WorldWideScience

Sample records for aqueous solution x-ray

  1. Investigation of the Ionic Hydration in Aqueous Salt Solutions by Soft X-ray Emission Spectroscopy.

    Science.gov (United States)

    Jeyachandran, Y L; Meyer, F; Benkert, A; Bär, M; Blum, M; Yang, W; Reinert, F; Heske, C; Weinhardt, L; Zharnikov, M

    2016-08-11

    Understanding the molecular structure of the hydration shells and their impact on the hydrogen bond (HB) network of water in aqueous salt solutions is a fundamentally important and technically relevant question. In the present work, such hydration effects were studied for a series of representative salt solutions (NaCl, KCl, CaCl2, MgCl2, and KBr) by soft X-ray emission spectroscopy (XES) and resonant inelastic soft X-ray scattering (RIXS). The oxygen K-edge XES spectra could be described with three components, attributed to initial state HB configurations in pure water, water molecules that have undergone an ultrafast dissociation initiated by the X-ray excitation, and water molecules in contact with salt ions. The behavior of the individual components, as well as the spectral shape of the latter component, has been analyzed in detail. In view of the role of ions in such effects as protein denaturation (i.e., the Hofmeister series), we discuss the ion-specific nature of the hydration shells and find that the results point to a predominant role of anions as compared to cations. Furthermore, we observe a concentration-dependent suppression of ultrafast dissociation in all salt solutions, associated with a significant distortion of intact HB configurations of water molecules facilitating such a dissociation. PMID:27442708

  2. Structure of MgSO4 in Concentrated Aqueous Solutions by X-Ray Diffraction

    Institute of Scientific and Technical Information of China (English)

    CAO Ling-di; FANG Yan; FANG Chun-hui

    2011-01-01

    Detailed time-and-space-averaged structure of MgSO4 in the concentrated aqueous solutions was investigated via X-ray diffraction with an X'pert Pro θ-θ diffractometer at 298 K, yielding structural function and radial distribution function(RDF). The developed KURVLR program was employed for the theoretical investigation in consideration of the ionic hydration and ion association. Multi-peaks Gaussian fitting method was applied to deconvolving the overlapping bands of Differential radial distribution function(DRDF). The calculation of the geometric model shows that octahedrally six-coordinated Mg(H2O)62+, with an Mg2+…Ow bond length of 0.201 nm dominates in the solutions. There exists contact ion-pair(CIP) in the more concentrated solution(1:18, H2O/salt molar ratio) with a coordination number of 0.8 and a characteristic Mg…S distance of 0.340 nm. The result indicates the hydrated SO42ion happens in the solution. The S…Ow bond distance was determined to be 0.382 nm with a coordination number of 13. The fraction of CIP increases significantly with the increasing concentration. The symmetry of the hydration structure of sulfate ion is lowered by forming complex with magnesium ion.

  3. Quantitative interpretation of molecular dynamics simulations for X-ray photoelectron spectroscopy of aqueous solutions

    Science.gov (United States)

    Olivieri, Giorgia; Parry, Krista M.; Powell, Cedric J.; Tobias, Douglas J.; Brown, Matthew A.

    2016-04-01

    Over the past decade, energy-dependent ambient pressure X-ray photoelectron spectroscopy (XPS) has emerged as a powerful analytical probe of the ion spatial distributions at the vapor (vacuum)-aqueous electrolyte interface. These experiments are often paired with complementary molecular dynamics (MD) simulations in an attempt to provide a complete description of the liquid interface. There is, however, no systematic protocol that permits a straightforward comparison of the two sets of results. XPS is an integrated technique that averages signals from multiple layers in a solution even at the lowest photoelectron kinetic energies routinely employed, whereas MD simulations provide a microscopic layer-by-layer description of the solution composition near the interface. Here, we use the National Institute of Standards and Technology database for the Simulation of Electron Spectra for Surface Analysis (SESSA) to quantitatively interpret atom-density profiles from MD simulations for XPS signal intensities using sodium and potassium iodide solutions as examples. We show that electron inelastic mean free paths calculated from a semi-empirical formula depend strongly on solution composition, varying by up to 30% between pure water and concentrated NaI. The XPS signal thus arises from different information depths in different solutions for a fixed photoelectron kinetic energy. XPS signal intensities are calculated using SESSA as a function of photoelectron kinetic energy (probe depth) and compared with a widely employed ad hoc method. SESSA simulations illustrate the importance of accounting for elastic-scattering events at low photoelectron kinetic energies (<300 eV) where the ad hoc method systematically underestimates the preferential enhancement of anions over cations. Finally, some technical aspects of applying SESSA to liquid interfaces are discussed.

  4. Soft X-ray absorption spectra of aqueous salt solutions with highly charged cations in liquid microjets

    Energy Technology Data Exchange (ETDEWEB)

    Schwartz, Craig P.; Uejio, Janel S.; Duffin, Andrew M.; Drisdell, Walter S.; Smith, Jared D.; Saykally, Richard J.

    2010-03-11

    X-ray absorption spectra of 1M aqueous solutions of indium (III) chloride, yttrium (III) bromide, lanthanum (III) chloride, tin (IV) chloride and chromium (III) chloride have been measured at the oxygen K-edge. Relatively minor changes are observed in the spectra compared to that of pure water. SnCl{sub 4} and CrCl{sub 3} exhibit a new onset feature which is attributed to formation of hydroxide or other complex molecules in the solution. At higher energy, only relatively minor, but salt-specific changes in the spectra occur. The small magnitude of the observed spectral changes is ascribed to offsetting perturbations by the cations and anions.

  5. Joint Analysis of Radiative and Non-Radiative Electronic Relaxation Upon X-ray Irradiation of Transition Metal Aqueous Solutions

    Science.gov (United States)

    Golnak, Ronny; Bokarev, Sergey I.; Seidel, Robert; Xiao, Jie; Grell, Gilbert; Atak, Kaan; Unger, Isaak; Thürmer, Stephan; Aziz, Saadullah G.; Kühn, Oliver; Winter, Bernd; Aziz, Emad F.

    2016-04-01

    L-edge soft X-ray spectroscopy has been proven to be a powerful tool to unravel the peculiarities of electronic structure of transition metal compounds in solution. However, the X-ray absorption spectrum is often probed in the total or partial fluorescence yield modes, what leads to inherent distortions with respect to the true transmission spectrum. In the present work, we combine photon- and electron-yield experimental techniques with multi-reference first principles calculations. Exemplified for the prototypical FeCl2 aqueous solution we demonstrate that the partial yield arising from the Fe3s → 2p relaxation is a more reliable probe of the absorption spectrum than the Fe3d → 2p one. For the bonding-relevant 3d → 2p channel we further provide the basis for the joint analysis of resonant photoelectron and inelastic X-ray scattering spectra. Establishing the common energy reference allows to assign both spectra using the complementary information provided through electron-out and photon-out events.

  6. Practical guidelines for best practice on Total Reflection X-ray Fluorescence spectroscopy: Analysis of aqueous solutions

    Science.gov (United States)

    Riaño, Sofía; Regadío, Mercedes; Binnemans, Koen; Vander Hoogerstraete, Tom

    2016-10-01

    Despite the fact that Total Reflection X-ray Fluorescence (TXRF) is becoming more and more popular as a quantification technique in analytical chemistry due to its simplicity and robustness, there are still some key aspects related to the sample preparation that need to be improved. In this work, the effect of different parameters is investigated: measurement time, carrier position, sample volume and sample drying time. The measurement time and the sample volume on the carriers mainly affect the recovery rate and relative standard deviation of the quantified metal from aqueous solutions. The most important parameters that play a fundamental role in the calibration of a TXRF machine such as choice of the standard element and concentration ratio between the analyte and the standard are discussed. Practical and easy guidelines for the correct preparation of aqueous samples are presented. These can be used by both less and more experienced TXRF users, interested in measuring metal ion concentrations in aqueous samples.

  7. Joint Analysis of Radiative and Non-Radiative Electronic Relaxation Upon X-ray Irradiation of Transition Metal Aqueous Solutions

    OpenAIRE

    Ronny Golnak; Sergey I. Bokarev; Robert Seidel; Jie Xiao; Gilbert Grell; Kaan Atak; Isaak Unger; Stephan Thürmer; Saadullah G. Aziz; Oliver Kühn; Bernd Winter; Emad F. Aziz

    2016-01-01

    L-edge soft X-ray spectroscopy has been proven to be a powerful tool to unravel the peculiarities of electronic structure of transition metal compounds in solution. However, the X-ray absorption spectrum is often probed in the total or partial fluorescence yield modes, what leads to inherent distortions with respect to the true transmission spectrum. In the present work, we combine photon- and electron-yield experimental techniques with multi-reference first principles calculations. Exemplifi...

  8. Joint analysis of radiative and non-radiative electronic relaxation upon X-ray irradiation of transition metal aqueous solutions

    OpenAIRE

    Golnak, Ronny; Sergey I. Bokarev; Seidel, Robert; Xiao, Jie; Grell, Gilbert; Atak, Kaan; Unger, Isaak; Thürmer, Stephan; Saadullah G. Aziz; Kühn, Oliver; Winter, Bernd; Emad F. Aziz

    2016-01-01

    L-edge soft X-ray spectroscopy has been proven to be a powerful tool to unravel the peculiarities of electronic structure of transition metal compounds in solution. However, the X-ray absorption spectrum is often probed in the total or partial fluorescence yield modes, what leads to inherent distortions with respect to the true transmission spectrum. In the present work, we combine photon- and electron-yield experimental techniques with multi-reference first principles calculations. Exemplifi...

  9. X-ray absorption microscopy of aqueous samples

    Science.gov (United States)

    Frazer, Brad; Gilbert, Benjamin; De Stasio, Gelsomina

    2002-03-01

    X-ray photoelectron emission microscopy (X-PEEM) is used for numerous applications in surface microchemical analysis of material science and biological specimens. We have reconfigured the MEPHISTO X-PEEM instrument that is installed at the University of Wisconsin Synchrotron Radiation Center to measure true x-ray transmission spectra by converting transmitted photons to photoelectrons via a thin photocathode layer of gold. We have also developed a method by which to introduce aqueous samples into ultrahigh vacuum. Hence x-ray spectroscopy can be performed on biologically relevant elements (such as K, Ca, etc.) in a physiological environment, i.e., in solution. More important, when coupled with X-PEEM imaging this technique may offer the unique and exciting possibility of studying living cells. We present initial x-ray absorption spectra of solutions of aqueous ionic and chelated Ca, with the aim of distinguishing bound and free ionic calcium in vivo.

  10. Synchrotron-based in situ soft X-ray microscopy of Ag corrosion in aqueous chloride solution

    Science.gov (United States)

    Bozzini, B.; D'Urzo, L.; Gianoncelli, A.; Kaulich, B.; Kiskinova, M.; Prasciolu, M.; Tadjeddine, A.

    2009-09-01

    In this paper we report an in situ X-ray microscopy study of a model metal electrochemistry system, incorporating faradaic reactivity: the anodic corrosion and cathodic electrodeposition of Ag in aqueous systems. The information at sub-μm scale about morpho-chemical evolution of the electrified interface, provided by this novel electroanalytical approach fosters fundamental understanding of important issues concerning material fabrication and stability, which are crucial in developing the next generation electrochemical technologies, such as fuel cells and biosensors. The key methodology challenge faced in this pilot electrochemical experiments is combining a three-electrode configuration and wet environment, which required metal electrodes suitable for transmitting soft X-rays and a sealed cell allowing working in high vacuum. This has been solved via lithographic fabrication route fabricating 75 nm thick Ag electrodes and using Si3N4 membranes as X-ray windows and electrode support. Imaging in the STXM mode with phase contrast allowed us to monitor the corrosion morphologies and metal outgrowth features. Localised thickness variation and the build-up of reaction products of electron density different from that of the starting material have been detected with high sensitivity.

  11. Synchrotron-based in situ soft X-ray microscopy of Ag corrosion in aqueous chloride solution

    Energy Technology Data Exchange (ETDEWEB)

    Bozzini, B; D' Urzo, L [Dipartimento di Ingegneria dell' Innovazione, Universita del Salento, via Monteroni, 73100 Lecce (Italy); Gianoncelli, A; Kaulich, B; Kiskinova, M [Sincrotrone Trieste S.C.p.A., ELETTRA, s.s. 14 km 163.5 in Area Science Park, 34012 Basovizza, Trieste (Italy); Prasciolu, M [CNR-INFM TASC National Laboratory S.S.14 Km 163.5, Area Science Park, 34012 Basovizza, Trieste (Italy); Tadjeddine, A, E-mail: alessandra.gianoncelli@elettra.trieste.i [3UDIL/CNRS, BP34 91898 Orsay Cedex (France)

    2009-09-01

    In this paper we report an in situ X-ray microscopy study of a model metal electrochemistry system, incorporating faradaic reactivity: the anodic corrosion and cathodic electrodeposition of Ag in aqueous systems. The information at sub-{mu}m scale about morpho-chemical evolution of the electrified interface, provided by this novel electroanalytical approach fosters fundamental understanding of important issues concerning material fabrication and stability, which are crucial in developing the next generation electrochemical technologies, such as fuel cells and biosensors. The key methodology challenge faced in this pilot electrochemical experiments is combining a three-electrode configuration and wet environment, which required metal electrodes suitable for transmitting soft X-rays and a sealed cell allowing working in high vacuum. This has been solved via lithographic fabrication route fabricating 75 nm thick Ag electrodes and using Si{sub 3}N{sub 4} membranes as X-ray windows and electrode support. Imaging in the STXM mode with phase contrast allowed us to monitor the corrosion morphologies and metal outgrowth features. Localised thickness variation and the build-up of reaction products of electron density different from that of the starting material have been detected with high sensitivity.

  12. Electron transfer during selenium reduction by iron surfaces in aqueous solution: High resolution X-ray absorption study

    Science.gov (United States)

    Kvashnina, K. O.; Butorin, S. M.; Cui, D.; Vegelius, J.; Puranen, A.; Gens, R.; Glatzel, P.

    2009-11-01

    We present a study of selenate (SeO42-) on an iron surface in ground water solution by X-ray absorption near-edge spectroscopy. Spectral sharpening is obtained by using the high energy resolution fluorescence detection technique that also efficiently suppresses the strong fluorescence signal from the Fe surface in the highly dilute samples (Se concentration < 3 ppm). We observe fully reduced Se on polished Fe surfaces while no changes are found for Se on oxidized Fe surface.

  13. Ultraviolet photochemical reaction of [Fe(III)(C2O4)3](3-) in aqueous solutions studied by femtosecond time-resolved X-ray absorption spectroscopy using an X-ray free electron laser.

    Science.gov (United States)

    Ogi, Y; Obara, Y; Katayama, T; Suzuki, Y-I; Liu, S Y; Bartlett, N C-M; Kurahashi, N; Karashima, S; Togashi, T; Inubushi, Y; Ogawa, K; Owada, S; Rubešová, M; Yabashi, M; Misawa, K; Slavíček, P; Suzuki, T

    2015-05-01

    Time-resolved X-ray absorption spectroscopy was performed for aqueous ammonium iron(III) oxalate trihydrate solutions using an X-ray free electron laser and a synchronized ultraviolet laser. The spectral and time resolutions of the experiment were 1.3 eV and 200 fs, respectively. A femtosecond 268 nm pulse was employed to excite [Fe(III)(C2O4)3](3-) in solution from the high-spin ground electronic state to ligand-to-metal charge transfer state(s), and the subsequent dynamics were studied by observing the time-evolution of the X-ray absorption spectrum near the Fe K-edge. Upon 268 nm photoexcitation, the Fe K-edge underwent a red-shift by more than 4 eV within 140 fs; however, the magnitude of the redshift subsequently diminished within 3 ps. The Fe K-edge of the photoproduct remained lower in energy than that of [Fe(III)(C2O4)3](3-). The observed red-shift of the Fe K-edge and the spectral feature of the product indicate that Fe(III) is upon excitation immediately photoreduced to Fe(II), followed by ligand dissociation from Fe(II). Based on a comparison of the X-ray absorption spectra with density functional theory calculations, we propose that the dissociation proceeds in two steps, forming first [(CO2 (•))Fe(II)(C2O4)2](3-) and subsequently [Fe(II)(C2O4)2](2-).

  14. Ultraviolet photochemical reaction of [Fe(III(C2O43]3− in aqueous solutions studied by femtosecond time-resolved X-ray absorption spectroscopy using an X-ray free electron laser

    Directory of Open Access Journals (Sweden)

    Y. Ogi

    2015-05-01

    Full Text Available Time-resolved X-ray absorption spectroscopy was performed for aqueous ammonium iron(III oxalate trihydrate solutions using an X-ray free electron laser and a synchronized ultraviolet laser. The spectral and time resolutions of the experiment were 1.3 eV and 200 fs, respectively. A femtosecond 268 nm pulse was employed to excite [Fe(III(C2O43]3− in solution from the high-spin ground electronic state to ligand-to-metal charge transfer state(s, and the subsequent dynamics were studied by observing the time-evolution of the X-ray absorption spectrum near the Fe K-edge. Upon 268 nm photoexcitation, the Fe K-edge underwent a red-shift by more than 4 eV within 140 fs; however, the magnitude of the redshift subsequently diminished within 3 ps. The Fe K-edge of the photoproduct remained lower in energy than that of [Fe(III(C2O43]3−. The observed red-shift of the Fe K-edge and the spectral feature of the product indicate that Fe(III is upon excitation immediately photoreduced to Fe(II, followed by ligand dissociation from Fe(II. Based on a comparison of the X-ray absorption spectra with density functional theory calculations, we propose that the dissociation proceeds in two steps, forming first [(CO2•Fe(II(C2O42]3− and subsequently [Fe(II(C2O42]2−.

  15. Crystalline self-assembly of organic molecules with metal ions at the air-aqueous solution interface. A grazing incidence X-ray scattering study

    DEFF Research Database (Denmark)

    Weissbuch, I.; Buller, R.; Kjær, K.;

    2002-01-01

    The advent of intense X-rays from synchrotron sources made possible to probe, at the molecular level, the structural aspects of self-assemblies generated at interfaces. Here we present the two-dimensional (2-D) packing arrangements of two-, three- and multi-component organo-metallic self-assembli...... amphiphiles; organization of ionophores in the presence of metal ions in membrane-like environment; self-assembly of 2 x 2 and 3 x 3 silver(I) grid-type complexes generated at the air-solution interface. (C) 2002 Elsevier Science B.V. All rights reserved.......-assemblies formed via interfacial reaction at the air-aqueous solution interface, as determined by grazing incidence X-ray diffraction (GIRD) and X-ray specular reflectivity techniques. GIXD yields structural information on the crystalline part of the Langmuir film, including the ions and counterions lateral order....... Specular reflectivity yields the electron density profile of the film in the direction normal to the air-solution interface and, by modeling, gives independent information on the structure of both crystalline and amorphous parts of the film. In particular, we focus on the following systems: ordering...

  16. In situ soft X-ray absorption spectroscopy investigation of electrochemical corrosion of copper in aqueous NaHCO3 solution

    Energy Technology Data Exchange (ETDEWEB)

    Jiang, Peng; Chen, Jeng-Lung; Borondics, Ferenc; Glans, Per-Anders; West, Mark W.; Chang, Ching-Lin; Salmeron, Miquel; Guo, Jinghua

    2010-03-31

    A novel electrochemical setup has been developed for soft x-ray absorption studies of the electronic structure of electrode materials during electrochemical cycling. In this communication we illustrate the operation of the cell with a study of the corrosion behavior of copper in aqueous NaHCO3 solution via the electrochemically induced changes of its electronic structure. This development opens the way for in situ investigations of electrochemical processes, photovoltaics, batteries, fuel cells, water splitting, corrosion, electrodeposition, and a variety of important biological processes.

  17. Nitrogen K-edge X-ray absorption near edge structure (XANES) spectra of purine-containing nucleotides in aqueous solution

    Science.gov (United States)

    Shimada, Hiroyuki; Fukao, Taishi; Minami, Hirotake; Ukai, Masatoshi; Fujii, Kentaro; Yokoya, Akinari; Fukuda, Yoshihiro; Saitoh, Yuji

    2014-08-01

    The N K-edge X-ray absorption near edge structure (XANES) spectra of the purine-containing nucleotide, guanosine 5'-monophosphate (GMP), in aqueous solution are measured under various pH conditions. The spectra show characteristic peaks, which originate from resonant excitations of N 1s electrons to π* orbitals inside the guanine moiety of GMP. The relative intensities of these peaks depend on the pH values of the solution. The pH dependence is explained by the core-level shift of N atoms at specific sites caused by protonation and deprotonation. The experimental spectra are compared with theoretical spectra calculated by using density functional theory for GMP and the other purine-containing nucleotides, adenosine 5'-monophosphate, and adenosine 5'-triphosphate. The N K-edge XANES spectra for all of these nucleotides are classified by the numbers of N atoms with particular chemical bonding characteristics in the purine moiety.

  18. An investigation into the subambient behavior of aqueous mannitol solutions using differential scanning calorimetry, cold stage microscopy, and X-ray diffractometry.

    Science.gov (United States)

    Kett, Vicky L; Fitzpatrick, Shaun; Cooper, Brett; Craig, Duncan Q M

    2003-09-01

    The subambient behavior of aqueous mannitol solutions is of considerable relevance to the preparation of freeze dried formulations. In this investigation the properties of 3% w/v mannitol solutions were investigated using differential scanning calorimetry (DSC), cold stage microscopy (CSM), and X-ray diffraction (XRD) to identify the thermal transitions and structural transformations undergone by this system. It was found that on cooling from ambient the system formed ice at circa -20 degrees C while a further exotherm was seen at approximately -30 degrees C. Upon reheating an endotherm was seen at circa -30 degrees C followed immediately by an exotherm at circa -25 degrees C. Temperature cycling indicated that the thermal transitions observed upon reheating were not reversible. Modulated temperature DSC (MTDSC) indicated that the transitions observed upon reheating corresponded to a glass transition immediately followed by recrystallization, XRD data showed that recrystallization was into the beta form. Annealing at -35 degrees C for 40 min prior to cooling and reheating resulted in a maximum enthalpy being observed for the reheating exotherm. It is concluded that on cooling 3% w/v aqueous mannitol solutions an amorphous phase is formed that subsequently recrystallises into the beta form. The study has also shown that DSC, CSM, and XRD are useful complementary techniques for the study of frozen systems.

  19. Competition between organics and bromide at the aqueous solution-air interface as seen from ozone uptake kinetics and X-ray photoelectron spectroscopy.

    Science.gov (United States)

    Lee, Ming-Tao; Brown, Matthew A; Kato, Shunsuke; Kleibert, Armin; Türler, Andreas; Ammann, Markus

    2015-05-14

    A more detailed understanding of the heterogeneous chemistry of halogenated species in the marine boundary layer is required. Here, we studied the reaction of ozone (O3) with NaBr solutions in the presence and absence of citric acid (C6H8O7) under ambient conditions. Citric acid is used as a proxy for oxidized organic material present at the ocean surface or in sea spray aerosol. On neat NaBr solutions, the observed kinetics is consistent with bulk reaction-limited uptake, and a second-order rate constant for the reaction of O3 + Br(-) is 57 ± 10 M(-1) s(-1). On mixed NaBr-citric acid aqueous solutions, the uptake kinetics was faster than that predicted by bulk reaction-limited uptake and also faster than expected based on an acid-catalyzed mechanism. X-ray photoelectron spectroscopy (XPS) on a liquid microjet of the same solutions at 1.0 × 10(-3)-1.0 × 10(-4) mbar was used to obtain quantitative insight into the interfacial composition relative to that of the bulk solutions. It revealed that the bromide anion becomes depleted by 30 ± 10% while the sodium cation gets enhanced by 40 ± 20% at the aqueous solution-air interface of a 0.12 M NaBr solution mixed with 2.5 M citric acid in the bulk, attributed to the role of citric acid as a weak surfactant. Therefore, the enhanced reactivity of bromide solutions observed in the presence of citric acid is not necessarily attributable to a surface reaction but could also result from an increased solubility of ozone at higher citric acid concentrations. Whether the acid-catalyzed chemistry may have a larger effect on the surface than in the bulk to offset the effect of bromide depletion also remains open.

  20. EPR-Spin Trapping and Flow Cytometric Studies of Free Radicals Generated Using Cold Atmospheric Argon Plasma and X-Ray Irradiation in Aqueous Solutions and Intracellular Milieu.

    Directory of Open Access Journals (Sweden)

    Hidefumi Uchiyama

    Full Text Available Electron paramagnetic resonance (EPR-spin trapping and flow cytometry were used to identify free radicals generated using argon-cold atmospheric plasma (Ar-CAP in aqueous solutions and intracellularly in comparison with those generated by X-irradiation. Ar-CAP was generated using a high-voltage power supply unit with low-frequency excitation. The characteristics of Ar-CAP were estimated by vacuum UV absorption and emission spectra measurements. Hydroxyl (·OH radicals and hydrogen (H atoms in aqueous solutions were identified with the spin traps 5,5-dimethyl-1-pyrroline N-oxide (DMPO, 3,3,5,5-tetramethyl-1-pyrroline-N-oxide (M4PO, and phenyl N-t-butylnitrone (PBN. The occurrence of Ar-CAP-induced pyrolysis was evaluated using the spin trap 3,5-dibromo-4-nitrosobenzene sulfonate (DBNBS in aqueous solutions of DNA constituents, sodium acetate, and L-alanine. Human lymphoma U937 cells were used to study intracellular oxidative stress using five fluorescent probes with different affinities to a number of reactive species. The analysis and quantification of EPR spectra revealed the formation of enormous amounts of ·OH radicals using Ar-CAP compared with that by X-irradiation. Very small amounts of H atoms were detected whereas nitric oxide was not found. The formation of ·OH radicals depended on the type of rare gas used and the yield correlated inversely with ionization energy in the order of krypton > argon = neon > helium. No pyrolysis radicals were detected in aqueous solutions exposed to Ar-CAP. Intracellularly, ·OH, H2O2, which is the recombination product of ·OH, and OCl- were the most likely formed reactive oxygen species after exposure to Ar-CAP. Intracellularly, there was no practical evidence for the formation of NO whereas very small amounts of superoxides were formed. Despite the superiority of Ar-CAP in forming ·OH radicals, the exposure to X-rays proved more lethal. The mechanism of free radical formation in aqueous solutions and

  1. EPR-Spin Trapping and Flow Cytometric Studies of Free Radicals Generated Using Cold Atmospheric Argon Plasma and X-Ray Irradiation in Aqueous Solutions and Intracellular Milieu.

    Science.gov (United States)

    Uchiyama, Hidefumi; Zhao, Qing-Li; Hassan, Mariame Ali; Andocs, Gabor; Nojima, Nobuyuki; Takeda, Keigo; Ishikawa, Kenji; Hori, Masaru; Kondo, Takashi

    2015-01-01

    Electron paramagnetic resonance (EPR)-spin trapping and flow cytometry were used to identify free radicals generated using argon-cold atmospheric plasma (Ar-CAP) in aqueous solutions and intracellularly in comparison with those generated by X-irradiation. Ar-CAP was generated using a high-voltage power supply unit with low-frequency excitation. The characteristics of Ar-CAP were estimated by vacuum UV absorption and emission spectra measurements. Hydroxyl (·OH) radicals and hydrogen (H) atoms in aqueous solutions were identified with the spin traps 5,5-dimethyl-1-pyrroline N-oxide (DMPO), 3,3,5,5-tetramethyl-1-pyrroline-N-oxide (M4PO), and phenyl N-t-butylnitrone (PBN). The occurrence of Ar-CAP-induced pyrolysis was evaluated using the spin trap 3,5-dibromo-4-nitrosobenzene sulfonate (DBNBS) in aqueous solutions of DNA constituents, sodium acetate, and L-alanine. Human lymphoma U937 cells were used to study intracellular oxidative stress using five fluorescent probes with different affinities to a number of reactive species. The analysis and quantification of EPR spectra revealed the formation of enormous amounts of ·OH radicals using Ar-CAP compared with that by X-irradiation. Very small amounts of H atoms were detected whereas nitric oxide was not found. The formation of ·OH radicals depended on the type of rare gas used and the yield correlated inversely with ionization energy in the order of krypton > argon = neon > helium. No pyrolysis radicals were detected in aqueous solutions exposed to Ar-CAP. Intracellularly, ·OH, H2O2, which is the recombination product of ·OH, and OCl- were the most likely formed reactive oxygen species after exposure to Ar-CAP. Intracellularly, there was no practical evidence for the formation of NO whereas very small amounts of superoxides were formed. Despite the superiority of Ar-CAP in forming ·OH radicals, the exposure to X-rays proved more lethal. The mechanism of free radical formation in aqueous solutions and an

  2. Nitrogen K-edge X-ray absorption near edge structure (XANES) spectra of purine-containing nucleotides in aqueous solution

    Energy Technology Data Exchange (ETDEWEB)

    Shimada, Hiroyuki; Fukao, Taishi; Minami, Hirotake; Ukai, Masatoshi [Department of Applied Physics, Tokyo University of Agriculture and Technology, Koganei-shi, Tokyo 184-8588 (Japan); Fujii, Kentaro; Yokoya, Akinari [Advanced Science Research Center, Japan Atomic Energy Agency, Tokai-mura, Naka-gun, Ibaraki 319-1195 (Japan); Fukuda, Yoshihiro; Saitoh, Yuji [Synchrotron Radiation Research Center, Japan Atomic Energy Agency, Sayo-gun, Hyougo 679-5148 (Japan)

    2014-08-07

    The N K-edge X-ray absorption near edge structure (XANES) spectra of the purine-containing nucleotide, guanosine 5{sup ′}-monophosphate (GMP), in aqueous solution are measured under various pH conditions. The spectra show characteristic peaks, which originate from resonant excitations of N 1s electrons to π* orbitals inside the guanine moiety of GMP. The relative intensities of these peaks depend on the pH values of the solution. The pH dependence is explained by the core-level shift of N atoms at specific sites caused by protonation and deprotonation. The experimental spectra are compared with theoretical spectra calculated by using density functional theory for GMP and the other purine-containing nucleotides, adenosine 5{sup ′}-monophosphate, and adenosine 5{sup ′}-triphosphate. The N K-edge XANES spectra for all of these nucleotides are classified by the numbers of N atoms with particular chemical bonding characteristics in the purine moiety.

  3. Antimony(III) complexing with O-bearing organic ligands in aqueous solution: An X-ray absorption fine structure spectroscopy and solubility study

    Science.gov (United States)

    Tella, Marie; Pokrovski, Gleb S.

    2009-01-01

    The stability and structure of aqueous complexes formed by trivalent antimony (Sb III) with carboxylic acids (acetic, adipic, malonic, lactic, oxalic, tartaric, and citric acid), phenols (catechol), and amino acids (glycine) having O- and N-functional groups (carboxyl, alcoholic hydroxyl, phenolic hydroxyl and amine) typical of natural organic matter, were determined at 20 and 60 °C from solubility and X-ray absorption fine structure (XAFS) spectroscopy measurements. In organic-free aqueous solutions and in the presence of acetic, adipic, malonic acids and glycine, both spectroscopic and solubility data are consistent with the dominant formation of Sb III hydroxide species, Sb(OH)3-nn+,Sb(OH)30andSb(OH)4-, at strongly acid, acid-to-neutral and basic pH, respectively, demonstrating negligible complexing with mono-functional organic ligands (acetic) or those having non adjacent carboxylic groups (adipic, malonic). In contrast, in the presence of poly-functional carboxylic and hydroxy-carboxylic acids and catechol, Sb III forms stable 1:1 and 1:2 complexes with the studied organic ligands over a wide pH range typical of natural waters (3 cycle. Stability constants for these species, generated from Sb 2O 3 (rhomb.) solubility experiments, were used to model Sb complexing with natural humic acids possessing the same functional groups as those investigated in this study. Our predictions show that in an aqueous solution of pH between 2 and 10, containing 1 μg/L of Sb and 5 mg/L of dissolved organic carbon (DOC), up to 35% of total dissolved Sb binds to aqueous organic matter via carboxylic and hydroxy-carboxylic groups. This amount of complexed Sb for typical natural DOC concentrations is in agreement with that estimated from dialysis experiments performed with commercial humic acid in our work and those available in the literature for a range of standardized IHSS humic acids. Our results imply that a significant part of Sb is likely to be bound with humic acids via

  4. Synchrotron x-ray spectroscopy of EuHN O3 aqueous solutions at high temperatures and pressures and Nb-bearing silicate melt phases coexisting with hydrothermal fluids using a modified hydrothermal diamond anvil cell and rail assembly

    Science.gov (United States)

    Mayanovic, Robert A.; Anderson, Alan J.; Bassett, William A.; Chou, I.-Ming

    2007-01-01

    A modified hydrothermal diamond anvil cell (HDAC) rail assembly has been constructed for making synchrotron x-ray absorption spectroscopy, x-ray fluorescence, and x-ray mapping measurements on fluids or solid phases in contact with hydrothermal fluids up to ???900??C and 700 MPa. The diamond anvils of the HDAC are modified by laser milling grooves or holes, for the reduction of attenuation of incident and fluorescent x rays and sample cavities. The modified HDAC rail assembly has flexibility in design for measurement of light elements at low concentrations or heavy elements at trace levels in the sample and the capability to probe minute individual phases of a multiphase fluid-based system using focused x-ray microbeam. The supporting rail allows for uniform translation of the HDAC, rotation and tilt stages, and a focusing mirror, which is used to illuminate the sample for visual observation using a microscope, relative to the direction of the incident x-ray beam. A structure study of Eu(III) aqua ion behavior in high-temperature aqueous solutions and a study of Nb partitioning and coordination in a silicate melt in contact with a hydrothermal fluid are described as applications utilizing the modified HDAC rail assembly. ?? 2007 American Institute of Physics.

  5. A different view of structure-making and structure-breaking in alkali halide aqueous solutions through x-ray absorption spectroscopy.

    Science.gov (United States)

    Waluyo, Iradwikanari; Nordlund, Dennis; Bergmann, Uwe; Schlesinger, Daniel; Pettersson, Lars G M; Nilsson, Anders

    2014-06-28

    X-ray absorption spectroscopy measured in transmission mode was used to study the effect of alkali and halide ions on the hydrogen-bonding (H-bonding) network of water. Cl(-) and Br(-) are shown to have insignificant effect on the structure of water while I(-) locally weakens the H-bonding, as indicated by a sharp increase of the main-edge feature in the x-ray absorption spectra. All alkali cations act as structure-breakers in water, weakening the H-bonding network. The spectral changes are similar to spectra of high density ices where the 2nd shell has collapsed due to a break-down of the tetrahedral structures, although here, around the ions, the breakdown of the local tetrahedrality is rather due to non-directional H-bonding to the larger anions. In addition, results from temperature-dependent x-ray Raman scattering measurements of NaCl solution confirm the H-bond breaking effect of Na(+) and the effect on the liquid as similar to an increase in temperature. PMID:24985653

  6. Amorphous supramolecular structure of carboxymethyl cellulose in aqueous solution at different pH values as determined by rheology, small angle X-ray and light scattering.

    Science.gov (United States)

    Dogsa, Iztok; Tomšič, Matija; Orehek, Janez; Benigar, Elizabeta; Jamnik, Andrej; Stopar, David

    2014-10-13

    Carboxymethyl cellulose (CMC) is one of the most widely used thickening agents in industry. The combination of small-angle X-ray scattering (SAXS), static and dynamic light scattering, as well as viscosity measurements and microscopy at different pH values was utilized to explore the physicochemical properties of CMC on a scale ranging from individual macromolecules to supramolecular assemblies. The supramolecular structure of CMC was represented as a set of characteristic sample subspaces based on SAXS data utilizing the string-of-beads model. The results indicate that at pH 7.0 individual CMC molecules are approximately uniformly distributed in a supramolecular structure owing to strong intra- and intermolecular repulsive interactions. The structure of CMC is most expanded at the value of pKa, where it has the largest radius of gyration, persistence length, and size of heterogeneous regions. Below pKa the majority of the CMC sample volume belongs to the low density subspaces. Most of CMC molecules, however, reside in a few high density subspaces. Dynamically, supramolecular structure of CMC is composed of fast diffusive relaxation processes embedded in a background of non-diffusive slow relaxation process at high pH and mostly slow relaxation processes at low pH. The rheological properties of CMC at different pH values were directly related to the CMC supramolecular structure in the aqueous environment. PMID:25037380

  7. On the attenuation of x-rays and gamma-rays in dilute solutions

    DEFF Research Database (Denmark)

    Gerward, Leif

    1996-01-01

    The theory of X-ray and gamma-ray attenuation in solutions is developed. The rule of mixture for the calculation of mass and linear attenuation coefficients is elaborated in the general case as well as in the limit of extreme dilution. The validity of the latter approximation is illustrated...... by the attenuation of 17.443 keV X-rays in aqueous solutions of NaCl. Copyright (C) 1996 Elsevier Science Ltd...

  8. A Solution to Hammer's X-ray Reconstruction Problem

    DEFF Research Database (Denmark)

    Gardner, Richard J.; Kiderlen, Markus

    2007-01-01

    We propose algorithms for reconstructing a planar convex body K from possibly noisy measurements of either its parallel X-rays taken in a fixed finite set of directions or its point X-rays taken at a fixed finite set of points, in known situations that guarantee a unique solution when the data...... is exact. The algorithms construct a convex polygon P(k) whose X-rays approximate (in the least squares sense) k equally spaced noisy X-ray measurements in each of the directions or at each of the points. It is shown that these procedures are strongly consistent, meaning that, almost surely, P(k) tends...... to K in the Hausdorff metric as k tends to infinity. This solves, for the first time in the strongest sense, Hammer’s X-ray problem published in 1963....

  9. An X-ray absorption spectroelectrochemical cell for radioactive solutions

    International Nuclear Information System (INIS)

    A spectroelectrochemical cell was designed and constructed for measurement of X-ray absorption spectra under electrochemical control of the redox potential of actinide-containing solutions. A first inactive test demonstrated the feasibility of an Ag anode as a non-gassing auxiliary electrode in chloride solutions. (orig.)

  10. Synchrotron X-ray induced solution precipitation of nanoparticles

    CERN Document Server

    Lee, H J; Hwu, Y; Tsai, W L

    2003-01-01

    By irradiating a solution in electroless Ni deposition using synchrotron X-rays, Ni composite was found to nucleate homogeneously and eventually precipitate in the form of nanoparticles. The size of the nanoparticles precipitated is rather uniform (100-300 nm depending on the applied temperature). By the addition of an organic acid, well-dispersed nanoparticles could be effectively deposited on glass substrate. The hydrated electrons (e sub a sub q sup -), products of radiolysis of water molecules by synchrotron X-rays, may be responsible for the effective reduction of the metal ions, resulting in homogeneous nucleation and nanoparticle formation. Our results suggest that synchrotron X-ray can be used to induce solution precipitation of nanoparticles and therefore lead to a new method of producing nanostructured particles and coating.

  11. Chemical Bonding in Aqueous Ferrocyanide: Experimental and Theoretical X-ray Spectroscopic Study

    CERN Document Server

    Engel, Nicholas; Suljoti, Edlira; Garcia-Diez, Raul; Lange, Kathrin M; Atak, Kaan; Golnak, Ronny; Kothe, Alexander; Dantz, Marcus; Kühn, Oliver; Aziz, Emad F

    2013-01-01

    Resonant inelastic X-ray scattering (RIXS) and X-ray absorption (XA) experiments at the iron L- and nitrogen K-edge are combined with high-level first principles restricted active space self-consistent field (RASSCF) calculations for a systematic investigation of the nature of the chemical bond in potassium ferrocyanide in aqueous solution. The atom- and site-specific RIXS excitations allow for direct observation of ligand-to-metal (Fe L-edge) and metal-to-ligand (N K-edge) charge transfer bands and thereby evidence for strong {\\sigma}-donation and {\\pi}-back-donation. The effects are identified by comparing experimental and simulated spectra related to both the unoccupied and occupied molecular orbitals in solution.

  12. Summary of existing information on gamma-ray and X-ray attenuation coefficients of solutions

    DEFF Research Database (Denmark)

    Singh, K.; Gerward, Leif

    2002-01-01

    Accurate values of X-ray and gamma-ray attenuation coefficients of different chemicals are required in spectrometry as well as in many other scientific, engineering and medical disciplines involving photon radiation. The current state of knowledge of experimental and theoretical gamma-ray and X-r......-ray attenuation coefficients in aqueous solutions of salts is presented and exemplified by recent work. The results presented provide a basis for studying X-ray and gamma-ray photon interactions with ions in solution (hydrated ions) rather than ion compounds in solid form.......Accurate values of X-ray and gamma-ray attenuation coefficients of different chemicals are required in spectrometry as well as in many other scientific, engineering and medical disciplines involving photon radiation. The current state of knowledge of experimental and theoretical gamma-ray and X...

  13. Small-angle X-ray scattering of solutions

    International Nuclear Information System (INIS)

    The use of synchrotron radiation in small-angle X-ray scattering (SAXS) techniques in biological structural studies is described. The main features of the monochromatic radiation systems and the white radiation systems are considered. The detectors, data acquisition and experimental procedures are briefly described. Experimental results are presented for 1) measurements on dilute solutions and weak scatterers, 2) measurement of conformational transitions, 3) contrast variation experiments, 4) time-resolved measurements and 5) complex contrast variation. (U.K.)

  14. Time Resolved X-Ray Scattering of molecules in Solution

    DEFF Research Database (Denmark)

    Brandt van Driel, Tim

    bringing the data from measurement to analysis. Bridging the experimental design and challenges of the experiments from X-ray synchrotrons to the newly available X-ray Free Electron Laser sources (XFEL).LCLS in California is the first XFEL to come online and delivers intense 30fs X-ray pulses, orders of...... purpose built CSPAD detector is presented and applied to the data to highlight the relevance of this work. Thereby showing the ability to capture a molecular movie on the sub-ps time-scale....

  15. A liquid flatjet system for solution phase soft-x-ray spectroscopy.

    Science.gov (United States)

    Ekimova, Maria; Quevedo, Wilson; Faubel, Manfred; Wernet, Philippe; Nibbering, Erik T J

    2015-09-01

    We present a liquid flatjet system for solution phase soft-x-ray spectroscopy. The flatjet set-up utilises the phenomenon of formation of stable liquid sheets upon collision of two identical laminar jets. Colliding the two single water jets, coming out of the nozzles with 50 μm orifices, under an impact angle of 48° leads to double sheet formation, of which the first sheet is 4.6 mm long and 1.0 mm wide. The liquid flatjet operates fully functional under vacuum conditions (soft-x-ray spectroscopy of aqueous solutions in transmission mode. We analyse the liquid water flatjet thickness under atmospheric pressure using interferomeric or mid-infrared transmission measurements and under vacuum conditions by measuring the absorbance of the O K-edge of water in transmission, and comparing our results with previously published data obtained with standing cells with Si3N4 membrane windows. The thickness of the first liquid sheet is found to vary between 1.4-3 μm, depending on the transverse and longitudinal position in the liquid sheet. We observe that the derived thickness is of similar magnitude under 1 bar and under vacuum conditions. A catcher unit facilitates the recycling of the solutions, allowing measurements on small sample volumes (∼10 ml). We demonstrate the applicability of this approach by presenting measurements on the N K-edge of aqueous NH4 (+). Our results suggest the high potential of using liquid flatjets in steady-state and time-resolved studies in the soft-x-ray regime. PMID:26798824

  16. A liquid flatjet system for solution phase soft-x-ray spectroscopy

    Directory of Open Access Journals (Sweden)

    Maria Ekimova

    2015-09-01

    Full Text Available We present a liquid flatjet system for solution phase soft-x-ray spectroscopy. The flatjet set-up utilises the phenomenon of formation of stable liquid sheets upon collision of two identical laminar jets. Colliding the two single water jets, coming out of the nozzles with 50 μm orifices, under an impact angle of 48° leads to double sheet formation, of which the first sheet is 4.6 mm long and 1.0 mm wide. The liquid flatjet operates fully functional under vacuum conditions (<10−3 mbar, allowing soft-x-ray spectroscopy of aqueous solutions in transmission mode. We analyse the liquid water flatjet thickness under atmospheric pressure using interferomeric or mid-infrared transmission measurements and under vacuum conditions by measuring the absorbance of the O K-edge of water in transmission, and comparing our results with previously published data obtained with standing cells with Si3N4 membrane windows. The thickness of the first liquid sheet is found to vary between 1.4–3 μm, depending on the transverse and longitudinal position in the liquid sheet. We observe that the derived thickness is of similar magnitude under 1 bar and under vacuum conditions. A catcher unit facilitates the recycling of the solutions, allowing measurements on small sample volumes (∼10 ml. We demonstrate the applicability of this approach by presenting measurements on the N K-edge of aqueous NH4+. Our results suggest the high potential of using liquid flatjets in steady-state and time-resolved studies in the soft-x-ray regime.

  17. High resolution X-ray emission spectroscopy of water and aqueous ions using the micro-jet technique

    International Nuclear Information System (INIS)

    Graphical abstract: Soft X-ray absorption (XA) and emission (XE) spectroscopy is a powerful method for probing the local electronic structure of light elements (e.g. C, O, N, S) and transition metals, which are all of importance for biochemical systems. Here, we report for the first time on the XE spectra of a liquid micro-jet sample in a vacuum environment. We developed a high resolution X-ray emission spectrometer and recorded the spectra of pure water in full agreement with those of the literature, as well as of an aqueous solution of NiCl2. For the latter system, ground state Hartree-Fock calculations using a self-consistent reaction field (SCRF) approach were carried out to specify the nature of the d-occupied orbital. Our results confirm the dark-channel-fluorescence-yield mechanism that we recently proposed for the case of metal ions in aqueous solutions. The ability to record absorption and emission spectra of an aqueous liquid-jet opens the way for the study of biochemical systems in physiological media. - Abstract: Soft X-ray absorption (XA) and emission (XE) spectroscopy is a powerful method for probing the local electronic structure of light elements (e.g. C, O, N, S) and transition metals, which are all of importance for biochemical systems. Here, we report for the first time on the XE spectra of a liquid micro-jet sample in a vacuum environment. We developed a high resolution X-ray emission spectrometer and recorded the spectra of pure water in full agreement with those of the literature, as well as of an aqueous solution of NiCl2. For the latter system, ground state Hartree-Fock calculations using a self-consistent reaction field (SCRF) approach were carried out to specify the nature of the d-occupied orbital. Our results confirm the dark-channel-fluorescence-yield mechanism that we recently proposed for the case of metal ions in aqueous solutions. The ability to record absorption and emission spectra of an aqueous liquid-jet opens the way for the

  18. High resolution X-ray emission spectroscopy of water and aqueous ions using the micro-jet technique

    Energy Technology Data Exchange (ETDEWEB)

    Lange, Kathrin M.; Koennecke, Rene; Ghadimi, Samira; Golnak, Ronny [Helmholtz-Zentrum Berlin fuer Materialien und Energie, c/o BESSY GmbH, Albert-Einstein-Strasse 15, 12489 Berlin (Germany); Soldatov, Mikhail A. [Helmholtz-Zentrum Berlin fuer Materialien und Energie, c/o BESSY GmbH, Albert-Einstein-Strasse 15, 12489 Berlin (Germany); Research Center for Nanoscale Structure of Matter, Southern Federal University, Sorge 5, Rostov-na-Donu 344090 (Russian Federation); Hodeck, Kai F. [Helmholtz-Zentrum Berlin fuer Materialien und Energie, c/o BESSY GmbH, Albert-Einstein-Strasse 15, 12489 Berlin (Germany); Soldatov, Alexander [Research Center for Nanoscale Structure of Matter, Southern Federal University, Sorge 5, Rostov-na-Donu 344090 (Russian Federation); Aziz, Emad F., E-mail: Emad.Aziz@helmholtz-berlin.de [Helmholtz-Zentrum Berlin fuer Materialien und Energie, c/o BESSY GmbH, Albert-Einstein-Strasse 15, 12489 Berlin (Germany); Freie Universitaet Berlin, FB Physik, Arnimallee 14, D-14195 Berlin (Germany)

    2010-11-25

    Graphical abstract: Soft X-ray absorption (XA) and emission (XE) spectroscopy is a powerful method for probing the local electronic structure of light elements (e.g. C, O, N, S) and transition metals, which are all of importance for biochemical systems. Here, we report for the first time on the XE spectra of a liquid micro-jet sample in a vacuum environment. We developed a high resolution X-ray emission spectrometer and recorded the spectra of pure water in full agreement with those of the literature, as well as of an aqueous solution of NiCl{sub 2}. For the latter system, ground state Hartree-Fock calculations using a self-consistent reaction field (SCRF) approach were carried out to specify the nature of the d-occupied orbital. Our results confirm the dark-channel-fluorescence-yield mechanism that we recently proposed for the case of metal ions in aqueous solutions. The ability to record absorption and emission spectra of an aqueous liquid-jet opens the way for the study of biochemical systems in physiological media. - Abstract: Soft X-ray absorption (XA) and emission (XE) spectroscopy is a powerful method for probing the local electronic structure of light elements (e.g. C, O, N, S) and transition metals, which are all of importance for biochemical systems. Here, we report for the first time on the XE spectra of a liquid micro-jet sample in a vacuum environment. We developed a high resolution X-ray emission spectrometer and recorded the spectra of pure water in full agreement with those of the literature, as well as of an aqueous solution of NiCl{sub 2}. For the latter system, ground state Hartree-Fock calculations using a self-consistent reaction field (SCRF) approach were carried out to specify the nature of the d-occupied orbital. Our results confirm the dark-channel-fluorescence-yield mechanism that we recently proposed for the case of metal ions in aqueous solutions. The ability to record absorption and emission spectra of an aqueous liquid-jet opens the

  19. Properties of aqueous nitrate and nitrite from x-ray absorption spectroscopy

    International Nuclear Information System (INIS)

    Nitrate and nitrite ions are of considerable interest, both for their widespread use in commercial and research contexts and because of their central role in the global nitrogen cycle. The chemistry of atmospheric aerosols, wherein nitrate is abundant, has been found to depend on the interfacial behavior of ionic species. The interfacial behavior of ions is determined largely by their hydration properties; consequently, the study of the hydration and interfacial behavior of nitrate and nitrite comprises a significant field of study. In this work, we describe the study of aqueous solutions of sodium nitrate and nitrite via X-ray absorption spectroscopy (XAS), interpreted in light of first-principles density functional theory electronic structure calculations. Experimental and calculated spectra of the nitrogen K-edge XA spectra of bulk solutions exhibit a large 3.7 eV shift between the XA spectra of nitrate and nitrite resulting from greater stabilization of the nitrogen 1s energy level in nitrate. A similar shift is not observed in the oxygen K-edge XA spectra of NO3− and NO2−. The hydration properties of nitrate and nitrite are found to be similar, with both anions exhibiting a similar propensity towards ion pairing

  20. Properties of aqueous nitrate and nitrite from x-ray absorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Smith, Jacob W.; Lam, Royce K.; Saykally, Richard J., E-mail: saykally@berkeley.edu [Department of Chemistry, University of California, Berkeley, California 94720 (United States); Chemical Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, California 94720 (United States); Shih, Orion [National Synchrotron Radiation Research Center, Hsinchu 30076, Taiwan (China); Rizzuto, Anthony M. [Department of Chemistry, University of California, Berkeley, California 94720 (United States); Prendergast, David [The Molecular Foundry, Lawrence Berkeley National Laboratory, Berkeley, California 94720 (United States)

    2015-08-28

    Nitrate and nitrite ions are of considerable interest, both for their widespread use in commercial and research contexts and because of their central role in the global nitrogen cycle. The chemistry of atmospheric aerosols, wherein nitrate is abundant, has been found to depend on the interfacial behavior of ionic species. The interfacial behavior of ions is determined largely by their hydration properties; consequently, the study of the hydration and interfacial behavior of nitrate and nitrite comprises a significant field of study. In this work, we describe the study of aqueous solutions of sodium nitrate and nitrite via X-ray absorption spectroscopy (XAS), interpreted in light of first-principles density functional theory electronic structure calculations. Experimental and calculated spectra of the nitrogen K-edge XA spectra of bulk solutions exhibit a large 3.7 eV shift between the XA spectra of nitrate and nitrite resulting from greater stabilization of the nitrogen 1s energy level in nitrate. A similar shift is not observed in the oxygen K-edge XA spectra of NO{sub 3}{sup −} and NO{sub 2}{sup −}. The hydration properties of nitrate and nitrite are found to be similar, with both anions exhibiting a similar propensity towards ion pairing.

  1. Properties of aqueous nitrate and nitrite from x-ray absorption spectroscopy

    Science.gov (United States)

    Smith, Jacob W.; Lam, Royce K.; Shih, Orion; Rizzuto, Anthony M.; Prendergast, David; Saykally, Richard J.

    2015-08-01

    Nitrate and nitrite ions are of considerable interest, both for their widespread use in commercial and research contexts and because of their central role in the global nitrogen cycle. The chemistry of atmospheric aerosols, wherein nitrate is abundant, has been found to depend on the interfacial behavior of ionic species. The interfacial behavior of ions is determined largely by their hydration properties; consequently, the study of the hydration and interfacial behavior of nitrate and nitrite comprises a significant field of study. In this work, we describe the study of aqueous solutions of sodium nitrate and nitrite via X-ray absorption spectroscopy (XAS), interpreted in light of first-principles density functional theory electronic structure calculations. Experimental and calculated spectra of the nitrogen K-edge XA spectra of bulk solutions exhibit a large 3.7 eV shift between the XA spectra of nitrate and nitrite resulting from greater stabilization of the nitrogen 1s energy level in nitrate. A similar shift is not observed in the oxygen K-edge XA spectra of NO3- and NO2-. The hydration properties of nitrate and nitrite are found to be similar, with both anions exhibiting a similar propensity towards ion pairing.

  2. Analysis of the Electronic Structure of Aqueous Urea and Its Derivatives: A Systematic Soft X-Ray-TD-DFT Approach.

    Science.gov (United States)

    Tesch, Marc F; Golnak, Ronny; Ehrhard, Felix; Schön, Daniela; Xiao, Jie; Atak, Kaan; Bande, Annika; Aziz, Emad F

    2016-08-16

    Soft X-ray emission (XE), absorption (XA), and resonant inelastic scattering (RIXS) experiments have been conducted at the nitrogen K-edge of urea and its derivatives in aqueous solution and were compared with density functional theory and time-dependent density functional theory calculations. This comprehensive study provides detailed information on the occupied and unoccupied molecular orbitals of urea, thiourea, acetamide, dimethylurea, and biuret at valence levels. By identifying the electronic transitions that contribute to the experimental spectral features, the energy gap between the highest occupied and the lowest unoccupied molecular orbital of each molecule is determined. Moreover, a theoretical approach is introduced to simulate resonant inelastic X-ray scattering spectra by adding an extra electron to the lowest unoccupied molecular orbital, thereby mimicking the real initial state of the core-electron absorption before the subsequent relaxation process. PMID:27416871

  3. X-ray Scattering Studies of Director Tumbling Dynamics in a Nematic Surfactant Solution

    Science.gov (United States)

    Caputo, F.; Burghardt, W.

    1998-03-01

    Many cationic surfactants self-assemble into wormlike micelles. At high concentrations, these micellar solutions may then form liquid crystalline nematic phases. Recent studies have demonstrated that the rheology of such solutions is quite similar to that observed in lyotropic liquid crystalline polymers, particularly with respect to stress oscillations in transient flows that are attributed to director tumbling. Here we present complementary rheological and x-ray scattering data on an aqueous solution of cetylpyridinium chloride/hexanol(Sample kindly supplied by L. Walker and J.-F. Berret) to compare the mechanical and structural response. Time-resolved synchtrotron x-ray scattering under shear(Experiments performed at DND-CAT at the APS) is used to measure the average micelle orientation state during transient flows such as step increases and decreases in shear rate, and reversals in flow direction. There is a strong connection between the rheology and the fluid structure: stress minima are well correlated with high instantaneous micellar orientation. The experimental observations are compared with the predictions of the Larson-Doi tumbling polydomain model, which captures many aspects of the observed behavior.

  4. Computer solutions for studying correlations between solar magnetic fields and Skylab X-ray observations

    Science.gov (United States)

    Teuber, D.; Tandberg-Hanssen, E.; Hagyard, M. J.

    1977-01-01

    A method is described which correlates the NASA-Marshall Space Flight Center (MSFC) Image Data Processing System (IDAPS) and MSFC magnetograph data to X-ray and H-alpha observations from the Skylab mission. Solutions of Laplace's equation in three dimensions, based on the magnetograph data, are convolved with observed X-ray and H-alpha regions. Matched filtering (template matching) provides a best fit of the observed X-ray regions to the computed total magnetic vector magnitude between 10,000 and 15,000 km above the photosphere.

  5. Determination of plutonium in nitric acid solutions using energy dispersive L X-ray fluorescence with a low power X-ray generator

    Energy Technology Data Exchange (ETDEWEB)

    Py, J. [Laboratoire Chrono-Environnement, UMR CNRS 6249, Université de Franche-Comté, 16 route de Gray, F-25030 Besançon (France); Commissariat à l’Énergie Atomique, Centre de Valduc, F-21120 Is-sur-Tille (France); Groetz, J.-E., E-mail: jegroetz@univ-fcomte.fr [Laboratoire Chrono-Environnement, UMR CNRS 6249, Université de Franche-Comté, 16 route de Gray, F-25030 Besançon (France); Hubinois, J.-C.; Cardona, D. [Commissariat à l’Énergie Atomique, Centre de Valduc, F-21120 Is-sur-Tille (France)

    2015-04-21

    This work presents the development of an in-line energy dispersive L X-ray fluorescence spectrometer set-up, with a low power X-ray generator and a secondary target, for the determination of plutonium concentration in nitric acid solutions. The intensity of the L X-rays from the internal conversion and gamma rays emitted by the daughter nuclei from plutonium is minimized and corrected, in order to eliminate the interferences with the L X-ray fluorescence spectrum. The matrix effects are then corrected by the Compton peak method. A calibration plot for plutonium solutions within the range 0.1–20 g L{sup −1} is given.

  6. Picosecond X-ray absorption spectroscopy: application to coordination chemistry compounds in solution

    OpenAIRE

    Saes, Melanie

    2004-01-01

    The photocycle of aqueous ruthenium-(trisbipyridine) [Ru(bpy)3]2+ was studied under high laser excitation intensities and high sample concentrations with picosecond resolved x-ray absorption spectroscopy. In a pump-probe scheme a femtosecond laser pulse promotes a 4d electron from the ruthenium to the ligand orbitals, thus creating a metal-to-ligand-charge-transfer (MLCT) complex. A hard x-ray pulse from a synchrotron source probes the ruthenium L3 and L2 edges, monitoring the electronic and ...

  7. Picosecond X-ray absorption spectroscopy: application to coordination chemistry compounds in solution

    OpenAIRE

    Saes, Melanie; Chergui, Majed

    2005-01-01

    The photocycle of aqueous ruthenium-(trisbipyridine) [Ru(bpy)3]2+ was studied under high laser excitation intensities and high sample concentrations with picosecond resolved x-ray absorption spectroscopy. In a pump-probe scheme a femtosecond laser pulse promotes a 4d electron from the ruthenium to the ligand orbitals, thus creating a metal-to-ligand-charge-transfer (MLCT) complex. A hard x-ray pulse from a synchrotron source probes the ruthenium L3 and L2 edges, monitoring the electronic and ...

  8. Ice Recrystallization in a Solution of a Cryoprotector and Its Inhibition by a Protein: Synchrotron X-Ray Diffraction Study.

    Science.gov (United States)

    Zakharov, Boris; Fisyuk, Alexander; Fitch, Andy; Watier, Yves; Kostyuchenko, Anastasia; Varshney, Dushyant; Sztucki, Michael; Boldyreva, Elena; Shalaev, Evgenyi

    2016-07-01

    Ice formation and recrystallization is a key phenomenon in freezing and freeze-drying of pharmaceuticals and biopharmaceuticals. In this investigation, high-resolution synchrotron X-ray diffraction is used to quantify the extent of disorder of ice crystals in binary aqueous solutions of a cryoprotectant (sorbitol) and a protein, bovine serum albumin. Ice crystals in more dilute (10 wt%) solutions have lower level of microstrain and larger crystal domain size than these in more concentrated (40 wt%) solutions. Warming the sorbitol-water mixtures from 100 to 228 K resulted in partial ice melting, with simultaneous reduction in the microstrain and increase in crystallite size, that is, recrystallization. In contrast to sorbitol solutions, ice crystals in the BSA solutions preserved both the microstrain and smaller crystallite size on partial melting, demonstrating that BSA inhibits ice recrystallization. The results are consistent with BSA partitioning into quasi-liquid layer on ice crystals but not with a direct protein-ice interaction and protein sorption on ice surface. The study shows for the first time that a common (i.e., not-antifreeze) protein can have a major impact on ice recrystallization and also presents synchrotron X-ray diffraction as a unique tool for quantification of crystallinity and disorder in frozen aqueous systems.

  9. In situ characterization of aluminum-containing mineral-microorganism aqueous suspensions using scanning transmission X-ray microscopy.

    Science.gov (United States)

    Yoon, Tae Hyun; Johnson, Stephen B; Benzerara, Karim; Doyle, Colin S; Tyliszczak, Tolek; Shuh, David K; Brown, Gordon E

    2004-11-23

    In situ characterization of colloidal particles under hydrous conditions is one of the key requirements for understanding their state of aggregation and impact on the transport of pollutants in aqueous environments. Scanning transmission X-ray microscopy (STXM) is one of the few techniques that can satisfy this need by providing element- and chemical-state-specific 2-D maps at a spatial resolution better than 50 nm using soft X-rays from synchrotron radiation wiggler or undulator sources tuned to the absorption edges of different elements. X-ray absorption near-edge structure (XANES) spectra can also be collected simultaneously at a similar spatial resolution and can provide phase identification in many cases. In this study, we report STXM images and XANES spectroscopy measurements at or above the Al K-edge (E = 1559.6 eV) of various Al-containing minerals and synthetic oxides [alpha-Al2O3 (corundum), gamma-Al2O3, gamma-AlOOH (boehmite), alpha-Al(OH)3 (bayerite), KAl2(AlSi3O10)(OH)2 (muscovite), (Al,Mg)8(Si4O10)4(OH)8.nH2O (montmorillonite), and Mg6Al2(OH)16CO3.4H2O (hydrotalcite)] and demonstrate the capability of this spectromicroscopic tool to identify different Al-containing mineral colloids in multiphase mixtures in aqueous solution. We also demonstrate that STXM imaging at or above the C K-edge (E = 284.2 eV) and Al K-edge can provide unique information on the interactions between bacteria and Al-containing nanoparticles in aqueous suspensions. STXM images of a mixture of Caulobacter crescentus and montmorillonite and corundum particles just above the C and Al K-edges show that the mineral particles and bacteria are closely associated in aggregates, which is likely due to the binding of bacteria to clay and corundum particles by extracellular polysaccharides.

