Laval, J.P. [Centre Européen de la Céramique, SPCTS, UMR-CNRS 7315, Université de Limoges, Faculté des Sciences, 12 rue Atlantis, 87068 Limoges (France); Dugne, O. [CEA, DEN, DTEC, SGCS, LMAC, Marcoule, 30207 Bagnols sur Cèze (France); Feraud, J.P. [CEA, DEN, DTEC, SGCS, LGCI, Marcoule, 30207 Bagnols sur Cèze (France); Arab-Chapelet, B. [CEA, DEN, DRCP, SCPS, LC2A, Marcoule, 30207 Bagnols sur Cèze (France)

    2015-01-15

    In the context of research on U/minor actinides for nuclear fuel reprocessing in the transmutation process, developments are first studied with surrogates containing uranium and lanthanides to facilitate testing. The tests consist of precipitating and calcining a hydrazinium uranium/cerium oxalate. The structure of this oxalate had not been previously determined, but was necessary to validate the physicochemical mechanisms involved. The present study, firstly demonstrates the structural similarity of the U/Ce oxalate phase (N{sub 2}H{sub 5},H){sub 2.9}U{sub 1.1}Ce{sub 0.9}(C{sub 2}O{sub 4}){sub 5}·10H{sub 2}O, synthesized using a vortex precipitator for continuous synthesis of actinide oxalates, with previously known oxalates, crystallizing in P6{sub 3}/mmc symmetry, obtained by more classical methods. This fast precipitation process induces massive nucleation of fine powders. Their structural and microstructural determination confirms that the raw and dried phases belong to the same structural family as (NH{sub 4}){sub 2}U{sub 2}(C{sub 2}O{sub 4}){sub 5}·0.7H{sub 2}O whose structure was described by Chapelet-Arab in P6{sub 3}/mmc symmetry, using single crystal data. However, they present an extended disorder inside the tunnels of the structure, even after drying at 100 °C, between water and hydrazinium ions. This disorder is directly related to the fast vortex method. This structure determination can be used as a basis for further semi-quantitative analysis on the U/minor actinides products formed under various experimental conditions. - Highlights: • Uranium cerium oxalate precipitate characterization by X-ray powder diffraction. • Morphology characterization by SEM analysis. • Structure determination by unit cell Rietveld refinement.

  15. Preparation and characterization of analcime powders by x-ray and sem analyses

    Czech Academy of Sciences Publication Activity Database

    Kohoutková, Martina; Kloužková, A.; Maixner, J.; Mrázová, M.

    2007-01-01

    Roč. 51, č. 1 (2007), s. 9-14 ISSN 0862-5468 R&D Projects: GA MPO 2A-1TP1/063 Institutional research plan: CEZ:AV0Z40320502 Keywords : analcime * hydrothermal synthesis * X-ray diffraction Subject RIV: CA - Inorganic Chemistry Impact factor: 0.488, year: 2007

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

    International Nuclear Information System (INIS)

    Pawloski, G.A.

    1986-01-01

    A method is described of quantitatively determining the mineral composition in a test sample containing a number (m) of minerals from a group (n) of known minerals, wherein n=13, where mless than or equal ton, by x-ray diffraction, comprising: determining from standard samples of the known minerals a set of (n) standard coefficients K/sub j/=(X/sub j//X/sub l/)(I/sub l//I/sub j/) for each mineral (j=2...n) in the group of known minerals (j=2...n) relative to one mineral (l) in the group selected as a reference mineral, where X is the weight fraction of the mineral in a standard sample, and I is the x-ray integrated intensity peak of each mineral obtained from the standard sample; obtaining an x-ray diffraction pattern of the test sample; identifying each of the (m) minerals in the test sample for the x-ray diffraction pattern; calculating the relative weight fractions X/sub j//X/sub l/ for each mineral (j=2...m) compared to the reference mineral (l) from the ratio of the measured highest integrated intensity peak I/sub j/ of each mineral in the test sample to the measured highest integrated intensity peak I/sub l/ of the reference mineral in the test sample, and from the previously determined standard coefficients, X/sub j//X/sub l/=K/sub j/(I/sub j//I/sub l/

  17. 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 lithium-ion batteries

    Science.gov (United States)

    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 ∼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 distribution-function (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 Li2MnSiO4 nanoparticles. The XRD patters of the discharged (lithiated) samples exhibit a long-range ordered structure characteristic of the (β) Li2MnSiO4 crystalline phase (space group Pmn21) 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.

  18. The structure of the coronal soft X-ray source associated with the dark filament disappearance of 1991 September 28 using the Yohkoh Soft X-ray Telescope

    Science.gov (United States)

    Mcallister, Alan; Uchida, Yutaka; Tsuneta, Saku; Strong, Keith T.; Acton, Loren W.; Hiei, Eijiro; Bruner, Marilyn E.; Watanabe, Takashi; Shibata, Kazunari

    1992-01-01

    The structure of the coronal soft X-ray source associated with the dark filament disappearance on September 28, 1991, observed with the Soft X-ray Telescope, is examined as a possible example of the 'eruption-reconnection' model of filament disappearance. The results suggest, however, that this model may not fit. There is a strong possibility that much of the dark filament mass remains in the heated unwinding axial field.

  19. Synthesis, X-ray crystal structure, DNA binding and Nuclease activity ...

    Indian Academy of Sciences (India)

    s12039-016-1125-x. Synthesis, X-ray crystal structure, DNA binding and Nuclease activity of lanthanide(III) complexes of 2-benzoylpyridine acetylhydrazone. KARREDDULA RAJA, AKKILI SUSEELAMMA and KATREDDI HUSSAIN REDDY. ∗.

  20. Structural and microstructural characterization of U{sub 3}Si{sub 2} nuclear fuel using X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Ichikawa, Rodrigo U.; Garcia, Rafael H.L.; Silva, Andre S.B. da; Saliba-Silva, Adonis M.; Lima, Nelson B.; Martinez, Luis G. [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Turrillas, Xavier, E-mail: ichikawa@usp.br, E-mail: rlgarcia@ipen.br, E-mail: andre.santos.silva@usp.br, E-mail: saliba@ipen.br, E-mail: nblima@ipen.br, E-mail: lgallego@ipen.br, E-mail: xturrillas@icmab.es [Institut de Ciència de Materials de Barcelona (ICMAB/CSIC), Cerdanyola de Vallès (Spain)

    2017-07-01

    In this work, two uranium silicide powdered samples, containing 67% and 42 mol% of Si, were analyzed using X-ray diffraction (named as {sup 67}Si and {sup 42}Si). For structural characterization, Rietveld refinement was used to estimate cell parameters, volume fraction (weight percent) of crystalline phases and atomic positions. For the main phases, X-ray line profile analysis (XLPA) was used to estimate mean crystallite sizes and micro strains. The {sup 67}Si sample presents higher content of USi{sub 2(}tetragonal) and the {sup 42}Si sample presents higher content of U{sub 3}Si{sub 2} (tetragonal) as identified and calculated from the XRD profiles. Overall there are no appreciable structural changes and the parameters refined are in good accordance with the ones reported in the literature. Mean crystallite sizes determined by XLPA revealed small crystallites of the order of 10{sup 1} nm and low micro strain for all samples. (author)

  1. The atomic scale structure of CXV carbon: wide-angle x-ray scattering and modeling studies.

    Science.gov (United States)

    Hawelek, L; Brodka, A; Dore, J C; Honkimaki, V; Burian, A

    2013-11-13

    The disordered structure of commercially available CXV activated carbon produced from finely powdered wood-based carbon has been studied using the wide-angle x-ray scattering technique, molecular dynamics and density functional theory simulations. The x-ray scattering data has been converted to the real space representation in the form of the pair correlation function via the Fourier transform. Geometry optimizations using classical molecular dynamics based on the reactive empirical bond order potential and density functional theory at the B3LYP/6-31g* level have been performed to generate nanoscale models of CXV carbon consistent with the experimental data. The final model of the structure comprises four chain-like and buckled graphitic layers containing a small percentage of four-fold coordinated atoms (sp(3) defects) in each layer. The presence of non-hexagonal rings in the atomic arrangement has been also considered.

  2. Sample cell for powder x-ray diffraction at up to 500 bars and 200 deg. C

    International Nuclear Information System (INIS)

    Jupe, Andrew C.; Wilkinson, Angus P.

    2006-01-01

    A low cost sample cell for powder diffraction at high pressure and temperature that employs either sapphire or steel pressure tubes is described. The cell can be assembled rapidly, facilitating the study of chemically reacting systems, and it provides good control of both pressure and temperature in a regimen where diamond anvil cells and multianvil apparatus cannot be used. The design provides a relatively large sample volume making it suitable for the study of quite large grain size materials, such as hydrating cement slurries. However, relatively high energy x rays are needed to penetrate the pressure tube

  3. A program for the derivation of crystal unit cell parameters from X-ray powder diffraction measurements

    International Nuclear Information System (INIS)

    Ferguson, I.F.; Rogerson, A.H.

    1984-01-01

    The program, FIRESTAR, determines the dimensions of a crystallographic unit cell from a set of X-ray powder diffraction measurements corresponding to a set of Bragg reflections, provided that the crystal system applicable is known and the Bragg reflections have been indexed. The program includes a range of possible extrapolation functions, and the data may be weighted. Provision is made for detecting and rejecting a single 'bad' measurement, and then rejecting measurements which lie outside an error limit set in the input data. (orig.)

  4. Photovoltaic X-ray detectors based on epitaxial GaAs structures

    Energy Technology Data Exchange (ETDEWEB)

    Achmadullin, R.A. [Institute of Radio Engineering and Electronics, Russian Academy of Sciences, 1 Ac. Vvedenski square, Fryazino 141190, Moscow region (Russian Federation); Artemov, V.V. [Shubnikov Institute of Crystallography, Russian Academy of Sciences, 59 Leninski pr., Moscow B-333, 117333 (Russian Federation); Dvoryankin, V.F. [Institute of Radio Engineering and Electronics, Russian Academy of Sciences, 1 Ac. Vvedenski square, Fryazino 141190, Moscow region (Russian Federation)]. E-mail: vfd217@ire216.msk.su; Dvoryankina, G.G. [Institute of Radio Engineering and Electronics, Russian Academy of Sciences, 1 Ac. Vvedenski square, Fryazino 141190, Moscow region (Russian Federation); Dikaev, Yu.M. [Institute of Radio Engineering and Electronics, Russian Academy of Sciences, 1 Ac. Vvedenski square, Fryazino 141190, Moscow region (Russian Federation); Ermakov, M.G. [Institute of Radio Engineering and Electronics, Russian Academy of Sciences, 1 Ac. Vvedenski square, Fryazino 141190, Moscow region (Russian Federation); Ermakova, O.N. [Institute of Radio Engineering and Electronics, Russian Academy of Sciences, 1 Ac. Vvedenski square, Fryazino 141190, Moscow region (Russian Federation); Chmil, V.B. [Scientific State Center, High Energy Physics Institute, Protvino, Moscow region (Russian Federation); Holodenko, A.G. [Scientific State Center, High Energy Physics Institute, Protvino, Moscow region (Russian Federation); Kudryashov, A.A.; Krikunov, A.I.; Petrov, A.G.; Telegin, A.A. [Institute of Radio Engineering and Electronics, Russian Academy of Sciences, 1 Ac. Vvedenski square, Fryazino 141190, Moscow region (Russian Federation); Vorobiev, A.P. [Scientific State Center, High Energy Physics Institute, Protvino, Moscow region (Russian Federation)

    2005-12-01

    A new type of the photovoltaic X-ray detector based on epitaxial p{sup +}-n-n'-n{sup +} GaAs structures which provides a high efficiency of charge collection in the non-bias operation mode at room temperature is proposed. The GaAs epitaxial structures were grown by vapor-phase epitaxy on heavily doped n{sup +}-GaAs(1 0 0) substrates. The absorption efficiency of GaAs X-ray detector is discussed. I-V and C-V characteristics of the photovoltaic X-ray detectors are analyzed. The built-in electric field profiles in the depletion region of epitaxial structures are measured by the EBIC method. Charge collection efficiency to {alpha}-particles and {gamma}-radiation are measured. The application of X-ray detectors is discussed.

  5. Effect of powder sample granularity on fluorescent intensity and on thermal parameters in x-ray diffraction Rietveld analysis

    International Nuclear Information System (INIS)

    Sparks, C.J.; Specht, E.D.; Ice, G.E.; Kumar, R.; Zschack, P.; Shiraishi, T.; Hisatsune, K.

    1991-01-01

    The effect of sample granularity on diffracted x-ray intensity was evaluated by measuring the 2θ dependence of x-ray fluorescence from various samples. Measurements were made in the symmetric geometry on samples ranging from single crystals to highly absorbing coarse powders. A characteristic shape for the absorption correction was observed. A demonstration of the sensitivity of Rietveld refined site occupation parameters is made on CuAu and Cu 50 Au 44 Ni 6 alloys refined with and without granularity corrections. These alloys provide a good example of the effect of granularity due to their large linear x-ray absorption coefficients. Sample granularity and refined thermal parameters obtained from the Rietveld analysis were found to be correlated. Without a granularity correction, the refined thermal parameters are too low and can actually become negative in an attempt to compensate for granularity. A general shape for granularity correction can be included in refinement procedures. If no granularity correction is included, data should be restricted to above 30 degrees 2θ, and thermal parameters should be ignored unless extreme precautions are taken to produce >5 μm particles and high packing densities

  6. Techniques for materials research with synchrotron radiation x-rays

    International Nuclear Information System (INIS)

    Bowen, D.K.

    1983-01-01

    A brief introductory survey is presented of the properties and generation of synchrotron radiation and the main techniques developed so far for its application to materials problems. Headings are:synchrotron radiation; X-ray techniques in synchrotron radiation (powder diffraction; X-ray scattering; EXAFS (Extended X-ray Absorption Fine Structure); X-ray fluorescent analysis; microradiography; white radiation topography; double crystal topography); future developments. (U.K.)

  7. Hard X-ray Microscopy with Elemental, Chemical and Structural Contrast

    International Nuclear Information System (INIS)

    Schroer, C.G.; Boye, P.; Feldkamp, J.P.

    2010-01-01

    We review hard X-ray microscopy techniques with a focus on scanning microscopy with synchrotron radiation. Its strength compared to other microscopies is the large penetration depth of hard x rays in matter that allows one to investigate the interior of an object without destructive sample preparation. In combination with tomography, local information from inside of a specimen can be obtained, even from inside special non-ambient sample environments. Different X-ray analytical techniques can be used to produce contrast, such as X-ray absorption, fluorescence, and diffraction, to yield chemical, elemental, and structural information about the sample, respectively. This makes X-ray microscopy attractive to many fields of science, ranging from physics and chemistry to materials, geo-, and environmental science, biomedicine, and nanotechnology. Our scanning microscope based on nanofocusing refractive X-ray lenses has a routine spatial resolution of about 100 nm and supports the contrast mechanisms mentioned above. In combination with coherent X-ray diffraction imaging, the spatial resolution can be improved to the 10 nm range. The current state-of-the-art of this technique is illustrated by several examples, and future prospects of the technique are given. (author)

  8. X-rays in protoplanetary disks : Their impact on the thermal and chemical structure, a grid of models

    NARCIS (Netherlands)

    Aresu, G.; Kamp, I.; Meijerink, R.; Woitke, P.; Thi, W. F.; Spaans, M.C.

    X-rays impact protoplanetary disks hydrostatic, thermal and chemical structure. The range of efficiency of X-rays is explored using a grid modelling approach: different parameters affects the structure of the disk, this determines different contribution of the X-ray radiation to the chemistry and

  9. Bone structure investigation using X-ray and neutron radiography techniques

    International Nuclear Information System (INIS)

    Kamali Moghaddam, K.; Taheri, T.; Ayubian, M.

    2008-01-01

    In this paper we report a study of the periodic variation of bone tissue humidity immediately after death using both neutron and X-ray radiography techniques. After death, bone tissue experiences sequential change over time. This change consists of organic and inorganic phase variations of the bone structure, as well as gradual reduction of the bone's water content. These variations are investigated by periodically imaging dead bone using X-ray and neutron radiography. Chemical separation techniques such as calcification and decalcification were used to separate the organic and inorganic phases of the bone. Comparison between X-ray and neutron radiographs of bone following phase separation can be potentially used to investigate the bone disease or to determine a cause of death. In our experiments, we use adult rat femur bones, and the interpretations of these results are presented based on our understanding of bone structure and images produced by neutron and X-ray photon interactions

  10. Bone structure investigation using X-ray and neutron radiography techniques

    Energy Technology Data Exchange (ETDEWEB)

    Kamali Moghaddam, K. [Nuclear Research Center (NRC), Atomic Energy Organization of Iran (AEOI), P.O. Box 11365-8486, Tehran (Iran, Islamic Republic of)], E-mail: kkamali@aeoi.org.ir; Taheri, T.; Ayubian, M. [Nuclear Research Center (NRC), Atomic Energy Organization of Iran (AEOI), P.O. Box 11365-8486, Tehran (Iran, Islamic Republic of)

    2008-01-15

    In this paper we report a study of the periodic variation of bone tissue humidity immediately after death using both neutron and X-ray radiography techniques. After death, bone tissue experiences sequential change over time. This change consists of organic and inorganic phase variations of the bone structure, as well as gradual reduction of the bone's water content. These variations are investigated by periodically imaging dead bone using X-ray and neutron radiography. Chemical separation techniques such as calcification and decalcification were used to separate the organic and inorganic phases of the bone. Comparison between X-ray and neutron radiographs of bone following phase separation can be potentially used to investigate the bone disease or to determine a cause of death. In our experiments, we use adult rat femur bones, and the interpretations of these results are presented based on our understanding of bone structure and images produced by neutron and X-ray photon interactions.

  11. Noninvasive 3D Structural Analysis of Arthropod by Synchrotron X-Ray Phase Contrast Tomography

    International Nuclear Information System (INIS)

    Yao, S.; Zong, Y.; Fan, J.; Sun, Z.; Jiang, H.

    2015-01-01

    X-ray imaging techniques significantly advanced our understanding of materials and biology, among which phase contrast X-ray microscopy has obvious advantages in imaging biological specimens which have low contrast by conventional absorption contrast microscopy. In this paper, three-dimensional microstructure of arthropod with high contrast has been demonstrated by synchrotron X-ray in-line phase contrast tomography. The external morphology and internal structures of an earthworm were analyzed based upon tomographic reconstructions with and without phase retrieval. We also identified and characterized various fine structural details such as the musculature system, the digestive system, the nervous system, and the circulatory system. This work exhibited the high efficiency, high precision, and wide potential applications of synchrotron X-ray phase contrast tomography in nondestructive investigation of low-density materials and biology.

  12. Rietveld refinement of the orthorhombic Pbca structures of Rb2CdSi5O12, Cs2MnSiO5O12, Cs2CoSi5O12 and Cs2NiSi5O12 leucites by synchrotron X-ray powder diffraction

    International Nuclear Information System (INIS)

    Bell, A.M.T.; Henderson, C.M.B.

    1996-01-01

    Analysis of high-resolution synchrotron X-ray powder diffraction patterns for hydrothermally synthesized Rb 2 CdSi 5 O 12 and Cs 2 MnSi 5 O 12 leucite analogues, and dry-synthesized Cs 2 CoSi 5 O 12 and Cs 2 NiSi 5 O 12 leucite analogues showed that they have an orthorhombic Pbca structure. The structures have been refined by the Rietveld method, showing that the tetrahedrally coordinated atoms (Si, Cd, Mn, Co and Ni) are ordered on separate sites. The Cs 2 MnSi 5 O 12 , Cs 2 CoSi 5 O 12 and Cs 2 NiSi 5 O 12 leucite samples are unusual in containing SiO 4 tetrahedra which are more distorted, on average, than the larger MnO 4 , CoO 4 and NiO 4 tetrahedra. The JCPDS file numbers for Rb 2 CdSi 5 O 12 , Cs 2 MnSi 5 O 12 and Cs 2 CoSi 5 O 12 are 46-1491, 46-1492 and 46-1493, respectively. (orig.)

  13. K(3)TaF(8) from laboratory X-ray powder data.

    Science.gov (United States)

    Smrcok, Lubomír; Cerný, Radovan; Boca, Miroslav; Macková, Iveta; Kubíková, Blanka

    2010-02-01

    The crystal structure of tripotassium octafluoridotantalate, K(3)TaF(8), determined from laboratory powder diffraction data by the simulated annealing method and refined by total energy minimization in the solid state, is built from discrete potassium cations, fluoride anions and monocapped trigonal-prismatic [TaF(7)](2-) ions. All six atoms in the asymmetric unit are in special positions of the P6(3)mc space group: the Ta and one F atom in the 2b (3m) sites, the K and two F atoms in the 6c (m) sites, and one F atom in the 2a (3m) site. The structure consists of face-sharing K(6) octahedra with a fluoride anion at the center of each octahedron, forming chains of composition [FK(3)](2+) running along [001] with isolated [TaF(7)](2-) trigonal prisms in between. The structure of the title compound is different from the reported structure of Na(3)TaF(8) and represents a new structure type.

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

    International Nuclear Information System (INIS)

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

    1999-01-01

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

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

    DEFF Research Database (Denmark)

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

    2013-01-01

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

  16. The 16th International Conference on X-ray Absorption Fine Structure (XAFS16)

    Science.gov (United States)

    Grunwaldt, J.-D.; Hagelstein, M.; Rothe, J.

    2016-05-01

    This preface of the proceedings volume of the 16th International Conference on X- ray Absorption Fine Structure (XAFS16) gives a glance on the five days of cutting-edge X-ray science which were held in Karlsruhe, Germany, August 23 - 28, 2015. In addition, several satellite meetings took place in Hamburg, Berlin and Stuttgart, a Sino-German workshop, three data analysis tutorials as well as special symposia on industrial catalysis and XFELs were held at the conference venue.

  17. Imaging properties of cerium doped Yttrium Aluminum Oxide (YAP:Ce) powder scintillating screens under X-ray excitation

    Energy Technology Data Exchange (ETDEWEB)

    Kalivas, N. [Greek Atomic Energy Commission, 15310 Ag. Paraskevi, P.O. Box 60092 (Greece); Valais, I. [Department of Medical Physics, Medical School, University of Patras, 26500 Patras (Greece)]|[Department of Medical Instruments Technology, Technological Educational Institution of Athens, Ag. Spyridonos Street, Aigaleo, 12210 Athens (Greece); Salemis, G.; Karagiannis, C.; Konstantinidis, A.; Nikolopoulos, D. [Department of Medical Instruments Technology, Technological Educational Institution of Athens, Ag. Spyridonos Street, Aigaleo, 12210 Athens (Greece); Loudos, G.; Sakelios, N.; Karakatsanis, N.; Nikita, K. [Department of Electrical and Computer Engineering, National Technical University of Athens, 9 Iroon Polytechniou, 15780 Zografos (Greece); Gayshan, V.L.; Gektin, A.V. [Institute of Scintillation Materials, Lenin Avenue 60, 310072 Kharkov (Ukraine); Sianoudis, I. [Department of Physics, Chemistry and Materials Technology, Technological Educational Institution of Athens, Aigaleo, 12210 Athens (Greece); Giokaris, N. [Physics Department National Capodistrian University of Athens, Panepistimioupolis Ilisia, 15771 Athens (Greece)]|[Institute of Accelerating Systems and Applications, P.O. Box 17214, 10024 Athens (Greece); Nomicos, C.D. [Department of Electronics, Technological Educational Institution of Athens, Aigaleo, 12210 Athens (Greece); Dimitropoulos, N. [Department of Medical Imaging, ' Euromedica' Medical Center, Mesogeion 2-4, 11527 Athens (Greece); Cavouras, D. [Department of Medical Instruments Technology, Technological Educational Institution of Athens, Ag. Spyridonos Street, Aigaleo, 12210 Athens (Greece); Panayiotakis, G. [Department of Medical Physics, Medical School, University of Patras, 26500 Patras (Greece); Kandarakis, I. [Department of Medical Instruments Technology, Technological Educational Institution of Athens, Ag. Spyridonos Street, Aigaleo, 12210 Athens (Greece)]. E-mail: kandarakis@teiath.gr

    2006-12-20

    The aim of the present study was to evaluate the imaging performance of YAP:Ce powder scintillating screens under exposure conditions employed in diagnostic radiology (50-140 kV). Various screens were prepared in our laboratory from YAP: Ce powder (Phosphor Technology, Ltd.), with coating thickness ranging from 53 to 110 mg/cm{sup 2}. The imaging performance of the screens was assessed by experimental determination of the modulation transfer function (MTF) and the noise transfer function (NTF). MTF was determined by the edge spread function (ESF) method while NTF was estimated by noise power spectrum (NPS) measurements after uniform screen irradiation. In addition, parameters related to overall image quality, such as the signal-to-noise ratio transfer (MTF/NTF), were estimated. MTF curves were affected by the beam hardening effects caused by the patient simulating 20 mm thick aluminum phantom. Under these conditions MTF values were found to increase with the mean X-ray photon energy. A similar effect was observed for NTF curves. Results were compared with data obtained on CsI:Tl scintillator. Taking into consideration the very fast response of YAP:Ce, these data may be of interest in designing X-ray imaging detectors.

  18. submitter Digital Image Correlation of 2D X-ray Powder Diffraction Data for Lattice Strain Evaluation

    CERN Document Server

    Zhang, Hongjia; Salvati, Enrico; Daisenberger, Dominik; Lunt, Alexander J G; Fong, Kai Soon; Song, Xu; Korsunsky, Alexander M

    2018-01-01

    High energy 2D X-ray powder diffraction experiments are widely used for lattice strain measurement. The 2D to 1D conversion of diffraction patterns is a necessary step used to prepare the data for full pattern refinement, but is inefficient when only peak centre position information is required for lattice strain evaluation. The multi-step conversion process is likely to lead to increased errors associated with the ‘caking’ (radial binning) or fitting procedures. A new method is proposed here that relies on direct Digital Image Correlation analysis of 2D X-ray powder diffraction patterns (XRD-DIC, for short). As an example of using XRD-DIC, residual strain values along the central line in a Mg AZ31B alloy bar after 3-point bending are calculated by using both XRD-DIC and the conventional ‘caking’ with fitting procedures. Comparison of the results for strain values in different azimuthal angles demonstrates excellent agreement between the two methods. The principal strains and directions are calculated...

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

    International Nuclear Information System (INIS)

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

    2004-01-01

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

  20. Laser plasmas as x-ray sources for lithographic imaging of submicron structures

    International Nuclear Information System (INIS)

    Bijkerk, F.; van Dorssen, G.E.; van der Wiel, M.J.

    1988-01-01

    Laser radiation can be used efficiently to generate x-rays for lithographic imaging of submicron patterns, e.g., for VLSI device fabrication. Due to their short wavelength and high average power, excimer lasers show much potential for this application. Results are presented of scaling studies for high repetition rate excimer laser application, using the frequency doubled output of a low repetition rate Nd:YAG/Glass laser. Spectral and spatial characteristics of x-ray emission of the laser plasma are shown. The power density in the laser focus was 3 x 10 12 W/cm 2 . With this source Si x-ray masks with submicron Au absorber profiles are imaged into high sensitivity x-ray photoresist. For the exposures 80 laser shots sufficed to yield high quality submicron structures. Extrapolation of the results to a high power excimer laser reduces the exposure time of the photoresists to several seconds, enabling a wafer throughput at an industrial level

  1. X-ray powder diffraction camera for high-field experiments

    International Nuclear Information System (INIS)

    Koyama, K; Mitsui, Y; Takahashi, K; Watanabe, K

    2009-01-01

    We have designed a high-field X-ray diffraction (HF-XRD) camera which will be inserted into an experimental room temperature bore (100 mm) of a conventional solenoid-type cryocooled superconducting magnet (10T-CSM). Using the prototype camera that is same size of the HF-XRD camera, a XRD pattern of Si is taken at room temperature in a zero magnetic field. From the obtained results, the expected ability of the designed HF-XRD camera is presented.

  2. Powder X-ray study of natural phyllipsites and their ionexchange forms

    International Nuclear Information System (INIS)

    Kirov, G.N.; Ivanov, Pl.; Chan Chong Hue

    1990-01-01

    Vein samples with 1.3-1.9 Si/Al ratio and prevalence of Ca over Na and phyllipsites from volcanic tuffs in saline alkaline lakes with 3.0-3.5 Si/Al ratio and very low calcium content have been studied as well as their exchange forms enriched by cations typical of the phyllipsite group. The X-ray study has been carried out with DRON-2.0 diffractometer with cobalt filtered radiation. Calculation of the lattice parameters has been performed. 3 figs., 1 tab., 8 refs

  3. X-ray laser diffraction for structure determination of the rhodopsin-arrestin complex

    Science.gov (United States)

    Zhou, X. Edward; Gao, Xiang; Barty, Anton; Kang, Yanyong; He, Yuanzheng; Liu, Wei; Ishchenko, Andrii; White, Thomas A.; Yefanov, Oleksandr; Han, Gye Won; Xu, Qingping; de Waal, Parker W.; Suino-Powell, Kelly M.; Boutet, Sébastien; Williams, Garth J.; Wang, Meitian; Li, Dianfan; Caffrey, Martin; Chapman, Henry N.; Spence, John C. H.; Fromme, Petra; Weierstall, Uwe; Stevens, Raymond C.; Cherezov, Vadim; Melcher, Karsten; Xu, H. Eric

    2016-04-01

    Serial femtosecond X-ray crystallography (SFX) using an X-ray free electron laser (XFEL) is a recent advancement in structural biology for solving crystal structures of challenging membrane proteins, including G-protein coupled receptors (GPCRs), which often only produce microcrystals. An XFEL delivers highly intense X-ray pulses of femtosecond duration short enough to enable the collection of single diffraction images before significant radiation damage to crystals sets in. Here we report the deposition of the XFEL data and provide further details on crystallization, XFEL data collection and analysis, structure determination, and the validation of the structural model. The rhodopsin-arrestin crystal structure solved with SFX represents the first near-atomic resolution structure of a GPCR-arrestin complex, provides structural insights into understanding of arrestin-mediated GPCR signaling, and demonstrates the great potential of this SFX-XFEL technology for accelerating crystal structure determination of challenging proteins and protein complexes.

  4. Absolute determination by X-ray diffraction of a binary or ternary mixture: nickel oxide and fluoride in a nickel powder (1960)

    International Nuclear Information System (INIS)

    Charpin, P.; Hauptman, A.

    1960-01-01

    The method employed is based upon the comparison between computed and measured intensities for conveniently selected X-Ray diffraction lines of each component of the powder. Care must be taken to allow for absorption, both inside each grain and in overall sample. This method has been applied to the determination of nickel oxide and fluoride in a nickel powder. (author) [fr

  5. Monitoring protein precipitates by in-house X-ray powder diffraction

    DEFF Research Database (Denmark)

    Ståhl, Kenny; Frankær, Christian Grundahl; Petersen, Jakob

    2013-01-01

    of such calculated powder patterns from insulin and lysozyme have been included in the powder diffraction database and successfully used for search-match identification. However, the fit could be much improved if peak asymmetry and multiple bulk-solvent corrections were included. When including a large number...

  6. High-resolution x-ray imaging using a structured scintillator

    Energy Technology Data Exchange (ETDEWEB)

    Hormozan, Yashar, E-mail: hormozan@kth.se; Sychugov, Ilya; Linnros, Jan [Materials and Nano Physics, School of Information and Communication Technology, KTH Royal Institute of Technology, Electrum 229, Kista, Stockholm SE-16440 (Sweden)

    2016-02-15

    Purpose: In this study, the authors introduce a new generation of finely structured scintillators with a very high spatial resolution (a few micrometers) compared to conventional scintillators, yet maintaining a thick absorbing layer for improved detectivity. Methods: Their concept is based on a 2D array of high aspect ratio pores which are fabricated by ICP etching, with spacings (pitches) of a few micrometers, on silicon and oxidation of the pore walls. The pores were subsequently filled by melting of powdered CsI(Tl), as the scintillating agent. In order to couple the secondary emitted photons of the back of the scintillator array to a CCD device, having a larger pixel size than the pore pitch, an open optical microscope with adjustable magnification was designed and implemented. By imaging a sharp edge, the authors were able to calculate the modulation transfer function (MTF) of this finely structured scintillator. Results: The x-ray images of individually resolved pores suggest that they have been almost uniformly filled, and the MTF measurements show the feasibility of a few microns spatial resolution imaging, as set by the scintillator pore size. Compared to existing techniques utilizing CsI needles as a structured scintillator, their results imply an almost sevenfold improvement in resolution. Finally, high resolution images, taken by their detector, are presented. Conclusions: The presented work successfully shows the functionality of their detector concept for high resolution imaging and further fabrication developments are most likely to result in higher quantum efficiencies.

  7. Structure elucidation of 3-[1-(6-methoxy-2-naphtyl)ethyl]-6-(2,4-dichlorophenyl)-7H-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazine, C23H18Cl2N4OS from synchrotron X-ray powder diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Gündoğdu, Gülsüm; Aytaç, Sevim Peri; Müller, Melanie; Tozkoparan, Birsen; Kaynak, Filiz Betül

    2017-12-01

    The 3-[1-(6-methoxy-2-naphtyl)ethyl]-6-(2,4-dichlorophenyl)-7H-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazine, C23H18Cl2N4OS compound was synthesized, as a member of the family of novel potential anticancer agents. The structure of the title compound was characterized by IR,1H-NMR, mass spectroscopy, and elemental analysis, previously. In this study, the crystal structure of this compound has been determined from synchrotron X-ray powder diffraction data. The crystal structure was solved by simulated annealing and the final structure was achieved by Rietveld refinement method using soft restrains on all interatomic bond lengths and angles. This compound crystallizes in space groupP21,Z= 2, with the unit-cell parametersa= 15.55645(11) Å,b= 8.61693(6) Å,c= 8.56702(6) Å,β= 104.3270(4)°, andV= 1112.68(1) Å3. In the crystal structure, strong C-H∙∙∙πand weak intermolecular hydrogen-bonding interactions link the molecules into a three-dimensional network. The molecules are in a head-to-head arrangement in the unit cell.

  8. Efficiency of Lu2SiO5:Ce (LSO) powder phosphor as X-ray to light converter under mammographic imaging conditions

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  9. X-ray absorption fine structure (XAFS) studies of cobalt silicide thin films

    International Nuclear Information System (INIS)

    Naftel, S.J.; Coulthard, I.; Hu, Y.; Sham, T.K.; Zinke-Allmang, M.

    1998-01-01

    Cobalt silicide thin films, prepared on Si(100) wafers, have been studied by X-ray absorption near edge structures (XANES) at the Si K-, L 2,3 - and Co K-edges utilizing both total electron (TEY) and fluorescence yield (FLY) detection as well as extended X-ray absorption fine structure (EXAFS) at the Co K-edge. Samples made using DC sputter deposition on clean Si surfaces and MBE were studied along with a bulk CoSi 2 sample. XANES and EXAFS provide information about the electronic structure and morphology of the films. It was found that the films studied have essentially the same structure as bulk CoSi 2 . Both the spectroscopy and materials characterization aspects of XAFS (X-ray absorption fine structures) are discussed

  10. Annealing induced atomic rearrangements on (Ga,In) (N,As) probed by hard X-ray photoelectron spectroscopy and X-ray absorption fine structure.

    Science.gov (United States)

    Ishikawa, Fumitaro; Higashi, Kotaro; Fuyuno, Satoshi; Morifuji, Masato; Kondow, Masahiko; Trampert, Achim

    2018-04-13

    We study the effects of annealing on (Ga 0.64 ,In 0.36 ) (N 0.045 ,As 0.955 ) using hard X-ray photoelectron spectroscopy and X-ray absorption fine structure measurements. We observed surface oxidation and termination of the N-As bond defects caused by the annealing process. Specifically, we observed a characteristic chemical shift towards lower binding energies in the photoelectron spectra related to In. This phenomenon appears to be caused by the atomic arrangement, which produces increased In-N bond configurations within the matrix, as indicated by the X-ray absorption fine structure measurements. The reduction in the binding energies of group-III In, which occurs concomitantly with the atomic rearrangements of the matrix, causes the differences in the electronic properties of the system before and after annealing.

  11. X-ray and photoelectron spectroscopy of the structure, reactivity, and electronic structure of semiconductor nanocrystals

    Energy Technology Data Exchange (ETDEWEB)

    Hamad, Kimberly Sue [Univ. of California, Berkeley, CA (United States)

    2000-01-01

    Semiconductor nanocrystals are a system which has been the focus of interest due to their size dependent properties and their possible use in technological applications. Many chemical and physical properties vary systematically with the size of the nanocrystal and thus their study enables the investigation of scaling laws. Due to the increasing surface to volume ratio as size is decreased, the surfaces of nanocrystals are expected to have a large influence on their electronic, thermodynamic, and chemical behavior. In spite of their importance, nanocrystal surfaces are still relatively uncharacterized in terms of their structure, electronic properties, bonding, and reactivity. Investigation of nanocrystal surfaces is currently limited by what techniques to use, and which methods are suitable for nanocrystals is still being determined. This work presents experiments using x-ray and electronic spectroscopies to explore the structure, reactivity, and electronic properties of semiconductor (CdSe, InAs) nanocrystals and how they vary with size. Specifically, x-ray absorption near edge spectroscopy (XANES) in conjunction with multiple scattering simulations affords information about the structural disorder present at the surface of the nanocrystal. X-ray photoelectron spectroscopy (XPS) and ultra-violet photoelectron spectroscopy (UPS) probe the electronic structure in terms of hole screening, and also give information about band lineups when the nanocrystal is placed in electric contact with a substrate. XPS of the core levels of the nanocrystal as a function of photo-oxidation time yields kinetic data on the oxidation reaction occurring at the surface of the nanocrystal.

  12. Crystal structure and charge density analysis of Li2NH by synchrotron X-ray diffraction

    International Nuclear Information System (INIS)

    Noritake, T.; Nozaki, H.; Aoki, M.; Towata, S.; Kitahara, G.; Nakamori, Y.; Orimo, S.

    2005-01-01

    Complex hydrides, such as lithium amide (LiNH 2 ) and lithium imide (Li 2 NH), have recently been noticed as one of the most promising materials for reversible hydrogen storage. In this paper, we reveal the bonding nature of hydrogen in Li 2 NH crystal by synchrotron powder X-ray diffraction measurement at room temperature. The crystal structure was refined by Rietveld method and the charge density distribution was analyzed by maximum entropy method (MEM). The Li 2 NH crystal is anti-fluorite type structure (space group Fm3-bar m) consisting of Li and NH. Hydrogen atom occupies randomly the 48h (Wyckoff notation) sites around N atom. The refined lattice constant is a=5.0742(2)A. The charge density distribution around NH anion in Li 2 NH is almost spherical. The number of electrons within the sphere around the Li and NH is estimated from the obtained charge density distribution. As the result, the ionic charge is expressed as [Li 0.99+ ] 2 [NH] 1.21- . Therefore, it is confirmed experimentally that Li 2 NH is ionically bonded

  13. Fabrication of high-aspect-ratio nano structures using a nano x-ray shadow mask

    International Nuclear Information System (INIS)

    Kim, Yong Chul; Lee, Seung S

    2008-01-01

    This paper describes a novel method for the fabrication of high-aspect-ratio nano structures (HAR-nano structures) using a nano x-ray shadow mask and deep x-ray lithography (DXRL). The nano x-ray shadow mask is fabricated by depositing an x-ray absorber layer (Au, 3 µm) onto the back side of a nano shadow mask. The nano shadow mask is produced with nano-sized apertures whose dimensions are reduced to several tens of nanometers by the accumulation of low-stress silicon nitride (Si x N y ) using the LPCVD process on the shadow mask. A shadow mask containing apertures with a size of 1 µm is fabricated on a bulk micromachined Si x N y membrane. The thickness of an absorber layer must be in the range of several tens of micrometers in order to obtain a contrast of more than 100 for the conventional DXRL process at the Pohang Light Source (PLS). However, a 3 µm thick absorber layer can provide a sufficient contrast if the modified DXRL of the central beam-stop method is used, which blocks high-energy x-rays. A nano shadow mask with 30 nm sized apertures is fabricated and a nano x-ray shadow mask with 250 nm sized apertures is fabricated by depositing a 3 µm thick absorber layer on a nano shadow mask with 500 nm sized apertures. HAR-nano structures (circles with a diameter of 420 nm and lines with a width of 274 nm) with aspect ratios of over 10:1 on a 3.2 µm SU-8 are successfully fabricated by using the nano x-ray shadow mask and the central beam-stop method

  14. Modeling Radiation Effects of Ultrasoft X Rays on the Basis of Amorphous Track Structure.

    Science.gov (United States)

    Buch, Tamara; Scifoni, Emanuele; Krämer, Michael; Durante, Marco; Scholz, Michael; Friedrich, Thomas

    2018-01-01

    There is experimental evidence that ultrasoft X rays (0.1-5 keV) show a higher biological effectiveness than high-energy photons. Similar to high-LET radiation, this is attributed to a rather localized dose distribution associated with a considerably smaller range of secondary electrons, which results in an increasing yield of double-strand breaks (DSBs) and potentially more complex lesions. We previously reported on the application of the Giant LOop Binary LEsion (GLOBLE) model to ultrasoft X rays, in which experimental values of the relative biological effectiveness (RBE) for DSB induction were used to show that this increasing DSB yield was sufficient to explain the enhanced effectiveness in the cell inactivation potential of ultrasoft X rays. Complementary to GLOBLE, we report here on a modeling approach to predict the increased DSB yield of ultrasoft X rays on the basis of amorphous track structure formed by secondary electrons, which was derived from Monte Carlo track structure simulations. This procedure is associated with increased production of single-strand break (SSB) clusters, which are caused by the highly localized energy deposition pattern induced by low-energy photons. From this, the RBE of ultrasoft X rays can be determined and compared to experimental data, showing that the inhomogeneity of the energy deposition pattern represents the key variable to describe the increased biological effectiveness of ultrasoft X rays. Thus, this work demonstrates an extended applicability of the amorphous track structure concept and tests its limits with respect to its predictive power. The employed model mechanism offers a possible explanation for how the cellular response to ultrasoft X rays is directly linked to the energy deposition properties on the nanometric scale.

  15. 3D visualization of subcellular structures of Schizosaccharomyces pombe by hard X-ray tomography.

    Science.gov (United States)

    Yang, Y; Li, W; Liu, G; Zhang, X; Chen, J; Wu, W; Guan, Y; Xiong, Y; Tian, Y; Wu, Z

    2010-10-01

    Cellular structures of the fission yeast, Schizosaccharomyces pombe, were examined by using hard X-ray tomography. Since cells are nearly transparent to hard X-rays, Zernike phase contrast and heavy metal staining were introduced to improve image contrast. Through using such methods, images taken at 8 keV displayed sufficient contrast for observing cellular structures. The cell wall, the intracellular organelles and the entire structural organization of the whole cells were visualized in three-dimensional at a resolution better than 100 nm. Comparison between phase contrast and absorption contrast was also made, indicating the obvious advantage of phase contrast for cellular imaging at this energy. Our results demonstrate that hard X-ray tomography with Zernike phase contrast is suitable for cellular imaging. Its unique abilities make it have potential to become a useful tool for revealing structural information from cells, especially thick eukaryotic cells. © 2010 The Authors Journal compilation © 2010 The Royal Microscopical Society.

  16. X-ray-to-current signal conversion characteristics of trench-structured photodiodes for direct-conversion-type silicon X-ray sensor

    International Nuclear Information System (INIS)

    Ariyoshi, Tetsuya; Funaki, Shota; Sakamoto, Kenji; Baba, Akiyoshi; Arima, Yutaka

    2017-01-01

    To reduce the radiation dose required in medical X-ray diagnoses, we propose a high-sensitivity direct-conversion-type silicon X-ray sensor that uses trench-structured photodiodes. This sensor is advantageous in terms of its long device lifetime, noise immunity, and low power consumption because of its low bias voltage. With this sensor, it is possible to detect X-rays with almost 100% efficiency; sensitivity can therefore be improved by approximately 10 times when compared with conventional indirect-conversion-type sensors. In this study, a test chip was fabricated using a single-poly single-metal 0.35 μm process. The formed trench photodiodes for the X-ray sensor were approximately 170 and 300 μm deep. At a bias voltage of 25 V, the absorbed X-ray-to-current signal conversion efficiencies were 89.3% (theoretical limit; 96.7%) at a trench depth of 170 μm and 91.1% (theoretical limit; 94.3%) at a trench depth of 300 μm. (author)

  17. Batch crystallization of rhodopsin for structural dynamics using an X-ray free-electron laser

    Energy Technology Data Exchange (ETDEWEB)

    Wu, Wenting; Nogly, Przemyslaw; Rheinberger, Jan; Kick, Leonhard M.; Gati, Cornelius; Nelson, Garrett; Deupi, Xavier; Standfuss, Jörg; Schertler, Gebhard; Panneels, Valérie, E-mail: valerie.panneels@psi.ch [Paul Scherrer Institute, OFLC/103, 5232 Villigen-PSI (Switzerland)

    2015-06-27

    A new batch preparation method is presented for high-density micrometre-sized crystals of the G protein-coupled receptor rhodopsin for use in time-resolved serial femtosecond crystallography at an X-ray free-electron laser using a liquid jet. Rhodopsin is a membrane protein from the G protein-coupled receptor family. Together with its ligand retinal, it forms the visual pigment responsible for night vision. In order to perform ultrafast dynamics studies, a time-resolved serial femtosecond crystallography method is required owing to the nonreversible activation of rhodopsin. In such an approach, microcrystals in suspension are delivered into the X-ray pulses of an X-ray free-electron laser (XFEL) after a precise photoactivation delay. Here, a millilitre batch production of high-density microcrystals was developed by four methodical conversion steps starting from known vapour-diffusion crystallization protocols: (i) screening the low-salt crystallization conditions preferred for serial crystallography by vapour diffusion, (ii) optimization of batch crystallization, (iii) testing the crystal size and quality using second-harmonic generation (SHG) imaging and X-ray powder diffraction and (iv) production of millilitres of rhodopsin crystal suspension in batches for serial crystallography tests; these crystals diffracted at an XFEL at the Linac Coherent Light Source using a liquid-jet setup.

  18. Rapid X-ray crystal structure analysis in few second measurements using microstrip gas chamber

    CERN Document Server

    Ochi, A; Tanimori, T; Ohashi, Y; Toyokawa, H; Nishi, Y; Nishi, Y; Nagayoshi, T; Koishi, S

    2001-01-01

    X-ray crystal structure analysis using microstrip gas chamber was successfully carried out in a measurement time within a few seconds. The continuous rotation photograph method, in which most of the diffraction peaks can be obtained within one continuous rotation of the sample crystal (without stopping or oscillation), was applied for this measurement. As an example, the structure of a single crystal of ammonium bitartrate (r=1 mm, spherical) was measured. Diffraction spots from the sample, which were sufficient to obtain crystal structure, were successfully obtained by taking only 2 s measurements with a commercially available laboratory X-ray source.

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

    International Nuclear Information System (INIS)

    Fernandes, P.

    2007-04-01

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

  20. Characterization of monoclinic crystals in tablets by pattern-fitting procedure using X-ray powder diffraction data.

    Science.gov (United States)

    Yamamura, Shigeo; Momose, Yasunori

    2003-06-18

    The purpose of this study is to characterize the monoclinic crystals in tablets by using X-ray powder diffraction data and to evaluate the deformation feature of crystals during compression. The monoclinic crystals of acetaminophen and benzoic acid were used as the samples. The observed X-ray diffraction intensities were fitted to the analytic expression, and the fitting parameters, such as the lattice parameters, the peak-width parameters, the preferred orientation parameter and peak asymmetric parameter were optimized by a non-linear least-squares procedure. The Gauss and March distribution functions were used to correct the preferred orientation of crystallites in the tablet. The March function performed better in correcting the modification of diffraction intensity by preferred orientation of crystallites, suggesting that the crystallites in the tablets had fiber texture with axial orientation. Although a broadening of diffraction peaks was observed in acetaminophen tablets with an increase of compression pressure, little broadening was observed in the benzoic tablets. These results suggest that "acetaminophen is a material consolidating by fragmentation of crystalline particles and benzoic acid is a material consolidating by plastic deformation then occurred rearrangement of molecules during compression". A pattern-fitting procedure is the superior method for characterizing the crystalline drugs of monoclinic crystals in the tablets, as well as orthorhombic isoniazid and mannitol crystals reported in the previous paper.

  1. X-Ray structure and biophysical properties of rabbit fibroblast growth factor 1

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Jihun; Blaber, Sachiko I.; Irsigler, Andre; Aspinwall, Eric; Blaber, Michael; (FSU)

    2010-01-14

    The rabbit is an important and de facto animal model in the study of ischemic disease and angiogenic therapy. Additionally, fibroblast growth factor 1 (FGF-1) is emerging as one of the most important growth factors for novel pro-angiogenic and pro-arteriogenic therapy. However, despite its significance, the fundamental biophysical properties of rabbit FGF-1, including its X-ray structure, have never been reported. Here, the cloning, crystallization, X-ray structure and determination of the biophysical properties of rabbit FGF-1 are described. The X-ray structure shows that the amino-acid differences between human and rabbit FGF-1 are solvent-exposed and therefore potentially immunogenic, while the biophysical studies identify differences in thermostability and receptor-binding affinity that distinguish rabbit FGF-1 from human FGF-1.

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

    Directory of Open Access Journals (Sweden)

    Íris Duarte

    2016-09-01

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

  3. Spectroscopic and X-ray Diffraction Study of Structural Disorder in Cryomilled and Amorphous Griseofulvin

    International Nuclear Information System (INIS)

    Zarow, A.; Zhou, B.; Wang, X.; Pinal, R.; Iqbal, Z.

    2011-01-01

    Structural disorder induced by cryogenic milling and by heating to the amorphous phase in the active pharmaceutical ingredient Griseofulvin has been studied using Raman spectroscopy, X-ray powder diffraction (XRPD), and fluorescence spectroscopy. A broad, exciting-frequency-independent scattering background in the Raman spectra and changes in intensities and splitting of some of the Raman lines due to lattice and molecular modes have been observed. In the cryomilled samples this strong background is deconvoluted into two components: one due to lattice disorder induced by cryomilling and the other due to Mie scattering from nanosized crystallites. A single-component background scattering attributed to lattice disorder is seen in the Raman spectrum of the amorphous sample. Fluorescence measurements showed an intrinsic fluorescence signal in as-received Griseofulvin that does not correspond to the inelastic background in the Raman spectra and, moreover, decreases in intensity upon cryomilling, thus excluding an assignment of the Raman background intensity to impurity- or molecular-defect-induced fluorescence. Wide-angle XRPD measurements on cryomilled Griseofulvin shows a broad two-component background consistent with the background-scattering component in the Raman data associated with lattice disorder, but at longer correlation lengths. Persistence of this disorder to even longer lengths is evident in small-angle synchrotron XRPD data on micronized Griseofulvin taken as a function of temperature from the crystalline to the amorphous phase.

  4. ZDS - a computer program for analysis of X-ray powder diffraction patterns

    International Nuclear Information System (INIS)

    Ondrus, P.

    1993-01-01

    The ZDS system creates an integrated environment of procedures for complete and precise analysis of raw powder diffraction patterns. The basis of the ZDS system is a graphic control centre for easy and user-friendly application of all included procedures. It offers a number of application procedures without an interaction with any data base. The program operates either in an automatic or manual mode. The manual mode makes possible specialized applications. The input and output of the data are compatible with Philips and Siemens powder diffraction software. The ZDS system runs with Intel 80286 or 80386-based PC computers with or without math-coprocesor. (orig.)

  5. Characterization of (1 1 1) surface tailored Pt nanoparticles by electrochemistry and X-ray powder diffraction

    International Nuclear Information System (INIS)

    Beyerlein, K.R.; Solla-Gullon, J.; Herrero, E.; Garnier, E.; Pailloux, F.; Leoni, M.; Scardi, P.; Snyder, R.L.; Aldaz, A.; Feliu, J.M.

    2010-01-01

    Platinum nanoparticles with a mean size of 8.7 nm were synthesized by a salt reduction reaction having polyhedron shapes with preferential (1 1 1) surfaces. In situ electrochemical characterization of nanoparticles was performed which confirmed the existence of mostly (1 1 1) surface sites in the sample. The effect of this surface in the electrooxidation of CO was measured. Debye Function Analysis (DFA) and Whole Powder Pattern Modelling (WPPM) of the measured X-ray diffraction pattern were carried out to obtain statistical information on the particle size and shape present in the sample. Both analyses determined that the octahedron particle shape was the most abundant which was also consistent with TEM observations. The existence of a small percentage of single twinned particles was determined by DFA, WPPM, as well as analysis of HRTEM images.

  6. X-ray fluorescence spectrometric and optical emission spectographic analysis of thoria in thoriated copper metal powder

    International Nuclear Information System (INIS)

    Chandola, L.C.; Khanna, P.P.

    1984-01-01

    Two methods, one using the X-ray fluorescence (XRF) spectrometric technique and another using optical emission spectrographic (OES) technique are described for the determination of thoria in the concentration range 0.5-10% in thoriated copper metal powder. The precision of XRF method is superior to OES method but when sample quantity is very small, the OES method is useful. For XRF method, 500 mg sample is mixed with boric acid binding material and converted to a tablet for analysis. For OES method, only 200 mg sample is needed which is glued to the flat ends of two graphite electrodes for excitation by AC arc. The precision obtained in XRF is better than +-1% and in OES it is +-23%. (author)

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

    Science.gov (United States)

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

    2015-06-01

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

  8. FIST - a suite of X-ray powder crystallography programs for use with a HP-65 calculator

    International Nuclear Information System (INIS)

    Ferguson, I.F.; Turek, M.

    1977-12-01

    Programs for X-ray powder crystallography are defined for use with a Hewlett Packard HP-65 (programmable) pocket calculator. These include the prediction of all Bragg reflections for defined P-, F-, I-cubic, tetragonal, hexagonal and orthorhombic cells; the calculation of the position of a specific Bragg reflection from defined unit cells with all symmetries except triclinic; interconversion of theta, 2theta, sin 2 theta and d, as well as the calculation of the Nelson-Riley function; the computation of crystal densities; the interconversion of rhombohedral and hexagonal unit cells, lsub(c) determinations for graphite, the calculation of a and c for boron carbide; and Miller index transformations between various unit cells. (author)

  9. Communication: The electronic structure of matter probed with a single femtosecond hard x-ray pulse

    Directory of Open Access Journals (Sweden)

    J. Szlachetko

    2014-03-01

    Full Text Available Physical, biological, and chemical transformations are initiated by changes in the electronic configuration of the species involved. These electronic changes occur on the timescales of attoseconds (10−18 s to femtoseconds (10−15 s and drive all subsequent electronic reorganization as the system moves to a new equilibrium or quasi-equilibrium state. The ability to detect the dynamics of these electronic changes is crucial for understanding the potential energy surfaces upon which chemical and biological reactions take place. Here, we report on the determination of the electronic structure of matter using a single self-seeded femtosecond x-ray pulse from the Linac Coherent Light Source hard x-ray free electron laser. By measuring the high energy resolution off-resonant spectrum (HEROS, we were able to obtain information about the electronic density of states with a single femtosecond x-ray pulse. We show that the unoccupied electronic states of the scattering atom may be determined on a shot-to-shot basis and that the measured spectral shape is independent of the large intensity fluctuations of the incoming x-ray beam. Moreover, we demonstrate the chemical sensitivity and single-shot capability and limitations of HEROS, which enables the technique to track the electronic structural dynamics in matter on femtosecond time scales, making it an ideal probe technique for time-resolved X-ray experiments.

  10. Photovoltaic x-ray detectors based on the GaAs epitaxial structures

    CERN Document Server

    Akhmadullin, R A; Dvoryankina, G G; Dikaev, Y M; Ermakov, M G; Ermakova, O N; Krikunov, A I; Kudryashov, A A; Petrov, A G; Telegin, A A

    2002-01-01

    The new photovoltaic detector of the X-ray radiation is proposed on the basis of the GaAs epitaxial structures, which operates with high efficiency of the charge carriers collection without shift voltage and at the room temperature. The structures are grown by the method of the gas-phase epitaxy on the n sup + -type highly-alloyed substrates. The range of sensitivity to the X-ray radiation is within the range of effective energies from 8 up to 120 keV. The detector maximum response in the current short circuit mode is determined

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

    International Nuclear Information System (INIS)

    Antonio, M.R.; Soderholm, L.

    1995-01-01

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

  12. Method of evaluation of structural (screen) and quantum graininess of X-ray pictures

    Energy Technology Data Exchange (ETDEWEB)

    Gurvich, A M; Shamanov, A A; Erofeeva, N D [Nauchno-Issledovatel' skij Inst. Rentgenologii i Radiologii, Moscow (USSR)

    1979-03-01

    Proposed is a method for quantitative determination of graininess of X-ray pictures (gamma-ray images), the graininess being conditioned by the structure of amplifying screens and quantum fluctuations. The method is based on the determination of threshold brightness at which the picture graininess becomes obvious. It is shown that at low effective quantum energy (Esub(eff.) <= 50 keV) the graininess observed is for the most part structural (screen). Its growth is connected with quantum fluctuations when increasing Esub(eff.) up to 150 keV and using screens with high output values of X-ray luminescence and the coefficient of spectral accordance to the film.

  13. X-ray absorption in GaGdN: A study of local structure

    Science.gov (United States)

    Martínez-Criado, G.; Sancho-Juan, O.; Garro, N.; Sans, J. A.; Cantarero, A.; Susini, J.; Roever, M.; Mai, D.-D.; Bedoya-Pinto, A.; Malindretos, J.; Rizzi, A.

    2008-07-01

    In this study, we report on the incorporation of dilute Gd amounts into GaN films grown by molecular beam epitaxy. A combination of x-ray fluorescence with x-ray absorption spectroscopic techniques enabled us to examine not only the distribution of rare earth atoms in the GaN matrix but also the short-range structural order. Our results show Gd atoms in a trivalent state with tetrahedral coordination, thus substituting Ga in the wurtzite GaN structure.

  14. X-ray absorption in GaGdN: A study of local structure

    International Nuclear Information System (INIS)

    Martinez-Criado, G.; Sans, J. A.; Susini, J.; Sancho-Juan, O.; Cantarero, A.; Garro, N.; Roever, M.; Mai, D.-D.; Bedoya-Pinto, A.; Malindretos, J.; Rizzi, A.

    2008-01-01

    In this study, we report on the incorporation of dilute Gd amounts into GaN films grown by molecular beam epitaxy. A combination of x-ray fluorescence with x-ray absorption spectroscopic techniques enabled us to examine not only the distribution of rare earth atoms in the GaN matrix but also the short-range structural order. Our results show Gd atoms in a trivalent state with tetrahedral coordination, thus substituting Ga in the wurtzite GaN structure

  15. Structural mechanics of the solar-A Soft X-ray Telescope

    Science.gov (United States)

    Jurcevich, B. K.; Bruner, M. E.; Gowen, K. F.

    1992-01-01

    The Soft X-ray Telescope (SXT) is one of four major instruments that constitute the payload of the NASA-Japanese mission YOHKOH (formerly known as Solar-A), scheduled to be launched in August, 1991. This paper describes the design of the SXT, the key system requirements, and the SXT optical and structural systems. Particular attention is given to the design considerations for stiffness and dimensional stability, temperature compensation, and moisture sensitivyty control. Consideration is also given to the X-ray mirror, the aspect telescope, the entrance filters, the mechanical structure design, the aft support plate and mount, the SXT finite element model, and other subsystems.

  16. Purification, crystallization and preliminary X-ray structure analysis of the laccase from Ganoderma lucidum

    International Nuclear Information System (INIS)

    Lyashenko, Andrey V.; Belova, Oksana; Gabdulkhakov, Azat G.; Lashkov, Alexander A.; Lisov, Alexandr V.; Leontievsky, Alexey A.; Mikhailov, Al’bert M.

    2011-01-01

    The purification, crystallization and preliminary X-ray structure analysis of the laccase from G. lucidum are reported. The ligninolytic enzymes of the basidiomycetes play a key role in the global carbon cycle. A characteristic property of these enzymes is their broad substrate specificity, which has led to their use in various biotechnologies, thus stimulating research into the three-dimensional structures of ligninolytic enzymes. This paper presents the purification, crystallization and preliminary X-ray analysis of the laccase from the ligninolytic basidiomycete Ganoderma lucidum

  17. X-ray diffraction study of the structure of detonation nanodiamonds

    International Nuclear Information System (INIS)

    Ozerin, A. N.; Kurkin, T. S.; Ozerina, L. A.; Dolmatov, V. Yu.

    2008-01-01

    The spatial structure of aggregates formed by detonation nanodiamonds is investigated using the wide-angle and small-angle X-ray scattering techniques. The effective sizes of crystallites and the crystallite size distribution function are determined. The shape of scattering aggregates is restored from the small-angle X-ray scattering data. An analysis of the results obtained allowed the conclusion that the nanodiamond aggregates have an extended spatial structure composed of nine to ten clusters, each involving four to five crystallites with a crystal lattice of the diamond type

  18. Reflections on hard X-ray photon-in/photon-out spectroscopy for electronic structure studies

    Energy Technology Data Exchange (ETDEWEB)

    Glatzel, Pieter, E-mail: glatzel@esrf.fr [European Synchrotron Radiation Facility, 6 Rue Jules Horowitz, 38043 Grenoble (France); Weng, Tsu-Chien; Kvashnina, Kristina; Swarbrick, Janine; Sikora, Marcin [European Synchrotron Radiation Facility, 6 Rue Jules Horowitz, 38043 Grenoble (France); Gallo, Erik [European Synchrotron Radiation Facility, 6 Rue Jules Horowitz, 38043 Grenoble (France); Department of Inorganic, Physical and Materials Chemistry, INSTM Reference Center and NIS Centre of Excellence, Università di Torino, Via P. Giuria 7, I-10125 Torino (Italy); Smolentsev, Nikolay [European Synchrotron Radiation Facility, 6 Rue Jules Horowitz, 38043 Grenoble (France); Research Center for Nanoscale Structure of Matter, Southern Federal University, str. Zorge 5, 344090 Rostov-on-Don (Russian Federation); Mori, Roberto Alonso [European Synchrotron Radiation Facility, 6 Rue Jules Horowitz, 38043 Grenoble (France)

    2013-06-15

    Highlights: ► Overview of some recent developments in hard X-ray RXES/RIXS. ► Evaluation of spectral line broadening in RXES/RIXS. ► Modelling of RXES/RIXS by ground state DFT calculations. ► Discussion on when HERFD provides a good approximation to XAS. -- Abstract: An increasing community of researchers in various fields of natural sciences is combining X-ray absorption with X-ray emission spectroscopy (XAS–XES) to study electronic structure. With the applications becoming more diverse, the objectives and the requirements in photon-in/photon-out spectroscopy are becoming broader. It is desirable to find simple experimental protocols, robust data reduction and theoretical tools that help the experimentalist to understand their data and learn about the electronic structure. This article presents a collection of considerations on non-resonant and resonant XES with the aim to guide the experimentalist to make good use of this technique.

  19. Investigation of nanoscale structures by small-angle X-ray scattering in a radiochromic dosimeter

    DEFF Research Database (Denmark)

    Skyt, Peter Sandegaard; Jensen, Grethe Vestergaard; Wahlstedt, Isak Hannes

    2014-01-01

    This study examines the nanoscale structures in a radiochromic dosimeter that was based on leuco-malachite-green dye and the surfactant sodium dodecyl sulfate (SDS) suspended in a gelatin matrix. Small-angle X-ray scattering was used to investigate the structures of a range of compositions...

  20. X-ray structure amplitudes for GaAs and InP

    International Nuclear Information System (INIS)

    Pietsch, U.

    1985-01-01

    The structure amplitudes of GaAs and InP are calculated taking into account the nonspherical parts of the valence electron density by means of a static bond charge model. The best known temperature factors and dispersion coefficients are employed. The calculated structure amplitudes should help determining exactly the shape of X-ray diffraction patterns. (author)

  1. Composite structure of helicopter rotor blades studied by neutron- and X-ray radiography

    International Nuclear Information System (INIS)

    Balasko, M.; Veres, I.; Molnar, Gy.; Balasko, Zs.; Svab, E.

    2004-01-01

    In order to inspect the possible defects in the composite structure of helicopter rotor blades combined neutron- and X-ray radiography investigations were performed at the Budapest Research Reactor. Imperfections in the honeycomb structure, resin rich or starved areas at the core-honeycomb surfaces, inhomogeneities at the adhesive filling and water percolation at the sealing interfaces of the honeycomb sections were discovered

  2. Composite structure of helicopter rotor blades studied by neutron- and X-ray radiography

    Science.gov (United States)

    Balaskó, M.; Veres, I.; Molnár, Gy.; Balaskó, Zs.; Sváb, E.

    2004-07-01

    In order to inspect the possible defects in the composite structure of helicopter rotor blades combined neutron- and X-ray radiography investigations were performed at the Budapest Research Reactor. Imperfections in the honeycomb structure, resin rich or starved areas at the core-honeycomb surfaces, inhomogeneities at the adhesive filling and water percolation at the sealing interfaces of the honeycomb sections were discovered.

  3. X-ray propagation through a quasi-ordered multilayered structure ...

    African Journals Online (AJOL)

    We investigate the propagation of short wavelength transverse electric x-rays through a quasiordered (Fibonacci) atomically commensurate multilayered structure using a transfer matrix model which treats each atomic plane as a diffraction unit. The reflectance spectrum has a rich structure being dominated by peaks ...

  4. Recording of X-ray diffraction patterns for the investigation of transient changes in the crystalline structure of materials subjected to the action of shock waves

    International Nuclear Information System (INIS)

    Jamet, F.; Thomer, G.

    An arrangement including a flash X-ray tube and an image intensifier has been designed and built in order to record X-ray diffraction patterns with exposure times of the order of 100nsec. This arrangement allows Laue patterns (polychromatic radiation) as well as powder patterns (copper K(α) radiation) to be recorded. Examples for record are shown. As an application to the investigation of transient changes in crystalline structures, the Debye-Scherrer patterns of potassium chloride undergoing the dynamic action of shock waves were recorded. The first results achieved are discussed [fr

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

    DEFF Research Database (Denmark)

    Shen, Yanbin; Pedersen, Erik Ejler; Christensen, Mogens

    2014-01-01

    An electrochemical cell has been designed for powder X-ray diffraction (PXRD) studies of lithium ion batteries (LIB) and sodium ion batteries (SIB) in operando with high time resolution using conventional powder X-ray diffractometer. The cell allows for studies of both anode and cathode electrode...... to operate and maintain. Test examples on lithium insertion/extraction in two spinel-type LIB electrode materials (Li4Ti5O12 anode and LiMn2O4 cathode) are presented as well as first results on sodium extraction from a layered SIB cathode material (Na0.84Fe0.56Mn0.44O2)....

  6. X-ray detectors for structure investigations constructed at JINR

    Energy Technology Data Exchange (ETDEWEB)

    Chernenko, S P [LHE Joint Institute for Nuclear Research, 141980 Dubna (Russian Federation); Cheremukhina, G A [LHE Joint Institute for Nuclear Research, 141980 Dubna (Russian Federation); Fateev, O V [LHE Joint Institute for Nuclear Research, 141980 Dubna (Russian Federation); Smykov, L P [LHE Joint Institute for Nuclear Research, 141980 Dubna (Russian Federation); Vasiliev, S E [LHE Joint Institute for Nuclear Research, 141980 Dubna (Russian Federation); Zanevsky, Yu V [LHE Joint Institute for Nuclear Research, 141980 Dubna (Russian Federation); Kheiker, D M [Institute of Crystallography, Leninsky prosp. 59, 117333 Moscow (Russian Federation); Popov, A N [Institute of Crystallography, Leninsky prosp. 59, 117333 Moscow (Russian Federation)

    1994-09-01

    The performance characteristics of a few high resolution position-sensitive detectors constructed at JINR are presented. The detectors supplied with original software operate with an IBM PC/AT. One of these devices has been succesfully applied for protein molecule structure investigations and the other for studies of the structure-forming process during combustion. The preliminary parameters of the high count rate MWPC with parallel electronics and the testing results of the microstrip detector are given. ((orig.))

  7. A structural study of bone changes in knee osteoarthritis by synchrotron-based X-ray fluorescence and X-ray absorption spectroscopy techniques

    Science.gov (United States)

    Sindhupakorn, Bura; Thienpratharn, Suwittaya; Kidkhunthod, Pinit

    2017-10-01

    Osteoarthritis (OA) is characterized by degeneration of articular cartilage and thickening of subchondral bone. The present study investigated the changing of biochemical components of cartilage and bone compared between normal and OA people. Using Synchrotron-based X-ray fluorescence (SR-XRF) and X-ray absorption spectroscopy (XAS) techniquesincluding X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) were employed for the bone changes in kneeosteoarthritisstudies. The bone samples were collected from various osteoarthritis patients with both male and female in the ages range between 20 and 74 years old. SR-XRF results excited at 4240 eV for Ca elements show a majority three main groups, based on their XRF intensities, 20-36 years, 40-60 years and over 70 years, respectively. By employing XAS techniques, XANES features can be used to clearly explain in term of electronic transitions occurring in bone samples which are affected from osteoarthritis symptoms. Moreover, a structural change around Ca ions in bone samples is obviously obtained by EXAFS results indicating an increase of Ca-amorphous phase when the ages increase.

  8. Target surface structure effects on x-ray generation from laser produced plasma

    Energy Technology Data Exchange (ETDEWEB)

    Nishikawa, Tadashi; Nakano, Hidetoshi; Uesugi, Naoshi [NTT Basic Research Laboratories, Atsugi, Kanagawa (Japan)

    2000-03-01

    We demonstrated two different methods to increase the x-ray conversion efficiency of laser-produced plasma by modifying the target surface structure. One way is making a rectangular groove on a target surface and confining a laser-produced plasma in it. By the plasma collision process, a time and wavelength (4-10 nm) integrated soft x-ray fluence enhancement of 35 times was obtained at a groove width of 20 {mu}m and a groove depth of 100 {mu}m on a Nd-doped glass target. The other way is making an array of nanoholes on an alumina target and increasing the laser interaction depth with it. The x-ray fluence enhancement increases as the ionization level of Al becomes higher and the x-ray wavelength becomes shorter. Over 50-fold enhancement was obtained at a soft x-ray wavelength around 6 nm, which corresponds to the emission from Al{sup 8+,9+} ions. (author)

  9. Target surface structure effects on x-ray generation from laser produced plasma

    International Nuclear Information System (INIS)

    Nishikawa, Tadashi; Nakano, Hidetoshi; Uesugi, Naoshi

    2000-01-01

    We demonstrated two different methods to increase the x-ray conversion efficiency of laser-produced plasma by modifying the target surface structure. One way is making a rectangular groove on a target surface and confining a laser-produced plasma in it. By the plasma collision process, a time and wavelength (4-10 nm) integrated soft x-ray fluence enhancement of 35 times was obtained at a groove width of 20 μm and a groove depth of 100 μm on a Nd-doped glass target. The other way is making an array of nanoholes on an alumina target and increasing the laser interaction depth with it. The x-ray fluence enhancement increases as the ionization level of Al becomes higher and the x-ray wavelength becomes shorter. Over 50-fold enhancement was obtained at a soft x-ray wavelength around 6 nm, which corresponds to the emission from Al 8+,9+ ions. (author)

  10. Large-area soft x-ray projection lithography using multilayer mirrors structured by RIE

    Science.gov (United States)

    Rahn, Steffen; Kloidt, Andreas; Kleineberg, Ulf; Schmiedeskamp, Bernt; Kadel, Klaus; Schomburg, Werner K.; Hormes, F. J.; Heinzmann, Ulrich

    1993-01-01

    SXPL (soft X-ray projection lithography) is one of the most promising applications of X-ray reflecting optics using multilayer mirrors. Within our collaboration, such multilayer mirrors were fabricated, characterized, laterally structured and then used as reflection masks in a projecting lithography procedure. Mo/Si-multilayer mirrors were produced by electron beam evaporation in UHV under thermal treatment with an in-situ X-ray controlled thickness in the region of 2d equals 14 nm. The reflectivities measured at normal incidence reached up to 54%. Various surface analysis techniques have been applied in order to characterize and optimize the X-ray mirrors. The multilayers were patterned by reactive ion etching (RIE) with CF(subscript 4), using a photoresist as the etch mask, thus producing X-ray reflection masks. The masks were tested in the synchrotron radiation laboratory of the electron accelerator ELSA at the Physikalisches Institut of Bonn University. A double crystal X-ray monochromator was modified so as to allow about 0.5 cm(superscript 2) of the reflection mask to be illuminated by white synchrotron radiation. The reflected patterns were projected (with an energy of 100 eV) onto the resist (Hoechst AZ PF 514), which was mounted at an average distance of about 7 mm. In the first test-experiments, structure sizes down to 8 micrometers were nicely reproduced over the whole of the exposed area. Smaller structures were distorted by Fresnel-diffraction. The theoretically calculated diffraction images agree very well with the observed images.

  11. Analysis of powdered milk by PIXE (Proton Induced X-ray Emission)

    International Nuclear Information System (INIS)

    Desales Galeana, G.

    1990-01-01

    The purpose of this work was to establish the conditions to analyze elements of Z>15 in powdered milk samples using the PIXE technique. Ten different commercial samples were analyzed: 2 full-cream, 3 half-cream and 5 for infant feeding. They were all purchased in Toluca City, Mexico. Thick targets were prepared and irradiated with 1.5 and 3 MeV protons beam in Mexico's Nuclear Center Tandem Van de Graff Accelerator. The obtained data were analyzed by two computers programs. Iron, the reference element was analyzed by atomic absorption spectrometry. Concentrations of the following elements: phosphorus, chlorine, potassium, calcium, chrome, iron, cobalt, nickel, copper, zinc, bromine, rubidium, molybdenum and cadmium were evaluated. The concentrations of the first four elements were usually high, whereas those of the other elements remained in some ppm. The experimental conditions set up in this work were suitable for the analysis of powdered milk and can be applied to other organic samples (Author)

  12. Forming a structure of the CoNiFe alloys by X-ray irradiation

    Science.gov (United States)

    Valko, Natalia; Kasperovich, Andrey; Koltunowicz, Tomasz N.

    The experimental data of electrodeposition kinetics researches and structure formation of ternary CoNiFe alloys deposited onto low-carbon steel 08kp in the presence of X-rays are presented. Relations of deposit rate, current efficiencies, element and phase compositions of CoNiFe coatings formed from sulfate baths with respect to cathode current densities (0.5-3A/dm2), electrolyte composition and irradiation were obtained. It is shown that, the CoNiFe coatings deposited by the electrochemical method involving exposure of the X-rays are characterized by more perfect morphology surfaces with less developed surface geometry than reference coatings. The effect of the X-ray irradiation on the electrodeposition of CoNiFe coatings promotes formatting of alloys with increased electropositive component and modified phase composition.

  13. Structure investigation of metal ions clustering in dehydrated gel using x-ray anomalous dispersion effect

    CERN Document Server

    Soejima, Y; Sugiyama, M; Annaka, M; Nakamura, A; Hiramatsu, N; Hara, K

    2003-01-01

    The structure of copper ion clusters in dehydrated N-isopropylacrylamide/sodium acrylate (NIPA/SA) gel has been studied by means of small angle X-ray scattering (SAXS) method. In order to distinguish the intensity scattered by Cu ions, the X-ray anomalous dispersion effect around the Cu K absorption edge has been coupled with SAXS. It is found that the dispersion effect dependent on the incident X-ray energy is remarkable only at the momentum transfer q = 0.031 A sup - sup 1 , where a SAXS peak is observed. The results indicate that copper ions form clusters in the dehydrated gel, and that the mean size of clusters is the same as that of SA clusters produced by microphase separation. It is therefore naturally presumed that copper ions are adsorbed into the SA molecules. On the basis of the presumption, a mechanism is proposed for microphase-separation and clustering of Cu ions.

  14. Two-dimensional imaging detectors for structural biology with X-ray lasers.

    Science.gov (United States)

    Denes, Peter

    2014-07-17

    Our ability to harness the advances in microelectronics over the past decade(s) for X-ray detection has resulted in significant improvements in the state of the art. Biology with X-ray free-electron lasers present daunting detector challenges: all of the photons arrive at the same time, and individual high peak power pulses must be read out shot-by-shot. Direct X-ray detection in silicon pixel detectors--monolithic or hybrid--are the standard for XFELs today. For structural biology, improvements are needed for today's 10-100 Hz XFELs, and further improvements are required for tomorrow's 10+ kHz XFELs. This article will discuss detector challenges, why they arise and ways to overcome them, along with the current state of the art. © 2014 The Author(s) Published by the Royal Society. All rights reserved.

  15. Rapid characterization of a nanomaterial structure using X-ray reciprocal-lattice-space imaging

    International Nuclear Information System (INIS)

    Sakata, Osami; Yoshimoto, Mamoru; Miki, Kazushi

    2006-01-01

    The X-ray reciprocal-lattice-space imaging method is able to record the reciprocal-lattice-space of nanostructure by sample-and-detector fixed geometry. This method was developed by the surface structure analysis beam line BL13XU of SPring-8. Outline of the X-ray diffraction method and basic principles of the X-ray reciprocal-lattice-space imaging method, and application examples are stated. The method is able to find out the Bragg conditions of nanostructure of surface in the atmosphere. The reciprocal-lattice of the embedded trace atomic wires was observed. The trace atoms of Bi atomic wires embedded in silicone showed the diffraction signal and image by a short exposure time. This method is useful at rapid non-destructive measurement of nanostructure. (S.Y.)

  16. Parameter study of self-absorption effects in Total Reflection X-ray Fluorescence-X-ray Absorption Near Edge Structure analysis of arsenic

    International Nuclear Information System (INIS)

    Meirer, F.; Pepponi, G.; Streli, C.; Wobrauschek, P.; Kregsamer, P.; Zoeger, N.; Falkenberg, G.

    2008-01-01

    Total reflection X-ray Fluorescence (TXRF) analysis in combination with X-ray Absorption Near Edge Structure (XANES) analysis is a powerful method to perform chemical speciation studies at trace element levels. However, when measuring samples with higher concentrations and in particular standards, damping of the oscillations is observed. In this study the influence of self-absorption effects on TXRF-XANES measurements was investigated by comparing measurements with theoretical calculations. As(V) standard solutions were prepared at various concentrations and dried on flat substrates. The measurements showed a correlation between the damping of the oscillations and the As mass deposited. A Monte-Carlo simulation was developed using data of the samples shapes obtained from confocal white light microscopy. The results showed good agreement with the measurements; they confirmed that the key parameters are the density of the investigated atom in the dried residues and the shape of the residue, parameters that combined define the total mass crossed by a certain portion of the incident beam. The study presents a simple approach for an a priori evaluation of the self-absorption in TXRF X-ray absorption studies. The consequences for Extended X-ray Absorption Fine Structure (EXAFS) and XANES measurements under grazing incidence conditions are discussed, leading to the conclusion that the damping of the oscillations seems to make EXAFS of concentrated samples non feasible. For XANES 'fingerprint' analysis samples should be prepared with a deposited mass and sample shape leading to an acceptable absorption for the actual investigation

  17. Synthesis, characterization, x-ray structure and antimicrobial activity ...

    African Journals Online (AJOL)

    intermolecular N3—H1N1•••O1 hydrogen bonds. (Table 2), resulting in the formation of zigzag layers lying parallel to (100) (Fig. 2b). The existence of π•••π interactions involving the centroid of the N4/C9-C13 pyridine ring (π•••π distance = 3.5108(18) Å) further stabilize the molecular packing. The structure of compound 2.

  18. Surface extended x-ray absorption fine structure of low-Z absorbates using fluorescence detection

    International Nuclear Information System (INIS)

    Stoehr, J.; Kollin, E.B.; Fischer, D.A.; Hastings, J.B.; Zaera, F.; Sette, F.

    1985-05-01

    Comparison of x-ray fluorescence yield (FY) and electron yield surface extended x-ray absorption fine structure spectra above the S K-edge for c(2 x 2) S on Ni(100) reveals an order of magnitude higher sensitivity of the FY technique. Using FY detection, thiophene (C 4 H 4 S) chemisorption on Ni(100) is studied with S coverages down to 0.08 monolayer. The molecule dissociates at temperatures as low as 100K by interaction with fourfold hollow Ni sites. Blocking of these sites by oxygen leaves the molecule intact

  19. Measurements of ionic structure in shock compressed lithium hydride from ultrafast x-ray Thomson scattering.

    Science.gov (United States)

    Kritcher, A L; Neumayer, P; Brown, C R D; Davis, P; Döppner, T; Falcone, R W; Gericke, D O; Gregori, G; Holst, B; Landen, O L; Lee, H J; Morse, E C; Pelka, A; Redmer, R; Roth, M; Vorberger, J; Wünsch, K; Glenzer, S H

    2009-12-11

    We present the first ultrafast temporally, spectrally, and angularly resolved x-ray scattering measurements from shock-compressed matter. The experimental spectra yield the absolute elastic and inelastic scattering intensities from the measured density of free electrons. Laser-compressed lithium-hydride samples are well characterized by inelastic Compton and plasmon scattering of a K-alpha x-ray probe providing independent measurements of temperature and density. The data show excellent agreement with the total intensity and structure when using the two-species form factor and accounting for the screening of ion-ion interactions.

  20. Covering complete proteomes with X-ray structures: a current snapshot

    Energy Technology Data Exchange (ETDEWEB)

    Mizianty, Marcin J.; Fan, Xiao; Yan, Jing; Chalmers, Eric; Woloschuk, Christopher [University of Alberta, Edmonton, Alberta T6G 2V4 (Canada); Joachimiak, Andrzej, E-mail: andrzejj@anl.gov [Argonne National Laboratory, Argonne, IL 60439 (United States); Kurgan, Lukasz, E-mail: andrzejj@anl.gov [University of Alberta, Edmonton, Alberta T6G 2V4 (Canada)

    2014-11-01

    The current and the attainable coverage by X-ray structures of proteins and their functions on the scale of the ‘protein universe’ are estimated. A detailed analysis of the coverage across nearly 2000 proteomes from all superkingdoms of life and functional annotations is performed, with particular focus on the human proteome and the family of GPCR proteins. Structural genomics programs have developed and applied structure-determination pipelines to a wide range of protein targets, facilitating the visualization of macromolecular interactions and the understanding of their molecular and biochemical functions. The fundamental question of whether three-dimensional structures of all proteins and all functional annotations can be determined using X-ray crystallography is investigated. A first-of-its-kind large-scale analysis of crystallization propensity for all proteins encoded in 1953 fully sequenced genomes was performed. It is shown that current X-ray crystallographic knowhow combined with homology modeling can provide structures for 25% of modeling families (protein clusters for which structural models can be obtained through homology modeling), with at least one structural model produced for each Gene Ontology functional annotation. The coverage varies between superkingdoms, with 19% for eukaryotes, 35% for bacteria and 49% for archaea, and with those of viruses following the coverage values of their hosts. It is shown that the crystallization propensities of proteomes from the taxonomic superkingdoms are distinct. The use of knowledge-based target selection is shown to substantially increase the ability to produce X-ray structures. It is demonstrated that the human proteome has one of the highest attainable coverage values among eukaryotes, and GPCR membrane proteins suitable for X-ray structure determination were determined.