  10. Aqueous Cu(II)-organic complexation studied in situ using soft X-ray and vibrational spectroscopies.

    Science.gov (United States)

    Phillips, Courtney L; Regier, Tom Z; Peak, Derek

    2013-12-17

    In situ aqueous solutions containing copper-ligand mixtures were measured at the Cu L-edge using X-ray absorption near edge structure (XANES) and with attenuated total reflectance infrared (ATR-FTIR) spectroscopies. Copper complexation with environmentally relevant ligands such as EDTA, citrate, and malate provided a bridge between spectroscopic studies and general environmental behavior and will allow for future study of complex environmental samples. XANES results show that the lowest unoccupied molecular orbital (LUMO) energy is governed by the ligand field strength and is related to Lewis acid/base properties of the ligand functional groups. Complementary ATR-FTIR studies confirmed the importance of water molecules in the structure of these Cu-ligand complexes and provided in-depth structural analysis to support the XANES data. Copper-malate is shown to have a 5/6-O-ring structure, and Cu-ethylenediaminetetraacetate has pentadentate coordination. Cu L-edge XANES also revealed direct Cu-N coordination in these aqueous solutions with amide functional groups.

  11. X-ray Amorphous Phases in Antarctica Dry Valley Soils: Insight into Aqueous Alteration Processes on Mars?

    Science.gov (United States)

    Ming, D. W.; Morris, R. V.; Rampe, E. B.; Quinn, J. E.; Graff, T. G.

    2015-12-01

    The Chemistry and Mineralogy (CheMin) instrument onboard the Mars Curiosity rover has detected abundant amounts (approx. 25-30 wt. %) of X-ray amorphous materials in a windblown deposit (Rocknest) and in a sedimentary mudstone (Cumberland and John Klein) in Gale crater. On Earth, X-ray amorphous components are common in soils and sediments, but usually not as abundant as detected in Gale crater. One hypothesis for the abundant X-ray amorphous materials on Mars is limited interaction of liquid water with surface materials, kinetically inhibiting maturation to more crystalline phases. The objective of this study was to characterize the chemistry and mineralogy of soils formed in the Antarctica Dry Valleys, one of the driest locations on Earth. Two soils were characterized from different elevations, including a low elevation, coastal, subxerous soil in Taylor Valley and a high elevation, ultraxerous soil in University Valley. A variety of techniques were used to characterize materials from each soil horizon, including Rietveld analysis of X-ray diffraction data. For Taylor Valley soil, the X-ray amorphous component ranged from about 4 wt. % in the upper horizon to as high as 15 wt. % in the lowest horizon just above the permafrost layer. Transmission electron microscopy indicated that the presence of short-range ordered (SRO) smectite was the most likely candidate for the X-ray amorphous materials in the Taylor Valley soils. The SRO smectite is likely an aqueous alteration product of mica inherited from granitic materials during glaciation of Taylor Valley. The drier University Valley soil had lower X-ray amorphous contents of about 5 wt. % througout the profile. The X-ray amorphous materials in University Valley are attributed to nanoparticles of TiO2 and possibly amorphous SiO2. The high abundance of X-ray amorphous materials in Taylor Valley is surprising for one of the driest places on Earth. These materials may have been physically and chemical altered during

  12. Studies of ionic liquid solutions by soft X-ray absorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Rodrigues, Fabio [Departamento de Quimica Fundamental, Instituto de Quimica, Universidade de Sao Paulo, CP 26.077, CEP 05513-970, Sao Paulo, SP (Brazil); Nascimento, Gustavo M. do [Departamento de Quimica Fundamental, Instituto de Quimica, Universidade de Sao Paulo, CP 26.077, CEP 05513-970, Sao Paulo, SP (Brazil)], E-mail: morari@yahoo.com; Santos, Paulo S. [Departamento de Quimica Fundamental, Instituto de Quimica, Universidade de Sao Paulo, CP 26.077, CEP 05513-970, Sao Paulo, SP (Brazil)

    2007-03-15

    Soft X-ray spectroscopies give specific information about the electronic structure around light elements. The high absorption of soft X-rays by almost every molecule, including air, requires studies under vacuum, which represents a great limitation. Solids with high vapor pressure and liquids are very difficult to be studied, making solution chemistry almost neglected. This work explores the use of ionic liquids, organic liquids with very low vapor pressure, as media to study chemical solutions using soft X-ray. N 1s spectra are reported of ionic liquid solutions of 1-methyl-3alkyl-imidazolium cation with different anions and chain lengths, and urea/choline chloride mixtures (a deep eutectic solvent) with several solutes including dyes (Janus Green B and Congo Red), synthetic polymers (polyaniline) and nitrate salts. While there are significant problems with the signal of the solvent, the results do show that it is possible to detect solute signals, and further to see spectral changes attributed to solvent-solute interactions.

  13. X-ray studies of mixed surfactants at the hexane-water interface and thin aqueous films

    Science.gov (United States)

    Pingali, Sai Venkatesh

    The interface between water and mixed surfactant solutions of CH3(CH2)19OH and CF3(CF 2)7(CH2)2OH in hexane was studied with interfacial tension and X-ray reflectivity measurements. Measurements of the tension as a function of temperature for a range of total bulk surfactant concentrations (m) and for three different values of the molal ratio of fluorinated to total surfactant concentration (X 2 = 0.25, 0.28 and 0.5) determined that the interface can be in three different monolayer phases. X-ray reflectivity study of four different compositions as a function of temperature demonstrates that phases 1 and 2 correspond to an interface fully covered by only one of the surfactants (liquid monolayer of CH3(CH2)19OH in phase I and a solid condensed monolayer of CF3(CF2)7(CH2) 2OH in phase 2). The liquid monolayer of CH3(CH2) 19OH undergoes a transition to the solid monolayer of CF3(CF 2)7(CH2)2OH with increasing temperature. Phase 3 and the transition regions between Phases 1 and 2 consist of a mixed monolayer at the interface that contains domains of the two surfactants. A simple model is presented that predicts the basic features of the domain coverage as a function of temperature for the mixed surfactant system from the behavior of the single surfactant systems. Spontaneous thin film formation in a biphase system consisting of PEG, potassium phosphates and water was studied using X-ray reflectivity and off-specular diffuse scattering. Two aqueous phases, PEG-rich and salt-rich phases are formed by varying the overall salt concentration from 12--29 wt/wt% for fixed overall PEG concentration of 13 wt/wt%. Two classes of thin film formation are observed---the thickness of the spontaneously formed film is same as the drop spreading film for systems 12--18% and the thickness of the spontaneously formed film is different from the drop spreading film for systems 23% and 29%. Although system 12% is in the 12--18% class, its behavior is different from the rest. Layer thickness

  14. Quantitative determination of uranium in organic solution by X-ray fluorescence

    International Nuclear Information System (INIS)

    An X-ray fluorescent method for the determination of uranium in tributilphosphate-kerosene-nitriacid solution has been developed. Chemical properties of the matrix elements were studied in order to select a convenient procedure to determine samples and standards on the same way. The method avoids the destruction of the organic material and has proved to be very useful for the fast control of uranium concentration. (Author)

  15. Small angle X-ray and neutron scattering from solutions of biological macromolecules

    CERN Document Server

    Svergun, Dmitri I; May, Roland P; Timmins, Peter A

    2013-01-01

    In this book, following the presentation of the basics of scattering from isotropic macromolecular solutions, modern instrumentation, experimental practice and advanced analysis techniques are explained. Advantages of X-rays (rapid data collection, small sample volumes) and of neutrons (contrast variation by hydrogen/deuterium exchange) are specifically highlighted. Examples of applications of the technique to different macromolecular systems are considered with specific emphasis on the synergistic use of SAXS/SANS with other structural, biophysical and computational techniques.

  16. Solution Phase Molecular Dynamics Probed with Synchrotron Hard X-rays

    Science.gov (United States)

    March, Anne; Doumy, Gilles; Kanter, Elliot; Southworth, Stephen; Young, Linda; Nemeth, Zoltan; Vankó, Gyorgy; Assefa, Tadesse; Gawelda, Wojciech

    2013-05-01

    The ability to measure short-lived transient states during a chemical reaction is key to understanding many important processes such as oxygen binding in hemeproteins and electron transport in photosynthesis. Time resolved hard x-ray spectroscopies, which are based on laser-pump/x-ray-probe methods, are a unique tool because unlike UV-VIS techniques they are element specific and can provide electronic and structural information with atomic resolution in the vicinity of a particular atom or ion. These characteristics make them particularly powerful for studying molecules in complex environments such as solutions. Using a MHz, picosecond, high average power laser system implemented at Sector 7ID-D of the Advanced Photon Source we have been developing time resolved x-ray emission techniques to track the evolution of photoexcited molecules in solution. We will present recent studies which include the ligand substitution reaction and hydrated electron formation in the coordination complex ferrocyanide Fe(CN)64-. This work was supported by the Chemical Sciences, Geosciences, and Biosciences Division and the Advanced Photon Source by the Office of Basic Energy Sciences, Office of Science, US Dept of Energy, Contract DE-AC02-06CH11357.

  17. State-Dependent Electron Delocalization Dynamics at the Solute-Solvent Interface: Soft-X-Ray Absorption Spectroscopy and Ab Initio Calculations

    OpenAIRE

    Sergey I. Bokarev; Dantz, Marcus; Suljoti, Edlira; Kühn, Oliver; Emad F. Aziz

    2013-01-01

    Non-radiative decay channels in the L-edge fluorescence spectra from transition metal-aqueous solutions give rise to spectral dips in X-ray transmission spectra. Their origin is unraveled here using partial and inverse partial fluorescence yields on the micro-jet combined with multi-reference ab initio electronic structure calculations. Comparing Fe2+, Fe3+, and Co2+ systems we demonstrate unequivocally that spectral dips are due to a state-dependent electron delocalization within the manifol...

  18. Soft X-ray induced modifications of PVA-based microbubbles in aqueous environment: a microspectroscopy study.

    Science.gov (United States)

    Tzvetkov, George; Fernandes, Paulo; Wenzel, Stephan; Fery, Andreas; Paradossi, Gaio; Fink, Rainer H

    2009-02-21

    We use scanning-transmission X-ray microspectroscopy (STXM) for in situ characterization of the physicochemical changes in air-filled poly(vinyl alcohol) (PVA) based microbubbles upon soft X-ray irradiation. The microbubbles were illuminated directly in aqueous suspension with 520 eV X-rays and a continuous shrinkage of the particles with an illumination time/radiation dose was observed. Utilizing the intrinsic absorption properties of the species and the high spatial resolution of the STXM, the modifications of the particles' structure were simultaneously recognized. A thorough characterization of the microbubble volume, membrane thickness and absorption coefficient was performed by quantitative fitting of the radial transmittance profiles of the targeted microbubbles. Apart from the observed volume contraction, there was no significant change in the shell thickness. The chemical changes in the membranes were clarified via C K-edge near-edge X-ray absorption fine structure (NEXAFS) spectroscopy. It was revealed that the observed structural alterations go along with a continuous degradation of the PVA network associated with formation of carbonyl- and carboxyl-containing species as well as an increased content of unsaturated bonds.

  19. The Transient Accereting X-Ray Pulsar XTE J1946+274: Stability of the X-Ray Properties at Low Flux and Updated Orbital Solution

    CERN Document Server

    Marcu-Cheatham, Diana M; Kühnel, Matthias; Müller, Sebastian; Falkner, Sebastian; Caballero, Isabel; Finger, Mark H; Jenke, Peter J; Wilson-Hodge, Colleen A; Fürst, Felix; Grinberg, Victoria; Hemphill, Paul B; Kreykenbohm, Ingo; Klochkov, Dmitry; Rothschild, Richard E; Terada, Yukikatsu; Enoto, Teruaki; Iwakiri, Wataru; Wolff, Michael T; Becker, Peter A; Wood, Kent S; Wilms, Jöern

    2015-01-01

    We present a timing and spectral analysis of the X-ray pulsar XTE J1946+274 observed with Suzaku during an outburst decline in 2010 October and compare with previous results. XTE J1946+274 is a transient X-ray binary consisting of a Be-type star and a neutron star with a 15.75 s pulse period in a 172 d orbit with 2-3 outbursts per orbit during phases of activity. We improve the orbital solution using data from multiple instruments. The X-ray spectrum can be described by an absorbed Fermi-Dirac cutoff power law model along with a narrow Fe K line at 6.4 keV and a weak Cyclotron Resonance Scattering Feature (CRSF) at ~35 keV. The Suzaku data are consistent with the previously observed continuum flux versus iron line flux correlation expected from fluorescence emission along the line of sight. However, the observed iron line flux is slightly higher, indicating the possibility of a higher iron abundance or the presence of non-uniform material. We argue that the source most likely has only been observed in the sub...

  20. The Transient Accreting X-Ray Pulsar XTE J1946+274: Stability of X-Ray Properties at Low Flux and Updated Orbital Solution

    Science.gov (United States)

    Marcu-Cheatham, Diana M.; Pottschmidt, Katja; Kühnel, Matthias; Müller, Sebastian; Falkner, Sebastian; Caballero, Isabel; Finger, Mark H.; Jenke, Peter J.; Wilson-Hodge, Colleen A.; Fürst, Felix; Grinberg, Victoria; Hemphill, Paul B.; Kreykenbohm, Ingo; Klochkov, Dmitry; Rothschild, Richard E.; Terada, Yukikatsu; Enoto, Teruaki; Iwakiri, Wataru; Wolff, Michael T.; Becker, Peter A.; Wood, Kent S.; Wilms, Jörn

    2015-12-01

    We present a timing and spectral analysis of the X-ray pulsar XTE J1946+274 observed with Suzaku during an outburst decline in 2010 October and compare with previous results. XTE J1946+274 is a transient X-ray binary consisting of a Be-type star and a neutron star with a 15.75 s pulse period in a 172 days orbit with 2-3 outbursts per orbit during phases of activity. We improve the orbital solution using data from multiple instruments. The X-ray spectrum can be described by an absorbed Fermi-Dirac cut-off power-law model along with a narrow Fe Kα line at 6.4 keV and a weak Cyclotron Resonance Scattering Feature (CRSF) at ˜35 keV. The Suzaku data are consistent with the previously observed continuum flux versus iron line flux correlation expected from fluorescence emission along the line of sight. However, the observed iron line flux is slightly higher, indicating the possibility of a higher iron abundance or the presence of non-uniform material. We argue that the source most likely has only been observed in the subcritical (non-radiation dominated) state since its pulse profile is stable over all observed luminosities and the energy of the CRSF is approximately the same at the highest (˜5 × 1037 erg s-1) and lowest (˜5 × 1036 erg s-1) observed 3-60 keV luminosities.

  1. Determination of Vanadium and Titanium in oil using aqueous calibration curves by X-ray fluorescence

    International Nuclear Information System (INIS)

    It is shown that the determination of minor elements in oil can be realized with high accuracy and precision using standard aqueous solutions. The relationship Ii/(Ia-Io)=KCi must be used, where Ii concentration Ci, Ia is the intensity of the scattered radiation of 5.894 keV from a Fe-55 radioisotope source and K is a constant. Io is calculated through the equation Ii/K(Ia-Io)=Ji/K(Ja-Io), where Ii and Ia are measured from the spectrum of an aqueous standard; Ji and Ja are measured from the spectrum of an oil sample, which has a concentration of the element i equal to that in the aqueous solution. The relationship Ii/Ia=KCi, used in previous work, does not include the term Io, therefore it must be used only for semi-quantitative analysis. An experiment on the determination of vanadium and titanium in standard oils (CONOSTAN S-12 and CONOSTAN S-21) confirmed this derivation. Reproducibility equal or below 5 and accuracy of 7 were achieved. (author)

  2. Ion distributions at charged aqueous surfaces: Synchrotron X-ray scattering studies

    Energy Technology Data Exchange (ETDEWEB)

    Bu, Wei [Iowa State Univ., Ames, IA (United States)

    2009-01-01

    Surface sensitive synchrotron X-ray scattering studies were performed to obtain the distribution of monovalent ions next to a highly charged interface at room temperature. To control surface charge density, lipids, dihexadecyl hydrogen-phosphate (DHDP) and dimysteroyl phosphatidic acid (DMPA), were spread as monolayer materials at the air/water interface, containing CsI at various concentrations. Five decades in bulk concentrations (CsI) are investigated, demonstrating that the interfacial distribution is strongly dependent on bulk concentration. We show that this is due to the strong binding constant of hydronium H3O+ to the phosphate group, leading to proton-transfer back to the phosphate group and to a reduced surface charge. Using anomalous reflectivity off and at the L3 Cs+ resonance, we provide spatial counterion (Cs+) distributions next to the negatively charged interfaces. The experimental ion distributions are in excellent agreement with a renormalized surface charge Poisson-Boltzmann theory for monovalent ions without fitting parameters or additional assumptions. Energy Scans at four fixed momentum transfers under specular reflectivity conditions near the Cs+ L3 resonance were conducted on 10-3 M CsI with DHDP monolayer materials on the surface. The energy scans exhibit a periodic dependence on photon momentum transfer. The ion distributions obtained from the analysis are in excellent agreement with those obtained from anomalous reflectivity measurements, providing further confirmation to the validity of the renormalized surface charge Poisson-Boltzmann theory for monovalent ions. Moreover, the dispersion corrections f0 and f00 for Cs+ around L3 resonance, revealing the local environment of a Cs+ ion in the solution at the interface, were extracted simultaneously with output of ion distributions.

  3. A new supramolecular compound of chrome(III): Synthesis, spectroscopic characterization, X-ray crystal structure, DFT, and solution studies

    Science.gov (United States)

    Eshtiagh-Hosseini, Hossein; Yousefi, Zakieh; Mirzaei, Masoud; Chen, Ya-Guang; Ali Beyramabadi, S.; Shokrollahi, Ardeshir; Aghaei, Roghayyeh

    2010-06-01

    A new supramolecular compound of Cr(III) atom was synthesized and characterized by using elemental analysis, FTIR spectroscopy, UV-vis, and single crystal X-ray diffraction method. The chemical formula and space group of the resulting compound is (2-apymH)[Cr(pydc) 2]·2H 2O ( 1) (pydc = 2,6-pyridinedicarboxylate, 2-apym = 2-aminopyrimidine) and P2 1/ c where the final R value is 0.0157 for 3896 reflections collected. The [Cr(pydc) 2] - anions and the (2-apymH) + moiety form a three-dimensional solid state structure by a variety of noncovalent interactions such as ion pairing and hydrogen bonds interactions. On the basis of crystallographic data, it can be seen that Cr(III) atom is six-coordinated by two (pydc) 2- groups. With respect to bond lengths and angles, it is observed that coordination sphere around Cr(III) atom is a distorted octahedral. Furthermore, DFT calculation and solution study have been completely performed on 1 where corresponding data showed that obtained results from DFT and solution studies have good agreement with X-ray crystallography results. The optimized geometry confirms that the C-O (bonded) bond length of (pydc) 2- ligand in its complex form has been increased compared with the free ligand. The evidence shows that C-O (bonded) is weakened upon formation of complex, while C dbnd O (free) converted to double bond. Anionic complex possesses 90 occupied molecular orbitals and 3 half-occupied ones (91-93). A comparison between the stoichiometry of the crystalline complex in pydcH 2-2-apym-Cr system and the results obtained from solution studies clearly revealed that the CrL 2QH is the most abundant species existing in aqueous solution possesses a stoichiometry similar to that of the complex which was obtained in the solid state.

  4. X-ray absorption spectroscopy of hemes and hemeproteins in solution: multiple scattering analysis.

    Science.gov (United States)

    D'Angelo, Paola; Lapi, Andrea; Migliorati, Valentina; Arcovito, Alessandro; Benfatto, Maurizio; Roscioni, Otello Maria; Meyer-Klaucke, Wolfram; Della-Longa, Stefano

    2008-11-01

    A full quantitative analysis of Fe K-edge X-ray absorption spectra has been performed for hemes in two porphynato complexes, that is, iron(III) tetraphenylporphyrin chloride (Fe(III)TPPCl) and iron(III) tetraphenylporphyrin bis(imidazole) (Fe(III)TPP(Imid)2), in two protein complexes whose X-ray structure is known at atomic resolution (1.0 A), that is, ferrous deoxy-myoglobin (Fe(II)Mb) and ferric aquo-myoglobin (Fe(III)MbH2O), and in ferric cyano-myoglobin (Fe(III)MbCN), whose X-ray structure is known at lower resolution (1.4 A). The analysis has been performed via the multiple scattering approach, starting from a muffin tin approximation of the molecular potential. The Fe-heme structure has been obtained by analyzing independently the Extended X-ray Absorption Fine Structure (EXAFS) region and the X-ray Absorption Near Edge Structure (XANES) region. The EXAFS structural results are in full agreement with the crystallographic values of the models, with an accuracy of +/- 0.02 A for Fe-ligand distances, and +/-6 degrees for angular parameters. All the XANES features above the theoretical zero energy (in the lower rising edge) are well accounted for by single-channel calculations, for both Fe(II) and Fe(III) hemes, and the Fe-N p distance is determined with the same accuracy as EXAFS. XANES evaluations of Fe-5th and Fe-6th ligand distances are determined with 0.04-0.07 A accuracy; a small discrepancy with EXAFS (0.01 to 0.05 A beyond the statistical error), is found for protein compounds. Concerns from statistical correlation among parameters and multiple minima in the parameter space are discussed. As expected, the XANES accuracy is slightly lower than what was found for polarized XANES on Fe(III)MbCN single crystal (0.03-0.04 A), and states the actual state-of-the-art of XANES analysis when used to extract heme-normal parameters in a solution spectrum dominated by heme-plane scattering. PMID:18837548

  5. A liquid flatjet system for solution phase soft-x-ray spectroscopy

    OpenAIRE

    Maria Ekimova; Wilson Quevedo; Manfred Faubel; Philippe Wernet; Nibbering, Erik T. J.

    2015-01-01

    We present a liquid flatjet system for solution phase soft-x-ray spectroscopy. The flatjet set-up utilises the phenomenon of formation of stable liquid sheets upon collision of two identical laminar jets. Colliding the two single water jets, coming out of the nozzles with 50 μm orifices, under an impact angle of 48° leads to double sheet formation, of which the first sheet is 4.6 mm long and 1.0 mm wide. The liquid flatjet operates fully functional under vacuum conditions (

  6. Introducing a standard method for experimental determination of the solvent response in laser pump, x-ray probe time-resolved wide-angle x-ray scattering experiments on systems in solution

    DEFF Research Database (Denmark)

    Kjær, Kasper Skov; Brandt van Driel, Tim; Kehres, Jan;

    2013-01-01

    In time-resolved laser pump, X-ray probe wide-angle X-ray scattering experiments on systems in solution the structural response of the system is accompanied by a solvent response. The solvent response is caused by reorganization of the bulk solvent following the laser pump event, and in order...... response-the solvent term-experimentally when applying laser pump, X-ray probe time-resolved wide-angle X-ray scattering. The solvent term describes difference scattering arising from the structural response of the solvent to changes in the hydrodynamic parameters: pressure, temperature and density. We...... is demonstrated to exhibit first order behaviour with respect to the amount of energy deposited in the solution. We introduce a standardized method for recording solvent responses in laser pump, X-ray probe time-resolved X-ray wide-angle scattering experiments by using dye mediated solvent heating. Furthermore...

  7. Characterization of the Aqueous Uranyl-Silicate Complex Using X-Ray Absorption Spectroscopy and Ab Initio Modeling

    Science.gov (United States)

    Vu, M.; Massey, M.; Huang, P.

    2015-12-01

    The speciation of aqueous uranium ions is an important factor in predicting its mobility and fate in the environment. Two major controls on speciation are pH and the presence of complexing ligands. For the case of aqueous uranyl, UO22+(aq), some common complexes include uranyl-hydroxy, uranyl-carbonato, and uranyl-calcium-carbonato complexes, all of which differ in chemical reactivity and mobility. Uranyl-silicate complexes are also known but remain poorly characterized. In this work, we studied uranyl speciation in a series of aqueous solutions of 0.1 mM uranyl and 2 mM silicate with pH ranging from 4 to 7. Extended X-Ray Absorption Fine Structure (EXAFS) spectra of these samples were recorded at the Stanford Synchrotron Radiation Lightsource (SLAC National Accelerator Laboratory). Of particular note are the uranyl and silicate concentrations employed in our experiments, which are lower than conditions in previously reported EXAFS studies and approach conditions in natural groundwater systems. Preliminary analyses of EXAFS data indicate that uranyl speciation changes across the pH range, consistent with published thermodynamic data that suggest uranyl-silicate complexes may be important for pH ~ 5 and below, while uranyl-carbonato complexes become dominant at circumneutral pH. To guide the interpretation of the EXAFS data, molecular-scale simulations were carried out using density functional theory. We considered two classes of models: (i) hydrated clusters, and (ii) ab initio molecular dynamics simulations of 3D-periodic models involving uranyl and silicate in water. These calculations reveal that at pH ~ 5, the uranyl speciation is the [UO2(H2O)4H3SiO4]+ complex formed by the substitution of an equatorial uranyl water with a monodentate silicate ligand. The evidence from experiments and simulations provide a consistent picture for the uranyl-silicate complex, which may be important in the transport of uranyl in acidic, silicate-rich waters.

  8. 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.

  9. Solution synchrotron x-ray diffraction reveals structural details of lipid domains in ternary mixtures

    Science.gov (United States)

    Yuan, Jing; Kiss, Alexander; Pramudya, Yohanes H.; Nguyen, Lam T.; Hirst, Linda S.

    2009-03-01

    The influence of cholesterol on lipid bilayer structure is significant and the effect of cholesterol on lipid sorting and phase separation in lipid-raft-forming model membrane systems has been well investigated by microscopy methods on giant vesicles. An important consideration however is the influence of fluorescence illumination on the phase state of these lipids and this effect must be carefully minimized. In this paper, we show that synchrotron x-ray scattering on solution lipid mixtures is an effective alternative technique for the identification and characterization of the lo (liquid ordered) and ld (liquid disordered) phases. The high intensity of synchrotron x rays allows the observation of up to 5 orders of diffraction from the lo phase, whereas only two are clearly visible when the ld phase alone is present. This data can be collected in ˜1min/sample , allowing rapid generation of phase data. In this paper, we measure the lamellar spacing in both the liquid-ordered and liquid-disordered phases simultaneously, as a function of cholesterol concentration in two different ternary mixtures. We also observe evidence of a third gel-phaselike population at 10-12mol% cholesterol and determine the thickness of the bilayer for this phase. Importantly we are able to look at phase coexistence in the membrane independent of photoeffects.

  10. Solution Synchrotron X-ray Diffraction Reveals Structural Details of Lipid Domains in Ternary Mixtures

    Energy Technology Data Exchange (ETDEWEB)

    Yuan, J.; Kiss, A; Pramudya, Y; Nguyen, L; Hirst, L

    2009-01-01

    The influence of cholesterol on lipid bilayer structure is significant and the effect of cholesterol on lipid sorting and phase separation in lipid-raft-forming model membrane systems has been well investigated by microscopy methods on giant vesicles. An important consideration however is the influence of fluorescence illumination on the phase state of these lipids and this effect must be carefully minimized. In this paper, we show that synchrotron x-ray scattering on solution lipid mixtures is an effective alternative technique for the identification and characterization of the l o (liquid ordered) and l d (liquid disordered) phases. The high intensity of synchrotron x rays allows the observation of up to 5 orders of diffraction from the l o phase, whereas only two are clearly visible when the l d phase alone is present. This data can be collected in approximately 1 min/sample, allowing rapid generation of phase data. In this paper, we measure the lamellar spacing in both the liquid-ordered and liquid-disordered phases simultaneously, as a function of cholesterol concentration in two different ternary mixtures. We also observe evidence of a third gel-phaselike population at 10-12 mol % cholesterol and determine the thickness of the bilayer for this phase. Importantly we are able to look at phase coexistence in the membrane independent of photoeffects.

  11. Uranium and plutonium solution assays by transmission-corrected x-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Ryon, R W; Ruhter, W D; Rudenko, V; Sirontinin, A; Petrov, A A

    1999-09-08

    We have refined and tested a previously developed x-ray fluorescence analysis technique for uranium and plutonium solutions that compensates for variations in the absorption of the exciting gamma rays and fluorescent x-rays. We use {sup 57}Co to efficiently excite the K lines of the elements, and a mixed {sup 57}Co plus {sup 153}Gd transmission source to correct for variations in absorption. The absorption correction is a unique feature of our technique. It is possible to accurately calibrate the system with a single solution standard. There does not need to be a close match in composition (i.e., absorption) between the standard(s) and solutions to be analyzed. Specially designed equipment incorporates a planar intrinsic germanium detector, excitation and transmission radioisotopes, and specimen holder. The apparatus can be inserted into a rubber glove of a glovebox, keeping the apparatus outside and the solutions inside the glovebox, thereby protecting the user and the equipment from possible contamination. An alternate design may be used in chemical reprocessing plants, providing continuous monitoring, by measuring the trans-actinides through stainless steel piping. This technique has been tested at the Bochvar Research Institute of Inorganic Materials in Moscow for possible use in the Russian complex of nuclear facilities. This is part of a cooperative program between laboratories in the United States and Russia to strengthen systems of nuclear materials protection, control, and accountability (MPC and A). A part of this program is to accurately measure and track inventories of materials, thus the need for good non-destructive analytical techniques such as the one described here.

  12. Aqueous phase synthesis of upconversion nanocrystals through layer-by-layer epitaxial growth for in vivo X-ray computed tomography

    KAUST Repository

    Li, Feifei

    2013-05-21

    Lanthanide-doped core-shell upconversion nanocrystals (UCNCs) have tremendous potential for applications in many fields, especially in bio-imaging and medical therapy. As core-shell UCNCs are mostly synthesized in organic solvents, tedious organic-aqueous phase transfer processes are usually needed for their use in bio-applications. Herein, we demonstrate the first example of one-step synthesis of highly luminescent core-shell UCNCs in the "aqueous" phase under mild conditions using innocuous reagents. A microwave-assisted approach allowed for layer-by-layer epitaxial growth of a hydrophilic NaGdF4 shell on NaYF4:Yb, Er cores. During this process, surface defects of the nanocrystals could be gradually passivated by the homogeneous shell deposition, resulting in obvious enhancement in the overall upconversion emission efficiency. In addition, the up-down conversion dual-mode luminescent NaYF4:Yb, Er@NaGdF4:Ce, Ln (Eu, Tb, Sm, Dy) nanocrystals were also synthesized to further validate the successful formation of the core-shell structure. More significantly, based on their superior solubility and stability in water solution, high upconversion efficiency and Gd-doped predominant X-ray absorption, the as-prepared NaYF4:Yb, Er@NaGdF4 core-shell UCNCs exhibited high contrast in in vitro cell imaging and in vivo X-ray computed tomography (CT) imaging, demonstrating great potential as multiplexed luminescent biolabels and CT contrast agents.

  13. Extracting water and ion distributions from solution x-ray scattering experiments.

    Science.gov (United States)

    Nguyen, Hung T; Pabit, Suzette A; Pollack, Lois; Case, David A

    2016-06-01

    Small-angle X-ray scattering measurements can provide valuable information about the solvent environment around biomolecules, but it can be difficult to extract solvent-specific information from observed intensity profiles. Intensities are proportional to the square of scattering amplitudes, which are complex quantities. Amplitudes in the forward direction are real, and the contribution from a solute of known structure (and from the waters it excludes) can be estimated from theory; hence, the amplitude arising from the solvent environment can be computed by difference. We have found that this "square root subtraction scheme" can be extended to non-zero q values, out to 0.1 Å(-1) for the systems considered here, since the phases arising from the solute and from the water environment are nearly identical in this angle range. This allows us to extract aspects of the water and ion distributions (beyond their total numbers), by combining experimental data for the complete system with calculations for the solutes. We use this approach to test molecular dynamics and integral-equation (3D-RISM (three-dimensional reference interaction site model)) models for solvent structure around myoglobin, lysozyme, and a 25 base-pair duplex DNA. Comparisons can be made both in Fourier space and in terms of the distribution of interatomic distances in real space. Generally, computed solvent distributions arising from the MD simulations fit experimental data better than those from 3D-RISM, even though the total small-angle X-ray scattering patterns are very similar; this illustrates the potential power of this sort of analysis to guide the development of computational models. PMID:27276943

  14. X-ray solution scattering of An α-amylase inhibitor from wheat indicates the presence of a long shaped tetramer in solution

    International Nuclear Information System (INIS)

    Full text. Triticum aestivum (wheat) grains have a large variety of α-amylase inhibitors. One of them, highly active against human salivary α-amylase, was extracted and purified according to the method described by Granum and Whitaker (J. Food Bioc., 1,385-401,1977). The protein was crystallized and its diffraction data suggested strongly the presence of a tetramer in the asymmetric unit with local symmetry 222 (Acta Cryst. D, submitted). A parallel X-ray solution scattering experiment has been performed using an aqueous solution at 5mg/mL concentration. The obtained data was used for a shape determination (Svergun, Acta Cryst. A50, 391-402, 1994), which revealed an elongated particle with dimensions 85 x 40 x 35 A. (author)

  15. Precipitation of neptunium dioxide from aqueous solution

    Energy Technology Data Exchange (ETDEWEB)

    Roberts, K E

    1999-12-01

    Tens of thousands of metric tons of highly radioactive, nuclear waste have been generated in the US. Currently, there is no treatment or disposal facility for these wastes. Of the radioactive elements in high-level nuclear waste, neptunium (Np) is of particular concern because it has a long half-life and may potentially be very mobile in groundwaters associated with a proposed underground disposal site at Yucca Mountain, Nevada. Aqueous Np concentrations observed in previous, short-term solubility experiments led to calculated potential doses exceeding proposed long-term regulatory limits. However, thermodynamic data for Np at 25 C showed that these observed aqueous Np concentrations were supersaturated with respect to crystalline NpO{sub 2}. It was hypothesized that NpO{sub 2} is the thermodynamically stable solid phase in aqueous solution, but it is slow to form in an aqueous solution of NpO{sub 2}{sup +} on the time scale of previous experiments. The precipitation of NpO{sub 2} would provide significantly lower aqueous Np concentrations leading to calculated doses below proposed regulatory limits. To test this hypothesis, solubility experiments were performed at elevated temperature to accelerate any slow precipitation kinetics. Ionic NpO{sub 2}{sup +} (aq) was introduced into very dilute aqueous solutions of NaCl with initial pH values ranging from 6 to 10. The reaction vessels were placed in an oven and allowed to react at 200 C until steady-state aqueous Np concentrations were observed. In all cases, aqueous Np concentrations decreased significantly from the initial value of 10{sup {minus}4} M. The solids that formed were analyzed by x-ray powder diffraction, x-ray absorption spectroscopy, and scanning electron microscopy. The solids were determined to be high-purity crystals of NpO{sub 2}. This is the first time that crystalline NpO{sub 2} has been observed to precipitate from NpO{sub 2}{sup +}(aq) in near-neutral aqueous solutions. The results obtained

  16. K-edge x-ray fluorescence analysis for actinide and heavy elements solution concentration measurements

    International Nuclear Information System (INIS)

    Advantages of using Co-57 as an exciter for K XRFA include: a compact design that requires no x-ray tubes; the exciter-detector assembly locates remote from support electronics; on-line, at-line, or off-line configurations for monitor/measurements; systems that can be run by semi-skilled technicians, once programmed; and operated via remote terminals with results sent to control rooms; heavy element concentrations that are measurable thru industrial pipes; independent of minor changes in solution matrix or source half life with concentration results reported in near-real-time; a dynamic range of measurable concentrations that is greater than 104; measurement times that are reasonable even at 1 gram/liter; and for nuclear safeguards, it provides the <0.5% accuracy required by DOE for the accountability of U, Pu, or both, once the system is calibrated

  17. X-ray computed tomography system for laboratory small-object imaging: Enhanced tomography solutions.

    Science.gov (United States)

    Kharfi, F; Yahiaoui, M L; Boussahoul, F

    2015-07-01

    A portable X-ray tomography system has been installed and actually being tested at our medical imaging laboratory. This tomography system employs a combination of scintillator screen and CCD camera as image detector. The limit of spatial resolution of 290 μm of this imaging system is determined by the establishment of its modulation transfer function (MTF). In this work, we present attempts to address some issues such as limited resolution and low contrast through the development of affordable post-acquisition solutions based on the application of super-resolution method (projection onto convex sets, POCS) to create new projections set enabling the reconstruction of an improved 3D image in terms of contrast, resolution and noise. In addition to small-object examination, this tomography system is used for hands-on training activities involving students and scientists.

  18. Aqueous polyethylene oxide solutions

    International Nuclear Information System (INIS)

    A number of aspects concerning the reorientation of polymer, water and ion hydration complexes have been studied in aqueous solution of polyethylene oxide (PEO). The polymer dynamics are investigated by 1H-PEO and 13C-PEO nuclear relaxation experiments. 162 refs.; 30 figs.; 19 tabs

  19. Treatment of Aqueous Solutions

    NARCIS (Netherlands)

    Van Spronsen, J.; Witkamp, G.J.

    2013-01-01

    The invention is directed to a process for the recovery or removal of one or more crystallizable compounds from an aqueous solution containing, apart from the said crystallizable compounds, one or more organic or inorganic scale- forming or scale-inducing materials having a lower solubility in water

  20. Astrophysical parameters and orbital solution of the peculiar X-ray transient IGR J00370+6122

    Science.gov (United States)

    González-Galán, A.; Negueruela, I.; Castro, N.; Simón-Díaz, S.; Lorenzo, J.; Vilardell, F.

    2014-06-01

    Context. BD + 60° 73 is the optical counterpart of the X-ray source IGR J00370+6122, a probable accretion-powered X-ray pulsar. The X-ray light curve of this binary system shows clear periodicity at 15.7 d, which has been interpreted as repeated outbursts around the periastron of an eccentric orbit. Aims: We aim to characterise the binary system IGR J00370+6122 by deriving its orbital and physical parameters. Methods: We obtained high-resolution spectra of BD + 60° 73 at different epochs. We used the fastwind code to generate a stellar atmosphere model to fit the observed spectrum and obtain physical magnitudes. The synthetic spectrum was used as a template for cross-correlation with the observed spectra to measure radial velocities. The radial velocity curve provided an orbital solution for the system. We also analysed the RXTE/ASM and Swift/BAT light curves to confirm the stability of the periodicity. Results: BD + 60° 73 is a BN0.7 Ib low-luminosity supergiant located at a distance ~3.1 kpc, in the Cas OB4 association. We derive Teff = 24 000 K and log gc = 3.0, and chemical abundances consistent with a moderately high level of evolution. The spectroscopic and evolutionary masses are consistent at the 1-σ level with a mass M∗ ≈ 15 M⊙. The recurrence time of the X-ray flares is the orbital period of the system. The neutron star is in a high-eccentricity (e = 0.56 ± 0.07) orbit, and the X-ray emission is strongly peaked around orbital phase φ = 0.2, though the observations are consistent with some level of X-ray activity happening at all orbital phases. Conclusions: The X-ray behaviour of IGR J00370+6122 is reminiscent of "intermediate" supergiant X-ray transients, though its peak luminosity is rather low. The orbit is somewhat wider than those of classical persistent supergiant X-ray binaries, which when combined with the low luminosity of the mass donor, explains the low X-ray luminosity. IGR J00370+6122 will very likely evolve towards a persistent

  1. State-Dependent Electron Delocalization Dynamics at the Solute-Solvent Interface: Soft X-ray Absorption Spectroscopy and Ab Initio Calculations

    CERN Document Server

    Bokarev, Sergey I; Suljoti, Edlira; Kühn, Oliver; Aziz, Emad F

    2013-01-01

    Non-radiative decay channels in the L-edge fluorescence spectra from transition metal-aqueous solutions give rise to spectral dips in X-ray transmission spectra. Their origin is unraveled here using partial and inverse partial fluorescence yields on the micro-jet combined with multi-reference ab initio electronic structure calculations. Comparing Fe2+, Fe3+, and Co2+ systems we demonstrate unequivocally that spectral dips are due to a state-dependent electron delocalization within the manifold of d-orbitals.

  2. 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

  3. Particle-induced x-ray emission: Instrumentation, calibration, and application to contact lens solutions and fulvic acid solutions

    Energy Technology Data Exchange (ETDEWEB)

    Jenson, D.D.

    1989-01-01

    An expression was derived describing the profile of the proton beam at the PIXE target position. The expression was used to predict the profile for several experimental configurations. The profile was experimentally measured. The PIXE system was calibrated using solutions and commercial foils. Experimental data was adjusted for all absorbers and interferences, and a quadratic relationship was determined relating calibration factor and atomic number for each series of X-ray transitions. Calibration factors were determined for all elements above aluminum, for both a pinhole filter and a 14-mil mylar filter. A group of contact lens solutions was analyzed using PIXE, ICP, and ISE. A digestion method was developed for removal. of chloride ion. Cluster analysis was used to classify the data. A commercial humic acid was separated into three fractions. The fulvic acid was characterized, and separations of metal-fulvic acid complexes from metal ions in solution were attempted using ultrafiltration.

  4. X-ray imager using solution processed organic transistor arrays and bulk heterojunction photodiodes on thin, flexible plastic substrate

    NARCIS (Netherlands)

    Gelinck, G.H.; Kumar, A.; Moet, D.; Steen, J.L. van der; Shafique, U.; Malinowski, P.E.; Myny, K.; Rand, B.P.; Simon, M.; Rütten, W.; Douglas, A.; Jorritsma, J.; Heremans, P.L.; Andriessen, H.A.J.M.

    2013-01-01

    We describe the fabrication and characterization of large-area active-matrix X-ray/photodetector array of high quality using organic photodiodes and organic transistors. All layers with the exception of the electrodes are solution processed. Because it is processed on a very thin plastic substrate o

  5. ``Ordered'' structure in dilute solutions of sodium polystyrenesulfonates as studied by small-angle x-ray scattering

    Science.gov (United States)

    Ise, Norio; Okubo, Tsuneo; Kunugi, Shigeru; Matsuoka, Hideki; Yamamoto, K.; Ishii, Yasuo

    1984-10-01

    The small angle x-ray scattering measurements were performed for aqueous solutions of sodium polystyrenesulfonates having relatively narrow molecular weight distributions. As was observed for other synthetic macroions, polynucleotide and proteins, a single, broad peak was observed. The scattering vector at the peak position (Sm) was shifted toward larger values with increasing polymer concentration and toward lower values with increasing salt concentration, which confirmed earlier observations with polyacrylate and poly-L-lysine. The molecular weight dependence of the scattering behavior, which was earlier observed, was confirmed to be true for samples with Mw of 74 000, 18 000, and 4600. The mixture of two fractions with different Mw's gave a scattering curve which was again different from the composite curve obtained with the parent curves before mixing. A similar situation was observed for the mixture of polystyrenesulfonate and polyacrylate. Thus, it was concluded that the observed single peak indicates the presence of an intermolecular ordering, not an intramolecular ordering. The intermacroion distance (2Dexp) was thus calculated by using the Bragg equation. 2Dexp decreased with increasing polymer concentration and increased (not decreased) with increasing concentration of added salt and Mw. The 2Dexp values thus obtained were smaller beyond the experimental error than 2D0, a theoretical distance calculated from the concentration by assuming the uniform distribution of the macroions throughout the solution and the 2D0/2Dexp value amounted to 3.5 for high molecular weight samples. This fact indicates the presence of an intermacroion attractive interaction. When two fractions with different Mw's were compared at a given number concentration of macroions, the 2Dexp value for the sample of a larger Mw was smaller than that for the fraction of a smaller Mw. This implies that the attraction must be intensified, though unexpectedly, with increasing valency of the

  6. Solution of the inverse problem of images reconstruction by the X-ray phase contrast method

    International Nuclear Information System (INIS)

    In the approximation of geometrical optics of the wave theory of X-ray diffraction an inverse problem of reconstruction of an internal structure of objects on the base of data of X-ray phase contrast method with the crystal-analyzer, located in Bragg geometry is analytically solved. It is shown, that the approximation of geometrical optics is fair, if the characteristic sizes of object exceed radius of the first Fresnel zone and the extinction length

  7. X-ray absorption studies of graphite intercalates and metal-ammonia solutions

    International Nuclear Information System (INIS)

    X-ray absorption spectroscopy (XAS) was used to study the arsenic fluorocomplexes, including the AsF5 and AsF6- intercalates of graphite, and rubidium metal-ammonia solutions. The As-F distances obtained for AsF3 and AsF5 gas are both in excellent agreement with electron diffraction data (within 0.004 A). A superior measurement which is significantly shorter than the accepted value of the bond distance in an undistorted AsF6- octahedra is reported. Both the XAES and EXAFS data presented support the hypothesis that the AsF5 oxidizes graphite upon intercalation to produce AsF6- and AsF3 intercalant species. Changes in the Rb K-edge features which are consistent with the known properties of Rb-NH3 are correlated with conductivity and delocalization of the solvated electrons. In the XAES region, intensity and position changes of absorption transitions are explained. In the EXAFS region, the Rb-N bond distance and the relative number of nitrogen atoms in the first shell are measured. XAS has been shown to provide unique information about the nature of the metal-ammonia phase separation, phase transition, and density fluctuations

  8. Observing Solvation Dynamics with Simultaneous Femtosecond X-ray Emission Spectroscopy and X-ray Scattering

    DEFF Research Database (Denmark)

    Haldrup, Kristoffer; Gawelda, Wojciech; Abela, Rafael;

    2016-01-01

    rearrangement of the solute with X-ray emission spectroscopy, thus establishing time zero for the ensuing X-ray diffuse scattering analysis. The simultaneously recorded X-ray diffuse scattering atterns reveal slower subpicosecond dynamics triggered by the intramolecular structural dynamics of the photoexcited......, confirming previous ab initio molecular dynamics simulations. Structural changes in the aqueous solvent associated with density and temperature changes occur with similar to 1 ps time constants, characteristic for structural dynamics in water. This slower time scale of the solvent response allows us...

  9. 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.

  10. Influence of supersaturation on structure of sodium aluminate solutions with medium concentration: a solution X-ray diffraction study

    Institute of Scientific and Technical Information of China (English)

    李洁; 陈启元; 尹周澜; 张平民; 李元高

    2002-01-01

    Influence of supersaturation on the structure of a series of freshly prepared supersaturated sodium aluminate solutions with medium concentration was investigated by solution X-ray diffraction. Experimental results show that the basic Al-containing species in all kinds of supersaturated solution is four-coordinated ions. Opposite to Al-O distance contracted in highly concentrated solution, a little expand of the Al-O distance from 1.75 to 1.85 occurs with increasing supersaturation, which is consistent with the occurrence of oligomeric aluminate species. Meanwhile, O-O distance in the first shell of H2O-H2O(OH) in supersaturated sodium aluminate solution is obviously longer than in hydroxide sodium solution and becomes longer and longer with increasing supersaturation. Na-O bond length is about 2.4 and changes little with supersaturation. The reason for Al-O bond expanding with supersaturation and its influence on the stability of solution was discussed.

  11. Precipitation of gold by the reaction of aqueous gold(III)-chloride with cyanobacteria at 25-80 C -- Studied by x-ray absorption spectroscopy

    International Nuclear Information System (INIS)

    The mechanisms of gold precipitation by the interaction of cyanobacteria (Plectonema boryanum UTEX 485) and gold(III) chloride aqueous solutions (7.6 mmol/L final gold) have been studied at 25, 60, and 80 C, using both laboratory and real-time synchrotron radiation absorption spectroscopy experiments. Addition of aqueous gold(III) chloride to the cyanobacterial culture initially promoted the precipitation of amorphous gold(I) sulfide at the cell walls and finally caused the formation of octahedral (111) platelets (<1 to 6 (micro)m) of gold metal near cell surfaces and in solutions. X-ray absorption spectroscopy results confirmed that the reduction mechanism of gold(III) chloride to elemental gold by cyanobacteria involves the formation of an intermediate Au(I) species, gold(I) sulfide, with sulfur originating from cyanobacterial proteins, presumably cysteine or methionine. Although the bioreduction of gold(III) chloride to gold(I) sulfide was relatively rapid at all temperatures, the reaction rate increased with the increase in temperature. At the completion of the experiments, elemental gold was the major species present at all temperatures

  12. Calibration of X-ray densitometers for the determination of uranium and plutonium concentrations in reprocessing input and product solutions

    International Nuclear Information System (INIS)

    In June 1985 a calibration exercise has been carried out, which included the calibration of the KfK K-Edge Densitometer for uranium assay in the uranium product solutions from reprocessing, and the calibration of the Hybrid K-Edge/K-XRF Instrument for the determination of total uranium and plutonium in reprocessing input solutions. The calibration measuremnts performed with the two X-ray densitometers are described and analyzed, and calibration constants are evaluated from the obtained results. (orig.)

  13. X-ray Emission from Eta Carinae near Periastron in 2009 I: A Two State Solution

    CERN Document Server

    Hamaguchi, Kenji; Russell, Christopher; Pollock, Andrew M T; Gull, Theodore R; Teodoro, Mairan; Madura, Thomas I; Damineli, Augusto; Pittard, Julian M

    2014-01-01

    X-ray emission from the supermassive binary system Eta Carinae declines sharply around periastron. This X-ray minimum has two distinct phases - the lowest flux phase in the first ~3 weeks and a brighter phase thereafter. In 2009, the Chandra X-ray Observatory monitored the first phase five times and found the lowest observed flux at ~1.9e-12 ergs cm-2 s-1 (3-8 keV). The spectral shape changed such that the hard band above ~4 keV dropped quickly at the beginning and the soft band flux gradually decreased to its lowest observed value in ~2 weeks. The hard band spectrum had begun to recover by that time. This spectral variation suggests that the shocked gas producing the hottest X-ray gas near the apex of the wind-wind collision (WWC) is blocked behind the dense inner wind of the primary star, which later occults slightly cooler gas downstream. Shocked gas previously produced by the system at earlier orbital phases is suggested to produce the faint residual X-ray emission seen when the emission near the apex is ...

  14. In-Situ Synchrotron X-ray Study of the Phase and Texture Evolution of Ceria and Superconductor Films Deposited by Chemical Solution Method

    DEFF Research Database (Denmark)

    Yue, Zhao; Grivel, Jean-Claude; He, Dong;

    2012-01-01

    In situ synchrotron x-ray diffraction is used to study the phase and texture formation of ceria based films and superconductor films deposited by the chemical solution method on technical substrates. Combined analysis using in situ synchrotron x-ray diffraction, thermogravimetry/differential ther......In situ synchrotron x-ray diffraction is used to study the phase and texture formation of ceria based films and superconductor films deposited by the chemical solution method on technical substrates. Combined analysis using in situ synchrotron x-ray diffraction, thermogravimetry...

  15. X-ray Emission From Eta Carinae near Periastron in 2009 I: A Two State Solution

    Science.gov (United States)

    Hamaguchi, Kenji; Corcoran, Michael F.; Russell, Christopher; Pollock, Andrew M. T.; Gull, Theodore R.; Teodoro, Mairan; Madura, Thomas I.; Damineli, Augusto; Pittard, Julian M.

    2014-01-01

    X-ray emission from the supermassive binary system Eta Carinae declines sharply around periastron. This X-ray minimum has two distinct phases the lowest flux phase in the first 3 weeks and a brighter phase thereafter. In 2009, the Chandra X-ray Observatory monitored the first phase five times and found the lowest observed flux at 1.91012 ergs/sq cm/s (38 keV). The spectral shape changed such that the hard band above 4 keV dropped quickly at the beginning and the soft band flux gradually decreased to its lowest observed value in 2 weeks. The hard band spectrum had begun to recover by that time. This spectral variation suggests that the shocked gas producing the hottest X-ray gas near the apex of the wind-wind collision (WWC) is blocked behind the dense inner wind of the primary star, which later occults slightly cooler gas down-stream. Shocked gas previously produced by the system at earlier orbital phases is suggested to produce the faint residual X-ray emission seen when the emission near the apex is completely blocked by the primary wind. The brighter phase is probably caused by the re-appearance of the WWC plasma, whose emissivity significantly declined during the occultation. We interpret this to mean that the X-ray minimum is produced by a hybrid mechanism of an occultation and a decline in emissivity of the WWC shock. We constrain timings of superior conjunction and periastron based on these results.

  16. Polycrystalline lead iodide films produced by solution evaporation and tested in the mammography X-ray energy range

    Science.gov (United States)

    Condeles, J. F.; Mulato, M.

    2016-02-01

    Lead iodide polycrystalline films have been deposited on corning glass substrates using solution evaporation in oven. Films 6 μm-thick were obtained with full coverage of the substrates as verified by scanning electron microscopy. Some pin-holes were observable. X-ray diffraction revealed a crystalline structure corresponding to the 4 H-PbI2 polytype formation. Polarized Raman scattering experiments indicated a lamellar structure. Anisotropy was also investigated using depolarization ratio calculations. The optical and electrical properties of the samples were investigated using photoluminescence and dark conductivity as a function of temperature, respectively. Activation energies of 0.10 up to 0.89 eV were related to two main electrical transport mechanisms. Films were also exposed to X-ray irradiation in the mammography X-ray energy range. The detector produced was also exposed to X-ray from 5 mR up to 1450 mR. A linear response was observed as a function of dose with a slope of 0.52 nA/mm2 per mR.

  17. X-ray characterization of tripyridinium bis[tetrabromidoferrate(III)] bromide asymmetric unit in solution by Debye function analysis

    Science.gov (United States)

    Baniasadi, F.; Sahraei, N.; Fathi, M. B.; Tehranchi, M. M.; Safari, N.; Amani, V.

    2016-09-01

    Abundant asymmetric unit of the [FeBr4]2[py.H]3Br magnetic molecule in the acetonitrile solvent was characterized via Debye function analysis (DFA) of the X-ray powder diffraction pattern from dilute solution. A diluted solution of the material in acetonitrile solvent has been prepared to reduce, as far as possible, the interaction between the molecular units. The X-ray diffraction from the sample was measured and Debye function simulations of three out of ten chemically plausible molecular units were observed to suitably comply with the experimental results. These three configurations were further optimized with first-principles method in the framework of density functional theory (DFT) and the most stable structure according to the calculated total energy is presented.

  18. Determination of Fe, Cr, Ni, and Sn in zircaloy-2 by solution method of fluorescent x-ray analysis

    International Nuclear Information System (INIS)

    The rapid solution method of fluorescent X-ray analysis of the alloying elements contained in Zircaloy-2 was studied. The preparation of standard samples and the analytical procedure are presented. A portion of the solution of a sample dissolved in nitric acid-hydrofluoric acid was measured in the stream of helium with an X-ray fluorescent instrument. The resulting counts were compared with those of the calibration curve obtained from the synthesized standard samples, and the amount of each element was consequently determined. The results obtained agreed quite well with the certificated value of each standard. Therefore, the method has been proved to be satisfactory for the control analysis of Zircaloy-2. (Nishino, S.)

  19. Analysis of the aggregation structure from amphiphilic block copolymers in solutions by small-angle x-ray scattering

    CERN Document Server

    Rong Li Xia; Wang Jun; Wei Liu He; Li Fu Mian; Li Zi Chen

    2002-01-01

    The aggregation structure of polystyrene-p vinyl benzoic amphiphilic block copolymers which were prepared in different conditions was investigated by synchrotron radiation small-angle x-ray scattering (SAXS). The micelle was self-assembled in selective solvents of the block copolymers. Authors' results demonstrate that the structure of the micelle depends on the factors, such as the composition of the copolymers, the nature of the solvent and the concentration of the solution

  20. Numerical Solution of the Radiative Transfer Equation: X-Ray Spectral Formation from Cylindrical Accretion onto a Magnetized Neutron Star

    Science.gov (United States)

    Fairnelli, R.; Ceccobello, C.; Romano, P.; Titarchuk, L.

    2011-01-01

    Predicting the emerging X-ray spectra in several astrophysical objects is of great importance, in particular when the observational data are compared with theoretical models. This requires developing numerical routines for the solution of the radiative transfer equation according to the expected physical conditions of the systems under study. Aims. We have developed an algorithm solving the radiative transfer equation in the Fokker-Planck approximation when both thermal and bulk Comptonization take place. The algorithm is essentially a relaxation method, where stable solutions are obtained when the system has reached its steady-state equilibrium. Methods. We obtained the solution of the radiative transfer equation in the two-dimensional domain defined by the photon energy E and optical depth of the system pi using finite-differences for the partial derivatives, and imposing specific boundary conditions for the solutions. We treated the case of cylindrical accretion onto a magnetized neutron star. Results. We considered a blackbody seed spectrum of photons with exponential distribution across the accretion column and for an accretion where the velocity reaches its maximum at the stellar surface and at the top of the accretion column, respectively. In both cases higher values of the electron temperature and of the optical depth pi produce flatter and harder spectra. Other parameters contributing to the spectral formation are the steepness of the vertical velocity profile, the albedo at the star surface, and the radius of the accretion column. The latter parameter modifies the emerging spectra in a specular way for the two assumed accretion profiles. Conclusions. The algorithm has been implemented in the XPEC package for X-ray fitting and is specifically dedicated to the physical framework of accretion at the polar cap of a neutron star with a high magnetic field (approx > 10(exp 12) G). This latter case is expected to be of typical accreting systems such as X-ray

  1. Instability of Solution of Phase Retrieval in Direct Diffraction Phase-Contrast Imaging with Partially Coherent X-Ray Source

    Institute of Scientific and Technical Information of China (English)

    GUO Hua; HAN Shen-Sheng

    2006-01-01

    The theoretical model of direct diffraction phase-contrast imaging with partially coherent x-ray source is expressedby an operator of multiple integral. It is presented that the integral operator is linear. The problem of its phaseretrieval is described by solving an operator equation of multiple integral. It is demonstrated that the solution ofthe phase retrieval is unstable. The numerical simulation is performed and the result validates that the solutionof the phase retrieval is unstable.

  2. X-Ray Solution Scattering Study of Four Escherichia coli Enzymes Involved in Stationary-Phase Metabolism.

    Directory of Open Access Journals (Sweden)

    Liubov A Dadinova

    Full Text Available The structural analyses of four metabolic enzymes that maintain and regulate the stationary growth phase of Escherichia coli have been performed primarily drawing on the results obtained from solution small angle X-ray scattering (SAXS and other structural techniques. The proteins are (i class I fructose-1,6-bisphosphate aldolase (FbaB; (ii inorganic pyrophosphatase (PPase; (iii 5-keto-4-deoxyuronate isomerase (KduI; and (iv glutamate decarboxylase (GadA. The enzyme FbaB, that until now had an unknown structure, is predicted to fold into a TIM-barrel motif that form globular protomers which SAXS experiments show associate into decameric assemblies. In agreement with previously reported crystal structures, PPase forms hexamers in solution that are similar to the previously reported X-ray crystal structure. Both KduI and GadA that are responsible for carbohydrate (pectin metabolism and acid stress responses, respectively, form polydisperse mixtures consisting of different oligomeric states. Overall the SAXS experiments yield additional insights into shape and organization of these metabolic enzymes and further demonstrate the utility of hybrid methods, i.e., solution SAXS combined with X-ray crystallography, bioinformatics and predictive 3D-structural modeling, as tools to enrich structural studies. The results highlight the structural complexity that the protein components of metabolic networks may adopt which cannot be fully captured using individual structural biology techniques.

  3. Guanosine Quadruplexes in Solution: A Small-Angle X-Ray Scattering Analysis of Temperature Effects on Self-Assembling of Deoxyguanosine Monophosphate

    Directory of Open Access Journals (Sweden)

    P. Mariani

    2010-01-01

    Full Text Available We investigated quadruplex formation in aqueous solutions of 2′-deoxyriboguanosine 5′-monophosphate, d(pG, which takes place in the absence of the covalent axial backbone. A series of in-solution small angle X-ray scattering experiments on d(pG have been performed as a function of temperature in the absence of excess salt, at a concentration just above the critical one at which self-assembling occurs. A global fit approach has been used to derive composition and size distribution of the scattering particles as a function of temperature. The obtained results give thermodynamical justification for the observed phase-behavior, indicating that octamer formation is essential for quadruplex elongation. Our investigation shows that d(pG quadruplexes are very suitable to assess the potential of G-quadruplex formation and to study the self-assembling thermodynamics.

  4. Reciprocal Grids: A Hierarchical Algorithm for Computing Solution X-ray Scattering Curves from Supramolecular Complexes at High Resolution.