  1. Covering complete proteomes with X-ray structures: a current snapshot

    International Nuclear Information System (INIS)

    Mizianty, Marcin J.; Fan, Xiao; Yan, Jing; Chalmers, Eric; Woloschuk, Christopher; Joachimiak, Andrzej; Kurgan, Lukasz

    2014-01-01

    The current and the attainable coverage by X-ray structures of proteins and their functions on the scale of the ‘protein universe’ are estimated. A detailed analysis of the coverage across nearly 2000 proteomes from all superkingdoms of life and functional annotations is performed, with particular focus on the human proteome and the family of GPCR proteins. Structural genomics programs have developed and applied structure-determination pipelines to a wide range of protein targets, facilitating the visualization of macromolecular interactions and the understanding of their molecular and biochemical functions. The fundamental question of whether three-dimensional structures of all proteins and all functional annotations can be determined using X-ray crystallography is investigated. A first-of-its-kind large-scale analysis of crystallization propensity for all proteins encoded in 1953 fully sequenced genomes was performed. It is shown that current X-ray crystallographic knowhow combined with homology modeling can provide structures for 25% of modeling families (protein clusters for which structural models can be obtained through homology modeling), with at least one structural model produced for each Gene Ontology functional annotation. The coverage varies between superkingdoms, with 19% for eukaryotes, 35% for bacteria and 49% for archaea, and with those of viruses following the coverage values of their hosts. It is shown that the crystallization propensities of proteomes from the taxonomic superkingdoms are distinct. The use of knowledge-based target selection is shown to substantially increase the ability to produce X-ray structures. It is demonstrated that the human proteome has one of the highest attainable coverage values among eukaryotes, and GPCR membrane proteins suitable for X-ray structure determination were determined

  2. Precision mechanical structure of an ultra-high-resolution spectrometer for inelastic X-ray scattering instrument

    Science.gov (United States)

    Shu, Deming; Shvydko, Yuri; Stoupin, Stanislav A.; Khachatryan, Ruben; Goetze, Kurt A.; Roberts, Timothy

    2015-04-14

    A method and an ultrahigh-resolution spectrometer including a precision mechanical structure for positioning inelastic X-ray scattering optics are provided. The spectrometer includes an X-ray monochromator and an X-ray analyzer, each including X-ray optics of a collimating (C) crystal, a pair of dispersing (D) element crystals, anomalous transmission filter (F) and a wavelength (W) selector crystal. A respective precision mechanical structure is provided with the X-ray monochromator and the X-ray analyzer. The precision mechanical structure includes a base plate, such as an aluminum base plate; positioning stages for D-crystal alignment; positioning stages with an incline sensor for C/F/W-crystal alignment, and the positioning stages including flexure-based high-stiffness structure.

  3. Order-disorder-reorder process in thermally treated dolomite samples: a combined powder and single-crystal X-ray diffraction study

    Science.gov (United States)

    Zucchini, A.; Comodi, P.; Katerinopoulou, A.; Balic-Zunic, T.; McCammon, C.; Frondini, F.

    2012-04-01

    A combined powder and single-crystal X-ray diffraction analysis of dolomite [CaMg(CO3)2] heated to 1,200°C at 3 GPa was made to study the order-disorder-reorder process. The order/disorder transition is inferred to start below 1,100°C, and complete disorder is attained at approximately 1,200°C. Twinned crystals characterized by high internal order were found in samples annealed over 1,100°C, and their fraction was found to increase with temperature. Evidences of twinning domains combined with probable remaining disordered portions of the structure imply that reordering processes occur during the quench. Twin domains are hereby proposed as a witness to thermally induced intra-layer-type cation disordering.

  4. Quantitative determination of amorphous content in ceramic materials using x-ray powder diffraction

    International Nuclear Information System (INIS)

    Kuchinski, M.A.; Hubbard, C.R.

    1988-01-01

    A quantitative technique which employs a modified method of additions approach to analyze for low amorphous content in crystalline matrices was developed and tested. Known amounts of amorphous material are added to the starting powder. The method uses the ratio of a measure of the intensity of the amorphous phase corrected for background to the background corrected intensity of a reference line from a crystalline phase. The amorphous spiking phase must be close in composition to the amorphous phase existing in the analyte. A critical step of the method is to correctly establish the background intensity. A completely crystalline material of similar scattering power was used to establish background intensity

  5. Addressing source-induced structural vibrations in an interventional X-ray system

    NARCIS (Netherlands)

    Van Pinxteren, J.A.W.; Vermeulen, J.P.M.B.; van Loon, R.J.A.; van Schothorst, G.; Billington, D.; Phillips, D.

    2017-01-01

    Interventional radiology is a medical discipline, in which imaging equipment is used to diagnose and treat diseases throughout the human body. Dedicated systems, based on X-ray, computed tomography and ultrasound technology, allow for 2D and 3D imaging of (contrast enhanced) physical structures.

  6. Structural investigation of bistrifluron using x-ray crystallography, NMR spectroscopy, and molecular modeling

    CERN Document Server

    Moon, J K; Rhee, S K; Kim, G B; Yun, H S; Chung, B J; Lee, S S; Lim, Y H

    2002-01-01

    A new insecticide, bistrifluron acts as an inhibitor of insect development and interferes with the cuticle formation of insects. Since it shows low acute oral and dermal toxicities, it can be one of potent insecticides. Based on X-ray crystallography, NMR spectroscopy and molecular modeling, the structural studies of bistrifluron have been carried out.

  7. Analysis of stresses and strains in the materials with limiting structure using x-ray

    International Nuclear Information System (INIS)

    Imafuku, Muneyuki

    2010-01-01

    This review outlines the principle of analysis and the measuring instruments using X-ray for the stresses and strains in the materials with limiting structure. Further the several experimental examples are shown. This method is expected to be useful widely for the characterization evaluation, the reliability insurance, and the development of materials. (M.H.)

  8. The x-ray structure and MNDO calculations of a-terthienyl: a model for polythiophenes

    NARCIS (Netherlands)

    Bolhuis, van F.; Wynberg, H.; Havinga, E.E.; Meijer, E.W.; Staring, E.G.J.

    1989-01-01

    The x-ray structure of a-terthienyl reveals 2 identical, crystallog.-independent mols. in the unit cell. Neighboring thiophene moieties in a-terthienyl are placed antiparallel, while the mol. is almost planar, with torsional angles between the rings of about 6-9 Deg. MNDO calcns. of a-terthienyl

  9. Extended X-ray absorption fine structure investigation of nitrogen stabilized expanded austenite

    DEFF Research Database (Denmark)

    Oddershede, Jette; Christiansen, Thomas; Ståhl, Kenny

    2010-01-01

    As-delivered austenitic stainless steel and nitrogen stabilized expanded austenite, both fully nitrided and denitrided (in H2), were investigated with Cr, Fe and Ni extended X-ray absorption fine structure. The data shows pronounced short-range ordering of Cr and N. For the denitrided specimen...

  10. Grating-based X-ray tomography of 3D food structures

    DEFF Research Database (Denmark)

    Miklos, Rikke; Nielsen, Mikkel Schou; Einarsdottir, Hildur

    2016-01-01

    A novel grating based X-ray phase-contrast tomographic method has been used to study how partly substitution of meat proteins with two different types of soy proteins affect the structure of the formed protein gel in meat emulsions. The measurements were performed at the Swiss synchrotron radiati...

  11. Depth profiling of marker layers using x-ray waveguide structures

    International Nuclear Information System (INIS)

    Gupta, Ajay; Rajput, Parasmani; Saraiya, Amit; Reddy, V. R.; Gupta, Mukul; Bernstorff, Sigrid; Amenitsch, H.

    2005-01-01

    It is demonstrated that x-ray waveguide structures can be used for depth profiling of a marker layer inside the guiding layer with an accuracy of better than 0.2 nm. A combination of x-ray fluorescence and x-ray reflectivity measurements can provide detailed information about the structure of the guiding layer. The position and thickness of the marker layer affect different aspects of the angle-dependent x-ray fluorescence pattern, thus making it possible to determine the structure of the marker layer in an unambiguous manner. As an example, effects of swift heavy ion irradiation on a Si/M/Si trilayer (M=Fe, W), forming the cavity of the waveguide structure, have been studied. It is found that in accordance with the prediction of thermal spike model, Fe is much more sensitive to swift heavy ion induced modifications as compared to W, even in thin film form. However, a clear evidence of movement of the Fe marker layer towards the surface is observed after irradiation, which cannot be understood in terms of the thermal spike model alone

  12. Depth profiling of marker layers using x-ray waveguide structures

    Science.gov (United States)

    Gupta, Ajay; Rajput, Parasmani; Saraiya, Amit; Reddy, V. R.; Gupta, Mukul; Bernstorff, Sigrid; Amenitsch, H.

    2005-08-01

    It is demonstrated that x-ray waveguide structures can be used for depth profiling of a marker layer inside the guiding layer with an accuracy of better than 0.2 nm. A combination of x-ray fluorescence and x-ray reflectivity measurements can provide detailed information about the structure of the guiding layer. The position and thickness of the marker layer affect different aspects of the angle-dependent x-ray fluorescence pattern, thus making it possible to determine the structure of the marker layer in an unambiguous manner. As an example, effects of swift heavy ion irradiation on a Si/M/Si trilayer ( M=Fe , W), forming the cavity of the waveguide structure, have been studied. It is found that in accordance with the prediction of thermal spike model, Fe is much more sensitive to swift heavy ion induced modifications as compared to W, even in thin film form. However, a clear evidence of movement of the Fe marker layer towards the surface is observed after irradiation, which cannot be understood in terms of the thermal spike model alone.

  13. The 1s x-ray absorption pre-edge structures in transition metal oxides

    NARCIS (Netherlands)

    de Groot, Frank|info:eu-repo/dai/nl/08747610X; Vanko, Gyoergy; Glatzel, Pieter

    2009-01-01

    We develop a general procedure to analyse the pre-edges in 1s x-ray absorption near edge structure (XANES) of transition metal oxides and coordination complexes. Transition metal coordination complexes can be described from a local model with one metal ion. The 1s 3d quadrupole transitions are

  14. Stigmasterol from Eichhornia crassipes (water hyacinth) : Isolation, characterization and X-ray structure

    Digital Repository Service at National Institute of Oceanography (India)

    Singh, K.S.; Sawant, S.G.; PrabhaDevi; Kaminsky, W.

    >H48O by combination of NMR and mass spectroscopic data The sterol was fully characterized by FTIR,NMR(1H13C) and mass spectral data Solid state structure of the sterol was determined by single crystal X-Ray diffraction...

  15. Total chemical synthesis and X-ray structure of kaliotoxin by racemic protein crystallography.

    Science.gov (United States)

    Pentelute, Brad L; Mandal, Kalyaneswar; Gates, Zachary P; Sawaya, Michael R; Yeates, Todd O; Kent, Stephen B H

    2010-11-21

    Here we report the total synthesis of kaliotoxin by 'one pot' native chemical ligation of three synthetic peptides. A racemic mixture of D- and L-kaliotoxin synthetic protein molecules gave crystals in the centrosymmetric space group P1 that diffracted to atomic-resolution (0.95 Å), enabling the X-ray structure of kaliotoxin to be determined by direct methods.

  16. Dark-field X-ray microscopy for multiscale structural characterization

    DEFF Research Database (Denmark)

    Simons, Hugh; King, A.; Ludwig, W.

    2015-01-01

    of the interactions between crystalline elements is a key step towards the formulation and validation of multiscale models that account for the entire heterogeneity of a material. Furthermore, dark-field X-ray microscopy is well suited to applied topics, where the structural evolution of internal nanoscale elements...

  17. THE X-RAY STRUCTURE AND THE 13 C NMR DATA OF ...

    African Journals Online (AJOL)

    The alkaloids pellitorine and chelerythrine acetonate were isolated from the stem bark of Zanthoxylum davyi together with methyl octadecyl ketone, lupeol and hesperidin. The alkaloid skimmianie was isolated from the leaves. The X-Ray structure of chelerythrine acetonate was also determined. Key Words: Zanthoxylum ...

  18. Controlled agglomeration of Tb-doped Y2O3 nanocrystals studied by x-ray absorption fine structure, x-ray excited luminescence, and photoluminescence

    International Nuclear Information System (INIS)

    Soo, Y.L.; Huang, S.W.; Kao, Y.H.; Chhabra, V.; Kulkarni, B.; Veliadis, J.V.; Bhargava, R.N.

    1999-01-01

    Local environment surrounding Y atoms in Y 2 O 3 :Tb nanocrystals under various heat treatment conditions has been investigated by using the extended x-ray absorption fine structure (EXAFS) technique. X-ray excited luminescence (XEL) with the incident x-ray energy near Y K edge and Tb L edges has also been measured to investigate the mechanisms of x-ray-to-visible down conversion in these doped nanoparticles. The observed changes in EXAFS, XEL, and photoluminescent data can be explained on the basis of increased average size of the nanoparticles as confirmed by transmission electron microscopy studies. Our results thus demonstrate that the doped nanoparticles can agglomerate to a controllable degree by varying the heat treatment temperature. At higher temperatures, the local environment surrounding Y atoms in the nanoparticles is found to become similar to that in bulk Y 2 O 3 while the XEL output still shows the characteristics of nanocrystals. These results indicate that appropriate heat treatment can afford an effective means to control the intensity and signal-to-background ratio of green luminescence output of these doped nanocrystal phosphors, potentially useful for some device applications. copyright 1999 American Institute of Physics

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

  20. Characterization of atmospheric aerosols using Synchroton radiation total reflection X-ray fluorescence and Fe K-edge total reflection X-ray fluorescence-X-ray absorption near-edge structure

    Energy Technology Data Exchange (ETDEWEB)

    Fittschen, U.E.A. [Department of Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, 20146 Hamburg (Germany)], E-mail: ursula.fittschen@chemie.uni-hamburg.de; Meirer, F. [Atominstitut, Vienna University of Technology, Stadionallee 2, 1020 Wien (Austria)], E-mail: fmeirer@ati.ac.at; Streli, C. [Atominstitut, Vienna University of Technology, Stadionallee 2, 1020 Wien (Austria)], E-mail: streli@ati.ac.at; Wobrauschek, P. [Atominstitut, Vienna University of Technology, Stadionallee 2, 1020 Wien (Austria)], E-mail: wobi@ati.ac.at; Thiele, J. [Department of Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, 20146 Hamburg (Germany)], E-mail: Julian.Thiele@gmx.de; Falkenberg, G. [Hamburger Synchrotronstrahlungslabor at Deutsches Elektronen-Synchrotron DESY, Notkestr. 85, 22603 Hamburg (Germany)], E-mail: falkenbe@mail.desy.de; Pepponi, G. [ITC-irst, Via Sommarive 18, 38050 Povo (Trento) (Italy)], E-mail: pepponi@itc.it

    2008-12-15

    In this study a new procedure using Synchrotron total reflection X-ray fluorescence (SR-TXRF) to characterize elemental amounts in atmospheric aerosols down to particle sizes of 0.015 um is presented. The procedure was thoroughly evaluated regarding bounce off effects and blank values. Additionally the potential of total reflection X-ray fluorescence-X-ray absorption near edge structure (SR-TXRF-XANES) for speciation of FeII/III down to amounts of 34 pg in aerosols which were collected for 1 h is shown. The aerosols were collected in the city of Hamburg with a low pressure Berner impactor on Si carriers covered with silicone over time periods of 60 and 20 min each. The particles were collected in four and ten size fractions of 10.0-8.0 {mu}m, 8.0-2.0 {mu}m, 2.0-0.13 {mu}m 0.13-0.015 {mu}m (aerodynamic particle size) and 15-30 nm, 30-60 nm, 60-130 nm, 130-250 nm, 250-500 nm, 0.5-1 {mu}m, 1-2 {mu}m, 2-4 {mu}m, 4-8 {mu}m, 8-16 {mu}m. Prior to the sampling 'bounce off' effects on Silicone and Vaseline coated Si carriers were studied with total reflection X-ray fluorescence. According to the results silicone coated carriers were chosen for the analysis. Additionally, blank levels originating from the sampling device and the calibration procedure were studied. Blank levels of Fe corresponded to 1-10% of Fe in the aerosol samples. Blank levels stemming from the internal standard were found to be negligible. The results from the Synchroton radiation total reflection X-ray fluorescence analysis of the aerosols showed that 20 min of sampling time gave still enough sample material for elemental determination of most elements. For the determination of the oxidation state of Fe in the aerosols different Fe salts were prepared as a reference from suspensions in isopropanol. The results from the Fe K-edge Synchroton radiation total reflection X-ray fluorescence-X-ray absorption near-edge structure analysis of the aerosol samples showed that mainly Fe(III) was present in

  1. Characterization of atmospheric aerosols using Synchroton radiation total reflection X-ray fluorescence and Fe K-edge total reflection X-ray fluorescence-X-ray absorption near-edge structure

    International Nuclear Information System (INIS)

    Fittschen, U.E.A.; Meirer, F.; Streli, C.; Wobrauschek, P.; Thiele, J.; Falkenberg, G.; Pepponi, G.

    2008-01-01

    In this study a new procedure using Synchrotron total reflection X-ray fluorescence (SR-TXRF) to characterize elemental amounts in atmospheric aerosols down to particle sizes of 0.015 um is presented. The procedure was thoroughly evaluated regarding bounce off effects and blank values. Additionally the potential of total reflection X-ray fluorescence-X-ray absorption near edge structure (SR-TXRF-XANES) for speciation of FeII/III down to amounts of 34 pg in aerosols which were collected for 1 h is shown. The aerosols were collected in the city of Hamburg with a low pressure Berner impactor on Si carriers covered with silicone over time periods of 60 and 20 min each. The particles were collected in four and ten size fractions of 10.0-8.0 μm, 8.0-2.0 μm, 2.0-0.13 μm 0.13-0.015 μm (aerodynamic particle size) and 15-30 nm, 30-60 nm, 60-130 nm, 130-250 nm, 250-500 nm, 0.5-1 μm, 1-2 μm, 2-4 μm, 4-8 μm, 8-16 μm. Prior to the sampling 'bounce off' effects on Silicone and Vaseline coated Si carriers were studied with total reflection X-ray fluorescence. According to the results silicone coated carriers were chosen for the analysis. Additionally, blank levels originating from the sampling device and the calibration procedure were studied. Blank levels of Fe corresponded to 1-10% of Fe in the aerosol samples. Blank levels stemming from the internal standard were found to be negligible. The results from the Synchroton radiation total reflection X-ray fluorescence analysis of the aerosols showed that 20 min of sampling time gave still enough sample material for elemental determination of most elements. For the determination of the oxidation state of Fe in the aerosols different Fe salts were prepared as a reference from suspensions in isopropanol. The results from the Fe K-edge Synchroton radiation total reflection X-ray fluorescence-X-ray absorption near-edge structure analysis of the aerosol samples showed that mainly Fe(III) was present in all particle size fractions

  2. Structure analysis of InN film using extended X-ray absorption fine structure method

    Energy Technology Data Exchange (ETDEWEB)

    Miyajima, T.; Kobayashi, T.; Hirata, S. [Core Technology Development Center, Core Technology and Network Company, Sony Corporation, 4-14-1 Asahi-cho, Atsugi, Kanagawa 243-0014 (Japan); Kudo, Y.; Liu, K.L. [Technology Solutions Center, Sony Corporation, 4-16-1 Okata, Atsugi, Kanagawa 243-0021 (Japan); Uruga, T.; Honma, T. [Japan Synchrotron Radiation Research Institute, Mikazuki-cho, Hyogo 679-5198 (Japan); Saito, Y.; Hori, M.; Nanishi, Y. [Department of Photonics, Ritsumeikan University, 1-1-1 Noji-Higashi, Kusatsu, Shiga 525-8577 (Japan)

    2002-12-01

    We investigated the local atomic structure around In atoms of MBE-grown InN which has a direct bandgap energy of 0.8 eV, using extended X-ray absorption fine structure (EXAFS) oscillation of In K-edge. The signals from the first-nearest neighbor atoms (N) and second-nearest atoms (In) from In atoms were clearly observed and the atomic bond length of In-N and In-In was estimated to be d{sub In-N}=0.215 nm and d{sub In-In}=0.353 nm, respectively. The In-N bond length of d{sub In-In}=0.353 nm was closed to the a-axis lattice constant of a=0.3536 nm, which was determined using X-ray diffraction measurements. The obtained local atomic structure agreed with the calculated ideal structure. We conclude, therefore, that the InN film with a bandgap energy of 0.8 eV has a high structural symmetry in the range of a few A around In atoms. (Abstract Copyright [2002], Wiley Periodicals, Inc.)

  3. Structure analysis of InN film using extended X-ray absorption fine structure method

    International Nuclear Information System (INIS)

    Miyajima, T.; Kobayashi, T.; Hirata, S.; Kudo, Y.; Liu, K.L.; Uruga, T.; Honma, T.; Saito, Y.; Hori, M.; Nanishi, Y.

    2002-01-01

    We investigated the local atomic structure around In atoms of MBE-grown InN which has a direct bandgap energy of 0.8 eV, using extended X-ray absorption fine structure (EXAFS) oscillation of In K-edge. The signals from the first-nearest neighbor atoms (N) and second-nearest atoms (In) from In atoms were clearly observed and the atomic bond length of In-N and In-In was estimated to be d In-N =0.215 nm and d In-In =0.353 nm, respectively. The In-N bond length of d In-In =0.353 nm was closed to the a-axis lattice constant of a=0.3536 nm, which was determined using X-ray diffraction measurements. The obtained local atomic structure agreed with the calculated ideal structure. We conclude, therefore, that the InN film with a bandgap energy of 0.8 eV has a high structural symmetry in the range of a few A around In atoms. (Abstract Copyright [2002], Wiley Periodicals, Inc.)

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

    International Nuclear Information System (INIS)

    Wertz, D.L.; Bissell, M.

    1994-01-01

    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 -1 to 7.5 angstrom -1 where s = (4π/λ) sinΘ. 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 87 . For coals with lower carbon content, Hirsch proposed much smaller lamellae; C 19 for a coal with 80% carbon, and C 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

  5. An investigation of X-ray luminosity versus crystalline powder granularity

    International Nuclear Information System (INIS)

    Janecek, Martin; Borade, Ramesh; Bourret-Courchesne, Edith; Derenzo, Stephen E.

    2011-01-01

    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 4 Ge 3 O 12 (BGO), Lu 2 SiO 5 :Ce 3+ (LSO), YAlO 3 :Ce 3+ (YAP:Ce), and CsBa 2 I 5 :Eu 2+ (CBI) luminosities as a function of crystalline grain size. The highest luminosities were measured for 600- to 1000-μm crystal grain sizes for BGO and LSO, for 310- to 600-μm crystal grain sizes for CBI, and for crystal grains larger than 165 μm 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-μm crystal grain size range down to the 20- to 36-μm 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-μm crystal grains to the 20- to 36-μm range, and CBI exhibited a luminosity decrease of 98% when the grain size decreased from the 310- to 600-μm crystal grain range to the 36- to 50-μm range. We were able to very accurately estimate full-size crystal luminosities from crystalline grains that are larger than 90 μm.

  6. Evaluation of laboratory powder X-ray micro-diffraction for applications in the fields of cultural heritage and forensic science

    Czech Academy of Sciences Publication Activity Database

    Švarcová, Silvie; Kočí, Eva; Bezdička, Petr; Hradil, David; Hradilová, J.

    2010-01-01

    Roč. 398, č. 2 (2010), s. 1061-1076 ISSN 1618-2642 R&D Projects: GA AV ČR KJB200320901 Institutional research plan: CEZ:AV0Z40320502 Keywords : powder X-ray micro-diffraction * quantitative phase analysis * forensic Subject RIV: CA - Inorganic Chemistry Impact factor: 3.841, year: 2010

  7. Thermal expansion behavior study of Co nanowire array with in situ x-ray diffraction and x-ray absorption fine structure techniques

    Science.gov (United States)

    Mo, Guang; Cai, Quan; Jiang, Longsheng; Wang, Wei; Zhang, Kunhao; Cheng, Weidong; Xing, Xueqing; Chen, Zhongjun; Wu, Zhonghua

    2008-10-01

    In situ x-ray diffraction and x-ray absorption fine structure techniques were used to study the structural change of ordered Co nanowire array with temperature. The results show that the Co nanowires are polycrystalline with hexagonal close packed structure without phase change up until 700 °C. A nonlinear thermal expansion behavior has been found and can be well described by a quadratic equation with the first-order thermal expansion coefficient of 4.3×10-6/°C and the second-order thermal expansion coefficient of 5.9×10-9/°C. The mechanism of this nonlinear thermal expansion behavior is discussed.

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

    Energy Technology Data Exchange (ETDEWEB)

    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.

  9. Electronic structure of molecules of substituted benzenes by x-ray spectroscopy. I. Nitrobenzene

    International Nuclear Information System (INIS)

    Yumatov, V.D.; Murakhtanov, V.V.; Salakhutdinov, N.F.; Okotrub, A.V.; Mazalov, L.N.; Logunova, L.G.; Koptyug, V.A.; Furin, G.G.

    1988-01-01

    The electronic structure of the nitrobenzene molecule has been studied by x-ray spectroscopy with the aid of quantum-chemical calculations. The structure of the molecular orbitals of nitrobenzene has been compared with the structure of benzene and nitrogen dioxide. It has been shown in the framework of a fragment-by-fragment analysis that the interaction of the highest occupied π orbitals of the benzene ring and the nitro group is weak

  10. Application of the X-ray diffractometer DRON to the study of long period structures

    International Nuclear Information System (INIS)

    Gordelij, V.I.; Lushchikov, V.I.; Syrykh, A.G.; Cherezon, V.G.

    1991-01-01

    It is shown that the stock-produced X-ray diffractometer DRON can be adapted for the study of long period structures up to ∼150 A. The experimental data on small-angle diffraction spectra, measured on it, from both lamellar and lateral structures of biological and lipid membranes are reported. The data show that lattice constants of these structures could be determined within the accuracy of 1 A. 15 refs.; 7 figs

  11. Atomic structure of large angle grain boundaries determined by quantitative X-ray diffraction techniques

    International Nuclear Information System (INIS)

    Fitzsimmons, M.R.; Sass, S.L.

    1988-01-01

    Quantitative X-ray diffraction techniques have been used to determine the atomic structure of the Σ = 5 and 13 [001] twist boundaries in Au with a resolution of 0.09 Angstrom or better. The reciprocal lattices of these boundaries were mapped out using synchrotron radiation. The atomic structures were obtained by testing model structures against the intensity observations with a chi square analysis. The boundary structure were modeled using polyhedra, including octahedra, special configurations of tetrahedra and Archimedian anti-prisms, interwoven together by the boundary symmetry. The results of this work point to the possibility of obtaining general rules for grain boundary structure based on X-ray diffraction observations that give the atomic positions with high resolution

  12. Pollen structure visualization using high-resolution laboratory-based hard X-ray tomography.

    Science.gov (United States)

    Li, Qiong; Gluch, Jürgen; Krüger, Peter; Gall, Martin; Neinhuis, Christoph; Zschech, Ehrenfried

    2016-10-14

    A laboratory-based X-ray microscope is used to investigate the 3D structure of unstained whole pollen grains. For the first time, high-resolution laboratory-based hard X-ray microscopy is applied to study pollen grains. Based on the efficient acquisition of statistically relevant information-rich images using Zernike phase contrast, both surface- and internal structures of pine pollen - including exine, intine and cellular structures - are clearly visualized. The specific volumes of these structures are calculated from the tomographic data. The systematic three-dimensional study of pollen grains provides morphological and structural information about taxonomic characters that are essential in palynology. Such studies have a direct impact on disciplines such as forestry, agriculture, horticulture, plant breeding and biodiversity. Copyright © 2016 Elsevier Inc. All rights reserved.

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

    Science.gov (United States)

    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.

  14. On the response of Y3Al5O12: Ce (YAG: Ce) powder scintillating screens to medical imaging X-rays

    International Nuclear Information System (INIS)

    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.

    2005-01-01

    The aim of this study was to examine Y 3 Al 5 O 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 166mg/cm 2 were prepared in our laboratory by sedimentation of Y 3 Al 5 O 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 (80-120kVp) 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 (ηC ∼0.03-0.05) and light attenuation coefficients (σ∼26.5cm 2 /g) were derived through this fitting. Y 3 Al 5 O 12 :Ce showed peak emission in the wavelength range 530-550nm. The light emission efficiency was found to be maximum for the 107mg/cm 2 layer. Due to its 'green' emission spectrum, Y 3 Al 5 O 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 3 Al 5 O 12 :Ce could be considered for application in X-ray imaging especially in various digital detectors

  15. Structure investigation, spectral, thermal, X-ray and mass characterization of piroxicam and its metal complexes

    Science.gov (United States)

    Zayed, M. A.; Nour El-Dien, F. A.; Mohamed, Gehad G.; El-Gamel, Nadia E. A.

    2004-10-01

    [M(H 2L) 2](A) 2. yH 2O (where H 2L: neutral piroxicam (Pir), A: Cl - in case of Ni(II) or acetate anion in case of Cu(II) and Zn(II) ions and y=0-2.5) and [M(H 2L) 3](A) z. yH 2O (A: SO 42- in case of Fe(II) ion ( z=1) or Cl - in case of Fe(III) ( z=3) and Co(II) ions ( z=2) and y=1-4) chelates are prepared and characterized using elemental analyses, IR, magnetic and electronic reflectance measurements, mass spectra and thermal analyses. IR spectra reveal that Pir behaves a neutral bidentate ligand coordinated to the metal ions through the pyridyl-N and carbonyl-O of the amide moiety. The reflectance and magnetic moment measurements reveal that these chelates have tetrahedral, square planar and octahedral geometrical structures. Mass spectra and thermal analyses are also used to confirm the proposed formulae and the possible fragments resulted from fragmentation of Pir and its chelates. The thermal behaviour of the chelates (TGA and DTA) are discussed in detail and the thermal stability of the anhydrous chelates follow the order Ni(II)≅Cu(II)X-ray powder diffraction was also used as a confirmatory tool to elucidate the crystallinity of the chelates.

  16. X-ray and neutron powder investigations of pure and yttrium doped CeO2 at temperatures up to 1600 K

    International Nuclear Information System (INIS)

    Berber, K.; Martin, U.; Mursic, Z.; Schneider, J.; Boysen, H.; Frey, F.

    1991-01-01

    Ceria, CeO 2 powders and sintermaterials with different amounts of yttria, Y 2 O 3 , (0-10 mole %) were investigated up to 1600 K by X-ray and neutron powder diffraction. In the sample with 3 mole % yttria the onset of a solid-state reaction or a kind of phase change at 900 K is indicated by a change of the lattice expansion coefficient and by an increase of the slope of the B iso (T) curve. Microstrains are present in the sintered material above 900 K. Anharmonic contributions to the temperature factor of the oxygens become significant at higher temperatures. We deduce from a non-zero part B T ≠0 some static disorder within the O-sublattice. Pdf-maps of the oxygens show clearly deformations of the 'normal' isotropic behaviour, but exceptional smearing out or even closed pathways are not observed. Thus, the superior anionic conductivity of this material is not reflected by the features of the averaged structure. It is most likely due to a disordered 'interface-structure' between ordered domains. A temperature dependent 'structured' background scattering supports this conclusion. (author) 6 figs., 9 refs

  17. Dual-energy X-ray absorptiometry for the simultaneous determination of Density and Moisture Content in Porous Structural Materials

    DEFF Research Database (Denmark)

    Hansen, Kurt Kielsgaard; Jensen, Signe Kamp; Gerward, Leif

    1999-01-01

    The paper describes the dual-energy x-ray equipment, which consists of a x-ray source, filters and a detector. The x-ray beam can be moved automatically in two dimensions relative to a fixed specimen. The purpose of the equipment is to measure simultaneously the density and moisture content...... in porous materials relevant for the building industry. The theory of dual-energy x-ray absorptiometry (DEXA) is presented. DEXA results on two combinations of aluminium and acrylic plastic are compared with corresponding values calculated from the geometry of the experimental setup. The results from the x......-ray measurements show good agreement with results from the two standard materials which imitate water in a porous material. On this background the dual-energy x-ray absorptiometry measurement principle can be used on porous structural materials....

  18. 3D observation of the solidified structures by x-ray micro computerized tomography

    International Nuclear Information System (INIS)

    Yasuda, Hideyuki; Ohnaka, Itsuo; Tsuchiyama, Akira; Nakano, Tsukasa; Uesugi, Kentaro

    2003-01-01

    The high flux density of the monochromatized and well-collimated X-ray and the high-resolution detector provide a new 3D observation tool for microstructures of metallic alloys and ceramics. The X-ray micro computerized tomography in BL47XU of SPring-8 (SP-μCT) was applied to observe microstructures produced through the eutectic reaction for Sn-based alloys and an Al 2 O 3 -Y 2 O 3 oxide system. The constituent phases in the eutectic structures were three-dimensionally identified, in which the lamellar spacing ranged from several to 10 μm. Since the 3D structure of the unidirectionally solidified specimens contains history of the eutectic structure formation, the 3D structure obtained by SP-μCT gives useful information to consider the microstructure evolution. (author)

  19. Three dimensional analysis of coelacanth body structure by computer graphics and X-ray CT images

    International Nuclear Information System (INIS)

    Suzuki, Naoki; Hamada, Takashi.

    1990-01-01

    Three dimensional imaging processes were applied for the structural and functional analyses of the modern coelacanth (Latimeria chalumnae). Visualization of the obtained images is performed with computer graphics on the basis of serial images by an X-ray CT scanning method. Reconstruction of three dimensional images of the body structure of coelacanth using the volume rendering and surface rendering methods provides us various information about external and internal shapes of this exquisite fish. (author)

  20. Atomic structure of machined semiconducting chips: An x-ray absorption spectroscopy study

    Energy Technology Data Exchange (ETDEWEB)

    Paesler, M.; Sayers, D.

    1988-12-01

    X-ray absorption spectroscopy (XAS) has been used to examine the atomic structure of chips of germanium that were produced by single point diamond machining. It is demonstrated that although the local (nearest neighbor) atomic structure is experimentally quite similar to that of single crystal specimens information from more distant atoms indicates the presence of considerable stress. An outline of the technique is given and the strength of XAS in studying the machining process is demonstrated.

  1. Study on mineral components of rat calvaria by means of X-ray powder diffraction analysis and Raman microprobe spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Tamura, Norihiro [Meikai Univ., Sakado, Saitama (Japan). School of Dentistry

    2000-07-01

    The present study was designed to examine the occurrence of the precursor minerals of hydroxyapatite (HA) during the process of HA formation in the rat calvaria. Dried and powdered rat calvaria and synthetic samples, such as HA, dicalcium phosphate dihydrate (DCPD), octacalcium phosphate (OCP), ({beta}-calcium pyrophosphate) and ({beta}-tricalcium phosphate), were used. Determinations were carried out by X-ray powder diffraction and Raman microprobe spectrometry. In general, significant widening of the diffraction peaks was shown to occur after the plasma ashing was performed for the X-ray diffraction. As a result, two adjacent peaks seen normally in the diffraction angles (2 {theta}) 30-35 deg, which is a characteristic feature of HA, were found to fuse with each other, forming a widened single peak. Also, there was a tendency for the intensity of the diffraction peaks to increase with age. With regard to the effect of plasma ashing on the crystallograms of synthetic specimens, all specimens manifested sharp peak patterns except DCPD and OCP. In contrast, a widening of diffraction peaks was observed in the DCPD and OCP samples, indicating that crystallinity had changed during the pretreatment. Results obtained from both vital and synthetic samples after heat treatment at 1000 deg C were as follow: Clearcut diffraction patterns, characteristics of HA, were obtained in all of the calvaria samples. Further, {beta}-TCP was produced by heat treatment of OCP, and its pattern was detected in the samples from rats younger than 6 days of age. Amounts of {beta}-TCP in percentage were disclosed to be 40.2% in embryonal samples, 28.4% in newborn samples, and 18.6% in 6-day-old samples. But no {beta}-TCP could be detected in the 12-week-old samples, indicating that the amount of {beta}-TCP in calvaria decreased with age. We also found that ashing pretreatment did not cause any changes in the samples of HA, {beta}-CPP, and {beta}-TCP. Further, DCPD and {beta}-CPP samples shared

  2. Study on mineral components of rat calvaria by means of X-ray powder diffraction analysis and Raman microprobe spectroscopy

    International Nuclear Information System (INIS)

    Tamura, Norihiro

    2000-01-01

    The present study was designed to examine the occurrence of the precursor minerals of hydroxyapatite (HA) during the process of HA formation in the rat calvaria. Dried and powdered rat calvaria and synthetic samples, such as HA, dicalcium phosphate dihydrate (DCPD), octacalcium phosphate (OCP), (β-calcium pyrophosphate) and (β-tricalcium phosphate), were used. Determinations were carried out by X-ray powder diffraction and Raman microprobe spectrometry. In general, significant widening of the diffraction peaks was shown to occur after the plasma ashing was performed for the X-ray diffraction. As a result, two adjacent peaks seen normally in the diffraction angles (2 θ) 30-35 deg, which is a characteristic feature of HA, were found to fuse with each other, forming a widened single peak. Also, there was a tendency for the intensity of the diffraction peaks to increase with age. With regard to the effect of plasma ashing on the crystallograms of synthetic specimens, all specimens manifested sharp peak patterns except DCPD and OCP. In contrast, a widening of diffraction peaks was observed in the DCPD and OCP samples, indicating that crystallinity had changed during the pretreatment. Results obtained from both vital and synthetic samples after heat treatment at 1000 deg C were as follow: Clearcut diffraction patterns, characteristics of HA, were obtained in all of the calvaria samples. Further, β-TCP was produced by heat treatment of OCP, and its pattern was detected in the samples from rats younger than 6 days of age. Amounts of β-TCP in percentage were disclosed to be 40.2% in embryonal samples, 28.4% in newborn samples, and 18.6% in 6-day-old samples. But no β-TCP could be detected in the 12-week-old samples, indicating that the amount of β-TCP in calvaria decreased with age. We also found that ashing pretreatment did not cause any changes in the samples of HA, β-CPP, and β-TCP. Further, DCPD and β-CPP samples shared the same diffraction pattern, and OCP

  3. Magnetic and structural properties of Fe/Pd multilayers studied by magnetic x-ray dichroism and x-ray absorption spectroscopy

    International Nuclear Information System (INIS)

    Mini, S.M.; Fullerton, E.E.; Sowers, C.H.; Fontaine, A.; Pizzini, S.; Bommannavar, A.S.; Traverse, A.; Baudelet, F.

    1994-12-01

    The results of magnetic circular x-ray dichroism (MCXD) measurements and extended x-ray absorption fine structure measurements (EXAFS) of the Fe K-edges of textured Fe(110)/Pd(111) multilayers are reported. The EXAFS results indicates that the iron in the system goes from bcc to a more densely packed system as the thickness of the iron layer is decreased. The magnetic properties were measured by SQUID magnetometry from 5-350 K. For all the samples, the saturation magnetization was significantly enhanced over the bulk values indicating the interface Pd atoms are polarized by the Fe layer. The enhancement corresponds to a moment of ∼2.5μ B per interface Pd atom

  4. Synchrotron x-ray methods in studies of thin organic film structure

    International Nuclear Information System (INIS)

    Gentle, I.

    2002-01-01

    Full text: In recent years, the study of the structures of organic films as thin as a single monolayer has been revolutionized by methods that take advantage of the characteristics of synchrotron radiation. In particular, the methods of grazing incidence X-ray diffraction (GIXD) and X-ray reflectivity have led to a number of valuable insights into structural aspects of thin films at molecular resolution. Our group has been studying films formed at the air/water interface as insoluble monolayers and subsequently transferred to solid substrates using either the vertical (Langmuir-Blodgett) or horizontal (Langmuir-Schaeffer) methods. The main aim of these experiments is to exert control over film structure in the direction parallel to the substrate surface. This is highly desirable in order to design devices that exploit the optical and electrooptical properties of functional materials, but is difficult to do. By varying the chemical structure of the film materials and controlling deposition conditions a degree of control is possible, but only using synchrotron methods can it be easily verified. We have also developed a novel method of rapidly collecting data from GIXD measurements by the application of area detection (imaging plates), which has made possible measurements of dynamic processes such as in-situ annealing. Such measurements are not possible using traditional scanning methods. One area of current interest is films composed of porphyrins as functional materials, either alone or as mixed films with fatty acids. We have been investigating ways of assembling porphyrins in such a way as to overcome the tendency to aggregate, and to produce patterning and ordered structures in the plane of the interface. Examples will be given of how film composition and deposition method affects the final structure, and of how X-ray methods can be used to elucidate both the structures and the mechanisms. Copyright (2002) Australian X-ray Analytical Association Inc

  5. Structural dissection of human metapneumovirus phosphoprotein using small angle x-ray scattering.

    Science.gov (United States)

    Renner, Max; Paesen, Guido C; Grison, Claire M; Granier, Sébastien; Grimes, Jonathan M; Leyrat, Cédric

    2017-11-01

    The phosphoprotein (P) is the main and essential cofactor of the RNA polymerase (L) of non-segmented, negative-strand RNA viruses. P positions the viral polymerase onto its nucleoprotein-RNA template and acts as a chaperone of the nucleoprotein (N), thereby preventing nonspecific encapsidation of cellular RNAs. The phosphoprotein of human metapneumovirus (HMPV) forms homotetramers composed of a stable oligomerization domain (P core ) flanked by large intrinsically disordered regions (IDRs). Here we combined x-ray crystallography of P core with small angle x-ray scattering (SAXS)-based ensemble modeling of the full-length P protein and several of its fragments to provide a structural description of P that captures its dynamic character, and highlights the presence of varyingly stable structural elements within the IDRs. We discuss the implications of the structural properties of HMPV P for the assembly and functioning of the viral transcription/replication machinery.

  6. Structure of liposome encapsulating proteins characterized by X-ray scattering and shell-modeling

    International Nuclear Information System (INIS)

    Hirai, Mitsuhiro; Kimura, Ryota; Takeuchi, Kazuki; Hagiwara, Yoshihiko; Kawai-Hirai, Rika; Ohta, Noboru; Igarashi, Noriyuki; Shimuzu, Nobutaka

    2013-01-01

    Wide-angle X-ray scattering data using a third-generation synchrotron radiation source are presented. Lipid liposomes are promising drug delivery systems because they have superior curative effects owing to their high adaptability to a living body. Lipid liposomes encapsulating proteins were constructed and the structures examined using synchrotron radiation small- and wide-angle X-ray scattering (SR-SWAXS). The liposomes were prepared by a sequential combination of natural swelling, ultrasonic dispersion, freeze-throw, extrusion and spin-filtration. The liposomes were composed of acidic glycosphingolipid (ganglioside), cholesterol and phospholipids. By using shell-modeling methods, the asymmetric bilayer structure of the liposome and the encapsulation efficiency of proteins were determined. As well as other analytical techniques, SR-SWAXS and shell-modeling methods are shown to be a powerful tool for characterizing in situ structures of lipid liposomes as an important candidate of drug delivery systems

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

    International Nuclear Information System (INIS)

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

    1992-01-01

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

  8. Direct determination of trace elements in boron nitride powders by slurry sampling total reflection X-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    Amberger, Martin A.; Hoeltig, Michael; Broekaert, Jose A.C.

    2010-01-01

    The use of slurry sampling total reflection X-ray fluorescence spectrometry (SlS-TXRF) for the direct determination of Ca, Cr, Cu, Fe, Mn and Ti in four boron nitride powders has been described. Measurements of the zeta potential showed that slurries with good stabilities can be obtained by the addition of polyethylenimine (PEI) at a concentration of 0.1 wt.% and by adjusting the pH at 4. For the optimization of the concentration of boron nitride in the slurries the net line intensities and the signal to background ratios were determined for the trace elements Ca and Ti as well as for the internal standard element Ga in the case of concentrations of boron nitride ranging from 1 to 30 mg mL -1 . As a compromise with respect to high net line intensities and high signal to background ratios, concentrations of 5 mg mL -1 of boron nitride were found suitable and were used for all further measurements. The limits of detection of SlS-TXRF for the boron nitride powders were found to range from 0.062 to 1.6 μg g -1 for Cu and Ca, respectively. Herewith, they are higher than those obtained in solid sampling and slurry sampling graphite furnace atomic absorption spectrometry (SoS-GFAAS, SlS-GFAAS) as well as those of solid sampling electrothermal evaporation inductively coupled plasma optical emission spectrometry (SoS-ETV-ICP-OES). For Ca and Fe as well as for Cu and Fe, however, they were found to be lower than for GFAAS and for ICP-OES subsequent to wet chemical digestion, respectively. The universal applicability of SlS-TXRF to the analysis of samples with a wide variety of matrices could be demonstrated by the analysis of certified reference materials such as SiC, Al 2 O 3 , powdered bovine liver and borate ore with a single calibration. The correlation coefficients of the plots for the values found for Ca, Fe and Ti by SlS-TXRF in the boron nitride powders as well as in the before mentioned samples versus the reference values for the respective samples over a

  9. Direct determination of trace elements in boron nitride powders by slurry sampling total reflection X-ray fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Amberger, Martin A.; Hoeltig, Michael [University of Hamburg, Institute for Inorganic and Applied Chemistry, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany); Broekaert, Jose A.C., E-mail: jose.broekaert@chemie.uni-hamburg.d [University of Hamburg, Institute for Inorganic and Applied Chemistry, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany)

    2010-02-15

    The use of slurry sampling total reflection X-ray fluorescence spectrometry (SlS-TXRF) for the direct determination of Ca, Cr, Cu, Fe, Mn and Ti in four boron nitride powders has been described. Measurements of the zeta potential showed that slurries with good stabilities can be obtained by the addition of polyethylenimine (PEI) at a concentration of 0.1 wt.% and by adjusting the pH at 4. For the optimization of the concentration of boron nitride in the slurries the net line intensities and the signal to background ratios were determined for the trace elements Ca and Ti as well as for the internal standard element Ga in the case of concentrations of boron nitride ranging from 1 to 30 mg mL{sup -1}. As a compromise with respect to high net line intensities and high signal to background ratios, concentrations of 5 mg mL{sup -1} of boron nitride were found suitable and were used for all further measurements. The limits of detection of SlS-TXRF for the boron nitride powders were found to range from 0.062 to 1.6 mug g{sup -1} for Cu and Ca, respectively. Herewith, they are higher than those obtained in solid sampling and slurry sampling graphite furnace atomic absorption spectrometry (SoS-GFAAS, SlS-GFAAS) as well as those of solid sampling electrothermal evaporation inductively coupled plasma optical emission spectrometry (SoS-ETV-ICP-OES). For Ca and Fe as well as for Cu and Fe, however, they were found to be lower than for GFAAS and for ICP-OES subsequent to wet chemical digestion, respectively. The universal applicability of SlS-TXRF to the analysis of samples with a wide variety of matrices could be demonstrated by the analysis of certified reference materials such as SiC, Al{sub 2}O{sub 3}, powdered bovine liver and borate ore with a single calibration. The correlation coefficients of the plots for the values found for Ca, Fe and Ti by SlS-TXRF in the boron nitride powders as well as in the before mentioned samples versus the reference values for the respective

  10. Complementing high-throughput X-ray powder diffraction data with quantum-chemical calculations

    DEFF Research Database (Denmark)

    Naelapaa, Kaisa; van de Streek, Jacco; Rantanen, Jukka

    2012-01-01

    of piroxicam form III. These combined experimental/quantum-chemical methods can provide access to reliable structural information in the course of an intensive experimentally based solid-form screening activity or in other circumstances wherein single crystals might never be viable, for example, for polymorphs...

  11. The structural analysis of zinc borate glass by laboratory EXAFS and X-ray diffraction measurements

    International Nuclear Information System (INIS)

    Kajinami, Akihiko; Harada, Yasushi; Inoue, Shinsuke; Deki, Shigehito; Umesaki, Norimasa

    1999-01-01

    The structure of zinc borate glass has been investigated by laboratory EXAFS and X-ray diffraction measurement as preliminary investigations for the detailed study in SPring-8. The zinc borate glass was prepared in the range from 40 to 65 mol% of zinc oxide content. The X-ray diffraction was measured by horizontal θ-θ goniometer with 60 kV and 300 mA output of Mo target. The EXAFS of zinc borate glass was measured by laboratory EXAFS system with 20 kV, 100 mA output of Mo target for the K absorption edge of zinc atom. From the X-ray diffraction and the EXAFS measurements, it is found that the zinc ion is surrounded by four oxygen atoms and formed a tetrahedral structure whose (Zn-O) distance is about 2 A and that the structure is unchanged with the zinc oxide content. The diffraction data show that the neighboring structure of boron atom transforms from BO 4 tetrahedra to BO 3 tetragonal planar structure with increasing of the zinc oxide content. (author)

  12. A multiple CCD X-ray detector and its first operation with synchrotron radiation X-ray beam

    CERN Document Server

    Suzuki, M; Kumasaka, T; Sato, K; Toyokawa, H; Aries, I F; Jerram, P A; Ueki, T

    1999-01-01

    A 4x4 array structure of 16 identical CCD X-ray detector modules, called the multiple CCD X-ray detector system (MCCDX), was submitted to its first synchrotron radiation experiment at the protein crystallography station of the RIKEN beamline (BL45XU) at the SPring-8 facility. An X-ray diffraction pattern of cholesterol powder was specifically taken in order to investigate the overall system performance.

  13. Integrative structural modeling with small angle X-ray scattering profiles

    Directory of Open Access Journals (Sweden)

    Schneidman-Duhovny Dina

    2012-07-01

    Full Text Available Abstract Recent technological advances enabled high-throughput collection of Small Angle X-ray Scattering (SAXS profiles of biological macromolecules. Thus, computational methods for integrating SAXS profiles into structural modeling are needed more than ever. Here, we review specifically the use of SAXS profiles for the structural modeling of proteins, nucleic acids, and their complexes. First, the approaches for computing theoretical SAXS profiles from structures are presented. Second, computational methods for predicting protein structures, dynamics of proteins in solution, and assembly structures are covered. Third, we discuss the use of SAXS profiles in integrative structure modeling approaches that depend simultaneously on several data types.

  14. X-ray refractive index: A tool to determine the average composition in multilayer structures

    International Nuclear Information System (INIS)

    Miceli, P.F.; Neumann, D.A.; Zabel, H.

    1986-01-01

    We present a novel and simple method to determine the average composition of multilayers and superlattices by measuring the x-ray refractive index. Since these modulated structures exhibit Bragg reflections at small angles, by using a triple axis x-ray spectrometer we have accurately determined the peak shifts due to refraction in GaAs/Al/sub x/Ga/sub 1-x/As and Nb/Ta superlattices. Knowledge of the refractive index provides the average fractional composition of the periodic structure since the refractive index is a superposition of the refractive indices of the atomic constituents. We also present a critical discussion of the method and compare the values of the average fractional composition obtained in this manner to the values obtained from the lattice parameter change in the GaAs/Al/sub x/Ga/sub 1-x/As superlattices due to the Al

  15. Structured photocathodes for improved high-energy x-ray efficiency in streak cameras

    Energy Technology Data Exchange (ETDEWEB)

    Opachich, Y. P., E-mail: opachiyp@nv.doe.gov; Huffman, E.; Koch, J. A. [National Security Technologies, LLC, Livermore, California 94551 (United States); Bell, P. M.; Bradley, D. K.; Hatch, B.; Landen, O. L.; MacPhee, A. G.; Nagel, S. R. [Lawrence Livermore National Laboratory, Livermore, California 94551 (United States); Chen, N.; Gopal, A.; Udin, S. [Nanoshift LLC, Emeryville, California 94608 (United States); Feng, J. [Lawrence Berkeley National Laboratory, Berkeley, California 94720 (United States); Hilsabeck, T. J. [General Atomics, San Diego, California 92121 (United States)

    2016-11-15

    We have designed and fabricated a structured streak camera photocathode to provide enhanced efficiency for high energy X-rays (1–12 keV). This gold coated photocathode was tested in a streak camera and compared side by side against a conventional flat thin film photocathode. Results show that the measured electron yield enhancement at energies ranging from 1 to 10 keV scales well with predictions, and that the total enhancement can be more than 3×. The spatial resolution of the streak camera does not show degradation in the structured region. We predict that the temporal resolution of the detector will also not be affected as it is currently dominated by the slit width. This demonstration with Au motivates exploration of comparable enhancements with CsI and may revolutionize X-ray streak camera photocathode design.

  16. X-ray diffuse scattering effects from Coulomb-type defects in multilayered structures

    International Nuclear Information System (INIS)

    Olikhovskii, S.I.; Molodkin, V.B.; Skakunova, E.S.; Kislovskii, E.N.; Fodchuk, I.M.

    2009-01-01

    The theoretical X-ray diffraction model starting from Takagi-Taupin equation has been developed for the description of coherent and diffuse components of the rocking curve (RC) measured from the multilayered crystal structure with randomly distributed Coulomb-type defects in all the layers and substrate. The model describes both diffuse scattering (DS) intensity distribution and influence of DS on attenuation and angular redistribution of the coherent X-ray scattering intensity. By analyzing the total measured RC with using the proposed diffraction model, the chemical compositions, strains, and characteristics of dislocation loops in layers and substrate of the multilayered structure with InGaAsN/GaAs single quantum well have been determined. (Abstract Copyright [2009], Wiley Periodicals, Inc.)

  17. Soft x-ray measurement of internal tearing mode structure in a reversed-field pinch

    International Nuclear Information System (INIS)

    Chartas, G.; Hokin, S.

    1991-01-01

    The structure of internally resonant tearing modes has been studied in the Madison Symmetric Torus reversed-field pinch with a soft x-ray detector system consisting of an imaging array at one toroidal location and several detectors at different toroidal locations. The toroidal mode numbers of m = 1 structures are in the range n = -5, -6, -7. The modes propagate with phase velocity v = 1--6 x 10 6 cm/s, larger than the diamagnetic drift velocity v d ∼ 5 x 10 5 cm/s. Phase locking between modes with different n in manifested as a beating of soft x-ray signals which is found to be strongest near the resonant surfaces of the modes (r/a = 0.1 -- 0.5). 15 refs., 5 figs

  18. Structural characterization of oxidized allotaxially grown CoSi2 layers by x-ray scattering

    International Nuclear Information System (INIS)

    Kaendler, I. D.; Seeck, O. H.; Schlomka, J.-P.; Tolan, M.; Press, W.; Stettner, J.; Kappius, L.; Dieker, C.; Mantl, S.

    2000-01-01

    A series of buried CoSi 2 layers prepared by a modified molecular beam epitaxy process (allotaxy) and a subsequent wet-oxidation process was investigated by x-ray scattering. The oxidation time which determines the depth in which the CoSi 2 layers are located within the Si substrates has been varied during the preparation. The electron density profiles and the structure of the interfaces were extracted from specular reflectivity and diffuse scattering measurements. Crystal truncation rod investigations yielded the structure on an atomic level (crystalline quality). It turns out that the roughness of the CoSi 2 layers increases drastically with increasing oxidation time, i.e., with increasing depth of the buried layers. Furthermore, the x-ray data reveal that the oxidation growth process is diffusion limited. (c) 2000 American Institute of Physics

  19. Rietveld refinement of KLaTiO4 from X-ray powder data

    Directory of Open Access Journals (Sweden)

    Bai-Chuan Zhu

    2011-04-01

    Full Text Available Potassium lanthanum titanate(IV, KLaTiO4, has been synthesized by conventional solid-state reaction. It crystallizes isotypically with the NaLnTiO4 (Ln = La, Pr, Nd, Sm, Eu, Gd, Y and Lu family. Five of the six atoms in the asymmetric unit (one K, one La, one Ti and two O atoms are situated on sites with 4mm symmetry, whereas one O atom has 2mm. site symmetry. The crystal structure can be described as being composed of single layers of distorted corner-sharing TiO6 octahedra extending parallel to (001. The layers are alternately separated by K+ and La3+ cations along [001]. The coordination number of both K+ and La3+ cations is nine, resulting in distorted KO9 and LaO9 polyhedra.

  20. Structural shielding of medical X-ray rooms for diagnostic installations

    International Nuclear Information System (INIS)

    Rabitsch, H.

    1979-06-01

    In Part I (RIG 8), the various design procedures for shielding against X-rays are discussed and compared. In particular, this comparison is carried out between the shielding obtained conforming to the Austrian Regulations for Radiation Protection and that obtained from the DIN-standard DIN 6812; this latter includes the various operating conditions of diagnostic installations up to 150 kV. Several examples for particular structural shielding components in medical radiation rooms are given. (author)

  1. single crystal growth, x-ray structure analysis, optical band gap

    African Journals Online (AJOL)

    2015-09-01

    Sep 1, 2015 ... Hg...Hgand Cl...Cl interactions are stabilizing the structures in 3D pattern. UV-vis absorption spectra illustrate the change in opticalband gap from 3.01eVto 3.42eV on replacing the metal halide group.Raman and Hyper-Raman tensors calculations were performed based on single crystal X-ray data and the ...

  2. Structural transformation of compressed solid Ar: An x-ray diffraction study to 114 GPa

    International Nuclear Information System (INIS)

    Errandonea, D.; Boehler, R.; Japel, S.; Mezouar, M.; Benedetti, L. R.

    2006-01-01

    Room temperature angle-dispersive x-ray diffraction measurements on solid Ar up to 114 GPa reveal evidence of a structural phase transformation after stress relaxation by laser heating. Beyond 49.6 GPa, Ar exhibits the coexistence of fcc and hcp phases with an increasing hcp/fcc ratio, similar to the observation made recently on krypton and xenon. From the present results, we estimate the fcc-to-hcp transition to be completed at 300 GPa

  3. Total reflection X-ray fluorescence analysis with synchrotron radiation monochromatized by multilayer structures

    International Nuclear Information System (INIS)

    Rieder, R.; Wobrauschek, P.; Ladisich, W.; Streli, C.; Aiginger, H.; Garbe, S.; Gaul, G.; Knoechel, A.; Lechtenberg, F.

    1995-01-01

    To achieve lowest detection limits in total reflection X-ray fluorescence analysis (TXRF) synchrotron radiation has been monochromatized by a multilayer structure to obtain a relative broad energy band compared to Bragg single crystals for an efficient excitation. The energy has been set to 14 keV, 17.5 keV, 31 keV and about 55 keV. Detection limits of 20 fg and 150 fg have been achieved for Sr and Cd, respectively. ((orig.))

  4. Study of the argyrophil structures of thymus connective tissue after exposure to X-rays

    International Nuclear Information System (INIS)

    Beletskij, V.K.; Beletskaya, L.V.; Akademiya Meditsinskikh Nauk SSSR, Moscow. Inst. Ehpidemiologii i Mikrobiologii)

    1980-01-01

    Studied are argyrophil structures of thymus connective tissue - histiocytes (appendiculate macrophages) and reticuline fibers after the bulk of lymphoid cells has migrated from the organ due to irradiation of animals with X-rays. 10 intact and 16 experimental guinea pigs subjected to the whole-body irradiation with X-rays in the dose of 1000-3000 rad have been used for investigations. It is shown that argyrophil stroma elements of thymus connective tissue, histiocytes and reticular cells, are rather resistant to X-rays and preserve their argyrophily property in the irradiation with high doses, as well as the epithelial cells of the organ. Paraplastic structures in irradiated animals are expressed more completely being demasked as a result of lymphocyte migration and death. The expressed hypertrophy and proliferation of reticular cells and appendiculate macrophages are probably the response to the alternative process in the organ tissues caused by irradiation. A close structural connection of reticular and epithelial tissues on the territory of both layers of thymus sections is noted

  5. Structural Modification of Cobalt Catalysts: Effect of Wetting Studied by X-Ray and Infrared Techniques

    Directory of Open Access Journals (Sweden)

    Khodakov A.

    1999-07-01

    Full Text Available The effect of wetting on the structure and localisation of cobalt species on various supports (Al2O3, SiO2, TiO2, HZSM-5 zeolite was studied using X-ray diffraction, Fourier transform infrared spectroscopy with CO as a molecular probe, X-ray photoelectron spectroscopy and extended X-ray absorption fine structure analysis. Aqueous impregnation to incipient wetness of reduced and passivated cobalt catalysts results, even in the absence of any promoter, in a considerable decrease in the concentration of Co crystalline phases and modifies the surface sites. The decrease in the concentration of Co3O4 crystallites was especially pronounced on silica supported catalysts prepared via impregnation of cobalt and on a mixture of Co3O4 and HZSM-5 zeolite. Saturation with water of the passivated Co/SiO2 sample results in an amorphous solid with a local structure close to that of Co2SiO4. For Co/Al2O3 and Co/TiO2 catalysts, the effect of wetting on the concentration of Co3O4 crystalline phase was considerably smaller.

  6. Predicting X-ray diffuse scattering from translation–libration–screw structural ensembles

    International Nuclear Information System (INIS)

    Van Benschoten, Andrew H.; Afonine, Pavel V.; Terwilliger, Thomas C.; Wall, Michael E.; Jackson, Colin J.; Sauter, Nicholas K.; Adams, Paul D.; Urzhumtsev, Alexandre; Fraser, James S.

    2015-01-01

    A method of simulating X-ray diffuse scattering from multi-model PDB files is presented. Despite similar agreement with Bragg data, different translation–libration–screw refinement strategies produce unique diffuse intensity patterns. Identifying the intramolecular motions of proteins and nucleic acids is a major challenge in macromolecular X-ray crystallography. Because Bragg diffraction describes the average positional distribution of crystalline atoms with imperfect precision, the resulting electron density can be compatible with multiple models of motion. Diffuse X-ray scattering can reduce this degeneracy by reporting on correlated atomic displacements. Although recent technological advances are increasing the potential to accurately measure diffuse scattering, computational modeling and validation tools are still needed to quantify the agreement between experimental data and different parameterizations of crystalline disorder. A new tool, phenix.diffuse, addresses this need by employing Guinier’s equation to calculate diffuse scattering from Protein Data Bank (PDB)-formatted structural ensembles. As an example case, phenix.diffuse is applied to translation–libration–screw (TLS) refinement, which models rigid-body displacement for segments of the macromolecule. To enable the calculation of diffuse scattering from TLS-refined structures, phenix.tls-as-xyz builds multi-model PDB files that sample the underlying T, L and S tensors. In the glycerophosphodiesterase GpdQ, alternative TLS-group partitioning and different motional correlations between groups yield markedly dissimilar diffuse scattering maps with distinct implications for molecular mechanism and allostery. These methods demonstrate how, in principle, X-ray diffuse scattering could extend macromolecular structural refinement, validation and analysis

  7. Predicting X-ray diffuse scattering from translation–libration–screw structural ensembles

    Energy Technology Data Exchange (ETDEWEB)

    Van Benschoten, Andrew H. [University of California San Francisco, San Francisco, CA 94158 (United States); Afonine, Pavel V. [Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Terwilliger, Thomas C.; Wall, Michael E. [Los Alamos National Laboratory, Los Alamos, NM 87545 (United States); Jackson, Colin J. [Australian National University, Canberra, ACT 2601 (Australia); Sauter, Nicholas K. [Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Adams, Paul D. [Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); University of California Berkeley, Berkeley, CA 94720 (United States); Urzhumtsev, Alexandre [Institut de Génétique et de Biologie Moléculaire et Cellulaire, CNRS–INSERM–UdS, 1 Rue Laurent Fries, BP 10142, 67404 Illkirch (France); Université de Lorraine, BP 239, 54506 Vandoeuvre-les-Nancy (France); Fraser, James S., E-mail: james.fraser@ucsf.edu [University of California San Francisco, San Francisco, CA 94158 (United States)

    2015-07-28

    A method of simulating X-ray diffuse scattering from multi-model PDB files is presented. Despite similar agreement with Bragg data, different translation–libration–screw refinement strategies produce unique diffuse intensity patterns. Identifying the intramolecular motions of proteins and nucleic acids is a major challenge in macromolecular X-ray crystallography. Because Bragg diffraction describes the average positional distribution of crystalline atoms with imperfect precision, the resulting electron density can be compatible with multiple models of motion. Diffuse X-ray scattering can reduce this degeneracy by reporting on correlated atomic displacements. Although recent technological advances are increasing the potential to accurately measure diffuse scattering, computational modeling and validation tools are still needed to quantify the agreement between experimental data and different parameterizations of crystalline disorder. A new tool, phenix.diffuse, addresses this need by employing Guinier’s equation to calculate diffuse scattering from Protein Data Bank (PDB)-formatted structural ensembles. As an example case, phenix.diffuse is applied to translation–libration–screw (TLS) refinement, which models rigid-body displacement for segments of the macromolecule. To enable the calculation of diffuse scattering from TLS-refined structures, phenix.tls-as-xyz builds multi-model PDB files that sample the underlying T, L and S tensors. In the glycerophosphodiesterase GpdQ, alternative TLS-group partitioning and different motional correlations between groups yield markedly dissimilar diffuse scattering maps with distinct implications for molecular mechanism and allostery. These methods demonstrate how, in principle, X-ray diffuse scattering could extend macromolecular structural refinement, validation and analysis.

  8. Transmission X-ray scattering as a probe for complex liquid-surface structures

    Energy Technology Data Exchange (ETDEWEB)

    Fukuto, Masafumi; Yang, Lin; Nykypanchuk, Dmytro; Kuzmenko, Ivan

    2016-01-28

    The need for functional materials calls for increasing complexity in self-assembly systems. As a result, the ability to probe both local structure and heterogeneities, such as phase-coexistence and domain morphologies, has become increasingly important to controlling self-assembly processes, including those at liquid surfaces. The traditional X-ray scattering methods for liquid surfaces, such as specular reflectivity and grazing-incidence diffraction, are not well suited to spatially resolving lateral heterogeneities due to large illuminated footprint. A possible alternative approach is to use scanning transmission X-ray scattering to simultaneously probe local intermolecular structures and heterogeneous domain morphologies on liquid surfaces. To test the feasibility of this approach, transmission small- and wide-angle X-ray scattering (TSAXS/TWAXS) studies of Langmuir films formed on water meniscus against a vertically immersed hydrophilic Si substrate were recently carried out. First-order diffraction rings were observed in TSAXS patterns from a monolayer of hexagonally packed gold nanoparticles and in TWAXS patterns from a monolayer of fluorinated fatty acids, both as a Langmuir monolayer on water meniscus and as a Langmuir–Blodgett monolayer on the substrate. The patterns taken at multiple spots have been analyzed to extract the shape of the meniscus surface and the ordered-monolayer coverage as a function of spot position. These results, together with continual improvement in the brightness and spot size of X-ray beams available at synchrotron facilities, support the possibility of using scanning-probe TSAXS/TWAXS to characterize heterogeneous structures at liquid surfaces.

  9. PREFACE: Structure and dynamics determined by neutron and x-ray scattering Structure and dynamics determined by neutron and x-ray scattering

    Science.gov (United States)

    Müller-Buschbaum, Peter

    2011-06-01

    Neutron and x-ray scattering have emerged as powerful methods for the determination of structure and dynamics. Driven by emerging new, powerful neutron and synchrotron radiation sources, the continuous development of new instrumentation and novel scattering techniques gives rise to exciting possibilities. For example, in situ observations become possible via a high neutron or x-ray flux at the sample and, as a consequence, morphological transitions with small time constants can be detected. This special issue covers a broad range of different materials from soft to hard condensed matter. Hence, different material classes such as colloids, polymers, alloys, oxides and metals are addressed. The issue is dedicated to the 60th birthday of Professor Winfried Petry, scientific director of the Research Neutron Source Heinz Maier-Leibnitz (FRM-II), Germany, advisor at the physics department for the Bayerische Elite-Akademie, chair person of the Arbeitsgemeinschaft Metall- und Materialphysik of the German Physical Society (DPG) and a member of the professional council of the German Science Foundation (Deutsche Forschungsgemeinschaft, DFG). We would like to acknowledge and thank all contributors for their submissions, which made this special issue possible in the first place. Moreover, we would like to thank the staff at IOP Publishing for helping us with the administrative aspects and for coordinating the refereeing process, and Valeria Lauter for the beautiful cover artwork. Finally, to the readers, we hope that you find this special issue a valuable resource that provides insights into the present possibilities of neutron and x-ray scattering as powerful tools for the investigation of structure and dynamics. Structure and dynamics determined by neutron and x-ray scattering contents In situ studies of mass transport in liquid alloys by means of neutron radiography F Kargl, M Engelhardt, F Yang, H Weis, P Schmakat, B Schillinger, A Griesche and A Meyer Magnetic spin

  10. X-ray photoemission electron microscopy, a tool for the investigation of complex magnetic structures

    International Nuclear Information System (INIS)

    Scholl, Andreas; Ohldag, Hendrik; Nolting, Frithjof; Stohr, Joachim; Padmore, Howard A.

    2001-01-01

    X-ray Photoemission Electron Microscopy unites the chemical specificity and magnetic sensitivity of soft x-ray absorption techniques with the high spatial resolution of electron microscopy. The discussed instrument possesses a spatial resolution of better than 50 nm and is located at a bending magnet beamline at the Advanced Light Source, providing linearly and circularly polarized radiation between 250 and 1300 eV. We will present examples which demonstrate the power of this technique applied to problems in the field of thin film magnetism. The chemical and elemental specificity is of particular importance for the study of magnetic exchange coupling because it allows separating the signal of the different layers and interfaces in complex multi-layered structures

  11. Template assisted self-assembly of iron oxide nanoparticles: An x-ray structural analysis

    Energy Technology Data Exchange (ETDEWEB)

    Mishra, D. [Department of Physics, Ruhr-University Bochum, 44780 Bochum (Germany); Institut fuer Optik und Atomare Physik, Technische Universitaet Berlin, Strasse des 17. Juni 135, 10623 Berlin (Germany); Zabel, H. [Department of Physics, Ruhr-University Bochum, 44780 Bochum (Germany); Ulyanov, S. V. [St.-Petersburg State University, Ul' yanovskaya ul.1, Petrodvorets, St.-Petersburg 198904 (Russian Federation); St.-Petersburg University of Commerce and Economics, St.-Petersburg 194018 (Russian Federation); Romanov, V. P. [St.-Petersburg State University, Ul' yanovskaya ul.1, Petrodvorets, St.-Petersburg 198904 (Russian Federation); Uzdin, V. M. [St.-Petersburg State University, Ul' yanovskaya ul.1, Petrodvorets, St.-Petersburg 198904 (Russian Federation); St.-Petersburg National Research University of Information Technologies, Mechanics and Optics, 49, Kronverkskij, St.-Petersburg 197101 (Russian Federation)

    2014-02-07

    We have fabricated by e-beam lithography periodic arrays of rectangular shaped trenches of different widths into Si substrates. The trenches were filled with iron oxide nanoparticles, 20 nm in diameter, by spin-coating them onto the Si substrate. The trenches have the purpose to assist the self-assembly of the iron oxide nanoparticles. Using x-ray scattering techniques, we have analyzed the structure factor of the trenches before and after filling in order to determine the filling factor. We present a theoretical analysis of the x-ray scattering function within the distorted-wave Born approximation and we present a quantitative comparison between theory and experiment.

  12. Template assisted self-assembly of iron oxide nanoparticles: An x-ray structural analysis

    International Nuclear Information System (INIS)

    Mishra, D.; Zabel, H.; Ulyanov, S. V.; Romanov, V. P.; Uzdin, V. M.

    2014-01-01

    We have fabricated by e-beam lithography periodic arrays of rectangular shaped trenches of different widths into Si substrates. The trenches were filled with iron oxide nanoparticles, 20 nm in diameter, by spin-coating them onto the Si substrate. The trenches have the purpose to assist the self-assembly of the iron oxide nanoparticles. Using x-ray scattering techniques, we have analyzed the structure factor of the trenches before and after filling in order to determine the filling factor. We present a theoretical analysis of the x-ray scattering function within the distorted-wave Born approximation and we present a quantitative comparison between theory and experiment

  13. X-ray absorption study of the electronic structure of Mn-doped amorphous Si

    Energy Technology Data Exchange (ETDEWEB)

    Arenholz, Elke; Zeng, Li; Huegel, A.; Helgren, E.; Hellman, F.; Piamonteze, C.; Arenholz, E.

    2008-03-08

    The electronic structure of Mn in amorphous Si (a-Mn{sub x}Si{sub 1?x}) is studied by X-ray absorption spectroscopy at the Mn L{sub 3,2} edges for x = 0.005-0.18. Except the x = 0.005 sample, which shows a slight signature of Mn{sup 2+} atomic multiplets associated with a local Mn moment, all samples have broad and featureless L{sub 3,2} absorption peaks, corresponding to an itinerant state for all 3d electrons. The broad X-ray absorption spectra exclude the possibility of a localized 3d moment and explain the unexpectedly quenched Mn moment in this magnetically-doped amorphous semiconductor. Such a fully delocalized d state of Mn dopant in Si has not been previously suggested.

  14. Determining biological fine structure by differential absorption of soft x-rays

    International Nuclear Information System (INIS)

    Panessa-Warren, B.J.; Warren, J.B.

    1979-06-01

    The use of soft x-ray contact microscopy in examining histochemically treated human tissue embedded in plastic and exposed as unstained thin sections is demonstrated. When our preliminary data revealed that we could clearly image not only the histochemical reaction product, but the unstained biological fine structure of the surrounding tissues, we decided to test our hypothesis further and see if we could image unstained biological molecular aggregates as well. For this part of the investigation, we chose to examine hydrated proteoglycan aggregates. Proteoglycans are an essential component of the organic matrix of cartilage, and play a primary role in the retention and maintenance of extracellular water. To avoid any artifacts due to the introduction of exogeneous materials, and examine the proteoglycan aggregates in their hydrated, natural configuration, we made contact x-ray images of isolated proteoglycan aggregates in water

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

    Energy Technology Data Exchange (ETDEWEB)

    Chagas, L.H.; De Carvalho, G.S.G. [Universidade Federal de Juiz de Fora, Departamento de Química, Grupo de Físico-Química de Sólidos e Interfaces, 36036-330 Juiz de Fora, MG (Brazil); San Gil, R.A.S. [Universidade Federal do Rio de Janeiro, Instituto de Química, 21949-900 Rio de Janeiro, RJ (Brazil); Chiaro, S.S.X. [PETROBRAS-CENPES, 21941-915 Rio de Janeiro, RJ (Brazil); Leitão, A.A. [Universidade Federal de Juiz de Fora, Departamento de Química, Grupo de Físico-Química de Sólidos e Interfaces, 36036-330 Juiz de Fora, MG (Brazil); Diniz, R., E-mail: renata.diniz@ufjf.edu.br [Universidade Federal de Juiz de Fora, Departamento de Química, Grupo de Físico-Química de Sólidos e Interfaces, 36036-330 Juiz de Fora, MG (Brazil)

    2014-01-01

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

  16. X-ray absorption near edge structure (XANES) study of some hydroxamic mixed ligand copper complexes

    International Nuclear Information System (INIS)

    Mishra, A; Parsai, N; Shrivastava, B D; Soni, N

    2012-01-01

    With the advent of modern bright synchrotron radiation sources, X-ray absorption spectra has emerged as a powerful technique for local structure determination, which can be applied to any type of material. The X-ray absorption measurements of four hydroxamic mixed ligand copper complexes have been performed at the recently developed BL-8 Dispersive EXAFS beamline at 2.5 GeV Indus-2 synchrotron at RRCAT, Indore, India. The X-ray absorption near edge structure (XANES) data obtained has been processed using data analysis program Athena. The energies of the K absorption edge, chemical shifts, edge-widths, shifts of the principal absorption maximum in the complexes have been determined. The values of the chemical shift suggest that copper is in oxidation state +2 in all of the complexes. The chemical shift data has been utilized to estimate effective nuclear charge on copper atom. The order of the chemical shifts has been correlated to the relative ionic character of the bonding in these complexes.

  17. Si K EDGE STRUCTURE AND VARIABILITY IN GALACTIC X-RAY BINARIES

    Energy Technology Data Exchange (ETDEWEB)

    Schulz, Norbert S.; Corrales, Lia; Canizares, Claude R. [Kavli Institute for Astrophysics and Space Research, Massachusetts Institute of Technology, Cambridge, MA 02139 (United States)

    2016-08-10

    We survey the Si K edge structure in various absorbed Galactic low-mass X-ray binaries (LMXBs) to study states of silicon in the inter- and circum-stellar medium. The bulk of these LMXBs lie toward the Galactic bulge region and all have column densities above 10{sup 22} cm{sup −2}. The observations were performed using the Chandra High Energy Transmission Grating Spectrometer. The Si K edge in all sources appears at an energy value of 1844 ± 0.001 eV. The edge exhibits significant substructure that can be described by a near edge absorption feature at 1849 ± 0.002 eV and a far edge absorption feature at 1865 ± 0.002 eV. Both of these absorption features appear variable with equivalent widths up to several mÅ. We can describe the edge structure using several components: multiple edge functions, near edge absorption excesses from silicates in dust form, signatures from X-ray scattering optical depths, and a variable warm absorber from ionized atomic silicon. The measured optical depths of the edges indicate much higher values than expected from atomic silicon cross sections and interstellar medium abundances, and they appear consistent with predictions from silicate X-ray absorption and scattering. A comparison with models also indicates a preference for larger dust grain sizes. In many cases, we identify Si xiii resonance absorption and determine ionization parameters between log ξ = 1.8 and 2.8 and turbulent velocities between 300 and 1000 km s{sup −1}. This places the warm absorber in close vicinity of the X-ray binaries. In some data, we observe a weak edge at 1.840 keV, potentially from a lesser contribution of neutral atomic silicon.

  18. Stacking Faults and Polytypes for Layered Double Hydroxides: What Can We Learn from Simulated and Experimental X-ray Powder Diffraction Data?

    Science.gov (United States)

    Sławiński, Wojciech A; Sjåstad, Anja Olafsen; Fjellvåg, Helmer

    2016-12-19

    Layered double hydroxides (LDH) are a broad group of widely studied materials. The layered character of those materials and their high flexibility for accommodating different metals and anions make them technologically interesting. The general formula for the LDH compound is [M 1-x II M x III (OH) 2 ][A n- ] x/n ·mH 2 O, where M II is a divalent metal cation which can be substituted by M III trivalent cation, and A n- is a charge compensating anion located between positively charged layers. In this paper we present a comprehensive study on possible structural disorder in LDH. We show how X-ray powder diffraction (XRPD) can be used to reveal important features of the LDH crystal structure such as stacking faults, random interlayer shifts, anion-molecule orientation, crystal water content, distribution of interlayer distances, and also LDH slab thickness. All calculations were performed using the Discus package, which gives a better flexibility in defining stacking fault sequences, simulating and refining XRPD patterns, relative to DIFFaX, DIFFaX+, and FAULTS. Finally, we show how the modeling can be applied to two LDH samples: Ni 0.67 Cr 0.33 (OH) 2 (CO 3 ) 0.16 ·mH 2 O (3D structure) and Mg 0.67 Al 0.33 (OH) 2 (NO 3 ) 0.33 (2D layered structure).

  19. Phase and Chemical Composition Analysis on Neolithic Painted Ceramics Sherds Using Synchrotron Radiation X-Ray Powder Diffraction (SRXPD)

    International Nuclear Information System (INIS)

    Constantinescu, B.

    2003-01-01

    Full text: Synchrotron Radiation X-ray Powder Diffraction studies were performed at the wiggler beamline 1711 of MAX II Synchrotron accelerator from Lund, Sweden, in the frame of EU FPV Access to Large Scale Facilities programme. Diffraction data were collected using radiation of wavelength 1.36 A, which was detected by a Brucker system with a Smart 1000 CCD detector. The main goal of our studies was to distinguish different clays and mineral pigments of various Neolithic pottery-producing centres on Romanian territory in relation with possible inter-regional trade route connections. As main results we can mention: - identification of black pigment composition from Cucuteni (Northern Moldavia), Ariusd (South-Eastern Transylvania) and Cris-Starcevo (Oltenia) type pottery (VI - IV Millennia B. Chr.) as a combination of jacobsite, bixbyite (Manganese oxides), magnetite and goethite (Iron oxides) originary from North Moldova mineral deposits of Iacobeni (150 km up on the river Bistritza from analyzed Cucuteni archaeological sites), and as a combination of pyrolusite, magnetite and hematite for Cris-Starcevo samples, probably from local clay (enriched in Mn-Fe oxides) - identification of white pigment composition as calcite (CaCO3) for Cris- Starcevo culture sites from Central Transylvania (from the local abundant chalk deposits) and as calcium silicates mixed with illite (K, H2))Al2[(H2O, OH)2]AlSi3O10 for Cucuteni culture sites - identification of read-brown pigment composition as various mixtures of hematite - goethite - magnetite, all of local provenance - identification of all examined sherds as having local provenance for the clay The main conclusion is that during Neolithic period, the pottery workshops, largely extended on Romanian territory, used local clays but traded black mineral pigments across the Carpathian mountains (Cucuteni and Ariusd areas are separated by these mountains by easily crossed by passes along small rivers)

  20. Energetic electron processes fluorescence effects for structured nanoparticles X-ray analysis and nuclear medicine applications

    Energy Technology Data Exchange (ETDEWEB)

    Taborda, A.; Desbrée, A. [Institut de Radioprotection et de Sûreté Nucléaire (IRSN), PRP-HOM/SDI/LEDI, BP-17, 31, Avenue de la Division Leclerc, 92262 Fontenay-aux-Roses (France); Carvalho, A. [IEQUALTECS, Lda, Rua Dr. Francisco Sá Carneiro, 36, 2500-065 S. Gregório CLD (Portugal); Chaves, P.C. [C" 2TN, Campus Tecnológico e Nuclear, Instituto Superior Técnico, Universidade de Lisboa, EN10 km 139.7, 2685-066 Bobadela LRS (Portugal); Reis, M.A., E-mail: mareis@ctn.tecnico.ulisboa.pt [IEQUALTECS, Lda, Rua Dr. Francisco Sá Carneiro, 36, 2500-065 S. Gregório CLD (Portugal); C" 2TN, Campus Tecnológico e Nuclear, Instituto Superior Técnico, Universidade de Lisboa, EN10 km 139.7, 2685-066 Bobadela LRS (Portugal)

    2016-08-15

    Superparamagnetic iron oxide (SPIO) nanoparticles are widely used as contrast agents for nuclear magnetic resonance imaging (MRI), and can be modified for improved imaging or to become tissue-specific or even protein-specific. The knowledge of their detailed elemental composition characterisation and potential use in nuclear medicine applications, is, therefore, an important issue. X-ray fluorescence techniques such as particle induced X-ray emission (PIXE) or X-ray fluorescence spectrometry (XRF), can be used for elemental characterisation even in problematic situations where very little sample volume is available. Still, the fluorescence coefficient of Fe is such that, during the decay of the inner-shell ionised atomic structure, keV Auger electrons are produced in excess to X-rays. Since cross-sections for ionisation induced by keV electrons, for low atomic number atoms, are of the order of 10{sup 3} barn, care should be taken to account for possible fluorescence effects caused by Auger electrons, which may lead to the wrong quantification of elements having atomic number lower than the atomic number of Fe. Furthermore, the same electron processes will occur in iron oxide nanoparticles containing {sup 57}Co, which may be used for nuclear medicine therapy purposes. In the present work, simple approximation algorithms are proposed for the quantitative description of radiative and non-radiative processes associated with Auger electrons cascades. The effects on analytical processes and nuclear medicine applications are quantified for the case of iron oxide nanoparticles, by calculating both electron fluorescence emissions and energy deposition on cell tissues where the nanoparticles may be embedded.