    Science.gov (United States)

    Ginsburg, Avi; Ben-Nun, Tal; Asor, Roi; Shemesh, Asaf; Ringel, Israel; Raviv, Uri

    2016-08-22

    In many biochemical processes large biomolecular assemblies play important roles. X-ray scattering is a label-free bulk method that can probe the structure of large self-assembled complexes in solution. As we demonstrate in this paper, solution X-ray scattering can measure complex supramolecular assemblies at high sensitivity and resolution. At high resolution, however, data analysis of larger complexes is computationally demanding. We present an efficient method to compute the scattering curves from complex structures over a wide range of scattering angles. In our computational method, structures are defined as hierarchical trees in which repeating subunits are docked into their assembly symmetries, describing the manner subunits repeat in the structure (in other words, the locations and orientations of the repeating subunits). The amplitude of the assembly is calculated by computing the amplitudes of the basic subunits on 3D reciprocal-space grids, moving up in the hierarchy, calculating the grids of larger structures, and repeating this process for all the leaves and nodes of the tree. For very large structures, we developed a hybrid method that sums grids of smaller subunits in order to avoid numerical artifacts. We developed protocols for obtaining high-resolution solution X-ray scattering data from taxol-free microtubules at a wide range of scattering angles. We then validated our method by adequately modeling these high-resolution data. The higher speed and accuracy of our method, over existing methods, is demonstrated for smaller structures: short microtubule and tobacco mosaic virus. Our algorithm may be integrated into various structure prediction computational tools, simulations, and theoretical models, and provide means for testing their predicted structural model, by calculating the expected X-ray scattering curve and comparing with experimental data. PMID:27410762

  5. Exploring hardness enhancement in superhard tungsten tetraboride-based solid solutions using radial X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Xie, Miao; Turner, Christopher L. [Department of Chemistry and Biochemistry, UCLA, Los Angeles, California 90095 (United States); Mohammadi, Reza [Department of Chemistry and Biochemistry, UCLA, Los Angeles, California 90095 (United States); Department of Materials Science and Engineering, UCLA, Los Angeles, California 90095 (United States); Kaner, Richard B., E-mail: kaner@chem.ucla.edu, E-mail: akavner@ucla.edu, E-mail: tolbert@chem.ucla.edu; Tolbert, Sarah H., E-mail: kaner@chem.ucla.edu, E-mail: akavner@ucla.edu, E-mail: tolbert@chem.ucla.edu [Department of Chemistry and Biochemistry, UCLA, Los Angeles, California 90095 (United States); Department of Materials Science and Engineering, UCLA, Los Angeles, California 90095 (United States); The California NanoSystems Institute (CNSI), UCLA, Los Angeles, California 90095 (United States); Kavner, Abby, E-mail: kaner@chem.ucla.edu, E-mail: akavner@ucla.edu, E-mail: tolbert@chem.ucla.edu [Department of Earth, Planetary, and Space Sciences, UCLA, Los Angeles, California 90095 (United States)

    2015-07-27

    In this work, we explore the hardening mechanisms in WB{sub 4}-based solid solutions upon addition of Ta, Mn, and Cr using in situ radial X-ray diffraction techniques under non-hydrostatic pressure. By examining the lattice-supported differential strain, we provide insights into the mechanism for hardness increase in binary solid solutions at low dopant concentrations. Speculations on the combined effects of electronic structure and atomic size in ternary WB{sub 4} solid solutions containing Ta with Mn or Cr are also included to understand the extremely high hardness of these materials.

  6. Exploring hardness enhancement in superhard tungsten tetraboride-based solid solutions using radial X-ray diffraction

    International Nuclear Information System (INIS)

    In this work, we explore the hardening mechanisms in WB4-based solid solutions upon addition of Ta, Mn, and Cr using in situ radial X-ray diffraction techniques under non-hydrostatic pressure. By examining the lattice-supported differential strain, we provide insights into the mechanism for hardness increase in binary solid solutions at low dopant concentrations. Speculations on the combined effects of electronic structure and atomic size in ternary WB4 solid solutions containing Ta with Mn or Cr are also included to understand the extremely high hardness of these materials

  7. Relaxation Processes in Aqueous Systems upon X-ray Ionization: Entanglement of Electronic and Nuclear Dynamics.

    Science.gov (United States)

    Slavíček, Petr; Kryzhevoi, Nikolai V; Aziz, Emad F; Winter, Bernd

    2016-01-21

    The knowledge of primary processes following the interaction of high-energy radiation with molecules in liquid phase is rather limited. In the present Perspective, we report on a newly discovered type of relaxation process involving simultaneous autoionization and proton transfer between adjacent molecules, so-called proton transfer mediated charge separation (PTM-CS) process. Within PTM-CS, transients with a half-transferred proton are formed within a few femtoseconds after the core-level ionization event. Subsequent nonradiative decay of the highly nonequilibrium transients leads to a series of reactive species, which have not been considered in any high-energy radiation process in water. Nonlocal electronic decay processes are surprisingly accelerated upon proton dynamics. Such strong coupling of electronic and nuclear dynamics is a general phenomenon for hydrogen-bonded systems, however, its probability correlates strongly with hydration geometry. We suggest that the newly observed processes will impact future high-energy radiation-chemistry-relevant modeling, and we envision application of autoionization spectroscopy for identification of solution structure details. PMID:26712083

  8. X-Ray Crystallography Reagent

    Science.gov (United States)

    Morrison, Dennis R. (Inventor); Mosier, Benjamin (Inventor)

    2003-01-01

    Microcapsules prepared by encapsulating an aqueous solution of a protein, drug or other bioactive substance inside a semi-permeable membrane by are disclosed. The microcapsules are formed by interfacial coacervation under conditions where the shear forces are limited to 0-100 dynes per square centimeter at the interface. By placing the microcapsules in a high osmotic dewatering solution. the protein solution is gradually made saturated and then supersaturated. and the controlled nucleation and crystallization of the protein is achieved. The crystal-filled microcapsules prepared by this method can be conveniently harvested and stored while keeping the encapsulated crystals in essentially pristine condition due to the rugged. protective membrane. Because the membrane components themselves are x-ray transparent, large crystal-containing microcapsules can be individually selected, mounted in x-ray capillary tubes and subjected to high energy x-ray diffraction studies to determine the 3-D smucture of the protein molecules. Certain embodiments of the microcapsules of the invention have composite polymeric outer membranes which are somewhat elastic, water insoluble, permeable only to water, salts, and low molecular weight molecules and are structurally stable in fluid shear forces typically encountered in the human vascular system.

  9. Improvement of a high pressure cell with diamond windows for solution X-ray scattering of proteins

    CERN Document Server

    Nishikawa, Y; Inoko, Y; Moritoki, M

    2001-01-01

    An improved high pressure (up to 500 MPa) cell with diamond windows was developed for small-angle X-ray scattering of protein solutions. When the diamond window was subjected to high pressure, many streaks of parasitic scattering appeared. By changing the wavelength and performing simulations, it was concluded that they are Kossel lines. In order to obtain quantitative scattering data, it is essential that Kossel lines do not interfere with the beamstop. The performance of the improved cell was tested by using Apo-ferritin solutions.

  10. Astrophysical parameters and orbital solution of the peculiar X-ray transient IGR J00370+6122

    CERN Document Server

    González-Galán, A; Castro, N; Simón-Díaz, S; Lorenzo, J; Vilardell, F

    2014-01-01

    BD+6073 is the optical counterpart of the X-ray source IGR J00370+6122, a probable accretion-powered X-ray pulsar. The X-ray light curve of this binary system shows clear periodicity at 15.7 d, which has been interpreted as repeated outbursts around the periastron of an eccentric orbit. We obtained high-resolution spectra of BD+6073 at different epochs. We used the FASTWind code to generate a stellar atmosphere model to fit the observed spectrum and obtain physical magnitudes. The synthetic spectrum was used as a template for cross-correlation with the observed spectra to measure radial velocities. The radial velocity curve provided an orbital solution for the system. We have also analysed the RXTE/ASM and Swift/BAT light curves to confirm the stability of the periodicity. BD +6073 is a BN0.7 Ib low-luminosity supergiant located at an approximate distance of 3.1 kpc, in the CasOB4 association. We derive Teff=24000 K and log gc=3.0, and chemical abundances consistent with a moderately high level of evolution. ...

  11. Determination of zirconium and hafnium in zirconium process stream solutions from Zirconium Extraction Plant by ED X-Ray Fluorescence Spectrometry (EDXRFS)

    International Nuclear Information System (INIS)

    Energy dispersive X-Ray fluorescence (EDXRFS) method is developed and standardized for the determination of Zr and Hf contents on routine basis in various process stream solutions covering a wide range of concentrations from Zirconium Extraction Plant at Nuclear Fuel Complex. From the results Zirconium Oxide (ZrO2) and Hafnium oxide (HfO2) were calculated for reporting purpose. The method has been applied to aqueous stream samples. Except for dilution, not much sample preparation was involved in the analysis and accordingly the experimental parameters were optimized. The results from EDXRFS method are compared with gravimetric (phallic acid precipitation) method and WDXRFS method and are found to be in good agreement. A RSD ≤ 2% has been achieved in both the cases. (author)

  12. Induced alignment of a solution-cast discotic hexabenzocoronene derivative for electronic devices investigated by surface X-ray diffraction

    DEFF Research Database (Denmark)

    Bunk, Oliver; Nielsen, Martin Meedom; Sølling, Theis Ivan;

    2003-01-01

    crystalline HBC-C8,2 majority phases result. In all three phases, the HBC-C8,2 molecules self-organize into columns which are uniaxially aligned along the direction defined by the PTFE macromolecules of the substrate. The three phases are quite similar, the major difference being their orientation......A surface X-ray diffraction study is presented showing that highly ordered and uniaxially aligned hexa(3,7-dimethyl-octanyl)hexa-peri-hexabenzocoronene (HBC-C8,2) films can be fabricated by crystallization from solution onto friction-transferred poly(tetrafluoroethylene) (PTFE) layers. Three...

  13. Study of an X-ray fluorescence thin film method for the determination of uranium in low activity solutions

    International Nuclear Information System (INIS)

    The application of the X-ray fluorescence thin film technique to the uranium determination in nitric solutions for a concentration range from 1 g/l to 100 g/l and activity levels under 5 mCi/ml is studied. The most suited excitation and measurement conditions are also studied and the uranium matrix effect correction, which is performed through the double dilution, αUU interaction coefficient calculation and internal standard methods, is discussed. The specimen preparation is satisfactorily accomplished by using P.V.C. filters fixed on aluminium supports. (Author) 18 refs

  14. Probing Reaction Dynamics of Transition-Metal Complexes in Solution via Time-Resolved X-ray Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Huse, Nils; Khalil, Munira; Kim, Tae Kyu; Smeigh, Amanda L.; Jamula, Lindsey; McCusker, James K.; Schoenlein, Robert W.

    2009-05-24

    We report measurements of the photo-induced Fe(II) spin crossover reaction dynamics in solution via time-resolved x-ray absorption spectroscopy. EXAFS measurements reveal that the iron?nitrogen bond lengthens by 0.21+-0.03 Angstrom in the high-spin transient excited state relative to the ground state. XANES measurements at the Fe L-edge show directly the influence of the structural change on the ligand-field splitting of the Fe(II) 3d orbitals associated with the spin transition.

  15. Probing reaction dynamics of transition-metal complexes in solution via time-resolved X-ray spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Huse, Nils [Chemical Sciences Division, Lawrence Berkeley National Laboratory, 1Cyclotron Road, Berkeley, CA 94720 (United States); Khalil, Munira [Department of Chemistry, University of Washington, Seattle, WA 98195 (United States); Kim, Tae Kyu [Department of Chemistry, Pusan National University, Busan 609-735 (Korea, Republic of); Smeigh, Amanda L; Jamula, Lindsey; McCusker, James K [Department of Chemistry, Michigan State University, East Lansing, MI 48824 (United States); Schoenlein, Robert W, E-mail: nhuse@lbl.go, E-mail: rwschoenlein@lbl.go [Materials Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, CA (United States)

    2009-02-01

    We report measurements of the photoinduced Fe{sup II} spin crossover reaction dynamics in solution via time-resolved x-ray absorption spectroscopy. EXAFS measurements reveal that the iron-nitrogen bond lengthens by 0.21+-0.03 A in the high-spin transient excited state relative to the ground state. XANES measurements at the Fe L-edge show directly the influence of the structural change on the ligand-field splitting of the Fe{sup II} 3d orbitals associated with the spin transition.

  16. Surface complexation and precipitate geometry for aqueous Zn(II) sorption on ferrihydrite I: X-ray absorption extended fine structure spectroscopy analysis

    Science.gov (United States)

    Waychunas, G.A.; Fuller, C.C.; Davis, J.A.

    2002-01-01

    "Two-line" ferrihydrite samples precipitated and then exposed to a range of aqueous Zn solutions (10-5 to 10-3 M), and also coprecipitated in similar Zn solutions (pH 6.5), have been examined by Zn and Fe K-edge X-ray absorption spectroscopy. Typical Zn complexes on the surface have Zn-O distances of 1.97(0.2) A?? and coordination numbers of about 4.0(0.5), consistent with tetrahedral oxygen coordination. This contrasts with Zn-O distances of 2.11(.02) A?? and coordination numbers of 6 to 7 in the aqueous Zn solutions used in sample preparation. X-ray absorption extended fine structure spectroscopy (EXAFS) fits to the second shell of cation neighbors indicate as many as 4 Zn-Fe neighbors at 3.44(.04) A?? in coprecipitated samples, and about two Zn-Fe neighbors at the same distance in adsorption samples. In both sets of samples, the fitted coordination number of second shell cations decreases as sorption density increases, indicating changes in the number and type of available complexing sites or the onset of competitive precipitation processes. Comparison of our results with the possible geometries for surface complexes and precipitates suggests that the Zn sorption complexes are inner sphere and at lowest adsorption densities are bidentate, sharing apical oxygens with adjacent edge-sharing Fe(O,OH)6 octahedra. Coprecipitation samples have complexes with similar geometry, but these are polydentate, sharing apices with more than two adjacent edge-sharing Fe(O,OH)6 polyhedra. The results are inconsistent with Zn entering the ferrihydrite structure (i.e., solid solution formation) or formation of other Zn-Fe precipitates. The fitted Zn-Fe coordination numbers drop with increasing Zn density with a minimum of about 0.8(.2) at Zn/(Zn + Fe) of 0.08 or more. This change appears to be attributable to the onset of precipitation of zinc hydroxide polymers with mainly tetrahedral Zn coordination. At the highest loadings studied, the nature of the complexes changes further

  17. Small-angle X-ray scattering study on pectin-chitosan mixed solutions and thermoreversible gels.

    Science.gov (United States)

    Ventura, Irit; Bianco-Peled, Havazelet

    2015-06-01

    Hot solutions containing pectin and chitosan with pectin weight fraction of 0.75, in acidic pH, demonstrate gelation occurring upon cooling to room temperature. This study explores the origin of this gelation using small angle X-ray scattering (SAXS) as the main experimental tool. Modeling SAXS patterns revealed rigid rod conformation in chitosan solutions, whereas pectin formed a self-avoiding chain. In addition, nanometric aggregates were detected in pectin solutions. Pectin and chitosan in mixed solutions adopted a similar semiflexible conformation. The only sample that created a visually stable gel displayed a different pattern, characteristic to polymers gels. Manipulating the composition by adding urea and salts highlighted the important role of hydrogen bonding, which governs the gelation mechanism. Nevertheless, electrostatic interactions were also found to take part in the gelation. To the best of our knowledge, this is the first comprehensive and systematic SAXS study on these pectin-chitosan mixtures.

  18. Radiation chemical effects of X-rays on liquids

    Energy Technology Data Exchange (ETDEWEB)

    Holroyd, R.A.; Preses, J.M.

    1998-11-01

    This review describes some of the chemical changes induced by photoelectrons which are released in liquids when X-rays are absorbed. Both experimental studies and theory are discussed. In part 1, the basic processes occurring upon absorption of X-rays are described. Parts 2 and 3 deal with hydrocarbon liquids; in part 2 the ion yields, including effects at K-edges, and in part 3, the yields of excited states. Part 4 discusses chemical effects of X-rays in aqueous solutions. The authors end with a summary of future needs and directions.

  19. X-ray CT-Derived Soil Characteristics Explain Varying Air, Water, and Solute Transport Properties across a Loamy Field

    DEFF Research Database (Denmark)

    Paradelo Pérez, Marcos; Katuwal, Sheela; Møldrup, Per;

    2016-01-01

    when the limiting macroporosity (the minimum macroporosity for every 0.6-mm layer along the soil column) was used, suggesting that soil layers with the narrowest macropore section restricted the flow through the whole soil column. Water, air, and solute transport were related with the CT......The characterization of soil pore space geometry is important for explaining fluxes of air, water, and solutes through soil and understanding soil hydrogeochemical functions. X-ray computed tomography (CT) can be applied for this characterization, and in this study CT-derived parameters were used...... to explain water, air, and solute transport through soil. Forty-five soil columns (20 by 20 cm) were collected from an agricultural field in Estrup, Denmark, and subsequently scanned using a medical CT scanner. Nonreactive tracer leaching experiments were performed in the laboratory along with measurements...

  20. PSSP, a Computer Program for the Crystal Structure Solution of Molecular Materials from X-ray Powder Diffraction Data

    Energy Technology Data Exchange (ETDEWEB)

    Pagola, S.; Stephens, P

    2010-01-01

    This work describes the computer program PSSP (powder structure solution program) for the crystal structure solution of molecular solids from X-ray powder diffraction data. This direct-space structure solution program uses the simulated annealing global optimization algorithm to minimize the difference between integrated intensities calculated from trial models and those extracted in a Le Bail fit of the experimental pattern, using a cost function for dealing with peak overlap through defined intensity correlation coefficients, computationally faster to calculate than R{sub wp}. The methodology outlined is applicable to organic solids composed of moderately complex rigid and flexible molecules, using diffraction data up to relatively low resolution. PSSP performance tests using 11 molecular solids with six to 20 degrees of freedom are analyzed.

  1. Numerical solution of the radiative transfer equation: X-ray spectral formation from cylindrical accretion onto a magnetized neutron star

    CERN Document Server

    Farinelli, R; Romano, P; Titarchuk, L

    2011-01-01

    Predicting the emerging X-ray spectra in several astrophysical objects is of great importance, in particular when the observational data are compared with theoretical models. To this aim, we have developed an algorithm solving the radiative transfer equation in the Fokker-Planck approximation when both thermal and bulk Comptonization take place. The algorithm is essentially a relaxation method, where stable solutions are obtained when the system has reached its steady-state equilibrium. We obtained the solution of the radiative transfer equation in the two-dimensional domain defined by the photon energy E and optical depth of the system tau using finite-differences for the partial derivatives, and imposing specific boundary conditions for the solutions. We treated the case of cylindrical accretion onto a magnetized neutron star. We considered a blackbody seed spectrum of photons with exponential distribution across the accretion column and for an accretion where the velocity reaches its maximum at the stellar...

  2. Red mercuric iodide crystals obtained by isothermal solution evaporation: Characterization for mammographic X-ray imaging detectors

    Energy Technology Data Exchange (ETDEWEB)

    Caldeira, A.M.F.; Ugucioni, J.C.; Mulato, M.

    2014-02-11

    Millimeter-sized mercury iodide crystals were obtained by the isothermal evaporation technique using dimethylformamide (DMF), diethyl-ether/DMF mixture and THF. Different concentrations (18 mM and 400 mM) and solution temperature (25–80 °C) were used to obtain varied evaporation rates (0.1×10{sup −4}–5000×10{sup −4} ml/h). Different crystal sizes and shapes were obtained by changing solvents, mixture and initial solution volume. According to X-ray diffraction the samples are monocrystalline. The top surface was investigated by SEM. Optical band-gaps above 2 eV were obtained from photoacoustic spectroscopy. Photoluminescence spectra indicated band-to-band electronic transitions, and the presence of sub-band gap states. Excitons, structural defects and the presence of impurities are discussed and correlated to the electrical measurements. Crystals obtained using pure DMF as solvent showed better general properties, including under the exposure to mammographic X-ray energy range that led to sensibility of about 25 μC/Rcm{sup 2}.

  3. Valence Electronic Structure of Aqueous Solutions: Insights from Photoelectron Spectroscopy

    Science.gov (United States)

    Seidel, Robert; Winter, Bernd; Bradforth, Stephen E.

    2016-05-01

    The valence orbital electron binding energies of water and of embedded solutes are crucial quantities for understanding chemical reactions taking place in aqueous solution, including oxidation/reduction, transition-metal coordination, and radiation chemistry. Their experimental determination based on liquid-photoelectron spectroscopy using soft X-rays is described, and we provide an overview of valence photoelectron spectroscopy studies reported to date. We discuss principal experimental aspects and several theoretical approaches to compute the measured binding energies of the least tightly bound molecular orbitals. Solutes studied are presented chronologically, from simple electrolytes, via transition-metal ion solutions and several organic and inorganic molecules, to biologically relevant molecules, including aqueous nucleotides and their components. In addition to the lowest vertical ionization energies, the measured valence photoelectron spectra also provide information on adiabatic ionization energies and reorganization energies for the oxidation (ionization) half-reaction. For solutes with low solubility, resonantly enhanced ionization provides a promising alternative pathway.

  4. Femtosecond laser-induced hard X-ray generation in air from a solution flow of Au nano-sphere suspension using an automatic positioning system.

    Science.gov (United States)

    Hsu, Wei-Hung; Masim, Frances Camille P; Porta, Matteo; Nguyen, Mai Thanh; Yonezawa, Tetsu; Balčytis, Armandas; Wang, Xuewen; Rosa, Lorenzo; Juodkazis, Saulius; Hatanaka, Koji

    2016-09-01

    Femtosecond laser-induced hard X-ray generation in air from a 100-µm-thick solution film of distilled water or Au nano-sphere suspension was carried out by using a newly-developed automatic positioning system with 1-µm precision. By positioning the solution film for the highest X-ray intensity, the optimum position shifted upstream as the laser power increased due to breakdown. Optimized positioning allowed us to control X-ray intensity with high fidelity. X-ray generation from Au nano-sphere suspension and distilled water showed different power scaling. Linear and nonlinear absorption mechanism are analyzed together with numerical modeling of light delivery. PMID:27607607

  5. Solution of the effects of twinning in femtosecond X-ray protein nanocrystallography

    International Nuclear Information System (INIS)

    With the development of the XFEL (X-ray free electron laser), high quality diffraction patterns from nanocrystals have been achieved. The nanocrystals with different sizes and random orientations are injected to the XFEL beams and the diffraction patterns can be obtained by the so-called diffraction-and-destruction mode. The recovery of orientations is one of the most critical steps in reconstructing the 3D structure of nanocrystals. There is already an approach to solve the orientation problem by using the automated indexing software in crystallography. However, this method cannot distinguish the twin orientations in the cases of the symmetries of Bravais lattices higher than the point groups. Here we propose a new method to solve this problem. The shape transforms of nanocrystals can be determined from all of the intensities around the diffraction spots, and then Fourier transformation of a single crystal cell is obtained. The actual orientations of the patterns can be solved by comparing the values of the Fourier transformations of the crystal cell on the intersections of all patterns. This so-called multiple-common-line method can distinguish the twin orientations in the XFEL diffraction patterns successfully. (authors)

  6. A Compton-thin Solution for the Suzaku X-ray Spectrum of the Seyfert 2 Galaxy Mkn 3

    CERN Document Server

    Yaqoob, T; Scholtes, A; Gottlieb, A; Turner, T J

    2015-01-01

    Mkn 3 is a Seyfert 2 galaxy that is widely regarded as an exemplary Compton-thick AGN. We study the Suzaku X-ray spectrum using models of the X-ray reprocessor that self-consistently account for the Fe K$\\alpha$ fluorescent emission line and the associated Compton-scattered, or reflection, continuum. We find a solution in which the average global column density, $0.234^{+0.012}_{-0.010} \\times 10^{24} \\ \\rm cm^{-2}$, is very different to the line-of-sight column density, $0.902^{+0.012}_{-0.013} \\times 10^{24} \\ \\rm cm^{-2}$. The global column density is $\\sim 5$ times smaller than that required for the matter distribution to be Compton-thick. Our model accounts for the profiles of the Fe K$\\alpha$ and Fe K$\\beta$ lines, and the Fe K edge remarkably well, with a solar abundance of Fe. The matter distribution could consist of a clumpy medium with a line-of-sight column density higher than the global average. A uniform, spherically-symmetric distribution alone cannot simultaneously produce the correct fluoresce...

  7. X-ray investigation of gene-engineered human insulin crystallized from a solution containing polysialic acid

    International Nuclear Information System (INIS)

    Crystals of insulin have been grown from a solution containing insulin and polysialic acid and the three-dimensional structure of insulin in these crystals has been solved at 1.6 Å resolution. Attempts to crystallize the noncovalent complex of recombinant human insulin with polysialic acid were carried out under normal and microgravity conditions. Both crystal types belonged to the same space group, I213, with unit-cell parameters a = b = c = 77.365 Å, α = β = γ = 90.00°. The reported space group and unit-cell parameters are almost identical to those of cubic insulin reported in the PDB. The results of X-ray studies confirmed that the crystals obtained were cubic insulin crystals and that they contained no polysialic acid or its fragments. Electron-density maps were calculated using X-ray diffraction sets from earth-grown and microgravity-grown crystals and the three-dimensional structure of the insulin molecule was determined and refined. The conformation and secondary-structural elements of the insulin molecule in different crystal forms were compared

  8. X-Ray Inactivation of Foot-and-Mouth Disease Virus and Vesicular Stomatitis Virus in Aqueous Media

    International Nuclear Information System (INIS)

    Radiation induced modifications to the biological activities and morphology of viruses are very dependent upon the techniques used in irradiation. Inactivation of foot-and-mouth disease virus and vesicular stomatitis virus by the effects of X-irradiation in dilute aqueous solutions has been studied and the post-irradiation effects and virus sensitization effects are described. Comparisons are made between X-radiation and hydrogen peroxide as virus inactivating agents. Survival curves resulting from these modes of inactivation give information on the reaction kinetics and on the function of the virus protein. Virus morphology, as detected in electron micrographs, is more readily changed by irradiation in solution (indirect effect) than by irradiation of the virus in the frozen state (direct effect). In each case the observed physical changes are related to loss of infectivity and the results are shown to be consistent with the inactivation processes previously inferred. (author)

  9. Pervaporation of Aqueous Solution of Acetaldehyde Through ZSM-5 Filled PDMS Composite Membrane

    Institute of Scientific and Technical Information of China (English)

    伍艳辉; 谭惠芬; 李佟茗; 金源

    2012-01-01

    Hydrophobic ZSM-5 zeolite filled polydimethylsiloxane (PDMS) composite membranes with Nylon micro-filtration membrane as the support layer were prepared to separate acetaldehyde from its aqueous solution. The composite membranes were characterized by Fourier transform infrared spectroscopy and X-ray diffraction. Their structural morphology and thermal stability were also examined. The swelling study showed that the composite membranes presented higher degree of swelling in aqueous solution of acetaldehyde than in pure water at 25℃,

  10. Solvation dynamics monitored by combined X-ray spectroscopies and scattering: photoinduced spin transition in aqueous [Fe(bpy)3]2+

    DEFF Research Database (Denmark)

    Bressler, C.; Gawelda, W.; Galler, A.;

    2014-01-01

    between intramolecular dynamics and the intermolecular caging solvent response with 100 ps time resolution. On this time scale the ultrafast spin transition including intramolecular geometric structure changes as well as the concomitant bulk solvent heating process due to energy dissipation from......We have studied the photoinduced low spin (LS) to high spin (HS) conversion of aqueous Fe(bpy)3 with pulse-limited time resolution. In a combined setup permitting simultaneous X-ray diffuse scattering (XDS) and spectroscopic measurements at a MHz repetition rate we have unraveled the interplay...

  11. Austenitic and duplex stainless steels in simulated physiological solution characterized by electrochemical and X-ray photoelectron spectroscopy studies.

    Science.gov (United States)

    Kocijan, Aleksandra; Conradi, Marjetka; Schön, Peter M

    2012-04-01

    A study of oxide layers grown on 2205 duplex stainless steel (DSS) and AISI 316L austenitic stainless steel in simulated physiological solution is presented here in order to establish the possibility of replacement of AISI 316 L with 2205 DSS in biomedical applications. The results of the potentiodynamic measurements show that the extent of the passive range significantly increased for DSS 2205 compared to AISI 316L stainless steel. Cyclic voltammetry was used to investigate electrochemical processes taking place on the steel surfaces. Oxide layers formed by electrochemical oxidation at different oxidation potentials were studied by X-ray photoelectron spectroscopy, and their compositions were analyzed as a function of depth. The main constituents on both the investigated materials were Cr- and Fe-oxides. Atomic force microscopy topography studies revealed the higher corrosion resistance of the DSS 2205 compared to the AISI 316L under the chosen experimental conditions. PMID:22331841

  12. Comparative structural stability of natural clays and zeolites in contact with 60Co2+ aqueous solutions

    International Nuclear Information System (INIS)

    The ability of synthetic and natural Mexican zeolites and clays to remove radioactive Co from aqueous solutions is discussed. In the various samples, crystallinity was determined by X-ray diffraction. The amount of radionuclide sorbed by the aluminosilicates was determined by γ-spectrometry. (author) 4 refs.; 1 tab

  13. Quantitative analysis of trace palladium contamination in solution using electrochemical X-ray fluorescence (EC-XRF).

    Science.gov (United States)

    Ayres, Zoë J; Newton, Mark E; Macpherson, Julie V

    2016-06-01

    The application of electrochemical X-ray fluorescence (EC-XRF), for the detection of palladium (Pd) contamination in a range of solutions containing electrochemically active compounds, present in excess and relevant to the pharmaceutical and food industries, is reported. In EC-XRF, EC is used to electrochemically pre-concentrate metal on an electrode under forced convection conditions, whilst XRF is employed to spectroscopically quantify the amount of metal deposited, which quantitatively correlates with the original metal concentration in solution. Boron doped diamond is used as the electrode due to its very wide cathodic window and the fact that B and C are non-interfering elements for XRF analysis. The effect of several parameters on the Pd XRF signal intensity are explored including: deposition potential (Edep), deposition time (tdep) and Pd(2+) concentration, [Pd(2+)]. Under high deposition potentials (Edep = -1.5 V), the Pd XRF peak intensity varies linearly with both tdep and [Pd(2+)]. Quantification of [Pd(2+)] is demonstrated in the presence of excess acetaminophen (ACM), l-ascorbic acid, caffeine and riboflavin. We show the same Pd XRF signal intensity (for [Pd(2+)] = 1.1 μM and tdep = 325 s) is observed, i.e. same amount of Pd is deposited on the electrode surface, irrespective of whether these redox active molecules are present or absent. For tdep = 900 s we report a limit of detection for [Pd(2+)] of 3.6 ppb (34 nM). Even lower LODs are possible by increasing tdep or by optimising the X-ray source specifically for Pd. The work presented for Pd detection in the presence of ACM, achieves the required detection sensitivity stipulated by international pharmacopeia guidelines. PMID:27118639

  14. 2010 Water & Aqueous Solutions

    Energy Technology Data Exchange (ETDEWEB)

    Dor Ben-Amotz

    2010-08-13

    Water covers more than two thirds of the surface of the Earth and about the same fraction of water forms the total mass of a human body. Since the early days of our civilization water has also been in the focus of technological developments, starting from converting it to wine to more modern achievements. The meeting will focus on recent advances in experimental, theoretical, and computational understanding of the behavior of the most important and fascinating liquid in a variety of situations and applications. The emphasis will be less on water properties per se than on water as a medium in which fundamental dynamic and reactive processes take place. In the following sessions, speakers will discuss the latest breakthroughs in unraveling these processes at the molecular level: Water in Solutions; Water in Motion I and II; Water in Biology I and II; Water in the Environment I and II; Water in Confined Geometries and Water in Discussion (keynote lecture and poster winners presentations).

  15. The Orbital Solution and Spectral Classification of the High-Mass X-Ray Binary IGR J01054-7253 in the Small Magellanic Cloud

    CERN Document Server

    Townsend, L J; Corbet, R H D; McBride, V A; Hill, A B; Bird, A J; Schurch, M P E; Haberl, F; Sturm, R; Pathak, D; van Soelen, B; Bartlett, E S; Drave, S P; Udalski, A

    2010-01-01

    We present X-ray and optical data on the Be/X-ray binary (BeXRB) pulsar IGR J01054-7253 = SXP11.5 in the Small Magellanic Cloud (SMC). Rossi X-ray Timing Explorer (RXTE) observations of this source in a large X-ray outburst reveal an 11.483 +/- 0.002s pulse period and show both the accretion driven spin-up of the neutron star and the motion of the neutron star around the companion through Doppler shifting of the spin period. Model fits to these data suggest an orbital period of 36.3 +/- 0.4d and Pdot of (4.7 +/- 0.3) x 10^{-10} ss^{-1}. We present an orbital solution for this system, making it one of the best described BeXRB systems in the SMC. The observed pulse period, spin-up and X-ray luminosity of SXP11.5 in this outburst are found to agree with the predictions of neutron star accretion theory. Timing analysis of the long-term optical light curve reveals a periodicity of 36.70 +/- 0.03d, in agreement with the orbital period found from the model fit to the X-ray data. Using blue-end spectroscopic observat...

  16. X-ray solution scattering of squid heavy meromyosin: strengthening the evidence for an ancient compact off state.

    Directory of Open Access Journals (Sweden)

    Richard E Gillilan

    Full Text Available The overall conformations of regulated myosins or heavy meromyosins from chicken/turkey, scallop, tarantula, limulus, and scorpion sources have been studied by a number of techniques, including electron microscopy, sedimentation, and pulsed electron paramagnetic resonance. These studies have indicated that the binding of regulatory ions changes the conformation of the molecule from a compact shape found in the "off" state of the muscle to extended relationships between the tail and independently mobile heads that predominate in the "on" state. Here we strengthen the argument for the generality of this conformational change by using small angle X-ray scattering on heavy meromyosin from squid. Small angle X-ray scattering allows the protein to be visualized in solution under mild and relatively physiological conditions, and squid differs from the other species studied by at least 500 million years of evolution. Analysis of the data indicates that upon addition of Ca(2+ the radius of gyration increases. Differences in the squid "on" and "off" states are clearly distinguishable as bimodal and unimodal pair distance distribution functions respectively. These observations are consistent with a Ca(2+-free squid heavy meromyosin that is compact, but which becomes extended when Ca(2+ is bound. Further, the scattering profile derived from the current model of tarantula heavy meromyosin in the "off" state is in excellent agreement with the measured "off" state scattering profile for squid heavy meromyosin. The previous and current studies together provide significant evidence that regulated myosin's compact off-state conformation is an ancient trait, inherited from a common ancestor during divergent evolution.

  17. Applied radiation physics: The use of x-rays for the structural characterization of aqueous emulsions and the development of new insect sterilization protocols

    Science.gov (United States)

    Brar, Ramaninder K.

    X-rays have great potential of applications in a wide variety of fields. This dissertation presents the use of x-rays for the structural characterization of aqueous emulsions and for insect sterilization. The stabilization of hydrophobic colloids, such as oil droplets, in water has attracted scientist for a variety of scientific, pharmaceutical and industrial applications. Several studies have been done to understand the stability of oil-in-water emulsions. The work of Pashley and his coworkers has demonstrated that the removal of dissolved gasses from water enhances the dispersion of hydrophobic oil in water and these surfactant-free emulsions do not lose their stability when the previously removed gasses are reintroduced. However, very little is known about the structure and stability of these emulsions over time or even to what extent they form. The formation of a stable emulsion in the complete absence of a surfactant could provide an alternative approach to a physiologically safe drug carrier. In this dissertation we demonstrate the formation of stabilized surfactant-free degassed emulsions of hydrocarbons - hexane, heptane and octane and silicone oil in ultra-pure water. The enhancement of dispersion of oil droplets by degassing was large for highly hydrophobic silicone oil. Turbidity measurements and small angle x-ray scattering results show that the uniformly dispersed oil droplets weakly aggregate over a period of several hours. Gentle perturbation re-generates the dispersion to nearly initial conditions. The control of insect species for the protection of crops, livestock, and prevention of disease, such as dengue fever and malaria, is a high priority in today's global economy. Sterile Insect Technique (SIT), a method of insect extermination without the use of pesticides, has proven very effective in eradicating certain dipteran insect populations. However, when standard sterilization methods developed for dipterans are applied to mosquito populations

  18. Succinic acid in aqueous solution : connecting microscopic surface composition and macroscopic surface tension

    OpenAIRE

    Werner, Josephina; Julin, Jan; Dalirian, Maryam; Prisle, Nønne; Öhrwall, Gunnar; Persson, Ingmar; Björneholm, Olle; Riipinen, Ilona

    2014-01-01

    The water vapor interface of aqueous solutions of succinic acid, where pH values and bulk concentrations were varied, has been studied using surface sensitive X-ray photoelectron spectroscopy (XPS) and molecular dynamics (MD) simulations. It was found that succinic acid has a considerably higher propensity to reside in the aqueous surface region than its deprotonated form, which is effectively depleted from the surface due to the two strongly hydrated carboxylate groups. From both XPS experim...

  19. Detection of copper ions from aqueous solutions using layered double hydroxides thin films deposited by PLD

    Science.gov (United States)

    Vlad, A.; Birjega, R.; Matei, A.; Luculescu, C.; Nedelcea, A.; Dinescu, M.; Zavoianu, R.; Pavel, O. D.

    2015-10-01

    Layered double hydroxides (LDHs) thin films with Mg-Al were deposited using pulsed laser deposition (PLD) technique. We studied the ability of our films to detect copper ions in aqueous solutions. Copper is known to be a common pollutant in water, originating from urban and industrial waste. Clay minerals, including layered double hydroxides (LDHs), can reduce the toxicity of such wastes by adsorbing copper. We report on the uptake of copper ions from aqueous solution on LDH thin films obtained via PLD. The obtained thin films were characterized using X-ray Diffraction, Atomic Force Microscopy, and Scanning Electron Microscopy with Energy Dispersive X-ray analysis. The results in this study indicate that LDHs thin films obtained by PLD have potential as an efficient adsorbent for removing copper from aqueous solution.

  20. X-Rays

    Science.gov (United States)

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

  1. Corrosion behavior of bulk metallic glasses in different aqueous solutions

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    The corrosion behavior of as-cast fully amorphous, structural relaxed amorphous and crystallized Fe65.5Cr4Mo4Ga4P12C5B5.5 bulk metallic glasses (BMGs) in NaCl, HCl and NaOH solutions was investigated by electrochemical polarization and immersion methods. X-ray photoelectron spectroscopy measurements was used to analyze the changes of the elements on the alloy surface before and after immersion in various solutions. The corrosion resistance of the Fe65.5Cr4Mo4Ga4P12C5B5.5 BMG was better than its structural relaxation/crystallization counterparts and common alloys (such as stainless steel, carbonized steel, and steel) in the selected aqueous solutions. The high corrosion resistance of this alloy in corrosive solutions leads to the formation of Fe-, Cr- and Mo-enriched protective thin surface films.

  2. Hardware solutions for the 65k pixel X-ray camera module of 75 μm pixel size

    Science.gov (United States)

    Kasinski, K.; Maj, P.; Grybos, P.; Koziol, A.

    2016-02-01

    We present three hardware solutions designed for a detector module built with a 2 cm × 2 cm hybrid pixel detector built from a single 320 or 450 μ m thick silicon sensor designed and fabricated by Hamamatsu and two UFXC32k readout integrated circuits (128 × 256 pixels with 75μ m pitch, designed in CMOS 130 nm at AGH-UST). The chips work in a single photon counting mode and provide ultra-fast X-ray imaging. The presented hardware modules are designed according to requirements of various tests and applications: ṡDevice A: a fast and flexible system for tests with various radiation sources. ṡDevice B: a standalone, all-in-one imaging device providing three standard interfaces (USB 2.0, Ethernet, Camera Link) and up to 640 MB/s bandwidth. ṡDevice C: a prototype large-area imaging system. The paper shows the readout system structure for each case with highlighted circuit board designs with details on power distribution and cooling on both FR4 and LTCC (low temperature co-fired ceramic) based circuits.

  3. Hardware solutions for the 65k pixel X-ray camera module of 75 μm pixel size

    International Nuclear Information System (INIS)

    We present three hardware solutions designed for a detector module built with a 2 cm ×2 cm hybrid pixel detector built from a single 320 or 450 μm thick silicon sensor designed and fabricated by Hamamatsu and two UFXC32k readout integrated circuits (128×256 pixels with 75μm pitch, designed in CMOS 130 nm at AGH-UST). The chips work in a single photon counting mode and provide ultra-fast X-ray imaging. The presented hardware modules are designed according to requirements of various tests and applications: ⋅Device A: a fast and flexible system for tests with various radiation sources. ⋅Device B: a standalone, all-in-one imaging device providing three standard interfaces (USB 2.0, Ethernet, Camera Link) and up to 640 MB/s bandwidth. ⋅Device C: a prototype large-area imaging system. The paper shows the readout system structure for each case with highlighted circuit board designs with details on power distribution and cooling on both FR4 and LTCC (low temperature co-fired ceramic) based circuits

  4. Chest x-ray

    Science.gov (United States)

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

  5. Arsenic(III) adsorption from aqueous solutions on novel carbon cryogel/ceria nanocomposite

    OpenAIRE

    Tamara Minović Arsić; Ana Kalijadis; Branko Matović; Milovan Stoiljković; Jelena Pantić; Jovan Jovanović; Rada Petrović; Bojan Jokić; Biljana Babić

    2016-01-01

    Carbon cryogel/ceria composite, with 10 wt.% of ceria, was synthesized by mixing of ceria and carbon cryogel (CC). The sample was characterized by field emission scanning electron microscopy, nitrogen adsorption and X-ray diffraction. The adsorption of arsenic(III) ions from aqueous solutions on carbon cryogel/ceria nanocomposite was studied as a function of time, solution pH and As(III) ion concentration. The results are correlated with previous investigations of adsorption mechanism of arse...

  6. Radiolysis of Aqueous Toluene Solutions

    International Nuclear Information System (INIS)

    Aqueous toluene solutions have been irradiated with Co γ-rays. In unbuffered solutions the various cresol isomers are formed in a total yield of 0.45, 0.87 and 0.94 molecules/100 eV absorbed energy in argon-, N2O- and air - saturated solutions, respectively. The yields are reduced in acid (pH 3) solutions (G 0.14, 0.14 and 0.52, respectively) but the reduction is compensated by the formation of 1,2-di-phenylethane in yields of 0.49 and 1.60 in argon- and N2O-saturated solutions, respectively. Benzyl radicals are formed through an acid catalysed water elimination reaction from the initially formed hydroxymethylcyclohexadienyl radical. Phenyltolylmethanes, dimethylbiphenyls and partly reduced dimers are also formed during the radiolysis. Hydrogen is formed in the same yield as the molecular yield, g(H2). Xylene isomers and benzene are formed in trace quantities. The most remarkable effects of the addition of Fe(III) ions to deaerated acid toluene solutions are the formation of benzyl alcohol and benzaldehyde and an increase in the yield of 1,2-diphenylethane

  7. DEHYDRATION CONDENSATION IN AQUEOUS SOLUTION

    Energy Technology Data Exchange (ETDEWEB)

    Steinman, Gary; Kenyon, Dean H.; Calvin, Melvin

    1965-04-01

    EARLIER investigations have demonstrated that di-cyandiamide (DCDA), the dimer of cyanamide, can successfully promote the dehydration condensation of: (1) glucose and orthophosphate to give glucose-6-phosphate; (2) adenosine and orthophosphate to give adenosine-5'-monophosphate; (3) orthophosphate to give pyrophosphate; (4) alanine to give alanylalanine and alanylalanylalanine. These reactions were carried out in dilute aqueous solutions in the dark. (It was also demonstrated that the combination of ultra-violet light and dicyandiamide could promote the synthesis of dipeptides. This observation has since been confirmed by other investigators.) These experiments were designed to demonstrate one possible means by which such compounds could have been formed on the prebiotic Earth, thus providing materials needed for the origin of living systems. Dicyandiamide itself could have been, present on the primitive Earth as was demonstrated with the ultra-violet irradiation of cyanide solution.

  8. Resonant inelastic X-ray scattering as a probe of molecular structure and electron dynamics in solutions

    International Nuclear Information System (INIS)

    Resonant inelastic X-ray scattering (RIXS) technique is applied to gain insight into the local electronic structure in liquid phase. The approach combines a liquid micro-jet and an X-ray emission spectrometer (XES) both installed in the recently developed LiXEdrom experimental station. Here we demonstrate how the combined approach enables investigation of the hydrogen bonding network in water and of chemical bonding in different solvents. In addition, the probe of energy transfer and electron dynamics at the metal–solvent interface is achieved by comparing the integrated RIXS intensities of the different radiative decay channels of the 2p core-hole of 3d transition-metals. The integrated RIXS intensities build the partial and the inverse partial X-ray fluorescence yields that allow for absorption measurements free from background signal of other elements or saturation effects

  9. Solution NMR and X-ray Crystal Structures of Membrane-associated Lipoprotein-17 Domain Reveal a Novel Fold

    Energy Technology Data Exchange (ETDEWEB)

    R Mani; S Vorobiev; G Swapna; H Neely; H Janjua; C Ciccosanti; D Xiao; J Hunt; G Montelione; et al.

    2011-12-31

    The conserved Lipoprotein-17 domain of membrane-associated protein Q9PRA0{_}UREPA from Ureaplasma parvum was selected for structure determination by the Northeast Structural Genomics Consortium, as part of the Protein Structure Initiative's program on structure-function analysis of protein domains from large domain sequence families lacking structural representatives. The 100-residue Lipoprotein-17 domain is a 'domain of unknown function' (DUF) that is a member of Pfam protein family PF04200, a large domain family for which no members have characterized biochemical functions. The three-dimensional structure of the Lipoprotein-17 domain of protein Q9PRA0{_}UREPA was determined by both solution NMR and by X-ray crystallography at 2.5 {angstrom}. The two structures are in good agreement with each other. The domain structure features three {alpha}-helices, {alpha}1 through {alpha}3, and five {beta}-strands. Strands {beta}1/{beta}2, {beta}3/{beta}4, {beta}4/{beta}5 are anti-parallel to each other. Strands {beta}1 and {beta}2 are orthogonal to strands {beta}3, {beta}4, {beta}5, while helix {alpha}3 is formed between the strands {beta}3 and {beta}4. One-turn helix {alpha}2 is formed between the strands {beta}1 and {beta}2, while helix {alpha}1 occurs in the N-terminal polypeptide segment. Searches of the Protein Data Bank do not identify any other protein with significant structural similarity to Lipoprotein-17 domain of Q9PRA0{_}UREPA, indicating that it is a novel protein fold.

  10. X-ray emission from η Carinae near periastron in 2009. I. A two-state solution

    Energy Technology Data Exchange (ETDEWEB)

    Hamaguchi, Kenji; Corcoran, Michael F. [CRESST and X-ray Astrophysics Laboratory, NASA/GSFC, Greenbelt, MD 20771 (United States); Russell, Christopher M. P. [Faculty of Engineering, Hokkai-Gakuen University, Toyohira-ku, Sapporo 062-8605 (Japan); Pollock, A. M. T. [European Space Agency, Apartado 78, Villanueva de la Cañada, E-28691 Madrid (Spain); Gull, Theodore R.; Teodoro, Mairan; Madura, Thomas I. [Astrophysics Science Division, NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Damineli, Augusto [Instituto de Astronomia, Geofísica e Ciências Atmosféricas, Universidade de São Paulo, Rua do Matão 1226, Cidade Universitária, São Paulo 05508-900 (Brazil); Pittard, Julian M. [School of Physics and Astronomy, The University of Leeds, Woodhouse Lane, Leeds LS2 9JT (United Kingdom)

    2014-04-01

    X-ray emission from the supermassive binary system η Car declines sharply around periastron. This X-ray minimum has two distinct phases—the lowest flux phase in the first ∼3 weeks and a brighter phase thereafter. In 2009, the Chandra X-ray Observatory monitored the first phase five times and found the lowest observed flux at ∼1.9 × 10{sup –12} erg cm{sup –2} s{sup –1} (3-8 keV). The spectral shape changed such that the hard band above ∼4 keV dropped quickly at the beginning and the soft band flux gradually decreased to its lowest observed value in ∼2 weeks. The hard band spectrum had begun to recover by that time. This spectral variation suggests that the shocked gas producing the hottest X-ray gas near the apex of the wind-wind collision (WWC) is blocked behind the dense inner wind of the primary star, which later occults slightly cooler gas downstream. Shocked gas previously produced by the system at earlier orbital phases is suggested to produce the faint residual X-ray emission seen when the emission near the apex is completely blocked by the primary wind. The brighter phase is probably caused by the re-appearance of the WWC plasma, whose emissivity significantly declined during the occultation. We interpret this to mean that the X-ray minimum is produced by a hybrid mechanism of an occultation and a decline in the emissivity of the WWC shock. We constrain timings of superior conjunction and periastron based on these results.

  11. Radiolysis of Aqueous Benzene Solutions

    International Nuclear Information System (INIS)

    Aerated and deaerated aqueous solutions of benzene have been irradiated with 60Co γ-rays. The products of radiolysis in deaerated, unbuffered or acid, solutions were phenol, biphenyl, hydrogen and in acid solutions also hydrogen peroxide with the following yields: G(phenol) = 0. 37 (0. 37), G(biphenyl) = 1.3 (1.7), G(H2) = 0.44 (0. 43) and G(H2O2) = 0 (0.60), the figures in brackets giving the results for acid solutions. The results are shown to agree with the conclusion that k(e-aq + H2O2) >> k(H + H2O2). Furthermore, the results indicate that a competition takes place between the reactions: 2 C6H6OH · -> dimer -> biphenyl. C6H7 · + C6H6OH · -> dimer -> biphenyl. The yields in aerated, unbuffered or acid, solutions were: G(phenol) = 2.1 (2.3), G(biphenyl) = 0 (0), and G(H2O2) = 2.2 (3.1), the figures in brackets being valid for acid solutions. The ratio k(H + C6H6)/k(H + O2) was 1.4x10-2. The results indicate that peroxides, or more probably hydroperoxides, take part in the reactions. After the addition of Fe2+ or Fe3+ to aerated acid solutions G(phenol) was increased to 6.6 and 3.4 respectively. Oxygen was consumed more rapidly in the presence of Fe. Reaction mechanisms are discussed

  12. Phosphors for X-ray intensification screens

    International Nuclear Information System (INIS)

    An improved rare earth oxyhalide phosphor for x-ray intensification screens is described. The phosphors, of formula LnOX.T where Ln = La or Gd, X = Cl or Br and T = Tm or Tb, are mixed with a small amount of a trivalent antimony compound. The addition of antimony overcomes ageing due to attack by atmospheric moisture and renders the phosphor freeflowing so that dispersions can be readily made. Preferably the phosphor is washed with an aqueous solution of the antimony compound and the compound is the fluoride, chloride or butoxide, or potassium antimony tartrate. (U.K.)

  13. The solvent shell structure of aqueous iodide: X-ray absorption spectroscopy and classical, hybrid QM/MM and full quantum molecular dynamics simulations

    Energy Technology Data Exchange (ETDEWEB)

    Pham, V.T. [Ecole Polytechnique Federale de Lausanne, Laboratoire de spectroscopie ultrarapide, ISIC, FSB-BSP, CH-1015 Lausanne (Switzerland); Tavernelli, I. [Ecole Polytechnique Federale de Lausanne, Laboratoire de chimie et biochimie computationnelles, ISIC, FSB-BSP, CH-1015 Lausanne (Switzerland); Milne, C.J.; van der Veen, R.M. [Ecole Polytechnique Federale de Lausanne, Laboratoire de spectroscopie ultrarapide, ISIC, FSB-BSP, CH-1015 Lausanne (Switzerland); D' Angelo, P. [Dipartimento di Chimica, Universita di Roma ' La Sapienza' , Ple A. Moro 5, 00185 Roma (Italy); Bressler, Ch. [Ecole Polytechnique Federale de Lausanne, Laboratoire de spectroscopie ultrarapide, ISIC, FSB-BSP, CH-1015 Lausanne (Switzerland); Chergui, M., E-mail: Majed.Chergui@epfl.ch [Ecole Polytechnique Federale de Lausanne, Laboratoire de spectroscopie ultrarapide, ISIC, FSB-BSP, CH-1015 Lausanne (Switzerland)

    2010-05-25

    Graphical abstract: The L{sub 3}-edge EXAFS spectra of aqueous iodide are compared to classical, QM/MM and DFT-based molecular dynamics simulations. The QM/MM simulations reproduce best the experimental data. An anisotropy of the solvation shell is also identified. - Abstract: The L{sub 3} X-ray absorption spectrum of aqueous iodide is reported, and its EXAFS is compared to theoretical spectra reconstructed from the radial distribution function of the iodide hydration obtained from classical, hybrid Quantum Mechanics Molecular Mechanics, (QM/MM) and full quantum (density functional theory, DFT) molecular dynamics simulations. Since EXAFS is mainly sensitive to short distances around the iodide ion, it is a direct probe of the local solvation structure. The comparison shows that QM/MM simulations deliver a satisfactory description of the EXAFS signal, while nonpolarizable classical simulations are somewhat less satisfactory and DFT-based simulations perform poorly. We also identify a weak anisotropy of the water solvation shell around iodide, which may be of importance in electron photoejection experiments.

  14. Thoracic spine x-ray

    Science.gov (United States)

    Vertebral radiography; X-ray - spine; Thoracic x-ray; Spine x-ray; Thoracic spine films; Back films ... care provider's office. You will lie on the x-ray table in different positions. If the x-ray ...

  15. Studies of protein structure in solution and protein folding using synchrotron small-angle x-ray scattering

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Lingling

    1996-04-01

    Synchrotron small angle x-ray scattering (SAXS) has been applied to the structural study of several biological systems, including the nitrogenase complex, the heat shock cognate protein (hsc70), and lysozyme folding. The structural information revealed from the SAXS experiments is complementary to information obtained by other physical and biochemical methods, and adds to our knowledge and understanding of these systems.

  16. Analytical Instrument of X-ray Fluorescence Determine Concentration of U and Pu in Organic Solution at the Same Time

    Institute of Scientific and Technical Information of China (English)

    2011-01-01

    An instrument is developed to measure the concentration of U, Pu and the intensity of gamma ray in samples of 1AP organic phase at the same time. The Ag cold cathode is used to excite L series X-ray fluorescence of U and Pu. The Si-pin detector is

  17. X-ray absorption spectra of nucleotides (AMP, GMP, and CMP) in liquid water solutions near the nitrogen K-edge

    Science.gov (United States)

    Ukai, Masatoshi; Yokoya, Akinari; Fujii, Kentaro; Saitoh, Yuji

    2010-07-01

    The X-ray absorption of nucleotides (adenosine-5'-monophosphate, guanosine 5'-monophosphate, and cytidine 5'-monophosphate) are measured in both water solutions and thin solid films at X-ray energies near the nitrogen K-edge in the 'water-window' region. Each spectrum corresponds to the selective excitation of a nucleobase site in a nucleotide, and thus has features similar to the spectrum of the corresponding nucleobase. An additional new peak in the energy region of the nitrogen 1s → π* resonance is observed for each nucleotide. No significant difference between the water solutions and thin solid films is found, which might be attributable to the hydrophobic properties of a nucleobase in a nucleotide.

  18. Evidence for lattice strain and non-ideal behaviour in the (La1-xEux)PO4 solid solution from X-ray diffraction and vibrational spectroscopy

    Science.gov (United States)

    Geisler, Thorsten; Popa, Karin; Konings, Rudy

    2016-06-01

    The monazite-type solid solution of LaPO_4 and EuPO_4 has been studied by X-ray diffraction, infrared (IR) and Raman spectroscopic techniques. A substantial excess molar volume has been derived from the X-ray data, and the Raman and IR spectra show band broadening typical for mixing of cations of different size on the cation sublattice. The IR spectra were interpreted by the autocorrelation method and the excess autocorrelation parameter Δ{corr}^{ex} shows clear deviation from ideal solution behaviour, similar to the observed broadening of the Raman bands. The results can be interpreted in terms of local lattice strains resulting from the ion size effects of substitution of La^{3+} by Eu^{3+}, and correlate very well with calorimetric measurements of the excess enthalpy that was previously measured.

  19. Topical Review: Molecular reaction and solvation visualized by time-resolved X-ray solution scattering: Structure, dynamics, and their solvent dependence

    Directory of Open Access Journals (Sweden)

    Kyung Hwan Kim

    2014-01-01

    Full Text Available Time-resolved X-ray solution scattering is sensitive to global molecular structure and can track the dynamics of chemical reactions. In this article, we review our recent studies on triiodide ion (I3– and molecular iodine (I2 in solution. For I3–, we elucidated the excitation wavelength-dependent photochemistry and the solvent-dependent ground-state structure. For I2, by combining time-slicing scheme and deconvolution data analysis, we mapped out the progression of geminate recombination and the associated structural change in the solvent cage. With the aid of X-ray free electron lasers, even clearer observation of ultrafast chemical events will be made possible in the near future.

  20. Guest–Host Interactions Investigated by Time-Resolved X-ray Spectroscopies and Scattering at MHz Rates

    DEFF Research Database (Denmark)

    Haldrup, Martin Kristoffer; Vanko, G.; Gawelda, W.;

    2012-01-01

    We have studied the photoinduced low spin (LS) to high spin (HS) conversion of [Fe(bipy)3]2+ in aqueous solution. In a laser pump/X-ray probe synchrotron setup permitting simultaneous, time-resolved X-ray diffuse scattering (XDS) and X-ray spectroscopic measurements at a 3.26 MHz repetition rate......, as is the solvent heating due to the initial energy dissipation from the excited HS molecule. Combining information from X-ray emission spectroscopy and scattering, the excitation fraction as well as the temperature and density changes of the solvent can be closely followed on the subnanosecond time scale of the HS...

  1. X-ray (image)

    Science.gov (United States)

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

  2. Dental x-rays

    Science.gov (United States)

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

  3. X-ray apparatus

    International Nuclear Information System (INIS)

    A diagnostic x-ray device, readily convertible between conventional radiographic and tomographic operating modes, is described. An improved drive system interconnects and drives the x-ray source and the imaging device through coordinated movements for tomography

  4. Dental x-rays

    Science.gov (United States)

    X-ray - teeth; Radiograph - dental; Bitewings; Periapical film; Panoramic film; Digital image ... dentist's office. There are many types of dental x-rays. Some of them are: Bitewing. Shows the crown ...

  5. MCM-41 impregnated with A zeolite precursor: Synthesis, characterization and tetracycline antibiotics removal from aqueous solution

    OpenAIRE

    Liu, Minmin; Hou, Li-an; Yu, Shuili; Xi, Beidou; Zhao, Ying; Xia, Xunfeng

    2013-01-01

    In this paper, the MCM-41 has been modified by impregnation with zeolite A to prepare a kind of new adsorbent. The adsorption of TC from aqueous solutions onto modified MCM-41 has been studied. It was discovered that the adsorption capability of zeolite A modified MCM-41 (A-MCM-41) increased dramatically after modification. The modified MCM-41 was characterized by X-ray diffraction (XRD), nitrogen adsorption–desorption, Fourier Transform Infrared (FTIR) analysis, Transmission electron microsc...

  6. THE REMOVAL OF REACTIVE RED 228 DYE FROM AQUEOUS SOLUTIONS BY CHITOSAN-MODIFIED FLAX SHIVE

    OpenAIRE

    Hao Feng; Jian Li; Lijuan Wang

    2011-01-01

    Flax shive (FS) is a byproduct from flax fiber separation. The use of absorbent prepared from chitosan-modified flax shive (CFS) has been studied for removal of reactive red dye (RR228) from aqueous solutions. CFS was characterized by the Brunauer-Emmett-Teller (BET) method, Scanning Electron Microscopy (SEM), Fourier Transform Infrared spectrometry (FTIR), and X-ray photoelectron spectroscopy (XPS). A batch adsorption study was conducted under various contact time, initial concentration, sol...

  7. Removal of Indigo Carmine Dye from Aqueous Solution Using Magnesium Hydroxide as an Adsorbent

    OpenAIRE

    Thimmasandra Narayan Ramesh; Vani Pavagada Sreenivasa

    2015-01-01

    Magnesium hydroxide is used as an adsorbent for the removal of indigo carmine dye from aqueous solution. We have investigated the effectiveness of removal of indigo carmine dye from aqueous solutions at pH 6-7 and 12-13 using magnesium hydroxide thereby varying the dose of the adsorbent, concentration of the dye, duration, and temperature. Structural transformations of adsorbent during the adsorption process at different pH values are monitored using powder X-ray diffraction and infrared spec...

  8. X-Rays

    Science.gov (United States)

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

  9. Chest X-Ray

    Medline Plus

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

  10. X-Ray Imaging

    Science.gov (United States)

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

  11. X-ray investigation of gene-engineered human insulin crystallized from a solution containing polysialic acid

    Science.gov (United States)

    Timofeev, V. I.; Chuprov-Netochin, R. N.; Samigina, V. R.; Bezuglov, V. V.; Miroshnikov, K. A.; Kuranova, I. P.

    2010-01-01

    Attempts to crystallize the noncovalent complex of recombinant human insulin with polysialic acid were carried out under normal and microgravity conditions. Both crystal types belonged to the same space group, I213, with unit-cell parameters a = b = c = 77.365 Å, α = β = γ = 90.00°. The reported space group and unit-cell parameters are almost identical to those of cubic insulin reported in the PDB. The results of X-ray studies confirmed that the crystals obtained were cubic insulin crystals and that they contained no polysialic acid or its fragments. Electron-density maps were calculated using X-ray diffraction sets from earth-grown and microgravity-grown crystals and the three-dimensional structure of the insulin molecule was determined and refined. The conformation and secondary-structural elements of the insulin molecule in different crystal forms were compared. PMID:20208155

  12. Solution of some critical problems in X-ray fluorescence. II - Determination of Nb and Ta traces in concentrates

    International Nuclear Information System (INIS)

    Two straightforward methods are proposed for quantitative analysis of Nb and Ta traces in heavy fractions of mineral samples by using X-ray fluorescence technique. The first one consist in calculating the background intensity by the weighted average of the asymmetrical intensities values mesured in each side of Nb Kα line. The second method corrects the overlap of Th Lβ and Ta Lα by the experimentally obtained ratios between different Th excitation lines. (author)

  13. Intermolecular bonding of hemin in solution and in solid state probed by N K-edge X-ray spectroscopies.

    Science.gov (United States)

    Golnak, Ronny; Xiao, Jie; Atak, Kaan; Stevens, Joanna S; Gainar, Adrian; Schroeder, Sven L M; Aziz, Emad F

    2015-11-21

    X-ray absorption/emission spectroscopy (XAS/XES) at the N K-edge of iron protoporphyrin IX chloride (FePPIX-Cl, or hemin) has been carried out for dissolved monomers in DMSO, dimers in water and for the solid state. This sequence of samples permits identification of characteristic spectral features associated with the hemin intermolecular bonding. These characteristic features are further analyzed and understood at the molecular orbital (MO) level based on the DFT calculations.