  1. Electronic structure and optical properties of CdS{sub x}Se{sub 1−x} solid solution nanostructures from X-ray absorption near edge structure, X-ray excited optical luminescence, and density functional theory investigations

    Energy Technology Data Exchange (ETDEWEB)

    Murphy, M. W. [DESY (Deutsches Elektronen-Synchrotron), FS-PEX, Notkestrasse 85, 22607 Hamburg (Germany); Yiu, Y. M., E-mail: yyiu@uwo.ca; Sham, T. K. [Department of Chemistry, University of Western Ontario, London, ON N6A5B7 (Canada); Ward, M. J. [Cornell High Energy Synchrotron Source (CHESS), Cornell University, Ithaca, NY 14853 (United States); Liu, L. [Institute of Functional Nano and Soft Materials (FUNSOM) and Soochow University-Western University Center for Synchrotron Radiation Research, Soochow University, Suzhou, Jiangsu, 215123 (China); Hu, Y. [Canadian Light Source, University of Saskatchewan, Saskatoon, SK S7N2V3 (Canada); Zapien, J. A. [Center Of Super-Diamond and Advanced Films (COSDAF) and Department of Physics and Materials Science, City University of Hong Kong, Hong Kong SAR (China); Liu, Yingkai [Institute of Physics and Electronic Information, Yunnan Normal University, Kunming, Yunnan, 650500 (China)

    2014-11-21

    The electronic structure and optical properties of a series of iso-electronic and iso-structural CdS{sub x}Se{sub 1−x} solid solution nanostructures have been investigated using X-ray absorption near edge structure, extended X-ray absorption fine structure, and X-ray excited optical luminescence at various absorption edges of Cd, S, and Se. It is found that the system exhibits compositions, with variable local structure in-between that of CdS and CdSe accompanied by tunable optical band gap between that of CdS and CdSe. Theoretical calculation using density functional theory has been carried out to elucidate the observations. It is also found that luminescence induced by X-ray excitation shows new optical channels not observed previously with laser excitation. The implications of these observations are discussed.

  2. Anomalous scattering, transport, and spatial distribution of X-ray fluorescence at the exit of polycapillary structures

    Energy Technology Data Exchange (ETDEWEB)

    Mazuritskiy, M. I., E-mail: mazurmik@gmail.com; Lerer, A. M.; Makhno, P. V. [Southern Federal University (Russian Federation)

    2016-12-15

    The angular distribution of the X-ray intensity at the exit of microchannel plates at grazing incidence of monochromatic radiation on the walls of microcapillaries has been investigated. The angles and energies of the primary radiation quanta at which the synchrotron beam excites X-ray fluorescence propagating inside polycapillary structures have been determined. The angular dependences of the intensity distribution of X-rays transmitted through the microcapillaries have been studied theoretically and experimentally for energies corresponding to the region of anomalous dispersion near the L{sub 2,3} absorption edges of silicon. The propagation of waves in hollow polycapillary waveguides, the excitation of X-ray fluorescence, and the X-ray diffraction at the exit of microchannel plates have been modeled mathematically. The mathematical model takes into account the presence of a transition layer on the microchannel surface.

  3. The effect of SNR structure on non-equilibrium X-ray spectra

    International Nuclear Information System (INIS)

    Hamilton, A.J.S.; Sarazin, C.L.

    1983-01-01

    A technique is presented for characterizing the ionization structure and consequent thermal X-ray emission of a SNR when non-equilibrium ionization effects are important. The technique allows different theoretical SNR models to be compared and contrasted rapidly in advance of detailed numerical computations. In particular it is shown that the spectrum of a Sedov remnant can probably be applied satisfactorily in a variety of SNR structures, including the reverse shock model advocated by Chevalier (1982) for Type I SN, the isothermal similarity solution of Solinger, Rappaport and Buff (1975), and various inhomogenous or 'messy' structures. (Auth.)

  4. Silicon Σ13(5 0 1) grain boundary interface structure determined by bicrystal Bragg rod X-ray scattering

    International Nuclear Information System (INIS)

    Howes, P.B.; Rhead, S.; Roy, M.; Nicklin, C.L.; Rawle, J.L.; Norris, C.A.

    2013-01-01

    The atomic structure of the silicon Σ13(5 0 1) symmetric tilt grain boundary interface has been determined using Bragg rod X-ray scattering. In contrast to conventional structural studies of grain boundary structure using transmission electron microscopy, this approach allows the non-destructive measurement of macroscopic samples. The interface was found to have a single structure that is fully fourfold coordinated. X-ray diffraction data were measured at Beamline I07 at the Diamond Light Source

  5. X-ray structure analyses of biological molecules and particles in Japan. A brief history and future prospect

    International Nuclear Information System (INIS)

    Nakasako, Masayoshi; Yamamoto, Masaki

    2015-01-01

    In Japan, X-ray structure analyses of molecules and particles from biology started in the 1970s. The structure analysis methods have been developed through the innovation of various techniques in advance, and have contributed for understanding the elementary and microscopic processes in life. Here we summarize briefly the history of X-ray structure analyses for structural biology in Japan and think about the prospect. (author)

  6. Providing x-rays

    International Nuclear Information System (INIS)

    Mallozzi, P.J.; Epstein, H.M.

    1985-01-01

    This invention provides an apparatus for providing x-rays to an object that may be in an ordinary environment such as air at approximately atmospheric pressure. The apparatus comprises: means (typically a laser beam) for directing energy onto a target to produce x-rays of a selected spectrum and intensity at the target; a fluid-tight enclosure around the target; means for maintaining the pressure in the first enclosure substantially below atmospheric pressure; a fluid-tight second enclosure adjoining the first enclosure, the common wall portion having an opening large enough to permit x-rays to pass through but small enough to allow the pressure reducing means to evacuate gas from the first enclosure at least as fast as it enters through the opening; the second enclosure filled with a gas that is highly transparent to x-rays; the wall of the second enclosure to which the x-rays travel having a portion that is highly transparent to x-rays (usually a beryllium or plastic foil), so that the object to which the x-rays are to be provided may be located outside the second enclosure and adjacent thereto and thus receive the x-rays substantially unimpeded by air or other intervening matter. The apparatus is particularly suited to obtaining EXAFS (extended x-ray fine structure spectroscopy) data on a material

  7. Phase transitions of Cu.sub.3+x./sub.Si observed by temperature-dependent x-ray powder diffraction

    Czech Academy of Sciences Publication Activity Database

    Correa, Cinthia Antunes; Poupon, Morgane; Kopeček, Jaromír; Král, Robert; Zemenová, Petra; Lecourt, J.; Barrier, N.; Brázda, Petr; Klementová, Mariana; Palatinus, Lukáš

    2017-01-01

    Roč. 91, Dec (2017), s. 129-139 ISSN 0966-9795 R&D Projects: GA ČR GC15-08842J Institutional support: RVO:68378271 Keywords : X-ray powder diffraction * differential scanning calorimetry * phase transitions * Cu3+xSi Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.) Impact factor: 3.140, year: 2016

  8. Small-angle x-ray scattering investigation of the solution structure of troponin C

    International Nuclear Information System (INIS)

    Hubbard, S.R.; Hodgson, K.O.; Doniach, S.

    1988-01-01

    X-ray crystallographic studies of troponin C have revealed a novel protein structure consisting of two globular domains, each containing two Ca 2+ -binding sites, connected via a nine-turn alpha-helix, three turns of which are fully exposed to solvent. Since the crystals were grown at pH approximately 5, it is of interest to determine whether this structure is applicable to the protein in solution under physiological conditions. We have used small-angle x-ray scattering to examine the solution structure of troponin C at pH 6.8 and the effect of Ca 2+ on the structure. The scattering data are consistent with an elongated structure in solution with a radius of gyration of approximately 23.0 A, which is quite comparable to that computed for the crystal structure. The experimental scattering profile and the scattering profile computed from the crystal structure coordinates do, however, exhibit differences at the 40-A level. A weak Ca 2+ -facilitated dimerization of troponin C was observed. The data rule out large Ca 2+ -induced structural changes, indicating rather that the molecule with Ca 2+ bound is only slightly more compact than the Ca 2+ -free molecule

  9. Structure of 3 at.% and 9 at.% Si-doped HfO{sub 2} from combined refinement of X-ray and neutron diffraction patterns

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, Lili [Department of Materials Science and Engineering, North Carolina State University, NC 27695 (United States); School of Information Science and Technology, Northwest University, Xi' an 710127 (China); Hou, Dong; Usher, Tedi-Marie; Iamsasri, Thanakorn; Fancher, Chris M.; Forrester, Jennifer S. [Department of Materials Science and Engineering, North Carolina State University, NC 27695 (United States); Nishida, Toshikazu [Department of Electrical and Computer Engineering, University of Florida, FL 32611 (United States); Moghaddam, Saeed [Department of Mechanical and Aerospace Engineering, University of Florida, FL 32611 (United States); Jones, Jacob L., E-mail: jacobjones@ncsu.edu [Department of Materials Science and Engineering, North Carolina State University, NC 27695 (United States)

    2015-10-15

    The crystal structure of 3 at.% and 9 at.% Si-doped HfO{sub 2} powder was determined through refinements using X-ray and neutron diffraction patterns. The lattice parameters, atomic positions, dopant occupancy, and the second phase fraction were determined with high precision using a combined full pattern fitting via the Rietveld method. The results show that both 3 at.% and 9 at.% Si-doped HfO{sub 2} powder exhibit the monoclinic crystal structure with P 1 2{sub 1}/c 1 space group. Through the combined refinement, the crystal structure parameters, especially for the positions and occupancies of the lighter atoms, were more precisely determined compared to independent X-ray diffraction refinement. Although the ionic radius of Si{sup 4+} is smaller than Hf{sup 4+}, with increasing Si occupancy, the unit cell volume slightly increases; possible mechanisms for this effect are discussed. Moreover, the refined results provide evidence of the existence of a non-equilibrium phase of Hf{sub x}Si{sub 1−x}O{sub 2}. The second phase (SiO{sub 2}) fraction is determined as 0.17 at.% for 3 at.% Si-doped HfO{sub 2} powders and 1.7 at.% for 9 at.% Si-doped HfO{sub 2} powders. - Highlights: • X-ray and neutron diffraction patterns were used to determine crystal structure. • Results from independent refinements and a combined refinement were compared. • Highly precise structural parameters were obtained by the combined refinement. • Structural data of 3 at.% and 9 at.% Si-doped HfO{sub 2} are provided. • The unit cell volume slightly increases with Si concentration from 3 to 9 at.%.

  10. Utility Of Stress-Texture Characteristics Of Structural Materials By X-Ray Technique

    Directory of Open Access Journals (Sweden)

    Bonarski J.T.

    2015-09-01

    Full Text Available The article presents the results of residual stress analysis in selected metal-metal joints manufactured by conventional welding and explosive merging. The X-ray diffraction technique applied for advanced stress-texture measurements and data processing revealed directions and values of the principal stresses and their configuration on the surface of the examined structural elements. The obtained stress topography of the joint intersections indicates a possible path of potential cracking formed during the exploitation process and thus it becomes a very useful tool in the diagnostics of structural elements.

  11. X-ray structural investigation into complexes of p-aminobenzoic acid and metals

    International Nuclear Information System (INIS)

    Amiraslanov, I.R.; Musaev, F.N.; Mamedov, Kh.S.

    1982-01-01

    X-ray structural investigation of p-aminobenzoatodiaqua-strontium Sr(H 2 NC 6 H 4 COO) 2 x2H 2 o' was carried out. Crystals were rhombic: a=6.86(1), b=13.39(2), c=18.58(2) A, V=1705 A, Z=4, space group P2 1 2 1 2 1 . The basis of the structure was formed by infinite along the axis a chains of strontium atom octavertices articulated with common oxygen vertices. Sr-O bond lengths were 2.46-2.74 A; the distance between strontium neighbour - ring atom 4.07(1) A. Bond angles were presented

  12. Structure of ordered polyelectrolyte films from atomic-force microscopy and X-ray reflectivity data

    International Nuclear Information System (INIS)

    Belyaev, V.V.; Tolstikhina, A.L.; Stepina, N.D.; Kayushina, R.L.

    1998-01-01

    The possible application of atomic-force microscopy and X-ray reflectometry methods to structural studies of polyelectrolyte films obtained due to alternating adsorption of oppositely charged polyanion [sodium polysterenesulfonate (PSS)] and polycation [poly(allylamine) hydrochloride (PAA)] layers on solid substrates has been considered. The atomic-force microscopy study has revealed the characteristic features of the surface topography of samples consisting of different numbers of polyelectrolyte layers deposited from solutions characterized by different ionic strength values. It is shown that the shape of the reflectivity curves obtained from thin polyelectrolyte films depends on their surface structure

  13. Structural studies of disordered materials using high-energy x-ray diffraction from ambient to extreme conditions

    Energy Technology Data Exchange (ETDEWEB)

    Kohara, Shinji [Japan Synchrotron Radiation Research Institute (SPring-8/JASRI), 1-1-1 Kouto, Sayo, Hyogo 679-5198 (Japan); Itou, Masayoshi [Japan Synchrotron Radiation Research Institute (SPring-8/JASRI), 1-1-1 Kouto, Sayo, Hyogo 679-5198 (Japan); Suzuya, Kentaro [Japan Atomic Energy Agency (J-PARC/JAEA), Tokai, Naka, Ibaraki 319-1195 (Japan); Inamura, Yasuhiro [Japan Atomic Energy Agency (J-PARC/JAEA), Tokai, Naka, Ibaraki 319-1195 (Japan); Sakurai, Yoshiharu [Japan Synchrotron Radiation Research Institute (SPring-8/JASRI), 1-1-1 Kouto, Sayo, Hyogo 679-5198 (Japan); Ohishi, Yasuo [Japan Synchrotron Radiation Research Institute (SPring-8/JASRI), 1-1-1 Kouto, Sayo, Hyogo 679-5198 (Japan); Takata, Masaki [Japan Synchrotron Radiation Research Institute (SPring-8/JASRI), 1-1-1 Kouto, Sayo, Hyogo 679-5198 (Japan)

    2007-12-19

    High-energy x-rays from a synchrotron radiation source allow us to obtain high-quality diffraction data for disordered materials from ambient to extreme conditions, which is necessary for revealing the detailed structures of glass, liquid and amorphous materials. We introduced high-energy x-ray diffraction beamlines and a dedicated diffractometer for glass, liquid and amorphous materials at SPring-8 and report the recent developments of ancillary equipment. Furthermore, the structures of liquid and amorphous materials determined from the high-energy x-ray diffraction data obtained at SPring-8 are discussed.

  14. Structural investigation of semi-conductor nanostructures by x-ray diffraction

    International Nuclear Information System (INIS)

    Stangl, J.

    2003-01-01

    Full text: Semiconductor nanostructures present a topic of increasing interest due to their potential for new device concepts, as well as from a scientific point of view. In structures with dimensions smaller than the DeBroglie wavelength of electrons or holes, quantum confinement effects determine the electronic and optical properties. For the understanding of such structures, their structural investigation, i.e., the determination of size, shape, chemical composition and strain state is mandatory. X-ray diffraction is a powerful technique for this purpose. In particular, the strain fields within nanostructures as well as in the surrounding matrix can be determined with high precision. Using synchrotron radiation sources, also the distribution of chemical composition within objects with typically several nm height and 10 to 100 nm width can be established. With x-ray diffraction, the non-destructive investigation of uncapped and buried structures is possible. The latter is important, as for applications buried structures are needed, and during capping the structural properties may change considerably. Here, we will focus on so-called self-assembled nanostructures, which form during the deposition of different semiconductors on top of each other. In contrast to structures etched after growth of planar layers, self organized islands or wires are virtually defect-free and hence promising for applications. Different scattering techniques sensitive to shape and/or composition and strain will be discussed. (author)

  15. The determination of the crystal structures of some uranium compounds by means of x-ray and neutron diffraction

    International Nuclear Information System (INIS)

    Adrian, H.W.W.

    1977-10-01

    In industrial uranium processing or reprocessing procedures, aqueous uranyl nitrate solutions are an intermediate product. The compounds, whose structures are reported, might prove valuable as alternative crystallization products to existing methods of extracting the uranium from solution. The compounds are obtained by the addition of hydroxylammonium to the uranyl nitrate solution and are of the general formula UO 2 (NH 2 0) 2 .xH 2 0, where x can take the values zero, two, three and four. In addition a compound of the formula UO 2 (NH 2 0) 2 .2(NH 2 CH).2H 2 0 was obtained. The UO 2 (NH 2 0) compound crystallized in a monoclinic crystal form. Crystals large enough for neutron diffraction were not obtained. The structure of the UO 2 (NH 2 0) 2 .2H 2 0 could not be solved because only disordered crystalline material was available. The structure of UO 2 (NH 2 0) 2 .3H 2 0 was solved by means of room- and low-temperature neutron diffraction. The unit cell is orthorhombic. The structure of α-UO 2 (NH 2 0) 2 .4H 2 0 was investigated by means of room-temperature x-ray and room- and low-temperature neutron diffraction. The unit cell is triclinic. This compound strongly resembles the trihydrate. The UO 2 (NH 2 0) 2 .2(NH 2 0H).2H 2 0 compound gave crystals large enough for single crystal x-ray but not neutron diffraction. The unit cell is orthorhombic. The characteristic powder patterns (indexed except for the dihydrate compound) of the above compounds are reported [af

  16. Poly[μ-(1-azaniumylethane-1,1-diyl)- bis(hydrogen phosphonato)sodium]: A powder X-ray diffraction study

    International Nuclear Information System (INIS)

    Rukiah, M.; Assaad, T.

    2015-01-01

    The title two-dimensional coordination polymer, [Na(C2H8NO6P2)]n, was characterized using powder X-ray diffraction data and its structure refined using the Rietveld method. The asymmetric unit contains one Na(+) cation and one (1-azaniumylethane-1,1-diyl)bis(hydrogen phosphonate) anion. The central Na(+) cation exhibits distorted octahedral coordination geometry involving two deprotonated O atoms, two hydroxy O atoms and two double-bonded O atoms of the bisphosphonate anion. Pairs of sodium-centred octahedra share edges and the pairs are in turn connected to each other by the biphosphonate anion to form a two-dimensional network parallel to the (001) plane. The polymeric layers are connected by strong O-H...O hydrogen bonding between the hydroxy group and one of the free O atoms of the bisphosphonate anion to generate a three-dimensional network. Further stabilization of the crystal structure is achived by N-H...O and O-H...O hydrogen bonding.(author)

  17. Electronic structure and X-ray spectroscopic properties of YbNi_2P_2

    International Nuclear Information System (INIS)

    Shcherba, I.D.; Bekenov, L.V.; Antonov, V.N.; Noga, H.; Uskokovic, D.; Zhak, O.; Kovalska, M.V.

    2016-01-01

    Highlights: • We present new experimental and theoretical data for YbNi_2P_2. • The presence of divalent and trivalent Yb ion found in YbNi_2P_2. • The calculation show good agreement with the experimental measurements. - Abstract: X-ray absorption spectrum at the Yb L_3 edge and X-ray emission spectra of Ni and P at the K and L_2_,_3 edges have been studied experimentally and theoretically in the mixed valent compound YbNi_2P_2 with ThCr_2Si_2 type crystal structure. The electronic structure of YbNi_2P_2 is investigated using the fully relativistic Dirac linear muffin-tin orbital (LMTO) band-structure method. The effect of the spin–orbit (SO) interaction and Coulomb repulsion U on the electronic structure of YbNi_2P_2 is examined in the frame of the LSDA + SO + U method. The core-hole effect in the final states as well as the effect of the electric quadrupole E_2 transitions have been investigated. A good agreement between the theory and the experiment was found. Both the trivalent and the divalent Yb ions in YbNi_2P_2 are reflected in the experimentally measured Yb L_3 X-ray absorption spectrum simultaneously. We found that the best agreement between the experimental spectrum and sum of the theoretically calculated Yb"2"+ and Yb"3"+ spectra is achieved with 73% ytterbium ions in 2+ state and 27% ions in 3+ state.

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

    International Nuclear Information System (INIS)

    Tanner, B.K.

    1983-01-01

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

  19. Serial data acquisition for the X-ray plasma diagnostics with selected GEM detector structures

    International Nuclear Information System (INIS)

    Czarski, T.; Chernyshova, M.; Pozniak, K.T.; Kasprowicz, G.; Zabolotny, W.; Kolasinski, P.; Krawczyk, R.; Wojenski, A.; Zienkiewicz, P.

    2015-01-01

    The measurement system based on GEM—Gas Electron Multiplier detector is developed for X-ray diagnostics of magnetic confinement tokamak plasmas. The paper is focused on the measurement subject and describes the fundamental data processing to obtain reliable characteristics (histograms) useful for physicists. The required data processing have two steps: 1—processing in the time domain, i.e. events selections for bunches of coinciding clusters, 2—processing in the planar space domain, i.e. cluster identification for the given detector structure. So, it is the software part of the project between the electronic hardware and physics applications. The whole project is original and it was developed by the paper authors. The previous version based on 1-D GEM detector was applied for the high-resolution X-ray crystal spectrometer KX1 in the JET tokamak. The current version considers 2-D detector structures for the new data acquisition system. The fast and accurate mode of data acquisition implemented in the hardware in real time can be applied for the dynamic plasma diagnostics. Several detector structures with single-pixel sensors and multi-pixel (directional) sensors are considered for two-dimensional X-ray imaging. Final data processing is presented by histograms for selected range of position, time interval and cluster charge values. Exemplary radiation source properties are measured by the basic cumulative characteristics: the cluster position distribution and cluster charge value distribution corresponding to the energy spectra. A shorter version of this contribution is due to be published in PoS at: 1 st EPS conference on Plasma Diagnostics

  20. Small angle neutron and x-ray scattering studies of self-assembled nano structured materials

    International Nuclear Information System (INIS)

    Choi, Sung Min

    2009-01-01

    Full text: Small angle neutron and x-ray scattering are very powerful techniques to investigate nano structured materials. In this presentation, examples of nano structured materials investigated by neutron and x-ray scattering will be presented. Part I: The unique anisotropic physical properties of columnar discotic liquid crystals (DLCs) have attracted considerable interest for their potential applications as electronic devices. For many practical applications, however, it is crucial to obtain uniaxially oriented and highly ordered columnar superstructures of DLC molecules covering macroscopic area. Here, we present a simple and straight-forward approach to fabricate uniaxially oriented and highly ordered columnar superstructures of cobalt octa(n-decylthio) porphyrazine (CoS 1 0), a discotic supra-molecule, in bulk and on substrates [1] over a macroscopic length scale, utilizing an applied magnetic field and the interaction of CoS 1 0 with an OTS-functionalized substrate. The details of the oriented and ordered columnar nano-structures are investigated by SANS and GISAXS. Part II: Self-assembly of one-dimensional (1D) nanoparticles with metallic or semiconducting properties into highly ordered superstructures using various interactions has been of great interest as a route towards materials with new functionalities. Here, we report a new phase diagram of negatively charged 1D nanoparticle (cROD) and cationic liposome (CL) complexes in water which exhibit three different highly ordered phases [2]. Small angle neutron and x-ray scattering measurements show that the cROD-CL complexes exhibit three different highly ordered phases, intercalated lamellar, doubly intercalated lamellar and centered rectangular phases, depending on particle curvature and electrostatic interactions. The new phase diagram can be used to understand and design new highly ordered self-assemblies of 1D nanoparticles in soft matter which provide new functionalities. (author)

  1. Serial data acquisition for the X-ray plasma diagnostics with selected GEM detector structures

    Science.gov (United States)

    Czarski, T.; Chernyshova, M.; Pozniak, K. T.; Kasprowicz, G.; Zabolotny, W.; Kolasinski, P.; Krawczyk, R.; Wojenski, A.; Zienkiewicz, P.

    2015-10-01

    The measurement system based on GEM—Gas Electron Multiplier detector is developed for X-ray diagnostics of magnetic confinement tokamak plasmas. The paper is focused on the measurement subject and describes the fundamental data processing to obtain reliable characteristics (histograms) useful for physicists. The required data processing have two steps: 1—processing in the time domain, i.e. events selections for bunches of coinciding clusters, 2—processing in the planar space domain, i.e. cluster identification for the given detector structure. So, it is the software part of the project between the electronic hardware and physics applications. The whole project is original and it was developed by the paper authors. The previous version based on 1-D GEM detector was applied for the high-resolution X-ray crystal spectrometer KX1 in the JET tokamak. The current version considers 2-D detector structures for the new data acquisition system. The fast and accurate mode of data acquisition implemented in the hardware in real time can be applied for the dynamic plasma diagnostics. Several detector structures with single-pixel sensors and multi-pixel (directional) sensors are considered for two-dimensional X-ray imaging. Final data processing is presented by histograms for selected range of position, time interval and cluster charge values. Exemplary radiation source properties are measured by the basic cumulative characteristics: the cluster position distribution and cluster charge value distribution corresponding to the energy spectra. A shorter version of this contribution is due to be published in PoS at: 1st EPS conference on Plasma Diagnostics

  2. Electronic structure of polycrystalline cadmium dichloride studied by X-ray spectroscopies and ab initio calculations

    International Nuclear Information System (INIS)

    Demchenko, I.N.; Chernyshova, M.; Stolte, W.C.; Speaks, D.T.; Derkachova, A.

    2012-01-01

    The electronic structure of cadmium dichloride has been studied by X-ray absorption near edge structure (XANES) and, for the first time, by resonant inelastic X-ray scattering (RIXS) at the Cl K edge. Good agreement was obtained between the non-resonant X-ray emission (XES) along with XANES experimental spectra and the calculated Cl 3p local partial density of states (DOS). The calculations were performed using the full-potential linearized-augmented-plane-wave with the local orbitals (FP-(L)APW l o) method utilized in the WIEN2k code. It was shown that the position of the RIXS band in CdCl 2 follows a linear dispersion according to the Raman–Stokes law if the excitation energy is tuned below the absorption threshold. The situation changes for core excitation above the photoabsorption threshold where the dispersion relation is split into two branches. The position of the resonant contribution does not depend on the excitation energy, while the excitonic sideband follows the Raman–Stoke law. Combined XANES and RIXS measurements compared to calculated band structure allowed us to determine the direct band gap of CdCl 2 to be at 5.7 ± 0.05 eV. -- Highlights: ► XANES at the K edge of Cl and related emission KV band interpreted within the ab initio DFT formalism. ► Two dominant contributions observed in RIXS data: the resonant and the excitonic ones. ► The dispersion relation below the absorption threshold follows Raman–Stokes law. ► Dispersion above the threshold splits into two qualitatively different relations. ► Overlapping of XAS spectrum with RIXS one makes possible to estimate direct band gap value to be 5.7 eV.

  3. Structural analysis of radiation damage in zircon and thorite: An X-ray absorption spectroscopic study

    International Nuclear Information System (INIS)

    Farges, F.; Calas, G.

    1991-01-01

    Metamictization effects have been investigated in zircon, thorite, uranothorite, and thorogummite using X-ray absorption spectroscopy at Zr-K, Th-L III edges. Extended X-ray absorption fine structure (EXAFS) spectra of metamict samples are characterized by a major contribution due to the O nearest neighbors with some contributions from next-nearest neighbors (Si and Zr in zircon, Si in thorite). In zircon, Zr-O distances decrease by ∼0.1 angstrom while the coordination number of Zr decreases from 8 to 7. In contrast, the eightfold coordination of Th in crystalline thorite is preserved in metamict thorite, Si second neighbors around Zr or Th are generally observed in metamict samples with distances close to those measured in crystalline phases. No other contribution to EXAFS is observed in thorite, but Zr-Zr distances are observed in zircon. They decrease by ca. 0.3 Angstrom as a function of zircon metamictization. Metamictization processes are characterized by a loss of medium range order. There is no evidence for decomposition into crystalline oxides. The structural interpretation of EXAFS data must take into account the creation of O vacancies arising from a displacement or tilting of the SiO 4 tetrahedra during metamictization of zircon-like structures. If the cation can take a lower coordination number (as in the case of Zr), a coordination change allows the local structure to be partly maintained during metamictization. If not, as for Th, the local structure is rapidly destroyed

  4. Analysis of inner structure changes of concretes exposed to high temperatures using micro X-ray computed tomography

    OpenAIRE

    Sitek, L. (Libor); Bodnárová, L.; Souček, K. (Kamil); Staš, L. (Lubomír); Gurková, L. (Lucie)

    2015-01-01

    The X-ray Computed Tomography (X-ray CT) repr esents a progressive non-destructive metho d of analysing the inner structure of materials. The method was used for monitoring changes in inner structure of concrete samples of different composition before and after their exposure to various thermal loads. Eight types of concrete samples were prepared which differed by cement and aggregate types. We intentionally used such composition of concrete mixtures which increased their resist...

  5. Characterization of the electronic structure of C50Cl10 by means of soft x-ray spectroscopies

    International Nuclear Information System (INIS)

    Brena, Barbara; Luo Yi

    2005-01-01

    The electronic structure of the last synthesized fullerene molecule, the C 50 Cl 10 , has been characterized by theoretical simulation of x-ray photoelectron spectroscopy, ultraviolet photoelectron spectroscopy, and near-edge x-ray-absorption fine structure. All the calculations were performed at the gradient-corrected and hybrid density-functional theory levels. The combination of these techniques provides detailed information about the valence band and the unoccupied molecular orbitals, as well as about the carbon core orbitals

  6. The atomic structure of Fe100-xCux nanoalloys: X-ray absorption analysis

    International Nuclear Information System (INIS)

    Kravtsova, A.N.; Yalovega, G.E.; Soldatov, A.V.; Yan, W.S.; Wei, S.Q.

    2009-01-01

    The local atomic structure of Fe 100-x Cu x nanoalloys (x = 0, 10, 20, 40, 60, 70, 80 and 100%) has been investigated by X-ray absorption near edge structure (XANES) analysis. Local environment around copper and iron atoms in Fe 100-x Cu x has been studied by comparing the experimental XANES with corresponding theoretical spectra calculated for several structural models. It has been established that the most probable structure of the Fe 100-x Cu x nanoalloys for a low concentration of copper (x = 10-20%) is a homogenous bcc structure, for a high copper concentration (x = 60-80%)-a homogenous fcc structure, while at an intermediate copper concentration (about 40%) the nanoalloys have an inhomogeneous structure consisting of clusters of fcc solid solution (90%) and of clusters of bcc solid solution (10%)

  7. Robust, high-throughput solution structural analyses by small angle X-ray scattering (SAXS)

    Energy Technology Data Exchange (ETDEWEB)

    Hura, Greg L.; Menon, Angeli L.; Hammel, Michal; Rambo, Robert P.; Poole II, Farris L.; Tsutakawa, Susan E.; Jenney Jr, Francis E.; Classen, Scott; Frankel, Kenneth A.; Hopkins, Robert C.; Yang, Sungjae; Scott, Joseph W.; Dillard, Bret D.; Adams, Michael W. W.; Tainer, John A.

    2009-07-20

    We present an efficient pipeline enabling high-throughput analysis of protein structure in solution with small angle X-ray scattering (SAXS). Our SAXS pipeline combines automated sample handling of microliter volumes, temperature and anaerobic control, rapid data collection and data analysis, and couples structural analysis with automated archiving. We subjected 50 representative proteins, mostly from Pyrococcus furiosus, to this pipeline and found that 30 were multimeric structures in solution. SAXS analysis allowed us to distinguish aggregated and unfolded proteins, define global structural parameters and oligomeric states for most samples, identify shapes and similar structures for 25 unknown structures, and determine envelopes for 41 proteins. We believe that high-throughput SAXS is an enabling technology that may change the way that structural genomics research is done.

  8. Raphide crystal structure in agave tequilana determined by x-ray originating from synchrotron radiation

    International Nuclear Information System (INIS)

    Tadokoro, Makoto; Ozawa, Yoshiki; Mitsumi, Minoru; Toriumi, Kohshiro; Ogura, Tetsuya

    2005-01-01

    The first single crystal structure of small natural raphides in an agave plant is completely determined using an intense X-ray originating from a synchrotron radiation. The SEM image shows that the tip of the crystal is approximately hundreds of nanometer in width sharply grow to stick to the tissue of herbivorous vermin. Furthermore, the crystal develops cracks that propagate at an inclination of approximately 45deg towards the direction of crystal growth such that the crystal easily splits into small pieces in the tissue. (author)

  9. Diffuse x-ray scattering study of interfacial structure of self-assembled conjugated polymers

    International Nuclear Information System (INIS)

    Wang Jun; Park, Y.J.; Lee, K.-B.; Hong, H.; Davidov, D.

    2002-01-01

    The interfacial structures of self-assembled heterostructures through alternate deposition of conjugated and nonconjugated polymers were studied by x-ray reflectivity and nonspecular scattering. We found that the interfacial width including the effects of both interdiffusion and interfacial roughness (correlated) was mainly contributed by the latter one. The self-assembled deposition induced very small interdiffusion between layers. The lateral correlation length ξ parallel grew as a function of deposition time (or film thickness) described by a power law ξ parallel ∝t β/H and was also observed from the off-specular scattering

  10. Malnutrition and myelin structure: an X-ray scattering study of rat sciatic and optic nerves

    International Nuclear Information System (INIS)

    Vargas, V.; Vargas, R.; Marquez, G.; Vonasek, E.; Mateu, L.; Luzzati, V.; Borges, J.

    2000-01-01

    Taking advantage of the fast and accurate X-ray scattering techniques recently developed in our laboratory, we tackled the study of the structural alterations induced in myelin by malnutrition. Our work was performed on sciatic and optic nerves dissected from rats fed with either a normal or a low-protein caloric diet, as a function of age (from birth to 60 days). By way of electrophysiological controls we also measured (on the sciatic nerves) the height and velocity of the compound action potential. Malnutrition was found to decrease the amount of myelin and to impair the packing order of the membranes in the sheaths. (orig.)

  11. A method for assessing the structural shielding in diagnostic x-ray facilities

    International Nuclear Information System (INIS)

    Almeida, F.; Martinez de la Fuente, O.; Perez, C.

    1992-01-01

    The design of each X-Ray medical facility involves, in order to guarantee the optimun levels of Radiologic safety for everybody who could be exposed during the performance of the examinations the need of assessing the required shieldings for the room which contains the emiter tubes. In such sense, this paper gives a number of criteria to calculate the structural requirements for the diverse configurations which exist in Health Centres using the method proposed by NCRP in its Report 49 as a reference. (author)

  12. Extended X-ray absorption fine structure (EXAFS) studies of supported catalysts

    International Nuclear Information System (INIS)

    Joyner, R.W.

    1979-01-01

    Since the rebirth of interest in extended X-ray absorption fine structure there have been several studies of systems of catalytic interest. This note is a preliminary account of an investigation of supported platinum catalysts and NiO/Al 2 O 3 catalysts. Experiments were performed on pressed disc samples at the DESY synchrotron, Hamburg, using the EXAFS spectrometer. The synchrotron operated at 7 GeV energy with a circulating current of approximately 4 mA; spectrum accumulation time was typically 45 minutes. (author)

  13. Near-Edge X-ray Absorption Fine Structure Spectroscopy of Diamondoid Thiol Monolayers on Gold

    Energy Technology Data Exchange (ETDEWEB)

    Willey, T M; Fabbri, J; Lee, J I; Schreiner, P; Fokin, A A; Tkachenko, B A; Fokina, N A; Dahl, J; Carlson, B; Vance, A L; Yang, W; Terminello, L J; van Buuren, T; Melosh, N

    2007-11-27

    Diamondoids, hydrocarbon molecules with cubic-diamond-cage structures, have unique properties with potential value for nanotechnology. The availability and ability to selectively functionalize this special class of nanodiamond materials opens new possibilities for surface-modification, for high-efficiency field emitters in molecular electronics, as seed crystals for diamond growth, or as robust mechanical coatings. The properties of self-assembled monolayers (SAMs) of diamondoids are thus of fundamental interest for a variety of emerging applications. This paper presents the effects of thiol substitution position and polymantane order on diamondoid SAMs on gold using near-edge X-ray absorption fine structure spectroscopy (NEXAFS) and X-ray photoelectron spectroscopy (XPS). A framework to determine both molecular tilt and twist through NEXAFS is presented and reveals highly ordered diamondoid SAMs, with the molecular orientation controlled by the thiol location. C 1s and S 2p binding energies are lower in adamantane thiol than alkane thiols on gold by 0.67 {+-} 0.05 eV and 0.16 {+-} 0.04 eV respectively. These binding energies vary with diamondoid monolayer structure and thiol substitution position, consistent with different amounts of steric strain and electronic interaction with the substrate. This work demonstrates control over the assembly, in particular the orientational and electronic structure, providing a flexible design of surface properties with this exciting new class of diamond clusters.

  14. Non-destructive X-ray examination of weft knitted wire structures

    Science.gov (United States)

    Obermann, M.; Ellouz, M.; Aumann, S.; Martens, Y.; Bartelt, P.; Klöcker, M.; Kordisch, T.; Ehrmann, A.; Weber, M. O.

    2016-07-01

    Conductive yarns or wires are often integrated in smart textiles to enable data or energy transmission. In woven fabrics, these conductive parts are fixed at defined positions and thus protected from external loads. Knitted fabrics, however, have relatively loose structures, resulting in higher impacts of possible mechanical forces on the individual yarns. Hence, metallic wires with smaller diameters in particular are prone to break when integrated in knitted fabrics. In a recent project, wires of various materials including copper, silver and nickel with diameters varying between 0.05 mm and 0.23 mm were knitted in combination with textile yarns. Hand flat knitting machines of appropriate gauges were used to produce different structures. On these samples, non-destructive examinations, using an industrial X-ray system Seifert x|cube (225 kV) equipped with a minifocus X-ray tube, were carried out, directly after knitting as well as after different mechanical treatments (tensile, burst, and washing tests). In this way, structural changes of the stitch geometry could be visualized before failure. In this paper, the loop geometries in the knitted fabrics are depicted depending on knitted structures, wire properties and the applied mechanical load. Consequently, it is shown which metallic wires and yarns are most suitable to be integrated into knitted smart textiles.

  15. Soft x-ray absorption spectroscopy on Co doped ZnO: structural distortions and electronic structure

    International Nuclear Information System (INIS)

    Kowalik, I A; Guziewicz, E; Godlewski, M; Arvanitis, D

    2016-01-01

    We present soft x-ray absorption spectra from a series of Co doped ZnO films. We discuss systematic variations of the Co L-edge white line intensity and multiplet features for this series of samples. We document sizeable differences in the electronic state of the Co ionic cores, as well as in the local environment of the host lattice atoms, characterised by means of x-ray absorption spectra at the O K-edge and Zn L-edges. Model calculations allow to correlate the observed effects to small structural distortions of the ZnO lattice. (paper)

  16. Quantitation of polymorphic impurity in entecavir polymorphic mixtures using powder X-ray diffractometry and Raman spectroscopy.

    Science.gov (United States)

    Kang, Yanlei; Shao, Zhanying; Wang, Qiang; Hu, Xiurong; Yu, Dongdong

    2018-05-26

    Entecavir was used for the treatment of chronic hepatitis B through inhibiting hepatitis B virus. The anhydrous form of entecavir (ENT-A) often appeared as impurity polymorph in the manufacturing process of entecavir monohydrate (ENT-H) such as granulation, drying and compression. Since different crystal forms might affect drug bioavailability and therapeutic effect, it was vital to control the ENT-A content of the drug product. The work aimed to develop useful methods to assess ENT-A weight percentage in ENT-H. Powder X-ray diffractometry (PXRD) and Raman spectrometric methods were applied. Binary mixtures with different ratios of pure ENT-H and pure ENT-A were scanned using PXRD and Raman to obtain spectra. Then peak heights and peak areas versus weight percentage were used to construct calibration curves. The best linear regression analysis data for PXRD and Raman method were found to be R 2  = 0.9923 and R 2  = 0.9953, in the weight ratio range of 2.1-20.2% w/w% of ENT-A in binary mixtures. Limit of detection (LOD) of ENT-A was 0.38% and limit of quantitation (LOQ) was 1.15% for PXRD method. LOD and LOQ for Raman method were 0.48% and 1.16%. The results showed that PXRD and Raman methods: both were precise and accurate, and could be used for measurement of ENT-A content in the selected weight percentage range. Partial least squares (PLS) algorithm with four data pre-processing methods: including multiplicative scatter correlation (MSC), standard normal variate (SNV), first and second derivatives were applied and evaluated using prediction errors. The best performance of PLS was R 2  = 0.9958 with RMSEC (0.44%) and RMSEP (0.65%). Multivariate analysis for Raman spectra showed similar good results with univariate analysis, and would be an advantageous method when there were overlapped peaks in the spectra. In summary, the proposed PXRD and Raman method could be developed for the quality control of ENT-H. And Raman was a more promising method in

  17. The aquatic hyphomycete Heliscus lugdunensis protects its hyphae tip cells from cadmium: A micro X-ray fluorescence and X-ray absorption near edge structure spectroscopy study

    Science.gov (United States)

    Isaure, Marie-Pierre; Leyh, Benjamin; Salomé, Murielle; Krauss, Gerd-Joachim; Schaumlöffel, Dirk; Dobritzsch, Dirk

    2017-11-01

    Aquatic fungi can be used to evaluate the functioning of natural ecosystems. Heliscus lugdunensis is an early colonizer of allochthone leafs. Since this aquatic hyphomycete is able to develop in metal contaminated habitats and tolerates cadmium, it appears to be a good candidate to investigate adaptation to metal pollution. This study aimed at examining the sequestration of Cd in the hyphae of H. lugdunensis, and particularly the role of the tip cells. For that, H. lugdunensis growth was evaluated under various Cd concentrations, and a combination of synchrotron micro X-ray fluorescence and X-ray absorption near edge structure spectroscopy was carried out to determine the compartments of Cd accumulation and the Cd chemical species, respectively. Results showed that the hyphal tip cells were depleted in Cd, and that the metal was stored in older cells. Cd was mainly associated with sulfur ligands and to a lesser extent bound to phosphates and carboxyl/hydroxyl groups from cell wall and/or organic acids. Finally, the aquatic fungus was able to maintain the tip cell as a functional system, thus allowing the colonization of contaminated environments.