  14. Shielding chalculations in x-rays installations for medical diagnosis. description of the method and computational solution

    International Nuclear Information System (INIS)

    Shielding requirements for x-rays diagnostic installations are investigated. The description of an entirely analytical method for calculation of thickness, based in the papers of Simpkin and NCRP49, is presented. Considerations described in specialized method to solving this problem. A program for microcomputer IBM and compatibles ones is available for estimation of minimum shielding requirements in lead, concrete and steel. Similar results were obtained from comparing with others authors

  15. 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

  16. Local Liquid Holdups and Hysteresis in a 2-D Packed Bed Using X-ray Radiography

    OpenAIRE

    Basavaraj, MG; Gupta, GS; K Naveen; Rudolph, V.; Bali, R

    2005-01-01

    An X-ray visualization technique has been used for the quantitative determination of local liquid holdups distribution and liquid holdup hysteresis in a nonwetting twodimensional (2-D) packed bed. A medical diagnostic X-ray unit has been used to image the local holdups in a 2-D cold model having a random packing of expanded polystyrene beads. An aqueous barium chloride solution was used as a fluid to achieve good contrast on X-ray images. To quantify the local liquid holdup, a simple calibrat...

  17. Combined operando X-ray diffraction-electrochemical impedance spectroscopy detecting solid solution reactions of LiFePO4 in batteries.

    Science.gov (United States)

    Hess, Michael; Sasaki, Tsuyoshi; Villevieille, Claire; Novák, Petr

    2015-01-01

    Lithium-ion batteries are widely used for portable applications today; however, often suffer from limited recharge rates. One reason for such limitation can be a reduced active surface area during phase separation. Here we report a technique combining high-resolution operando synchrotron X-ray diffraction coupled with electrochemical impedance spectroscopy to directly track non-equilibrium intermediate phases in lithium-ion battery materials. LiFePO4, for example, is known to undergo phase separation when cycled under low-current-density conditions. However, operando X-ray diffraction under ultra-high-rate alternating current and direct current excitation reveal a continuous but current-dependent, solid solution reaction between LiFePO4 and FePO4 which is consistent with previous experiments and calculations. In addition, the formation of a preferred phase with a composition similar to the eutectoid composition, Li0.625FePO4, is evident. Even at a low rate of 0.1C, ∼20% of the X-ray diffractogram can be attributed to non-equilibrium phases, which changes our understanding of the intercalation dynamics in LiFePO4. PMID:26345306

  18. Combined operando X-ray diffraction-electrochemical impedance spectroscopy detecting solid solution reactions of LiFePO4 in batteries

    Science.gov (United States)

    Hess, Michael; Sasaki, Tsuyoshi; Villevieille, Claire; Novák, Petr

    2015-09-01

    Lithium-ion batteries are widely used for portable applications today; however, often suffer from limited recharge rates. One reason for such limitation can be a reduced active surface area during phase separation. Here we report a technique combining high-resolution operando synchrotron X-ray diffraction coupled with electrochemical impedance spectroscopy to directly track non-equilibrium intermediate phases in lithium-ion battery materials. LiFePO4, for example, is known to undergo phase separation when cycled under low-current-density conditions. However, operando X-ray diffraction under ultra-high-rate alternating current and direct current excitation reveal a continuous but current-dependent, solid solution reaction between LiFePO4 and FePO4 which is consistent with previous experiments and calculations. In addition, the formation of a preferred phase with a composition similar to the eutectoid composition, Li0.625FePO4, is evident. Even at a low rate of 0.1C, ~20% of the X-ray diffractogram can be attributed to non-equilibrium phases, which changes our understanding of the intercalation dynamics in LiFePO4.

  19. Combined operando X-ray diffraction-electrochemical impedance spectroscopy detecting solid solution reactions of LiFePO4 in batteries.

    Science.gov (United States)

    Hess, Michael; Sasaki, Tsuyoshi; Villevieille, Claire; Novák, Petr

    2015-09-08

    Lithium-ion batteries are widely used for portable applications today; however, often suffer from limited recharge rates. One reason for such limitation can be a reduced active surface area during phase separation. Here we report a technique combining high-resolution operando synchrotron X-ray diffraction coupled with electrochemical impedance spectroscopy to directly track non-equilibrium intermediate phases in lithium-ion battery materials. LiFePO4, for example, is known to undergo phase separation when cycled under low-current-density conditions. However, operando X-ray diffraction under ultra-high-rate alternating current and direct current excitation reveal a continuous but current-dependent, solid solution reaction between LiFePO4 and FePO4 which is consistent with previous experiments and calculations. In addition, the formation of a preferred phase with a composition similar to the eutectoid composition, Li0.625FePO4, is evident. Even at a low rate of 0.1C, ∼20% of the X-ray diffractogram can be attributed to non-equilibrium phases, which changes our understanding of the intercalation dynamics in LiFePO4.

  20. Combined operando X-ray diffraction–electrochemical impedance spectroscopy detecting solid solution reactions of LiFePO4 in batteries

    Science.gov (United States)

    Hess, Michael; Sasaki, Tsuyoshi; Villevieille, Claire; Novák, Petr

    2015-01-01

    Lithium-ion batteries are widely used for portable applications today; however, often suffer from limited recharge rates. One reason for such limitation can be a reduced active surface area during phase separation. Here we report a technique combining high-resolution operando synchrotron X-ray diffraction coupled with electrochemical impedance spectroscopy to directly track non-equilibrium intermediate phases in lithium-ion battery materials. LiFePO4, for example, is known to undergo phase separation when cycled under low-current-density conditions. However, operando X-ray diffraction under ultra-high-rate alternating current and direct current excitation reveal a continuous but current-dependent, solid solution reaction between LiFePO4 and FePO4 which is consistent with previous experiments and calculations. In addition, the formation of a preferred phase with a composition similar to the eutectoid composition, Li0.625FePO4, is evident. Even at a low rate of 0.1C, ∼20% of the X-ray diffractogram can be attributed to non-equilibrium phases, which changes our understanding of the intercalation dynamics in LiFePO4. PMID:26345306

  1. High performance x-ray imaging detectors on foil using solution-processed organic photodiodes with extremely low dark leakage current (Presentation Recording)

    Science.gov (United States)

    Kumar, Abhishek; Moet, Date; van der Steen, Jan Laurens; van Breemen, Albert; Shanmugam, Santhosh; Gilot, Jan; Andriessen, Ronn; Simon, Matthias; Ruetten, Walter; Douglas, Alexander; Raaijmakers, Rob; Malinowski, Pawel E.; Myny, Kris; Gelinck, Gerwin

    2015-10-01

    High performance X-ray imaging detectors on foil using solution-processed organic photodiodes with extremely low dark leakage current Abhishek Kumara, Date Moeta, Albert van Breemena, Santhosh Shanmugama, Jan-Laurens van der Steena, Jan Gilota, Ronn Andriessena, Matthias Simonb, Walter Ruettenb, Alexander U. Douglasb, Rob Raaijmakersc, Pawel E. Malinowskid, Kris Mynyd and Gerwin H. Gelincka,e a. Holst Centre/TNO, High Tech Campus 31, Eindhoven 5656 AE, The Netherlands b. Philips Research, High Tech Campus 34, 5656 AE Eindhoven, The Netherlands c. Philips Healthcare, Veenpluis 6-8, 5684 PC Best, The Netherlands d. Department of Large Area Electronics, imec vzw, Kapeldreef 75, Leuven B3001, Belgium e. Applied Physics Department, TU Eindhoven, Eindhoven, The Netherlands We demonstrate high performance X-ray imaging detectors on foil suitable for medical grade X-ray imaging applications. The detectors are based on solution-processed organic photodiodes forming bulk-heterojunctions from photovoltaic donor and acceptor blend. The organic photodiodes are deposited using an industrially compatible slot die coating technique with end of line processing temperature below 100°C. These photodiodes have extremely low dark leakage current density of 10-7 mA/cm2 at -2V bias with very high yield and have peak absorption around 550 nm wavelength. We combine these organic photodiodes with high mobility metal oxide semiconductor based thin film transistor arrays with high pixel resolution of 200ppi on thin plastic substrate. When combined with a typical CsI(TI) scintillator material on top, they are well suited for low dose X-ray imaging applications. The optical crosstalk is insignificant upto resolution of 200 ppi despite the fact that the photodiode layer is one continuous layer and is non-pixelated. Low processing temperatures are another key advantage since they can be fabricated on plastic substrate. This implies that we can make X-ray detectors on flexible foil. Those

  2. Synchrotron X-ray diffraction study of the Ba1−xSrSnO3 solid solution

    International Nuclear Information System (INIS)

    At room temperature the sequence of phases with increasing amounts of strontium in the stannate perovskite system Ba1−xSrSnO3 has been established from high resolution synchrotron X-ray powder diffraction. The observed sequence orthorhombic (Pbnm), orthorhombic (Ibmm), tetragonal (I4/mcm), and cubic (Pm3-bar m) is a consequence of the sequential introduction of cooperative tilting of the corner sharing SnO6 octahedra. The cell volume changes smoothly across the series with no obvious discontinuities associated with the phase transitions. - Graphical abstract: Portions of the synchrotron X-ray diffraction profiles (λ=0.82453 Å) from selected Ba1−xSrxSnO3 samples together with the results of fitting by the Rietveld method. Highlights: ► Structures of the stannate perovskites Ba1−xSrSnO3 refined from synchrotron XRD. ► The sequence Pm3-bar m→I4/mcm→Ibmm→Pbnm results from tilting of the octahedra. ► The tilting maintains optimal bonding of the cations seen from the BVS analysis

  3. Solution small-angle x-ray scattering as a screening and predictive tool in the fabrication of asymmetric block copolymer membranes

    KAUST Repository

    Dorin, Rachel Mika

    2012-05-15

    Small-angle X-ray scattering (SAXS) analysis of the diblock copolymer poly(styrene-b-(4-vinyl)pyridine) in a ternary solvent system of 1,4-dioxane, tetrahydrofuran, and N,N-dimethylformamide, and the triblock terpolymer poly(isoprene-b-styrene-b-(4-vinyl)-pyridine) in a binary solvent system of 1,4-dioxane and tetrahydrofuran, reveals a concentration-dependent onset of ordered structure formation. Asymmetric membranes fabricated from casting solutions with polymer concentrations at or slightly below this ordering concentration possess selective layers with the desired nanostructure. In addition to rapidly screening possible polymer solution concentrations, solution SAXS analysis also predicts hexagonal and square pore lattices of the final membrane surface structure. These results suggest solution SAXS as a powerful tool for screening casting solution concentrations and predicting surface structure in the fabrication of asymmetric ultrafiltration membranes from self-assembled block copolymers. (Figure presented) © 2012 American Chemical Society.

  4. X-Ray Polarimetry

    CERN Document Server

    Kaaret, Philip

    2014-01-01

    We review the basic principles of X-ray polarimetry and current detector technologies based on the photoelectric effect, Bragg reflection, and Compton scattering. Recent technological advances in high-spatial-resolution gas-filled X-ray detectors have enabled efficient polarimeters exploiting the photoelectric effect that hold great scientific promise for X-ray polarimetry in the 2-10 keV band. Advances in the fabrication of multilayer optics have made feasible the construction of broad-band soft X-ray polarimeters based on Bragg reflection. Developments in scintillator and solid-state hard X-ray detectors facilitate construction of both modular, large area Compton scattering polarimeters and compact devices suitable for use with focusing X-ray telescopes.

  5. X-Ray Polarimetry

    OpenAIRE

    Kaaret, Philip

    2014-01-01

    We review the basic principles of X-ray polarimetry and current detector technologies based on the photoelectric effect, Bragg reflection, and Compton scattering. Recent technological advances in high-spatial-resolution gas-filled X-ray detectors have enabled efficient polarimeters exploiting the photoelectric effect that hold great scientific promise for X-ray polarimetry in the 2-10 keV band. Advances in the fabrication of multilayer optics have made feasible the construction of broad-band ...

  6. BioSAXS Sample Changer: a robotic sample changer for rapid and reliable high-throughput X-ray solution scattering experiments

    Energy Technology Data Exchange (ETDEWEB)

    Round, Adam, E-mail: around@embl.fr; Felisaz, Franck [European Molecular Biology Laboratory, Grenoble Outstation, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France); Université Grenoble Alpes–EMBL–CNRS, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France); Fodinger, Lukas; Gobbo, Alexandre [European Molecular Biology Laboratory, Grenoble Outstation, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France); Huet, Julien [European Molecular Biology Laboratory, Grenoble Outstation, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France); Université Grenoble Alpes–EMBL–CNRS, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France); Villard, Cyril [European Molecular Biology Laboratory, Grenoble Outstation, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France); Blanchet, Clement E., E-mail: around@embl.fr [EMBL c/o DESY, Notkestrasse 85, 22603 Hamburg (Germany); Pernot, Petra; McSweeney, Sean [ESRF, 6 Rue Jules Horowitz, 38000 Grenoble (France); Roessle, Manfred; Svergun, Dmitri I. [EMBL c/o DESY, Notkestrasse 85, 22603 Hamburg (Germany); Cipriani, Florent, E-mail: around@embl.fr [European Molecular Biology Laboratory, Grenoble Outstation, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France); Université Grenoble Alpes–EMBL–CNRS, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France)

    2015-01-01

    A robotic sample changer for solution X-ray scattering experiments optimized for speed and to use the minimum amount of material has been developed. This system is now in routine use at three high-brilliance European synchrotron sites, each capable of several hundred measurements per day. Small-angle X-ray scattering (SAXS) of macromolecules in solution is in increasing demand by an ever more diverse research community, both academic and industrial. To better serve user needs, and to allow automated and high-throughput operation, a sample changer (BioSAXS Sample Changer) that is able to perform unattended measurements of up to several hundred samples per day has been developed. The Sample Changer is able to handle and expose sample volumes of down to 5 µl with a measurement/cleaning cycle of under 1 min. The samples are stored in standard 96-well plates and the data are collected in a vacuum-mounted capillary with automated positioning of the solution in the X-ray beam. Fast and efficient capillary cleaning avoids cross-contamination and ensures reproducibility of the measurements. Independent temperature control for the well storage and for the measurement capillary allows the samples to be kept cool while still collecting data at physiological temperatures. The Sample Changer has been installed at three major third-generation synchrotrons: on the BM29 beamline at the European Synchrotron Radiation Facility (ESRF), the P12 beamline at the PETRA-III synchrotron (EMBL@PETRA-III) and the I22/B21 beamlines at Diamond Light Source, with the latter being the first commercial unit supplied by Bruker ASC.

  7. Salt Dependence of the Radius of Gyration and Flexibility of Single-stranded DNA in Solution probed by Small-angle X-ray Scattering

    Energy Technology Data Exchange (ETDEWEB)

    Sim, Adelene Y.L.; Lipfert, Jan; Herschlag, Daniel; Doniach, Sebastian

    2012-07-06

    Short single-stranded nucleic acids are ubiquitous in biological processes and understanding their physical properties provides insights to nucleic acid folding and dynamics. We used small angle x-ray scattering to study 8-100 residue homopolymeric single-stranded DNAs in solution, without external forces or labeling probes. Poly-T's structural ensemble changes with increasing ionic strength in a manner consistent with a polyelectrolyte persistence length theory that accounts for molecular flexibility. For any number of residues, poly-A is consistently more elongated than poly-T, likely due to the tendency of A residues to form stronger base-stacking interactions than T residues.

  8. Revised Ionic Radii of Lanthanoid(III) Ions in Aqueous Solution

    International Nuclear Information System (INIS)

    A new set of ionic radii in aqueous solution has been derived for lanthanoid(III) cations starting from a very accurate experimental determination of the ion water distances obtained from extended X-ray absorption fine structure (EXAFS) data. At variance with previous results, a very regular. trend has been obtained, as expected for this series of elements. A general procedure to compute ionic radii in solution by combining the EXAFS technique and molecular dynamics (MD) structural data has been developed. This method can be applied to other ions allowing one to determine ionic radii in solution with an accuracy comparable to that of the Shannon crystal ionic radii. (authors)

  9. Interfacial Thermodynamics of Coexisting Aqueous Polymer Solutions

    NARCIS (Netherlands)

    Vis, M.

    2015-01-01

    Phase separation is commonly observed when two different polymers are present in aqueous solution, forming aqueous two-phase systems which typically consist for 90% of water. It is demonstrated that the presence of charge on one of the polymers results in an electric potential difference between the

  10. Kinetics of ptaquiloside hydrolysis in aqueous solution

    DEFF Research Database (Denmark)

    Ayala-Luis, Karina B.; Bildsøe Hansen, Pernille; Rasmussen, Lars Holm;

    2006-01-01

    of the toxin, a full understanding of the PTA degradation in aqueous environments is important. The kinetics of PTA hydrolysis was examined at 22C in aqueous buffered solutions (pH 2.88–8.93). The reaction was found to follow first-order kinetics with respect to PTA at all pH and temperature conditions. At p...

  11. On the nature of lithium biphenyl in ethereal solvents. A critical analysis unifying DFT calculations, physicochemical data in solution, and a X-ray structure.

    Science.gov (United States)

    de la Viuda, Mónica; Yus, Miguel; Guijarro, Albert

    2011-12-15

    The lithium ion is an important type of electrolyte that has technological applications in the manufacture of lithium ion cells; therefore, a better understanding of the nature of its solutions is desirable. When associated to the radical anion of biphenyl in an organic solvent, it forms conducting solutions comparable to strong electrolytes such as lithium perchlorate. We have studied the lithium biphenyl solution in dimethoxyethane using DFT calculations. The nature of these ionic solutions is described in terms of a dynamic equilibrium between different types of ionic associations, the composition of which depends on the solvent and the temperature. The X-ray structure of [Li(+)·4C(5)H(10)O][C(12)H(10)(•-)], a solvent-separated ion pair of lithium biphenyl complexed with tetrahydropyran, is reported. Its main structural characteristics coincide with the calculated one, which we think is the dominant species at room temperature, in agreement with the available physicochemical data.

  12. Tannin (Polyphenol) Stability in Aqueous Solutions

    Science.gov (United States)

    Understanding the chemical stability of tannins (polyphenolics) in soils is critical to understanding their biological activities and fate. We examined the stability of chemically defined tannins in aqueous solutions under conditions simulating natural and laboratory conditions. We evaluated tanni...

  13. Calorimetric studies of macromolecular aqueous solutions

    NARCIS (Netherlands)

    Blandamer, M.J; Cullis, P.M.; Engberts, J.B.F.N.

    1996-01-01

    Both titration and differential scanning microcalorimetric techniques are shown to yield important information concerning the properties of macromolecules in aqueous solution. Application of titration calorimetry is examined in me context of deaggregation of canonic micelles (e.g. hexadecyltrimethyl

  14. Heterojunction of Zinc Blende/Wurtzite in Zn1-xCdxS Solid Solution for Efficient Solar Hydrogen Generation: X-ray Absorption/Diffraction Approaches.

    Science.gov (United States)

    Hsu, Ying-Ya; Suen, Nian-Tzu; Chang, Chung-Chieh; Hung, Sung-Fu; Chen, Chi-Liang; Chan, Ting-Shan; Dong, Chung-Li; Chan, Chih-Chieh; Chen, San-Yuan; Chen, Hao Ming

    2015-10-14

    In the past decade, inorganic semiconductors have been successfully demonstrated as light absorbers in efficient solar water splitting to generate chemical fuels. Pseudobinary semiconductors Zn1-xCdxS (0≤x≤1) have exhibited a superior photocatalytic reactivity of H2 production from splitting of water by artificial solar irradiation without any metal catalysts. However, most studies had revealed that the extremely high efficiency with an optimal content of Zn1-xCdxS solid solution was determined as a result of elevating the conduction band minimum (CBM) and the width of bandgap. In addition to corresponding band structure and bandgap, the local crystal structure should be taken into account as well to determine its photocatalytic performance. Herein, we demonstrated the correlations between the photocatalytic activity and structural properties that were first studied through synchrotron X-ray diffraction and X-ray absorption spectroscopy. The crystal structure transformed from zinc blende to coexisted phases of major zinc blende and minor wurtzite phases at a critical point. The heterojunction formed by coexistence of zinc blende and wurtzite phases in the Zn1-xCdxS solid solution can significantly improve the separation and migration of photoinduced electron-hole pairs. Besides, X-ray absorption spectra and UV-vis spectra revealed that the bandgap of the Zn0.45Cd0.55S sample extended into the region of visible light because of the incorporation of Cd element in the sample. These results provided a significant progress toward the realization of the photoelectrochemical mechanism in heterojunction between zinc blende and wurtzite phases, which can effectively separate the charge-carriers and further suppress their recombination to enhance the photocatalytic reactivity. PMID:26402651

  15. Relaxation of the structure of simple metal ion complexes in aqueous solutions at up to supercritical conditions

    Science.gov (United States)

    Mayanovic, Robert A.; Jayanetti, Sumedha; Anderson, Alan J.; Bassett, William A.; Chou, I.-Ming

    2003-01-01

    Recently x-ray absorption fine structure (XAFS) studies of various ions in aqueous solutions showed a variation of cation-ligand bond lengths, often coupled with other structure changes, with increasing temperatures. Thus, the variations of the structure of several metal ion complexes with temperature based on observations from the X-ray absorption fine structure (XAFS) studies in the hope that it will stimulate the development of either first- principles theory or molecular dynamics simulations that might adequately describes these results are discussed.

  16. X-ray - skeleton

    Science.gov (United States)

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

  17. Extremity x-ray

    Science.gov (United States)

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

  18. X-ray interferometers

    International Nuclear Information System (INIS)

    An improved type of amplitude-division x-ray interferometer is described. The wavelength at which the interferometer can operate is variable, allowing the instrument to be used to measure x-ray wavelength, and the angle of inclination is variable for sample investigation. (U.K.)

  19. Look fast: Crystallization of conjugated molecules during solution shearing probed in-situ and in real time by X-ray scattering

    KAUST Repository

    Smilgies, Detlef Matthias

    2012-12-20

    High-speed solution shearing, in which a drop of dissolved material is spread by a coating knife onto the substrate, has emerged as a versatile, yet simple coating technique to prepare high-mobility organic thin film transistors. Solution shearing and subsequent drying and crystallization of a thin film of conjugated molecules is probed in situ using microbeam grazing incidence wide-angle X-ray scattering (μGIWAXS). We demonstrate the advantages of this approach to study solution based crystal nucleation and growth, and identify casting parameter combinations to cast highly ordered and laterally aligned molecular thin films. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. BioSAXS Sample Changer: a robotic sample changer for rapid and reliable high-throughput X-ray solution scattering experiments

    Science.gov (United States)

    Round, Adam; Felisaz, Franck; Fodinger, Lukas; Gobbo, Alexandre; Huet, Julien; Villard, Cyril; Blanchet, Clement E.; Pernot, Petra; McSweeney, Sean; Roessle, Manfred; Svergun, Dmitri I.; Cipriani, Florent

    2015-01-01

    Small-angle X-ray scattering (SAXS) of macromolecules in solution is in increasing demand by an ever more diverse research community, both academic and industrial. To better serve user needs, and to allow automated and high-throughput operation, a sample changer (BioSAXS Sample Changer) that is able to perform unattended measurements of up to several hundred samples per day has been developed. The Sample Changer is able to handle and expose sample volumes of down to 5 µl with a measurement/cleaning cycle of under 1 min. The samples are stored in standard 96-well plates and the data are collected in a vacuum-mounted capillary with automated positioning of the solution in the X-ray beam. Fast and efficient capillary cleaning avoids cross-contamination and ensures reproducibility of the measurements. Independent temperature control for the well storage and for the measurement capillary allows the samples to be kept cool while still collecting data at physiological temperatures. The Sample Changer has been installed at three major third-generation synchrotrons: on the BM29 beamline at the European Synchrotron Radiation Facility (ESRF), the P12 beamline at the PETRA-III synchrotron (EMBL@PETRA-III) and the I22/B21 beamlines at Diamond Light Source, with the latter being the first commercial unit supplied by Bruker ASC. PMID:25615861

  1. Femtosecond X-ray solution scattering reveals that bond formation mechanism of a gold trimer complex is independent of excitation wavelength.

    Science.gov (United States)

    Kim, Kyung Hwan; Kim, Jong Goo; Oang, Key Young; Kim, Tae Wu; Ki, Hosung; Jo, Junbeom; Kim, Jeongho; Sato, Tokushi; Nozawa, Shunsuke; Adachi, Shin-Ichi; Ihee, Hyotcherl

    2016-07-01

    The [Au(CN)2 (-)]3 trimer in water experiences a strong van der Waals interaction between the d(10) gold atoms due to large relativistic effect and can serve as an excellent model system to study the bond formation process in real time. The trimer in the ground state (S0) exists as a bent structure without the covalent bond between the gold atoms, and upon the laser excitation, one electron in the antibonding orbital goes to the bonding orbital, thereby inducing the formation of a covalent bond between gold atoms. This process has been studied by various time-resolved techniques, and most of the interpretation on the structure and dynamics converge except that the structure of the first intermediate (S1) has been debated due to different interpretations between femtosecond optical spectroscopy and femtosecond X-ray solution scattering. Recently, the excitation wavelength of 267 nm employed in our previous scattering experiment was suggested as the culprit for misinterpretation. Here, we revisited this issue by performing femtosecond X-ray solution scattering with 310 nm excitation and compared the results with our previous study employing 267 nm excitation. The data show that a linear S1 structure is formed within 500 fs regardless of excitation wavelength and the structural dynamics observed at both excitation wavelengths are identical to each other within experimental errors. PMID:27191012

  2. BioSAXS Sample Changer: a robotic sample changer for rapid and reliable high-throughput X-ray solution scattering experiments.

    Science.gov (United States)

    Round, Adam; Felisaz, Franck; Fodinger, Lukas; Gobbo, Alexandre; Huet, Julien; Villard, Cyril; Blanchet, Clement E; Pernot, Petra; McSweeney, Sean; Roessle, Manfred; Svergun, Dmitri I; Cipriani, Florent

    2015-01-01

    Small-angle X-ray scattering (SAXS) of macromolecules in solution is in increasing demand by an ever more diverse research community, both academic and industrial. To better serve user needs, and to allow automated and high-throughput operation, a sample changer (BioSAXS Sample Changer) that is able to perform unattended measurements of up to several hundred samples per day has been developed. The Sample Changer is able to handle and expose sample volumes of down to 5 µl with a measurement/cleaning cycle of under 1 min. The samples are stored in standard 96-well plates and the data are collected in a vacuum-mounted capillary with automated positioning of the solution in the X-ray beam. Fast and efficient capillary cleaning avoids cross-contamination and ensures reproducibility of the measurements. Independent temperature control for the well storage and for the measurement capillary allows the samples to be kept cool while still collecting data at physiological temperatures. The Sample Changer has been installed at three major third-generation synchrotrons: on the BM29 beamline at the European Synchrotron Radiation Facility (ESRF), the P12 beamline at the PETRA-III synchrotron (EMBL@PETRA-III) and the I22/B21 beamlines at Diamond Light Source, with the latter being the first commercial unit supplied by Bruker ASC. PMID:25615861

  3. Femtosecond X-ray solution scattering reveals that bond formation mechanism of a gold trimer complex is independent of excitation wavelength

    Directory of Open Access Journals (Sweden)

    Kyung Hwan Kim

    2016-07-01

    Full Text Available The [Au(CN2−]3 trimer in water experiences a strong van der Waals interaction between the d10 gold atoms due to large relativistic effect and can serve as an excellent model system to study the bond formation process in real time. The trimer in the ground state (S0 exists as a bent structure without the covalent bond between the gold atoms, and upon the laser excitation, one electron in the antibonding orbital goes to the bonding orbital, thereby inducing the formation of a covalent bond between gold atoms. This process has been studied by various time-resolved techniques, and most of the interpretation on the structure and dynamics converge except that the structure of the first intermediate (S1 has been debated due to different interpretations between femtosecond optical spectroscopy and femtosecond X-ray solution scattering. Recently, the excitation wavelength of 267 nm employed in our previous scattering experiment was suggested as the culprit for misinterpretation. Here, we revisited this issue by performing femtosecond X-ray solution scattering with 310 nm excitation and compared the results with our previous study employing 267 nm excitation. The data show that a linear S1 structure is formed within 500 fs regardless of excitation wavelength and the structural dynamics observed at both excitation wavelengths are identical to each other within experimental errors.

  4. Synchrotron small angle x-ray scattering study of dye-sensitized/-unsensitized TiO2 nanoparticle colloidal solution

    Institute of Scientific and Technical Information of China (English)

    Hong Xin-Guo; Du Lu-Chao; Ye Man-Ping; Weng Yu-Xiang

    2004-01-01

    The wide-gap semiconductor TiO2 nanoparticles with and without dye sensitization have been studied by small angle x-ray scattering using synchrotron radiation. Surface properties of the colloidal TiO2 nanoparticles have been analysed in terms of the surface fractal dimensions (Ds), showing that Ds changes from 3.25 to 2.34 when TiO2nanoparticles are sensitized by ATRA (all-trans-retinoic acid), which reveals that the surface of the particles become relatively smooth after dye sensitization. The size distribution of gyration radius of TiO2 nanoparticles in the colloids M(Rg) has been successfully determined by the Shull-Roess method. The main peak of M(Rg) for the unsensitized TiO2colloid is located at 2.1nm, corresponding to a spherical diameter of 5.4nm, and this value for the ATRA sensitized TiO2increases to 2.4nm, indicating a spherical diameter of 6.4nm. Such a size enlargement of TiO2 nanoparticles suggests that there is a coating of ATRA on the TiO2 surface, supporting the view that a monolayer of the dye has been attached to the surface of the TiO2 nanoparticle.

  5. 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.

  6. Phase and Texture of Solution-Processed Copper Phthalocyanine Thin Films Investigated by Two-Dimensional Grazing Incidence X-Ray Diffraction

    Directory of Open Access Journals (Sweden)

    Lulu Deng

    2011-07-01

    Full Text Available The phase and texture of a newly developed solution-processed copper phthalocyanine (CuPc thin film have been investigated by two-dimensional grazing incidence X-ray diffraction. The results show that it has β phase crystalline structure, with crystallinity greater than 80%. The average size of the crystallites is found to be about 24 nm. There are two different arrangements of crystallites, with one dominating the diffraction pattern. Both of them have preferred orientation along the thin film normal. Based on the similarities to the vacuum deposited CuPc thin films, the new solution processing method is verified to offer a good alternative to vacuum process, for the fabrication of low cost small molecule based organic photovoltaics.

  7. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... Resources Professions Site Index A-Z X-ray (Radiography) - Bone Bone x-ray uses a very small ... X-ray (Radiography)? What is Bone X-ray (Radiography)? An x-ray (radiograph) is a noninvasive medical ...

  8. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... Professions Site Index A-Z X-ray (Radiography) - Bone Bone x-ray uses a very small dose ... limitations of Bone X-ray (Radiography)? What is Bone X-ray (Radiography)? An x-ray (radiograph) is ...

  9. Lumbosacral spine x-ray

    Science.gov (United States)

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

  10. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... News Physician Resources Professions Site Index A-Z X-ray (Radiography) - Bone Bone x-ray uses a very ... of Bone X-ray (Radiography)? What is Bone X-ray (Radiography)? An x-ray (radiograph) is a noninvasive ...

  11. Abdomen X-Ray (Radiography)

    Science.gov (United States)

    ... News Physician Resources Professions Site Index A-Z X-ray (Radiography) - Abdomen Abdominal x-ray uses a very ... of an abdominal x-ray? What is abdominal x-ray? An x-ray (radiograph) is a noninvasive medical ...

  12. X-ray lasers

    CERN Document Server

    Elton, Raymond C

    2012-01-01

    The first in its field, this book is both an introduction to x-ray lasers and a how-to guide for specialists. It provides new entrants and others interested in the field with a comprehensive overview and describes useful examples of analysis and experiments as background and guidance for researchers undertaking new laser designs. In one succinct volume, X-Ray Lasers collects the knowledge and experience gained in two decades of x-ray laser development and conveys the exciting challenges and possibilities still to come._Add on for longer version of blurb_M>The reader is first introduced

  13. Femtosecond time-resolved X-ray absorption spectroscopy of liquid using a hard X-ray free electron laser in a dual-beam dispersive detection method.

    Science.gov (United States)

    Obara, Yuki; Katayama, Tetsuo; Ogi, Yoshihiro; Suzuki, Takayuki; Kurahashi, Naoya; Karashima, Shutaro; Chiba, Yuhei; Isokawa, Yusuke; Togashi, Tadashi; Inubushi, Yuichi; Yabashi, Makina; Suzuki, Toshinori; Misawa, Kazuhiko

    2014-01-13

    We present femtosecond time-resolved X-ray absorption spectroscopy of aqueous solution using a hard x-ray free electron laser (SACLA) and a synchronized Ti:sapphire laser. The instrumental response time is 200 fs, and the repetition rate of measurement is 10 Hz. A cylindrical liquid beam 100 μm in diameter of aqueous ammonium iron(III) oxalate solution is photoexcited at 400 nm, and the transient X-ray absorption spectra are measured in the K-edge region of iron, 7.10 - 7.26 keV, using a dual X-ray beam dispersive detection method. Each of the dual beams has the pulse energy of 1.4 μJ, and pump-induced absorbance change on the order of 10(-3) is successfully detected. The photoexcited iron complex exhibits a red shifted iron K-edge with the appearance time constant of 260 fs. The X-ray absorption difference spectra, with and without the pump pulses, are independent of time delay after 1.5 ps up to 100 ps, indicating that the photoexcited species is long-lived.

  14. X-Ray Diffraction.

    Science.gov (United States)

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

    1980-01-01

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

  15. Medical X-Rays

    Science.gov (United States)

    ... The Conference of Radiation Control Program Directors (CRCPD) publishes Suggested State Regulations for the Control of Radiation , ... eSubmitter Guidance for Industry and Food and Drug Administration Staff - Assembler's Guide to Diagnostic X-Ray Equipment ...

  16. Chest X-Ray

    Medline Plus

    Full Text Available ... However, it’s important to consider the likelihood of benefit to your health. While a chest x-ray use a tiny dose of ionizing radiation, the benefit of an accurate diagnosis far outweighs any risk. ...

  17. Chest X-Ray

    Medline Plus

    Full Text Available ... chest x-ray is used to evaluate the lungs, heart and chest wall and may be used ... diagnose and monitor treatment for a variety of lung conditions such as pneumonia, emphysema and cancer. A ...

  18. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... drawer under the table holds the x-ray film or image recording plate . Sometimes the x-ray ... extended over the patient while an x-ray film holder or image recording plate is placed beneath ...

  19. Columnar molecular aggregation in the aqueous solutions of disodium cromoglycate

    Science.gov (United States)

    Agra-Kooijman, Dena M.; Singh, Gautam; Lorenz, Alexander; Collings, Peter J.; Kitzerow, Heinz-S.; Kumar, Satyendra

    2014-06-01

    Stack, chimneylike, and threadlike assemblies have previously been proposed for the structure of disodium cromoglycate (DSCG) aggregates in aqueous solutions. The results of the synchrotron x-ray scattering investigations reported here reveal the formation of simple columnar assemblies with π-π stacking at a separation of 3.4 Å between the DSCG molecules. Lateral separation between the assemblies is concentration and temperature dependent, varying from ˜35 to 42 Å in the orientationally ordered nematic (N) phase and from 27 to 32 Å in the columnar or middle (M) phase having long range lateral positional order. The assemblies' length depends on concentration and consists of ˜23 molecules in the N phase, becoming three to ten times larger in the M phase. The scission energy is concentration dependent in the N phase with values ˜7.19 ± 0.14 kBT (15 wt %), 2.73 ± 0.4 kBT (20 wt %), and 3.05 ± 0.2 kBT (25 wt %). Solutions of all concentrations undergo a spinodal decomposition at temperatures above ˜40 °C, resulting in DSCG-rich regions with the M phase and water-rich regions in the N and isotropic phases.

  20. Hydrophobic Solvation: Aqueous Methane Solutions

    Science.gov (United States)

    Konrod, Oliver; Lankau, Timm

    2007-01-01

    A basic introduction to concept of a solvation shell around an apolar solute as well as its detection is presented. The hydrophobic solvation of toluene is found to be a good teaching example which connects macroscopic, phenomenological thermodynamic results with an atomistic point of view.

  1. Issues in Freeze Drying of Aqueous Solutions

    Institute of Scientific and Technical Information of China (English)

    王维; 陈墨; 陈国华

    2012-01-01

    Freeze drying or lyophilization of aqueous solutions is widely used in pharmaceutical industry. The in-creased importance Of the process is gaining a worldwide interest of research. A growing body of literature has demonstrated that the scientific approach can result in improved product quality with minimum trial and error em-piricism. Formulation and process development need a systematical understanding of the physical chemistry of freezing and freeze drying, material science and mechanisms of heat and mass transfer. This paper presents an overview on freeze ding of aqueous solutions based on publications in the past few decades. The important issuesof the process are analyzed.

  2. Thermodynamic modeling of poorly complexing metals in concentrated electrolyte solutions: an X-ray absorption and UV-Vis spectroscopic study of Ni(II) in the NiCl2-MgCl2-H2O system.

    Science.gov (United States)

    Zhang, Ning; Brugger, Joël; Etschmann, Barbara; Ngothai, Yung; Zeng, Dewen

    2015-01-01

    Knowledge of the structure and speciation of aqueous Ni(II)-chloride complexes is important for understanding Ni behavior in hydrometallurgical extraction. The effect of concentration on the first-shell structure of Ni(II) in aqueous NiCl2 and NiCl2-MgCl2 solutions was investigated by Ni K edge X-ray absorption (XAS) and UV-Vis spectroscopy at ambient conditions. Both techniques show that no large structural change (e.g., transition from octahedral to tetrahedral-like configuration) occurs. Both methods confirm that the Ni(II) aqua ion (with six coordinated water molecules at RNi-O = 2.07(2) Å) is the dominant species over the whole NiCl2 concentration range. However, XANES, EXAFS and UV-Vis data show subtle changes at high salinity (> 2 mol∙kg(-1) NiCl2), which are consistent with the formation of small amounts of the NiCl+ complex (up to 0.44(23) Cl at a Ni-Cl distance of 2.35(2) Å in 5.05 mol∙kg(-1) NiCl2) in the pure NiCl2 solutions. At high Cl:Ni ratio in the NiCl2-MgCl2-H2O solutions, small amounts of [NiCl2]0 are also present. We developed a speciation-based mixed-solvent electrolyte (MSE) model to describe activity-composition relationships in NiCl2-MgCl2-H2O solutions, and at the same time predict Ni(II) speciation that is consistent with our XAS and UV-Vis data and with existing literature data up to the solubility limit, resolving a long-standing uncertainty about the role of chloride complexing in this system. PMID:25885410

  3. Thermodynamic modeling of poorly complexing metals in concentrated electrolyte solutions: an X-ray absorption and UV-Vis spectroscopic study of Ni(II in the NiCl2-MgCl2-H2O system.

    Directory of Open Access Journals (Sweden)

    Ning Zhang

    Full Text Available Knowledge of the structure and speciation of aqueous Ni(II-chloride complexes is important for understanding Ni behavior in hydrometallurgical extraction. The effect of concentration on the first-shell structure of Ni(II in aqueous NiCl2 and NiCl2-MgCl2 solutions was investigated by Ni K edge X-ray absorption (XAS and UV-Vis spectroscopy at ambient conditions. Both techniques show that no large structural change (e.g., transition from octahedral to tetrahedral-like configuration occurs. Both methods confirm that the Ni(II aqua ion (with six coordinated water molecules at RNi-O = 2.07(2 Å is the dominant species over the whole NiCl2 concentration range. However, XANES, EXAFS and UV-Vis data show subtle changes at high salinity (> 2 mol∙kg(-1 NiCl2, which are consistent with the formation of small amounts of the NiCl+ complex (up to 0.44(23 Cl at a Ni-Cl distance of 2.35(2 Å in 5.05 mol∙kg(-1 NiCl2 in the pure NiCl2 solutions. At high Cl:Ni ratio in the NiCl2-MgCl2-H2O solutions, small amounts of [NiCl2]0 are also present. We developed a speciation-based mixed-solvent electrolyte (MSE model to describe activity-composition relationships in NiCl2-MgCl2-H2O solutions, and at the same time predict Ni(II speciation that is consistent with our XAS and UV-Vis data and with existing literature data up to the solubility limit, resolving a long-standing uncertainty about the role of chloride complexing in this system.

  4. Investigation of the topological shape of bovine serum albumin in solution by small-angle x-ray scattering at Beijing synchrotron radiation facility

    International Nuclear Information System (INIS)

    This paper reports that at a newly constructed small-angle x-ray scattering station of Beijing Synchrotron Radiation Facility, the topological shape of ligand-free bovine serum albumin in solution has been investigated. An appropriate scattering curve is obtained and the calculated value of the gyration radius is 31.2ű0.25A (1Å=0.1 nm) which is coincident with other ones' results. It finds that the low-resolution structure models obtained by making use of ab initio reconstruction methods are fitting the crystal structure of human serum albumin very well. All of these results perform the potential of the beamline to apply to structural biology studies. The characteristics, the defects, and the improving measures of the station in future are also discussed. (condensed matter: structure, thermal and mechanical properties)

  5. Solution properties of a hydrophobically associating polyacrylamide and its polyelectrolyte derivatives determined by Light Scattering, Small Angle X-ray Scattering and viscometry

    Energy Technology Data Exchange (ETDEWEB)

    Maia, Ana M.S.; Vidal, Rosangela R.L.; Balaban, Rosangela C., E-mail: balaban@supercabo.com.b [Universidade Federal do Rio Grande do Norte (LAPET/DQ/UFRN), Natal, RN (Brazil). Dept. de Quimica. Lab. de Pesquisa em Petroleo; Villetti, Marcos A. [Universidade Federal de Santa Maria (DF/UFSM), RS (Brazil). Dept. de Fisica; Borsali, Redouane [Universite Bordeaux 1, Pessac Cedex (France)

    2011-07-01

    A hydrophobically-modified polyacrylamide and two partially hydrolyzed derivatives containing hydrophobic and carboxylic groups were prepared by micellar polymerization and post hydrolysis. The molecular weight, second virial coefficient and radius of gyration were determined by static light scattering (SLS). Dynamic light scattering (DLS) and small-angle X-ray scattering (SAXS) were employed to determine the aggregate formation and type of chain packing in the semidilute regime, respectively. The behavior of solutions in dilute and semidilute regimes was also studied by viscometry and rheology. The hydrophobically-modified polyacrylamide showed a tendency to form aggregates due to the hydrophobic groups, but not enough to increase apparent viscosity. The partially hydrolyzed derivatives did not show the same aggregate-forming tendency. Rather, they exhibited anisotropic behavior, due to the charge density introduced into the polymer chain, which led to a more elongated macromolecular conformation and higher viscosity. (author)

  6. Evaluation of an L/sub III/ x-ray absorption-edge densitometer for assay of mixed uranium-plutonium solutions

    International Nuclear Information System (INIS)

    An L/sub III/ x-ray absorption-edge densitometer (XRAED), designed and built at Los Alamos Scientific Laboratory, has been evaluated at Savannah River Laboratory for the assay of uranium and plutonium in process solutions. Fro 2000-second data collection, the precisions (95% confidence level) for uranium assays varied +- 1.04% at 10 g of uranium per liter to 0.34% at 45 g/L, and plutonium assays varied from +- 6.7% at 2 g of plutonium per liter to +- 2.2% at 10 g/L. Hydroxylamine nitrate, a reducing agent used in solvent extraction tests, affect the accuracies of both uranium and plutonium assay by densitometry, and plutonium analysis by coulometry. It appears that the XRAED could be used to control the SRL miniature mixer-settlers, but additional testing will be needed to demonstrate that XRAED accuracy is sufficient for accountability of special nuclear materials

  7. Tetraethyl Orthosilicate Coated Hydroxyapatite Powders for Lead Ions Removal from Aqueous Solutions

    Directory of Open Access Journals (Sweden)

    Rodica V. Ghita

    2014-01-01

    Full Text Available The goal of this study was to synthetize and characterize a porous material based on tetraethyl orthosilicate (TEOS coated hydroxyapatite (HApTh after removal experiments of Pb2+ ions from aqueous solutions. In order to study the morphology and composition, the samples obtained after removal experiments of Pb2+ ions from aqueous solution with the initial Pb2+ ion concentrations of the aqueous solutions were 0.1 g·L−1 (HApTh-50 and 0.9 g·L−1 (HApTh-450 have been investigated by scanning electron microscopy (SEM equipped with an energy dispersive X-ray spectrometer (EDS, Fourier transform infrared spectroscopy (FTIR, and transmission electron microscopy (TEM. Removal experiments of Pb2+ ions were carried out in aqueous solutions with controlled concentration of Pb2+. After the removal experiment of Pb2+ ions from solutions, porous hydroxyapatite nanoparticles were transformed into HApTh-50 and HApTh-450 due to the adsorption of Pb2+ ions followed by a cation exchange reaction. The obtained results show that the porous HApTh nanopowders could be used for Pb2+ ions removal from aqueous solutions.

  8. Laser plasma x-ray source for ultrafast time-resolved x-ray absorption spectroscopy.

    Science.gov (United States)

    Miaja-Avila, L; O'Neil, G C; Uhlig, J; Cromer, C L; Dowell, M L; Jimenez, R; Hoover, A S; Silverman, K L; Ullom, J N

    2015-03-01

    We describe a laser-driven x-ray plasma source designed for ultrafast x-ray absorption spectroscopy. The source is comprised of a 1 kHz, 20 W, femtosecond pulsed infrared laser and a water target. We present the x-ray spectra as a function of laser energy and pulse duration. Additionally, we investigate the plasma temperature and photon flux as we vary the laser energy. We obtain a 75 μm FWHM x-ray spot size, containing ∼10(6) photons/s, by focusing the produced x-rays with a polycapillary optic. Since the acquisition of x-ray absorption spectra requires the averaging of measurements from >10(7) laser pulses, we also present data on the source stability, including single pulse measurements of the x-ray yield and the x-ray spectral shape. In single pulse measurements, the x-ray flux has a measured standard deviation of 8%, where the laser pointing is the main cause of variability. Further, we show that the variability in x-ray spectral shape from single pulses is low, thus justifying the combining of x-rays obtained from different laser pulses into a single spectrum. Finally, we show a static x-ray absorption spectrum of a ferrioxalate solution as detected by a microcalorimeter array. Altogether, our results demonstrate that this water-jet based plasma source is a suitable candidate for laboratory-based time-resolved x-ray absorption spectroscopy experiments.

  9. Laser plasma x-ray source for ultrafast time-resolved x-ray absorption spectroscopy

    Directory of Open Access Journals (Sweden)

    L. Miaja-Avila

    2015-03-01

    Full Text Available We describe a laser-driven x-ray plasma source designed for ultrafast x-ray absorption spectroscopy. The source is comprised of a 1 kHz, 20 W, femtosecond pulsed infrared laser and a water target. We present the x-ray spectra as a function of laser energy and pulse duration. Additionally, we investigate the plasma temperature and photon flux as we vary the laser energy. We obtain a 75 μm FWHM x-ray spot size, containing ∼106 photons/s, by focusing the produced x-rays with a polycapillary optic. Since the acquisition of x-ray absorption spectra requires the averaging of measurements from >107 laser pulses, we also present data on the source stability, including single pulse measurements of the x-ray yield and the x-ray spectral shape. In single pulse measurements, the x-ray flux has a measured standard deviation of 8%, where the laser pointing is the main cause of variability. Further, we show that the variability in x-ray spectral shape from single pulses is low, thus justifying the combining of x-rays obtained from different laser pulses into a single spectrum. Finally, we show a static x-ray absorption spectrum of a ferrioxalate solution as detected by a microcalorimeter array. Altogether, our results demonstrate that this water-jet based plasma source is a suitable candidate for laboratory-based time-resolved x-ray absorption spectroscopy experiments.

  10. Quasi-Immiscible Spreading of Aqueous Surfactant Solutions on Entangled Aqueous Polymer Solution Subphases

    OpenAIRE

    Sharma, Ramankur; Corcoran, Timothy E.; Garoff, Stephen; Przybycien, Todd M.; Swanson, Ellen R.; Tilton, Robert D.

    2013-01-01

    Motivated by the possibility of enhancing aerosol drug delivery to mucus-obstructed lungs, the spreading of a drop of aqueous surfactant solution on a physically entangled aqueous poly(acrylamide) solution subphase that mimics lung airway surface liquid was investigated. Sodium dodecyl sulfate was used as the surfactant. To visualize spreading of the drop and mimic the inclusion of a drug substance, fluorescein, a hydrophilic and non-surface active dye, was added to the surfactant solution. T...

  11. Aqueous Solution Chemistry on Mars

    Science.gov (United States)

    Quinn, R.; Hecht, M.; Kounaves, S.; Young, S.; West, S.; Fisher, A.; Grunthaner, P.

    2007-12-01

    Currently en route to Mars, the Phoenix mission carries four wet chemistry cells designed to perform basic solution chemistry on martian soil. The measurement objectives are typical of those that would be performed on an unknown sample on Earth, including detection of common anions and cations, total conductivity, pH, redox potential, cyclic voltammetry (CV), etc. Both the challenge and the novelty arise from the necessity to perform these measurements with severely constrained resources in a harsh and (literally) alien environment. Sensors for all measurements are integrated into a common "beaker," with the ability to perform a two-point calibration of some sensors using a pair of low-concentration solutions. Sulfate measurement is performed with a crude titration. While most measurements use ion selective electrodes, halide interferences are resolved by independent chronopotentiometry (CP) measurements. No preconditioning of the soil-water mixture is possible, nor is any physical characterization of the introduced soil sample beyond coarse visual inspection. Among the idiosyncrasies of the measurement is the low external pressure, which requires that the analysis be performed close to the boiling point of water under an atmosphere consisting almost entirely of water vapor. Despite these liabilities, however, extensive laboratory characterization has validated the basic approach, and protocols for both CV and CP have been developed and tested. Enhancing the value of the measurement is the suite of coordinated observations, such as microscopy and evolved gas analysis, to be performed by other Phoenix instruments.

  12. Dodecylsulfate and dodecybenzenesulfonate intercalated hydrotalcites as adsorbent materials for the removal of BBR acid dye from aqueous solutions

    OpenAIRE

    Mohamed Bouraada; Mohand Said Ouali; Louis Charles de Ménorval

    2016-01-01

    Two modified layered double hydroxides (HT) have been synthesized by intercalating both sodium dodecylsulfate (SDS) and sodium dodecylbenzenesulfonate (SDBS) surfactants into Mg-Al layered double hydroxides using the calcination–rehydratation method. The prepared materials HT-SDS and HT-SDBS were characterized by X-ray diffraction, FTIR, thermal analysis and BET. The obtained materials were used for Brilliant Blue R (BBR) dye removal from aqueous solution. Batch studies were carried out to ad...

  13. Solid State Conductivity of Optimized Polypyrrole Coatings on Iron Obtained from Aqueous Sodium Salicylate Solution Determined by Impedance Spectroscopy

    OpenAIRE

    Włodarczyk, Karolina; Singer, Ferdinand; Jasiński, Piotr; Virtanen, Sannakaisa

    2014-01-01

    In this work the optimization procedure for corrosion resistance, surface analysis and electrical properties of PPy-Fe electrodes have been examined. Polypyrrole (PPy) film was electrochemically synthesized in a one step process from an aqueous solution of sodium salicylate and pyrrole with certain concentrations, different parameters and type of polymerization process. The PPy-Fe electrodes were analyzed using scanning electron microscopy (SEM) and x-ray photoelectron spectroscopy (XPS). The...

  14. Radium removal from aqueous sulphate solutions

    International Nuclear Information System (INIS)

    A process for removing radium from an aqueous sulphate solution also containing magnesium is claimed. The pH of the solution is less than 10. A soluble barium salt is added to the solution to precipitate radium as barium radium sulphate. The pH of the solution is then raised to at least 11 to precipitate an insoluble magnesium compound which collects the barium radium sulphate precipitate. The precipitates are separated from the solution. If the sulphate solution contains dissolved magnesium and other impurities at a pH not greater than 7, then the first step in the process involves raising the pH of the solution to a value not greater than 10 to precipitate some of the magnesium and a substantial proportion of the other impurities and separating the precipitate from the solution. The radium removal is a step in the treatment of liquids resulting from the sulphuric acid leaching of uranium ores

  15. Biosorption of arsenic from aqueous solution using dye waste.

    Science.gov (United States)

    Nigam, Shubha; Vankar, Padma S; Gopal, Krishna

    2013-02-01

    The purpose of this study is to examine on removal of arsenic from water by biosorption through potential application of herbal dye wastes. Four different flower dye residues (after extraction of natural dye) viz. Hibiscus rosasinensis, Rosa rosa, Tagetes erecta, and Canna indica were utilized successfully for the removal of arsenic from aqueous solution. Batch studies were carried out for various parameters viz. pH, sorbent dose, contact time, initial metal ion concentration, and temperature. Data were utilized for isothermal, kinetic, and thermodynamic studies. Scanning electron microscopy (SEM), energy-dispersive x-ray spectroscopy (EDAX), and Fourier transform infrared (FTIR) analyses of biomass were performed. The results showed that 1 g/100 ml for 5.0-5.5 h contact time at pH 6.0-7.5 with agitation rate 150 rpm provided 98, 96, 92, and 85 % maximum absorption of arsenic by R. rosa, H. rosasinensis, T. erecta, and C. indica, respectively, at initial concentration of 500 ppb. Data followed Langmuir isotherm showing sorption to be monolayer on heterogeneous surface of biosorbent. Negative values of ΔG° indicated spontaneous nature, whereas ΔH° indicates exothermic nature of system followed by pseudo-first-order adsorption kinetics. FTIR results showed apparent changes in functional group regions after metal chelation. SEM and EDAX analyses showed the changes in surface morphology of all test biosorbents. Herbal dye wastes, used as biosorbent, exhibited significant (85-98 %) removal of arsenic from aqueous solution. Hence, these biosorbents are cost-effective, easily available, eco-friendly, and comparatively more effective than other biosorbents already in use. These may be used to remove arsenic and other toxic metals from water. PMID:22661261

  16. X-ray Pulsars

    CERN Document Server

    Walter, Roland

    2016-01-01

    X-ray pulsars shine thanks to the conversion of the gravitational energy of accreted material to X-ray radiation. The accretion rate is modulated by geometrical and hydrodynamical effects in the stellar wind of the pulsar companions and/or by instabilities in accretion discs. Wind driven flows are highly unstable close to neutron stars and responsible for X-ray variability by factors $10^3$ on time scale of hours. Disk driven flows feature slower state transitions and quasi periodic oscillations related to orbital motion and precession or resonance. On shorter time scales, and closer to the surface of the neutron star, X-ray variability is dominated by the interactions of the accreting flow with the spinning magnetosphere. When the pulsar magnetic field is large, the flow is confined in a relatively narrow accretion column, whose geometrical properties drive the observed X-ray emission. In low magnetized systems, an increasing accretion rate allows the ignition of powerful explosive thermonuclear burning at t...

  17. Aqueous solutions of ionic liquids: microscopic assembly

    NARCIS (Netherlands)

    J.M. Vicent-Luna; D. Dubbeldam; P. Gómez-Álvarez; S. Calero

    2016-01-01

    Aqueous solutions of ionic liquids are of special interest, due to the distinctive properties of ionic liquids, in particular, their amphiphilic character. A better understanding of the structure-property relationships of such systems is hence desirable. One of the crucial molecular-level interactio

  18. Water & Aqueous Solutions. Final Progress Report

    Energy Technology Data Exchange (ETDEWEB)

    None

    2002-08-09

    The Gordon Research Conference (GRC) on Water & Aqueous Solutions was held at Holderness School, New Hampshire, 8/4/02 thru 8/9/02. Emphasis was placed on current unpublished research and discussion of the future target areas in this field.

  19. Morphology of polysorbate 80 (Tween 80) micelles in aqueous dimethyl sulfoxide solutions

    OpenAIRE

    Aizawa, Hideki

    2010-01-01

    The structures of micelles of the surfactant polysorbate 80 (Tween 80) in 0–50% aqueous dimethyl sulfoxide (DMSO) solutions (pH 7.2, ionic strength 2.44 mM) were investigated by means of small-angle X-ray scattering. At DMSO concentrations of 0–20%, core–shell cylinder micelles formed, and at 30–50% DMSO, core–shell discus micelles formed, that is, changing the hydrophobicity of the DMSO solvent mixture changed the micelles from core–shell cylinder micelles to core–shell discus micelles....

  20. Electrochemical deposition of coatings of highly entropic alloys from non-aqueous solutions

    Directory of Open Access Journals (Sweden)

    Jeníček V.

    2016-03-01

    Full Text Available The paper deals with electrochemical deposition of coatings of highly entropic alloys. These relatively new materials have been recently intensively studied. The paper describes the first results of electrochemical coating with highly entropic alloys by deposition from non-aqueous solutions. An electrochemical device was designed and coatings were deposited. The coatings were characterised with electronic microscopy scanning, atomic absorption spectrometry and X-ray diffraction methods and the combination of methods of thermic analysis of differential scanning calorimetry and thermogravimetry.

  1. Hydration properties and ionic radii of actinide(III) ions in aqueous solution

    International Nuclear Information System (INIS)

    Ionic radii of actinide(III) cations (from U(III) to Cf(III)) in aqueous solution have been derived for the first time starting from accurate experimental determination of the ion-water distances obtained by combining extended X-ray absorption fine structure (EXAFS) results and molecular dynamics (MD) structural data. A strong analogy has been found between the lanthanide and actinide series concerning hydration properties. The existence of a contraction of the An-O distance along the series has been highlighted, while no decrease of the hydration number is evident up to Cf(III). (authors)

  2. Morphology of modified biochar and its potential for phenol removal from aqueous solutions

    OpenAIRE

    Kostas A. Komnitsas; Dimitra eZaharaki

    2016-01-01

    In the present study, the efficiency of phenol removal from synthetic aqueous solutions by chemically modified biochar with the use of 1M KOH or 1M FeCl3 was investigated. Initially, biochar was produced after slow pyrolysis of three different agricultural wastes, namely pistachio (Pistacia vera L.) shells, pecan (Carya illinoinensis) shells and wood sawdust. The quality of biochar was assessed by evaluating its main properties, such as pH, surface area, porosity and C content. X-ray diffract...

  3. SEPARATION OF SCANDIUM FROM AQUEOUS SOLUTIONS

    Science.gov (United States)

    Peppard, D.F.; Nachtman, E.S.

    1958-02-25

    This patent relates to a process for the separation of scandium from yttrium, thorium, and trivalent rare earths and with their separation from each other. It has been found that scandium and yttrium can be separated from trivalent rare earths in acidic solution, for example, a solution 6 M in HCl, by contacting with tributyl phosphate, whereupon the scandum is preferentially extracted into the organic phase, leaving the yttrium and trivalent rare earths in the aqueous phase.

  4. Solution structure of the complex between CR2 SCR 1-2 and C3d of human complement: an X-ray scattering and sedimentation modelling study.

    Science.gov (United States)

    Gilbert, Hannah E; Eaton, Julian T; Hannan, Jonathan P; Holers, V Michael; Perkins, Stephen J

    2005-02-25

    Complement receptor type 2 (CR2, CD21) forms a tight complex with C3d, a fragment of C3, the major complement component. Previous crystal structures of the C3d-CR2 SCR 1-2 complex and free CR2 SCR 1-2 showed that the two SCR domains of CR2 form contact with each other in a closed V-shaped structure. SCR 1 and SCR 2 are connected by an unusually long eight-residue linker peptide. Medium-resolution solution structures for CR2 SCR 1-2, C3d, and their complex were determined by X-ray scattering and analytical ultracentrifugation. CR2 SCR 1-2 is monomeric. For CR2 SCR 1-2, its radius of gyration R(G) of 2.12(+/-0.05) nm, its maximum length of 10nm and its sedimentation coefficient s20,w(o) of 1.40(+/-0.03) S do not agree with those calculated from the crystal structures, and instead suggest an open structure. Computer modelling of the CR2 SCR1-2 solution structure was based on the structural randomisation of the eight-residue linker peptide joining SCR 1 and SCR 2 to give 9950 trial models. Comparisons with the X-ray scattering curve indicated that the most favoured arrangements for the two SCR domains corresponded to an open V-shaped structure with no contacts between the SCR domains. For C3d, X-ray scattering and sedimentation velocity experiments showed that it exists as a monomer-dimer equilibrium with a dissociation constant of 40 microM. The X-ray scattering curve for monomeric C3d gave an R(G) value of 1.95 nm, and this together with its s20,w(o) value of 3.17 S gave good agreement with the monomeric C3d crystal structure. Modelling of the C3d dimer gave good agreements with its scattering and ultracentrifugation parameters. For the complex, scattering and ultracentrifugation experiments showed that there was no dimerisation, indicating that the C3d dimerisation site was located close to the CR2 SCR 1-2 binding site. The R(G) value of 2.44(+/-0.1) nm, its length of 9 nm and its s20,w(o) value of 3.45(+/-0.01) S showed that its structure was not much more

  5. EXAFS study of the speciation of protactinium(V) in aqueous hydrofluoric acid solutions.

    Science.gov (United States)

    De Sio, Stéphanie M; Wilson, Richard E

    2014-12-01

    The speciation of protactinium(V) in hydrofluoric acid (HF) solutions was studied using X-ray absorption spectroscopy. Extended X-ray absorption fine structure measurements were performed on an aqueous solution of 0.05 M protactinium(V) with various HF concentrations ranging from 0.5 to 27 M in order to probe the protactinium coordination sphere with respect to the identity and number of coordinating ligands. The resulting fits to the spectra suggest the presence of an eight-coordinate homoleptic fluoro complex in highly concentrated fluoride solutions (27 M), with equilibrium between seven- and eight-coordinate fluoro complexes at moderate acidities, and in more dilute solutions, results indicate that one water molecule is likely to replace a fluoride in the first coordination sphere, at a distance of 2.54-2.57 Å. Comparisons of this chemistry with group V metals, niobium and tantalum, are presented, and the potential implications for these results on the hydrolytic behavior of protactinium in aqueous systems are discussed.