  18. 5 K extended X-ray absorption fine structure and 40 K 10-s resolved extended X-ray absorption fine structure studies of photolyzed carboxymyoglobin

    International Nuclear Information System (INIS)

    Teng, T.Y.; Huang, H.W.; Olah, G.A.

    1987-01-01

    A previous extended X-ray absorption fine structure (EXAFS) study of photolyzed carboxymyoglobin (MbCO) has provoked much discussion on the heme structure of the photoproduct (Mb*CO). The EXAFS interpretation that the Fe-Co distance increases by no more than 0.05 A following photodissociation has been regarded as inconsistent with optical, infrared, and magnetic susceptibility studies. The present experiment was performed with well-characterized dry film samples in which MbCO molecules were embedded in a poly(vinyl alcohol) matrix. The sample had a high protein concentration (12 mM) to yield adequate EXAFS signals but was very thin (40 μm) so that complete photolysis could be easily achieved by a single flash from a xenon lamp. Although the electronic state of Mb*CO resembles that of deoxymyoglobin (deoxy-Mb), direct comparison of EXAFS spectra indicates that structurally Mb*CO is much closer to MbCO than to deoxy-Mb. Our EXAFS analysis shows that photolysis of MbCO at 5 K leads to a stable intermediate state in which CO has moved away from iron by a distance of 0.27-0.45 A, but the 5-coordinate heme structure is strained in a form similar to that of MbCO; the resolution of the CO position depends on the structure parameters of MbCO which we use as a reference for the analysis of Mb*CO. At 40 K, from 1 to 10 s after photolysis, 42% of the photoproduct has relaxed to the ground state, and the EXAFS spectrum of the remaining photoproduct is indistinguishable from that of the 5 K photoproduct

  19. Magnetic and electronic properties of RNiO{sub 3} (R = Pr, Nd, Eu, Ho and Y) perovskites studied by resonant soft x-ray magnetic powder diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Bodenthin, Y; Staub, U; Piamonteze, C; Garcia-Fernandez, M [Swiss Light Source, Paul Scherrer Institut, CH-5232 Villigen PSI (Switzerland); Martinez-Lope, M J; Alonso, J A, E-mail: urs.staub@psi.ch [Instituto de Ciencia de Materiales de Madrid, CSIC, Cantoblanco, E-28049 Madrid (Spain)

    2011-01-26

    Soft x-ray resonant magnetic powder diffraction of the (1/2 0 1/2) reflection at the Ni L{sub 2,3} edges is used to study the magnetic and electronic properties of a series of RNiO{sub 3} materials (with R = Pr, Nd, Eu, Ho and Y) below the metal-insulator transition. The polarization and energy dependence of the reflection gives further support for a non-collinear magnetic structure and charge disproportionation in the whole RNiO{sub 3} series. Only small changes in the spectra of the magnetic (1/2 0 1/2) reflection and in the absorption spectra could be detected. The results are discussed with comparison to charge transfer multiplet calculations. Our results emphasize that the lighter and heavier RNiO{sub 3} compounds are very similar from the point of view of their local electronic and magnetic state despite the strong change of the metal-to-insulator transition temperature.

  20. Analysis of a nanocrystalline polymer dispersion of ebselen using solid-state NMR, Raman microscopy, and powder X-ray diffraction.

    Science.gov (United States)

    Vogt, Frederick G; Williams, Glenn R

    2012-07-01

    Nanocrystalline drug-polymer dispersions are of significant interest in pharmaceutical delivery. The purpose of this work is to demonstrate the applicability of methods based on two-dimensional (2D) and multinuclear solid-state NMR (SSNMR) to a novel nanocrystalline pharmaceutical dispersion of ebselen with polyvinylpyrrolidone-vinyl acetate (PVP-VA), after initial characterization with other techniques. A nanocrystalline dispersion of ebselen with PVP-VA was prepared and characterized by powder X-ray diffraction (PXRD), confocal Raman microscopy and mapping, and differential scanning calorimetry (DSC), and then subjected to detailed 1D and 2D SSNMR analysis involving ¹H, ¹³C, and ⁷⁷Se isotopes and ¹H spin diffusion. PXRD was used to show that dispersion contains nanocrystalline ebselen in the 35-60 nm size range. Confocal Raman microscopy and spectral mapping were able to detect regions where short-range interactions may occur between ebselen and PVP-VA. Spin diffusion effects were analyzed using 2D SSNMR experiments and are able to directly detect interactions between ebselen and the surrounding PVP-VA. The methods used here, particularly the 2D SSNMR methods based on spin diffusion, provided detailed structural information about a nanocrystalline polymer dispersion of ebselen, and should be useful in other studies of these types of materials.

  1. Solid state structural investigations of the bis(chalcone) compound with single crystal X-ray crystallography, DFT, gamma-ray spectroscopy and chemical spectroscopy methods

    Science.gov (United States)

    Yakalı, Gül; Biçer, Abdullah; Eke, Canel; Cin, Günseli Turgut

    2018-04-01

    A bis(chalcone), (2E,6E)-2,6-bis((E)-3phenylallidene)cyclohexanone, was characterized by 1H NMR, 13C NMR, FTIR, UV-Vis spectroscopy, gamma-ray spectroscopy and single crystal X- ray structural analysis. The optimized molecular structure of the compound is calculated using DFT/B3LYP with 6-31G (d,p) level. The calculated geometrical parameters are in good agreement with the experimental data obtained from our reported X-ray structure. The powder and single crystal compounds were gama-irradiated using clinical electron linear accelerator and 60Co gamma-ray source, respectively. Spectral studies (1H NMR, 13C NMR, FTIR and UV-Vis) of powder chalcone compound were also investigated before and after irradiation. Depending on the irradiation notable changes were observed in spectral features powder sample. Single crystal X-ray diffraction investigation shows that both unirradiated and irradiated single crystal samples crystallizes in a orthorhombic crystal system in the centrosymmetric space group Pbcn and exhibits an C-H..O intramolecular and intermolecular hydrogen bonds. The crystal packing is stabilised by strong intermolecular bifurcate C-H..O hydrogen bonds and π…π stacking interactions. The asymmetric unit of the title compound contains one-half of a molecule. The other half of the molecule is generated with (1-x,y,-3/2-z) symmetry operator. The molecule is almost planar due to having π conjugated system of chalcones. However, irradiated single crystal compound showed significant changes lattice parameters, crystal volume and density. According to results of gamma-ray spectroscopy, radioactive elements of powder compound which are 123Sb(n,g),124Sb,57Fe(g,p),56Mn, 55Mn(g,n), and 54Mn were determined using photoactivation analysis. However, the most intensive gamma-ray energy signals are 124Sb.

  2. CheShift-2 resolves a local inconsistency between two X-ray crystal structures

    International Nuclear Information System (INIS)

    Vila, Jorge A.; Sue, Shih-Che; Fraser, James S.; Scheraga, Harold A.; Dyson, H. Jane

    2012-01-01

    Since chemical shifts provide important and relatively accessible information about protein structure in solution, a Web server, CheShift-2, was developed for structure interrogation, based on a quantum mechanics database of 13 C α chemical shifts. We report the application of CheShift-2 to a local inconsistency between two X-ray crystal structures (PDB IDs 1IKN and 1NFI) of the complex between the p65/p50 heterodimer of NFκB and its inhibitor IκBα. The availability of NMR resonance assignments that included the region of the inconsistency provided an opportunity for independent validation of the CheShift-2 server. Application of the server showed that the 13 C α chemical shifts measured for the Gly270-Pro281 sequence close to the C-terminus of IκBα were unequivocally consistent with the backbone structure modeled in the 1IKN structure, and were inconsistent with the 1NFI structure. Previous NOE measurements had demonstrated that the position of a tryptophan ring in the region immediately N-terminal in this region was not consistent with either structure. Subsequent recalculation of the local structure in this region, based on the electron density of the deposited structure factors for 1IKN, confirmed that the local backbone structure was best modeled by 1IKN, but that the rotamer of Trp258 is consistent with the 1NFI structure, including the presence of a hydrogen bond between the ring NεH of Trp258 and the backbone carbonyl group of Gln278. The consensus between all of these measures suggests that the CheShift-2 server operates well under circumstances in which backbone chemical shifts are available but where local plasticity may render X-ray structural data ambiguous.

  3. Particle-scale structure in frozen colloidal suspensions from small-angle x-ray scattering

    KAUST Repository

    Spannuth, Melissa; Mochrie, S. G. J.; Peppin, S. S. L.; Wettlaufer, J. S.

    2011-01-01

    During directional solidification of the solvent in a colloidal suspension, the colloidal particles segregate from the growing solid, forming high-particle-density regions with structure on a hierarchy of length scales ranging from that of the particle-scale packing to the large-scale spacing between these regions. Previous work has concentrated mostly on the medium- to large-length scale structure, as it is the most accessible and thought to be more technologically relevant. However, the packing of the colloids at the particle scale is an important component not only in theoretical descriptions of the segregation process, but also to the utility of freeze-cast materials for new applications. Here we present the results of experiments in which we investigated this structure across a wide range of length scales using a combination of small-angle x-ray scattering and direct optical imaging. As expected, during freezing the particles were concentrated into regions between ice dendrites forming a microscopic pattern of high- and low-particle-density regions. X-ray scattering indicates that the particles in the high-density regions were so closely packed as to be touching. However, the arrangement of the particles does not conform to that predicted by standard interparticle pair potentials, suggesting that the particle packing induced by freezing differs from that formed during equilibrium densification processes. © 2011 American Physical Society.

  4. Structure in defocused beams of x-ray mirrors: causes and possible solutions

    Science.gov (United States)

    Sutter, John P.; Alcock, Simon G.; Rust, Fiona; Wang, Hongchang; Sawhney, Kawal

    2014-09-01

    Grazing incidence mirrors are now a standard optic for focusing X-ray beams. Both bimorph and mechanically bendable mirrors are widely used at Diamond Light Source because they permit a wide choice of focal lengths. They can also be deliberately set out of focus to enlarge the X-ray beam, and indeed many beamline teams now wish to generate uniform beam spots of variable size. However, progress has been slowed by the appearance of fine structure in these defocused beams. Measurements showing the relationship between the medium-frequency polishing error and this structure over a variety of beam sizes will be presented. A theoretical model for the simulations of defocused beams from general mirrors will then be developed. Not only the figure error and its first derivative the slope error, but also the second derivative, the curvature error, must be considered. In conclusion, possible ways to reduce the defocused beam structure by varying the actuators' configuration and settings will be discussed.

  5. Particle-scale structure in frozen colloidal suspensions from small-angle x-ray scattering

    KAUST Repository

    Spannuth, Melissa

    2011-02-01

    During directional solidification of the solvent in a colloidal suspension, the colloidal particles segregate from the growing solid, forming high-particle-density regions with structure on a hierarchy of length scales ranging from that of the particle-scale packing to the large-scale spacing between these regions. Previous work has concentrated mostly on the medium- to large-length scale structure, as it is the most accessible and thought to be more technologically relevant. However, the packing of the colloids at the particle scale is an important component not only in theoretical descriptions of the segregation process, but also to the utility of freeze-cast materials for new applications. Here we present the results of experiments in which we investigated this structure across a wide range of length scales using a combination of small-angle x-ray scattering and direct optical imaging. As expected, during freezing the particles were concentrated into regions between ice dendrites forming a microscopic pattern of high- and low-particle-density regions. X-ray scattering indicates that the particles in the high-density regions were so closely packed as to be touching. However, the arrangement of the particles does not conform to that predicted by standard interparticle pair potentials, suggesting that the particle packing induced by freezing differs from that formed during equilibrium densification processes. © 2011 American Physical Society.

  6. Characterization of the Electronic Structure of Silicon Nanoparticles Using X-ray Absorption and Emission

    Energy Technology Data Exchange (ETDEWEB)

    Vaverka, April Susan Montoya [Univ.of California, Davis, CA (United States)

    2008-01-01

    Resolving open questions regarding transport in nanostructures can have a huge impact on a broad range of future technologies such as light harvesting for energy. Silicon has potential to be used in many of these applications. Understanding how the band edges of nanostructures move as a function of size, surface termination and assembly is of fundamental importance in understanding the transport properties of these materials. In this thesis work I have investigated the change in the electronic structure of silicon nanoparticle assemblies as the surface termination is changed. Nanoparticles are synthesized using a thermal evaporation technique and sizes are determined using atomic force microscopy (AFM). By passivating the particles with molecules containing alcohol groups we are able to modify the size dependent band edge shifts. Both the valence and conduction bands are measured using synchrotron based x-ray absorption spectroscopy (XAS) and soft x-ray fluorescence (SXF) techniques. Particles synthesized via recrystallization of amorphous silicon/SiO2 multilayers of thicknesses below 10 nm are also investigated using the synchrotron techniques. These samples also show quantum confinement effects but the electronic structure is different from those synthesized via evaporation methods. The total bandgap is determined for all samples measured. The origins of these differences in the electronic structures are discussed.

  7. Time-Resolved Soft X-ray Diffraction Reveals Transient Structural Distortions of Ternary Liquid Crystals

    Directory of Open Access Journals (Sweden)

    Klaus Mann

    2009-11-01

    Full Text Available Home-based soft X-ray time-resolved scattering experiments with nanosecond time resolution (10 ns and nanometer spatial resolution were carried out at a table top soft X-ray plasma source (2.2–5.2 nm. The investigated system was the lyotropic liquid crystal C16E7/paraffin/glycerol/formamide/IR 5. Usually, major changes in physical, chemical, and/or optical properties of the sample occur as a result of structural changes and shrinking morphology. Here, these effects occur as a consequence of the energy absorption in the sample upon optical laser excitation in the IR regime. The liquid crystal shows changes in the structural response within few hundred nanoseconds showing a time decay of 182 ns. A decrease of the Bragg peak diffracted intensity of 30% and a coherent macroscopic movement of the Bragg reflection are found as a response to the optical pump. The Bragg reflection movement is established to be isotropic and diffusion controlled (1 μs. Structural processes are analyzed in the Patterson analysis framework of the time-varying diffraction peaks revealing that the inter-lamellar distance increases by 2.7 Å resulting in an elongation of the coherently expanding lamella crystallite. The present studies emphasize the possibility of applying TR-SXRD techniques for studying the mechanical dynamics of nanosystems.

  8. X-ray crystallography

    Science.gov (United States)

    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.

  9. Determination of line profiles on nano-structured surfaces using EUV and x-ray scattering

    Science.gov (United States)

    Soltwisch, Victor; Wernecke, Jan; Haase, Anton; Probst, Jürgen; Schoengen, Max; Krumrey, Michael; Scholze, Frank; Pomplun, Jan; Burger, Sven

    2014-09-01

    Non-imaging techniques like X-ray scattering are supposed to play an important role in the further development of CD metrology for the semiconductor industry. Grazing Incidence Small Angle X-ray Scattering (GISAXS) provides directly assessable information on structure roughness and long-range periodic perturbations. The disadvantage of the method is the large footprint of the X-ray beam on the sample due to the extremely shallow angle of incidence. This can be overcome by using wavelengths in the extreme ultraviolet (EUV) spectral range, EUV small angle scattering (EUVSAS), which allows for much steeper angles of incidence but preserves the range of momentum transfer that can be observed. Generally, the potentially higher momentum transfer at shorter wavelengths is counterbalanced by decreasing diffraction efficiency. This results in a practical limit of about 10 nm pitch for which it is possible to observe at least the +/- 1st diffraction orders with reasonable efficiency. At the Physikalisch-Technische Bundesanstalt (PTB), the available photon energy range extends from 50 eV up to 10 keV at two adjacent beamlines. PTB commissioned a new versatile Ellipso-Scatterometer which is capable of measuring 6" square substrates in a clean, hydrocarbon-free environment with full flexibility regarding the direction of the incident light polarization. The reconstruction of line profiles using a geometrical model with six free parameters, based on a finite element method (FEM) Maxwell solver and a particle swarm based least-squares optimization yielded consistent results for EUV-SAS and GISAXS. In this contribution we present scatterometry data for line gratings and consistent reconstruction results of the line geometry for EUV-SAS and GISAXS.

  10. Interests and instrument: a micro-history of object Wh.3469 (X-ray powder diffraction camera, ca. 1940).

    Science.gov (United States)

    Scheffler, Robin Wolfe

    2009-12-01

    This paper presents a micro-history of an object in the collection of the Whipple Museum of the History of Science (accession no. Wh.3469), with an emphasis on how Wh.3469 reflects a hybrid of two different interwar British X-ray crystallographic communities, namely those based in WL Bragg's physics laboratory at the Victoria University of Manchester and the Crystallographic Laboratory at the University of Cambridge. It explores connections between Wh.3469's final design and construction and the different interests each community had in X-ray crystallography.

  11. Protein NMR Structures Refined with Rosetta Have Higher Accuracy Relative to Corresponding X-ray Crystal Structures

    Science.gov (United States)

    2014-01-01

    We have found that refinement of protein NMR structures using Rosetta with experimental NMR restraints yields more accurate protein NMR structures than those that have been deposited in the PDB using standard refinement protocols. Using 40 pairs of NMR and X-ray crystal structures determined by the Northeast Structural Genomics Consortium, for proteins ranging in size from 5–22 kDa, restrained Rosetta refined structures fit better to the raw experimental data, are in better agreement with their X-ray counterparts, and have better phasing power compared to conventionally determined NMR structures. For 37 proteins for which NMR ensembles were available and which had similar structures in solution and in the crystal, all of the restrained Rosetta refined NMR structures were sufficiently accurate to be used for solving the corresponding X-ray crystal structures by molecular replacement. The protocol for restrained refinement of protein NMR structures was also compared with restrained CS-Rosetta calculations. For proteins smaller than 10 kDa, restrained CS-Rosetta, starting from extended conformations, provides slightly more accurate structures, while for proteins in the size range of 10–25 kDa the less CPU intensive restrained Rosetta refinement protocols provided equally or more accurate structures. The restrained Rosetta protocols described here can improve the accuracy of protein NMR structures and should find broad and general for studies of protein structure and function. PMID:24392845

  12. X-ray absorption spectroscopy investigation of structurally modified lithium niobate crystals

    Energy Technology Data Exchange (ETDEWEB)

    Vitova, Tonya

    2008-02-15

    The type and concentration of impurity centers in different valence states are crucial for tuning the photorefractive properties of doped Lithium Niobate (LN) crystals. X-ray Absorption Spectroscopy (XAS) is an appropriate tool for studying the local structure of impurity centers. XAS combined with absorption in UV/VIS/IR and High Resolution X-ray Emission Spectroscopy (HRXES) provide information about the valence state of the dopant ions in as-grown, reduced or oxidized doped LN crystals. Cu (Cu{sup 1+} and Cu{sup 2+}) and Fe (Fe{sup 2+} and Fe{sup 3+}) atoms are found in two different valence states, whereas there are indications for a third Mn valency, in addition to Mn{sup 2+} and Mn{sup 3+} in manganese-doped LN crystals. One of the charge compensation mechanisms during reduction of copper- doped LN crystals is outgassing of oxygen atoms. Cu ions in the reduced crystals have at least two different site symmetries: twofold (Cu{sup 1+}) and sixfold (Cu{sup 2+}) coordinated by O atoms. Fe and Mn atoms are coordinated by six O atoms. Cu and Fe ions are found to occupy only Li sites, whereas Mn ions are also incorporated into Li and Nb sites. The refractive index change in LN crystals irradiated with {sup 3}He{sup 2+} ions is caused by structurally disordered centers, where Nb atoms are displaced from normal crystallographic sites and Li or/and O vacancies are present. (orig.)

  13. X-ray absorption spectroscopy investigation of structurally modified lithium niobate crystals

    International Nuclear Information System (INIS)

    Vitova, Tonya

    2008-02-01

    The type and concentration of impurity centers in different valence states are crucial for tuning the photorefractive properties of doped Lithium Niobate (LN) crystals. X-ray Absorption Spectroscopy (XAS) is an appropriate tool for studying the local structure of impurity centers. XAS combined with absorption in UV/VIS/IR and High Resolution X-ray Emission Spectroscopy (HRXES) provide information about the valence state of the dopant ions in as-grown, reduced or oxidized doped LN crystals. Cu (Cu 1+ and Cu 2+ ) and Fe (Fe 2+ and Fe 3+ ) atoms are found in two different valence states, whereas there are indications for a third Mn valency, in addition to Mn 2+ and Mn 3+ in manganese-doped LN crystals. One of the charge compensation mechanisms during reduction of copper- doped LN crystals is outgassing of oxygen atoms. Cu ions in the reduced crystals have at least two different site symmetries: twofold (Cu 1+ ) and sixfold (Cu 2+ ) coordinated by O atoms. Fe and Mn atoms are coordinated by six O atoms. Cu and Fe ions are found to occupy only Li sites, whereas Mn ions are also incorporated into Li and Nb sites. The refractive index change in LN crystals irradiated with 3 He 2+ ions is caused by structurally disordered centers, where Nb atoms are displaced from normal crystallographic sites and Li or/and O vacancies are present. (orig.)

  14. Evaluation of osteoporotic bone structure through synchrotron radiation X-ray microfluorescence images

    Energy Technology Data Exchange (ETDEWEB)

    Lima, I. [Nuclear Engineering Program/COPPE/UFRJ, P.O. Box 68509, Av. Horacio Macedo 2030, Sala I-133, Cidade Universitaria, 21941-914 Rio de Janeiro, RJ (Brazil)], E-mail: inaya@lin.ufrj.br; Anjos, M.J. [Nuclear Engineering Program/COPPE/UFRJ, P.O. Box 68509, Av. Horacio Macedo 2030, Sala I-133, Cidade Universitaria, 21941-914 Rio de Janeiro, RJ (Brazil); Physics Institute, UERJ (Brazil); Farias, M.L.F. [University Hospital, UFRJ (Brazil); Pantaleao, T.U.; Correa da Costa, V.M. [Biophysics Institute, UFRJ (Brazil); Lopes, R.T. [Nuclear Engineering Program/COPPE/UFRJ, P.O. Box 68509, Av. Horacio Macedo 2030, Sala I-133, Cidade Universitaria, 21941-914 Rio de Janeiro, RJ (Brazil)

    2008-12-15

    The abnormal accumulation or deficiency of trace elements may theoretically impair the formation of bone and contribute to osteoporosis. In this context, the knowledge of major and trace elements is very important in order to clarify many issues regarding diseases of the bone, such as osteoporosis, that remain unresolved. Several kinds of imaging techniques can be useful to access morphology and the minerals present in osteoporotic bones. In this work, synchrotron radiation X-ray microfluorescence was used as an X-ray imaging technique to investigate bone structures. Therefore, this research aims to improve the knowledge about some aspects of bone quality. The measurements were carried out at the Brazilian Synchrotron Laboratory Light Laboratory, in Brazil. A white beam with an energy range of 4-23 keV, a 45 deg./45 deg. geometry and a capillary optics were used. It was demonstrated that bone quality can and must be evaluated not only by considering the architecture of bones but also by taking into account the concentration and the distribution of minerals. Our results showed that the elemental distributions in bone zones on a micron scale were very helpful to understand functions in those structures.

  15. Electronic structure of human hemoglobin: ultrasoft X-ray emission study

    International Nuclear Information System (INIS)

    Soldatov, A.V.; Kravtsova, A.N.; Fedorovich, E.N.; Kurmaev, E.Z.; Moewes, A.

    2004-01-01

    Full text: The iron L 2,3 and carbon, nitrogen and oxygen Kα X-ray emission spectra (XES) of human hemoglobin have been recorded at the soft X-ray spectroscopy endstation on Undulator Beam line 8.0 at Advanced Light Source (ALS) located at the Lawrence Berkeley National Laboratory. The theoretical calculations of Fe L 3 -XES have been performed using ab initio code FEFF8.2. The calculations have been carried out for the structure of hemoglobin presented in PDB (entry 3HHB) as well as for the molecule with symmetrical heme plane. It was found that the Fe L 3 emission spectrum calculated for the ideal molecule agrees slightly better with the experiment as compared with those calculated for the real molecule. Thus, one can use the structure of the ideal molecule for theoretical Fe L 3 -XES simulations. The theoretical analysis has shown that the fist peak of experimental Fe L 3 - emission spectrum is enhanced by the nearest nitrogen atoms lying in heme plane around the central iron atom. The theoretical C K- and N K-XES spectra of hemoglobin have been calculated. A good agreement between theoretical and experimental spectra has been obtained. The distribution of the partial electronic densities of states in the valence and conduction bands of hemoglobin has been determined

  16. Conceptual Design of Dielectric Accelerating Structures for Intense Neutron and Monochromatic X-ray Sources

    Science.gov (United States)

    Blanovsky, Anatoly

    2004-12-01

    Bright compact photon sources, which utilize electron beam interaction with periodic structures, may benefit a broad range of medical, industrial and scientific applications. A class of dielectric-loaded periodic structures for hard and soft X-ray production has been proposed that would provide a high accelerating gradient when excited by an external RF and/or primary electron beam. Target-distributed accelerators (TDA), in which an additional electric field compensates for lost beam energy in internal targets, have been shown to provide the necessary means to drive a high flux subcritical reactor (HFSR) for nuclear waste transmutation. The TDA may also be suitable for positron and nuclear isomer production, X-ray lithography and monochromatic computer tomography. One of the early assumptions of the theory of dielectric wake-field acceleration was that, in electrodynamics, the vector potential was proportional to the scalar potential. The analysis takes into consideration a wide range of TDA design aspects including the wave model of observed phenomena, a layered compound separated by a Van der Waals gap and a compact energy source based on fission electric cells (FEC) with a multistage collector. The FEC is a high-voltage power source that directly converts the kinetic energy of the fission fragments into electrical potential of about 2MV.

  17. Heterophase fluctuation of omega phase and X-ray diffuse scattering from dual phase structure

    International Nuclear Information System (INIS)

    Farjami, Susan; Kubo, Hiroshi

    2003-01-01

    Heterophase fluctuation of athermal omega embryos has been analyzed by assuming a dual phase structure of omega embryos composed of omega and bcc matrix phase. The two-dimensional modulation of dual phase was suggested from the quantitative estimation of coherent free energy of omega embryos using microscopic theory of elasticity and the Landau anharmonic theory for phase transformation. The X-ray diffraction theory was developed in connection to the formation of omega embryos having the dual phase structure. The offset of the diffuse peak position from the ideal omega point in the X-ray diffraction pattern is attributed to the dual phase (incommensurate phase) of omega embryos. It was also shown that the ellipsoidal shape of the diffuse intensity tailing toward the fundamental spot of the matrix phase is originated from the equilibrium shape of the omega embryo. The quantitative estimation of elastic energy modulus (EEM) in the disordered bcc matrix and in the ordered bcc matrix indicates a difference in the deviation amount of the minimum point k(q m ) from the ideal omega point k(q ω ) and a difference in the elliptical shape of embryos

  18. Morphological and structural characterization of PHBV/organoclay nanocomposites by small angle X-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Carli, Larissa N., E-mail: lncarli@ucs.br [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 9500, Porto Alegre, 91501-970, RS (Brazil); Centro de Ciencias Exatas e Tecnologia, Universidade de Caxias do Sul, Rua Francisco Getulio Vargas, 1130, Caxias do Sul, 95070-560, RS (Brazil); Bianchi, Otavio, E-mail: obianchi@ucs.br [Centro de Ciencias Exatas e Tecnologia, Universidade de Caxias do Sul, Rua Francisco Getulio Vargas, 1130, Caxias do Sul, 95070-560, RS (Brazil); Machado, Giovanna, E-mail: giovannamachado@uol.com.br [Centro de Tecnologias Estrategicas do Nordeste, Av. Prof. Luiz Freire, 01, Cidade Universitaria, Recife, 50740-540, PE (Brazil); Programa de Pos-Graduacao de Materiais, Universidade Federal de Pernambuco, Av. Prof. Moraes Rego, 1235, Recife, 50670-901, PE (Brazil); Crespo, Janaina S., E-mail: jscrespo@ucs.br [Centro de Ciencias Exatas e Tecnologia, Universidade de Caxias do Sul, Rua Francisco Getulio Vargas, 1130, Caxias do Sul, 95070-560, RS (Brazil); Mauler, Raquel S., E-mail: raquel.mauler@ufrgs.br [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 9500, Porto Alegre, 91501-970, RS (Brazil)

    2013-03-01

    In this work, the morphological and structural behaviors of poly(hydroxybutyrate-co-hydroxyvalerate) (PHBV) nanocomposites were investigated using small angle X-ray scattering (SAXS), wide angle X-ray diffraction (WAXD) and transmission electron microscopy (TEM). The nanocomposites with 1, 3 and 5 wt.% of organically modified montmorillonite Cloisite Registered-Sign 30B (OMMT) were prepared by melt processing in a twin screw extruder using two different processing conditions (low and high shear intensity). The lamellar long period of the polymer was lower for the nanocomposites, with high polydispersity values. However, the crystalline thickness increased with the clay content and was independent of the processing conditions. This behavior resulted in a high linear crystallinity of the nanocomposites with 3 and 5 wt.% OMMT. The disruption factor ({beta}) was in agreement with the WAXD and TEM findings, indicating a good dispersion of the nanoparticles in the PHBV matrix with 3 wt.% of OMMT during the high shear intensity of melt processing. Highlights: Black-Right-Pointing-Pointer SAXS was used for morphological and crystalline studies of PHBV/OMMT nanocomposites. Black-Right-Pointing-Pointer The crystalline structure was influenced by the presence of clay. Black-Right-Pointing-Pointer The degree of clay dispersion in a polymer matrix was quantified. Black-Right-Pointing-Pointer The morphology comprised exfoliated particles, nanoscale and microscale clusters. Black-Right-Pointing-Pointer The results obtained by SAXS agreed well with TEM and WAXD results.

  19. Layered structure analysis of multilayers by X-ray reflectometry using the Cu-Kβ line

    International Nuclear Information System (INIS)

    Usami, Katsuhisa; Ueda, Kazuhiro; Hirano, Tatsumi; Hoshiya, Hiroyuki; Narishige, Shinji.

    1997-01-01

    The suitability of X-ray reflectometry using the Cu-K β line for layered structure analysis of NiFe/Cu/NiFe/Ta layered films was studied. Structural parameters such as film thickness, density, and interface width can be determined more accurately than by Cu-K α1 X-ray reflectometry, owing to the abnormal dispersion effect. The standard deviations in determination of film thicknesses were within ±0.3% for NiFe and Ta films and ±0.03 nm for 2 nm Cu film. Those for the densities and interface widths were within ±2% and ±0.04 nm for all films, respectively. Analysis of some layered films regarding the change in Cu film thickness showed that in all these samples the density of the films most closely reflected the density of bulk material, and the interface width between the upper NiFe and Cu films increased with increasing Cu film thickness. (author)

  20. Local layer structure of smectic liquid crystals by X-ray micro-diffraction

    CERN Document Server

    Takanishi, Y

    2003-01-01

    The local layer structure of smectic liquid crystal has been measured using time-resolved synchrotron X-ray micro-diffraction. Typical layer disorders observed in surface stabilized (anti-) ferroelectric liquid crystals, i.e. a stripe texture, a needed-like defect and a zigzag defect, are directly analyzed. The detailed analysis slows that the surface anchoring force due to the interaction between the liquid crystal molecule and the alignment thin film plays an important role to realize both the static and dynamic local layer structures. The layer structure of the circular domain observed in the liquid crystal of bent-shaped molecules found to depend on the applied electric field though the optical micrograph shows little difference. The frustrated, double and single layer structures of the bent-shaped molecule liquid crystal are determined depending on the terminal alkyl chain length. (author)

  1. X-ray free electron laser and its application to 3-dimensional imaging of non-crystalline nano-structure

    International Nuclear Information System (INIS)

    Ishikawa, Tetsuya

    2007-01-01

    The Laser in the X-ray region has been anticipated to be realized as a light source to probe the nano-world. Free electron lasers using high energy electron accelerators have been promising the candidates. The finding of the principle of Self-Amplified Spontaneous Emission (SASE) resolved the technological difficulties accompanying the X-ray free electron laser, and the construction of large scale SASE facilities started in western countries. In Japan the construction of an SASE facility started in 2006 to be completed in 2010 at the site of the large synchrotron radiation facility, SPring-8 positioned as a 'critical technology of national importance' by the Japanese government. The principle of the X-ray free electron laser is explained and the outline of the Japanese facility construction plan is presented. Also the application of the X-ray laser to the imaging of non-crystalline nano-structure is introduced. (K.Yoshida)

  2. Microscopic bosonization of band structures: x-ray processes beyond the Fermi edge

    Science.gov (United States)

    Snyman, Izak; Florens, Serge

    2017-11-01

    Bosonization provides a powerful analytical framework to deal with one-dimensional strongly interacting fermion systems, which makes it a cornerstone in quantum many-body theory. However, this success comes at the expense of using effective infrared parameters, and restricting the description to low energy states near the Fermi level. We propose a radical extension of the bosonization technique that overcomes both limitations, allowing computations with microscopic lattice Hamiltonians, from the Fermi level down to the bottom of the band. The formalism rests on the simple idea of representating the fermion kinetic term in the energy domain, after which it can be expressed in terms of free bosonic degrees of freedom. As a result, one- and two-body fermionic scattering processes generate anharmonic boson-boson interactions, even in the forward channel. We show that up to moderate interaction strengths, these non-linearities can be treated analytically at all energy scales, using the x-ray emission problem as a showcase. In the strong interaction regime, we employ a systematic variational solution of the bosonic theory, and obtain results that agree quantitatively with an exact diagonalization of the original one-particle fermionic model. This provides a proof of the fully microscopic character of bosonization, on all energy scales, for an arbitrary band structure. Besides recovering the known x-ray edge singularity at the emission threshold, we find strong signatures of correlations even at emission frequencies beyond the band bottom.

  3. Tin( ii ) ketoacidoximates: synthesis, X-ray structures and processing to tin( ii ) oxide

    KAUST Repository

    Khanderi, Jayaprakash

    2015-10-21

    Tin(ii) ketoacidoximates of the type [HONCRCOO]Sn (R = Me 1, CHPh 2) and (MeONCMeCOO)Sn] NH·2HO 3 were synthesized by reacting pyruvate- and hydroxyl- or methoxylamine RONH (R = H, Me) with tin(ii) chloride dihydrate SnCl·2HO. The single crystal X-ray structure reveals that the geometry at the Sn atom is trigonal bipyramidal in 1, 2 and trigonal pyramidal in 3. Inter- or intramolecular hydrogen bonding is observed in 1-3. Thermogravimetric (TG) analysis shows that the decomposition of 1-3 to SnO occurs at ca. 160 °C. The evolved gas analysis during TG indicates complete loss of the oximato ligand in one step for 1 whereas a small organic residue is additionally removed at temperatures >400 °C for 2. Above 140 °C, [HONC(Me)COO]Sn (1) decomposes in air to spherical SnO particles of size 10-500 nm. Spin coating of 1 on Si or a glass substrate followed by heating at 200 °C results in a uniform film of SnO. The band gap of the produced SnO film and nanomaterial was determined by diffuse reflectance spectroscopy to be in the range of 3.0-3.3 eV. X-ray photoelectron spectroscopy indicates surface oxidation of the SnO film to SnO in ambient atmosphere.

  4. The complex ion structure of warm dense carbon measured by spectrally resolved x-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Kraus, D.; Barbrel, B.; Falcone, R. W. [Department of Physics, University of California, Berkeley, California 94720 (United States); Vorberger, J. [Max-Planck-Institut für Physik komplexer Systeme, Nöthnitzer Straße 38, 01187 Dresden (Germany); Helfrich, J.; Frydrych, S.; Ortner, A.; Otten, A.; Roth, F.; Schaumann, G.; Schumacher, D.; Siegenthaler, K.; Wagner, F.; Roth, M. [Institut für Kernphysik, Technische Universität Darmstadt, Schlossgartenstraße 9, 64289 Darmstadt (Germany); Gericke, D. O.; Wünsch, K. [Centre for Fusion, Space and Astrophysics, Department of Physics, University of Warwick, Coventry CV4 7AL (United Kingdom); Bachmann, B.; Döppner, T. [Lawrence Livermore National Laboratory, Livermore, California 94550 (United States); Bagnoud, V.; Blažević, A. [GSI Helmholtzzentrum für Schwerionenforschung GmbH, Planckstraße 1, 64291 Darmstadt (Germany); and others

    2015-05-15

    We present measurements of the complex ion structure of warm dense carbon close to the melting line at pressures around 100 GPa. High-pressure samples were created by laser-driven shock compression of graphite and probed by intense laser-generated x-ray sources with photon energies of 4.75 keV and 4.95 keV. High-efficiency crystal spectrometers allow for spectrally resolving the scattered radiation. Comparing the ratio of elastically and inelastically scattered radiation, we find evidence for a complex bonded liquid that is predicted by ab-initio quantum simulations showing the influence of chemical bonds under these conditions. Using graphite samples of different initial densities we demonstrate the capability of spectrally resolved x-ray scattering to monitor the carbon solid-liquid transition at relatively constant pressure of 150 GPa. Showing first single-pulse scattering spectra from cold graphite of unprecedented quality recorded at the Linac Coherent Light Source, we demonstrate the outstanding possibilities for future high-precision measurements at 4th Generation Light Sources.

  5. Finite difference method calculations of X-ray absorption fine structure for copper

    Energy Technology Data Exchange (ETDEWEB)

    Bourke, J.D. [School of Physics, University of Melbourne, Parkville, Vic 3010 (Australia); Chantler, C.T. [School of Physics, University of Melbourne, Parkville, Vic 3010 (Australia)]. E-mail: chantler@physics.unimelb.edu.au; Witte, C. [School of Physics, University of Melbourne, Parkville, Vic 3010 (Australia)

    2007-01-15

    The finite difference method is extended to calculate X-ray absorption fine structure (XAFS) for solid state copper. These extensions include the incorporation of a Monte Carlo frozen phonon technique to simulate the effect of thermal vibrations under a correlated Debye-Waller model, and the inclusion of broadening effects from inelastic processes. Spectra are obtained over an energy range in excess of 300 eV above the K absorption edge-more than twice the greatest energy range previously reported for a solid state calculation using this method. We find this method is highly sensitive to values of the photoelectron inelastic mean free path, allowing us to probe the accuracy of current models of this parameter, particularly at low energies. We therefore find that experimental data for the photoelectron inelastic mean free path can be obtained by this method. Our results compare favourably with high precision measurements of the X-ray mass attenuation coefficient for copper, reaching agreement to within 3%, and improving previous results using the finite difference method by an order of magnitude.

  6. Complex Structure of Galaxy Cluster Abell 1689: Evidence for a Merger from X-Ray Data?

    Energy Technology Data Exchange (ETDEWEB)

    Andersson, K

    2004-01-29

    Abell 1689 is a galaxy cluster at z = 0:183 where previous measurements of its mass using various techniques gave discrepant results. We present a new detailed measurement of the mass with the data based on X-ray observations with the European Photon Imaging Camera aboard the XMM-Newton Observatory, determined by using an unparameterized deprojection technique. Fitting the total mass profile to a Navarro-Frenk-White model yields halo concentration c = 7.2{sub -2.4}{sup +1.6} and r{sub 200} = 1.13 {+-} 0.21 h{sup -1} Mpc, corresponding to a mass which is less than half of what is found from gravitational lensing. Adding to the evidence of substructure from optical observations, X-ray analysis shows a highly asymmetric temperature profile and a non-uniform redshift distribution implying large scale relative motion of the gas. A lower than expected gas mass fraction f{sub gas} = 0.072 {+-} 0.008 (for a flat {Lambda}CDM cosmology) suggests a complex spatial and/or dynamical structure. We also find no signs of any additional absorbing component previously reported on the basis of the Chandra data, confirming the XMM low energy response using data from ROSAT.

  7. Extended x-ray absorption fine structure: Studies of zinc-neutralized sulfonated polystyrene ionomers

    International Nuclear Information System (INIS)

    Ding, Y.S.; Yarusso, D.J.; Pan, H.K.D.; Cooper, S.L.

    1984-01-01

    Extended x-ray absorption fine structure (EXAFS) measurements were performed on a series of zinc-neutralized sulfonated polystyrene ionomers and the local structure around the zinc atom was determined. An interference effect in the EXAFS signal between sulfur and oxygen atoms was found to be significant in these materials. A model for the local structure in the zinc-neutralized sulfonated polystyrene ionomers is proposed which suggests a highly ordered tetrahedral coordination of oxygen around the zinc atoms at a distance of 1.97 +- 0.02 A. In addition there are four sulfur atoms and four oxygen atoms at a distance of 3.15 +- 0.05 A. No zinc-zinc coordination within 5 A was detected in this study

  8. Structure factor of dimyristoylphosphatidylcholine unilamellar vesicles: small-angle x-ray scattering study

    International Nuclear Information System (INIS)

    Kiselev, M.A.; Aksenov, V.L.; Lombardo, D.; Kisselev, A.M.; Lesieur, P.

    2003-01-01

    Small-angle X-ray scattering (SAXS) experiments have been performed on dimyristoylphosphatidylcholine (DMPC) unilamellar vesicles in 40% aqueous sucrose solution. Model of separated form factors was applied for the evaluation of SAXS curves from large unilamellar vesicles. For the first time vesicle structure factor, polydispersity, average radius and membrane thickness were calculated simultaneously from the SAXS curves at T=30 deg C for DMPC concentrations in the range from 15 to 75 mM (1-5% w/w). Structure factor correction to the scattering curve was shown to be negligibly small for the lipid concentration of 15 mM (1% w/w). It was proved to be necessary to introduce structure factor correction to the scattering curves for lipid concentrations ≥ 30 mM (2% w/w)

  9. Structure-activity relationships of heterogeneous catalysts from time-resolved X-ray absorption spectroscopy

    International Nuclear Information System (INIS)

    Ressler, T.; Jentoft, R.E.; Wienold, J.; Girgsdies, F.; Neisius, T.; Timpe, O.

    2003-01-01

    Knowing the composition and the evolution of the bulk structure of a heterogeneous catalyst under working conditions (in situ) is a pre-requisite for understanding structure-activity relationships. X-ray absorption spectroscopy can be employed to study a catalytically active material in situ. In addition to steady-state investigations, the technique permits experiments with a time-resolution in the sub-second range to elucidate the solid-state kinetics of the reactions involved. Combined with mass spectrometry, the evolution of the short-range order structure of a heterogeneous catalyst, the average valence of the constituent metals, and the phase composition can be obtained. Here we present results obtained from time-resolved studies on the reduction of MoO 3 in propene and in propene and oxygen

  10. Ultrasmall-angle X-ray scattering analysis of photonic crystal structure

    International Nuclear Information System (INIS)

    Abramova, V. V.; Sinitskii, A. S.; Grigor'eva, N. A.; Grigor'ev, S. V.; Belov, D. V.; Petukhov, A. V.; Mistonov, A. A.; Vasil'eva, A. V.; Tret'yakov, Yu. D.

    2009-01-01

    The results of an ultrasmall-angle X-ray scattering study of iron(III) oxide inverse opal thin films are presented. The photonic crystals examined are shown to have fcc structure with amount of stacking faults varying among the samples. The method used in this study makes it possible to easily distinguish between samples with predominantly twinned fcc structure and nearly perfect fcc stacking. The difference observed between samples fabricated under identical conditions is attributed to random layer stacking in the self-assembled colloidal crystals used as templates for fabricating the inverse opals. The present method provides a versatile tool for analyzing photonic crystal structure in studies of inverse opals made of various materials, colloidal crystals, and three-dimensional photonic crystals of other types.

  11. Structure Factor of Dimyristoylphosphatidylcholine Unilamellar Vesicles Small-Angle X-Ray Scattering Study

    CERN Document Server

    Kiselev, M A; Kisselev, A M; Lesieur, P; Aksenov, V L

    2003-01-01

    Small-angle X-ray scattering (SAXS) experiments have been performed on dimyristoylphosphatidylcholine (DMPC) unilamellar vesicles in 40 % aqueous sucrose solution. Model of separated form factors was applied for the evaluation of SAXS curves from large unilamellar vesicles. For the first time vesicle structure factor, polydispersity, average radius and membrane thickness were calculated simultaneously from the SAXS curves at T=306{\\circ}C for DMPC concentrations in the range from 15 to 75 mM (1-5 % w/w). Structure factor correction to the scattering curve was shown to be negligibly small for the lipid concentration of 15 mM (1 % w/w). It was proved to be necessary to introduce structure factor correction to the scattering curves for lipid concentrations {\\ge}30 mM (2 % w/w).

  12. High pressure study of nanostructured Cu2Sb by X-ray Diffraction, Extended X-ray Absorption fine structure and Raman measurements

    International Nuclear Information System (INIS)

    Souza, Sergio Michielon de; Triches, Daniela Menegon; Lima, Joao Cardoso de; Polian, Alain

    2016-01-01

    Full text: Nanostructured tetragonal Cu 2 Sb was prepared by mechanical alloying and its stability was studied as a function of pressure using synchrotron X-ray diffraction (XRD) Extended X-Ray Absorption Fine Structure (EXAFS) and Raman spectroscopy. The high pressure XRD data were collected at 0.6, 1.1, 2.2, 3.4, 5.0, 7.1, 8.0, 9.9, 14.8, 18.7, 23.2, 29.3 and 40.6 GPa in the ELETTRA synchrotron (Italy) with λ = 0.68881 Å. The high pressure EXAFS measurements were carried out in the Soleil synchrotron (France) in 0.6, 1.8, 3.0, 4.5, 6.1, 8.0, 10.3, 12.7, 15.5, 18.0, 19.0, 20.0, 22.1, 23.9, 26.3 and 29.4 GPa and the high pressure Raman spectroscopy in the Institut de Mineralogie et de Physique des Milieux Condenses (France) collected at 0.1, 1.6, 3.7, 6.7, 11.2, 15.1, 19.4, 24.5, 30.8, 36.3, 41.3 and 44.5 GPa. The results show high structural and optical phase stability. The moduli bulk and its derivatives were obtained by using the Birch-Murnaghan equation of states to the XRD and EXAFS results. The evolution of the Raman modes and the bulk moduli were used to obtain the Grueneisen parameters. (author)

  13. Cell-free protein synthesis for structure determination by X-ray crystallography.

    Science.gov (United States)

    Watanabe, Miki; Miyazono, Ken-ichi; Tanokura, Masaru; Sawasaki, Tatsuya; Endo, Yaeta; Kobayashi, Ichizo

    2010-01-01

    Structure determination has been difficult for those proteins that are toxic to the cells and cannot be prepared in a large amount in vivo. These proteins, even when biologically very interesting, tend to be left uncharacterized in the structural genomics projects. Their cell-free synthesis can bypass the toxicity problem. Among the various cell-free systems, the wheat-germ-based system is of special interest due to the following points: (1) Because the gene is placed under a plant translational signal, its toxic expression in a bacterial host is reduced. (2) It has only little codon preference and, especially, little discrimination between methionine and selenomethionine (SeMet), which allows easy preparation of selenomethionylated proteins for crystal structure determination by SAD and MAD methods. (3) Translation is uncoupled from transcription, so that the toxicity of the translation product on DNA and its transcription, if any, can be bypassed. We have shown that the wheat-germ-based cell-free protein synthesis is useful for X-ray crystallography of one of the 4-bp cutter restriction enzymes, which are expected to be very toxic to all forms of cells retaining the genome. Our report on its structure represents the first report of structure determination by X-ray crystallography using protein overexpressed with the wheat-germ-based cell-free protein expression system. This will be a method of choice for cytotoxic proteins when its cost is not a problem. Its use will become popular when the crystal structure determination technology has evolved to require only a tiny amount of protein.

  14. Phase Transformation and Lithiation Effect on Electronic Structure of LixFePO4 : An In-Depth Study by Soft X-ray and Simulations

    NARCIS (Netherlands)

    Liu, Xiaosong; Liu, Jun; Qiao, Ruimin; Yu, Yan; Li, Hong; Suo, Liumin; Hu, Yong-sheng; Chuang, Yi-De; Shu, Guojiun; Chou, Fangcheng; Weng, Tsu-Chien; Nordlund, Dennis; Sokaras, Dimosthenis; Wang, Yung Jui; Lin, Hsin; Barbiellini, Bernardo; Bansil, Arun; Song, Xiangyun; Liu, Zhi; Yan, Shishen; Liu, Gao; Qjao, Shan; Richardson, Thomas J.; Prendergast, David; Hussain, Zahid; de Groot, Frank M. F.|info:eu-repo/dai/nl/08747610X; Yang, Wanli

    2012-01-01

    Through soft X-ray absorption spectroscopy, hard X-ray Raman scattering, and theoretical simulations, we provide the most in-depth and systematic study of the phase transformation and (de)lithiation effect on electronic structure in LixFePO4 nanoparticles and single crystals. Soft X-ray reveals

  15. Structural Characterization of Doped GaSb Single Crystals by X-ray Topography

    Energy Technology Data Exchange (ETDEWEB)

    Honnicke, M.G.; Mazzaro, I.; Manica, J.; Benine, E.; M da Costa, E.; Dedavid, B. A.; Cusatis, C.; Huang, X. R.

    2009-09-13

    We characterized GaSb single crystals containing different dopants (Al, Cd and Te), grown by the Czochralski method, by x-ray topography and high angular resolution x-ray diffraction. Lang topography revealed dislocations parallel and perpendicular to the crystal's surface. Double-crystal GaSb 333 x-ray topography shows dislocations and vertical stripes than can be associated with circular growth bands. We compared our high-angular resolution x-ray diffraction measurements (rocking curves) with the findings predicted by the dynamical theory of x-ray diffraction. These measurements show that our GaSb single crystals have a relative variation in the lattice parameter ({Delta}d/d) on the order of 10{sup -5}. This means that they can be used as electronic devices (detectors, for example) and as x-ray monochromators.

  16. Fine surface structure of unfixed and hydrated macrophages observed by laser-plasma x-ray contact microscopy

    International Nuclear Information System (INIS)

    Yamamoto, Yoshimasa; Friedman, Herman; Yoshimura, Hideyuki; Kinjo, Yasuhito; Shioda, Seiji; Debari, Kazuhiro; Shinohara, Kunio; Rajyaguru, Jayshree; Richardson, Martin

    2000-01-01

    A compact, high-resolution, laser-plasma, x-ray contact microscope using a table-top Nd:glass laser system has been developed and utilized for the analysis of the surface structure of live macrophages. Fine fluffy surface structures of murine peritoneal macrophages, which were live, hydrolyzed and not sliced and stained, were observed by the x-ray microscope followed by analysis using an atomic force microscopy. In order to compare with other techniques, a scanning electron microscopy (SEM) was utilized to observe the surface structure of the macrophages. The SEM offered a fine whole cell image of the same macrophages, which were fixed and dehydrated, but the surfaces were ruffled and different from that of x-ray images. A standard light microscope was also utilized to observe the shape of live whole macrophages. Light microscopy showed some fluffy surface structures of the macrophages, but the resolution was too low to observe the fine structures. Thus, the findings of fine fluffy surface structures of macrophages by x-ray microscopy provide valuable information for studies of phagocytosis, cell spreading and adherence, which are dependent on the surface structure of macrophages. Furthermore, the present study also demonstrates the usefulness of x-ray microscopy for analysis of structures of living cells

  17. X-ray detector

    International Nuclear Information System (INIS)

    Whetten, N.R.; Houston, J.M.

    1977-01-01

    An ionization chamber for use in determining the spatial distribution of x-ray photons in tomography systems comprises a plurality of substantially parallel, planar anodes separated by parallel, planar cathodes and enclosed in a gas of high atomic weight at a pressure from approximately 10 atmospheres to approximately 50 atmospheres. The cathode and anode structures comprise metals which are substantially opaque to x-ray radiation and thereby tend to reduce the resolution limiting effects of x-ray fluoresence in the gas. In another embodiment of the invention the anodes comprise parallel conductive bars disposed between two planar cathodes. Guard rings eliminate surface leakage currents between adjacent electrodes. 8 figures

  18. xMDFF: molecular dynamics flexible fitting of low-resolution X-ray structures

    International Nuclear Information System (INIS)

    McGreevy, Ryan; Singharoy, Abhishek; Li, Qufei; Zhang, Jingfen; Xu, Dong; Perozo, Eduardo; Schulten, Klaus

    2014-01-01

    A new real-space refinement method for low-resolution X-ray crystallography is presented. The method is based on the molecular dynamics flexible fitting protocol targeted at addressing large-scale deformations of the search model to achieve refinement with minimal manual intervention. An explanation of the method is provided, augmented by results from the refinement of both synthetic and experimental low-resolution data, including an independent electrophysiological verification of the xMDFF-refined crystal structure of a voltage-sensor protein. X-ray crystallography remains the most dominant method for solving atomic structures. However, for relatively large systems, the availability of only medium-to-low-resolution diffraction data often limits the determination of all-atom details. A new molecular dynamics flexible fitting (MDFF)-based approach, xMDFF, for determining structures from such low-resolution crystallographic data is reported. xMDFF employs a real-space refinement scheme that flexibly fits atomic models into an iteratively updating electron-density map. It addresses significant large-scale deformations of the initial model to fit the low-resolution density, as tested with synthetic low-resolution maps of d-ribose-binding protein. xMDFF has been successfully applied to re-refine six low-resolution protein structures of varying sizes that had already been submitted to the Protein Data Bank. Finally, via systematic refinement of a series of data from 3.6 to 7 Å resolution, xMDFF refinements together with electrophysiology experiments were used to validate the first all-atom structure of the voltage-sensing protein Ci-VSP

  19. xMDFF: molecular dynamics flexible fitting of low-resolution X-ray structures

    Energy Technology Data Exchange (ETDEWEB)

    McGreevy, Ryan; Singharoy, Abhishek [University of Illinois at Urbana-Champaign, Urbana, IL 61801 (United States); Li, Qufei [The University of Chicago, Chicago, IL 60637 (United States); Zhang, Jingfen; Xu, Dong [University of Missouri, Columbia, MO 65211 (United States); Perozo, Eduardo [The University of Chicago, Chicago, IL 60637 (United States); Schulten, Klaus, E-mail: kschulte@ks.uiuc.edu [University of Illinois at Urbana-Champaign, Urbana, IL 61801 (United States); University of Illinois at Urbana-Champaign, Urbana, IL 61801 (United States)

    2014-09-01

    A new real-space refinement method for low-resolution X-ray crystallography is presented. The method is based on the molecular dynamics flexible fitting protocol targeted at addressing large-scale deformations of the search model to achieve refinement with minimal manual intervention. An explanation of the method is provided, augmented by results from the refinement of both synthetic and experimental low-resolution data, including an independent electrophysiological verification of the xMDFF-refined crystal structure of a voltage-sensor protein. X-ray crystallography remains the most dominant method for solving atomic structures. However, for relatively large systems, the availability of only medium-to-low-resolution diffraction data often limits the determination of all-atom details. A new molecular dynamics flexible fitting (MDFF)-based approach, xMDFF, for determining structures from such low-resolution crystallographic data is reported. xMDFF employs a real-space refinement scheme that flexibly fits atomic models into an iteratively updating electron-density map. It addresses significant large-scale deformations of the initial model to fit the low-resolution density, as tested with synthetic low-resolution maps of d-ribose-binding protein. xMDFF has been successfully applied to re-refine six low-resolution protein structures of varying sizes that had already been submitted to the Protein Data Bank. Finally, via systematic refinement of a series of data from 3.6 to 7 Å resolution, xMDFF refinements together with electrophysiology experiments were used to validate the first all-atom structure of the voltage-sensing protein Ci-VSP.

  20. X-ray magnetic microscopy for correlations between magnetic domains and crystal structure

    International Nuclear Information System (INIS)

    Denbeaux, G.; Anderson, E.; Bates, B.; Chao, W.; Liddle, J.A.; Harteneck, B.; Pearson, A.; Salmassi, F.; Schneider, G.; Fischer, P.; Eimuller, T.; Taylor, S.; Chang, H.; Kusinski, G.J.

    2002-01-01

    Accurately determining the resolution of x-ray microscopes has been a challenge because good test patterns for x-ray microscopy have been hard to make. We report on a sputter-deposited multilayer imaged in cross section as a test pattern with small features and high aspect ratios. One application of high-resolution imaging is magnetic materials. Off-axis bend magnet radiation is known to have a component of circular polarization which can be used for x-ray magnetic circular dichroism. We calculate the integrated circular polarization collected by the illumination optics in the XM-1 full-field x-ray microscope. (authors)

  1. Variability: A X-ray ruler for the AGN structure model

    Directory of Open Access Journals (Sweden)

    Guainazzi M.

    2012-12-01

    Full Text Available Validating our understanding of the innermost structure of Active Galactic Nuclei (AGN would require resolving sub-parsec scales. Lacking adequate direct imaging, X-ray astronomy can still contribute to this undertaking through the study of spectral variability on time-scales from days to years. This bears information on the location of gaseous and dusty systems in the innermost regions around the accreting supermassive black hole. In this paper I discuss the application of this concept in two specific contexts: a “fast” column density variations in heavily obscured AGN; b reverberation of optically-thick reprocessing. These results lend support to a scenario where obscuration and optically thick reprocessing are due to a variety of different systems, ranging from the Broad Line Regions to a clumpy structure extended on larger scales up to hundreds of parsecs.

  2. Electronic Structures of Purple Bronze KMo6O17 Studied by X-Ray Photoemission Spectra

    Science.gov (United States)

    Qin, Xiaokui; Wei, Junyin; Shi, Jing; Tian, Mingliang; Chen, Hong; Tian, Decheng

    X-ray photoemission spectroscopy study has been performed for the purple bronze KMo6O17. The structures of conduction band and valence band are analogous to the results of ultraviolet photoemission spectra and are also consistent with the model of Travaglini et al., but the gap between conduction and valence band is insignificant. The shape of asymmetric and broadening line of O-1s is due to unresolved contributions from the many inequivalent oxygen sites in this crystal structure. Mo 3d core-level spectrum reveals that there are two kinds of valence states of Molybdenum (Mo+5 and Mo+6). The calculated average valence state is about +5.6, which is consistent with the expectation value from the composition of this material. The tail of Mo-3d spectrum toward higher binding energy is the consequence of the excitation of electron-hole pairs with singularity index of 0.21.

  3. Probing chemistry within the membrane structure of wood with soft X-ray spectral microscopy

    International Nuclear Information System (INIS)

    Cody, George D.

    2000-01-01

    Scanning Transmission Soft X-ray spectral microscopy on Carbon's 1s absorption edge reveals the distribution of structural biopolymers within cell membrane regions of modern cedar and oak. Cellulose is extremely susceptible to beam damage. Spectroscopic studies of beam damage reveals that the chemical changes resulting from secondary electron impact may be highly selective and is consistent with hydroxyl eliminations and structural rearrangement of pyranose rings in alpha-cellulose to hydroxyl substituted γ pyrones. A study of acetylated cellulose demonstrates significantly different chemistry; principally massive decarboxylation. Defocusing the beam to a 2 μm spot size allows for the acquisition of 'pristine' cellulose spectra. Spectral deconvolution is used to assess the distribution of lignin and cellulose in the different regions of the cell membrane. Using the intensity of the hydroxylated aromatic carbons 1s-π * transition, the ratio of coniferyl and syringyl based lignin within the middle lamellae and secondary cell wall of oak, an angiosperm can be determined

  4. Soft x-ray resonant diffraction study of magnetic structure in magnetoelectric Y-type hexaferrite

    Science.gov (United States)

    Ueda, H.; Tanaka, Y.; Wakabayashi, Y.; Kimura, T.

    2018-05-01

    The effect of magnetic field on the magnetic structure associated with magnetoelectric properties in a Y-type hexaferrite, Ba1.3Sr0.7CoZnFe11AlO22, was investigated by utilizing the soft x-ray resonant diffraction technique. In this hexaferrite, the so-called alternating longitudinal conical phase is stabilized at room temperature and zero magnetic field. Below room temperature, however, this phase is transformed into the so-called transverse conical phase by applying an in-plane magnetic field (≈ 0.3 T). The transverse conical phase persists even after removing the magnetic field. The magnetoelectricity, which is magnetically-induced electric polarization, observed in the hexaferrite is discussed in terms of the temperature-dependent magnetic structure at zero field.

  5. A method for measuring the time structure of synchrotron x-ray beams

    International Nuclear Information System (INIS)

    Moses, W.W.; Derenzo, S.E.

    1989-08-01

    We describe a method employing a plastic scintillator coupled to a fast photomultiplier tube to generate a timing pulse from the x-ray bursts emitted from a synchrotron radiation source. This technique is useful for performing synchrotron experiments where detailed knowledge of the timing distribution is necessary, such as time resolved spectroscopy or fluorescence lifetime experiments. By digitizing the time difference between the timing signal generated on one beam crossing with the timing signal generated on the next beam crossing, the time structure of a synchrotron beam can be analyzed. Using this technique, we have investigated the single bunch time structure at the National Synchrotron Light Source (NSLS) during pilot runs in January, 1989, and found that the majority of the beam (96%) is contained in one rf bucket, while the remainder of the beam (4%) is contained in satellite rf buckets preceeding and following the main rf bucket by 19 ns. 1 ref., 4 figs

  6. On the Origin of Hard X-ray Structures in the VELA Supernova Remnant

    Science.gov (United States)

    Gvaramadze, V. V.

    1998-12-01

    We propose an alternative explanation for the origin of two hard X-ray structures recently discovered in the central part of the Vela supernova remnant (SNR) by Willmore et al. (1992, MNRAS, 254, 139) and Markwardt & Ogelman (1995, Nature, 375, 40; 1997, ApJ, 480, L13), and interpreted as a plerion and a pulsar jet respectively. We suggest that the first structure is a dense material shed by the supernova progenitor star during the red supergiant stage, and reheated after the supernova exploded, while the "jet" is simply a dense filament in the Vela SNR's general shell, whose origin is connected with the Rayleigh-Taylor instability in the (main-sequence) wind-driven shell reaccelerated by the supernova blast wave.

  7. The structure of para-toluidine by X-ray and neutron diffraction

    International Nuclear Information System (INIS)

    Bertinotti, A.L.

    1965-12-01

    The crystal and molecular structure of para-toluidine has been solved by X-ray and neutron diffraction counter techniques. The molecules are arranged in the form of infinite chains in the crystal, each molecule being linked to two neighbours by hydrogen bonds. The presence of the H bonds makes clear the difference in the melting points between para-toluidine and benzene hydrocarbons of related symmetry and molecular weight. Their direction accounts for the (001) cleavage and the growth anisotropy of crystals from supersaturated vapour phase. A structure-seeking method by computer has been elaborated, using lattice energy calculations applied to molecules treated as rigid bodies and making use of a simplex method for function minimization without calculation of derivatives. The way the available information is handled allows to increase the range of convergence, as shown in the case of para-toluidine. (author) [fr

  8. A comparison of X-ray and calculated structures of the enzyme MTH1.

    Science.gov (United States)

    Ryan, Hannah; Carter, Megan; Stenmark, Pål; Stewart, James J P; Braun-Sand, Sonja B

    2016-07-01

    Modern computational chemistry methods provide a powerful tool for use in refining the geometry of proteins determined by X-ray crystallography. Specifically, computational methods can be used to correctly place hydrogen atoms unresolved by this experimental method and improve bond geometry accuracy. Using the semiempirical method PM7, the structure of the nucleotide-sanitizing enzyme MTH1, complete with hydrolyzed substrate 8-oxo-dGMP, was optimized and the resulting geometry compared with the original X-ray structure of MTH1. After determining hydrogen atom placement and the identification of ionized sites, the charge distribution in the binding site was explored. Where comparison was possible, all the theoretical predictions were in good agreement with experimental observations. However, when these were combined with additional predictions for which experimental observations were not available, the result was a new and alternative description of the substrate-binding site interaction. An estimate was made of the strengths and weaknesses of the PM7 method for modeling proteins on varying scales, ranging from overall structure to individual interatomic distances. An attempt to correct a known fault in PM7, the under-estimation of steric repulsion, is also described. This work sheds light on the specificity of the enzyme MTH1 toward the substrate 8-oxo-dGTP; information that would facilitate drug development involving MTH1. Graphical Abstract Overlay of the backbone traces of the two MTH1 protein chains (green and orange respectively) in PDB 3ZR0 and the equivalent PM7 structures (magenta and cyan respectively) each optimized separately.

  9. X-ray structural studies of quinone reductase 2 nanomolar range inhibitors

    Energy Technology Data Exchange (ETDEWEB)

    Pegan, Scott D.; Sturdy, Megan; Ferry, Gilles; Delagrange, Philippe; Boutin, Jean A.; Mesecar, Andrew D. (IdRS); (Purdue); (Colorado); (UIC)

    2011-09-06

    Quinone reductase 2 (QR2) is one of two members comprising the mammalian quinone reductase family of enzymes responsible for performing FAD mediated reductions of quinone substrates. In contrast to quinone reductase 1 (QR1) which uses NAD(P)H as its co-substrate, QR2 utilizes a rare group of hydride donors, N-methyl or N-ribosyl nicotinamide. Several studies have linked QR2 to the generation of quinone free radicals, several neuronal degenerative diseases, and cancer. QR2 has been also identified as the third melatonin receptor (MT3) through in cellulo and in vitro inhibition of QR2 by traditional MT3 ligands, and through recent X-ray structures of human QR2 (hQR2) in complex with melatonin and 2-iodomelatonin. Several MT3 specific ligands have been developed that exhibit both potent in cellulo inhibition of hQR2 nanomolar, affinity for MT3. The potency of these ligands suggest their use as molecular probes for hQR2. However, no definitive correlation between traditionally obtained MT3 ligand affinity and hQR2 inhibition exists limiting our understanding of how these ligands are accommodated in the hQR2 active site. To obtain a clearer relationship between the structures of developed MT3 ligands and their inhibitory properties, in cellulo and in vitro IC{sub 50} values were determined for a representative set of MT3 ligands (MCA-NAT, 2-I-MCANAT, prazosin, S26695, S32797, and S29434). Furthermore, X-ray structures for each of these ligands in complex with hQR2 were determined allowing for a structural evaluation of the binding modes of these ligands in relation to the potency of MT3 ligands.

  10. Structural characterization of cellulosic materials using x-ray and neutron scattering

    Energy Technology Data Exchange (ETDEWEB)

    Penttila, P.

    2013-11-01

    Cellulosic biomass can be used as a feedstock for sustainable production of biofuels and various other products. A complete utilization of the raw material requires understanding on its structural aspects and their role in the various processes. In this thesis, x-ray and neutron scattering methods were applied to study the structure of various cellulosic materials and how they are affected in different processes. The obtained results were reviewed in the context of a model for the cellulose nanostructure. The dimensions of cellulose crystallites and the crystallinity were determined with wide-angle x-ray scattering (WAXS), whereas the nanoscale fibrillar structure of cellulose was characterized with small-angle x-ray and neutron scattering (SAXS and SANS). The properties determined with the small-angle scattering methods included specific surface areas and distances characteristic of the packing of cellulose microfibrils. Also other physical characterization methods, such as x-ray microtomography, infrared spectroscopy, and solid-state NMR were utilized in this work. In the analysis of the results, a comprehensive understanding of the structural changes throughout a range of length scales was aimed at. Pretreatment of birch sawdust by pressurized hot water extraction was observed to increase the crystal width of cellulose, as determined with WAXS, even though the cellulose crystallinity was slightly decreased. A denser packing of microfibrils caused by the removal of hemicelluloses and lignin in the extraction was evidenced by SAXS. This resulted in the opening of new pores between the microfibril bundles and an increase of the specific surface area. Enzymatic hydrolysis of microcrystalline cellulose (MCC) did not lead to differences in the average crystallinity or crystal size of the hydrolysis residues, which was explained to be caused by limitations due to the large size of the enzymes as compared to the pores inside the fibril aggregates. The SAXS intensities

  11. Structural changes of green roof growing substrate layer studied by X-ray CT

    Science.gov (United States)

    Jelinkova, Vladimira; Sacha, Jan; Dohnal, Michal; Snehota, Michal

    2017-04-01

    Increasing interest in green infrastructure linked with newly implemented legislation/rules/laws worldwide opens up research potential for field of soil hydrology. A better understanding of function of engineered soils involved in green infrastructure solutions such as green roofs or rain garden is needed. A soil layer is considered as a highly significant component of the aforesaid systems. In comparison with a natural soil, the engineered soil is assumed to be the more challenging case due to rapid structure changes early stages after its build-up. The green infrastructure efficiency depends on the physical and chemical properties of the soil, which are, in the case of engineered soils, a function of its initial composition and subsequent soil formation processes. The project presented in this paper is focused on fundamental processes in the relatively thick layer of engineered soil. The initial structure development, during which the pore geometry is altered by the growth of plant roots, water influx, solid particles translocation and other soil formation processes, is investigated with the help of noninvasive imaging technique  X-ray computed tomography. The soil development has been studied on undisturbed soil samples taken periodically from green roof test system during early stages of its life cycle. Two approaches and sample sizes were employed. In the first approach, undisturbed samples (volume of about 63 cm3) were taken each time from the test site and scanned by X-ray CT. In the second approach, samples (volume of about 630 cm3) were permanently installed at the test site and has been repeatedly removed to perform X-ray CT imaging. CT-derived macroporosity profiles reveal significant temporal changes of soil structure. Clogging of pores by fine particles and fissures development are two most significant changes that would affect the green roof system efficiency. This work has been supported by the Ministry of Education, Youth and Sports within

  12. Extended x-ray absorption fine structure (EXAFS): a novel probe for local structure of glassy solids

    International Nuclear Information System (INIS)

    Wong, J.

    1979-01-01

    The extended x-ray absorption fine structure (EXAFS) is the oscillation in the absorption coefficient extending a few hundred eVs on the high energy side of an x-ray absorption edge. This mode of spectroscopy has recently been realized to be a powerful tool in probing the local atomic structure of all states of matter, particularly with the advent of intense synchrotron radiation. More importantly is the unique ability of EXAFS to probe the structure and dynamics around individual atomic species in a multi-atomic system. In this paper, the physical processes associated with the EXAFS phenomenon will be discussed. Experimental results obtained at the Stanford Synchrotron Radiation Laboratory on some oxide and metallic glasses will be presented. The local structure in these materials are elucidated using a Fourier transform technique

  13. Nanoscale characterization of local structures and defects in photonic crystals using synchrotron-based transmission soft X-ray microscopy

    Science.gov (United States)

    Nho, Hyun Woo; Kalegowda, Yogesh; Shin, Hyun-Joon; Yoon, Tae Hyun

    2016-01-01

    For the structural characterization of the polystyrene (PS)-based photonic crystals (PCs), fast and direct imaging capabilities of full field transmission X-ray microscopy (TXM) were demonstrated at soft X-ray energy. PS-based PCs were prepared on an O2-plasma treated Si3N4 window and their local structures and defects were investigated using this label-free TXM technique with an image acquisition speed of ~10 sec/frame and marginal radiation damage. Micro-domains of face-centered cubic (FCC (111)) and hexagonal close-packed (HCP (0001)) structures were dominantly found in PS-based PCs, while point and line defects, FCC (100), and 12-fold symmetry structures were also identified as minor components. Additionally, in situ observation capability for hydrated samples and 3D tomographic reconstruction of TXM images were also demonstrated. This soft X-ray full field TXM technique with faster image acquisition speed, in situ observation, and 3D tomography capability can be complementally used with the other X-ray microscopic techniques (i.e., scanning transmission X-ray microscopy, STXM) as well as conventional characterization methods (e.g., electron microscopic and optical/fluorescence microscopic techniques) for clearer structure identification of self-assembled PCs and better understanding of the relationship between their structures and resultant optical properties. PMID:27087141

  14. The stoichiometry of synthetic alunite as a function of hydrothermal aging investigated by solid-state NMR spectroscopy, powder X-ray diffraction and infrared spectroscopy

    DEFF Research Database (Denmark)

    Grube, Elisabeth; Nielsen, Ulla Gro

    2015-01-01

    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...... 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....

  15. The origin of luminescence from di[4-(4-diphenylaminophenyl)phenyl]sulfone (DAPSF), a blue light emitter: an X-ray excited optical luminescence (XEOL) and X-ray absorption near edge structure (XANES) study.

    Science.gov (United States)

    Zhang, Duo; Zhang, Hui; Zhang, Xiaohong; Sham, Tsun-Kong; Hu, Yongfeng; Sun, Xuhui

    2016-03-07

    The electronic structure and optical properties of di[4-(4-diphenylaminophenyl)phenyl]sulfone (denoted as DAPSF), a highly efficient fluorophor, have been investigated using X-ray excited optical luminescence (XEOL) and X-ray absorption near edge structure (XANES) spectroscopy at excitation energies across the C, N, O K-edges and the sulfur K-edge. The results indicate that the blue luminescence is mainly related to the sulfur functional group.

  16. Where Water is Oxidized to Dioxygen: Structure of the Photosynthetic Mn4Ca Cluster from X-ray Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Yano, Junko; Yano, Junko; Yachandra, Vittal K.

    2007-10-24

    Light-driven oxidation of water to dioxygen in plants, algae and cyanobacteria iscatalyzed within photosystem II (PS II) by a Mn4Ca cluster. Although the cluster has been studied by many different methods, the structure and the mechanism have remained elusive. X-ray absorption and emission spectroscopy and EXAFS studies have been particularly useful in probing the electronic and geometric structure, and the mechanism of the water oxidation reaction. Recent progress, reviewed here, includes polarized X-ray absorption spectroscopy measurements of PS II single crystals. Analysis of those results has constrained the Mn4Ca cluster geometry to a setof three similar high-resolution structures. The structure of the cluster from the present study is unlike either the 3.0 or 3.5 Angstrom-resolution X-ray structures or other previously proposed models. The differences between the models derived from X-rayspectroscopy and crystallography are predominantly because of damage to the Mn4Ca cluster by X-rays under the conditions used for structure determination by X-ray crystallography. X-ray spectroscopy studies are also used for studying the changes in the structure of the Mn4Ca catalytic center as it cycles through the five intermediate states known as the Si-states (i=0-4). The electronic structure of the Mn4Ca cluster has been studied more recently using resonant inelastic X-ray scattering spectroscopy (RIXS), in addition to the earlier X-ray absorption and emission spectroscopy methods. These studies are revealing that the assignment of formaloxidation states is overly simplistic. A more accurate description should consider the charge density on the Mn atoms that includes the covalency of the bonds and delocalization of the charge over the cluster. The geometric and electronic structure of the Mn4Ca cluster in the S-states derived from X-ray spectroscopy are leading to a detailed understanding of the mechanism of the O-O bond formation during the photosynthetic water

  17. An instrument for in situ time-resolved X-ray imaging and diffraction of laser powder bed fusion additive manufacturing processes

    Science.gov (United States)

    Calta, Nicholas P.; Wang, Jenny; Kiss, Andrew M.; Martin, Aiden A.; Depond, Philip J.; Guss, Gabriel M.; Thampy, Vivek; Fong, Anthony Y.; Weker, Johanna Nelson; Stone, Kevin H.; Tassone, Christopher J.; Kramer, Matthew J.; Toney, Michael F.; Van Buuren, Anthony; Matthews, Manyalibo J.

    2018-05-01

    In situ X-ray-based measurements of the laser powder bed fusion (LPBF) additive manufacturing process produce unique data for model validation and improved process understanding. Synchrotron X-ray imaging and diffraction provide high resolution, bulk sensitive information with sufficient sampling rates to probe melt pool dynamics as well as phase and microstructure evolution. Here, we describe a laboratory-scale LPBF test bed designed to accommodate diffraction and imaging experiments at a synchrotron X-ray source during LPBF operation. We also present experimental results using Ti-6Al-4V, a widely used aerospace alloy, as a model system. Both imaging and diffraction experiments were carried out at the Stanford Synchrotron Radiation Lightsource. Melt pool dynamics were imaged at frame rates up to 4 kHz with a ˜1.1 μm effective pixel size and revealed the formation of keyhole pores along the melt track due to vapor recoil forces. Diffraction experiments at sampling rates of 1 kHz captured phase evolution and lattice contraction during the rapid cooling present in LPBF within a ˜50 × 100 μm area. We also discuss the utility of these measurements for model validation and process improvement.

  18. Multi-scale characteristics of coal structure by x-ray computed tomography (x-ray CT), scanning electron microscope (SEM) and mercury intrusion porosimetry (MIP)

    Science.gov (United States)

    Cai, Ting-ting; Feng, Zeng-chao; Zhou, Dong

    2018-02-01

    It is of great benefit to study the material and structural heterogeneity of coal for better understanding the coalbed methane (CBM) storage and enrichment. In this paper, multi-scale X-ray computed tomography (CT), scanning electron microscope (SEM) and mercury intrusion porosimetry (MIP) at multi scales were conducted to thoroughly study the material distribution, heterogeneity, pore development, porosity and permeability of coal. It is suitable and reasonable to divide the testing samples into three structural categories by average density and heterogeneity degree, and the meso structure in the three categories accords with the morphology on SEM images. The pore size distribution and pore development of each subsample cannot be correspondingly related to their respective structure category or morphology due to different observation scales, while the macro pore size development, accumulated macro pore volume and macro pores porosity accord with the meso structure category and morphology information by CT and SEM at the same scale very well. Given the effect of macro pores on permeability and the contribution of micro pores to CBM storage capacity, reservoirs with developed micro pores and macro pores may be the most suitable coal reservoir for CBM exploitation.

  19. X-ray photoelectron spectra structure and chemical bonding in AmO2

    Directory of Open Access Journals (Sweden)

    Teterin Yury A.

    2015-01-01

    Full Text Available Quantitative analysis was done of the X-ray photoelectron spectra structure in the binding energy range of 0 eV to ~35 eV for americium dioxide (AmO2 valence electrons. The binding energies and structure of the core electronic shells (~35 eV-1250 eV, as well as the relativistic discrete variation calculation results for the Am63O216 and AmO8 (D4h cluster reflecting Am close environment in AmO2 were taken into account. The experimental data show that the many-body effects and the multiplet splitting contribute to the spectral structure much less than the effects of formation of the outer (0-~15 eV binding energy and the inner (~15 eV-~35 eV binding energy valence molecular orbitals. The filled Am 5f electronic states were shown to form in the AmO2 valence band. The Am 6p electrons participate in formation of both the inner and the outer valence molecular orbitals (bands. The filled Am 6p3/2 and the O 2s electronic shells were found to make the largest contributions to the formation of the inner valence molecular orbitals. Contributions of electrons from different molecular orbitals to the chemical bond in the AmO8 cluster were evaluated. Composition and sequence order of molecular orbitals in the binding energy range 0-~35 eV in AmO2 were established. The experimental and theoretical data allowed a quantitative scheme of molecular orbitals for AmO2, which is fundamental for both understanding the chemical bond nature in americium dioxide and the interpretation of other X-ray spectra of AmO2.

  20. X-ray absorption spectroscopy: EXAFS and XANES - A versatile tool to study the atomic and electronic structure of materials

    International Nuclear Information System (INIS)

    Alp, E.E.; Mini, S.M.; Ramanathan, M.

    1990-01-01

    X-ray absorption spectroscopy (XAS) had been an essential tool to gather spectroscopic information about atomic energy level structure in the early decades of this century. The correct interpretation of the oscillatory structure in the x-ray absorption cross-section above the absorption edge has transformed XAS from a spectroscopic tool to a structural technique. EXAFS (Extended X-ray Absorption Fine Structure) yields information about the interatomic distances, near neighbor coordination numbers, and lattice dynamics. XANES (X-ray Absorption Near Edge Structure), on the other hand, gives information about the valence state, energy bandwidth and bond angles. Today, there are about 50 experimental stations in various synchrotrons around the world dedicated to collecting x-ray absorption data from the bulk and surfaces of solids and liquids. In this chapter, they will give the basic principles of XAS, explain the information content of essentially two different aspects of the absorption process leading to EXAFS and XANES, and discuss the source and sample limitations

  1. Probing Photoinduced Structural Phase Transitions by Fast or Ultra-Fast Time-Resolved X-Ray Diffraction

    Science.gov (United States)

    Cailleau, Hervé Collet, Eric; Buron-Le Cointe, Marylise; Lemée-Cailleau, Marie-Hélène Koshihara, Shin-Ya

    A new frontier in the field of structural science is the emergence of the fast and ultra-fast X-ray science. Recent developments in time-resolved X-ray diffraction promise direct access to the dynamics of electronic, atomic and molecular motions in condensed matter triggered by a pulsed laser irradiation, i.e. to record "molecular movies" during the transformation of matter initiated by light pulse. These laser pump and X-ray probe techniques now provide an outstanding opportunity for the direct observation of a photoinduced structural phase transition as it takes place. The use of X-ray short-pulse of about 100ps around third-generation synchrotron sources allows structural investigations of fast photoinduced processes. Other new X-ray sources, such as laser-produced plasma ones, generate ultra-short pulses down to 100 fs. This opens the way to femtosecond X-ray crystallography, but with rather low X-ray intensities and more limited experimental possibilities at present. However this new ultra-fast science rapidly progresses around these sources and new large-scale projects exist. It is the aim of this contribution to overview the state of art and the perspectives of fast and ultra-fast X-ray scattering techniques to study photoinduced phase transitions (here, the word ultra-fast is used for sub-picosecond time resolution). In particular we would like to largely present the contribution of crystallographic methods in comparison with optical methods, such as pump-probe reflectivity measurements, the reader being not necessary familiar with X-ray scattering. Thus we want to present which type of physical information can be obtained from the positions of the Bragg peaks, their intensity and their shape, as well as from the diffuse scattering beyond Bragg peaks. An important physical feature is to take into consideration the difference in nature between a photoinduced phase transition and conventional homogeneous photoinduced chemical or biochemical processes where

  2. X-ray characterisation of nanostructured materials

    DEFF Research Database (Denmark)

    Oddershede, Jette

    X-ray powder di®raction (XRPD) is an excellent tool for characterising the bulk structure of crystalline materials. Along with the growing interest in exploiting materials with decreasing particle sizes and increasing number of defects, factors that complicate the traditional interpretation...... of the experi- mental XRPD patterns, the need for new interpretation methods has arisen. The method described in the present thesis is by no means new, in fact it was developed by Debye in 1915. However, the Debye method it is rather computationally heavy, so in practise it is only applicable to the X-ray char...

  3. Grazing angle X-ray fluorescence from periodic structures on silicon and silica surfaces

    International Nuclear Information System (INIS)

    Nowak, S.H.; Banaś, D.; Błchucki, W.; Cao, W.; Dousse, J.-Cl.; Hönicke, P.; Hoszowska, J.; Jabłoński, Ł.; Kayser, Y.; Kubala-Kukuś, A.; Pajek, M.; Reinhardt, F.; Savu, A.V.; Szlachetko, J.