  6. X-ray astronomy

    International Nuclear Information System (INIS)

    This book contains the lectures, and the most important seminars held at the NATO meeting on X-Ray astronomy in Erice, July 1979. The meeting was an opportune forum to discuss the results of the first 8-months of operation of the X-ray satellite, HEAO-2 (Einstein Observatory) which was launched at the end of 1978. Besides surveying these results, the meeting covered extragalactic astronomy, including the relevant observations obtained in other portions of the electromagnetic spectrum (ultra-violet, optical, infrared and radio). The discussion on galactic X-ray sources essentially covered classical binaries, globular clusters and bursters and its significance to extragalactic sources and to high energy astrophysics was borne in mind. (orig.)

  7. Uranium biosorption from aqueous solution onto Eichhornia crassipes.

    Science.gov (United States)

    Yi, Zheng-ji; Yao, Jun; Chen, Hui-lun; Wang, Fei; Yuan, Zhi-min; Liu, Xing

    2016-04-01

    Batch experiments were conducted to investigate the biosorption of U(VI) from aqueous solutions onto the nonliving biomass of an aquatic macrophyte Eichhornia crassipes. The results showed that the adsorption of U(VI) onto E. crassipes was highly pH-dependent and the best pH for U(VI) removal was 5.5. U(VI) adsorption proceeded rapidly with an equilibrium time of 30 min and conformed to pseudo-second-order kinetics. The Langmuir isotherm model was determined to best describe U(VI) biosorption with a maximum monolayer adsorption capacity of 142.85 mg/g. Thermodynamic calculation results indicated that the U(VI) biosorption process was spontaneous and endothermic. Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy analysis implied that the functional groups (amino, hydroxyl, and carboxyl) may be responsible for the U(VI) adsorption process, in which the coordination and ion exchange mechanisms could be involved. We conclude that E. crassipes biomass is a promising biosorbent for the removal of uranium pollutants. PMID:26854553

  8. Investigation of optical spacer layers from solution based precursors for polymer solar cells using X-ray reflectometry

    DEFF Research Database (Denmark)

    Andersen, Philip Hvidthøft Delff; Skårhøj, Jakob; Andreasen, Jens Wenzel;

    2009-01-01

    Optical spacer layers based on titaniumalkoxide precursor solutions were prepared by spin-coating on top of bulk heterojunction layers based on poly-3-hexylthiophene (P3HT) and phenyl-C61-butyric acid methylester (PCBM). Models and experiment have shown that the performance of polymer solar cells...

  9. CRL X-RAY TUBE

    OpenAIRE

    Kolchevsky, N. N.; Petrov, P. V.

    2015-01-01

    A novel types of X-ray tubes with refractive lenses are proposed. CRL-R X-ray tube consists of Compound Refractive Lens- CRL and Reflection X-ray tube. CRL acts as X-ray window. CRL-T X-ray consists of CRL and Transmission X-ray tube. CRL acts as target for electron beam. CRL refractive lens acts as filter, collimator, waveguide and focusing lens. Properties and construction of the CRL X-ray tube are discussed.

  10. Structural analysis of flexible proteins in solution by SmallAngle X-ray Scattering combined with crystallography

    Energy Technology Data Exchange (ETDEWEB)

    Tsutakawa, Susan E.; Hura, Greg L.; Frankel, Ken A.; Cooper,Priscilla K.; Tainer, John A.

    2006-05-25

    In the last few years, SAXS of biological materials has been rapidly evolving and promises to move structural analysis to a new level. Recent innovations in SAXS data analysis allow ab initio shape predictions of proteins in solution. Furthermore, experimental scattering data can be compared to calculated scattering curves from the growing data base of solved structures and also identify aggregation and unfolded proteins. Combining SAXS results with atomic resolution structures enables detailed characterizations in solution of mass, radius, conformations, assembly, and shape changes associated with protein folding and functions. SAXS can efficiently reveal the spatial organization of protein domains, including domains missing from or disordered in known crystal structures, and establish cofactor or substrate-induced conformational changes. For flexible domains or unstructured regions that are not amenable for study by many other structural techniques, SAXS provides a unique technology. Here, we present SAXS shape predictions for PCNA that accurately predict a trimeric ring assembly and for a full-length DNA repair glycosylase with a large unstructured region. These new results in combination with illustrative published data show how SAXS combined with high resolution crystal structures efficiently establishes architectures, assemblies, conformations, and unstructured regions for proteins and protein complexes in solution.

  11. The 4D evolution of porosity during ongoing pressure-solution processes in NaCl using x-ray microtomography

    Science.gov (United States)

    Macente, Alice; Fusseis, Florian; Butler, Ian; Tudisco, Erika; Hall, Stephen; Andò, Edward

    2016-04-01

    Pressure-solution creep is a common deformation mechanism in the upper crust. It represents a mass transfer via dissolution-reprecipitation that critically affects the hydraulic properties of rocks. Successful management of safe radioactive storage sites in rock-salt deposits critically depends on an accurate knowledge of the hydro-mechanical behaviour of salt deposits. Despite numerous lab experiments that have been conducted, many aspects of pressure-solution are still poorly understood. There is little knowledge about the spatio-temporal evolution of porosity and permeability during pressure-solution creep. While rates of pressure-solution creep in silicates and carbonates are slow, which makes laboratory investigations of these materials impractical, compaction experiments have demonstrated that NaCl samples deform sufficiently fast to study pressure-solution creep in a lab environment at room temperature and modest loads. We present results from novel experiments that quantify the 4-dimensional (three spatial dimensions plus time) evolution of pressure-solution processes using in-situ x-ray microtomography. Our experiments are performed in custom made x-ray transparent presses. 5 mm diameter NaCl powder samples with a grain size of 250-300 μm are loaded dry into the press and pre-compacted to produce a starting aggregated material. The sample is then flooded with saturated NaCl solution and loaded uniaxially by means of a pneumatic actuator to a constant uniaxial stress. Different sample mixtures were tested, as well as different uniaxial loads. The resulting deformation of the samples is documented in 3-dimensional microtomographic datasets, acquired at regular time intervals. Image analysis allowed characterization of the microstructural evolution of the NaCl grains and the spatio-temporal distribution of porosity during ongoing mechanical and chemical compaction. The microtomography data have also been analysed with 3D Digital Image Correlation (3D-DIC or

  12. Removal of Indigo Carmine Dye from Aqueous Solution Using Magnesium Hydroxide as an Adsorbent

    Directory of Open Access Journals (Sweden)

    Thimmasandra Narayan Ramesh

    2015-01-01

    Full Text Available Magnesium hydroxide is used as an adsorbent for the removal of indigo carmine dye from aqueous solution. We have investigated the effectiveness of removal of indigo carmine dye from aqueous solutions at pH 6-7 and 12-13 using magnesium hydroxide thereby varying the dose of the adsorbent, concentration of the dye, duration, and temperature. Structural transformations of adsorbent during the adsorption process at different pH values are monitored using powder X-ray diffraction and infrared spectroscopy. Different types of adsorption isotherm models were evaluated and it was found that Langmuir isotherm fits well at both pH values (6-7 and 12-13. Adsorption of indigo carmine onto magnesium hydroxide at pH 6-7/pH 12-13 follows pseudo-second order rate kinetics.

  13. Structure and dynamics of a polysaccharide matrix: aqueous solutions of bacterial levan.

    Science.gov (United States)

    Benigar, Elizabeta; Dogsa, Iztok; Stopar, David; Jamnik, Andrej; Kralj Cigić, Irena; Tomšič, Matija

    2014-04-15

    The polysaccharide levan is a homopolymer of fructose and appears in nature as an important structural component of some bacterial biofilms. This paper reports the structural and dynamic properties of aqueous solutions of levan of various origin obtained from dynamic rheological, small-angle X-ray scattering, static and dynamic light scattering, as well as density and sound velocity measurements, determination of polymer branching after per-O-methylation, and microscopy. Besides samples of commercially available levan from Zymomonas mobilis and Erwinia herbicola, we also isolated, purified, and studied a levan sample from the biofilm of Bacillus subtilis. The results of dynamic rheological and light scattering measurements revealed very interesting viscoelastic properties of levan solutions even at very low polymer concentrations. The findings were complemented by small-angle X-ray scattering data that revealed some important differences in the structure of the aqueous levan solutions at the molecular level. Besides presenting detailed dynamic and structural results on the polysaccharide systems of various levans, one of the essential goals of this work was to point out the level of structural information that may be obtained for such polymer systems by combining basic physicochemical, rheological, and various light scattering techniques. PMID:24654746

  14. Chest X-Ray

    Medline Plus

    Full Text Available ... this Site RadiologyInfo.org is produced by: Image/Video Gallery Your radiologist explains chest x-ray. Transcript ... time! Spotlight Recently posted: Pediatric MRI Intravascular Ultrasound Video: Chest CT Video:Thyroid Ultrasound Video: Head CT ...

  15. Chest X-Ray

    Medline Plus

    Full Text Available ... Pediatric Ultrasound Video: Angioplasty & vascular stenting Video: Arthrography Radiology and You About this Site RadiologyInfo.org is ... radiologist explains chest x-ray. Transcript Welcome to Radiology Info dot org! Hello, I’m Dr. Geoffrey ...

  16. Chest X-Ray

    Medline Plus

    Full Text Available ... this Site RadiologyInfo.org is produced by: Image/Video Gallery Your radiologist explains chest x-ray. Transcript ... Recently posted: Focused Ultrasound for Uterine Fibroids Dementia Video: General Ultrasound Video: Pediatric Nuclear Medicine Radiology and ...

  17. Medical x-ray

    International Nuclear Information System (INIS)

    This book describes the fundamental subject about medical radiography. It is a multidisciplinary field that requires cross professional input from scientists, engineers and medical doctors. However, it is presented in simple language to suit different levels of readers from x-ray operators and radiographers to physists, general practitioners and radiology specialists.The book is written in accordance to the requirements of the standard syllabus approved by the Ministry of Health Malaysia for the training of medical x-ray operator and general practitioners. In general, the content is not only designed to provide relevant and essential subject for related professionals in medical radiological services such as x-ray operator, radiographer and radiologists, but also to address those in associated radiological services including nurses, medical technologists and physicists.The book is organized and arranged sequentially into 3 parts for easy reference: Radiation safety; X-ray equipment and associated facilities; Radiography practices. With proper grasping of all these parts, the radiological services could be provided with confident and the highest professional standard. Thus, medical imaging with highest quality that can provide useful diagnostic information at minimum doses and at cost effective could be assured

  18. Crystallization and preliminary X-ray diffraction analysis of two extracytoplasmic solute receptors of the DctP family from Bordetella pertussis

    Energy Technology Data Exchange (ETDEWEB)

    Rucktooa, Prakash; Huvent, Isabelle [UMR8161 CNRS Institut de Biologie de Lille, Laboratoire de Cristallographie Macromoléculaire, 1 Rue du Professeur Calmette, BP 447, 59021 Lille CEDEX (France); IFR 142, Institut Pasteur de Lille, 1 Rue du Professeur Calmette, BP 245, 59021 Lille CEDEX (France); Antoine, Rudy; Lecher, Sophie; Jacob-Dubuisson, Françoise, E-mail: francoise.jacob@ibl.fr [IFR 142, Institut Pasteur de Lille, 1 Rue du Professeur Calmette, BP 245, 59021 Lille CEDEX (France); INSERM-U629, Lille (France); Institut Pasteur de Lille, 1 Rue du Professeur Calmette, BP 245, 59021 Lille CEDEX (France); Villeret, Vincent, E-mail: francoise.jacob@ibl.fr; Bompard, Coralie [UMR8161 CNRS Institut de Biologie de Lille, Laboratoire de Cristallographie Macromoléculaire, 1 Rue du Professeur Calmette, BP 447, 59021 Lille CEDEX (France); IFR 142, Institut Pasteur de Lille, 1 Rue du Professeur Calmette, BP 245, 59021 Lille CEDEX (France)

    2006-10-01

    Sample preparation, crystallization and preliminary X-ray analysis are reported for two B. pertussis extracytoplasmic solute receptors. DctP6 and DctP7 are two Bordetella pertussis proteins which belong to the extracytoplasmic solute receptors (ESR) superfamily. ESRs are involved in the transport of substrates from the periplasm to the cytosol of Gram-negative bacteria. DctP6 and DctP7 have been crystallized and diffraction data were collected using a synchrotron-radiation source. DctP6 crystallized in space group P4{sub 1}2{sub 1}2, with unit-cell parameters a = 108.39, b = 108.39, c = 63.09 Å, while selenomethionyl-derivatized DctP7 crystallized in space group P2{sub 1}2{sub 1}2{sub 1}, with unit-cell parameters a = 64.87, b = 149.83, c = 170.65 Å. The three-dimensional structure of DctP7 will be determined by single-wavelength anomalous diffraction, while the DctP6 structure will be solved by molecular-replacement methods.

  19. Protein crowding in solution, frozen and freeze-dried states: small-angle neutron and X-ray scattering study of lysozyme/sorbitol/water systems

    Science.gov (United States)

    Krueger, Susan; Khodadadi, Sheila; Clark, Nicholas; McAuley, Arnold; Cristiglio, Viviana; Theyencheri, Narayanan; Curtis, Joseph; Shalaev, Evgenyi

    2015-03-01

    For effective preservation, proteins are often stored as frozen solutions or in glassy states using a freeze-drying process. However, aggregation is often observed after freeze-thaw or reconstitution of freeze-dried powder and the stability of the protein is no longer assured. In this study, small-angle neutron and X-ray scattering (SANS and SAXS) have been used to investigate changes in protein-protein interaction distances of a model protein/cryoprotectant system of lysozyme/sorbitol/water, under representative pharmaceutical processing conditions. The results demonstrate the utility of SAXS and SANS methods to monitor protein crowding at different stages of freezing and drying. The SANS measurements of solution samples showed at least one protein interaction peak corresponding to an interaction distance of ~ 90 Å. In the frozen state, two protein interaction peaks were observed by SANS with corresponding interaction distances at 40 Å as well as 90 Å. On the other hand, both SAXS and SANS data for freeze-dried samples showed three peaks, suggesting interaction distances ranging from ~ 15 Å to 170 Å. Possible interpretations of these interaction peaks will be discussed, as well as the role of sorbitol as a cryoprotectant during the freezing and drying process.

  20. Pyroelectric x-ray detectors and x-ray pyrometers

    International Nuclear Information System (INIS)

    This paper discusses pyroelectric detectors which are very promising x-ray detectors for intense pulsed x-ray/γ-ray measurements and can be used as x-ray pyrometers. They are fast, passive, and inherently flat in spectral response for low energy x-rays. The authors report tests of LiTaO3, Sr.5Ba.5Nb2O6 and LiNbO3 detectors at Nova laser with 1 ns low energy x-rays and at Zapp Z-pinch machine with 100 ns x-rays. The temporal and spectral responses are discussed

  1. Pyroelectric x-ray detectors and x-ray pyrometers

    International Nuclear Information System (INIS)

    Pyroelectric detectors are very promising x-ray detectors for intense pulsed x-ray/γ-ray measurements and can be used as x-ray pyrometers. They are fast, passive, and inherently flat in spectral response for low-energy x rays. We report our tests of LiTaO3 detectors at Nova laser with 1-ns low-energy x rays and at Zapp Z-pinch machine with 100-ns x rays. The temporal and spectral responses are discussed

  2. Removal of radium from aqueous sulphate solutions

    International Nuclear Information System (INIS)

    Radium is often present in ores and an aqueous solution associated with the ore may consequently contain dissolved radium. It is frequently necessary to remove radium from such solutions to reduce the total radium content to a prescribed low level before the solution can be returned to the environment. The present invention is based on the discovery that the total radium content can be reduced to a satisfactory level within a reasonable time by adding a soluble barium salt to a radium-containing sulphate solution which also contains dissolved magnesium at a pH not greater than about 0 to precipitate radium as barium radium sulphate, raising the pH to at least 11 to precipitate an insoluble magnesium compound which collects the barium radium sulphate precipitate, and separating substantially all of the precipitates from the solution

  3. Uranyl fluoride luminescence in acidic aqueous solutions

    International Nuclear Information System (INIS)

    Luminescence emission spectra and decay rates are reported for uranyl species in acidic aqueous solutions containing HF or added NaF. The longest luminescence lifetime, 0.269 ± 0.006 ms, was observed from uranyl in 1 M HF + 1 M HClO4 at 296 K and decreased with increasing temperature. Based on a luminescence dynamics model that assumes equilibrium among electronically excited uranyl fluoride species and free fluoride ion, this long lived uranyl luminescence in aqueous solution is attributed primarily to UO2F2. Studies on the effect of added LiNO3 or Na2WO4·2H2O showed relatively weak quenching of uranyl fluoride luminescence which suggests that high sensitivity determination of the UF6 content of WF6 gas should be feasible via uranyl luminescence analysis of hydrolyzed gas samples of impure WF6

  4. Zeolites as alcohol adsorbents from aqueous solutions

    Directory of Open Access Journals (Sweden)

    Cekova Blagica

    2006-01-01

    Full Text Available The potential usage of zeolites as adsorbents for the removal of organic molecules from water was investigated in a series of experiments with aqueous solutions of lower alcohols. This could represent a simple solution to the problem of cleaning up industrial wastewater as well as recovering valuable chemicals at relatively low costs. Adsorption isotherms of the Langmuir type were applied, and calculations showed that the amount of propanol adsorbed on silicalite corresponded to approximately 70% of the pore volume. The adsorption process is simple, and recovery of the more concentrated products is easily done by heat treatment and/or at lowered pressures. Adsorption experiments with aqueous acetone showed that silicalite had approximately the same adsorption capacity for acetone as for n-propanol. Heats of adsorption were determined calorimetrically.

  5. Sequestering of Cu(II) from aqueous solution using cassava peel (Manihot esculenta)

    Energy Technology Data Exchange (ETDEWEB)

    Kosasih, Aline Natasia; Febrianto, Jonathan [Department of Chemical Engineering, National Taiwan University of Science and Technology, 43, Sec. 4, Keelung Rd., Taipei 10607, Taiwan (China); Department of Chemical Engineering, Widya Mandala Surabaya Catholic University, Kalijudan 37, Surabaya 60114 (Indonesia); Sunarso, Jaka [School of Chemical Engineering, The University of Queensland, St. Lucia, QLD 4072 (Australia); Ju, Yi-Hsu [Department of Chemical Engineering, National Taiwan University of Science and Technology, 43, Sec. 4, Keelung Rd., Taipei 10607, Taiwan (China); Indraswati, Nani [Department of Chemical Engineering, Widya Mandala Surabaya Catholic University, Kalijudan 37, Surabaya 60114 (Indonesia); Ismadji, Suryadi, E-mail: suryadi@mail.wima.ac.id [Department of Chemical Engineering, National Taiwan University of Science and Technology, 43, Sec. 4, Keelung Rd., Taipei 10607, Taiwan (China); Department of Chemical Engineering, Widya Mandala Surabaya Catholic University, Kalijudan 37, Surabaya 60114 (Indonesia)

    2010-08-15

    Cassava peel is a prospective cheap biosorbent for metal ions sequestration. In this research, the ability of cassava peel to remove Cu(II) from aqueous solution was evaluated. Its physical characteristics were probed by nitrogen adsorption measurements and scanning electron microscopy while its biosorption mechanism was studied by Fourier Transform Infrared (FTIR), Scanning Electron Microscopy/Energy Dispersive using X-ray analysis-(SEM/EDX), X-ray mapping and X-ray Photoelectron Spectroscopy (XPS). Biosorption experiments were carried out isothermally at three different temperatures (30 deg. C, 45 deg. C and 60 deg. C) in a static mode. The maximum adsorption capacity (41.77 mg g{sup -1}) was attained at the highest temperature. The pH and particle size effects in relation to biosorption capacity were also discussed. In addition, Langmuir, Freundlich, Sips and Toth equations were tested for data correlation. Langmuir and Freundlich models were the best choices since they contained less parameter with equally good fitting performance in comparison to the other three parameters equations. For kinetic studies, sorption rates were better represented using a pseudo second-order expression in comparison to a more commonly used pseudo first-order equation. Also, thermodynamic variables showed that the process was spontaneous ({Delta}G < 0), endothermic ({Delta}H > 0) and irreversible ({Delta}S > 0).

  6. Sequestering of Cu(II) from aqueous solution using cassava peel (Manihot esculenta)

    International Nuclear Information System (INIS)

    Cassava peel is a prospective cheap biosorbent for metal ions sequestration. In this research, the ability of cassava peel to remove Cu(II) from aqueous solution was evaluated. Its physical characteristics were probed by nitrogen adsorption measurements and scanning electron microscopy while its biosorption mechanism was studied by Fourier Transform Infrared (FTIR), Scanning Electron Microscopy/Energy Dispersive using X-ray analysis-(SEM/EDX), X-ray mapping and X-ray Photoelectron Spectroscopy (XPS). Biosorption experiments were carried out isothermally at three different temperatures (30 deg. C, 45 deg. C and 60 deg. C) in a static mode. The maximum adsorption capacity (41.77 mg g-1) was attained at the highest temperature. The pH and particle size effects in relation to biosorption capacity were also discussed. In addition, Langmuir, Freundlich, Sips and Toth equations were tested for data correlation. Langmuir and Freundlich models were the best choices since they contained less parameter with equally good fitting performance in comparison to the other three parameters equations. For kinetic studies, sorption rates were better represented using a pseudo second-order expression in comparison to a more commonly used pseudo first-order equation. Also, thermodynamic variables showed that the process was spontaneous (ΔG 0) and irreversible (ΔS > 0).

  7. Studies on the X-Ray and Solution Structure of FeoB from Escherichia coli BL21.

    Science.gov (United States)

    Hagelueken, Gregor; Hoffmann, Jan; Schubert, Erik; Duthie, Fraser G; Florin, Nicole; Konrad, Lisa; Imhof, Diana; Behrmann, Elmar; Morgner, Nina; Schiemann, Olav

    2016-06-21

    The ferrous iron transporter FeoB is an important factor in the iron metabolism of many bacteria. Although several structural studies have been performed on its cytosolic GTPase domain (NFeoB), the full-length structure of FeoB remains elusive. Based on a crystal packing analysis that was performed on crystals of NFeoB, a trimeric structure of the FeoB channel was proposed, where the transport pore runs along the trimer axis. Because this trimer has not been observed in some subsequently solved structures of NFeoB homologs, it remains unclear whether or not the trimer is indeed functionally relevant. Here, pulsed electron-electron double resonance spectroscopy, negative stain electron microscopy, and native mass spectrometry are used to analyze the oligomeric state of different soluble and full-length FeoB constructs. The results show that the full-length protein is predominantly monomeric, whereas dimers and trimers are formed to a small percentage. Furthermore, the solution structure of the switch I region is analyzed by pulsed electron-electron double resonance spectroscopy and a new, to our knowledge, crystal structure of NFeoB from Escherichia coli BL21 is presented. PMID:27332122

  8. Does Dimeric Melittin Occur in Aqueous Solutions?

    OpenAIRE

    Schubert, D; Pappert, G.; Boss, K.

    1985-01-01

    Melittin, a peptide from bee venom, is known to undergo a monomer / tetramer conversion in aqueous solutions. We have studied the possible participation of dimers in the association equilibrium of melittin by sedimentation equilibrium experiments in the analytical ultracentrifuge and subsequent mathematical analysis of the concentration distributions obtained. It was found that the dimeric state is not significantly populated, the contribution of dimer to the total peptide weight probably bei...

  9. Aqueous solution dispersement of carbon nanotubes

    Science.gov (United States)

    Kim, Jae-Woo (Inventor); Park, Cheol (Inventor); Choi, Sang H. (Inventor); Lillehei, Peter T. (Inventor); Harrison, Joycelyn S. (Inventor)

    2011-01-01

    Carbon nanotubes (CNTs) are dispersed in an aqueous buffer solution consisting of at least 50 weight percent water and a remainder weight percent that includes a buffer material. The buffer material has a molecular structure defined by a first end, a second end, and a middle disposed between the first and second ends. The first end is a cyclic ring with nitrogen and oxygen heteroatomes, the middle is a hydrophobic alkyl chain, and the second end is a charged group.

  10. Theoretical study of the triplet excited state of PtPOP and the exciplexes M-PtPOP (M = Tl, Ag) in solution and comparison with ultrafast X-ray scattering results

    DEFF Research Database (Denmark)

    Kong, Qingyu; Kjær, Kasper S.; Haldrup, Martin Kristoffer;

    2012-01-01

    . Calculated results were compared with ultrafast X-ray solution scattering data. Time dependent DFT (TD-DFT) calculations with the B3PW91 functional and unrestricted open shell calculations with the mPBE functional produce good agreement with the experimental results. Compared to gas phase calculations...

  11. The removal of phenol from aqueous solutions by adsorption using surfactant-modified bentonite and kaolinite

    Energy Technology Data Exchange (ETDEWEB)

    Alkaram, Uday F.; Mukhlis, Abduljabar A. [Department of Chemistry, College of Education, Ibn Al-Haitham, University of Baghdad, Baghdad (Iraq); Al-Dujaili, Ammar H., E-mail: ahdujaili@yahoo.com [Department of Chemistry, College of Education, Ibn Al-Haitham, University of Baghdad, Baghdad (Iraq)

    2009-09-30

    The natural bentonite (BC) and kaolinite (KC) were modified with two surfactant of hexadecyltrimethylammonium bromide (HDTMA) and phenyltrimethylammonium bromide (PTMA) to form four kinds of organic-modified clays, i.e., HDTMA-bentonite (BHM), HDTMA-kaolinite (KHM), PTMA-bentonite (KPM) and PTMA-kaolinite (KPM). The modified minerals were characterized by X-ray fluorescence (XRF), X-ray diffraction (XRD) and FT-IR spectroscopy. The surface areas were determined using methylene blue adsorption method. Cation-exchange capacity (CEC) was estimated using an ethylenediamine complex of copper method and the modifier loading was calculated from the total carbon analysis. The ability of raw and organo-modified clays to remove phenol from aqueous solutions has been carried out as a function of contact time, pH and temperatures using a batch technique. The removal of phenol from aqueous solutions by modified clays seems to be more effective than unmodified samples. The adsorption capacity was found to increase with increasing temperature indication that the adsorptions were endothermic. The adsorption of phenol onto these clays was found to be increased by increasing of pH value and the adsorption patterns data are correlated well by Langmuir and Freundlich isotherm models and that the adsorption is physical in nature. The experimental data fitted very well with the pseudo-second-order kinetic model. The thermodynamic study of adsorption process showed that the adsorption of phenol with these six adsorbents was carried out spontaneously, and the process was endothermic in nature.

  12. OPTICAL PROPERTIES OF CARBAMIDE AQUEOUS SOLUTIONS

    Directory of Open Access Journals (Sweden)

    E. V. Avramenko

    2016-03-01

    Full Text Available Subject of Research. The paper presents the results of measurements of refractometric properties (refractive index n, its temperature factor dn/dt and the ultraviolet spectral absorption in carbonic acid diamide aqueous solutions (carbamide depending on solid residue mass fraction md = 0-50 % and on temperaturet = 10-70 °C.Method of Research. Laboratory methods ofliquid-phase medium refractometry and ultraviolet spectrophotometry were applied for the research. We carried out computational modeling of electronic states spectrum for the carbonic acid diamide molecule and theoretical calculation of the fundamental electronic absorption of the molecule in the ultraviolet wavelenght region.Main Results. We have established that the solution concentration md has a nonlinear character and may be represented by the quadratic polynomial with the error Δn= ± 0,0005. We have shown the refractive indexdependence on temperature n(t changes in linear fashion att = 10-70 °C.At that, the inclination of lines n(t increases at the increase of md; so, the temperature factor dn/dt may be approximated by the quadratic polynomial. Transmission spectra of solutions in the spectral region λ= 225-760 nm have no special features except for the sharp edge in the short-wavelength region; the fundamental electronic absorptionis responsible for it. We have established that dispersion dependences of the refraction index n(λ;md in aqueous solutions of carbamide at λ= 360-760 nm and at md = 0-50 % may be calculated with the satisfactory error without additional adjustable parameters from the ultraviolet absorption data in terms of the one-dimentional oscillator Lorentz model.PracticalRelevance. Representedmeasurements of carbonic acid diamide aqueous solutions optical properties may be applied for the adjustment and calibration of commercial refractometers at processing lines of the AdBlue reagent manufacture for the selective catalytic reduction (SCR of motor transport

  13. 21 CFR 524.1200b - Kanamycin ophthalmic aqueous solution.

    Science.gov (United States)

    2010-04-01

    ... § 524.1200b Kanamycin ophthalmic aqueous solution. (a) Specifications. The drug, which is in an aqueous solution including suitable and harmless preservatives and buffer substances, contains 10 milligrams of... 21 Food and Drugs 6 2010-04-01 2010-04-01 false Kanamycin ophthalmic aqueous solution....

  14. Ethylbenzene Removal from Aqueous Solutions by Nano Magnetic Particles

    Directory of Open Access Journals (Sweden)

    Mostafa Hadei

    2016-02-01

    Full Text Available Background and Objectives : Ethylbenzene (EB is a dangerously organic compound which the presence of this pollutant in water solutions can be considered as an environmental and public health hazard. In this study, nano magnetic particles (Fe 3 O 4 were used as an adsorbent to remove ethylbenzene from aqueous solutions. Methods : The specification of the adsorbent was investigated by transmission electronic microscope (TEM and X-ray diffraction (XRD pattern. A 4×4 factorial design including initial concentration of ethylbenzene, nano magnetic particles dose, contact time and pH were studied. Results : The results showed that the maximum ethylbenzene removal by nano magnetic particles was achieved in the following conditions; 100 mg.L -1 , 2000 mg.L -1 , 20 minutes and 8, in initial concentration, nano magnetic concentration, contact time and pH respectively. The most amounts of ethylbenzene adsorption and distribution ratio in optimum condition was 49.9 mg.g -1 and 261.9 l.g -1 respectively. The results demonstrated that the removal rate of ethylbenzene was higher in batch (99.8 % rather than continuous (97.4% condition. Conclusion: the removal rate of ethylbenzene was higher in batch rather than continuous condition.The study of isotherm showed that adsorption data follow up linear isotherm. Comparing adsorption rate of NM particles and other adsorbents proved that Fe 3 o 4 , as a material with high capacity of adsorption can apply for removing ethylbenzene as an efficient and also cheap adsorbent.  

  15. Novel magnetic Fe3O4-C nanoparticles as adsorbents for removal of organic dyes from aqueous solution

    International Nuclear Information System (INIS)

    Highlights: → In this work, novel magnetic Fe3O4-C nanoparticles have been synthesized and employed as high efficient adsorbent for removal cationic dyes from polluted water. → While up to now, little study is done on adsorption of dyes by the Fe3O4-C nanoparticles. → Hence, here we provide a simply and environment friendly method for removal of cationic dyes or other pollutants from water. - Abstract: The magnetic Fe3O4/C core-shell nanoparticles have been synthesized by a simple strategy and used as adsorbents for removal of organic dyes from aqueous solution. The resulting products are characterized by scanning electron microscope (SEM), energy dispersive X-ray spectrometry (EDX), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), Raman spectra and Fourier transform infrared spectra (FTIR). Adsorption performances of the nanomaterial adsorbents are tested with removal of methylene blue (MB) and cresol red (CR) from aqueous solution. The effects of solution pH value, adsorption time and capacity of the nanocomposites have been fully investigated. The results reveal that the nanospheres can be easily manipulated by an external magnetic field with high separation efficiency. In addition, the process is clean and safe for purifying water pollution. The prepared Fe3O4/C complex nanomaterials could thus be used as promising adsorbents for the remove organic dyes, especially, cationic dye, from polluted water.

  16. Comparative X-ray diffraction study of the crystalline microstructure of tetragonal and monoclinic vanadium-zirconium dioxide solid solutions produced from gel precursors

    Energy Technology Data Exchange (ETDEWEB)

    Kojdecki, Marek Andrzej [Wojskowa Akademia Techniczna, Warszawa (Poland). Inst. Matematyki i Kryptologii; Ruiz de Sola, Esther; Alarcon, Javier [Valencia Univ., Burjasot (Spain). Dept. de Quimica Inorganica; Serrano, Francisco Javier; Amigo, Jose Maria [Valencia Univ., Burjasot (Spain). Dept. de Geologia

    2009-04-15

    The microstructural characteristics of solid solutions, prepared by heating dried gel precursors with nominal compositions V{sub x}Zr{sub 1-x}O{sub 2} (0{<=}x{<=}0.1) at 723 and 1573 K, were determined from X-ray diffraction patterns. The crystalline microstructure of the resulting specimens, characterized by a prevalent crystallite shape, a volume-weighted crystallite size distribution and a second-order lattice strain distribution, was found to depend on the vanadium content. A characteristic feature of all size distributions was their bimodality, explained as a result of transformations between tetragonal and monoclinic phases during thermal treatment. A comparative study of the microstructure of both zirconia phases has been carried out, enabling reconstruction of a probable course of crystallization of both pure and vanadium-doped zirconias: on heating a sample, nucleation and the early growth stages involve crystallites of both phases; then on annealing and cooling, the crystallites of one phase transform into the other, depending on the thermal treatment temperature. Each logarithmic normal component of the crystallite size distribution of the resulting phase can be attributed to one of these processes. The limit of solubility of vanadium in tetragonal and monoclinic zirconia is estimated from the microstructural characteristics. (orig.)

  17. Synthesis and X-ray diffraction study of Cu{sub 2}ZnSn(S{sub x}Se{sub 1-x}){sub 4} solid solutions

    Energy Technology Data Exchange (ETDEWEB)

    Sheleg, A. U., E-mail: hurtavy@physics.by; Hurtavy, V. G.; Chumak, V. A. [State Scientific and Production Association “Scientific-Practical Materials Research Centre of the National Academy of Sciences of Belarus,” (Belarus)

    2015-09-15

    Quaternary compounds Cu{sub 2}ZnSnS{sub 4} and Cu{sub 2}ZnSnSe{sub 4} and solid solutions on their basis have been fabricated by one-temperature synthesis from elementary components: Cu, Zn, Sn, S, and Se. Single crystals of these compounds have been grown by the method of chemical gas-transport reactions from polycrystalline samples. The compositional dependence of the unit-cell parameters of Cu{sub 2}ZnSn(S{sub x}Se{sub 1–x}){sub 4} has been investigated by X-ray diffraction. It is found that parameters a and c linearly decrease with an increase in sulfur concentration in accordance with Vegard’s law. The temperature dependences of parameters a and thermalexpansion coefficients α{sub a} of Cu{sub 2}ZnSnS{sub 4} and Cu{sub 2}ZnSnSe{sub 4} single crystals in the range of 100–300 K are determined.

  18. Estimation of kinetic parameters of the passive state of carbon steel in mildly alkaline solutions from electrochemical impedance spectroscopic and X-ray photoelectron spectroscopic data

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, X.; Wren, J.C. [Department of Chemistry, University of Western Ontario, 1151 Richmond St, London, Ontario, N6A 5B7 (Canada); Betova, I. [Department of Chemistry, Technical University of Sofia, 1000 Sofia (Bulgaria); Bojinov, M., E-mail: martin@uctm.edu [Department of Physical Chemistry, University of Chemical Technology and Metallurgy, 1756 Sofia (Bulgaria)

    2011-07-01

    Highlights: > The passive state of carbon steel is described using the Mixed-Conduction Model for oxide films. > Kinetic parameters are estimated by comparison of the model to EIS and XPS data. > The passive film is intermediate between magnetite and maghemite. > Relevance of film growth and dissolution reactions for corrosion is discussed. - Abstract: The unambiguous interpretation of electrochemical impedance spectra of complex systems such as passive metals and alloys in terms of an unique kinetic model is often hampered by the large number of adjustable modeling parameters. In this paper, a combination of in situ electrochemical data and ex situ surface analytical information is employed to validate the estimates of kinetic and transport parameters of the passive state of carbon steel. For the purpose, electrochemical impedance spectroscopic and X-ray photoelectron spectroscopic data for the oxidation of carbon steel in mildly alkaline solutions are quantitatively compared with the predictions of the Mixed-Conduction Model for oxide films that represent the passive oxide as an intermediate phase between magnetite and maghemite. Estimates of the kinetic rate constants at the film interfaces, as well as the diffusion coefficients and field strength in the film are obtained and their relevance for the corrosion mechanism of carbon steel is discussed.

  19. X-ray diffraction

    International Nuclear Information System (INIS)

    We have been interested in structural elucidation by x-ray diffraction of compounds of biological interest. Understanding exactly how atoms are arranged in three-dimensional arrays as molecules can help explain the relationship between structure and functions. The species investigated may vary in size and shape; our recent studies included such diverse substances as antischistosomal drugs, a complex of cadmium with nucleic acid base, nitrate salts of adenine, and proteins

  20. Density of aqueous solutions of CO2

    Energy Technology Data Exchange (ETDEWEB)

    Garcia, Julio E.

    2001-10-10

    In this report, we present a numerical representation for the partial molar volume of CO2 in water and the calculation of the corresponding aqueous solution density. The motivation behind this work is related to the importance of having accurate representations for aqueous phase properties in the numerical simulation of carbon dioxide disposal into aquifers as well as in geothermal applications. According to reported experimental data the density of aqueous solutions of CO2 can be as much as 2-3% higher than pure water density. This density variation might produce an influence on the groundwater flow regime. For instance, in geologic sequestration of CO2, convective transport mixing might occur when, several years after injection of carbon dioxide has stopped, the CO2-rich gas phase is concentrated at the top of the formation, just below an overlaying caprock. In this particular case the heavier CO2 saturated water will flow downward and will be replaced by water with a lesser CO2 content.

  1. Aqueous solubility study of salts of benzylamine derivatives and p-substituted benzoic acid derivatives using X-ray crystallographic analysis

    DEFF Research Database (Denmark)

    Parshad, Henrik; Frydenvang, Karla Andrea; Liljefors, Tommy;

    2004-01-01

    Twenty two p-substituted benzoic acid derivates were used to prepare salts of N-methylbenzylamine (II) and N,N-dimethylbenzylamine (III), respectively. Only five salts of (II) and two salts of (III) were obtained in a crystalline state. The solubility of these salts was orders of magnitude higher...... than those reported for the corresponding salts of benzylamine (I). Thermal analysis indicated that the increased solubility was caused by reduced crystal lattice energy, which was most likely due to the reduced number of strong hydrogen bonds of the salt of (II) and (III). X-ray crystallographic...... analysis of p-hydroxybenzoic acid salt of (I), (II) and (III) suggested that the reduced number of hydrogen bonds caused the apparent higher solubility. Further analyses of seven salts of (I) were performed. It was not possible to identify any relationship between the number of hydrogen bonds...

  2. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... wrist, arm, elbow, shoulder, spine, pelvis, hip, thigh, knee, leg (shin), ankle or foot. top of page ... the patient standing upright, as in cases of knee x-rays. A portable x-ray machine is ...

  3. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... images for evaluation. National and international radiology protection organizations continually review and update the technique standards used by radiology professionals. Modern x-ray systems have very controlled x-ray beams and dose ...

  4. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... fracture. guide orthopedic surgery, such as spine repair/fusion, joint replacement and fracture reductions. look for injury, ... and Media Arthritis X-ray, Interventional Radiology and Nuclear Medicine Radiation Safety Images related to X-ray ( ...

  5. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... current x-ray images for diagnosis and disease management. top of page How is the procedure performed? ... top of page What are the benefits vs. risks? Benefits Bone x-rays are the fastest and ...

  6. Dental X-ray apparatus

    International Nuclear Information System (INIS)

    Intra-oral dental X-ray apparatus for panoramic radiography is described in detail. It comprises a tubular target carrier supporting at its distal end a target with an inclined forward face. Image definition is improved by positioning in the path of the X-rays a window of X-ray transmitting ceramic material, e.g. 90% oxide of Be, or Al, 7% Si02. The target carrier forms a probe which can be positioned in the patient's mouth. X-rays are directed forwardly and laterally of the target to an X-ray film positioned externally. The probe is provided with a detachable sleeve having V-form arms of X-ray opaque material which serve to depress the tongue out of the radiation path and also shield the roof of the mouth and other regions of the head from the X-ray pattern. A cylindrical lead shield defines the X-ray beam angle. (author)

  7. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... current x-ray images for diagnosis and disease management. top of page How is the procedure performed? ... position possible that still ensures x-ray image quality. top of page Who interprets the results and ...

  8. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... As a result, bones appear white on the x-ray, soft tissue shows up in shades of gray and air appears black. Until recently, x-ray images were maintained on large film sheets (much ...

  9. Panoramic Dental X-Ray

    Science.gov (United States)

    ... Physician Resources Professions Site Index A-Z Panoramic Dental X-ray Panoramic dental x-ray uses a ... a large photographic negative). Today, most images are digital files that are stored electronically. These stored images ...

  10. Influence of thermal treatment on bentonite used as adsorbent for Cd, Pb, Zn retention from mono-solute and poly-solute aqueous solutions

    Directory of Open Access Journals (Sweden)

    Susana Yamila Martinez Stagnaro

    2012-08-01

    Full Text Available The retentions of Zn, Cd and Pb cations by one treated bentonite up to 750 °C were analyzed. The retentions were evaluated by using mono-and poly-solute aqueous solutions of such cations. The adsorptions were carried out in batch system at room temperature. The solid/liquid ratio was 2% wt.v-1. The solids were characterized by X-ray diffraction, thermal and chemical analyses. The Zn cation from mono- or polysolute-solutions was retained in higher amount than Cd and Pb cations in similar solution types by bentonite. The retentions were effective up to 450 °C calcined bentonite, after that, the retention capacity decreased in concordance with dehydroxylation of the structure of clay minerals.

  11. NIR Spectroscopic Properties of Aqueous Acids Solutions

    Directory of Open Access Journals (Sweden)

    Mohd Zubir MatJafri

    2012-06-01

    Full Text Available Acid content is one of the important quality attributes in determining the maturity index of agricultural product, particularly fruits. Despite the fact that much research on the measurement of acidity in fruits through non-destructive spectroscopy analysis at NIR wavelengths between 700 to 1,000 nm has been conducted, the same response towards individual acids is not well known. This paper presents NIR spectroscopy analysis on aqueous citric, tartaric, malic and oxalic solutions through quantitative analysis by selecting a set of wavelengths that can best be used to measure the pH of the solutions. The aquaphotomics study of the acid solutions has generated R2 above 0.9 for the measurement of all acids. The most important wavelengths for pH are located at 918–925 nm and 990–996 nm, while at 975 nm for water.

  12. Optical manipulation of proteins in aqueous solution

    International Nuclear Information System (INIS)

    Optical trapping of lysozyme, cytochrome c, or myoglobin based on photon pressure generated by focusing 1064 nm laser beam in an aqueous solution was explored. For all the proteins, microparticle formation was observed at the focal point under an optical microscope. Furthermore, the microparticles were identified to the molecular assemblies of the corresponding protein by means of confocal Raman microspectroscopy. For lysozyme, molecular clusters in solution were optically trapped to form the microparticle and it took more than 1 h to produce the microparticle. By contrast, molecular assembling proceeded within 1 min for cytochrome c and myoglobin. Since heme in cytochrome c or myoglobin would have a high polarizability, that would contribute to rapid assembling of the protein. Thus we demonstrated that a focused laser beam was a powerful tool to manipulate protein molecules in solution.

  13. Hunting liquid micro-pockets in snow and ice: Phase transition in salt solutions at the bulk and interface with X-ray photoelectron spectroscopy.

    Science.gov (United States)

    Bartels-Rausch, Thorsten; Orlando, Fabrizio; Kong, Xiangrui; Waldner, Astrid; Artiglia, Luca; Ammann, Markus; Huthwelker, Thomas

    2016-04-01

    Sea salt, and in particular chloride, is an important reactant in the atmosphere. Chloride in air-borne sea salt aerosol is - once chemically converted to a molecular halogen (Cl2, BrCl) and released to the atmosphere - well known as important atmospheric reactant, driving large-scale changes to the atmospheric composition and in particular to ozone levels in remote areas, but also in coastal mega cities. Similar chemistry has been proposed for sea salt deposits in polar snow covers. A crucial factor determining the overall reactivity is the local physical environment of the chloride ion. For example, the reactivity of liquid aerosols decreases significantly upon crystallization. Surprisingly, the phases of NaCl-containing systems are still under debate, partially due to the limited availability of in situ measurements directly probing the local environment at the surface of frozen NaCl-water binary systems. Using core electron spectroscopy of the oxygen atoms in water, we previously showed that these systems follow the phase rules at the air-ice interface. This finding contrasts some earlier observations, where the presence of liquid below the eutectic point of bulk solutions was postulated. In the present study, we present new electron yield near-edge X-ray absorption fine structure spectroscopy (NEXAFS) data obtained at near-ambient pressures up to 20 mbar of NaCl frozen solutions. The method is sensitive to small changes in the local environment of the chlorine atom. The measurements were performed at the PHOENIX beamline at SLS. The study indicates frapant differences in the phases of NaCl - water mixtures at temperatures blow the freezing point for the surface of the ice vs. the bulk. This has significant impact on modelling chemical reactions in snow or ice and it's environmental consequences.

  14. Femtosecond X-Ray Scattering Study of Ultrafast Photoinduced Structural Dynamics in Solvated [Co(terpy)2]2+

    DEFF Research Database (Denmark)

    Biasin, Elisa; Brandt van Driel, Tim; Kjær, Kasper Skov;

    2016-01-01

    We study the structural dynamics of photoexcited [Co(terpy)2]2+ in an aqueous solution with ultrafast x-ray diffuse scattering experiments conducted at the Linac Coherent Light Source. Through direct comparisons with density functional theory calculations, our analysis shows that the...

  15. Aqueous Solution Vessel Thermal Model Development II

    Energy Technology Data Exchange (ETDEWEB)

    Buechler, Cynthia Eileen [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2015-10-28

    The work presented in this report is a continuation of the work described in the May 2015 report, “Aqueous Solution Vessel Thermal Model Development”. This computational fluid dynamics (CFD) model aims to predict the temperature and bubble volume fraction in an aqueous solution of uranium. These values affect the reactivity of the fissile solution, so it is important to be able to calculate them and determine their effects on the reaction. Part A of this report describes some of the parameter comparisons performed on the CFD model using Fluent. Part B describes the coupling of the Fluent model with a Monte-Carlo N-Particle (MCNP) neutron transport model. The fuel tank geometry is the same as it was in the May 2015 report, annular with a thickness-to-height ratio of 0.16. An accelerator-driven neutron source provides the excitation for the reaction, and internal and external water cooling channels remove the heat. The model used in this work incorporates the Eulerian multiphase model with lift, wall lubrication, turbulent dispersion and turbulence interaction. The buoyancy-driven flow is modeled using the Boussinesq approximation, and the flow turbulence is determined using the k-ω Shear-Stress-Transport (SST) model. The dispersed turbulence multiphase model is employed to capture the multiphase turbulence effects.

  16. X-ray Crystallography Facility

    Science.gov (United States)

    2000-01-01

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

  17. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... x-rays. top of page What does the equipment look like? The equipment typically used for bone x-rays consists of ... and joint abnormalities, such as arthritis. X-ray equipment is relatively inexpensive and widely available in emergency ...

  18. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... The x-ray tube is connected to a flexible arm that is extended over the patient while an x-ray film holder or image recording plate is placed beneath the patient. top of page How does the procedure work? X-rays are a form of radiation like ...

  19. Tunable X-ray source

    Science.gov (United States)

    Boyce, James R.

    2011-02-08

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

  20. X-ray selected BALQSOs

    CERN Document Server

    Page, M J; Ceballos, M; Corral, A; Ebrero, J; Esquej, P; Krumpe, M; Mateos, S; Rosen, S; Schwope, A; Streblyanska, A; Symeonidis, M; Tedds, J A; Watson, M G

    2016-01-01

    We study a sample of six X-ray selected broad absorption line (BAL) quasi-stellar objects (QSOs) from the XMM-Newton Wide Angle Survey. All six objects are classified as BALQSOs using the classic balnicity index, and together they form the largest sample of X-ray selected BALQSOs. We find evidence for absorption in the X-ray spectra of all six objects. An ionized absorption model applied to an X-ray spectral shape that would be typical for non-BAL QSOs (a power law with energy index alpha=0.98) provides acceptable fits to the X-ray spectra of all six objects. The optical to X-ray spectral indices, alpha_OX, of the X-ray selected BALQSOs, have a mean value of 1.69 +- 0.05, which is similar to that found for X-ray selected and optically selected non-BAL QSOs of similar ultraviolet luminosity. In contrast, optically-selected BALQSOs typically have much larger alpha_OX and so are characterised as being X-ray weak. The results imply that X-ray selection yields intrinsically X-ray bright BALQSOs, but their X-ray sp...

  1. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... lies. A drawer under the table holds the x-ray film or image recording plate . Sometimes the x-ray ... that is extended over the patient while an x-ray film holder or image recording plate is placed beneath ...

  2. X-Ray Exam: Ankle

    Science.gov (United States)

    ... Tropical Delight: Melon Smoothie Pregnant? Your Baby's Growth X-Ray Exam: Ankle KidsHealth > For Parents > X-Ray Exam: Ankle Print A A A Text Size ... español Radiografía: tobillo What It Is An ankle X-ray is a safe and painless test that uses ...

  3. X-Ray Exam: Finger

    Science.gov (United States)

    ... Tropical Delight: Melon Smoothie Pregnant? Your Baby's Growth X-Ray Exam: Finger KidsHealth > For Parents > X-Ray Exam: Finger Print A A A Text Size ... español Radiografía: dedo What It Is A finger X-ray is a safe and painless test that uses ...

  4. X-Ray Exam: Wrist

    Science.gov (United States)

    ... Tropical Delight: Melon Smoothie Pregnant? Your Baby's Growth X-Ray Exam: Wrist KidsHealth > For Parents > X-Ray Exam: Wrist Print A A A Text Size ... español Radiografía: muñeca What It Is A wrist X-ray is a safe and painless test that uses ...

  5. X-Ray Exam: Hip

    Science.gov (United States)

    ... Tropical Delight: Melon Smoothie Pregnant? Your Baby's Growth X-Ray Exam: Hip KidsHealth > For Parents > X-Ray Exam: Hip Print A A A Text Size ... español Radiografía: cadera What It Is A hip X-ray is a safe and painless test that uses ...

  6. X-Ray Exam: Forearm

    Science.gov (United States)

    ... Tropical Delight: Melon Smoothie Pregnant? Your Baby's Growth X-Ray Exam: Forearm KidsHealth > For Parents > X-Ray Exam: Forearm Print A A A Text Size ... español Radiografía: brazo What It Is A forearm X-ray is a safe and painless test that uses ...

  7. X-Ray Exam: Pelvis

    Science.gov (United States)

    ... Tropical Delight: Melon Smoothie Pregnant? Your Baby's Growth X-Ray Exam: Pelvis KidsHealth > For Parents > X-Ray Exam: Pelvis Print A A A Text Size ... español Radiografía: pelvis What It Is A pelvis X-ray is a safe and painless test that uses ...

  8. X-Ray Exam: Foot

    Science.gov (United States)

    ... Tropical Delight: Melon Smoothie Pregnant? Your Baby's Growth X-Ray Exam: Foot KidsHealth > For Parents > X-Ray Exam: Foot Print A A A Text Size ... español Radiografía: pie What It Is A foot X-ray is a safe and painless test that uses ...

  9. Two step formation of metal aggregates by surface X-ray radiolysis under Langmuir monolayers: 2D followed by 3D growth

    Directory of Open Access Journals (Sweden)

    Smita Mukherjee

    2015-12-01

    Full Text Available In order to form a nanostructured metallic layer below a Langmuir monolayer, radiolysis synthesis was carried out in an adapted geometry that we call surface X-ray radiolysis. In this procedure, an X-ray beam produced by a synchrotron beamline intercepts the surface of an aqueous metal-ion solution covered by a Langmuir monolayer at an angle of incidence below the critical angle for total internal reflection. Underneath the organic layer, the X-ray beam induces the radiolytic synthesis of a nanostructured metal–organic layer whose ultrathin thickness is defined by the vertical X-ray penetration depth. We have shown that increasing the X-ray flux on the surface, which considerably enhances the kinetics of the silver layer formation, results in a second growth regime of silver nanocrystals. Here the formation of the oriented thin layer is followed by the appearance of a 3D powder of silver clusters.

  10. Leaching of lead from zinc leach residue in acidic calcium chloride aqueous solution

    Science.gov (United States)

    Wang, Le; Mu, Wen-ning; Shen, Hong-tao; Liu, Shao-ming; Zhai, Yu-chun

    2015-05-01

    A process with potentially reduced environmental impacts and occupational hazards of lead-bearing zinc plant residue was studied to achieve a higher recovery of lead via a cost-effective and environmentally friendly process. This paper describes an optimization study on the leaching of lead from zinc leach residue using acidic calcium chloride aqueous solution. Six main process conditions, i.e., the solution pH value, stirring rate, concentration of CaCl2 aqueous solution, liquid-to-solid (L/S) ratio, leaching temperature, and leaching time, were investigated. The microstructure and components of the residue and tailing were characterized using scanning electron microscopy (SEM) and X-ray diffraction (XRD). On the basis of experimental results, the optimum reaction conditions were determined to be a solution pH value of 1, a stirring rate of 500 r·min-1, a CaCl2 aqueous solution concentration of 400 g·L-1, a liquid-to-solid mass ratio of 7:1, a leaching temperature of 80°C, and a leaching time of 45 min. The leaching rate of lead under these conditions reached 93.79%, with an iron dissolution rate of 19.28%. Silica did not take part in the chemical reaction during the leaching process and was accumulated in the residue.

  11. X-ray today

    Energy Technology Data Exchange (ETDEWEB)

    Neitzel, U. [Philips Medical Systems, Hamburg (Germany)

    2001-09-01

    The interest attracted by the new imaging modalities tends to overshadow the continuing importance of projection radiography and fluoroscopy. Nevertheless, projection techniques still represent by far the greatest proportion of diagnostic imaging examinations, and play an essential role in the growing number of advanced interventional procedures. This article describes some of the latest developments in X-ray imaging technology, using two products from the Philips range as examples: the Integris Allura cardiovascular system with 3D image reconstruction, and the BV Pulsera: a high-end, multi-functional mobile C-arm system with cardiac capabilities. (orig.)

  12. Pulse Radiolysis of Aqueous Thiocyanate Solution

    International Nuclear Information System (INIS)

    The pulse radiolysis of N2O saturated aqueous solutions of KSCN was studied under neutral pH conditions. The observed optical absorption spectrum of the SCN#lgbullet# radical in solution is more complex than previously reported, but it is in good agreement with that measured in the gas phase. Kinetic traces at 330 nm and 472 nm corresponding to SCN#lgbullet# and (SCN)2#lgbullet#-, respectively, were fit using a Monte Carlo simulation kinetic model. The rate coefficient for the oxidation of SCN- ions by OH radicals, an important reaction used in competition kinetics measurements, was found to be 1.4 ± 0.1 x 1010 M-1 s-1, about 30% higher than the normally accepted value. A detailed discussion of the reaction mechanism is presented

  13. Aqueous Solutions of Ionic Liquids: Microscopic Assembly.

    Science.gov (United States)

    Vicent-Luna, Jose Manuel; Dubbeldam, David; Gómez-Álvarez, Paula; Calero, Sofia

    2016-02-01

    Aqueous solutions of ionic liquids are of special interest, due to the distinctive properties of ionic liquids, in particular, their amphiphilic character. A better understanding of the structure-property relationships of such systems is hence desirable. One of the crucial molecular-level interactions that influences the macroscopic behavior is hydrogen bonding. In this work, we conduct molecular dynamics simulations to investigate the effects of ionic liquids on the hydrogen-bond network of water in dilute aqueous solutions of ionic liquids with various combinations of cations and anions. Calculations are performed for imidazolium-based cations with alkyl chains of different lengths and for a variety of anions, namely, [Br](-), [NO3](-), [SCN](-) [BF4](-), [PF6](-), and [Tf2N](-). The structure of water and the water-ionic liquid interactions involved in the formation of a heterogeneous network are analyzed by using radial distribution functions and hydrogen-bond statistics. To this end, we employ the geometric criterion of the hydrogen-bond definition and it is shown that the structure of water is sensitive to the amount of ionic liquid and to the anion type. In particular, [SCN](-) and [Tf2N](-) were found to be the most hydrophilic and hydrophobic anions, respectively. Conversely, the cation chain length did not influence the results.

  14. Cooperative protein structural dynamics of homodimeric hemoglobin linked to water cluster at subunit interface revealed by time-resolved X-ray solution scattering

    Directory of Open Access Journals (Sweden)

    Jong Goo Kim

    2016-03-01

    Full Text Available Homodimeric hemoglobin (HbI consisting of two subunits is a good model system for investigating the allosteric structural transition as it exhibits cooperativity in ligand binding. In this work, as an effort to extend our previous study on wild-type and F97Y mutant HbI, we investigate structural dynamics of a mutant HbI in solution to examine the role of well-organized interfacial water cluster, which has been known to mediate intersubunit communication in HbI. In the T72V mutant of HbI, the interfacial water cluster in the T state is perturbed due to the lack of Thr72, resulting in two less interfacial water molecules than in wild-type HbI. By performing picosecond time-resolved X-ray solution scattering experiment and kinetic analysis on the T72V mutant, we identify three structurally distinct intermediates (I1, I2, and I3 and show that the kinetics of the T72V mutant are well described by the same kinetic model used for wild-type and F97Y HbI, which involves biphasic kinetics, geminate recombination, and bimolecular CO recombination. The optimized kinetic model shows that the R-T transition and bimolecular CO recombination are faster in the T72V mutant than in the wild type. From structural analysis using species-associated difference scattering curves for the intermediates, we find that the T-like deoxy I3 intermediate in solution has a different structure from deoxy HbI in crystal. In addition, we extract detailed structural parameters of the intermediates such as E-F distance, intersubunit rotation angle, and heme-heme distance. By comparing the structures of protein intermediates in wild-type HbI and the T72V mutant, we reveal how the perturbation in the interfacial water cluster affects the kinetics and structures of reaction intermediates of HbI.

  15. X-ray absorption spectrum for guanosine-5{sup '}-monophosphate in water solution in the vicinity of the nitrogen K-edge observed in free liquid jet in vacuum

    Energy Technology Data Exchange (ETDEWEB)

    Ukai, Masatoshi [Department of Applied Physics, Tokyo University of Agriculture and Technology, Koganei-shi Tokyo 184-8588 (Japan)], E-mail: ukai3@cc.tuat.ac.jp; Yokoya, Akinari [Advanced Science Research Center, Japan Atomic Energy Agency (JAEA), Tokai-mura, Naka-gun, Ibaraki 319-1195 (Japan); Fujii, Kentaro [Advanced Science Research Center, Japan Atomic Energy Agency (JAEA), Tokai-mura, Naka-gun, Ibaraki 319-1195 (Japan); Synchrotron Radiation Research Center, Japan Atomic Energy Agency (JAEA), Sayo-gun, Hyogo 679-5148 (Japan); Saitoh, Yuji [Synchrotron Radiation Research Center, Japan Atomic Energy Agency (JAEA), Sayo-gun, Hyogo 679-5148 (Japan)

    2008-10-15

    A new spectroscopy for direct effect of radiation damage to nucleic acids such as DNA and RNA is underway using a liquid beam sample in vacuum combined with soft-X-ray synchrotron radiation. We show the X-ray absorption spectrum (XANES) of liquid phase water at X-ray photon energy in the vicinity of oxygen K-shell absorption edge obtained from total photoelectron yields ejected from a pure water beam. We confirm a 'liquid sample in vacuum' for the present experiment by the measurements of the temperature dependence of the XANES spectrum for a liquid beam of pure water. Shown is the first measurement of the XANES spectrum for guanosine-5{sup '}-monophosphate (GMP), which is one of the fundamental nucleotide unit for RNA, in water solution at X-ray photon energy in the vicinity of nitrogen K-shell absorption edge involved in the 'water-window' region, which corresponds to a selective excitation of guanine site.

  16. Demonstration of x-ray holography with an x-ray laser

    International Nuclear Information System (INIS)

    X-ray holography offers the potential for obtaining high resolution three-dimensional images of in vitro biological microstructures. Significant progress toward this goal has been achieved with holography systems using synchrotron x-ray sources and recently spatial resolutions as small as 40 nm have been demonstrated. These experiments required x-ray exposures of an hour or longer, which makes high spatial resolution difficult to achieve in live biological specimens because of blurring of the image. This blurring is caused by specimen motion and prohibits the imaging of dynamical processes within the specimen. A possible solution to this problem is to exploit the extremely high brightness and long coherence lengths produced by x-ray lasers and create the hologram with exposure times of less than 1 nsec. This report presents the results from an experiment in which an x-ray laser was used to produce x-ray holograms. The holography geometry used was a Gabor in-line type modified by the inclusion of a high reflectivity multi-layer x-ray mirror used as a narrow bandpass filter

  17. Catalyzed reduction of nitrate in aqueous solutions

    International Nuclear Information System (INIS)

    Sodium nitrate and other nitrate salts in wastes is a major source of difficulty for permanent disposal. Reduction of nitrate using aluminum metal has been demonstrated, but NH3, hydrazine, or organic compounds containing oxygen would be advantageous for reduction of nitrate in sodium nitrate solutions. Objective of this seed money study was to determine minimum conditions for reduction. Proposed procedure was batchwise heating of aqueous solutions in closed vessels with monitoring of temperatures and pressures. A simple, convenient apparatus and procedure were demonstrated for observing formation of gaseous products and collecting samples for analyses. The test conditions were 250 degree C and 1000 psi max. Any useful reduction of sodium nitrate to sodium hydroxide as the primary product was not found. The nitrate present at pHs 3 or NH4NO3 is easily decomposed, and the effect of nitromethane at these low pHs was confirmed. When acetic acid or formic acid was added, 21 to 56% of the nitrate in sodium nitrate solutions was reduced by methanol or formaldehyde. With hydrazine and acetic acid, 73 % of the nitrate was decomposed to convert NaNO3 to sodium acetate. With hydrazine and formic acid, 36% of the nitrate was decomposed. If these products are more acceptable for final disposal than sodium nitrate, the reagents are cheap and the conversion conditions would be practical for easy use. Ammonium acetate or formate salts did not significantly reduce nitrate in sodium nitrate solutions

  18. Biomimetic synthesis of CdS nanocrystals in aqueous solution of pepsin

    Energy Technology Data Exchange (ETDEWEB)

    Yang Lin [College of Chemistry and Environmental Science, Henan Normal University, Xinxiang 453007 (China)]. E-mail: yanglin1819@163.com; Shen Qingming [College of Chemistry and Environmental Science, Henan Normal University, Xinxiang 453007 (China)]. E-mail: qingming8@hotmail.com; Zhou Jianguo [College of Chemistry and Environmental Science, Henan Normal University, Xinxiang 453007 (China); Jiang Kai [College of Chemistry and Environmental Science, Henan Normal University, Xinxiang 453007 (China)

    2006-07-01

    CdS nanocrystals with an average width of about 6 nm and narrow size distribution were synthesized in aqueous solution of pepsin at room temperature. The obtained CdS nanocrystals were characterized by transmission electron microscopy (TEM), X-ray powder diffraction (XRD) and thermogravimetric analysis (TGA). The quantum-confined effect of the CdS nanocrystals is confirmed by the ultraviolet-visible (UV-vis) and photoluminescence (PL) spectrum. The results indicate that the pepsin not only induce the nucleation, but inhibit the further growth of CdS nanocrystals. The effect of Cd{sup 2+} on pepsin and the change of pepsin conformation were studied through Fourier transform infrared (FTIR) spectroscopy. The possible mechanism of CdS nanocrystals growth in the pepsin solution was also discussed.

  19. Glass-to-cryogenic-liquid transitions in aqueous solutions suggested by crack healing.

    Science.gov (United States)

    Kim, Chae Un; Tate, Mark W; Gruner, Sol M

    2015-09-22

    Observation of theorized glass-to-liquid transitions between low-density amorphous (LDA) and high-density amorphous (HDA) water states had been stymied by rapid crystallization below the homogeneous water nucleation temperature (∼235 K at 0.1 MPa). We report optical and X-ray observations suggestive of glass-to-liquid transitions in these states. Crack healing, indicative of liquid, occurs when LDA ice transforms to cubic ice at 160 K, and when HDA ice transforms to the LDA state at temperatures as low as 120 K. X-ray diffraction study of the HDA to LDA transition clearly shows the characteristics of a first-order transition. Study of the glass-to-liquid transitions in nanoconfined aqueous solutions shows them to be independent of the solute concentrations, suggesting that they represent an intrinsic property of water. These findings support theories that LDA and HDA ice are thermodynamically distinct and that they are continuously connected to two different liquid states of water. PMID:26351671

  20. Functionalized polymers for binding to solutes in aqueous solutions

    Science.gov (United States)

    Smith, Barbara F.; Robison, Thomas W.

    2006-11-21

    A functionalized polymer for binding a dissolved molecule in an aqueous solution is presented. The polymer has a backbone polymer to which one or more functional groups are covalently linked. The backbone polymer can be such polymers as polyethylenimine, polyvinylamine, polyallylamine, and polypropylamine. These polymers are generally water-soluble, but can be insoluble when cross-linked. The functional group can be for example diol derivatives, polyol derivatives, thiol and dithiol derivatives, guest-host groups, affinity groups, beta-diphosphonic acids, and beta-diamides

  1. Monochromatic X-Ray Induced Novel Synthesis of Plasmonic Nanostructure for Photovoltaic Application

    Science.gov (United States)

    Bharti, Amardeep; Bhardwaj, Richa; Agrawal, Ashish K.; Goyal, Navdeep; Gautam, Sanjeev

    2016-04-01

    It has been universally delineated that the plasmonic metal nanoparticles can enhance the efficiency of photovoltaic cell by increasing the probability of energetic solar photons capturing phenomena using localized surface plasmonic resonance response. In this paper, we developed a novel in-situ simple approach to synthesize noble plasmonic silver nanoparticles (AgNP) from aqueous poly-vinyl-pyrrolidone solution of metal salt using radiolysis of water via synchrotron monochromatic X-ray irradiation without any chemical reducing agent. X-ray irradiation of water produces hydrated electrons , superoxide and atom radicals , which triggers the reaction and reduces metal salt. X-ray radiolysis based synthesis provides the control over the reaction and prevent the formation of secondary products as occurs in case of chemical reduction route. In the previous studies, synchrotron “white” X-rays had been examined for the synthesis of metal nanoparticles, but that technique limits only upto the material synthesis while in this work we explored the role of “monochromatic” X-rays for the production of bulk amount of nanoparticles which would also provide the feasibility of in-situ characterization. Transmission electron micrographs show that the synthesized AgNP appears spherical with diameter of 2–6 nm and is in agreement with the size estimation from uv-vis spectra by “Mie theory”.

  2. Monochromatic X-Ray Induced Novel Synthesis of Plasmonic Nanostructure for Photovoltaic Application.

    Science.gov (United States)

    Bharti, Amardeep; Bhardwaj, Richa; Agrawal, Ashish K; Goyal, Navdeep; Gautam, Sanjeev

    2016-01-01

    It has been universally delineated that the plasmonic metal nanoparticles can enhance the efficiency of photovoltaic cell by increasing the probability of energetic solar photons capturing phenomena using localized surface plasmonic resonance response. In this paper, we developed a novel in-situ simple approach to synthesize noble plasmonic silver nanoparticles (AgNP) from aqueous poly-vinyl-pyrrolidone solution of metal salt using radiolysis of water via synchrotron monochromatic X-ray irradiation without any chemical reducing agent. X-ray irradiation of water produces hydrated electrons (e(-)aq), superoxide (O(-)2) and atom radicals H*, which triggers the reaction and reduces metal salt. X-ray radiolysis based synthesis provides the control over the reaction and prevent the formation of secondary products as occurs in case of chemical reduction route. In the previous studies, synchrotron "white" X-rays had been examined for the synthesis of metal nanoparticles, but that technique limits only upto the material synthesis while in this work we explored the role of "monochromatic" X-rays for the production of bulk amount of nanoparticles which would also provide the feasibility of in-situ characterization. Transmission electron micrographs show that the synthesized AgNP appears spherical with diameter of 2-6 nm and is in agreement with the size estimation from uv-vis spectra by "Mie theory". PMID:27094793

  3. Preparation and characterization of regenerated fiber from the aqueous solution of Bombyx mori cocoon silk fibroin

    Energy Technology Data Exchange (ETDEWEB)

    Zhu Zhenghua [Department of Biotechnology, Tokyo University of Agriculture and Technology, Koganei, Tokyo 184-8588 (Japan); Department of Application Engineering, ZheJiang Vocational College of Economic and Trade, HangZhou, ZheJiang 310018 (China); Imada, Takuzo [Department of Biotechnology, Tokyo University of Agriculture and Technology, Koganei, Tokyo 184-8588 (Japan); Asakura, Tetsuo, E-mail: asakura@cc.tuat.ac.jp [Department of Biotechnology, Tokyo University of Agriculture and Technology, Koganei, Tokyo 184-8588 (Japan)

    2009-10-15

    The regenerated silk fibers with high strength and high biodegradability were prepared from the aqueous solution of Bombyx mori silk fibroin from cocoons with wet spinning method. Although the tensile strength of the regenerated silk fibroin fiber, 210 MPa is still half of the strength of native silk fiber, the diameter of the fiber is about 100 {mu}m which is suitable for monofilament of suture together with high biodegradability. The high concentration (30%, w/v) of the aqueous solution of the silk fibroin which corresponds to the high concentration in the middle silkgland of silkworm was obtained. This was performed by adjusting the pH of the aqueous solution to 10.4 which corresponds to pK{sub a} value of the OH group of Tyr residues in the silk fibroin. The mixed solvent, methanol/acetic acid (7:3 in volume ratio) was used as coagulant solvent for preparing the regenerated fiber. The structural change of silk fibroin fiber by stretching was monitored with both {sup 13}C solid state NMR and X-ray diffraction methods, indicating that the high strength of the fiber is related with the long-range orientation of the silk fibroin chain with {beta}-sheet structure.

  4. Transparent conducting oxide films of group V doped titania prepared by aqueous chemical solution deposition

    Energy Technology Data Exchange (ETDEWEB)

    Elen, Ken [Inorganic and Physical Chemistry, Institute for Materials Research, Hasselt University, Agoralaan Building D, B-3590 Diepenbeek (Belgium); IMEC vzw division IMOMEC, Agoralaan Building D, B-3590 Diepenbeek (Belgium); Strategisch Initiatief Materialen (SIM), SoPPoM Program (Belgium); Capon, Boris [Strategisch Initiatief Materialen (SIM), SoPPoM Programm (Belgium); Coating and Contacting of Nanostructures, Ghent University, Krijgslaan 281 S1, B-9000 Ghent (Belgium); De Dobbelaere, Christopher [Inorganic and Physical Chemistry, Institute for Materials Research, Hasselt University, Agoralaan Building D, B-3590 Diepenbeek (Belgium); Dewulf, Daan [Inorganic and Physical Chemistry, Institute for Materials Research, Hasselt University, Agoralaan Building D, B-3590 Diepenbeek (Belgium); IMEC vzw division IMOMEC, Agoralaan Building D, B-3590 Diepenbeek (Belgium); Peys, Nick [Inorganic and Physical Chemistry, Institute for Materials Research, Hasselt University, Agoralaan Building D, B-3590 Diepenbeek (Belgium); IMEC vzw, Kapeldreef 75, B-3001 Heverlee (Belgium); Detavernier, Christophe [Coating and Contacting of Nanostructures, Ghent University, Krijgslaan 281 S1, B-9000 Ghent (Belgium); Hardy, An [Inorganic and Physical Chemistry, Institute for Materials Research, Hasselt University, Agoralaan Building D, B-3590 Diepenbeek (Belgium); IMEC vzw division IMOMEC, Agoralaan Building D, B-3590 Diepenbeek (Belgium); Van Bael, Marlies K., E-mail: marlies.vanbael@uhasselt.be [Inorganic and Physical Chemistry, Institute for Materials Research, Hasselt University, Agoralaan Building D, B-3590 Diepenbeek (Belgium); IMEC vzw division IMOMEC, Agoralaan Building D, B-3590 Diepenbeek (Belgium)

    2014-03-31

    Transparent conducting oxide (TCO) films of titania doped with vanadium (V), niobium (Nb) and tantalum (Ta) are obtained by aqueous Chemical Solution Deposition (CSD). The effect of the dopant on the crystallization and microstructure of the resulting films is examined by means of X-ray diffraction and electron microscopy. During annealing of the thin films, in-situ characterization of the crystal structure and sheet resistance is carried out. Niobium doped anatase films, obtained after annealing in forming gas, show a resistivity of 0,28 Ohm cm, which is the lowest resistivity reported for a solution deposited anatase-based TCO so far. Here, we demonstrate that aqueous CSD may provide a strategy for scalable TCO production in the future. - Highlights: • Aqueous chemical solution deposition of doped titanium dioxide • Doping delays the phase transition from anatase to rutile • Lowest resistivity after doping with niobium and annealing in Forming Gas • Transparency higher than 80% in the visible range of optical spectrum.

  5. Transparent conducting oxide films of group V doped titania prepared by aqueous chemical solution deposition

    International Nuclear Information System (INIS)

    Transparent conducting oxide (TCO) films of titania doped with vanadium (V), niobium (Nb) and tantalum (Ta) are obtained by aqueous Chemical Solution Deposition (CSD). The effect of the dopant on the crystallization and microstructure of the resulting films is examined by means of X-ray diffraction and electron microscopy. During annealing of the thin films, in-situ characterization of the crystal structure and sheet resistance is carried out. Niobium doped anatase films, obtained after annealing in forming gas, show a resistivity of 0,28 Ohm cm, which is the lowest resistivity reported for a solution deposited anatase-based TCO so far. Here, we demonstrate that aqueous CSD may provide a strategy for scalable TCO production in the future. - Highlights: • Aqueous chemical solution deposition of doped titanium dioxide • Doping delays the phase transition from anatase to rutile • Lowest resistivity after doping with niobium and annealing in Forming Gas • Transparency higher than 80% in the visible range of optical spectrum

  6. Tantalum/Copper X-Ray Targets

    Science.gov (United States)

    Waters, William J.; Edmonds, Brian

    1993-01-01

    Lewis Research Center developed unique solution to subsidiary problem of fabrication of x-ray target. Plasma spraying enabled fabrication of lightweight, high-performance targets. Power settings, atmosphere-control settings, rate of deposition, and other spraying parameters developed. Thin coats of tantalum successfully deposited on copper targets. Targets performed successfully in tests and satisfied all criteria expressed in terms of critical parameters. Significantly reduces projected costs of fabrication of targets and contributes to development of improved, long-lived, lightweight x-ray system.

  7. Bioactive and Antibacterial Glass Powders Doped with Copper by Ion-Exchange in Aqueous Solutions

    Directory of Open Access Journals (Sweden)

    Marta Miola

    2016-05-01

    Full Text Available In this work, two bioactive glass powders (SBA2 and SBA3 were doped with Cu by means of the ion-exchange technique in aqueous solution. SBA2 glass was subjected to the ion-exchange process by using different Cu salts (copper(II nitrate, chloride, acetate, and sulphate and concentrations. Structural (X-ray diffraction-XRD, morphological (Scanning Electron Microscopy-SEM, and compositional (Energy Dispersion Spectrometry-EDS analyses evidenced the formation of crystalline phases for glasses ion-exchanged in copper(II nitrate and chloride solutions; while the ion-exchange in copper(II acetate solutions lead to the incorporation of higher Cu amount than the ion-exchange in copper(II sulphate solutions. For this reason, the antibacterial test (inhibition halo towards S. aureus was performed on SBA2 powders ion-exchanged in copper(II acetate solutions and evidenced a limited antibacterial effect. A second glass composition (SBA3 was developed to allow a greater incorporation of Cu in the glass surface; SBA3 powders were ion-exchanged in copper(II acetate solutions (0.01 M and 0.05 M. Cu-doped SBA3 powders showed an amorphous structure; morphological analysis evidenced a rougher surface for Cu-doped powders in comparison to the undoped glass. EDS and X-ray photoelectron spectroscopy (XPS confirmed the Cu introduction as Cu(II ions. Bioactivity test in simulated body fluid (SBF showed that Cu introduction did not alter the bioactive behaviour of the glass. Finally, inhibition halo test towards S. aureus evidenced a good antimicrobial effect for glass powders ion-exchanged in copper(II acetate solutions 0.05 M.

  8. Topological X-Rays Revisited

    Science.gov (United States)

    Lynch, Mark

    2012-01-01

    We continue our study of topological X-rays begun in Lynch ["Topological X-rays and MRI's," iJMEST 33(3) (2002), pp. 389-392]. We modify our definition of a topological magnetic resonance imaging and give an affirmative answer to the question posed there: Can we identify a closed set in a box by defining X-rays to probe the interior and without…

  9. X-ray instrumentation for SR beamlines

    CERN Document Server

    Kovalchuk, M V; Zheludeva, S I; Aleshko-Ozhevsky, O P; Arutynyan, E H; Kheiker, D M; Kreines, A Y; Lider, V V; Pashaev, E M; Shilina, N Y; Shishkov, V A

    2000-01-01

    The main possibilities and parameters of experimental X-ray stations are presented: 'Protein crystallography', 'X-ray structure analysis', 'High-precision X-ray optics', 'X-ray crystallography and material science', 'X-ray topography', 'Photoelectron X-ray standing wave' that are being installed at Kurchatov SR source by A.V. Shubnikov Institute of Crystallography.

  10. Functionalization of Multiwalled Carbon Nanotubes by Solution Plasma Processing in Ammonia Aqueous Solution and Preparation of Composite Material with Polyamide 6

    Science.gov (United States)

    Shirafuji, Tatsuru; Noguchi, Yohei; Yamamoto, Taibou; Hieda, Junko; Saito, Nagahiro; Takai, Osamu; Tsuchimoto, Akiharu; Nojima, Kazuhiro; Okabe, Youji

    2013-12-01

    Solution plasma processing (SPP) has been performed on multiwalled carbon nanotubes (MWCNTs) in ammonia aqueous solution. The MWCNTs, which do not disperse in aqueous solution, uniformly dispersed after the SPP. Only 2 h was required to obtain 10 g of the dispersed MWCNTs, while 7 days and additional chemicals were required for 185 mg in a previous study. The X-ray photoelectron spectroscopy and Fourier-transform infrared spectroscopy of the SPP-treated MWCNTs revealed that nitrogen- and oxygen-containing groups are formed on the MWCNTs. Serious damage to the MWCNT structure was not observed in the Raman spectrum or transmission electron microscopy images of the SPP-treated MWCNTs. The composite materials prepared using polyamide 6 with the SPP-treated MWCNTs showed better tensile, bending, and impact strength than those prepared with nontreated MWCNTs.

  11. X-ray lithography sources

    International Nuclear Information System (INIS)

    Synchrotron from dipole magnets in electron storage rings has emerged as a useful source of x-rays for lithography. To meet the need for these sources numerous groups around the world have embarked on projects to design and construct storage rings for x-ray lithography. Both conventional electromagnets as well as superconducting (SC) dipoles have been incorporated into the various designs. An overview of the worldwide effort to produce commercial x-ray sources will be presented. To better illustrate the elements involved in these sources a closer examination of the Superconducting X-ray Lithography Source Project (SXLS) at BNL will be presented. 11 refs., 1 fig., 5 tabs

  12. Soft X-ray optics

    CERN Document Server

    Spiller, Eberhard A

    1993-01-01

    This text describes optics mainly in the 10 to 500 angstrom wavelength region. These wavelengths are 50 to 100 times shorter than those for visible light and 50 to 100 times longer than the wavelengths of medical x rays or x-ray diffraction from natural crystals. There have been substantial advances during the last 20 years, which one can see as an extension of optical technology to shorter wavelengths or as an extension of x-ray diffraction to longer wavelengths. Artificial diffracting structures like zone plates and multilayer mirrors are replacing the natural crystals of x-ray diffraction.

  13. X-ray Absorption Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Yano, Junko; Yachandra, Vittal K.

    2009-07-09

    This review gives a brief description of the theory and application of X-ray absorption spectroscopy, both X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS), especially, pertaining to photosynthesis. The advantages and limitations of the methods are discussed. Recent advances in extended EXAFS and polarized EXAFS using oriented membranes and single crystals are explained. Developments in theory in understanding the XANES spectra are described. The application of X-ray absorption spectroscopy to the study of the Mn4Ca cluster in Photosystem II is presented.

  14. X-ray Fluorescence Sectioning

    CERN Document Server

    Cong, Wenxiang

    2012-01-01

    In this paper, we propose an x-ray fluorescence imaging system for elemental analysis. The key idea is what we call "x-ray fluorescence sectioning". Specifically, a slit collimator in front of an x-ray tube is used to shape x-rays into a fan-beam to illuminate a planar section of an object. Then, relevant elements such as gold nanoparticles on the fan-beam plane are excited to generate x-ray fluorescence signals. One or more 2D spectral detectors are placed to face the fan-beam plane and directly measure x-ray fluorescence data. Detector elements are so collimated that each element only sees a unique area element on the fan-beam plane and records the x-ray fluorescence signal accordingly. The measured 2D x-ray fluorescence data can be refined in reference to the attenuation characteristics of the object and the divergence of the beam for accurate elemental mapping. This x-ray fluorescence sectioning system promises fast fluorescence tomographic imaging without a complex inverse procedure. The design can be ad...

  15. Characteristics and mechanisms of Ni(Ⅱ) removal from aqueous solution by Chinese loess

    Institute of Scientific and Technical Information of China (English)

    王艳; 唐晓武; 王恒宇

    2015-01-01

    Nickel is a toxic heavy metal among trace elements which has a detrimental impact on living organisms. There is growing need of finding an economic and effective solution for Ni(Ⅱ) immobilization in environments. Chinese loess was selected as adsorbent to remove Ni(Ⅱ) from aqueous solution. Adsorbent dosage, reaction time, solute concentration, temperature, and solution p H also have influences on efficiency of Ni(Ⅱ) removal. The monolayer adsorption capacity of loess towards Ni(Ⅱ) is determined to be about 15.61 mg/g. High temperature and p H favor the removal of Ni(Ⅱ) using Chinese loess soil and the optimal dosage of loess is determined to be 10 g/L. The kinetics and adsorption isotherms of the adsorption process can be best-fitted with the pseudo second order kinetics and Langmuir isothermal model, respectively. The thermodynamic analysis reveals that the adsorption process is spontaneous, endothermic and the system disorder increases with duration. Nickel ions can be removed with the removal efficiency of 98.5% at p H greater than or equal to 9.7. Further studies on loess and Ni(Ⅱ) laden loess(using X-Ray diffraction, Fourier transform infrared spectroscopy) and Ni(Ⅱ) species distribution at various p H have been conducted to discuss the adsorption mechanism. Loess soils in China have proven to be a potential adsorbent for Ni(Ⅱ) removal from aqueous solutions.

  16. Characteristics and mechanisms of Ni(II) removal from aqueous solution by Chinese loess

    Institute of Scientific and Technical Information of China (English)

    王艳; 唐晓武; 王恒宇

    2015-01-01

    Nickel is a toxic heavy metal among trace elements which has a detrimental impact on living organisms. There is growing need of finding an economic and effective solution for Ni(II) immobilization in environments. Chinese loess was selected as adsorbent to remove Ni(II) from aqueous solution. Adsorbent dosage, reaction time, solute concentration, temperature, and solution pH also have influences on efficiency of Ni(II) removal. The monolayer adsorption capacity of loess towards Ni(II) is determined to be about 15.61 mg/g. High temperature and pH favor the removal of Ni(II) using Chinese loess soil and the optimal dosage of loess is determined to be 10 g/L. The kinetics and adsorption isotherms of the adsorption process can be best-fitted with the pseudo second order kinetics and Langmuir isothermal model, respectively. The thermodynamic analysis reveals that the adsorption process is spontaneous, endothermic and the system disorder increases with duration. Nickel ions can be removed with the removal efficiency of 98.5% at pH greater than or equal to 9.7. Further studies on loess and Ni(II) laden loess (using X-Ray diffraction, Fourier transform infrared spectroscopy) and Ni(II) species distribution at various pH have been conducted to discuss the adsorption mechanism. Loess soils in China have proven to be a potential adsorbent for Ni(II) removal from aqueous solutions.

  17. X-Ray Attenuation Cell

    Energy Technology Data Exchange (ETDEWEB)

    Ryutov, D.; Toor, A.

    2000-03-03

    To minimize the pulse-to-pulse variation, the LCLS FEL must operate at saturation, i.e. 10 orders of magnitude brighter spectral brilliance than 3rd-generation light sources. At this intensity, ultra-high vacuums and windowless transport are required. Many of the experiments, however, will need to be conducted at a much lower intensity thereby requiring a reliable means to reduce the x-ray intensity by many orders of magnitude without increasing the pulse-to-pulse variation. In this report we consider a possible solution for controlled attenuation of the LCLS x-ray radiation. We suggest using for this purpose a windowless gas-filled cell with the differential pumping. Although this scheme is easily realizable in principle, it has to be demonstrated that the attenuator can be made short enough to be practical and that the gas loads delivered to the vacuum line of sight (LOS) are acceptable. We are not going to present a final, optimized design. Instead, we will provide a preliminary analysis showing that the whole concept is robust and is worth further study. The spatial structure of the LCLS x-ray pulse at the location of the attenuator is shown in Fig. 1. The central high-intensity component, due to the FEL, has a FWHM of {approx}100 {micro}m. A second component, due to the undulator's broad band spontaneous radiation is seen as a much lower intensity ''halo'' with a FWHM of 1 mm. We discuss two versions of the attenuation cell. The first is directed towards a controlled attenuation of the FEL up to the 4 orders of magnitude in the intensity, with the spontaneous radiation halo being eliminated by collimators. In the second version, the spontaneous radiation is not sacrificed but the FEL component (as well as the first harmonic of the spontaneous radiation) gets attenuated by a more modest factor up to 100. We will make all the estimates assuming that the gas used in the attenuator is Xenon and that the energy of the FEL is 8.25 keV. At

  18. Influence of interstitial solutions (H, N) on cerium electronic state in Ce-Fe intermetallic compounds: X-ray Absorption Spectroscopy (XAS) study

    International Nuclear Information System (INIS)

    It is presented an x-ray absorption spectroscopy (XAS) investigation performed at the L-edges of the rare-earth and at the K-edge of iron in the R-Fe intermetallic compounds (La, Ce)2Fe14BHχand Ce2Fe17(H,N)χ, to elucidate the role of the interstitial doping into the electronic and magnetic properties of these systems. Comparison with x-ray circular magnetic dichroism (XCMD) experiments has been carried out to clarify the localization of 4f magnetic moment at the Ce sites upon hydriding. Both XAS and XCMD results evidence the interplay between the structural and magnetic changes, that are associated to the modification of the hybridization between the Fe(3d) and Ce(5d) bands

  19. Combined operando X-ray diffraction–electrochemical impedance spectroscopy detecting solid solution reactions of LiFePO4 in batteries

    OpenAIRE

    Hess, Michael; Sasaki, Tsuyoshi; Villevieille, Claire; Novák, Petr

    2015-01-01

    Lithium-ion batteries are widely used for portable applications today; however, often suffer from limited recharge rates. One reason for such limitation can be a reduced active surface area during phase separation. Here we report a technique combining high-resolution operando synchrotron X-ray diffraction coupled with electrochemical impedance spectroscopy to directly track non-equilibrium intermediate phases in lithium-ion battery materials. LiFePO4, for example, is known to undergo phase se...

  20. Phase Changes of Monosulfoaluminate in NaCl Aqueous Solution

    Directory of Open Access Journals (Sweden)

    Seyoon Yoon

    2016-05-01

    Full Text Available Monosulfoaluminate (Ca4Al2(SO4(OH12∙6H2O plays an important role in anion binding in Portland cement by exchanging its original interlayer ions (SO42− and OH− with chloride ions. In this study, scanning transmission X-ray microscope (STXM, X-ray absorption near edge structure (XANES spectroscopy, and X-ray diffraction (XRD were used to investigate the phase change of monosulfoaluminate due to its interaction with chloride ions. Pure monosulfoaluminate was synthesized and its powder samples were suspended in 0, 0.1, 1, 3, and 5 M NaCl solutions for seven days. At low chloride concentrations, a partial dissolution of monosulfoaluminate formed ettringite, while, with increasing chloride content, the dissolution process was suppressed. As the NaCl concentration increased, the dominant mechanism of the phase change became ion exchange, resulting in direct phase transformation from monosulfoaluminate to Kuzel’s salt or Friedel’s salt. The phase assemblages of the NaCl-reacted samples were explored using thermodynamic calculations and least-square linear combination (LC fitting of measured XANES spectra. A comprehensive description of the phase change and its dominant mechanism are discussed.

  1. Non-abelian dark matter solutions for Galactic gamma-ray excess and Perseus 3.5 keV X-ray line

    Energy Technology Data Exchange (ETDEWEB)

    Cheung, Kingman [Department of Physics, National Tsing Hua University,Hsinchu 300, Taiwan (China); Division of Quantum Phases and Devices, School of Physics, Konkuk University,Seoul 143-701 (Korea, Republic of); Physics Division, National Center for Theoretical Sciences,Hsinchu, Taiwan (China); Huang, Wei-Chih [Department of Physics and Astronomy, University College London,London (United Kingdom); Tsai, Yue-Lin Sming [Kavli IPMU (WPI), The University of Tokyo,Kashiwa, Chiba 277-8583 (Japan)

    2015-05-26

    We attempt to explain simultaneously the Galactic center gamma-ray excess and the 3.5 keV X-ray line from the Perseus cluster based on a class of non-abelian SU(2) DM models, in which the dark matter and an excited state comprise a “dark” SU(2) doublet. The non-abelian group kinetically mixes with the standard model gauge group via dimensions-5 operators. The dark matter particles annihilate into standard model fermions, followed by fragmentation and bremsstrahlung, and thus producing a continuous spectrum of gamma-rays. On the other hand, the dark matter particles can annihilate into a pair of excited states, each of which decays back into the dark matter particle and an X-ray photon, which has an energy equal to the mass difference between the dark matter and the excited state, which is set to be 3.5 keV. The large hierarchy between the required X-ray and γ-ray annihilation cross-sections can be achieved by a very small kinetic mixing between the SM and dark sector, which effectively suppresses the annihilation into the standard model fermions but not into the excited state.

  2. Non-abelian Dark Matter Solutions for Galactic Gamma-ray Excess and Perseus 3.5 keV X-ray Line

    CERN Document Server

    Cheung, Kingman; Tsai, Yue-Lin Sming

    2014-01-01

    We attempt to explain simultaneously the Galactic center gamma-ray excess and the 3.5 keV X-ray line from the Perseus cluster based on a class of non-abelian $SU(2)$ DM models, in which the dark matter and an excited state comprise a "dark" $SU(2)$ doublet. The non-abelian group kinetically mixes with the standard model gauge group via dimensions-5 operators. The dark matter particles annihilate into standard model fermions, followed by fragmentation and bremsstrahlung, and thus producing a continuous spectrum of gamma-rays. On the other hand, the dark matter particles can annihilate into a pair of excited states, each of which decays back into the dark matter particle and an X-ray photon, which has an energy equal to the mass difference between the dark matter and the excited state, which is set to be 3.5 keV. The large hierarchy between the required X-ray and $\\gamma$-ray annihilation cross-sections can be achieved by a very small kinetic mixing between the SM and dark sector, which effectively suppresses t...

  3. The UV/optical lags in NGC 5548: It's not disc reprocessing and the soft X-ray excess is part of the solution

    CERN Document Server

    Gardner, Emma

    2016-01-01

    The new multi-wavelength monitoring campaign on NGC 5548 shows clearly that the variability of the UV/optical lightcurves lags by progressively longer times at longer wavelengths, as expected from reprocessing on optically thick material, but that the timescales are longer than for a standard Shakura-Sunyaev accretion disc. We build a full spectral-timing reprocessing model to simulate the UV/optical lightcurves of NGC 5548. We show that disc reprocessing of the hard X-ray lightcurve produces optical lightcurves with too much fast variability and the wrong lag time. Instead the data are consistent with reprocessing of the far UV (FUV) lightcurve. This requires an intervening structure preventing the hard X-rays from illuminating the disc. We propose this is the disc itself, due to UV line-pressure lifting the photosphere and increasing the scale-height. This UV-emitting region is less dense, so less able to thermalise, making low temperature Comptonised emission as required to produce the soft X-ray excess. H...

  4. Non-abelian dark matter solutions for Galactic gamma-ray excess and Perseus 3.5 keV X-ray line

    International Nuclear Information System (INIS)

    We attempt to explain simultaneously the Galactic center gamma-ray excess and the 3.5 keV X-ray line from the Perseus cluster based on a class of non-abelian SU(2) DM models, in which the dark matter and an excited state comprise a “dark” SU(2) doublet. The non-abelian group kinetically mixes with the standard model gauge group via dimensions-5 operators. The dark matter particles annihilate into standard model fermions, followed by fragmentation and bremsstrahlung, and thus producing a continuous spectrum of gamma-rays. On the other hand, the dark matter particles can annihilate into a pair of excited states, each of which decays back into the dark matter particle and an X-ray photon, which has an energy equal to the mass difference between the dark matter and the excited state, which is set to be 3.5 keV. The large hierarchy between the required X-ray and γ-ray annihilation cross-sections can be achieved by a very small kinetic mixing between the SM and dark sector, which effectively suppresses the annihilation into the standard model fermions but not into the excited state

  5. Radioisotope x-ray analysis

    International Nuclear Information System (INIS)

    Radioisotope x-ray fluorescence and x-ray preferential absorption (XRA) techniques are used extensively for the analysis of materials, covering such diverse applications as analysis of alloys, coal, environmental samples, paper, waste materials, and metalliferous mineral ores and products. Many of these analyses are undertaken in the harsh environment of industrial plants and in the field. Some are continuous on-line analyses of material being processed in industry, where instantaneous analysis information is required for the control of rapidly changing processes. Radioisotope x-ray analysis systems are often tailored to a specific but limited range of applications. They are simpler and often considerably less expensive than analysis systems based on x-ray tubes. These systems are preferred to x-ray tube techniques when simplicity, ruggedness, reliability, and cost of equipment are important; when minimum size, weight, and power consumption are necessary; when a very constant and predictable x-ray output is required; when the use of high-energy x-rays is advantageous; and when short x-ray path lengths are required to minimize the absorption of low-energy x-rays in air. This chapter reviews radioisotope XRF, preferential absorption, and scattering techniques. Some of the basic analysis equations are given. The characteristics of radioisotope sources and x-ray detectors are described, and then the x-ray analytical techniques are presented. The choice of radioisotope technique for a specific application is discussed. This is followed by a summary of applications of these techniques, with a more detailed account given of some of the applications, particularly those of considerable industrial importance. 79 refs., 28 figs., 7 tabs

  6. Biosorption of Fe(II) and Mn(II) Ions from Aqueous Solution by Rice Husk Ash

    OpenAIRE

    Ying Zhang; Jiaying Zhao; Zhao Jiang; Dexin Shan; Yan Lu

    2014-01-01

    Rice husk ash (RHA), an agricultural waste, was used as biosorbent for the removal of Iron(II) and Manganese(II) ions from aqueous solutions. The structural and morphological characteristics of RHA and its elemental compositions before and after adsorption of Fe(II) and Mn(II) were determined by scanning electron microscopic (SEM) and X-ray fluorescence (XRF) analyses. Batch experiments were carried out to determine the influence of initial pH, contact time, adsorbent dosage, and initial conc...

  7. Preparation and characterization of iron-copper binary oxide and its effective removal of antimony(III) from aqueous solution.

    Science.gov (United States)

    Li, Yongchao; Geng, Bing; Hu, Xiaoxian; Ren, Bozhi; Hursthouse, Andrew S

    2016-01-01

    An Fe-Cu binary oxide was fabricated through a simple co-precipitation process, and was used to remove Sb(III) from aqueous solution. X-ray diffraction, scanning electron microscopy, energy dispersive X-ray and N2 adsorption-desorption measurements demonstrated that the Fe-Cu binary oxide consisted of poorly ordered ferrihydrite and CuO, and its specific surface area was higher than both iron oxide and copper oxide. A comparative test indicated that Fe/Cu molar ratio of prepared binary oxide greatly influenced Sb(III) removal and the optimum Fe/Cu molar ratio was about 3/1. Moreover, a maximum adsorption capacity of 209.23 mg Sb(III)/g Fe-Cu binary oxide at pH 5.0 was obtained. The removal of Sb(III) by Fe-Cu binary oxide followed the Freundlich adsorption isotherm and the pseudo-second-order kinetics in the batch study. The removal of Sb(III) was not sensitive to solution pH. In addition, the release of Fe and Cu ions to water was very low when the pH was greater than 6.0. X-ray photoelectron spectroscopy analysis confirmed that the Sb(III) adsorbed on the surface was not oxidized to Sb(V). PMID:27438244

  8. Removal of Cr3+ from aqueous solution by biosorption with aerobic granules

    International Nuclear Information System (INIS)

    Aerobic granules were utilized as an effective biosorbent to remove Cr3+ from aqueous solution. The results showed that the initial pH, contact time, and Cr3+ concentration affected the biosorption process significantly. Both Freundlich and Langmuir isotherms were able to describe the equilibrium data reasonably with high correlation coefficients (R2 > 0.95) and pseudo-second-order model best fitted the biosorption process at experimental conditions. Moreover, Environmental Scanning Electronic microscope (ESEM), X-ray energy dispersion (EDX), and Fourier transform infrared (FTIR) analyses revealed that metal complexation, chemical precipitation, and ion exchange were involved in the removal of Cr3+ with aerobic granules. Further analysis by a metal ion fraction test demonstrated that metal complexation could be the dominant mechanism of biosorption, whereas chemical precipitation and ion exchange appeared only to have minor role in the overall Cr3+ biosorption process.

  9. Study on the adsorption of heavy metal ions from aqueous solution on modified SBA-15

    Directory of Open Access Journals (Sweden)

    Liliana Giraldo

    2013-01-01

    Full Text Available Amino-functionalized SBA-15 mesoporous silica was prepared, characterized, and used as an adsorbent for heavy metal ions. The organic - inorganic hybrid material was obtained by a grafting procedure using SBA-15 silica with 3-aminopropyl-triethoxysilane and bis(2,4,4-trimethylpentyl phosphinic acid (Cyanex 272, respectively. The structure and physicochemical properties of the materials were characterized by means of elemental analysis, X-ray diffraction (XRD, nitrogen adsorption - desorption, thermogravimetric analysis, FTIR spectroscopy and immersion calorimetry. The organic functional groups were successfully grafted onto the SBA-15 surface and the ordering of the support was not affected by the chemical modification. The behavior of the grafted solids was investigated for the adsorption of heavy metal ions from aqueous solutions. The hybrid materials showed high adsorption capacity and high selectivity for zinc ions. Other ions, such as cooper and cobalt were absorbed by the modified SBA-15 material.

  10. Removal of Lead (II Ions from Aqueous Solutions onto Activated Carbon Derived from Waste Biomass

    Directory of Open Access Journals (Sweden)

    Murat Erdem

    2013-01-01

    Full Text Available The removal of lead (II ions from aqueous solutions was carried out using an activated carbon prepared from a waste biomass. The effects of various parameters such as pH, contact time, initial concentration of lead (II ions, and temperature on the adsorption process were investigated. Energy Dispersive X-Ray Spectroscopy (EDS analysis after adsorption reveals the accumulation of lead (II ions onto activated carbon. The Langmuir and Freundlich isotherm models were applied to analyze equilibrium data. The maximum monolayer adsorption capacity of activated carbon was found to be 476.2 mg g−1. The kinetic data were evaluated and the pseudo-second-order equation provided the best correlation. Thermodynamic parameters suggest that the adsorption process is endothermic and spontaneous.

  11. Effect of polymer matrix on structure of Se particles formed in aqueous solutions during redox process

    Energy Technology Data Exchange (ETDEWEB)

    Suvorova, E. I., E-mail: suvorova@ns.crys.ras.ru; Klechkovskaya, V. V. [Shubnikov Institute of Crystallography of Russian Academy of Sciences (Russian Federation)

    2010-12-15

    Transmission electron microscopy and X-ray energy dispersive microanalysis study of the structure of particles formed during the reduction of Se(IV) to Se(0) in aqueous solutions in the presence of amphiphilic polymers showed the formation of Se/polymer composite particles. The content of carbon inside the particles can be as large as 80 at %. Polymers deeply influence the structure of particles. Depending on polymers, the composite particles may be unstable with time and they spontaneously evolve from Se/polymer composite particles to crystalline particles of monoclinic Se. For the stable ones, addition of bacterial cellulose Acetobacter xylinum gel-film can induce crystallization in the particles which expel the polymeric material. The Se/polymer composite particles and Se crystalline particles exhibit different sensitivity to electron irradiation and stiffness.

  12. Removal of hexavalent chromium from aqueous solution by calcined Zn/Al-LDHs.

    Science.gov (United States)

    Yang, Hui-Duo; Zhao, Yun-Peng; Li, Shi-Feng; Fan, Xing; Wei, Xian-Yong; Zong, Zhi-Min

    2016-01-01

    In this study, Zn/Al-layered double hydroxides (Zn/Al-LDHs) were synthesized by a co-precipitation method and characterized with X-ray diffraction, Fourier transform infrared spectroscopy, and scanning electron microscopy. Then the hexavalent chromium Cr(VI) adsorption experiments on calcined Zn/Al-LDHs were carried out to analyze the effects of pH, temperature, adsorption time, initial Cr(VI) concentration and adsorbent dosage on the removal of Cr(VI) from aqueous solutions. The maximum adsorption capacity for Cr(VI) on calcined Zn/Al-LDHs under optimal conditions was found to be over 120 mg/g. The kinetic and isotherm of Cr(VI) adsorption on calcined Zn/Al-LDHs can be described with the pseudo-second-order kinetic model and Langmuir isotherm, respectively. PMID:27387001

  13. First Observation of Electron Transfer Mediated Decay in Aqueous Solutions: A Novel Probe of Ion Pairing

    CERN Document Server

    Unger, I; Thürmer, S; Aziz, E F; Cederbaum, L S; Muchová, E; Slavíček, P; Winter, B; Kryzhevoi, N V

    2016-01-01

    A major goal of many spectroscopic techniques is to provide comprehensive information on the local chemical environment. Electron transfer mediated decay (ETMD) is a sensitive probe of the environment since it is actively involved in this non-local radiationless decay process through electron and energy transfer steps. We report the first experimental observation of ETMD in the liquid phase. Using liquid-jet X-ray photoelectron spectroscopy we explore LiCl aqueous solution, and detect low-energy electrons unambiguously emerging from the ETMD processes of core-ionized Li+. We interpret the experimental results with molecular dynamics and high-level ab initio calculations. By considering various solvation-structure models we show that both water molecules and Cl- anions can participate in ETMD, with each process having its characteristic spectral fingerprint. Different ion associations lead to different spectral shapes. The potential application of the unique sensitivity of the ETMD spectroscopy to the local hy...

  14. Rapid synthesis of CdSe nanocrystals in aqueous solution at room temperature

    Indian Academy of Sciences (India)

    Yilin Wang; Jian Ping Lu; Zhang Fa Tong

    2010-10-01

    Water-soluble thioglycolic acid-capped CdSe nanocrystals (NCs) were prepared in aqueous solution at room temperature. We investigated the effects of pH values on the fluorescence intensity of the as-prepared CdSe NCs, and discussed the influence of the initial pH values on the fluorescence property. Their mean diameter was estimated to be 1.9 nm depending on the initial pH values in the preparation, the photoluminescence quantum yield could reach as high as 1.9%, almost comparable to the CdSe NCs prepared by an organometallic route. Finally, the products were characterized by Fourier transform infrared spectrometry (FTIR), atomic force microscope (AFM) and X-ray powder diffraction (XRD). AFM image showed that the NCs were ball-shaped with good dispersibility. XRD analysis disclosed that the CdSe NCs were of cubic zinc-blended structure.

  15. 100-picosecond time-resolved X-ray absorption fine structure of FeII(1,10-phenanthroline)3

    International Nuclear Information System (INIS)

    Studying photo-induced molecular dynamics in liquid with sub-nanosecond time-resolution and sub-Angstrom spatial resolution gives information for understanding fundamental chemical process in the photo-induced cooperative phenomena of molecular systems and also for developing new materials and devices. Here, we present time-resolved X-ray absorption fine structure on the spin-crossover complex FeII tris-(1,10-phenanthroline) dissolved in aqueous solution. We utilized femtosecond laser at 400nm pulse for excitation and 100ps X-ray pulse for probe.

  16. 100-picosecond time-resolved X-ray absorption fine structure of FeII(1,10-phenanthroline)3

    Science.gov (United States)

    Sato, Tokushi; Nozawa, Shunsuke; Ichiyanagi, Kouhei; Tomita, Ayana; Ichikawa, Hirohiko; Chollet, Matthieu; Fujii, Hiroshi; Adachi, Shin-ichi; Koshihara, Shin-ya

    2009-02-01

    Studying photo-induced molecular dynamics in liquid with sub-nanosecond time-resolution and sub-Angstrom spatial resolution gives information for understanding fundamental chemical process in the photo-induced cooperative phenomena of molecular systems and also for developing new materials and devices. Here, we present time-resolved X-ray absorption fine structure on the spin-crossover complex FeII tris-(1,10-phenanthroline) dissolved in aqueous solution. We utilized femtosecond laser at 400nm pulse for excitation and 100ps X-ray pulse for probe.

  17. Cobalt separation present in aqueous solution using shell tamarind as bio sorbent

    International Nuclear Information System (INIS)

    In this work a new carbonaceous material is presented with improved adsorption properties obtained by a heart treatment about 5 min from the shell tamarind. It was found that the samples obtained carbonaceous adsorbents are effective in removing Co2+ (41 mg / g) ions in aqueous solutions. These samples were prepared from tamarind shell, urea, ammonium nitrate and water. The solution was subjected to a combustion process at different temperatures. Carbonaceous samples prepared in this manner were characterized by X-ray diffraction, infrared spectroscopy, scanning electron microscopy (Sem) and surface area measurements by Physisorption of N2. Changes in structure, morphology and texture were studied. The results show that this material is of great importance to the applications of adsorption of metal ions. The measurements of specific surface area (Bet) were 2.35 to 203.76 m2 g-1 with pore diameters between 2.31 and 15.63 nm, indicating that the samples obtained are predominantly meso porous. The combustion process of the solution proved to be advantageous to improve the textural properties of the tamarind shell. The obtained carbonaceous material plays an important role in adsorption to remove cobalt in aqueous solutions. (Author)

  18. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... clothing that might interfere with the x-ray images. Women should always inform their physician and x-ray ... small burst of radiation that passes through the body, recording an image on photographic film or a special detector. Different ...

  19. X-ray diagnostic equipment

    International Nuclear Information System (INIS)

    An X-ray tube is connected to several different image processing devices in X-ray diagnostic equipment. Only a single organ selector is allocated to it, for which the picture parameters for each image processing device are selected. The choice of the correct combination of picture parameters is made by means of a selector switch. (DG)

  20. X-ray tube arrangement

    International Nuclear Information System (INIS)

    An x-ray tube is described incorporating an elongated target/ anode over which the electron beam is deflected and from which x-rays are emitted. Improved methods of monitoring and controlling the amplitude of the beam deflection are presented. (U.K.)

  1. Raman spectroscopy application to analyses of components in aqueous solutions

    Science.gov (United States)

    Li, Gang; Zhang, Guoping

    2006-09-01

    The characterization of species in aqueous solutions has presented a challenge to analytical and physical chemist, because the JR absorption of the aqueous solvent is so intense that it becomes difficult to observe the solute in the water by JR absorption. In contrast, Raman spectrum of the solute is unaffected by the water, so the weak scattering of water makes the technique well suited to aqueous samples, and the Raman spectrum exhibits well-defined bands corresponding to fundamental modes of vibration. In addition, Raman spectroscopy has some inherent advantages in aqueous solution analysis, because the spectral features of signals from different species are much more distinct, and it provides characteristic signatures for samples, such as blood, protein and cholesterol. All the advantages make Raman spectroscopy be a potential alternative for the study of aqueous solutions. Now, Raman spectroscopy has been applied to studying samples in aqueous solutions, blood serum, intracellular protein levels. Now, industrial wasted water contains many organic contaminants, and it is necessary to determine and monitor these contaminants. The paper first introduces Raman spectroscopy, and then describes its applications to determining the components in aqueous solutions, analyzes and assignes the Raman spectra of o-dichlorobenzene, o-xylene, m-xyiene and p-xylene in detail. The experimental results demonstrate that Raman spectroscopy is a particularly powerful technique for aqueous solutions analyses.

  2. Acetic acid extraction from aqueous solutions using fatty acids

    NARCIS (Netherlands)

    IJmker, H.M.; Gramblicka, M.; Kersten, S.R.A.; Ham, van der A.G.J.; Schuur, B.

    2014-01-01

    A major challenge for production of acetic acid via bio-based routes is cost-effective concentration and purification of the acetic acid from the aqueous solutions, for which liquid–liquid extraction is a possible method. A main challenge in extraction of acetic acid from dilute aqueous solutions is

  3. ESR study on carboxymethyl chitosan radicals in an aqueous solution

    Energy Technology Data Exchange (ETDEWEB)

    Saiki, Seiichi, E-mail: saiki.seiichi@jaea.go.j [Graduate School of Engineering, University of Tokyo, 7-3-1 Hongo, Bunkyo, Tokyo 113-8656 (Japan); Quantum Beam Science Directorate, Japan Atomic Energy Agency, 1233 Watanuki, Takasaki, Gunma 370-1292 (Japan); Nagasawa, Naotsugu; Hiroki, Akihiro; Morishita, Norio; Tamada, Masao [Quantum Beam Science Directorate, Japan Atomic Energy Agency, 1233 Watanuki, Takasaki, Gunma 370-1292 (Japan); Muroya, Yusa; Kudo, Hisaaki [Graduate School of Engineering, University of Tokyo, 7-3-1 Hongo, Bunkyo, Tokyo 113-8656 (Japan); Katsumura, Yosuke [Graduate School of Engineering, The University of Tokyo, 7-3-1 Hongo, Bunkyo, Tokyo 113-8656 (Japan); Advanced Science Research Center, Japan Atomic Energy Agency, 2-4 Shirakata-Shirane, Tokai, Naka, Ibaraki 319-1195 (Japan)

    2010-03-15

    Carboxymethyl chitosan (CMCTS) at a highly concentrated aqueous solution forms hydrogel by ionizing irradiation. To study on radiation-induced reaction mechanism of CMCTS in an aqueous solution, CMCTS radicals formed by reactions with OH radical were observed by ESR method. As a result of ESR spectral analysis, CMCTS radicals were identified as radicals on carboxymethyl groups.

  4. Structure of aqueous sodium perchlorate solutions.

    Science.gov (United States)

    General, Ignacio J; Asciutto, Eliana K; Madura, Jeffry D

    2008-12-01

    Salt solutions have been the object of study of many scientists through history, but one of the most important findings came along when the Hofmeister series were discovered. Their importance arises from the fact that they influence the relative solubility of proteins, and solubility is directly related to one of today's holy grails: protein folding. In this work we characterize one of the more-destabilizing salts in the series, sodium perchlorate, by studying it as an aqueous solution at various concentrations ranging from 0.08 to 1.60 mol/L. Molecular dynamics simulations at room temperature permitted a detailed study of the organization of solvent and cosolvent, in terms of its radial distribution functions, along with the study of the structure of hydrogen bonds in the ions' solvation shells. We found that the distribution functions have some variations in their shape as concentration changes, but the position of their peaks is mostly unaffected. Regarding water, the most salient fact is the noticeable (although small) change in the second hydration shell and even beyond, especially for g(O(w)***O(w)), showing that the locality of salt effects should not be restricted to considerations of only the first solvation shell. The perturbation of the second shell also appears in the study of the HB network, where the difference between the number of HBs around a water molecule and around the Na(+) cation gets much smaller as one goes from the first to the second solvation shell, yet the difference is not negligible. Nevertheless, the effect of the ions past their first hydration shell is not enough to make a noticeable change in the global HB network. The Kirkwood-Buff theory of liquids was applied to our system, in order to calculate the activity derivative of the cosolvent. This coefficient, along with a previously calculated preferential binding, allowed us to establish that if a folded AP peptide is immersed in the studied solution, becoming the solute, then

  5. Removal of radium from aqueous solutions

    International Nuclear Information System (INIS)

    Adsorption of radium from aqueous solution with montmorillonite clay was investigated. Adsorption isotherm data of the radium and montmorillonite clay system were developed and fitted to both the Langmuir and Freundlich isotherm equations. The Langmuir isotherm equation was determined to be q = 6.700 C/1 + 8.447 x 10-5C and the Freundlich isotherm equation is q = 45.431 C/sup 1/1.401/. A rotary precoat filtration technique was used for dewatering the slurries of the montmorillonite clay and diatomaceous earth mixture. The rate of filtration was found to be a function of the weight percent of the clay, applied vacuum, drum speed and precoat thickness. The functional relationship is of the form Q = (0.682 + 0.035 X1 - 0.014 X2 + 0.140 X3 + 0.007 X1X2)/1 + (3.744 - 0.767 X3 + 0.079 X1X2)C125. 15 figures, 11 tables

  6. Self-Assembly of Amphiphilic Block Copolymers Containing Poly(n-octadecyl acrylate) Block in Aqueous Solution

    Energy Technology Data Exchange (ETDEWEB)

    Akiba, Isamu; Akino, Yusuke; Masunaga, Hiroyasu; Sakurai, Kazuo, E-mail: akiba@env.kitakyu-u.ac.jp

    2010-11-15

    Synchrotron small-angle X-ray scattering (SAXS) experiments were carried out for poly(acrylic acid)-block-poly(n-octadecyl acrylate) (PAA-b-PODA) and PAA-b-PODA-b-PAA micelles in aqueous solutions. SAXS results indicated that PAA-b-PODA and PAA-b-PODA-b-PAA formed core-shell micelles with disk-like morphology below melting temperature of PODA in aqueous solutions. The thickness of PAA-b-PODA (diblock copolymer) micelle was larger than that of PAA-b-PODA-b-PAA (triblock copolymer) micelle. The difference of sizes between these micelles was related to difference of molecular architectures of PAA-b-PODA and PAA-b-PODA-b-PAA. PAA-b-PODA micelle showed morphological transition from disk to spherical shape with elevating temperature. On the contrary, PAA-b-PODA-b-PAA micelle maintained disk-like shape above melting temperature, although enlargement of micelle thickness is caused.

  7. Self-Assembly of Amphiphilic Block Copolymers Containing Poly(n-octadecyl acrylate) Block in Aqueous Solution

    Science.gov (United States)

    Akiba, Isamu; Akino, Yusuke; Masunaga, Hiroyasu; Sakurai, Kazuo

    2010-11-01

    Synchrotron small-angle X-ray scattering (SAXS) experiments were carried out for poly(acrylic acid)-block-poly(n-octadecyl acrylate) (PAA-b-PODA) and PAA-b-PODA-b-PAA micelles in aqueous solutions. SAXS results indicated that PAA-b-PODA and PAA-b-PODA-b-PAA formed core-shell micelles with disk-like morphology below melting temperature of PODA in aqueous solutions. The thickness of PAA-b-PODA (diblock copolymer) micelle was larger than that of PAA-b-PODA-b-PAA (triblock copolymer) micelle. The difference of sizes between these micelles was related to difference of molecular architectures of PAA-b-PODA and PAA-b-PODA-b-PAA. PAA-b-PODA micelle showed morphological transition from disk to spherical shape with elevating temperature. On the contrary, PAA-b-PODA-b-PAA micelle maintained disk-like shape above melting temperature, although enlargement of micelle thickness is caused.

  8. Use of Raman spectroscopy to assess the efficiency of MgAl mixed oxides in removing cyanide from aqueous solutions

    Science.gov (United States)

    Cosano, Daniel; Esquinas, Carlos; Jiménez-Sanchidrián, César; Ruiz, José Rafael

    2016-02-01

    Calcining magnesium/aluminium layered double hydroxides (Mg/Al LDHs) at 450 °C provides excellent sorbents for removing cyanide from aqueous solutions. The process is based on the "memory effect" of LDHs; thus, rehydrating a calcined LDH in an aqueous solution restores its initial structure. The process, which conforms to a first-order kinetics, was examined by Raman spectroscopy. The metal ratio of the LDH was found to have a crucial influence on the adsorption capacity of the resulting mixed oxide. In this work, Raman spectroscopy was for the first time use to monitor the adsorption process. Based on the results, this technique is an effective, expeditious choice for the intended purpose and affords in situ monitoring of the adsorption process. The target solids were characterized by using various instrumental techniques including X-ray diffraction spectroscopy, which confirmed the layered structure of the LDHs and the periclase-like structure of the mixed oxides obtained by calcination.

  9. Manufacturing of patterned ZnO films with application for photoinitiated decolorization of malachite green in aqueous solutions

    Indian Academy of Sciences (India)

    Nina V Kaneva; Georgi G Yordanov; Ceco D Dushkin

    2010-04-01

    Patterned thin films, ZnO, are successfully prepared on glass substrates by the sol–gel method using dip-coating technique. The films, formed of ZnO nanocrystallites with hexagonal crystal structure, are characterized by means of scanning electron microscopy, Fourier transform infrared spectroscopy and X-ray diffraction. The as obtained ZnO films are studied with respect to photo-initiated bleaching of malachite green in aqueous solutions. The bleaching process is investigated at various initial concentrations of malachite green in the aqueous solutions by using ZnO films of different thicknesses. The obtained results are promising for the development of ZnO photocatalysts by the sol–gel method.

  10. In situ X-Ray diffraction study of hydrogen sorption in V-rich Ti–V–Cr bcc solid solutions

    Energy Technology Data Exchange (ETDEWEB)

    Planté, Damien [CNRS, Insitut NEEL, F-38042 Grenoble (France); Université Grenoble Alpes, Inst. NEEL, F-38042 Grenoble (France); Andrieux, Jérôme [ID15, ESRF, 6 rue Jules Horowitz, 38043 Grenoble (France); Université Claude Bernard Lyon 1, LMI – UMR CNRS N° 5615, 43 Bd du 11 novembre 1918, 69622 Villeurbanne Cedex (France); Laversenne, Laetitia [CNRS, Insitut NEEL, F-38042 Grenoble (France); Université Grenoble Alpes, Inst. NEEL, F-38042 Grenoble (France); Miraglia, Salvatore, E-mail: salvatore.miraglia@neel.cnrs.fr [CNRS, Insitut NEEL, F-38042 Grenoble (France); Université Grenoble Alpes, Inst. NEEL, F-38042 Grenoble (France)

    2015-11-05

    Alloying of vanadium with a combination of titanium and chromium has been investigated in this study. Hydrogenation/desorption of several alloys under similar experimental conditions has been performed and sequentially followed by means of in situ X-Ray powder diffraction. This latter technique has been used as a probe of formation or decomposition of hydrides. Geometrical effects are discussed and account for the observed similarities of the sorption properties. - Highlights: • In situ synchrotron XRD as a probe of formation/decomposition of hydrides. • Thermal stability of (Ti–Cr) alloyed vanadium-rich hydrides. • Discussion of the hydrides practicability.

  11. High-pressure x-ray diffraction study of U sub x La sub 1 sub - sub x S solid solution

    CERN Document Server

    Bihan, T L; Idiri, M; Heathman, S; Lindbaum, A

    2002-01-01

    X-ray diffraction measurements under pressure have been performed on seven different compositions in the U sub x La sub 1 sub - sub x S system (x = 0, 0.08, 0.40, 0.50, 0.60, 0.80, 1). All the compounds have the same structure (NaCl type) at ambient pressure, but show different behaviours under pressure. A transformation into the CsCl-type structure is only observed for x = 0.60, B sub 0 approx 100 GPa) and in the transition pressure (approx 30 GPa for low-uranium-content compounds and from 45 to 80 GPa for high concentrations).

  12. Increasing correlation length in bulk supercooled H2O, D2O, and NaCl solution determined from small angle x-ray scattering

    OpenAIRE

    Huang, Congcong; Weiss, T M; Nordlund, D.; Wikfeldt, K. T.; Pettersson, L. G. M.; Nilsson, A.

    2010-01-01

    Using small angle x-ray scattering, we find that the correlation length of bulk liquid water shows a steep increase as temperature decreases at subzero temperatures (supercooling) and that it can, similar to the thermodynamic response functions, be fitted to a power law. This indicates that the anomalous properties of water are attributable to fluctuations between low- and high-density regions with rapidly growing average size upon supercooling. The substitution of H2O with D2O, as well as th...

  13. Hexavalent chromium removal from aqueous solutions by a novel powder prepared from Colocasia esculenta leaves.

    Science.gov (United States)

    Nakkeeran, E; Saranya, N; Giri Nandagopal, M S; Santhiagu, A; Selvaraju, N

    2016-08-01

    In this study, batch removal of hexavalent chromium from aqueous solutions by powdered Colocasia esculenta leaves was investigated. Batch experiments were conducted to study the effects of adsorption of Cr(VI) at different pH values, initial concentrations, agitation speeds, temperatures, and contact times. The biosorbent was characterized by scanning electron microscopy, energy-dispersive X-ray spectroscopy, and Fourier transform infrared spectrometer analysis. The biosorptive capacity of the adsorbent was dependent on the pH of the chromium solution in which maximum removal was observed at pH 2. The adsorption equilibrium data were evaluated for various adsorption isotherm models, kinetic models, and thermodynamics. The equilibrium data fitted well with Freundlich and Halsey models. The adsorption capacity calculated was 47.62 mg/g at pH 2. The adsorption kinetic data were best described by pseudo-second-order kinetic model. Thus, Colocasia esculenta leaves can be considered as one of the efficient and cheap biosorbents for hexavalent chromium removal from aqueous solutions.

  14. Hexavalent chromium removal from aqueous solutions by a novel powder prepared from Colocasia esculenta leaves.

    Science.gov (United States)

    Nakkeeran, E; Saranya, N; Giri Nandagopal, M S; Santhiagu, A; Selvaraju, N

    2016-08-01

    In this study, batch removal of hexavalent chromium from aqueous solutions by powdered Colocasia esculenta leaves was investigated. Batch experiments were conducted to study the effects of adsorption of Cr(VI) at different pH values, initial concentrations, agitation speeds, temperatures, and contact times. The biosorbent was characterized by scanning electron microscopy, energy-dispersive X-ray spectroscopy, and Fourier transform infrared spectrometer analysis. The biosorptive capacity of the adsorbent was dependent on the pH of the chromium solution in which maximum removal was observed at pH 2. The adsorption equilibrium data were evaluated for various adsorption isotherm models, kinetic models, and thermodynamics. The equilibrium data fitted well with Freundlich and Halsey models. The adsorption capacity calculated was 47.62 mg/g at pH 2. The adsorption kinetic data were best described by pseudo-second-order kinetic model. Thus, Colocasia esculenta leaves can be considered as one of the efficient and cheap biosorbents for hexavalent chromium removal from aqueous solutions. PMID:26853060

  15. Semiconductor X-ray detectors

    CERN Document Server

    Lowe, Barrie Glyn

    2014-01-01

    Identifying and measuring the elemental x-rays released when materials are examined with particles (electrons, protons, alpha particles, etc.) or photons (x-rays and gamma rays) is still considered to be the primary analytical technique for routine and non-destructive materials analysis. The Lithium Drifted Silicon (Si(Li)) X-Ray Detector, with its good resolution and peak to background, pioneered this type of analysis on electron microscopes, x-ray fluorescence instruments, and radioactive source- and accelerator-based excitation systems. Although rapid progress in Silicon Drift Detectors (SDDs), Charge Coupled Devices (CCDs), and Compound Semiconductor Detectors, including renewed interest in alternative materials such as CdZnTe and diamond, has made the Si(Li) X-Ray Detector nearly obsolete, the device serves as a useful benchmark and still is used in special instances where its large, sensitive depth is essential. Semiconductor X-Ray Detectors focuses on the history and development of Si(Li) X-Ray Detect...