    2014-01-01

    Various 3-dimensional nano-scaled periodic structures with different configurations and periods deposited on the surface of silicon and silica substrates were investigated by means of the grazing incidence and grazing emission X-ray fluorescence techniques. Apart from the characteristics which are typical for particle- and layer-like samples, the measured angular intensity profiles show additional periodicity-related features. The latter could be explained by a novel theoretical approach based on simple geometrical optics (GO) considerations. The new GO-based calculations were found to yield results in good agreement with experiment, also in cases where other theoretical approaches are not valid, e.g., periodic particle distributions with an increased surface coverage

  4. Synthesis of hydroxyapatite and structural refinement by X-ray diffraction

    International Nuclear Information System (INIS)

    Araujo, Jorge Correa de

    2007-01-01

    A sample of hydroxyapatite was synthesized and its crystalline structure was analyzed by X-ray diffraction by means of the Rietveld method. Two functions were used to fit the peak profiles, modified Voigt (TCHZ) and Pearson VII. The occupational factors and lattice parameters obtained by both models show that the sample does not contain relevant cationic substitutions. The interatomic distances from Ca1 to oxygens O1, O2 and O3 were adequate for a pure hydroxyapatite without defect at site Ca1. Besides, the use of multiple lines in planes (300) and (002) associated with the model Pearson VII resulted in good agreement with the TCHZ model with respect to the size-strain effects with an ellipsoidal shape of crystallites. In conclusion, the procedures adopted in the synthesis of hydroxyapatite produced a pure and crystalline material. The experimental results of transmission electron microscopy confirmed the predicted shape of crystals. (author)

  5. Computed microtomography and X-ray fluorescence analysis for comprehensive analysis of structural changes in bone.

    Science.gov (United States)

    Buzmakov, Alexey; Chukalina, Marina; Nikolaev, Dmitry; Schaefer, Gerald; Gulimova, Victoria; Saveliev, Sergey; Tereschenko, Elena; Seregin, Alexey; Senin, Roman; Prun, Victor; Zolotov, Denis; Asadchikov, Victor

    2013-01-01

    This paper presents the results of a comprehensive analysis of structural changes in the caudal vertebrae of Turner's thick-toed geckos by computer microtomography and X-ray fluorescence analysis. We present algorithms used for the reconstruction of tomographic images which allow to work with high noise level projections that represent typical conditions dictated by the nature of the samples. Reptiles, due to their ruggedness, small size, belonging to the amniote and a number of other valuable features, are an attractive model object for long-orbital experiments on unmanned spacecraft. Issues of possible changes in their bone tissue under the influence of spaceflight are the subject of discussions between biologists from different laboratories around the world.

  6. X-ray diffraction and molecular-dynamics studies: Structural analysis of phases in diglyceride monolayers

    DEFF Research Database (Denmark)

    Peters, Günther H.J.; Larsen, Niels Bent; Bjørnholm, T.

    1998-01-01

    We report a detailed structural analysis of the phases of 1,2-sn-dipalmitoylglycerol Langmuir monolayers at room temperature. Pressure-induced transitions have been investigated by combination of molecular-dynamics simulations and grazing-incidence x-ray diffraction (XRD). The diglyceride film...... undergoes two phase transitions occurring at 38.3 and 39.8 Angstrom(2)/molecule. Simulation indicates that the first transition involves a reorientation of the headgroups while simulation and XRD show that in the second transition the order parameter is the tilt angle of the alkyl chains. A methodology......; At the lowest pressure the tilt angle reaches approximate to 14 degrees in a direction close to a nearest neighbor direction. Both arrangements of the alkyl chains are confirmed by XRD. For higher order and fractional order Bragg peaks, simulations predict higher intensities than observed with XRD. This may...

  7. Synthesis, X-ray crystal structure and theoretical calculations of antileishmanial neolignan analogues

    Energy Technology Data Exchange (ETDEWEB)

    Nascimento, Josenaide P. do; Santos, Lourivaldo S.; Carmo, Maria Carolina L. do; Brasil, Davi S.B.; Alves, Claudio N., E-mail: nahum@ufpa.b [Universidade Federal do Para (UFPA), Belem, PA (Brazil). Inst. de Ciencias Exatas e Naturais; Santos, Regina Helena A.; Tozzo, Erica; Ferreira, Janaina G. [Universidade de Sao Paulo (IQSC/USP), Sao Carlos, SP (Brazil). Inst. de Quimica

    2010-07-01

    The synthesis and X-ray crystal diffraction structure of two analogues of neolignans, 2-(4-chlorophenyl)-1-phenylethanone (20) and 2-[(4-chlorophenyl)thio]-1-(3,4-dimethoxyphenyl) propan-1-one (12) is described. The compound 12 presents activity against intracellular Leishmania donovani and Leishmania amazonensis amastigotes that cause cutaneous and visceral leishmaniasis. In addition, the density functional theory (DFT) with the B3LYP hybrid functional was employed to calculate a set of molecular descriptors for nineteen synthetic analogues of neolignans with antileishmanial activities. Afterwards, the stepwise discriminant analysis was performed to investigate possible relationship between the molecular descriptors and biological activities. Through this analysis the compounds were classified into two groups active and inactive according to their degree of biological activities, and the more important properties were charges on some key atoms, electronic affinity and ClogP. (author)

  8. Structural phase transition in lanthanum gallate as studied by Raman and X-ray diffraction measurements

    Energy Technology Data Exchange (ETDEWEB)

    Dhak, P.; Pramanik, P. [Department of Chemistry, Indian Institute of Technology, Kharagpur 721302 (India); Bhattacharya, S.; Roy, Anushree [Department of Physics, Indian Institute of Technology, Kharagpur 721302 (India); Achary, S.N.; Tyagi, A.K. [Chemistry Division, Bhabha Atomic Research Centre, Mumbai 400 085 (India)

    2011-08-15

    Lanthanum gallate (LaGaO{sub 3}) is known to undergo orthorhombic to rhombohedral first order phase transition at 150 C. In this article we have shown that by introducing 2% La deficiency in the system, coexistence of above two phases can be obtained at lower temperature and a complete phase transition occurs at 200 C. The evolution of structural parameters of the system with temperature is reported from X-ray diffraction measurements and Rietveld analysis of the diffraction patterns. The change in local octahedral distortion due to 2% La deficiency is revealed through the shift in the phonon modes of GaO{sub 6} octahedra, in both orthorhombic and rhombohedral phase. (Copyright copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  9. Study of thermal degradation of organic light emitting device structures by X-ray scattering

    International Nuclear Information System (INIS)

    Lee, Young-Joo; Lee, Heeju; Byun, Youngsuk; Song, Sanghoon; Kim, Je-Eun; Eom, Daeyong; Cha, Wonsuk; Park, Seong-Sik; Kim, Jinwoo; Kim, Hyunjung

    2007-01-01

    We report the process of thermal degradation of organic light emitting devices (OLEDs) having multilayered structure of [LiF/tris-(8-hydroxyquinoline) aluminum(Alq 3 )/N,N'-Bis(naphthalen-1-yl)-N,N'-bis(phenyl)benzidine (NPB)/copper phthalocyanine (CuPc)/indium tin oxide (ITO)/SiO 2 on a glass] by synchrotron X-ray scattering. The results show that the thermally induced degradation process of OLED multilayers has undergone several evolutions due to thermal expansion of NPB, intermixing between NPB, Alq 3 , and LiF layers, dewetting of NPB on CuPc, and crystallization of NPB and Alq 3 depending on the annealing temperature. The crystallization of NPB appears at 180 deg. C, much higher temperature than the glass transition temperature (T g = 96 deg. C) of NPB. The results are also compared with the findings from the atomic force microscope (AFM) images

  10. Determination of collagen fibril structure and orientation in connective tissues by X-ray diffraction

    Science.gov (United States)

    Wilkinson, S. J.; Hukins, D. W. L.

    1999-08-01

    Elastic scattering of X-rays can provide the following information on the fibrous protein collagen: its molecular structure, the axial arrangement of rod-like collagen molecules in a fibril, the lateral arrangement of molecules within a fibril, and the orientation of fibrils within a biological tissue. The first part of the paper reviews the principles involved in deducing this information. The second part describes a new computer program for measuring the equatorial intensity distribution, that provides information on the lateral arrangement of molecules within a fibril, and the angular distribution of the equatorial peaks that provides information on the orientation of fibrils. Orientation of fibrils within a tissue is quantified by the orientation distribution function, g( φ), which represents the probability of finding a fibril oriented between φ and φ+ δφ. The application of the program is illustrated by measurement of g( φ) for the collagen fibrils in demineralised cortical bone from cow tibia.

  11. X-ray diffractometric study on the near-surface layer structure in parallel glancing rays

    International Nuclear Information System (INIS)

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

    1988-01-01

    X-ray diffraction method is suggested to use to investigate thin films and near-surface layers under the conditions of total external reflection (TER) and in the geometry of parallel glancing rays. Experimental realization of the method using the DRON-30 diffractometer is described. Calculation for the required width of the aperture of Soller slot system is presented. The described diffraction scheme is used to investigate thin film crystal structure at glancing angles in the range from TER up to 8-10 deg. The thickness of the investigated layer in this case changes from 2.5-8 nm up to 10 3 nm. The suggested diffraction method in parallel glancing rays is especially important when investigating the films with thickness lower than 1000-2000A

  12. Redetermination of the borax structure from laboratory X-ray data at 145 K.

    Science.gov (United States)

    Gainsford, Graeme J; Kemmitt, Tim; Higham, Caleb

    2008-04-23

    THE TITLE COMPOUND, SODIUM TETRABORATE DECAHYDRATE (MINERAL NAME: borax), Na(2)[B(4)O(5)(OH)(4)]·8H(2)O, has been studied previously using X-ray [Morimoto (1956). Miner. J.2, 1-18] and neutron [Levy & Lisensky (1978). Acta Cryst. B34, 3502-3510] diffraction data. The structure contains tetra-borate anions [B(4)O(5)(OH)(4)](2-) with twofold rotation symmetry, which form hydrogen-bonded chains, and [Na(H(2)O)(6)] octa-hedra that form zigzag chains [Na(H(2)O)(4/2)(H(2)O)(2/1)]. The O-H bond distances obtained from the present redetermination at 145 K are shorter than those in the neutron study by an average of 0.127 (19) Å.

  13. Redetermination of the borax structure from laboratory X-ray data at 145 K

    Directory of Open Access Journals (Sweden)

    Caleb Higham

    2008-05-01

    Full Text Available The title compound, sodium tetraborate decahydrate (mineral name: borax, Na2[B4O5(OH4]·8H2O, has been studied previously using X-ray [Morimoto (1956. Miner. J. 2, 1–18] and neutron [Levy & Lisensky (1978. Acta Cryst. B34, 3502–3510] diffraction data. The structure contains tetraborate anions [B4O5(OH4]2− with twofold rotation symmetry, which form hydrogen-bonded chains, and [Na(H2O6] octahedra that form zigzag chains [Na(H2O4/2(H2O2/1]. The O—H bond distances obtained from the present redetermination at 145 K are shorter than those in the neutron study by an average of 0.127 (19 Å.

  14. Structural anisotropy in amorphous SnO2 film probed by X-ray absorption spectroscopy

    Science.gov (United States)

    Zhu, Q.; Ma, Q.; Buchholz, D. B.; Chang, R. P. H.; Bedzyk, M. J.; Mason, T. O.

    2013-07-01

    Polarization-dependent X-ray absorption measurements reveal the existence of structural anisotropy in amorphous (a-) SnO2 film. The anisotropy is readily seen for the second neighbor interaction whose magnitude differs along three measured directions. The differences can be well accounted for by 10%-20% variation in the Debye-Waller factor. Instead of a single Gaussian distribution found in crystalline SnO2, the Sn-O bond distribution is bimodal in a-SnO2 whose separation shows a weak angular dependence. The oxygen vacancies, existing in the a-SnO2 film in the order of 1021 cm-3, distribute preferentially along the film surface direction.

  15. Synthesis, X-ray crystal structure and theoretical calculations of antileishmanial neolignan analogues

    International Nuclear Information System (INIS)

    Nascimento, Josenaide P. do; Santos, Lourivaldo S.; Carmo, Maria Carolina L. do; Brasil, Davi S.B.; Alves, Claudio N.; Santos, Regina Helena A.; Tozzo, Erica; Ferreira, Janaina G.

    2010-01-01

    The synthesis and X-ray crystal diffraction structure of two analogues of neolignans, 2-(4-chlorophenyl)-1-phenylethanone (20) and 2-[(4-chlorophenyl)thio]-1-(3,4-dimethoxyphenyl) propan-1-one (12) is described. The compound 12 presents activity against intracellular Leishmania donovani and Leishmania amazonensis amastigotes that cause cutaneous and visceral leishmaniasis. In addition, the density functional theory (DFT) with the B3LYP hybrid functional was employed to calculate a set of molecular descriptors for nineteen synthetic analogues of neolignans with antileishmanial activities. Afterwards, the stepwise discriminant analysis was performed to investigate possible relationship between the molecular descriptors and biological activities. Through this analysis the compounds were classified into two groups active and inactive according to their degree of biological activities, and the more important properties were charges on some key atoms, electronic affinity and ClogP. (author)

  16. Some applications of nanometer scale structures for current and future X-ray space research

    DEFF Research Database (Denmark)

    Christensen, Finn Erland; Abdali, S; Frederiksen, P K

    1994-01-01

    Nanometer scale structures such as multilayers, gratings and natural crystals are playing an increasing role in spectroscopic applications for X-ray astrophysics. A few examples are briefly described as an introduction to current and planned applications pursued at the Danish Space Research...... Institute in collaboration with the FOM Institute for Plasma Physics, Nieuwegein, the Max-Planck-Institut für Extraterrestrische Physik, Aussenstelle Berlin, the Space Research Institute, Russian Academy of Sciences, the Smithsonian Astrophysical Observatory, Ovonics Synthetic Materials Company and Lawrence...... Livermore National Laboratory. These examples include : 1. the application of multilayered Si crystals for simultaneous spectroscopy in two energy bands one centred around the SK-emission near 2.45 keV and the other below the CK absorption edge at 0.284 keV; 2. the use of in-depth graded period multilayer...

  17. X-ray Crystal Structures Elucidate the Nucleotidyl Transfer Reaction of Transcript Initiation Using Two Nucleotides

    Energy Technology Data Exchange (ETDEWEB)

    M Gleghorn; E Davydova; R Basu; L Rothman-Denes; K Murakami

    2011-12-31

    We have determined the X-ray crystal structures of the pre- and postcatalytic forms of the initiation complex of bacteriophage N4 RNA polymerase that provide the complete set of atomic images depicting the process of transcript initiation by a single-subunit RNA polymerase. As observed during T7 RNA polymerase transcript elongation, substrate loading for the initiation process also drives a conformational change of the O helix, but only the correct base pairing between the +2 substrate and DNA base is able to complete the O-helix conformational transition. Substrate binding also facilitates catalytic metal binding that leads to alignment of the reactive groups of substrates for the nucleotidyl transfer reaction. Although all nucleic acid polymerases use two divalent metals for catalysis, they differ in the requirements and the timing of binding of each metal. In the case of bacteriophage RNA polymerase, we propose that catalytic metal binding is the last step before the nucleotidyl transfer reaction.

  18. Laboratory-based recording of holographic fine structure in X-ray absorption anisotropy using polycapillary optics

    Energy Technology Data Exchange (ETDEWEB)

    Dabrowski, K.M. [Institute of Physics, Jagiellonian University, Reymonta 4, 30-059 Krakow (Poland); Korecki, P., E-mail: pawel.korecki@uj.edu.pl [Institute of Physics, Jagiellonian University, Reymonta 4, 30-059 Krakow (Poland)

    2012-08-15

    Highlights: Black-Right-Pointing-Pointer Holographic fine structures in X-ray absorption recorded using a tabletop setup. Black-Right-Pointing-Pointer Setup based on polycapillary collimating optics and an HOPG crystal. Black-Right-Pointing-Pointer Demonstration of element sensitivity by detection of X-ray fluorescence. Black-Right-Pointing-Pointer Potential of laboratory-based experiments for heavily doped crystals and thin films. - Abstract: A tabletop setup composed of a collimating polycapillary optics and a highly oriented pyrolytic graphite monochromator (HOPG) was characterized and used for recording two-dimensional maps of X-ray absorption anisotropy (XAA). XAA originates from interference of X-rays directly inside the sample. Depending on experimental conditions, fine structures in XAA can be interpreted in terms of X-ray holograms or X-ray standing waves and can be used for an element selective atomic-resolved structural analysis. The implementation of polycapillary optics resulted in a two-order of magnitude gain in the radiant intensity (photons/s/solid angle) as compared to a system without optics and enabled efficient recording of XAA with a resolution of 0.15 Degree-Sign for Mo K{alpha} radiation. Element sensitivity was demonstrated by acquisition of distinct XAA signals for Ga and As atoms in a GaAs (1 1 1) wafer by using X-ray fluorescence as a secondary signal. These results indicate the possibility of performing laboratory-based XAA experiments for heavily doped single crystals or thin films. So far, because of the weak holographic modulation of XAA, such experiments could be only performed using synchrotron radiation.

  19. X-ray holographic imaging of magnetic order in meander domain structures

    Directory of Open Access Journals (Sweden)

    Jaouen Nicolas

    2013-01-01

    Full Text Available We performed x-ray holography experiments using synchrotron radiation. By analyzing the scattering of coherent circularly polarized x-rays tuned at the Co-2p resonance, we imaged perpendicular magnetic domains in a Co/Pd multilayer. We compare results obtained for continuous and laterally confined films.

  20. Simulation of x-rays in refractive structure by the Monte Carlo method using the supercomputer SKIF

    International Nuclear Information System (INIS)

    Yaskevich, Yu.R.; Kravchenko, O.I.; Soroka, I.I.; Chembrovskij, A.G.; Kolesnik, A.S.; Serikova, N.V.; Petrov, P.V.; Kol'chevskij, N.N.

    2013-01-01

    Software 'Xray-SKIF' for the simulation of the X-rays in refractive structures by the Monte-Carlo method using the supercomputer SKIF BSU are developed. The program generates a large number of rays propagated from a source to the refractive structure. The ray trajectory under assumption of geometrical optics is calculated. Absorption is calculated for each ray inside of refractive structure. Dynamic arrays are used for results of calculation rays parameters, its restore the X-ray field distributions very fast at different position of detector. It was found that increasing the number of processors leads to proportional decreasing of calculation time: simulation of 10 8 X-rays using supercomputer with the number of processors from 1 to 30 run-times equal 3 hours and 6 minutes, respectively. 10 9 X-rays are calculated by software 'Xray-SKIF' which allows to reconstruct the X-ray field after refractive structure with a special resolution of 1 micron. (authors)

  1. Evaluation of pore structures and cracking in cement paste exposed to elevated temperatures by X-ray computed tomography

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Kwang Yeom, E-mail: kimky@kict.re.kr [Korea Institute of Construction Technology, 283 Goyangdae-ro, Ilsanseo-gu, Goyang 411-712 (Korea, Republic of); Yun, Tae Sup, E-mail: taesup@yonsei.ac.kr [School of Civil and Environmental Engineering, Yonsei University, 50 Yonsei-ro, Seodaemun-gu, Seoul 120-749 (Korea, Republic of); Park, Kwang Pil, E-mail: bamtol97@kict.re.kr [Korea Institute of Construction Technology, 283 Goyangdae-ro, Ilsanseo-gu, Goyang 411-712 (Korea, Republic of)

    2013-08-15

    When cement-based materials are exposed to the high temperatures induced by fire, which can rapidly cause temperatures of over 1000 °C, the changes in pore structure and density prevail. In the present study, mortar specimens were subjected to a series of increasing temperatures to explore the temperature-dependent evolution of internal pore structure. High-performance X-ray computed tomography (CT) was used to observe the evolution of temperature-induced discontinuities at the sub-millimeter level. X-ray diffraction (XRD) and scanning electron microscopy (SEM) were employed to investigate the cause of physical changes in the heated mortar specimens. Results exhibit the changes in pore structure caused by elevated temperatures, and thermally induced fractures. We discuss the progressive formation of thermally induced fracture networks, which is a prerequisite for spalling failure of cement-based materials by fire, based on visual observations of the 3D internal structures revealed by X-ray CT.

  2. Evaluation of pore structures and cracking in cement paste exposed to elevated temperatures by X-ray computed tomography

    International Nuclear Information System (INIS)

    Kim, Kwang Yeom; Yun, Tae Sup; Park, Kwang Pil

    2013-01-01

    When cement-based materials are exposed to the high temperatures induced by fire, which can rapidly cause temperatures of over 1000 °C, the changes in pore structure and density prevail. In the present study, mortar specimens were subjected to a series of increasing temperatures to explore the temperature-dependent evolution of internal pore structure. High-performance X-ray computed tomography (CT) was used to observe the evolution of temperature-induced discontinuities at the sub-millimeter level. X-ray diffraction (XRD) and scanning electron microscopy (SEM) were employed to investigate the cause of physical changes in the heated mortar specimens. Results exhibit the changes in pore structure caused by elevated temperatures, and thermally induced fractures. We discuss the progressive formation of thermally induced fracture networks, which is a prerequisite for spalling failure of cement-based materials by fire, based on visual observations of the 3D internal structures revealed by X-ray CT

  3. X-Ray Absorption Near-Edge Structure (XANES) of Calcium L3,2 Edges of Various Calcium Compounds and X-Ray Excited Optical Luminescence (XEOL) Studies of Luminescent Calcium Compounds

    International Nuclear Information System (INIS)

    Ko, J. Y. Peter; Zhou Xingtai; Sham, T.-K.; Heigl, Franziskus; Regier, Tom; Blyth, Robert

    2007-01-01

    X-ray absorption at calcium L3,2 edges of various calcium compounds were measured using a high resolution Spherical Grating Monochromator (SGM) at the Canadian Light Source (CLS). We observe that each compound has its unique fine structure of L3,2 edges. This uniqueness is due to differences in local structure of compounds. We also performed (X-ray Excited Optical Luminescence) XEOL of selected luminescent calcium compounds to investigate their optical properties. XEOL is a photon-in-photon-out technique in which the optical luminescence that is excited by tunable x-rays from a synchrotron light source is monitored. Depending on excitation energy of the x-ray, relative intensities of luminescence peaks vary. Recent findings of the results will be presented here

  4. Higher order structure analysis of nano-materials by spectral reflectance of laser-plasma soft x-ray

    International Nuclear Information System (INIS)

    Azuma, Hirozumi; Takeichi, Akihiro; Noda, Shoji

    1995-01-01

    We have proposed a new experimental arrangement to measure spectral reflectance of nano-materials for analyzing higher order structure with laser-plasma soft x-rays. Structure modification of annealed Mo/Si multilayers and a nylon-6/clay hybrid with poor periodicity was investigated. The measurement of the spectral reflectance of soft x-rays from laser-produced plasma was found to be a useful method for the structure analysis of nano-materials, especially those of rather poor periodicity

  5. Advanced methods in X-ray and neutron structure analysis of materials

    International Nuclear Information System (INIS)

    1990-01-01

    The publication contains abstracts of 186 contributions presented at the international conference in the oral or poster form. Attention was paid particularly to crystal and molecular structures, diffraction analysis of physical phenomena, and to powder diffraction and real structures. (Z.M.)

  6. Structural investigations of LiFePO4 electrodes and in situ studies by Fe X-ray absorption spectroscopy

    International Nuclear Information System (INIS)

    Deb, Aniruddha; Bergmann, Uwe; Cramer, S.P.; Cairns, Elton J.

    2005-01-01

    Fe K-edge X-ray absorption near edge spectroscopy (XANES) and extended X-ray absorption fine structure (EXAFS) have been performed on electrodes containing LiFePO 4 to determine the local atomic and electronic structure and their stability with electrochemical cycling. A versatile electrochemical in situ cell has been constructed for long-term soft and hard X-ray experiments for the structural investigation on battery electrodes during the lithium-insertion/extraction processes. The device is used here for an X-ray absorption spectroscopic study of lithium insertion/extraction in a LiFePO 4 electrode, where the electrode contained about 7.7 mg of LiFePO 4 on a 20 μm thick Al-foil. Fe K-edge X-ray absorption near edge spectroscopy (XANES) and extended X-ray absorption fine structure (EXAFS) have been performed on this electrode to determine the local atomic and electronic structure and their stability with electrochemical cycling. The initial state (LiFePO 4 ) showed iron to be in the Fe 2+ state corresponding to the initial state (0.0 mAh) of the cell, whereas in the delithiated state (FePO 4 ) iron was found to be in the Fe 3+ state corresponding to the final charged state (3 mAh). XANES region of the XAS spectra revealed a high spin configuration for the two states (Fe (II), d 6 and Fe (III), d 5 ). The results confirm that the olivine structure of the LiFePO 4 and FePO 4 is retained by the electrodes in agreement with the XRD observations reported previously. These results confirm that LiFePO 4 cathode material retains good structural short-range order leading to superior cycling capability

  7. Local structure of metallic chips examined by X-ray microdiffraction

    International Nuclear Information System (INIS)

    Saksl, K.; Rokicki, P.; Siemers, C.; Ostroushko, D.; Bednarčík, J.; Rütt, U.

    2013-01-01

    Highlights: •We present a detailed microstructure and phase analysis of chips produced by cutting. •3D analysis proved mixed nature of shear bands propagation to the material. •We examine phase composition of the chips by focused X-ray beam. •Crystallites in segment and shear band change their orientation up to 10°. -- Abstract: Nickel-base alloys are used in high-temperature applications whenever steels or titanium alloys cannot be applied anymore. This class of alloys is furthermore used in low-temperature applications in the oil or gas industry in case the corrosion resistance of stainless steels in related liquid media is not sufficient and titanium alloys would be too expensive. Nickel-base alloys, however, due to their high strength and toughness can be machined only at low cutting speeds as otherwise poor surface quality and enhanced tool wear is observed. From all aspects influencing the machinability, the chip formation mechanism is the key factor and only a thorough understanding of this mechanism can lead to an optimisation of the cutting process. In the current study, a detailed microstructure and phase analysis of Alloy 625 chips produced in an orthogonal cutting process at conventional cutting speeds is presented. Utilising hard monochromatic X-rays focused down to micrometre size, microstructural differences between distinct structural units of the chips, namely, the segments and shear bands, are investigated. Scanning cross sections of the chips with this small beam allowed us to determine misorientation between the segments and shear bands crystal lattices which as we found are not changing abruptly but continuously, with an absolute difference up to 10°

  8. Interaction of femtosecond X-ray pulses with periodical multilayer structures

    International Nuclear Information System (INIS)

    Ksenzov, Dmitry

    2010-01-01

    The VUV Free Electron Laser FLASH operates in soft X-ray range and produces high-intensive pulse trains with few tens femtoseconds duration. The transversely fully coherent beam will open new experiments in solid state physics which can not be studied with present radiation sources. The study of the time dependent response of the multilayer to the X-ray pulse can provide insights into the process of interaction of highly intense FEL radiation with matter. To test the influence of electron excitation on the optical properties of boron carbide, the refractive index of B 4 C was measured near B K-edge by energy-resolved photon-in-photon-out method probing a Bragg reflection from periodical multilayers. The measured data clearly show that the variation of the fine structure of the Kabsorption edges due to the chemical nature of the absorber element. The knowledge obtained from experiments with continuous radiation was used to design the respective experiments with pulse from the FEL. In my thesis, it is proposed that the geometrical setup, where the incident pulse arrives from the FEL under the angle close to the 1st order ML Bragg peak, provides the most valuable information. Preliminary simulation considering form factors of neutral and ionized boron showed that due to ionization, pronounced changes in the reflectivity curve are expected. The proposed scheme can be the powerful tool to study the various processes within the electronic subsystem of the FEL pulse interaction with matter. This type of investigations gives a deep understanding of the nature of the electronic excitation and the recombination at the femtosecond scale. (orig.)

  9. Interaction of femtosecond X-ray pulses with periodical multilayer structures

    Energy Technology Data Exchange (ETDEWEB)

    Ksenzov, Dmitry

    2010-07-01

    The VUV Free Electron Laser FLASH operates in soft X-ray range and produces high-intensive pulse trains with few tens femtoseconds duration. The transversely fully coherent beam will open new experiments in solid state physics which can not be studied with present radiation sources. The study of the time dependent response of the multilayer to the X-ray pulse can provide insights into the process of interaction of highly intense FEL radiation with matter. To test the influence of electron excitation on the optical properties of boron carbide, the refractive index of B{sub 4}C was measured near B K-edge by energy-resolved photon-in-photon-out method probing a Bragg reflection from periodical multilayers. The measured data clearly show that the variation of the fine structure of the Kabsorption edges due to the chemical nature of the absorber element. The knowledge obtained from experiments with continuous radiation was used to design the respective experiments with pulse from the FEL. In my thesis, it is proposed that the geometrical setup, where the incident pulse arrives from the FEL under the angle close to the 1st order ML Bragg peak, provides the most valuable information. Preliminary simulation considering form factors of neutral and ionized boron showed that due to ionization, pronounced changes in the reflectivity curve are expected. The proposed scheme can be the powerful tool to study the various processes within the electronic subsystem of the FEL pulse interaction with matter. This type of investigations gives a deep understanding of the nature of the electronic excitation and the recombination at the femtosecond scale. (orig.)

  10. Local structure of metallic chips examined by X-ray microdiffraction

    Energy Technology Data Exchange (ETDEWEB)

    Saksl, K., E-mail: ksaksl@imr.saske.sk [Institut of Materials Research, Slovak Academy of Sciences, Watsonova 47, 040 01 Košice (Slovakia); Rokicki, P. [The Faculty of Mechanical Engineering and Aeronautics, Rzeszow University of Technology, Al. Powstancow Warszawy 12, 35-959 Rzeszow (Poland); Siemers, C. [Institut fuer Werkstoffe, Technische Universitaet Braunschweig, Langer Kamp 8, 38106 Braunschweig (Germany); Ostroushko, D. [Faculty of Metallurgy and Materials Engineering, VŠB – Technical University of Ostrava, 17.listopadu 15, 708 33 Ostrava (Czech Republic); Bednarčík, J.; Rütt, U. [HASYLAB at DESY, Notkestr. 85, D-22607 Hamburg (Germany)

    2013-12-25

    Highlights: •We present a detailed microstructure and phase analysis of chips produced by cutting. •3D analysis proved mixed nature of shear bands propagation to the material. •We examine phase composition of the chips by focused X-ray beam. •Crystallites in segment and shear band change their orientation up to 10°. -- Abstract: Nickel-base alloys are used in high-temperature applications whenever steels or titanium alloys cannot be applied anymore. This class of alloys is furthermore used in low-temperature applications in the oil or gas industry in case the corrosion resistance of stainless steels in related liquid media is not sufficient and titanium alloys would be too expensive. Nickel-base alloys, however, due to their high strength and toughness can be machined only at low cutting speeds as otherwise poor surface quality and enhanced tool wear is observed. From all aspects influencing the machinability, the chip formation mechanism is the key factor and only a thorough understanding of this mechanism can lead to an optimisation of the cutting process. In the current study, a detailed microstructure and phase analysis of Alloy 625 chips produced in an orthogonal cutting process at conventional cutting speeds is presented. Utilising hard monochromatic X-rays focused down to micrometre size, microstructural differences between distinct structural units of the chips, namely, the segments and shear bands, are investigated. Scanning cross sections of the chips with this small beam allowed us to determine misorientation between the segments and shear bands crystal lattices which as we found are not changing abruptly but continuously, with an absolute difference up to 10°.

  11. Potential application of microfocus X-ray techniques for quantitative analysis of bone structure

    International Nuclear Information System (INIS)

    Takahashi, Kenta

    2006-01-01

    With the progress of micro-focused X-ray computed tomography (micro-CT), it has become possible to evaluate the bone structure quantitatively and three-dimensionally. The advantages of micro-CT are that sample preparations are not required and that it provides not only two-dimensional parameters but also three-dimensional stereological indices. This study was carried out to evaluate the potential application of the micro-focus X-ray techniques for quantitative analysis of the new bone produced inside of a hollow chamber of the experimental titanium miniature implant. Twenty-five male wistar rats (9-weeks of age) received experimental titanium miniature implant that had a hollow chamber inside in the left side of the femur. The rats were sacrificed, then the femurs were excised at 4 weeks or 8 weeks after implantation. Micro-CT analysis was performed on the femur samples and the volume of the new bone induced in the hollow chamber of implant was calculated. Percentages of new bone area on the undecalcified histological slides were also measured, linear regression analysis was carried out. In order to evaluate the correlation between pixel numbers of undecalcified slide specimen and pixel numbers of micro-CT image. New bone formation occurred in experimental titanium miniature implant with a hollow chamber. The volume of new bone was measured by micro CT and the area percentage of new bone area against hollow chamber was calculated on the undecalcified slide. Linear regression analysis showed a high correlation between the pixel numbers of undecalcified slide specimen and pixel numbers of micro-CT image. Consequently, the new bone produced inside of the hollow chamber of the experimental titanium miniature implant could be quantified as three-dimensional stereological by micro-CT and its precision was supported by the high correlation between the measurement by micro-CT and conservative two-dimensional measurement of histological slide. (author)

  12. The equation of state of PbTiO sub 3 up to 37 GPa: a synchrotron x-ray powder diffraction study

    CERN Document Server

    Sani, A; Levy, D

    2002-01-01

    High-pressure synchrotron x-ray powder diffraction patterns were collected using ID09 of ESRF (Grenoble, France) for a powder sample of PbTiO sub 3 , placed in a diamond anvil cell. The patterns were collected at room temperature using nitrogen (up to 37 GPa) and methanol-ethanol solution (up to 7 GPa) as pressure-transmitting media. The bulk moduli were calculated for the first time using the Vinet equation of state and they were compared to those of isostructural compounds. The trend of the spontaneous polarization as a function of pressure confirms that the ferroelectric-paraelectric phase transition at 11.2 GPa possesses a second-order character.

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

    Science.gov (United States)

    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. Copyright © 2012 Elsevier B.V. All rights reserved.

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

    Energy Technology Data Exchange (ETDEWEB)

    Katsuya, Yoshio; Tanaka, Masahiko [Synchrotron X-ray Station at SPring-8, National Institute for Materials Science (NIMS), 1-1-1 Kouto, Sayo, Hyogo 679-5148 (Japan); Song, Chulho [Synchrotron X-ray Station at SPring-8, National Institute for Materials Science (NIMS), 1-1-1 Kouto, Sayo, Hyogo 679-5148 (Japan); Global Research Center for Environment and Energy based Nanomaterials Science (GREEN), Lithium Air Battery Specially Promoted Research Team, NIMS, 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan); Ito, Kimihiko; Kubo, Yoshimi [Global Research Center for Environment and Energy based Nanomaterials Science (GREEN), Lithium Air Battery Specially Promoted Research Team, NIMS, 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan); Sakata, Osami, E-mail: SAKATA.Osami@nims.go.jp [Synchrotron X-ray Station at SPring-8, National Institute for Materials Science (NIMS), 1-1-1 Kouto, Sayo, Hyogo 679-5148 (Japan); Global Research Center for Environment and Energy based Nanomaterials Science (GREEN), Lithium Air Battery Specially Promoted Research Team, NIMS, 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan); Synchrotron X-ray Group, Quantum Beam Unit, NIMS, 1-1-1 Kouto, Sayo, Hyogo 679-5148 (Japan)

    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.

  15. X-ray structure of imidazolonepropionase from Agrobacterium tumefaciens at 1.87 Å resolution

    Energy Technology Data Exchange (ETDEWEB)

    Tyagi, Rajiv; Kumaran, Desigan; Burley, Stephen K.; Swaminathan, Subramanyam (SGX); (BNL)

    2010-01-12

    Histidine degradation in Agrobacterium tumefaciens involves four enzymes, including histidase (EC 4.3.1.3), urocanase (EC 4.2.1.49), imidazolonepropionase (EC 3.5.2.7), and N-formylglutamate amidohydrolase (EC 3.5.3.8). The third enzyme of the pathway, imidazolone-propionase, a 45.6 kDa protein, catalyzes conversion of imidazolone-5-propanoate to N-forminio-L-glutamate. Initial studies of the role of imidazolonepropionase in histidine degradation were published in 1953. Subsequent publications have been limited to enzyme kinetics, crystallization, and a recently reported structure determination. The imidazolonepropionases are members of metallodepenent-hydrolases (or amidohydroase) superfamily, which includs ureases, adenosine deaminases, phosphotriesterases, dihydroorotases, allantoinases, hydantoinases, adenine and cytosine deaminases, imidazolonepropionases, aryldial-kylphosphatases, chlorohydrolases, and formylmethanofuran dehydroases. Proteins belonging to this large group share a common three-dimensional structural motif (an eightfold {alpha}/{beta} or TIM barrel) with similar active sites. Most superfamily members also share a conserved metal binding site, involving four histidine residues and one aspartic acid. Imidazolonepropionase is one of the targets selected for X-ray crystallpgrahpic structure determination by the New York Structural GenomiX Research Consortium (NYSGXRC) Target ID: 9252b to correlate the structure function relationship of poorly studied by important enzyme. Here they report the crystal structure of imidazolonepropionase from Agrobacterium tumefaciens determined at 1.87 {angstrom} resolution.

  16. Modeling the structure of RNA molecules with small-angle X-ray scattering data.

    Directory of Open Access Journals (Sweden)

    Michal Jan Gajda

    Full Text Available We propose a novel fragment assembly method for low-resolution modeling of RNA and show how it may be used along with small-angle X-ray solution scattering (SAXS data to model low-resolution structures of particles having as many as 12 independent secondary structure elements. We assessed this model-building procedure by using both artificial data on a previously proposed benchmark and publicly available data. With the artificial data, SAXS-guided models show better similarity to native structures than ROSETTA decoys. The publicly available data showed that SAXS-guided models can be used to reinterpret RNA structures previously deposited in the Protein Data Bank. Our approach allows for fast and efficient building of de novo models of RNA using approximate secondary structures that can be readily obtained from existing bioinformatic approaches. We also offer a rigorous assessment of the resolving power of SAXS in the case of small RNA structures, along with a small multimetric benchmark of the proposed method.

  17. Structural evaluation of an amyloid fibril model using small-angle x-ray scattering

    Science.gov (United States)

    Dahal, Eshan; Choi, Mina; Alam, Nadia; Bhirde, Ashwinkumar A.; Beaucage, Serge L.; Badano, Aldo

    2017-08-01

    Amyloid fibrils are highly structured protein aggregates associated with a wide range of diseases including Alzheimer’s and Parkinson’s. We report a structural investigation of an amyloid fibril model prepared from a commonly used plasma protein (bovine serum albumin (BSA)) using small-angle x-ray scattering (SAXS) technique. As a reference, the size estimates from SAXS are compared to dynamic light scattering (DLS) data and the presence of amyloid-like fibrils is confirmed using Congo red absorbance assay. Our SAXS results consistently show the structural transformation of BSA from spheroid to rod-like elongated structures during the fibril formation process. We observe the elongation of fibrils over two months with fibril length growing from 35.9  ±  3.0 nm to 51.5  ±  2.1 nm. Structurally metastable fibrils with distinct SAXS profiles have been identified. As proof of concept, we demonstrate the use of such distinct SAXS profiles to detect fibrils in the mixture solutions of two species by estimating their volume fractions. This easily detectable and well-characterized amyloid fibril model from BSA can be readily used as a control or standard reference to further investigate SAXS applications in the detection of structurally diverse amyloid fibrils associated with protein aggregation diseases.

  18. Dehydrogenation kinetics of pure and nickel-doped magnesium hydride investigated by in situ time-resolved powder X-ray diffraction

    DEFF Research Database (Denmark)

    Jensen, T.R.; Andreasen, A.; Vegge, Tejs

    2006-01-01

    The dehydrogenation kinetics of pure and nickel (Ni)-doped (2w/w%) magnesium hydride (MgH2) have been investigated by in situ time-resolved powder X-ray diffraction (PXD). Deactivated samples, i.e. air exposed, are investigated in order to focus on the effect of magnesium oxide (MgO) surface layers......, which might be unavoidable for magnesium (Mg)-based storage media for mobile applications. A curved position-sensitive detector covering 120 degrees in 20 and a rotating anode X-ray source provide a time resolution of 45 s and up to 90 powder pattems collected during an experiment under isothermal...... by the Johnson-Mehi-Avrami formalism in order to derive rate constants at different temperatures. The apparent activation energies for dehydrogenation of pure and Ni-doped magnesium hydride were E-A approximate to 300 and 250 kJ/mol, respectively. Differential scanning calorimetry gave, E-A = 270 k...

  19. In situ X-ray powder diffraction studies of the synthesis of graphene oxide and formation of reduced graphene oxide

    International Nuclear Information System (INIS)

    Storm, Mie Møller; Johnsen, Rune E.; Norby, Poul

    2016-01-01

    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. - Graphical abstract: In situ X-ray diffraction results for of the modified Hummers synthesis and the thermal reduction of graphene oxide, revealing three stages for both syntheses as well as new GO diffraction peaks and unidentified crystalline material for the Hummers synthesis and a disordered stage for the thermal reduction of graphene oxide. Display Omitted - Highlights: • Hummers synthesis consists of three stages: dissolution, intercalation and crystal. • GO is produced early on during the synthesis and display new diffraction peaks. • An unidentified triclinic phase is observed for the Hummers synthesis. • Thermal reduction of GO display three stages: GO, a disordered stage and rGO. • In situ XRD indicate reformation of rGO even for fast heated thermal reduction.

  20. In situ X-ray powder diffraction studies of the synthesis of graphene oxide and formation of reduced graphene oxide

    Energy Technology Data Exchange (ETDEWEB)

    Storm, Mie Møller, E-mail: mmst@dtu.dk; Johnsen, Rune E.; Norby, Poul

    2016-08-15

    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. - Graphical abstract: In situ X-ray diffraction results for of the modified Hummers synthesis and the thermal reduction of graphene oxide, revealing three stages for both syntheses as well as new GO diffraction peaks and unidentified crystalline material for the Hummers synthesis and a disordered stage for the thermal reduction of graphene oxide. Display Omitted - Highlights: • Hummers synthesis consists of three stages: dissolution, intercalation and crystal. • GO is produced early on during the synthesis and display new diffraction peaks. • An unidentified triclinic phase is observed for the Hummers synthesis. • Thermal reduction of GO display three stages: GO, a disordered stage and rGO. • In situ XRD indicate reformation of rGO even for fast heated thermal reduction.