  16. X-ray diffraction apparatus

    International Nuclear Information System (INIS)

    The invention provides an x-ray diffraction apparatus permitting the rotation of the divergence sit in conjunction with the rotation of the x-ray irradiated specimen, whereby the dimensions of the x-ray irradiated portion of the specimen remain substantially constant during the rotation of the specimen. In a preferred embodiment, the divergence slit is connected to a structural element linked with a second structural element connected to the specimen such that the divergence slit rotates at a lower angular speed than the specimen

  17. Ozone photolysis of paracetamol in aqueous solution.

    Science.gov (United States)

    Neamţu, Mariana; Bobu, Maria; Kettrup, Antonius; Siminiceanu, Ilie

    2013-01-01

    The degradation of a paracetamol (N-acetil-para-aminofenol) aqueous solution (C (0) P = 5 mmol L(-1)) is studied in a bench-scale setup by means of simple ozonation (O3) and ozonation catalyzed with UV light (O3/UV) in order to quantify the influence of UV light on the degradation process. The results have shown that under the adopted experimental conditions (25°C, applied ozone dose = 9.8 mg L(-1) and gas flow rate of 20 L h(-1)) both oxidative systems are capable of removing the substrate with mineralization degrees up to 51% for ozonation and 53% for O3/UV. HPICE chromatography allowed the detection of nitrate ions and maleic and oxalic acids as ultimate carboxylic acids. The experimental data have been interpreted through 5 indicators: the conversion of paracetamol (XP ), the conversion degree of TOC (XTOC ), the apparent rate constant (kap ), the Hatta number (Ha) and the enhancement factor (E). The main advantage of photo-ozonation compared to simple ozonation was a more advanced conversion (79% vs. 92% after 90 min). The paracetamol decay follows a pseudo-first-order reaction with a superior rate constant (higher by 54%) for the UV catalyzed system in comparison with direct ozonation. Mineralization is slightly accelerated (+4%) in the O3/UV system, due to the additional production of hydroxyl radicals induced by the UV light and a higher Hatta number (+24%). Nevertheless, the process was still in the slow reaction kinetic regime (Ha < 0.3), and the enhancement factor was not significantly increased. The results are useful for the design and scale-up of the gas-liquid processes. PMID:23647117

  18. Ozone photolysis of paracetamol in aqueous solution.

    Science.gov (United States)

    Neamţu, Mariana; Bobu, Maria; Kettrup, Antonius; Siminiceanu, Ilie

    2013-01-01

    The degradation of a paracetamol (N-acetil-para-aminofenol) aqueous solution (C (0) P = 5 mmol L(-1)) is studied in a bench-scale setup by means of simple ozonation (O3) and ozonation catalyzed with UV light (O3/UV) in order to quantify the influence of UV light on the degradation process. The results have shown that under the adopted experimental conditions (25°C, applied ozone dose = 9.8 mg L(-1) and gas flow rate of 20 L h(-1)) both oxidative systems are capable of removing the substrate with mineralization degrees up to 51% for ozonation and 53% for O3/UV. HPICE chromatography allowed the detection of nitrate ions and maleic and oxalic acids as ultimate carboxylic acids. The experimental data have been interpreted through 5 indicators: the conversion of paracetamol (XP ), the conversion degree of TOC (XTOC ), the apparent rate constant (kap ), the Hatta number (Ha) and the enhancement factor (E). The main advantage of photo-ozonation compared to simple ozonation was a more advanced conversion (79% vs. 92% after 90 min). The paracetamol decay follows a pseudo-first-order reaction with a superior rate constant (higher by 54%) for the UV catalyzed system in comparison with direct ozonation. Mineralization is slightly accelerated (+4%) in the O3/UV system, due to the additional production of hydroxyl radicals induced by the UV light and a higher Hatta number (+24%). Nevertheless, the process was still in the slow reaction kinetic regime (Ha < 0.3), and the enhancement factor was not significantly increased. The results are useful for the design and scale-up of the gas-liquid processes.

  19. Synchrotron X-ray diffraction study of the Ba{sub 1−x}SrSnO{sub 3} solid solution

    Energy Technology Data Exchange (ETDEWEB)

    Prodjosantoso, Anti K., E-mail: Prodjosantoso@yahoo.com [Jurusan Pendidikan Kimia, UNY Yogyakarta, DIY 55281 (Indonesia); Zhou, Qingdi; Kennedy, Brendan J. [School of Chemistry, The University of Sydney, Sydney, NSW 2006 (Australia)

    2013-04-15

    At room temperature the sequence of phases with increasing amounts of strontium in the stannate perovskite system Ba{sub 1−x}SrSnO{sub 3} has been established from high resolution synchrotron X-ray powder diffraction. The observed sequence orthorhombic (Pbnm), orthorhombic (Ibmm), tetragonal (I4/mcm), and cubic (Pm3-bar m) is a consequence of the sequential introduction of cooperative tilting of the corner sharing SnO{sub 6} octahedra. The cell volume changes smoothly across the series with no obvious discontinuities associated with the phase transitions. - Graphical abstract: Portions of the synchrotron X-ray diffraction profiles (λ=0.82453 Å) from selected Ba{sub 1−x}Sr{sub x}SnO{sub 3} samples together with the results of fitting by the Rietveld method. Highlights: ► Structures of the stannate perovskites Ba{sub 1−x}SrSnO{sub 3} refined from synchrotron XRD. ► The sequence Pm3-bar m→I4/mcm→Ibmm→Pbnm results from tilting of the octahedra. ► The tilting maintains optimal bonding of the cations seen from the BVS analysis.

  20. Photolysis of Periodate and Periodic Acid in Aqueous Solution

    DEFF Research Database (Denmark)

    Sehested, Knud; Kläning, U. K.

    1978-01-01

    The photochemistry of periodate and periodic acid in aqueous solution was studied (i) by quantum yield measurements at low light intensity (ii) by flash photolysis, and (iii) by photolysis of glassy samples at 77 K. The photochemical studies were supplemented with pulse radiolysis studies...... of aqueous periodate solutions and with kinetic studies using stopped-flow technique. In strongly alkaline solution the photodecomposition of periodate proceeds via formation of O– and IVI. At pH

  1. Phase transfer of platinum nanoparticles from aqueous to organic solutions using fatty amine molecules

    Indian Academy of Sciences (India)

    Ashavani Kumar; Hrushikesh M Joshi; Anandrao B Mandale; Rajendra Srivastava; Suguna D Adyanthaya; Renu Pasricha; Murali Sastry

    2004-08-01

    In this report we demonstrate a simple process based on amine chemistry for the phase transfer of platinum nanoparticles from an aqueous to an organic solution. The phase transfer was accomplished by vigorous shaking of a biphasic mixture of platinum nanoparticles synthesised in an aqueous medium and octadecylamine (ODA) in hexane. During shaking of the biphasic mixture, the aqueous platinum nanoparticles complex via either coordination bond formation or weak covalent interaction with the ODA molecules present in the organic phase. This process renders the nanoparticles sufficiently hydrophobic and dispersible in the organic phase. The ODA-stabilised platinum nanoparticles could be separated out from hexane in the form of a powder that is readily redispersible in weakly polar and nonpolar organic solvents. The ODA-capped platinum nanoparticles show high catalytic activity in hydrogenation reactions and this is demonstrated in the efficient conversion of styrene to ethyl benzene. The nature of binding of the ODA molecules to the platinum nanoparticles surface was characterised by thermogravimetry, transmission electron microscopy (TEM), X-ray photoemission spectroscopy (XPS) and Fourier transform infrared spectroscopy (FTIR).

  2. Analysis by synchrotron X-ray radiography of convection effects on the dynamic evolution of the solid-liquid interface and on solute distribution during the initial transient of solidification

    Energy Technology Data Exchange (ETDEWEB)

    Bogno, A., E-mail: abdoul-aziz.bogno@im2np.fr [Aix Marseille Universite, Campus Saint-Jerome, Case 142, 13397 Marseille Cedex 20 (France); CNRS, UMR 6242, Campus Saint-Jerome, Case 142, 13397 Marseille Cedex 20 (France); Nguyen-Thi, H. [Aix Marseille Universite, Campus Saint-Jerome, Case 142, 13397 Marseille Cedex 20 (France); CNRS, UMR 6242, Campus Saint-Jerome, Case 142, 13397 Marseille Cedex 20 (France); Buffet, A. [ESRF, Avenue des Martyrs, BP 220, 38048 Grenoble Cedex (France); Reinhart, G.; Billia, B.; Mangelinck-Noel, N.; Bergeon, N. [Aix Marseille Universite, Campus Saint-Jerome, Case 142, 13397 Marseille Cedex 20 (France); CNRS, UMR 6242, Campus Saint-Jerome, Case 142, 13397 Marseille Cedex 20 (France); Baruchel, J. [ESRF, Avenue des Martyrs, BP 220, 38048 Grenoble Cedex (France); Schenk, T. [LPM - ENSMN, Parc de Saurupt, 54042 Nancy Cedex (France)

    2011-06-15

    In situ monitoring of the initial transient of directional solidification was carried out by means of synchrotron X-ray radiography. Experiments with Al-4 wt.% Cu alloy samples were performed on beamline ID19 of the European Synchrotron Radiation Facility (ESRF) in a dedicated Bridgman-type furnace. X-ray radiography enabled a detailed analysis of the evolution over time of the solid-liquid interface macroscopic shape in interaction with convection in the melt. Lateral solute segregation induced by fluid flow resulted in a significant deformation of the solid-liquid interface. The time-dependent velocity of the solidification front was determined at different abscissa values along the curved interface during the solidification process, from the growth phase with a smooth interface to the onset of morphological instability. Further, using a novel quantitative image analysis technique we were able to measure longitudinal solute profiles in the melt during the initial transient. Solutal length was then deduced as well as concentration in the melt, both at the interface and far away from it. The influence of convection on growth velocity and the characteristic parameters of the solute boundary layer are discussed, and a comparison with the Warren and Langer model is also presented.

  3. Duodenal X-ray diagnostics

    International Nuclear Information System (INIS)

    The publication provides an overview of duodenal X-ray diagnostics with the aid of barium meals in 1362 patients. The introducing paragraphs deal with the topographic anatomy of the region and the methodics of X-ray investigation. The chapter entitled ''processes at the duodenum itself'' describes mainly ulcers, diverticula, congenital anomalies, tumors and inflammations. The neighbourhood processes comprise in the first place diseases having their origin at the pancreas and bile ducts. As a conclusion, endoscopic rectograde cholangio-pancreaticography and percutaneous transhepatic cholangiography are pointed out as advanced X-ray investigation methods. In the annex of X-ray images some of the described phenomena are shown in exemplary manner. (orig./MG)

  4. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... like a photographic negative). Today, most images are digital files that are stored electronically. These stored images ... and places the x-ray film holder or digital recording plate under the table in the area ...

  5. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... pregnant. Many imaging tests are not performed during pregnancy so as not to expose the fetus to ... See the Safety page for more information about pregnancy and x-rays. top of page What does ...

  6. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... the baby. See the Safety page for more information about pregnancy and x-rays. top of page ... procedure varies. See the Safety page for more information about radiation dose. Women should always inform their ...

  7. X-ray microtomographic scanners

    Energy Technology Data Exchange (ETDEWEB)

    Syryamkin, V. I., E-mail: klestov-simon@mail.ru; Klestov, S. A., E-mail: klestov-simon@mail.ru [National Research Tomsk State University, Tomsk, 634050 (Russian Federation)

    2015-11-17

    The article studies the operating procedures of an X-ray microtomographic scanner and the module of reconstruction and analysis 3D-image of a test sample in particular. An algorithm for 3D-image reconstruction based on image shadow projections and mathematical methods of the processing are described. Chapter 1 describes the basic principles of X-ray tomography and general procedures of the device developed. Chapters 2 and 3 are devoted to the problem of resources saving by the system during the X-ray tomography procedure, which is achieved by preprocessing of the initial shadow projections. Preprocessing includes background noise removing from the images, which reduces the amount of shadow projections in general and increases the efficiency of the group shadow projections compression. In conclusion, the main applications of X-ray tomography are presented.

  8. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... top of page What are the benefits vs. risks? Benefits Bone x-rays are the fastest and ... in the typical diagnostic range for this exam. Risks There is always a slight chance of cancer ...

  9. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... can be taken to the patient in a hospital bed or the emergency room. The x-ray ... and international radiology protection organizations continually review and update the technique standards used by radiology professionals. Modern ...

  10. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... the patient in a hospital bed or the emergency room. The x-ray tube is connected to ... equipment is relatively inexpensive and widely available in emergency rooms, physician offices, ambulatory care centers, nursing homes ...

  11. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... or in bones. top of page How should I prepare? Most bone x-rays require no special ... to 10 minutes. top of page What will I experience during and after the procedure? A bone ...

  12. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... the body absorb the x-rays in varying degrees. Dense bone absorbs much of the radiation while ... is further reviewed by committees from the American College of Radiology (ACR) and the Radiological Society of ...

  13. Dental X-ray apparatus

    International Nuclear Information System (INIS)

    Intra-oral dental X-ray apparatus for panoramic dental radiography is described in detail. It comprises an electron gun having an elongated tubular target carrier extending into the patient's mouth. The carrier supports an inclined target for direction of an X-ray pattern towards a film positioned externally of the patient's mouth. Image definition is improved by a focusing anode which focuses the electron beam into a sharp spot (0.05 to 0.10 mm diameter) on the target. The potential on the focusing anode is adjustable to vary the size of the spot. An X-ray transmitting ceramic (oxides of Be, Al and Si) window is positioned adjacent to the front face of the target. The electron beam can be magnetically deflected to change the X-ray beam direction. (author)

  14. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... during x-ray examinations to use the lowest radiation dose possible while producing the best images for evaluation. National and international radiology protection organizations continually review and update the technique standards ...

  15. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... technologist, an individual specially trained to perform radiology examinations, positions the patient on the x-ray table ... bone is forming), for comparison purposes. When the examination is complete, you may be asked to wait ...

  16. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... replacement and fracture reductions. look for injury, infection, arthritis , abnormal bone growths and bony changes seen in ... injuries, including fractures, and joint abnormalities, such as arthritis. X-ray equipment is relatively inexpensive and widely ...

  17. X-Ray Assembler Data

    Data.gov (United States)

    U.S. Department of Health & Human Services — Federal regulations require that an assembler who installs one or more certified components of a diagnostic x-ray system submit a report of assembly. This database...

  18. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... a large photographic negative). Today, most images are digital files that are stored electronically. These stored images ... and places the x-ray film holder or digital recording plate under the table in the area ...

  19. Corrosion fatigue behavior of high strength brass in aqueous solutions

    Energy Technology Data Exchange (ETDEWEB)

    Hamada, A.S.; Kassem, M.A.; Ramadan, R.M.; El-Zeky, M.A. [Suez Canal Univ., Dept. of Metallurgy and Materials Engineering (Egypt)

    2000-07-01

    Corrosion fatigue behavior of British Standard high strength brass, CZ 127 has been studied in various environments, 3.5%NaC1 solution and 3.5%NaC1 containing 1000ppm ammonia by applying the reverse bending technique, strain-controlled cyclic, at 67 cycles/min. Characteristics of the produced alloy were studied using differential thermal analysis with applying its results in heat treating of the alloy; metallographic examinations; hardness measurements; X-ray; and electrochemical behavior of the unstressed alloy. CZ 127 was fatigued at three different conditions, solution treated, peak aged, and over aged at a fixed strain amplitude, 0.03 5. Solution treated alloy gave the best fatigue properties in all environments tested among the other materials. Results of the alloy studied were compared with that obtained of 70/30 {alpha}-brass. Fracture surface of the fatigued alloy was examined using optical microscope and scanning electron microscope equipped with EDX. (author)

  20. Accelerator x-ray sources

    CERN Document Server

    Talman, Richard

    2007-01-01

    This first book to cover in-depth the generation of x-rays in particle accelerators focuses on electron beams produced by means of the novel Energy Recovery Linac (ERL) technology. The resulting highly brilliant x-rays are at the centre of this monograph, which continues where other books on the market stop. Written primarily for general, high energy and radiation physicists, the systematic treatment adopted by the work makes it equally suitable as an advanced textbook for young researchers.

  1. X-ray fluorescence holography

    CERN Document Server

    Hayashi, K; Takahashi, Y

    2003-01-01

    X-ray fluorescence holography (XFH) is a new structural analysis method of determining a 3D atomic arrangement around fluorescing atoms. We developed an XFH apparatus using advanced X-ray techniques and succeeded in obtaining high-quality hologram data. Furthermore, we introduced applications to the structural analysis of a thin film and the environment around dopants and, discussed the quantitative analysis of local lattice distortion. (author)

  2. Electromechanical x-ray generator

    Energy Technology Data Exchange (ETDEWEB)

    Watson, Scott A; Platts, David; Sorensen, Eric B

    2016-05-03

    An electro-mechanical x-ray generator configured to obtain high-energy operation with favorable energy-weight scaling. The electro-mechanical x-ray generator may include a pair of capacitor plates. The capacitor plates may be charged to a predefined voltage and may be separated to generate higher voltages on the order of hundreds of kV in the AK gap. The high voltage may be generated in a vacuum tube.

  3. X-ray Damage to the Mn4Ca Complex in Single Crystals ofPhotosystem II: A Case Study for Metalloprotein Crystallography

    Energy Technology Data Exchange (ETDEWEB)

    Yano, Junko; Kern, Jan; Irrgang, Klaus-Dieter; Latimer, Matthew; Bergmann, Uwe; Glatzel, Pieter; Pushkar, Yulia; Biesiadka, Jacek; Loll,Bernhard; Sauer, Kenneth; Messinger, Johannes; Zouni, Athina; Yachandra,Vittal K.

    2005-06-21

    X-ray absorption spectroscopy was used to measure the damage caused by exposure to X-rays to the Mn4Ca active site in single crystals of photosystem II, as a function of dose and energy of X-rays, temperature, and time. These studies reveal that the conditions used for structure determination by X-ray crystallography cause serious damage specifically to the metal-site structure. The X-ray absorption spectra show that the structure changes from one that is characteristic of a high-valent Mn4(III2,IV2) oxo-bridged Mn4Ca cluster, to that of Mn(II) in aqueous solution. This damage to the metal site occurs at a dose that is more than an order of magnitude lower than that resulting in loss of diffractivity, and commonly considered safe for protein crystallography. These results establish the first quantitative X-ray dose parameters applicable to redox-active metallo-proteins. This case study shows that a careful evaluation of the structural intactness of the active sites by spectroscopic techniques can validate structures derived from crystallography, and it can be a valuable complementary method before structure-function correlations of metallo-proteins can be made on the basis of high resolution X-ray crystal structures.

  4. X-ray damage to the Mn4Ca complex in single crystals of photosystem II: a case study for metalloprotein crystallography.

    Science.gov (United States)

    Yano, Junko; Kern, Jan; Irrgang, Klaus-Dieter; Latimer, Matthew J; Bergmann, Uwe; Glatzel, Pieter; Pushkar, Yulia; Biesiadka, Jacek; Loll, Bernhard; Sauer, Kenneth; Messinger, Johannes; Zouni, Athina; Yachandra, Vittal K

    2005-08-23

    X-ray absorption spectroscopy was used to measure the damage caused by exposure to x-rays to the Mn(4)Ca active site in single crystals of photosystem II as a function of dose and energy of x-rays, temperature, and time. These studies reveal that the conditions used for structure determination by x-ray crystallography cause serious damage specifically to the metal-site structure. The x-ray absorption spectra show that the structure changes from one that is characteristic of a high-valent Mn(4)(III(2),IV(2)) oxo-bridged Mn(4)Ca cluster to that of Mn(II) in aqueous solution. This damage to the metal site occurs at a dose that is more than one order of magnitude lower than the dose that results in loss of diffractivity and is commonly considered safe for protein crystallography. These results establish quantitative x-ray dose parameters that are applicable to redox-active metalloproteins. This case study shows that a careful evaluation of the structural intactness of the active site(s) by spectroscopic techniques can validate structures derived from crystallography and that it can be a valuable complementary method before structure-function correlations of metalloproteins can be made on the basis of high-resolution x-ray crystal structures.

  5. Heterogeneous photo-Fenton degradation of polyacrylamide in aqueous solution over Fe(III)-SiO2 catalyst

    International Nuclear Information System (INIS)

    This article presents preparation, characterization and evaluation of heterogeneous Fe(III)-SiO2 catalysts for the photo-Fenton degradation of polyacrylamide (PAM) in aqueous solution. Fe(III)-SiO2 catalysts are prepared by impregnation method with two iron salts as precursors, namely Fe(NO3)3 and FeSO4, and are characterized by Brunauer-Emmett-Teller (BET), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) methods. The irradiated Fe(III)-SiO2 is complexed with 1,10-phenanthroline, then is measured by UV-vis-diffuse reflectance spectroscopy (UV-vis-DRS) and XPS to confirm the oxidation state of Fe in solid state. By investigating the photo-Fenton degradation of PAM in aqueous solution, the results indicate that Fe(III)-SiO2 catalysts exhibit an excellent photocatalytic activity in the degradation of PAM. Moreover, the precursor species and the OH-/Fe mole ratio affect the photocatalytic activity of Fe(III)-SiO2 catalysts to a certain extent. Finally, the amount of Fe ions leaching from the Fe(III)-SiO2 catalysts is much low

  6. Removal of Cr(III) from aqueous solutions using zeolite NaY prepared from rice husk ash

    International Nuclear Information System (INIS)

    The efficiency of the synthesized zeolite NaY from rice husk ash (RHA) in the removal of Cr(III) from aqueous solution was studied. Zeolite NaY was synthesized from RHA via seeding technique and the identification of its structure was done by X-ray Diffraction (XRD) technique and the elemental analysis was carried out by X-ray Fluorescence (XRF). The physicochemical properties which were related to the use of the zeolite NaY as a sorbent was also investigated. The synthesized zeolite NaY has higher cation exchange capacity (CEC) than the commercial zeolite NaY due to the higher amount of sodium content in the synthesized as well as the lower ratio of silica to alumina. The synthesized zeolite NaY together with the commercial one as comparison was used in the sorption of the Cr(III) in aqueous solution by batch sorption experiments. The kinetic study showed that the Cr(III) uptake by both zeolites were based on the pseudo second order model. Synthesized zeolite NaY exhibited greater sorption capacities than the commercial zeolite NaY since the former has higher surface area and cation exchange capacity (CEC) and lower ratio of silica to alumina which have a tendency to provide more exchange sites. (author)

  7. Preparation and characterization of zirconia-loaded lignocellulosic butanol residue as a biosorbent for phosphate removal from aqueous solution

    Science.gov (United States)

    Zong, Enmin; Liu, Xiaohuan; Jiang, Jinhua; Fu, Shenyuan; Chu, Fuxiang

    2016-11-01

    Zirconium(IV) loaded lignocellulosic butanol residue (LBR-Zr) used for the adsorption of phosphate (P) ions from aqueous solution was synthesized and evaluated. The adsorption isotherms were fitted well with the Freundlich and Temkin modes. Thermodynamic analyses indicated that phosphate adsorption on the LBR-Zr increased with increasing temperature from 298 to 338 K. The kinetic datas were described better by the pseudo-second-order adsorption kinetic rate model. Increasing pH suppressed phosphate adsorption. Coexisting anions study exhibited that the incorporation of CO32- anion had the largest influence on the phosphate adsorption capacity. The mechanism of adsorption process on LBR-Zr was analyzed by FTIR (Fourier transform infrared spectroscopy), scanning electron microscope (SEM) with an EDX (energy dispersive X-ray) and X-ray photoelectron spectroscopy (XPS) technologies, respectively. The above results confirmed that surface hydroxyl groups on biosorbent LBR-Zr were replaced by phosphate. The LBR-Zr with good specific affinity towards phosphate was a promising biosorbent for phosphate removal from aqueous solution. The research would be beneficial for developing a promising, eco-friendly phosphate biosorbent from plentiful lignocellulosic butanol residue.

  8. The design and application of a new Bassett-type diamond anvil cell for spectroscopic analysis of supercritical aqueous solutions

    International Nuclear Information System (INIS)

    The Bassett-type hydrothermal diamond anvil cell has been modified to facilitate direct x-ray and Raman spectroscopic analysis of aqueous solutions and/or coexisting solid samples at temperatures and pressures above the critical point of water. The new cell provides more sample-detector geometry options for x-ray micro beam analysis and the reduced size of the cell affords a smaller working distance (≥ 14 mm) required for better Raman spectroscopic analysis and microscopic inspection. A shallow recess (300 × 300 × 26.5 μm) milled into one of the diamond anvils is used instead of a metal gasket to contain the aqueous solution. These modifications significantly improve our ability to directly monitor the composition and structure of supercritical fluids and have eliminated the problem of contamination due to the reaction of a metal gasket with supercritical water. The use of the modified hydrothermal diamond anvil cell to characterize the MoO3-H2O system up to 500 oC will be discussed. (author)

  9. X-ray diagnostic apparatus

    International Nuclear Information System (INIS)

    A falling load type X-ray diagnostic apparatus comprises a low voltage power source, AC-DC converting means connected to the low voltage power source so as to apply a rectified low DC voltage, chopping means connected to the AC-DC converting means and chopping said DC voltage into a low AC voltage, high voltage applying means for transforming said low AC voltage into a high AC voltage, said high AC voltage being applied as a tube voltage to an X-ray tube from which X-rays are irradiated toward an object to be examined, means for controlling a filament heating power of the X-ray tube, programming means for supplying a control signal to said filament heating control means so as to reduce the emission current of said X-ray tube during the irradiation, and chopper control means for controlling the chopping ratio of said chopping means by evaluating said rectified DC voltage with a preset tube voltage generated in said programming means, said programming means compensating said tube voltage by receiving said control signal in such a manner that said tube voltage is maintained substantially constant during the irradiation by varying said preset tube voltage so as to control the chopping ratio based upon the reduction of the filament heating power for the X-ray tube

  10. Low energy (soft) x rays

    International Nuclear Information System (INIS)

    Dosimetry of low-energy (soft) X rays produced by the SOFTEX Model CMBW-2 was performed using Nuclear Associates Type 30 - 330 PTW, Exradin Type A2, and Shonka-Wyckoff ionization chambers with a Keithley Model 602 electrometer. Thermoluminescent (BeO chip) dosimeters were used with a Harshaw Detector 2000-A and Picoammeter-B readout system. Beam quality measurements were made using aluminum absorbers; exposure rates were assessed by the current of the X-ray tube and by exposure times. Dose distributions were established, and the average factors for non-uniformity were calculated. The means of obtaining accurate absorbed and exposed doses using these methods are discussed. Survival of V79 cells was assessed by irradiating them with soft X rays, 200 kVp X rays, and 60Co gamma rays. The relative biological effectiveness (RBE) values for soft X rays with 0, 0.2, 0.7 mm added thicknesses of aluminum were 1.6, which were compared to 60Co. The RBE of 200 kVp X rays relative to 60Co was 1.3. Results of this study are available for reference in future RERF studies of cell survival. (author)

  11. Degradation of Hydrogenated Nitrile-butadiene Rubber in Aqueous Solutions of H2S or HCl

    Institute of Scientific and Technical Information of China (English)

    CONG Chuan-bo; CUI Can-can; MENG Xiao-yu; LU Shao-jie; ZHOU Qiong

    2013-01-01

    The degradation of hydrogenated nitrile-butadiene rubber(HNBR) soaped in aqueous solutions of H2S and HCl was investigated.The samples unexposed and exposed to different solutions were characterized by 13C nuclear magnetic resonance(13C NMR),X-ray photoelectron and infrared spectroscopies.In contrast to those of unexposed samples and samples soaped in HCl solution,the mechanical properties of samples exposed to H2S solution significantly deteriorated,in which the new groups of C(=O)-NH2,C-S-C and C=S emerged.The mechanism of C=S and C-S-C formation was speculated,except for that of the formation of group C(=O)-NH2,which was widely discussed in acidic condition such as HC1 solution.The formation of C-S-C was due to radical reaction initiated by mercapto radical and that of C=S was due to nucleophilic reaction initiated by mercapto cations.This finding is helpful to understanding the seal failure of HNBR in working environment containing H2S.

  12. Harmonic lasing in X-ray FELs

    Energy Technology Data Exchange (ETDEWEB)

    Schneidmiller, E.A.; Yurkov, M.V.

    2012-05-15

    Harmonic lasing in a free electron laser with a planar undulator (under the condition that the fundamental frequency is suppressed) might be a cheap and efficient way of extension of wavelength ranges of existing and planned X-ray FEL facilities. Contrary to nonlinear harmonic generation, harmonic lasing can provide much more intense, stable, and narrow-band FEL beam which is easier to handle due to the suppressed fundamental frequency. In this paper we perform a parametrization of the solution of the eigenvalue equation for lasing at odd harmonics, and present an explicit expression for FEL gain length, taking into account all essential effects. We propose and discuss methods for suppression of the fundamental harmonic. We also suggest a combined use of harmonic lasing and lasing at the retuned fundamental wavelength in order to reduce bandwidth and to increase brilliance of X-ray beam at saturation. Considering 3rd harmonic lasing as a practical example, we come to the conclusion that it is much more robust than usually thought, and can be widely used in the existing or planned X-ray FEL facilities. In particular, LCLS after a minor modification can lase to saturation at the 3rd harmonic up to the photon energy of 25-30 keV providing multi-gigawatt power level and narrow bandwidth. As for the European XFEL, harmonic lasing would allow to extend operating range (ultimately up to 100 keV), to reduce FEL bandwidth and to increase brilliance, to enable two-color operation for pump-probe experiments, and to provide more flexible operation at different electron energies. Similar improvements can be realized in other X-ray FEL facilities with gap-tunable undulators like FLASH II, SACLA, LCLS II, etc. Harmonic lasing can be an attractive option for compact X-ray FELs (driven by electron beams with a relatively low energy), allowing the use of the standard undulator technology instead of small-gap in-vacuum devices. Finally, in this paper we discover that in a part of the

  13. Synchrotron Small-Angle X-ray Scattering Study of Cross-Linked Polymeric Micelles.

    Science.gov (United States)

    Kim, Hyun-Chul; Jin, Kyeong Sik; Lee, Se Guen; Kim, Eunjoo; Lee, Sung Jun; Jeong, Sang Won; Lee, Seung Woo; Kim, Kwang-Woo

    2016-06-01

    Polymeric micelles of methoxypoly(ethylene glycol)-b-poly(lactide) containing lysine units (mPEG-PLA-Lys4) were cross-linked by reacting of lysine moieties with a bifunctional bis(N-hydroxy-succinimide ester). The micelles were characterized in aqueous solution using dynamic light scattering, transmission electron microscopy, and synchrotron small-angle X-ray scattering. The mPEG-PLA-Lys4 was synthesized through the ring-opening polymerization of N6-carbobenzyloxy-L-lysine N-carboxyanhydride with amine-terminated mPEG-PLA and subsequent deprotection. The polymeric micelles showed enhanced micelle stability after cross-linking, which was confirmed by adding sodium dodecyl sulfate as a destabilizing agent. The average diameters measured via dynamic light scattering were 19.1 nm and 29.2 nm for non-cross-linked polymeric micelles (NCPMs) and cross-linked polymeric micelles (CPMs), respectively. The transmission electron microscopy images showed that the size of the polymeric micelles increased slightly due to cross-linking, which was in good agreement with the DLS measurements. The overall structures and internal structural changes of NCPMs and CPMs in aqueous solution were studied in detail using synchrotron X-ray scattering method. According to the structural parameters of X-ray scattering analysis, CPMs with a more densely packed core structure were formed by reacting bifunctional cross-linking agents with lysine amino groups located in the innermost core of the polymeric micelles. PMID:27427731

  14. Ozone oxidation of cassava starch in aqueous solution at different pH.

    Science.gov (United States)

    Klein, Bruna; Vanier, Nathan Levien; Moomand, Khalid; Pinto, Vânia Zanella; Colussi, Rosana; da Rosa Zavareze, Elessandra; Dias, Alvaro Renato Guerra

    2014-07-15

    Ozone is a more powerful oxidant than common oxidising agents, such as sodium hypochlorite and hydrogen peroxide. It is considered as a safer starch modification method for both consumers and the environment. However, few studies have investigated the changes in starch properties associated with ozone treatment, particularly when applied in aqueous solution. This work aimed to evaluate the carbonyl and carboxyl contents, the X-ray diffraction patterns, the spectrum profiles of Fourier transform infrared spectroscopy, the pasting properties and the surface morphology of ozone-oxidised cassava starch during 60 min under different pH (3.5, 6.5 and 9.5) at 25°C. The pH 6.5 and 9.5 seemed to favour the cross-linking between the depolymerised starch molecules during ozonation. The pH 3.5 was more effective in reducing the peak viscosity, breakdown, setback and final viscosity of cassava starch during ozonation in aqueous solution. No differences in the granule surface morphology were observed in the ozone-treated cassava starches compared to native starch.

  15. Corrosion behaviour of galvanized steel and electroplating steel in aqueous solution: AC impedance study and XPS

    Energy Technology Data Exchange (ETDEWEB)

    Lebrini, M.; Fontaine, G. [Laboratoire des Procedes d' Elaboration des Revetements Fonctionnels, LSPES UMR CNRS 8008, ENSCL, BP 90108, F-59652 Villeneuve d' Ascq Cedex (France); Gengembre, L. [Unite de Catalyse et Chimie du solide UMR 8181 Bat C3, USTL, F-59655 Villeneuve d' Ascq Cedex (France); Traisnel, M. [Laboratoire des Procedes d' Elaboration des Revetements Fonctionnels, LSPES UMR CNRS 8008, ENSCL, BP 90108, F-59652 Villeneuve d' Ascq Cedex (France)], E-mail: Michel.Traisnel@ensc-lille.fr; Lerasle, O.; Genet, N. [TOTAL France, Centre de Recherche de Solaize, Chemin du canal, BP 22, F-69360 Solaize (France)

    2008-08-30

    The efficiency of a new triazole derivative, namely, 2-{l_brace}(2-hydroxyethyl)[(4-methyl-1H-1,2,3-benzotriazol-1-yl)methyl]amino{r_brace} ethanol (TTA) has been studied for corrosion inhibition of galvanized steel and electroplating steel in aqueous solution. Corrosion inhibition was studied using electrochemical impedance spectroscopy (EIS). These studies have shown that TTA was a very good inhibitor. Data obtained from EIS show a frequency distribution and therefore a modelling element with frequency dispersion behaviour, a constant phase element (CPE) has been used. The corrosion behaviour of galvanized steel and electroplating steel in aqueous solution was also investigated in the presence of 4-methyl-1H-benzotriazole (TTA unsubstituted) by EIS. These studies have shown that the ability of the molecule to adsorb on the steel surface was dependent on the group in triazole ring substituent. X-ray photoelectron spectroscopy surface analysis with TTA shows that it chemisorbed on surface of galvanized steel and electroplating steel.

  16. Adsorption of Pb(2+) from aqueous solution using spinel ferrite prepared from steel pickling sludge.

    Science.gov (United States)

    Fang, Binbin; Yan, Yubo; Yang, Yang; Wang, Fenglian; Chu, Zhen; Sun, Xiuyun; Li, Jiansheng; Wang, Lianjun

    2016-01-01

    In this paper, spinel ferrite with high crystallinity and high saturation magnetization was successfully prepared from steel pickling sludge by adding iron source and precipitator in the hydrothermal condition. The obtained spinel ferrite was characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), vibrating sample magnetometer (VSM), and Zeta potential methods and investigated as an adsorbent for removal of Pb(2+) from aqueous solution. Batch experiments were performed by varying the pH values, contact time, temperature and initial metal concentration. The result of pH impact showed that the adsorption of Pb(2+) was a pH dependent process, and the pH 5.8 ± 0.2 was found to be the optimum condition. The achieved experimental data were analyzed with various kinetic and isotherm models. The kinetic studies revealed that Pb(2+) adsorption onto spinel ferrite followed a pseudo-second order model, and the Langmuir isotherm model provided the perfect fit to the equilibrium experimental data. At different temperatures, the maximum Pb(2+) adsorption capacities calculated from the Langmuir equation were in the range of 126.5-175.4 mg/g, which can be in competition with other adsorbents. The thermodynamic results showed that the spinel ferrite could spontaneously and endothermically adsorb Pb(2+) from aqueous solution. The regeneration studies showed that spinel ferrite could be used five times (removal efficiency (%) >90%) by desorption with HNO3 reagent.

  17. Flow Instability of Soft Gels from Pluronic F108 Aqueous Solution Under Steady Shear

    Science.gov (United States)

    Park, Hanjin; Jung, Gyoo Yeol; Ryu, Chang Yeol

    2012-02-01

    Nonionic surfactants of Pluronic tri-block copolymers have received special interest during the past decades because of the temperature dependent self-assembly characteristics that would lead to the formation of hydrogels upon heating. Here, we investigate the gelation behavior of Pluronic F108, (PEO)132-(PPO)50-(PEO)132, aqueous solution with an aim to elucidate how the shear affects the thermo-reversible transitions between micellar liquids and hydrogels. Specifically, we have studied the rheological characteristics of soft gels as an intermediate state between liquid to hard gels. From steady shear experiments, we found that there exists a shear rate window, where the flow instability of soft gels is observed. On the contrary, non-Newtonian behaviors following power-law are still observed at the shear rates above and below the shear rate window showing the flow instability. Small angle x-ray scattering and dynamic light scattering experiments had been performed to reveal how the temperature dependent rheological behavior correlates with the structural changes in the micellar aqueous solutions of F108.

  18. Hydrothermal synthesis of silico-manganese nanohybrid for Cu(II) adsorption from aqueous solution

    Science.gov (United States)

    Zhu, Qiufeng; Wang, Liting; An, Zehuan; Ye, Hong; Feng, Xudong

    2016-05-01

    A novel silico-manganese nanohybrid adsorbent (SMNA) was synthesized by a facile hydrothermal method, and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), nitrogen adsorption-desorption, Fourier transform infrared spectroscopy (FT-IR) and zeta potential measurement. The adsorption of Cu(II) ions from aqueous solution on the SMNA was investigated with variations in contact time, pH and initial Cu(II) concentration. The results showed that hydrothermal method would generate nanowire/nanorod incomplete crystallite (δ-MnO2) adsorbent. The adsorption of Cu(II) onto SMNA increased sharply within 25 min and reached equilibrium gradually. The maximum adsorption capacities of SMNA for Cu(II) were ∼40-88 mg g-1, which was lower than δ-MnO2 (92.42 mg g-1) but had a lower pH dependency. As compared with δ-MnO2, higher adsorption capacities of SMNA (7.5-15 wt% of silica doping amount) for Cu(II) could be observed when pH of the aqueous solution was low (removal of Cu(II) by the as-prepared adsorbents was dominated by migration of Cu(II). The possibility of Cu(II) recovery was also investigated and it revealed that SMNA was a promising recyclable adsorbent for removal of heavy metal ions in water and wastewater treatment.

  19. Adsorption of Pb(2+) from aqueous solution using spinel ferrite prepared from steel pickling sludge.

    Science.gov (United States)

    Fang, Binbin; Yan, Yubo; Yang, Yang; Wang, Fenglian; Chu, Zhen; Sun, Xiuyun; Li, Jiansheng; Wang, Lianjun

    2016-01-01

    In this paper, spinel ferrite with high crystallinity and high saturation magnetization was successfully prepared from steel pickling sludge by adding iron source and precipitator in the hydrothermal condition. The obtained spinel ferrite was characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), vibrating sample magnetometer (VSM), and Zeta potential methods and investigated as an adsorbent for removal of Pb(2+) from aqueous solution. Batch experiments were performed by varying the pH values, contact time, temperature and initial metal concentration. The result of pH impact showed that the adsorption of Pb(2+) was a pH dependent process, and the pH 5.8 ± 0.2 was found to be the optimum condition. The achieved experimental data were analyzed with various kinetic and isotherm models. The kinetic studies revealed that Pb(2+) adsorption onto spinel ferrite followed a pseudo-second order model, and the Langmuir isotherm model provided the perfect fit to the equilibrium experimental data. At different temperatures, the maximum Pb(2+) adsorption capacities calculated from the Langmuir equation were in the range of 126.5-175.4 mg/g, which can be in competition with other adsorbents. The thermodynamic results showed that the spinel ferrite could spontaneously and endothermically adsorb Pb(2+) from aqueous solution. The regeneration studies showed that spinel ferrite could be used five times (removal efficiency (%) >90%) by desorption with HNO3 reagent. PMID:26942534

  20. Removal of Zinc from Aqueous Solutions by Magnetite Silica Core-Shell Nanoparticles

    Directory of Open Access Journals (Sweden)

    Masoomeh Emadi

    2013-01-01

    Full Text Available Magnetite silica core-shell nanoparticles (Fe3O4-SiO2 were synthesized and evaluated as a nanoadsorbent for removing Zn(II from aqueous solutions. The core-shell nanoparticles were prepared by combining coprecipitation and sol-gel methods. Nanoparticles were characterized by X-ray diffraction, transmission electron microscopy (TEM, and FT-IR. The magnetization values of nanoparticles were measured with vibrating sample magnetometer (VSM. The adsorption of Zn(II ions was examined by batch equilibrium technique. The effects of pH, initial Zn(II concentration, and contact time on the efficiency of Zn(II removal were studied. The equilibrium data, analyzed by using Langmuir and Freundlich isotherm models, showed better agreement with the former model. Using the Langmuir isotherm model, maximum capacity of the nanoadsorbent for Zn(II was found to be 119 mg g−1 at room temperature. Kinetic studies were conducted and the resulting data were analyzed using first- and second-order equations; pseudo-second-order kinetic equation was found to provide the best correlation. The adsorption and sedimentation times were very low. The nanoadsorbent can be easily separated from aqueous solution by a magnet. Repeated adsorption acid regeneration cycles were performed to examine the stability and reusability of the nanoadsorbent. The result of this study proved high stability and reusability of Fe3O4-SiO2 as an adsorbent for Zn(II ions.

  1. Alkaline deoxygenated graphene oxide as adsorbent for cadmium ions removal from aqueous solutions.

    Science.gov (United States)

    Liu, Jun; Du, Hongyan; Yuan, Shaowei; He, Wanxia; Yan, Pengju; Liu, Zhanhong

    2015-01-01

    Alkaline deoxygenated graphene oxide (aGO) was prepared through alkaline hydrothermal treatment and used as adsorbent to remove Cd(II) ions from aqueous solutions for the first time. The characterization results of transmission electron microscopy, X-ray diffraction, Raman spectroscopy, and Fourier transform infrared (FT-IR) spectra indicate that aGO was successfully synthesized. The batch adsorption experiments showed that the adsorption kinetics could be described by the pseudo-second-order kinetic model, and the isotherms equilibrium data were well fitted with the Langmuir model. The maximum adsorption capacity of Cd(II) on aGO was 156 mg/g at pH 5 and T=293 K. The adsorption thermodynamic parameters indicated that the adsorption process was a spontaneous and endothermic reaction. The mainly adsorption mechanism speculated from FT-IR results may be attributed to the electrostatic attraction between Cd2+ and negatively charged groups (-CO-) of aGO and cation-π interaction between Cd2+ and the graphene planes. The findings of this study demonstrate the potential utility of the nanomaterial aGO as an effective adsorbent for Cd(II) removal from aqueous solutions. PMID:26038925

  2. Aqueous systems and geothermal energy

    International Nuclear Information System (INIS)

    Significant unpublished results reported include: osmotic coefficients of KCl solutions vs. molality at 109 to 2010C; cadmium ion diffusivities in CaCl2 hydrous melts; a x-ray diffraction study of the uranyl complex in water; solubility of amorphous silica in aqueous NaNO3 solutions at 100 to 3000C; and corrosion of carbon steel by geothermal brine

  3. GENFIT: software for the analysis of small-angle X-ray and neutron scattering data of macro­molecules in solution

    Science.gov (United States)

    Spinozzi, Francesco; Ferrero, Claudio; Ortore, Maria Grazia; De Maria Antolinos, Alejandro; Mariani, Paolo

    2014-01-01

    Many research topics in the fields of condensed matter and the life sciences are based on small-angle X-ray and neutron scattering techniques. With the current rapid progress in source brilliance and detector technology, high data fluxes of ever-increasing quality are produced. In order to exploit such a huge quantity of data and richness of information, wider and more sophisticated approaches to data analysis are needed. Presented here is GENFIT, a new software tool able to fit small-angle scattering data of randomly oriented macromolecular or nanosized systems according to a wide list of models, including form and structure factors. Batches of curves can be analysed simultaneously in terms of common fitting parameters or by expressing the model parameters via physical or phenomenological link functions. The models can also be combined, enabling the user to describe complex heterogeneous systems. PMID:24904247

  4. GENFIT: software for the analysis of small-angle X-ray and neutron scattering data of macro-molecules in solution.

    Science.gov (United States)

    Spinozzi, Francesco; Ferrero, Claudio; Ortore, Maria Grazia; De Maria Antolinos, Alejandro; Mariani, Paolo

    2014-06-01

    Many research topics in the fields of condensed matter and the life sciences are based on small-angle X-ray and neutron scattering techniques. With the current rapid progress in source brilliance and detector technology, high data fluxes of ever-increasing quality are produced. In order to exploit such a huge quantity of data and richness of information, wider and more sophisticated approaches to data analysis are needed. Presented here is GENFIT, a new software tool able to fit small-angle scattering data of randomly oriented macromolecular or nanosized systems according to a wide list of models, including form and structure factors. Batches of curves can be analysed simultaneously in terms of common fitting parameters or by expressing the model parameters via physical or phenomenological link functions. The models can also be combined, enabling the user to describe complex heterogeneous systems.

  5. Center for X-Ray Optics, 1992

    International Nuclear Information System (INIS)

    This report discusses the following topics: Center for X-Ray Optics; Soft X-Ray Imaging wit Zone Plate Lenses; Biological X-Ray microscopy; Extreme Ultraviolet Lithography for Nanoelectronic Pattern Transfer; Multilayer Reflective Optics; EUV/Soft X-ray Reflectometer; Photoemission Microscopy with Reflective Optics; Spectroscopy with Soft X-Rays; Hard X-Ray Microprobe; Coronary Angiography; and Atomic Scattering Factors

  6. Nanoscale lubricating film formation by linear polymer in aqueous solution

    Science.gov (United States)

    Liu, Shuhai; Guo, Dan; Xie, Guoxin

    2012-11-01

    Film-forming properties of polymer in aqueous solution flowing through a nanogap have been investigated by using a thin film interferometry. The film properties of linear polymer in aqueous solution flowing through a confined nanogap depend on the ratio of water film thickness to averaged radius of polymer chains H0/RPolymer. It was found that the lubrication film thickness of linear polymer in aqueous solution decreases as the polymer molecular weight increasing when H0/RPolymer < 2 ˜ 3. A new lubrication map was proposed, which includes the lubrication regime of weak confinement influence, the lubrication regime of strong confinement influence (LRSCI), and the transition regime of confinement influence. It is very difficult to increase the lubrication film thickness using the higher molecule weight in the LRSCI regime. The lubrication mechanism inferred from our experimental results may help to better understand the dynamic film properties of linear polymer in aqueous solution flowing through a nanogap.

  7. Neutron and X-ray Detectors

    Energy Technology Data Exchange (ETDEWEB)

    Carini, Gabriella [SLAC National Accelerator Lab., Menlo Park, CA (United States); Denes, Peter [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Gruener, Sol [Cornell Univ., Ithaca, NY (United States); Lessner, Elianne [Dept. of Energy (DOE), Washington DC (United States). Office of Science Office of Basic Energy Sciences

    2012-08-01

    (and two computing hurdles that result from the corresponding increase in data volume) for the detector community to overcome in order to realize the full potential of BES neutron and X-ray facilities. Resolving these detector impediments will improve scientific productivity both by enabling new types of experiments, which will expand the scientific breadth at the X-ray and neutron facilities, and by potentially reducing the beam time required for a given experiment. These research priorities are summarized in the table below. Note that multiple, simultaneous detector improvements are often required to take full advantage of brighter sources. High-efficiency hard X-ray sensors: The fraction of incident particles that are actually detected defines detector efficiency. Silicon, the most common direct-detection X-ray sensor material, is (for typical sensor thicknesses) 100% efficient at 8 keV, 25%efficient at 20 keV, and only 3% efficient at 50 keV. Other materials are needed for hard X-rays. Replacement for 3He for neutron detectors: 3He has long been the neutron detection medium of choice because of its high cross section over a wide neutron energy range for the reaction 3He + n —> 3H + 1H + 0.764 MeV. 3He stockpiles are rapidly dwindling, and what is available can be had only at prohibitively high prices. Doped scintillators hold promise as ways to capture neutrons and convert them into light, although work is needed on brighter, more efficient scintillator solutions. Neutron detectors also require advances in speed and resolution. Fast-framing X-ray detectors: Today’s brighter X-ray sources make time-resolved studies possible. For example, hybrid X-ray pixel detectors, initially developed for particle physics, are becoming fairly mature X-ray detectors, with considerable development in Europe. To truly enable time-resolved studies, higher frame rates and dynamic range are required, and smaller pixel sizes are desirable. High-speed spectroscopic X-ray detectors

  8. Surface tension and related thermodynamic quantities of aqueous electrolyte solutions

    CERN Document Server

    Matubayasi, Norihiro

    2013-01-01

    Surface tension provides a thermodynamic avenue for analyzing systems in equilibrium and formulating phenomenological explanations for the behavior of constituent molecules in the surface region. While there are extensive experimental observations and established ideas regarding desorption of ions from the surfaces of aqueous salt solutions, a more successful discussion of the theory has recently emerged, which allows the quantitative calculation of the distribution of ions in the surface region. Surface Tension and Related Thermodynamic Quantities of Aqueous Electrolyte Solutions provides a d

  9. Biosorption of copper (II) ions from synthetic aqueous solutions by drying bed activated sludge

    Energy Technology Data Exchange (ETDEWEB)

    Benaissa, H., E-mail: ho_benaissa@yahoo.fr [Laboratory of Sorbent Materials and Water Treatment, Department of Chemistry, Faculty of Sciences, University of Tlemcen, P.O. Box 119, 13000 Tlemcen (Algeria); Elouchdi, M.A. [Laboratory of Sorbent Materials and Water Treatment, Department of Chemistry, Faculty of Sciences, University of Tlemcen, P.O. Box 119, 13000 Tlemcen (Algeria)

    2011-10-30

    Highlights: {yields} Dried activated sludge has been investigated for the removal of copper ions from aqueous synthetic solutions, in batch conditions. {yields} Copper uptake was time contact, initial copper concentration, initial pH solution and copper salt type dependent. {yields} Maximum copper uptake obtained was q{sub m} = 62.50 mg/g (0.556 mmol/g) under the investigated experimental conditions. - Abstract: In the present work, the usefulness of dried activated sludge has been investigated for the removal of copper ions from synthetic aqueous solutions. Kinetic data and equilibrium sorption isotherm were measured in batch conditions. The influence of some parameters such as: contact time, initial copper concentration, initial pH of solution and copper salt nature on copper biosorption kinetics has been studied. Copper uptake was time contact, initial copper concentration, initial pH solution and copper salt type dependent. Maximum copper sorption was found to occur at initial pH 5. Two simplified kinetic models including a first-order rate equation and a pseudo second-order rate equation were selected to describe the biosorption kinetics. The process followed a pseudo second-order rate kinetics. The process mechanism was found to be complex, consisting of external mass transfer and intraparticle mass transfer diffusion. Copper biosorption process was particle-diffusion-controlled, with some predominance of some external mass transfer at the initial stages for the different experimental parameters studied. Langmuir and Freundlich models were used to describe sorption equilibrium data at natural pH of solution. Results indicated that the Langmuir model gave a better fit to the experimental data than the Freundlich model. Maximum copper uptake obtained was q{sub m} = 62.50 mg/g (0.556 mmol/g) under the investigated experimental conditions. Scanning electron microscopy coupled with X-ray energy dispersed analysis for copper-equilibrated dried activated sludge

  10. Adsorption of Benzoic Acid in Aqueous Solution by Bagasse Fly Ash

    Science.gov (United States)

    Suresh, S.

    2012-09-01

    This paper reports the studies on the benzoic acid (BA) onto bagasse fly ash (BFA) was studied in aqueous solution in a batch system. Physico-chemical properties including surface area, surface texture of the GAC before and after BA adsorption onto BFA were analysed using X-ray diffractometer (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX). The optimum initial pH for the adsorption of BA was found to be 5.56. The adsorbent dose was 10 g/l for BFA and the equilibrium time 8 h of reaction. Pseudo first and second order models were used to find the adsorption kinetics. It was found that intraparticle diffusion played important role in the adsorption mechanisms of BA and the adsorption kinetics followed pseudo-second order kinetic model rather than the pseudo first order kinetic model. Isotherm data were generated for BA solution having initial concentrations of BA in the range of 10-200 mg/l for the BFA dosage of 10 g/l at temperatures of 288, 303, and 318 K. The adsorption of BA onto BFA was favorably influenced by an increase in temperature. Equilibrium data were well represented by the Redlich-Peterson isotherm model. Values of the change in entropy ( ΔS 0), heat of adsorption ( ΔH 0) for adsorption of BA on BFA was found to be 120.10 and 19.61 kJ/mol respectively. The adsorption of BA onto BFA was an endothermic reaction. Desorption of BA from BFA was studied by various solvents method. Acetic acid was found to be a better eluant for desorption of BA with a maximum desorption efficiency of 55.2 %. Owing to its heating value, spent BFA can be used as a co-fuel for the production of heat in boiler furnaces.

  11. Magnetic composite nanofibers fabricated by electrospinning of Fe3O4/gelatin aqueous solutions

    International Nuclear Information System (INIS)

    Graphical abstract: Superparamagnetic Fe3O4/GE composite nanofibers with saturation magnetization of 12.87 emμ g−1 were prepared from gelatin aqueous solution at an elevated temperature by electrospinning. - Highlights: • Electrospinning GE aqueous solution at higher temperature. • Presenting a simple and effective technique, combining wet blending with high temperature electrospinning to prepare magnetic composite nanofibers. • Developing composite nanofibers with higher superparamagnetic properties is expected to be useful in application for the biomedical field. - Abstract: We have fabricated magnetic composite nanofibers containing superparamagnetic Fe3O4 nanoparticles by the electrospinning method. Highly dispersed Fe3O4 magnetic nanoparticles were synthesized by one-step co-precipitation of Fe2+/Fe3+ under an alkaline condition with 4 wt% poly(vinyl alcohol) (PVA) aqueous solution as the stabilizer. Gelatin (GE) was used as a polymeric matrix for fabricating the nanocomposites. The prepared Fe3O4/GE composite nanofibers were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD), respectively. These composite nanofibers show uniform and continuous morphology with the Fe3O4 nanoparticles embedded in the nanofibers. By studying the magnetic properties of the Fe3O4/GE composite nanofibers, we confirm that the composite nanofibers possess superparamagnetic properties with a high saturated magnetization (Ms = 12.87 emμ g−1) at room temperature. The features of this approach for getting one-dimensional magnetic nanostructure are its simplicity, effectiveness and safety. The Fe3O4/GE nanofibers with superparamagnetic properties would be potentially applied in biomedical field

  12. X-ray Echo Spectroscopy

    Science.gov (United States)

    Shvyd'ko, Yuri

    2016-02-01

    X-ray echo spectroscopy, a counterpart of neutron spin echo, is being introduced here to overcome limitations in spectral resolution and weak signals of the traditional inelastic x-ray scattering (IXS) probes. An image of a pointlike x-ray source is defocused by a dispersing system comprised of asymmetrically cut specially arranged Bragg diffracting crystals. The defocused image is refocused into a point (echo) in a time-reversal dispersing system. If the defocused beam is inelastically scattered from a sample, the echo signal acquires a spatial distribution, which is a map of the inelastic scattering spectrum. The spectral resolution of the echo spectroscopy does not rely on the monochromaticity of the x rays, ensuring strong signals along with a very high spectral resolution. Particular schemes of x-ray echo spectrometers for 0.1-0.02 meV ultrahigh-resolution IXS applications (resolving power >108 ) with broadband ≃5 - 13 meV dispersing systems are introduced featuring more than 103 signal enhancement. The technique is general, applicable in different photon frequency domains.

  13. X-ray echo spectroscopy

    CERN Document Server

    Shvyd'ko, Yuri

    2015-01-01

    X-ray echo spectroscopy, a counterpart of neutron spin-echo, is being introduced here to overcome limitations in spectral resolution and weak signals of the traditional inelastic x-ray scattering (IXS) probes. An image of a point-like x-ray source is defocused by a dispersing system comprised of asymmetrically cut specially arranged Bragg diffracting crystals. The defocused image is refocused into a point (echo) in a time-reversal dispersing system. If the defocused beam is inelastically scattered from a sample, the echo signal acquires a spatial distribution, which is a map of the inelastic scattering spectrum. The spectral resolution of the echo spectroscopy does not rely on the monochromaticity of the x-rays, ensuring strong signals along with a very high spectral resolution. Particular schemes of x-ray echo spectrometers for 0.1--0.02-meV ultra-high-resolution IXS applications (resolving power $> 10^8$) with broadband $\\simeq$~5--13~meV dispersing systems are introduced featuring more than $10^3$ signal e...

  14. X-ray Echo Spectroscopy.

    Science.gov (United States)

    Shvyd'ko, Yuri

    2016-02-26

    X-ray echo spectroscopy, a counterpart of neutron spin echo, is being introduced here to overcome limitations in spectral resolution and weak signals of the traditional inelastic x-ray scattering (IXS) probes. An image of a pointlike x-ray source is defocused by a dispersing system comprised of asymmetrically cut specially arranged Bragg diffracting crystals. The defocused image is refocused into a point (echo) in a time-reversal dispersing system. If the defocused beam is inelastically scattered from a sample, the echo signal acquires a spatial distribution, which is a map of the inelastic scattering spectrum. The spectral resolution of the echo spectroscopy does not rely on the monochromaticity of the x rays, ensuring strong signals along with a very high spectral resolution. Particular schemes of x-ray echo spectrometers for 0.1-0.02 meV ultrahigh-resolution IXS applications (resolving power >10^{8}) with broadband ≃5-13  meV dispersing systems are introduced featuring more than 10^{3} signal enhancement. The technique is general, applicable in different photon frequency domains.

  15. Crowding and Anomalous Capacitance at an Electrode–Ionic Liquid Interface Observed Using Operando X-ray Scattering

    OpenAIRE

    Chu, Miaoqi; Miller, Mitchell; Dutta, Pulak

    2016-01-01

    Room temperature ionic liquids are widely recognized as novel electrolytes with properties very different from those of aqueous solutions, and thus with many potential applications, but observing how they actually behave at electrolytic interfaces has proved to be challenging. We have studied the voltage-dependent structure of [TDTHP]+[NTF2]− near its interface with an electrode, using in situ synchrotron X-ray reflectivity. An anion-rich layer develops at the interface above a threshold volt...

  16. Small angle X-ray scattering and transmission electron microscopy study of the Lactobacillus brevis S-layer protein

    Energy Technology Data Exchange (ETDEWEB)

    Jaeaeskelaeinen, Pentti [Department of Biomedical Engineering and Computational Science, PO Box 2200, FI-02015 Aalto University School of Science and Technology (Finland); Engelhardt, Peter [Haartman Institute, Department of Pathology, PO Box 21, FIN-00014 University of Helsinki (Finland); Hynoenen, Ulla; Palva, Airi [Department of Basic Veterinary Sciences, Division of Microbiology, FIN-00014 University of Helsinki (Finland); Torkkeli, Mika; Serimaa, Ritva, E-mail: ritva.serimaa@helsinki.f [Department of Physics, POB 64, 00014 University of Helsinki (Finland)

    2010-10-01

    The structure of self-assembly domain containing recombinant truncation mutants of Lactobacillus brevis surface layer protein SlpA in aqueous solution was studied using small-angle X-ray scattering and transmission electron microscopy. The proteins were found out to interact with each other forming stable globular oligomers of about 10 monomers. The maximum diameter of the oligomers varied between 75 A and 435 A.

  17. Small angle X-ray scattering and transmission electron microscopy study of the Lactobacillus brevis S-layer protein

    Science.gov (United States)

    Jääskeläinen, Pentti; Engelhardt, Peter; Hynönen, Ulla; Torkkeli, Mika; Palva, Airi; Serimaa, Ritva

    2010-10-01

    The structure of self-assembly domain containing recombinant truncation mutants of Lactobacillus brevis surface layer protein SlpA in aqueous solution was studied using small-angle X-ray scattering and transmission electron microscopy. The proteins were found out to interact with each other forming stable globular oligomers of about 10 monomers. The maximum diameter of the oligomers varied between 75 Å and 435 Å.

  18. Adsorption of sulphuric acid on smectite from acidic aqueous solutions Adsorção de ácido sulfúrico em esmectita de soluções aquosas ácidas

    OpenAIRE

    E. L. Tavani; C. Volzone

    1999-01-01

    The adsorption of sulphuric acid on smectite from acidic aqueous solutions was studied. The amounts of cations dissolved in each equilibrium solution were determined by chemical analysis. Simultaneously, the original smectite and the smectite after each test were characterized by infrared, X-ray diffraction and swelling index. The results obtained permitted us to determine that the substitutions of the exchange cations and the chemical attack occurred at very different acid concentrations and...

  19. Elimination of radical on the x-ray irradiated hydroxyapatite compounds

    Energy Technology Data Exchange (ETDEWEB)

    Ohta, M.; Yasuda, M.; Miyazawa, C.; Okamura, H.; Suzuki, Y. [Niigata Univ., Niigata, (Japan)

    2002-07-01

    We investigate the elimination of radical produced in a human tooth and synthetic calcium-deficient hydroxyapatite compounds after X-ray irradiation. Used samples were enamel and dentine of a human tooth and synthetic calcium-deficient hydroxyapatite (DAp), and stoichiometric hydroxyapatite (HAp). The ESR signal intensities at nearly g = 2 in the samples after X-ray irradiation were proportional to the absorbed dose in the range from 6 to 39 Gy. And these ESR signal intensities of the samples soaked in various ion containing fluids decreased with soaking time. Especially, the decrease in these ESR signal intensities was remarkably large in the samples soaked in Na{sub 2}HPO{sub 4} aqueous solution. This fact suggests that the surface layer of the samples easily dissolves in ion containing fluids.

  20. X-ray diffraction analysis of multilayer porous InP(001) structure

    International Nuclear Information System (INIS)

    Multilayer structures composed of four porous bilayers have been studied by high-resolution X-ray diffraction using synchrotron radiation, and the photoluminescence of these structures has been investigated at 4 K. The porous structures were formed by anodic oxidation of InP(001) substrates in aqueous HCl solution. The structural parameters of the sublayers were varied by changing the electrochemical etching mode (potentiostatic/galvanostatic). The X-ray scattering intensity maps near the InP 004 reflection are obtained. A model for scattering from such systems is proposed based on the statistical dynamical diffraction theory. Theoretical scattering maps have been fitted to the experimental ones. It is shown that a mathematical analysis of the scattering intensity maps makes it possible to determine the structural parameters of sublayers. The reconstructed parameters (thickness, strain, and porosity of sublayers and the shape and arrangement of pores) are in satisfactory agreement with the scanning electron microscopy data.

  1. SOMO (SOlution MOdeler) differences between X-Ray- and NMR-derived bead models suggest a role for side chain flexibility in protein hydrodynamics.

    Science.gov (United States)

    Rai, Nithin; Nöllmann, Marcelo; Spotorno, Bruno; Tassara, Giovanni; Byron, Olwyn; Rocco, Mattia

    2005-05-01

    Reduced numbers of frictional/scattering centers are essential for tractable hydrodynamic and small-angle scattering data modeling. We present a method for generating medium-resolution models from the atomic coordinates of proteins, basically by using two nonoverlapping spheres of differing radii per residue. The computed rigid-body hydrodynamic parameters of BPTI, RNase A, and lysozyme models were compared with a large database of critically assessed experimental values. Overall, very good results were obtained, but significant discrepancies between X-ray- and NMR-derived models were found. Interestingly, they could be accounted for by properly considering the extent to which highly mobile surface side chains differently affect translational/rotational properties. Models of larger structures, such as fibrinogen fragment D and citrate synthase, also produced consistent results. Foremost among this method's potential applications is the overall conformation and dynamics of modular/multidomain proteins and of supramolecular complexes. The possibility of merging data from high- and low-resolution structures greatly expands its scope.

  2. Dental X-ray apparatus

    International Nuclear Information System (INIS)

    Intra-oral X-ray apparatus which reduces the number of exposures necessary to obtain panoramic dental radiographs is described in detail. It comprises an electron gun, a tubular target carrier projecting from the gun along the beam axis and carrying at its distal end a target surrounded by a shield of X-ray opaque material. This shield extends forward and laterally of the target and has surfaces which define a wedge or cone-shaped radiation pattern delimited vertically by the root tips of the patient's teeth. A film holder is located externally of the patient's mouth. A disposable member can fit on the target carrier to depress the patient's tongue out of the radiation pattern and to further shield the roof of the mouth. The electron beam can be magnetically deflected to change the X-ray beam direction. (author)

  3. Phosphole complexes of Gold(I) halides: Comparison of solution and solid-state structures by a combination of solution and CP/MAS 31P NMR spectroscopy and x-ray crystallography

    International Nuclear Information System (INIS)

    A series of complexes of 1-phenyldibenzophosphole (DBP), 1-phenyl-3,4,-dimethylphosphole (DMPP), and triphenylphosphine of the type LnAuX (n = 1, L = DBP, DMPP, Ph3P, X = Cl, Br, I; n = 3, L = DBP, X = Cl, Br, I; n = 3, L = Ph3P, X = Cl; n = 4, L = DBP, DMPP, X = PF6) have been prepared and characterized. The structures of (DBP)AuCl (1), (DBP)3AuCl (2), and (DMPP)AuCl (3) have been determined from three-dimensional x-ray data collected by counter methods. Crystal structure of the complexes is reported. The CP/MAS 31P(1H) NMR spectrum of complex 1 shows two resonances in a 1:1 intensity ratio, and the CP/MAS 31P(1H) NMR spectrum of complex 3 shows three resonances in a 1:1:1 intensity ratio for reasons that are not yet understood. Though the three phospholes are crystallographically inequivalent (d(AuP) = 2.359 (1), 2.382 (1), and 2.374 (2) angstrom) the molecule has effective Cs symmetry as evidenced by the observation of two 31P resonances in a 2:1 intensity ratio in its CP/MAS 31P(1H) NMR spectrum. Variable-temperature 31P(1H) NMR spectra obtained on solutions of LAuCl + L in various ratios were analyzed to determine the nature of the species present in solution and to gain information regarding their relative stabilities as a function of the nature of the phosphine. 79 refs., 8 figs., 9 tabs

  4. Neutron and X-ray Detectors

    Energy Technology Data Exchange (ETDEWEB)

    Carini, Gabriella [SLAC National Accelerator Lab., Menlo Park, CA (United States); Denes, Peter [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Gruener, Sol [Cornell Univ., Ithaca, NY (United States); Lessner, Elianne [Dept. of Energy (DOE), Washington DC (United States). Office of Science Office of Basic Energy Sciences

    2012-08-01

    (and two computing hurdles that result from the corresponding increase in data volume) for the detector community to overcome in order to realize the full potential of BES neutron and X-ray facilities. Resolving these detector impediments will improve scientific productivity both by enabling new types of experiments, which will expand the scientific breadth at the X-ray and neutron facilities, and by potentially reducing the beam time required for a given experiment. These research priorities are summarized in the table below. Note that multiple, simultaneous detector improvements are often required to take full advantage of brighter sources. High-efficiency hard X-ray sensors: The fraction of incident particles that are actually detected defines detector efficiency. Silicon, the most common direct-detection X-ray sensor material, is (for typical sensor thicknesses) 100% efficient at 8 keV, 25%efficient at 20 keV, and only 3% efficient at 50 keV. Other materials are needed for hard X-rays. Replacement for 3He for neutron detectors: 3He has long been the neutron detection medium of choice because of its high cross section over a wide neutron energy range for the reaction 3He + n —> 3H + 1H + 0.764 MeV. 3He stockpiles are rapidly dwindling, and what is available can be had only at prohibitively high prices. Doped scintillators hold promise as ways to capture neutrons and convert them into light, although work is needed on brighter, more efficient scintillator solutions. Neutron detectors also require advances in speed and resolution. Fast-framing X-ray detectors: Today’s brighter X-ray sources make time-resolved studies possible. For example, hybrid X-ray pixel detectors, initially developed for particle physics, are becoming fairly mature X-ray detectors, with considerable development in Europe. To truly enable time-resolved studies, higher frame rates and dynamic range are required, and smaller pixel sizes are desirable. High-speed spectroscopic X-ray detectors

  5. The Million Optical - Radio/X-ray Associations (MORX) Catalogue

    CERN Document Server

    Flesch, Eric W

    2016-01-01

    This automated catalogue combines all the largest published optical, radio and X-ray sky catalogues to find probable radio/X-ray associations to optical objects, plus double radio lobes, using uniform processing against all input data. The total count is 1002855 optical objects so presented. Each object is displayed with J2000 astrometry, optical and radio/X-ray identifiers, red and blue photometry, and calculated probabilities and optical field solutions of the associations. This is the third and final edition of this method.

  6. X-ray imaging: Perovskites target X-ray detection

    Science.gov (United States)

    Heiss, Wolfgang; Brabec, Christoph

    2016-05-01

    Single crystals of perovskites are currently of interest to help fathom fundamental physical parameters limiting the performance of perovskite-based polycrystalline solar cells. Now, such perovskites offer a technology platform for optoelectronic devices, such as cheap and sensitive X-ray detectors.

  7. OPTIMISATION OF COPPER AND ZINC IONS REMOVAL FROM AQUEOUS SOLUTION BY COAL FLY ASH AS AN ADSORBENT

    Directory of Open Access Journals (Sweden)

    MOYO ,M

    2012-04-01

    Full Text Available Rapid urbanization and industrialization of our world has led to accumulation of enormous number of contaminants in our environment. Heavy metal ions hold a superlative position in that list and are responsible for contaminating soil, air and water in many parts of the world. Adsorption technology is emerging as a sustainable effective solution. The possibility of using Coal fly ash as an alternative adsorbent for divalent metal ions (Zn2+, Cu2+ removal from simulated solutions was studied. The coal fly ash was characterised by Brunauer Emmet Teller (BET, X-ray diffraction (XRD, X-ray Fluorescence Spectroscopy (XRF and Fourier transforminfrared (FT-IR. Optimum adsorption conditions were determined as a function of pH, adsorbent dosage and contact time for Zn2+ and Cu2+ removal. The adsorption of metal ions was found to be pH dependant.Equilibrium data fitted well to the Freundlich model with R2 values as 0.9932, 0.9971 for Cu2+, Zn2+, respectively. The study showed that disposed coal fly ash could be used as an efficient adsorbent material for the removal of metal ions from aqueous solution.

  8. Combined adsorption and reduction of Cr(VI) from aqueous solution on polyaniline/multiwalled carbon nanotubes composite

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Jiahong; Yin, Xiaolong; Ma, Hongrui [Shannxi University of Science and Technology, Xi' an (China); Tang, Wei [Shaanxi Research Institute of Agricultural Products Processing Technology, Xi' an (China)

    2015-09-15

    Polyaniline/multiwalled carbon nanotube (PANI-MWCNT) was prepared by bounding polyaniline on the surface of oxidized multiwalled carbon nanotube. The structure and surface properties of synthesized composites were characterized by Fourier transformed infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), transmission electron microscope (TEM), and its adsorption capability for aqueous Cr(VI) was also studied. Characterized results showed that polyaniline was successfully anchored on the surface of MWCNT. From adsorption experiments the maximum adsorption amount of Cr(VI) onto PANI-MWCNTs was 28.25, 31.75 and 36.76 mg·g{sup -1} at 15, 25 and 35 .deg. C. Thermodynamic parameters showed that the Cr(VI) adsorption process was endothermic, spontaneous and feasible. Cr(VI) adsorption followed pseudo-second-order kinetics. Cr(VI) adsorption on the adsorbent decreases with increasing solution pH. The presence of anions in solution almost has no effect on Cr(VI) adsorption, indicating good selectivity. XPS analysis confirms that electrostatic interaction, reduction and chelation contribute to enhanced Cr(VI) removal. Cr(VI) loaded absorbent can be readily desorbed in 0.1mol·L{sup -1} of NaOH solution, and the desorption rate was 84.12%.

  9. Removal of heavy metal ions from aqueous solution using red loess as an adsorbent

    Institute of Scientific and Technical Information of China (English)

    Shengtao Xing; Meiqing Zhao; Zichuan Ma

    2011-01-01

    The adsorption behaviors of heavy metals onto novel low-cost adsorbent,red loess,were investigated.Red loess was characterized by X-ray diffraction,scanning electron microscopy and Fourier transform infrared spectra.The results indicated that red loess mainly consisted of silicate,ferric and aluminum oxides.Solution pH,adsorbent dosage,initial metal concentration,contact time and temperature significantly influenced the efficiency of heavy metals removal.The adsorption reached equilibrium at 4 hr,and the experimental equilibrium data were fitted to Langmuir monolayer adsorption model.The adsorption of Cu(Ⅱ) and Zn(Ⅱ) onto red loess was endothermic,while the adsorption of Pb(Ⅱ) was exothermic.The maximum adsorption capacities of red loess for Pb(Ⅱ),Cu(Ⅱ)and Zn(Ⅱ) were estimated to be 113.6,34.2 and 17.5 mg/g,respectively at 25°C and pH 6.The maximum removal efficiencies were 100% for Pb(Ⅱ) at pH 7,100% for Cu(Ⅱ) at pH 8,and 80% for Zn(Ⅱ) at pH 8.The used adsorbents were readily regenerated using dilute HCI solution,indicating that red loess has a high reusability.All the above results demonstrated that red loess could be used as a possible alternative low-cost adsorbent for the removal of heavy metals from aqueous solution.

  10. Removal of Cu2+from Aqueous Solutions Using Na-A Zeolite from Oil Shale Ash

    Institute of Scientific and Technical Information of China (English)

    包维维; 刘璐; 邹海峰; 甘树才; 徐学纯; 季桂娟; 高桂梅; 郑克岩

    2013-01-01

    Na-A zeolite was synthesized using oil shale ash (OSA), which is a solid by-product of oil shale proc-essing. The samples were characterized by various techniques, such as scanning electron microscopy, X-ray diffrac-tion and Brunauer Emmet Teller method. The batch isothermal equilibrium adsorption experiments were performed to evaluate the ability of Na-A zeolite for removal of Cu (II) from aqueous solutions. The effects of operating pa-rameters, such as concentration of copper solutions, adsorbent dosages, pH value of solutions and temperature, on the adsorption efficiency were investigated. The equilibrium adsorption data were fitted with Langmuir and Freundlich models. The maximum adsorption capacity of Na-A zeolite obtained from the Langmuir adsorption iso-therm is 156.7 mg·g−1 of Cu (II). The increase of pH level in the adsorption process suggests that the uptake of heavy metals on the zeolite follows an ion exchange mechanism. The batch kinetic data fit the pseudo-second order equation well. The thermodynamic parameters, such as changes in Gibbs free energy (ΔG), enthalpy (ΔH) and en-tropy (ΔS), are used to predict the nature of the adsorption process. The negativeΔG values at different tempera-tures confirm that the adsorption processes are spontaneous.

  11. Wet etching of InSb surfaces in aqueous solutions: Controlled oxide formation

    Energy Technology Data Exchange (ETDEWEB)

    Aureau, D., E-mail: damien.aureau@chimie.uvsq.fr [Institut Lavoisier UVSQ-CNRS UMR 8180, 45 avenue des Etats Unis, Versailles, 78035 (France); Chaghi, R.; Gerard, I. [Institut Lavoisier UVSQ-CNRS UMR 8180, 45 avenue des Etats Unis, Versailles, 78035 (France); Sik, H.; Fleury, J. [Sagem Defense Sécurité, 72-74, rue de la tour Billy, 95101, Argenteuil Cedex (France); Etcheberry, A. [Institut Lavoisier UVSQ-CNRS UMR 8180, 45 avenue des Etats Unis, Versailles, 78035 (France)

    2013-07-01

    This paper investigates the wet etching of InSb surfaces by two different oxidant agents: Br{sub 2} and H{sub 2}O{sub 2} and the consecutive oxides generation onto the surfaces. The strong dependence between the chemical composition of the etching baths and the nature of the final surface chemistry of this low band-gap III–V semiconductor will be especially highlighted. One aqueous etching solution combined hydrobromic acid and Bromine (HBr–Br{sub 2}:H{sub 2}O) with adjusted concentrations. The other solution combines orthophosphoric and citric acids with hydrogen peroxide (H{sub 3}PO{sub 4}–H{sub 2}O{sub 2}:H{sub 2}O). Depending on its composition, each formulation gave rise to variable etching rate. The dosage of Indium traces in the etching solution by atomic absorption spectroscopy (AAS) gives the kinetic variation of the dissolution process. The variations on etching rates are associated to the properties and the nature of the formed oxides on InSb surfaces. Surface characterization is specifically performed by X-ray photoelectron spectroscopy (XPS). A clear evidence of the differences between the formed oxides is highlighted. Atomic force microscopy is used to monitor the surface morphology and pointed out that very different final morphologies can be reached. This paper presents new results on the strong variability of the InSb oxides in relation with the InSb reactivity toward environment interaction.

  12. [Synthesis of hydroxyapatite/magnetite/zeolite composite for Congo red removal from aqueous solution].

    Science.gov (United States)

    Fang, Qiao; Lin, Jian-Wei; Zhan, Yan-Hui; Yang, Meng-Juan; Zheng, Wen-Jing

    2014-08-01

    In this study, a novel hydroxyapatite/magnetite/zeolite (HAP/Fe3O4/Zeo) composite was prepared, characterized and used as an adsorbent to remove Congo red (CR) from aqueous solution. The adsorption characteristics of CR from aqueous solution on the HAP/Fe3O4/Zeo composite were investigated using batch experiments. Results showed that the HAP/Fe3O4/Zeo composite was effective for the removal of CR from aqueous solution. The CR adsorption capacity for the HAP/Fe3O4/Zeo composite decreased with solution pH increasing from 3 to 4 or solution pH increasing from 7 to 11, and remained basically unchanged with pH increasing from 4 to 7. The CR removal efficiency of the HAP/Fe3O4/Zeo composite increased with increasing adsorbent dosage, while the amount of CR adsorbed on the HAP/Fe3O4/Zeo composite decreased with increasing adsorbent dosage. The adsorption kinetic data of CR on the HAP/Fe3O4/Zeo composite well fitted a pseudo-second-order model. The equilibrium adsorption data of CR on the HAP/Fe3O4/Zeo composite could be described by the Langmuir and Freundlich isotherm models. The maximum monolayer adsorption capacity for CR derived from the Langmuir isotherm model was determined to be 117 mg x g(-1) at pH 7 and 303 K. The adsorption process of CR on the HAP/Fe3O4/Zeo composite was spontaneous and endothermic. The main mechanisms for the adsorption of CR on the HAP/Fe3O4/Zeo composite at pH 7 included surface complexation, hydrogen bonding and Lewis acid-base reaction. Thermal regeneration showed that the HAP/Fe3O4/Zeo composite could be used for five desorption-adsorption cycles with high removal efficiency for CR in each cycle. X-ray diffraction (XRD) analysis revealed that the HAP/Fe3O4/zeolite composite contained Fe3O4, and this composite had relatively high saturation magnetization. The HAP/Fe3O4/Zeo composite adsorbed with CR could be collected from aqueous solution under an external magnetic field quickly. Results of this study suggested that the HAP/Fe3O4/Zeo

  13. An in-situ X-ray absorption spectroelectrochemical study of the electroreduction of uranium ions in HCl, HNO{sub 3}, and Na{sub 2}CO{sub 3} solutions

    Energy Technology Data Exchange (ETDEWEB)

    Uehara, Akihiro; Fujii, Toshiyuki; Yamana, Hajimu [Kyoto Univ., Osaka (Japan). Div. of Nuclear Engineering Science; Okamoto, Yoshihiro [Japan Atomic Energy Agency, Ibaraki (Japan). Quantum Beam Science Directorate

    2016-04-01

    A spectroelectrochemical cell was fabricated for in-situ X-ray absorption spectroscopy (in-situ XAS). The XAS spectra of the uranium L{sub III} edge were monitored in electrolyte solutions during the electrochemical reduction. Tetravalent uranium, U{sup 4+}, in 1 mol dm{sup -3} (M) hydrochloric acid (HCl) was electrochemically prepared from hexavalent uranium, UO{sub 2}{sup 2+}, by constant current electrolysis, and the extended X-ray absorption fine structure (EXAFS) was analyzed. The concentration ratio of UO{sub 2}{sup 2+} and U{sup 4+}, which were formed via the disproportionation of pentavalent uranium, UO{sub 2}{sup +}, during the electrolysis, were calculated based on the intensity of the signal for the two axial oxygen atoms in the linear UO{sub 2}{sup 2+} unit, the U-O{sub ax}, bond that had a radial structural function. The apparent redox potential of the UO{sub 2}{sup 2+}/U{sup 4+} couple in 1 M HCl was determined based on the Nernst equation using the concentrations of UO{sub 2}{sup 2+} and U{sup 4+}. The electrode potential was shown to be close to the formal potential of the UO{sub 2}{sup 2+}/UO{sub 2}{sup +} couple as reported previously. This result indicates that the UO{sub 2}{sup +} that was formed electrochemically at the electrode disproportionated to form UO{sub 2}{sup 2+} and U{sup 4+} in the bulk solution. The in-situ XAS of UO{sub 2}{sup 2+} in 0.1 M nitric acid was also performed. The U{sup 4+} that formed was partially re-oxidized to UO{sub 2}{sup 2+} by the NO{sub 3}{sup -} present in the solution. The formation of the UO{sub 2}{sup +} carbonato complex was observed by in-situ XAS in a 1 M sodium carbonate solution during the bulk electrolysis. The edge jump of the X-ray absorption near edge structure (XANES) spectrum shifted from 17.164 to 17.163 keV, and the bond distances of U-O{sub ax} and U-O for CO{sub 3}{sup 2-} increased from 1.78 to 1.88 Aa and from 2.42 to 2.53 Aa, respectively, because of the reduction of the UO{sub 2}{sup 2

  14. Removal of Uranium From Aqueous Solution by Carbon Nanotubes.

    Science.gov (United States)

    Yu, Jing; Wang, Jianlong

    2016-10-01

    The adsorption of uranium onto carbon nanotubes (CNTs) was investigated. The effect of solution pH, contact time, initial uranium concentration, and temperature on the adsorption capacity of uranium was determined. CNTs were characterized by using scanning electron microscopy (SEM), transmission electron microscopy (TEM), powder x-ray diffraction (XRD), Raman spectra, and the Fourier infrared spectra (FTIR). The diameters of the CNTs varied from 10 to 50 nm in diameter and 1 ~ 2 μm in length. FTIR spectra analysis indicated that carboxyl groups were involved in adsorption of U(VI) by CNTs. The experimental results showed that U(VI) adsorption onto CNTs reached equilibrium within 10 min, and the removal efficiency was 95% at pH = 5. The adsorption kinetics of U(VI) could be described by a pseudo first-order kinetic model. The adsorption isotherm conformed to the Slips model. The adsorption process was spontaneous and endothermic. PMID:27575349

  15. Soft X-ray induced damage in PVA-based membranes in water environment monitored by X-ray absorption spectroscopy

    Science.gov (United States)

    Tzvetkov, George; Späth, Andreas; Fink, Rainer H.

    2014-10-01

    The effect of synchrotron X-ray flux in a soft X-ray scanning-transmission microspectroscope (STXM) instrument on the chemical structure of air-filled poly(vinyl alcohol) (PVA) based microbubbles and their stabilizing shell has been examined. Prolonged soft X-ray illumination of the particles in aqueous suspension leads to the breaking of the microbubbles' protective polymer shell and substantial chemical changes. The latter were clarified via a micro-spot C K-edge near-edge X-ray absorption fine structure (NEXAFS) spectroscopy with further respect to the absorbed X-ray doses. Our results revealed a continuous degradation of the PVA network associated with formation of carbonyl- and carboxyl-containing species as well as an increased content of unsaturated bonds. The observed effects must be taken into account in studies of micro- and nanostructured polymer materials utilizing X-rays.

  16. Application of a new adsorbent for fluoride removal from aqueous solutions

    International Nuclear Information System (INIS)

    Highlights: • A new adsorbent has been prepared. • The adsorbent is non-toxic and easy to synthesize. • HBO1 has displayed best capacity for the removal of fluoride. • Unlike most adsorbents, HBO1 is suitable for the removal of fluoride from water. • The process of removal has been optimized. -- Abstract: Hydrous bismuth oxides (HBOs) have been investigated as a possible adsorbent for fluoride removal from water. Apart from bismuth trioxide (Bi2O3) compound, three additional HBOs, named as HBO1, HBO2, and HBO3 were synthesized in the laboratory and examined for their relative potentials for fluoride removal from aqueous solutions. HBO1 was observed to have highest fluoride removal at 10 mg/L initial concentration in aqueous environment. Among competitive anions, sulfate and chloride affect the fluoride removal by HBO1 more adversely than bicarbonate. Characterization of HBOs using X-ray diffraction (XRD) pattern analyses indicated crystalline structures, and the broad chemical composition of materials showed successive increase of Bi(OH)3 from HBO1 to HBO3, with decrease of BiOCl in the same order. Fourier Transform Infrared (FTIR) spectroscopy analyses indicated presence of Bi-O bond and successively increasing number of peaks corresponding to OH ion from HBO1 to HBO3. Scanning Electron Microscopic (SEM) images of HBOs show rough and porous structure of the materials. Presence of higher proportion of chloride compound in HBO1 with respect to others appears to be the factor responsible for its better performance in fluoride removal from aqueous solutions

  17. Acidities of Water and Methanol in Aqueous Solution and DMSO

    Science.gov (United States)

    Gao, Daqing

    2009-01-01

    The relative acidities of water and methanol have been a nagging issue. In gas phase, methanol is more acidic than water by 36.0 kJ/mol; however, in aqueous solution, the acidities of methanol and water are almost identical. The acidity of an acid in solution is determined by both the intrinsic gas-phase ionization Gibbs energy and the solvent…

  18. Synthesis and Aqueous Solution Viscosity of Hydrophobically Modified Xanthan Gum

    Institute of Scientific and Technical Information of China (English)

    QIAN Xiao-lin; WU Wen-hui; YU Pei-zhi; WANG Jian-quan

    2007-01-01

    Two xanthan gum derivatives hydrophobically modified by 4 or 8 tetradecyl chains per 100 xanthan gum structure units were synthesized. The derivatives were studied by scanning electron microscope and pyrene fluorescence spectrometry. And the aqueous solution apparent viscosity of the derivatives was investigated. The results indicate that the network of the derivatives with more hydrophobic groups is closer and tighter. With increasing of alkyl chain substitution degree, the hydrophobically associating interactions enhance in aqueous solution. Aqueous solution apparent viscosity of the derivatives increases with increasing of polymer concentration and alkyl substitution degree, and decreases with the increase of temperature. In the brine solution, the strong viscosity enhancement phenomenon appears. The interaction between the derivatives and surfactant sodium dodecylbenzene sulfonate is strong.

  19. Phosphate removal from aqueous solutions by nanoscale zero-valent iron.

    Science.gov (United States)

    Wu, Donglei; Shen, Yanhong; Ding, Aqiang; Qiu, Mengyu; Yang, Qi; Zheng, Shuangshuang

    2013-01-01

    In this study, nanoscale zero-valent iron (NZVI) was synthesized by conventional liquid-phase chemical reduction methods without a support material and then characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM) and X-ray diffraction (XRD). The effect of NZVI particles on phosphate removal from aqueous solutions was examined. The results showed that the phosphate removal efficiency increased from 34.49% to 87.01% as the dosage of nanoscale iron particles increased from 100 to 600 mg L(-1) with an initial phosphate concentration of 10 mg L(-1), and the phosphate removal efficiency decreased from 72.89% to 51.39% as the initial phosphate concentration increased from 10 to 90 mg L(-1), with 400 mg L(-1) NZVI. Phosphate removal efficiencies of 99.41% and 95.09% were achieved at pH values of 2 and 4, respectively, with an initial phosphate concentration of 20 mg L(-1) and 400mg L(-1) NZVI. The use of NZVI particles synthesized in a carboxymethyl cellulose (CMC)-water solution significantly enhanced phosphate removal from an aqueous solution compared with the use of NZVI synthesized in an ethanol-water solution. NZVI particles achieved 71.34% phosphate removal, which was remarkably higher than that of microscale zero-valent iron (MZVI) particles (16.35%) with 10 mg L(-1) of phosphate and 400mg L(-1) iron. Based on the removal mechanism analysis performed in this study, we recommend that phosphate removal be accomplished by simultaneous adsorption and chemical precipitation. The XRD patterns of the NZVI before and after the reactions indicated the formation of crystalline vivianite (Fe3(PO4)2 x 8H2O) during the procedure.

  20. Application of Fe-Cu binary oxide nanoparticles for the removal of hexavalent chromium from aqueous solution.

    Science.gov (United States)

    Khan, Saif Ullah; Zaidi, Rumman; Hassan, Saeikh Z; Farooqi, I H; Azam, Ameer

    2016-01-01

    The adsorption process has been used as an effective technique for the removal of metal ions from aqueous solutions. Groundwater remediation by nanoparticles has received interest in recent years. In the present study, a binary metal oxide of Fe-Cu was prepared and used for the removal of hexavalent chromium from aqueous solution. Batch experiments were performed to investigate the effects of initial Cr (VI) concentration, dose of adsorbent, and pH of solution on the removal efficiency of Cr (VI). The prepared nanostructured Fe-Cu binary oxides were able to reduce the concentration of Cr (VI) in aqueous solution. Binary metal oxides nanoparticle exhibited an outstanding ability to remove Cr (VI) due to high surface area, low particle size, and high inherent activity. The percentage removal efficiency of Cr (VI) increased with nanoparticles doses (0.1 g L(-1)-2.5 g L(-1)), whereas it decreased with initial Cr (VI) concentration (1 mg L(-1)-25 mg L(-1)) and with pH (3-9). The Freundlich model was found to be the better fit for adsorption isotherm. The prepared nanomaterial was characterized using powder X-ray diffraction, scanning electron microscopy (SEM), and ultraviolet (UV)-visible spectroscopy. It showed that the Fe-Cu binary oxides were formed in single phase. SEM micrograph showed aggregates with many nano-sized particles. UV-visible spectroscopy showed quantum confinement effect. PMID:27386994

  1. X-ray hot plasma diagnostics

    International Nuclear Information System (INIS)

    X-ray plasma emission study is powerful diagnostic tool of hot plasmas. In this review article the main techniques of X-ray plasma emission measurement are shortly presented: X-ray spectrometry using absorbent filters, crystal and grating spectrometers, imaging techniques using pinhole cameras, X-ray microscopes and Fresnel zone plate cameras, X-ray plasma emission calorimetry. Advances in these techniques with examples for different hot plasma devices are also presentes. (author)

  2. X-ray imaging of radioresistant Deinococcus radiodurans

    Science.gov (United States)

    Takemoto, K.; Narumi, I.; Satoh, K.; Namba, H.; Kihara, H.

    2009-09-01

    Deinococcus radiodurans has been known to withstand radiation levels up to 1,000 times than that would kill normal human cells. To cope radiation damage during soft X-ray observation of living cells, D. radiodurans incubated with tellurium oxyanions was used as the X-ray microscopy sample. The first observation was successfully performed. In combination of antifreeze solution and subzero temperature, along with carbon window, the cell observation will be more closely to the living condition.

  3. X-ray fluorescence spectrometry

    International Nuclear Information System (INIS)

    The seventh edition of Philips' Review of Literature on x-ray fluorescence spectrometry starts with a list of conference proceedings on the subject, organised by the Philips organisation at regular intervals in various European countries. It is followed by a list of bulletins. The bibliography is subdivided according to spectra, equipment, applications and absorption analysis

  4. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... Images related to X-ray (Radiography) - Bone About this Site RadiologyInfo.org is produced by: Please note ... you can search the ACR-accredited facilities database . This website does not provide cost information. The costs ...

  5. X-ray backscatter imaging

    Science.gov (United States)

    Dinca, Dan-Cristian; Schubert, Jeffrey R.; Callerame, J.

    2008-04-01

    In contrast to transmission X-ray imaging systems where inspected objects must pass between source and detector, Compton backscatter imaging allows both the illuminating source as well as the X-ray detector to be on the same side of the target object, enabling the inspection to occur rapidly and in a wide variety of space-constrained situations. A Compton backscatter image is similar to a photograph of the contents of a closed container, taken through the container walls, and highlights low atomic number materials such as explosives, drugs, and alcohol, which appear as especially bright objects by virtue of their scattering characteristics. Techniques for producing X-ray images based on Compton scattering will be discussed, along with examples of how these systems are used for both novel security applications and for the detection of contraband materials at ports and borders. Differences between transmission and backscatter images will also be highlighted. In addition, tradeoffs between Compton backscatter image quality and scan speed, effective penetration, and X-ray source specifications will be discussed.

  6. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available Toggle navigation Test/Treatment Patient Type Screening/Wellness Disease/Condition Safety En Español More Info Images/Videos News Physician Resources Professions Site Index A-Z X-ray (Radiography) - Bone ...

  7. X-Ray Diffractive Optics

    Science.gov (United States)

    Dennis, Brian; Li, Mary; Skinner, Gerald

    2013-01-01

    X-ray optics were fabricated with the capability of imaging solar x-ray sources with better than 0.1 arcsecond angular resolution, over an order of magnitude finer than is currently possible. Such images would provide a new window into the little-understood energy release and particle acceleration regions in solar flares. They constitute one of the most promising ways to probe these regions in the solar atmosphere with the sensitivity and angular resolution needed to better understand the physical processes involved. A circular slit structure with widths as fine as 0.85 micron etched in a silicon wafer 8 microns thick forms a phase zone plate version of a Fresnel lens capable of focusing approx. =.6 keV x-rays. The focal length of the 3-cm diameter lenses is 100 microns, and the angular resolution capability is better than 0.1 arcsecond. Such phase zone plates were fabricated in Goddard fs Detector Development Lab. (DDL) and tested at the Goddard 600-microns x-ray test facility. The test data verified that the desired angular resolution and throughput efficiency were achieved.

  8. X-ray film processing

    International Nuclear Information System (INIS)

    X-ray films have to be highly sensitive, for radiation protection reasons. The films used in radiology are coated on both sides with a photosensitive emulsion. This applies to all dental films. Their properties and the development of the different exposed films are explained. (DG)

  9. X-rays and magnetism.

    Science.gov (United States)

    Fischer, Peter; Ohldag, Hendrik

    2015-09-01

    Magnetism is among the most active and attractive areas in modern solid state physics because of intriguing phenomena interesting to fundamental research and a manifold of technological applications. State-of-the-art synthesis of advanced magnetic materials, e.g. in hybrid structures paves the way to new functionalities. To characterize modern magnetic materials and the associated magnetic phenomena, polarized x-rays have emerged as unique probes due to their specific interaction with magnetic materials. A large variety of spectroscopic and microscopic techniques have been developed to quantify in an element, valence and site-sensitive way properties of ferro-, ferri-, and antiferromagnetic systems, such as spin and orbital moments, and to image nanoscale spin textures and their dynamics with sub-ns time and almost 10 nm spatial resolution. The enormous intensity of x-rays and their degree of coherence at next generation x-ray facilities will open the fsec time window to magnetic studies addressing fundamental time scales in magnetism with nanometer spatial resolution. This review will give an introduction into contemporary topics of nanoscale magnetic materials and provide an overview of analytical spectroscopy and microscopy tools based on x-ray dichroism effects. Selected examples of current research will demonstrate the potential and future directions of these techniques.

  10. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... over time. top of page What are the benefits vs. risks? Benefits Bone x-rays are the fastest and easiest ... cancer from excessive exposure to radiation. However, the benefit of an accurate diagnosis far outweighs the risk. ...

  11. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... over time. top of page What are the benefits vs. risks? Benefits Bone x-rays are the fastest and easiest ... evaluation. National and international radiology protection organizations continually review and update the technique standards used by radiology ...

  12. Bone X-Ray (Radiography)

    Medline Plus

    Full Text Available ... for more information about pregnancy and x-rays. A Word About Minimizing Radiation Exposure Special care is ... encourage linking to this site. × Recommend RadiologyInfo to a friend Send to (friend's e-mail address): From ( ...

  13. Removal of cationic dyes from aqueous solution using magnetic multi-wall carbon nanotube nanocomposite as adsorbent

    International Nuclear Information System (INIS)

    A magnetic multi-wall carbon nanotube (MMWCNT) nanocomposite was synthesized and was used as an adsorbent for removal of cationic dyes from aqueous solutions. The MMWCNT nanocomposite was composed of commercial multi-wall carbon nanotubes and iron oxide nanoparticles. The properties of this magnetic adsorbent were characterized by scanning electron microscopy, X-ray diffraction and BET surface area measurements. Adsorption characteristics of the MMWCNT nanocomposite adsorbent were examined using methylene blue, neutral red and brilliant cresyl blue as adsorbates. Experiments were carried out to investigate adsorption kinetics, adsorption capacity of the adsorbent and the effect of adsorption dosage and solution pH values on the removal of cationic dyes. Kinetic data were well fitted by a pseudo second-order model. Freundlich model was used to study the adsorption isotherms. The prepared MMWCNT adsorbent displayed the main advantage of separation convenience compared to the present adsorption treatment.

  14. High-Resolution X-ray Emission and X-ray Absorption Spectroscopy

    OpenAIRE

    de Groot, F. M. F.

    2001-01-01

    In this review, high-resolution X-ray emission and X-ray absorption spectroscopy will be discussed. The focus is on the 3d transition-metal systems. To understand high-resolution X-ray emission and reso-nant X-ray emission, it is first necessary to spend some time discussing the X-ray absorption process. Section II discusses 1s X-ray absorption, i.e., the K edges, and section III deals with 2p X-ray absorption, the L edges. X-ray emission is discussed in, respectively, the L edges. X-ray emis...

  15. High-Resolution X-ray Emission and X-ray Absorption Spectroscopy

    NARCIS (Netherlands)

    Groot, F.M.F. de

    2001-01-01

    In this review, high-resolution X-ray emission and X-ray absorption spectroscopy will be discussed. The focus is on the 3d transition-metal systems. To understand high-resolution X-ray emission and reso-nant X-ray emission, it is first necessary to spend some time discussing the X-ray absorption pro

  16. Zinc nanoparticles in solution by laser ablation technique

    Indian Academy of Sciences (India)

    S C Singh; R Gopal

    2007-06-01

    Colloidal zinc metallic nanoparticles are synthesized using pulsed laser ablation of metal plate in an aqueous solution of suitable surfactant to prevent aggregation. UV-visible absorption, TEM, small angle X-ray diffraction and wide-angle X-ray diffraction are used for the characterization of colloidal zinc metallic nanoparticles. Colloidal nanoparticles are found highly stable for a long time.

  17. Conductivity of Oxalic Acid in Aqueous Solution at Low Concentration

    Institute of Scientific and Technical Information of China (English)

    倪良; 韩世钧

    2005-01-01

    Oxalic acid is a weak and unsymmetrical bi-basic acid. There exist dissociation and association equilibria among the species in aqueous solution. The molar conductivity of the solution is the sum of the ionic contributions.Based on this idea, a new prediction equation of ionic conductivity was proposed at low concentration. The molar conductivities of the solution and its relevant ions were calculated respectively. The results obtained were in good agreement with those from experiments and the Quint-Viallard equation.

  18. Modeling reactive geochemical transport of concentrated aqueous solutions

    Science.gov (United States)

    Zhang, Guoxiang; Zheng, Zuoping; Wan, Jiamin

    2005-02-01

    Aqueous solutions with ionic strength larger than 1 M are usually considered concentrated aqueous solutions. These solutions can be found in some natural systems and are also industrially produced and released into accessible natural environments, and as such, they pose a big environmental problem. Concentrated aqueous solutions have unique thermodynamic and physical properties. They are usually strongly acidic or strongly alkaline, with the ionic strength possibly reaching 30 M or higher. Chemical components in such solutions are incompletely dissociated. The thermodynamic activities of both ionic and molecular species in these solutions are determined by the ionic interactions. In geological media the problem is further complicated by the interactions between the solutions and sediments and rocks. The chemical composition of concentrated aqueous solutions when migrating through the geological media may be drastically altered by these strong fluid-rock interactions. To effectively model reactive transport of concentrated aqueous solutions, we must take into account the ionic interactions. For this purpose we substantially extended an existing reactive transport code, BIO-CORE2D©, by incorporating a Pitzer ion interaction model to calculate the ionic activity. In the present paper, the model and two test cases of the model are briefly introduced. We also simulate a laboratory column experiment in which the leakage of highly alkaline waste fluid stored at Hanford (a U.S. Department of Energy site, located in Washington State) was studied. Our simulation captures the measured pH evolution and indicates that all the reactions controlling the pH evolution, including cation exchanges and mineral dissolution/precipitation, are coupled.

  19. Evaluating SAXS Results on Aqueous Solutions of Various Bacterial Levan utilizing the String-of-Beads Model.

    Science.gov (United States)

    Benigar, Elizabeta; Tomšič, Matija; Sretenovic, Simon; Stopar, David; Jamnik, Andrej; Dogsa, Iztok

    2015-01-01

    Polysaccharide levan is a homopolymer of fructose and is an important component of plants, yeast, fungi and some bacterial biofilms. In this paper we report on the structural properties of aqueous solutions of bacterial levan utilizing smallangle X-ray scattering and light microscopy. In addition to commercially available levan isolated from Zymomonas mobilis and Erwinia herbicola, we also studied levan isolated and purified from the biofilm of Bacillus subtilis. The smallangle X-ray scattering data were analyzed by the string-of-beads model that revealed qualitative differences in the structure of levan molecules. Levan can be represented as a semi-flexible chain that interacts intra- and inter-molecularly and therefore forms various suprastructures on larger size scales. Increasing the concentration of levan makes the levan structure more compact, which was observed on the nano as well as on the micro scale. The structures with most homogeneously distributed polymer local density were found in B. subtilis levan solutions. PMID:26454583

  20. X-ray reflectivity study of formation of multilayer porous anodic oxides of silicon.

    Energy Technology Data Exchange (ETDEWEB)

    Chu, Y.; Fenollosa, R.; Parkhutik, V.; You, H.

    1999-07-21

    The paper reports data on the kinetics of anodic oxide films growth on silicon in aqueous solutions of phosphoric acids as well as a study of the morphology of the oxides grown in a special regime of the oscillating anodic potential. X-ray reflectivity measurements were performed on the samples of anodic oxides using an intense synchrotron radiation source. They have a multilayer structure as revealed by theoretical fitting of the reflectivity data. The oscillations of the anodic potential are explained in terms of synchronized oxidation/dissolution reactions at the silicon surface and accumulation of mechanic stress in the oxide film.

  1. Molecular Weight and Aggregation of Erwinia Gum in Aqueous Solutions

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    Erwinia(E) gum is composed of glucose, fucose, galactose and glucuronic acid. The weight-average molecular weights Mw, number-average molecular weights Mn and intrinsic viscosities[η] of the four fractions and the unfractionated E gum in aqueous solutions at desired temperatures were studied by light scattering, membrane osmometry, size exclusion chromatography(SEC) and viscometry. The experimental results prove that E gum formed aggregates in the aqueous solution at 25 ℃ and the aggregates were broken gradually with increasing temperature. The dissociation of the aggregates of E gum in the aqueous solution started at 36 ℃, and was completed at around 90 ℃. The [η] values of E gum and its fractions are much higher than those of the conventional polymers with the similar molecular weights, and decrease with increasing NaCl concentration.

  2. Reorientation and Allied Dynamics in Water and Aqueous Solutions

    Science.gov (United States)

    Laage, Damien; Stirnemann, Guillaume; Sterpone, Fabio; Rey, Rossend; Hynes, James T.

    2011-05-01

    The reorientation of a water molecule is important for a host of phenomena, ranging over—in an only partial listing—the key dynamic hydrogen-bond network restructuring of water itself, aqueous solution chemical reaction mechanisms and rates, ion transport in aqueous solution and membranes, protein folding, and enzymatic activity. This review focuses on water reorientation and related dynamics in pure water, and for aqueous solutes with hydrophobic, hydrophilic, and amphiphilic character, ranging from tetra-methylurea to halide ions and amino acids. Attention is given to the application of theory, simulation, and experiment in the probing of these dynamics, in usefully describing them, and in assessing the description. Special emphasis is placed on a novel sudden, large-amplitude jump mechanism for water reorientation, which contrasts with the commonly assumed Debye rotational diffusion mechanism, characterized by small-amplitude angular motion. Some open questions and directions for further research are also discussed.

  3. 100-picosecond time-resolved X-ray absorption fine structure of Fe{sup II}(1,10-phenanthroline){sub 3}

    Energy Technology Data Exchange (ETDEWEB)

    Sato, Tokushi; Tomita, Ayana; Koshihara, Shin-ya [Department of Materials Science, Tokyo Institute of Technology (Japan); Nozawa, Shunsuke; Ichiyanagi, Kouhei; Ichikawa, Hirohiko; Adachi, Shin-ichi [Non-Equilibrium Dynamics Project, ERATO, JST (Japan); Chollet, Matthieu [Advanced Photon Source, Argonne, Chicago (United States); Fujii, Hiroshi, E-mail: skoshi@cms.titech.ac.j [Institute for Molecular Science, National Institutes of Natural Sciences (Japan)

    2009-02-01

    Studying photo-induced molecular dynamics in liquid with sub-nanosecond time-resolution and sub-Angstrom spatial resolution gives information for understanding fundamental chemical process in the photo-induced cooperative phenomena of molecular systems and also for developing new materials and devices. Here, we present time-resolved X-ray absorption fine structure on the spin-crossover complex Fe{sup II} tris-(1,10-phenanthroline) dissolved in aqueous solution. We utilized femtosecond laser at 400nm pulse for excitation and 100ps X-ray pulse for probe.

  4. Polypyrrole-polyaniline/Fe{sub 3}O{sub 4} magnetic nanocomposite for the removal of Pb(II) from aqueous solution

    Energy Technology Data Exchange (ETDEWEB)

    Afshar, Amirhossein; Sadjadi, Seyed Abolfazl Seyed; Mollahosseini, Afsaneh; Eskandarian, Mohammad Reza [Iran University of Science and Technology, Tehran (Iran, Islamic Republic of)

    2016-02-15

    Lead ion which is engaged in aqueous solution has been successfully removed. A novel technique was utilized for the separation and absorption of Pb(II) ions from aqueous solution. Magnetic Fe{sub 3}O{sub 4} coated with newly investigated polypyrrole-polyaniline nanocomposite was used for the removal of extremely noxious Pb(II). Characteristic of the prepared magnetic nanocomposite was done using X-ray diffraction pattern, Field emission scanning electron microscopy (FE-SEM), Fourier transform-infrared spectroscopy (FT-IR) and energy dispersive x-ray spectroscopy (EDX). Up to 100% adsorption was found with 20mg/L Pb(II) aqueous solution in the range of pH=8-10. Adsorption results illustrated that Pb(II) removal efficiency by the nanocomposite increased with an enhance in pH. Adsorption kinetics was best expressed by the pseudo-second-order rate form. Isotherm data fitted well to the Freundlich isotherm model. Upon using HCl and HNO{sub 3}, 75% PPy-PAn/Fe{sub 3}O{sub 4} nanocomposite, desorption experiment showed that regenerated adsorbent can be reused successfully for two successive adsorption-desorption cycles without appreciable loss of its original capacity.

  5. Morphology of modified biochar and its potential for phenol removal from aqueous solutions

    Directory of Open Access Journals (Sweden)

    Kostas A. Komnitsas

    2016-04-01

    Full Text Available In the present study, the efficiency of phenol removal from synthetic aqueous solutions by chemically modified biochar with the use of 1M KOH or 1M FeCl3 was investigated. Initially, biochar was produced after slow pyrolysis of three different agricultural wastes, namely pistachio (Pistacia vera L. shells, pecan (Carya illinoinensis shells and wood sawdust. The quality of biochar was assessed by evaluating its main properties, such as pH, surface area, porosity and C content. X-ray diffraction (XRD, Scanning Electron Microscopy (SEM and Fourier Transform Infrared Spectroscopy (FTIR were used for the identification of biochar’s structure. The efficiency of phenol removal from synthetic solutions was assessed with the use of kinetic and equilibrium experiments. The experimental results show that the KOH-modified biochar exhibited the highest phenol removal efficiency. Hydrophobic sorption on its surface is the main phenol removal mechanism. The pseudo-second order model fits best the kinetic data, while the Freundlich model, as deduced from an equilibrium study describes very well sorption of phenols on all biochars examined.

  6. Removal of Ni2+ from Aqueous Solutions by Adsorption Onto Magnetic Multiwalled Carbon Nanotube Nanocomposite

    Directory of Open Access Journals (Sweden)

    Konicki Wojciech

    2014-06-01

    Full Text Available The removal of Ni2+ from aqueous solution by magnetic multiwalled carbon nanotube nanocomposite (MMWCNTs-C was investigated. MMWCNTs-C was characterized by X-ray Diffraction method (XRD, High-Resolution Transmission Electron Microscopy (HRTEM, surface area (BET, and Fourier Transform-Infrared Spectroscopy (FTIR. The effects of initial concentration, contact time, solution pH, and temperature on the Ni2+ adsorption onto MMWCNTs-C were studied. The Langmuir and Freundlich isotherm models were applied to fit the adsorption data. The results showed that the adsorption isotherm data were fitted well to the Langmuir isotherm model with the maximum monolayer adsorption capacity of 2.11 mg g–1. The adsorption kinetics was best described by the pseudo-second-order model. The thermodynamic parameters, such as ΔHo, ΔGo and ΔSo, were also determined and evaluated. The adsorption of Ni2+ is generally spontaneous and thermodynamically favorable. The values of ΔHo and ΔGo indicate that the adsorption of Ni2+ onto MMWCNTs-C was a physisorption process.

  7. THE REMOVAL OF REACTIVE RED 228 DYE FROM AQUEOUS SOLUTIONS BY CHITOSAN-MODIFIED FLAX SHIVE

    Directory of Open Access Journals (Sweden)

    Hao Feng,

    2011-12-01

    Full Text Available Flax shive (FS is a byproduct from flax fiber separation. The use of absorbent prepared from chitosan-modified flax shive (CFS has been studied for removal of reactive red dye (RR228 from aqueous solutions. CFS was characterized by the Brunauer-Emmett-Teller (BET method, Scanning Electron Microscopy (SEM, Fourier Transform Infrared spectrometry (FTIR, and X-ray photoelectron spectroscopy (XPS. A batch adsorption study was conducted under various contact time, initial concentration, solution pH, and adsorbent dosage. It was found that the BET and Langmuir surface area of CFS were 1.772 m2 g-1 and 3.057 m2 g-1, respectively. Results showed that CFS has the same pores as FS and that the –NH2 group on CFS is the main adsorption site for dye sorption. Equilibrium adsorption capacity could be reached within 480 min, and RR228 uptake was satisfactory at a pH of 2.0. The percentage removal were 100%, 100%, 90%, and 85% at pH 2.0 under dye concentrations of 10 mg/L, 20 mg/L, 30 mg/L, and 40 mg/L, respectively. The adsorption accurately fitted a pseudo-second-order kinetic model and a Langmuir isotherm model. It is proposed that CFS could be applied as a low-cost absorbent in removal of dyes from wastewater.

  8. Alkali modified hydrochar of grape pomace as a perspective adsorbent of Pb(2+) from aqueous solution.

    Science.gov (United States)

    Petrović, Jelena T; Stojanović, Mirjana D; Milojković, Jelena V; Petrović, Marija S; Šoštarić, Tatjana D; Laušević, Mila D; Mihajlović, Marija L

    2016-11-01

    Hydrochar produced via hydrothermal carbonization of grape pomace was considered as novel sorbent of Pb(2+) from aqueous solution. In order to enhance the adsorption capacity, hydrochar was chemically modified using 2 M KOH solution. Both materials were characterized by Fourier transform infrared spectroscopy, scanning electron microscopy and X-ray diffraction technique. Batch experiments were performed to examine the effect of sorbent dosage, pH and contact time. Obtained results showed that the KOH treatment increased the sorption capacity of hydrochar from 27.8 mg g(-1) up to 137 mg g(-1) at pH 5. Adsorption of lead on either of the materials was achieved through ion-exchange mechanism, chemisorption and Pb(2+)-π interaction. The Sips isotherm model gave the best fit with the experimental data obtained for Pb(2+) sorption using activated hydrochar. The adsorption kinetic followed a pseudo second-order model. Thermodynamic parameters implied that the Pb(2+) binding for hydrochar surface was spontaneous and exothermic process. Findings from this work suggest that the hydrothermal carbonization is a promising route for production of efficient Pb (2+) sorbents for wastewater treatment. PMID:27494605

  9. Adsorptive removal of Congo red from aqueous solutions using crosslinked chitosan and crosslinked chitosan immobilized bentonite.

    Science.gov (United States)

    Huang, Ruihua; Zhang, Lujie; Hu, Pan; Wang, Jing

    2016-05-01

    Batch experiments were executed to investigate the removal of Congo red (CR) from aqueous solutions using the crosslinked chitosan (CCS) and crosslinked chitosan immobilized bentonite (CCS/BT composite). The CCS and CCS/BT composite were characterized by X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) techniques. The removal of CR was examined as a function of pH value of CR solution, contact time, and inorganic sodium salt and ionic strength. The equilibrium data of CCS and CCS/BT composite agreed well with the Langmuir model. The adsorption capacities of CCS and CCS/BT composite at 298K and natural pH value were 405 and 500mg/g, respectively. The kinetic data correlated well with the pseudo-second-order model. The adsorption of CR onto the CCS was mainly controlled by chemisorption while the adsorption of CR onto the CCS/BT composite was controlled by chemisorption and the electrostatic attraction. PMID:26820350

  10. Removal of Cu(II) from aqueous solutions using chemically modified chitosan

    International Nuclear Information System (INIS)

    Chemically modified chitosan namely epichlorohydrin cross-linked xanthate chitosan (ECXCs) has been used for the removal of Cu(II) ions from aqueous medium. The influence of various operating parameters such as pH, temperature, sorbent dosage, initial concentration of Cu(II) ions and contact time on the adsorption capacity of ECXCs has been investigated. Thermodynamic parameters namely ΔGo, ΔHo and ΔSo of the Cu(II) adsorption process have been calculated. Differential anodic stripping voltammetric technique was used to determine the concentration of Cu(II) in the test solution before and after adsorption. The nature of the possible adsorbent-metal ion interactions was studied by Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy. The studies showed that the adsorption of Cu(II) on ECXCs strongly depends on pH and temperature. The maximum adsorption capacity was observed at pH 5.0 and the adsorption capacity of ECXCs increased with increasing temperature indicating the endothermic nature of adsorption process. Langmuir and Freundlich adsorption equations were used to fit the experimental data. The adsorption process is found to follow the pseudo-second-order kinetic model. The maximum adsorption capacity was found to be 43.47 mg g-1 from the Langmuir isotherm model at 50 deg. C. During desorption studies 97-100% of adsorbed copper ion is released into solution in presence of 1N EDTA, HCl and H2SO4.

  11. Preparation of Amine-Modified Polyacrylonitrile Fibers: Copper Removalin Aqueous Solution.

    Science.gov (United States)

    Yang, Cai-Yu; Fang-Liu; Nguyen, Nhat Thien; Ma, Chih-Ming; Chang, Chang-Tang

    2016-02-01

    In this study, Polyacrylonitrile (PAN) fibers were prepared by a simple and effective electrospinning method. Subsequently, the PAN fibers were modified by diethylenetriamine (DETA) to produce aminated polyacrylonitrile (APAN) fibers. Finally, the adsorbability of copper ions on the surface of the fibers was examined in an aqueous solution. The characteristics of APAN fibers were analyzed using Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and X-ray diffraction (XRD); The surface amination was confirmed by FTIR. The adsorption data fitted well with the Freundlich isotherm. Thermodynamic parameters of the adsorption process were calculated. The standard Gibb's free energy change, standard enthalpy change, and standard entropy change was -1.46 KJ/mol, -54.72 kJ/mol, and -178.75 kJ/mol/K, respectively. Furthermore, the results show that adsorption of copper onto APAN fibers were spontaneous and exothermic in nature. The equilibrium adsorption capacity of PAN fibers was only 0.10 mg g(-1) for 10 mg L(-1) of copper solution removal under pH 6 and 298 K. In contrast, the equilibrium adsorption capacity of APAN fibers was 45.05 mg g(-1) under the same conditions. The prepared APAN fibers exhibit high efficiency for Cu(II) removal from Waste water and may be used as a reference for future investigation. PMID:27433707

  12. [Extraction of alpha-cypermethrin from aqueous methanol solutions].

    Science.gov (United States)

    Shormanov, V K; Chigareva, E N; Belousova, O V

    2010-01-01

    Alpha cypermethrin was extracted from aqueous methanol solutions using hydrophobic organic solvents. The efficiency of extraction was shown to depend on the chemical nature of the solvent, the water to methanol ratio, and saturation of the aqueous methanol layer with an electrolyte. Optimal extraction of alpha-cypermethrin was achieved using toluene as the solvent under desalinization conditions. The extraction factor for the removal of the sought amount of alpha-cypermethrin from the water-methanol solution (4:1) using various solvents was calculated.

  13. Ionisation constants of inorganic acids and bases in aqueous solution

    CERN Document Server

    Perrin, D D

    2013-01-01

    Ionisation Constants of Inorganic Acids and Bases in Aqueous Solution, Second Edition provides a compilation of tables that summarize relevant data recorded in the literature up to the end of 1980 for the ionization constants of inorganic acids and bases in aqueous solution. This book includes references to acidity functions for strong acids and bases, as well as details about the formation of polynuclear species. This text then explains the details of each column of the tables, wherein column 1 gives the name of the substance and the negative logarithm of the ionization constant and column 2

  14. Predicting accurate absolute binding energies in aqueous solution

    DEFF Research Database (Denmark)

    Jensen, Jan Halborg

    2015-01-01

    Recent predictions of absolute binding free energies of host-guest complexes in aqueous solution using electronic structure theory have been encouraging for some systems, while other systems remain problematic. In this paper I summarize some of the many factors that could easily contribute 1-3 kcal......-represented by continuum models. While I focus on binding free energies in aqueous solution the approach also applies (with minor adjustments) to any free energy difference such as conformational or reaction free energy differences or activation free energies in any solvent....

  15. Degradation kinetics of benzyl nicotinate in aqueous solution

    Directory of Open Access Journals (Sweden)

    Mbah C

    2010-01-01

    Full Text Available The degradation of benzyl nicotinate in aqueous solution over a pH range of 2.0-10.0 at 50±0.2 o was studied. The degradation was determined by high performance liquid chromatography. The degradation was observed to follow apparent first-order rate kinetics and the rate constant for the decomposition at 25 o was estimated by extrapolation. The reaction was shown to be hydroxide ion catalyzed and the Arrhenius plots showed the temperature dependence of benzyl nicotinate degradation. A significant increase in the stability of benzyl nicotinate was observed when glycerol or polyethylene glycol 400 was incorporated into the aqueous solution.

  16. Removal of Phosphate from Aqueous Solution with Modified Bentonite

    Institute of Scientific and Technical Information of China (English)

    唐艳葵; 童张法; 魏光涛; 李仲民; 梁达文

    2006-01-01

    Bentonite combined with sawdust and other metallic compounds was used to remove phosphate from aqueous solutions in this study. The adsorption characteristics of phosphate on the modified bentonite were investigated, including the effects of temperature, adsorbent dosage, initial concentration of phosphate and pH on removal of phosphate by conducting a series of batch adsorption experiments. The results showed that 98% of phosphate removal rate was obtained since sawdust and bentonite used in this investigation were abundantly and locally available. It is concluded that modified bentonite is a relatively efficient, low cost and easily available adsorbent for the removal of phosphate from aqueous solutions.

  17. Protein structure validation and analysis with X-ray crystallography.

    Science.gov (United States)

    Papageorgiou, Anastassios C; Mattsson, Jesse

    2014-01-01

    X-ray crystallography is the main technique for the determination of protein structures. About 85 % of all protein structures known to date have been elucidated using X-ray crystallography. Knowledge of the three-dimensional structure of proteins can be used in various applications in biotechnology, biomedicine, drug design, and basic research and as a validation tool for protein modifications, ligand binding, and structural authenticity. Moreover, the requirement for pure, homogeneous, and stable protein solutions in crystallizations makes X-ray crystallography beneficial in other fields of protein research as well. Here, we describe the technique of X-ray protein crystallography and the steps involved for a successful three-dimensional crystal structure determination.

  18. Glasslike Behavior in Aqueous Electrolyte Solutions

    CERN Document Server

    Turton, David A; Hefter, Glenn; Buchner, Richard; Wynne, Klaas; 10.1063/1.2906132

    2009-01-01

    When salts are added to water, the viscosity generally increases suggesting the ions increase the strength of the water's hydrogen-bond network. However, infrared pump-probe measurements on electrolyte solutions have found that ions have no influence on the rotational dynamics of water molecules implying no enhance-ment or breakdown of the hydrogen-bond network. Here we report optical Kerr-effect and dielectric relaxa-tion spectroscopic measurements, which have enabled us to separate the effects of rotational and transitional motions of the water molecules. These data show that electrolyte solutions behave like a supercooled liquid approaching a glass transition in which rotational and translational molecular motions are decoupled. It is now possible to understand previously conflicting viscosity data, nuclear magnetic resonance relaxation, and ultrafast infrared spectroscopy in a single unified picture.

  19. Glasslike behavior in aqueous electrolyte solutions.

    Science.gov (United States)

    Turton, David A; Hunger, Johannes; Hefter, Glenn; Buchner, Richard; Wynne, Klaas

    2008-04-28

    When salts are added to water, generally the viscosity increases, suggesting that the ions increase the strength of the water's hydrogen-bond network. However, infrared pump-probe measurements on electrolyte solutions have found that ions have no influence on the rotational dynamics of water molecules, implying no enhancement or breakdown of the hydrogen-bond network. Here, we report optical Kerr effect and dielectric relaxation spectroscopic measurements, which have enabled us to separate the effects of rotational and transitional motions of the water molecules. These data show that electrolyte solutions behave like a supercooled liquid approaching a glass transition in which rotational and translational molecular motions are decoupled. It is now possible to understand previously conflicting viscosity data, nuclear magnetic resonance relaxation, and ultrafast infrared spectroscopy in a single unified picture.

  20. Aviation security x-ray detection challenges

    Science.gov (United States)

    Harvey, T.

    2016-05-01

    In this paper, a review of the background and some drivers are provided for X-ray screening for aviation security. Some of the key considerations are highlighted along with impacts of the image-based approaches and signature approaches. The role of information theory is discussed along with some recent work that may influence the technical direction by posing the question: "what measurements, parameters and metrics should be considered in future system design?" A path forward should be based on information theory, however electronic machines will likely interface with humans and be dollar-cost driven, so ultimately solutions must consider additional parameters other than only technical performance factors.