WorldWideScience

Sample records for high-resolution structure determination

  1. High Resolution Powder Diffraction and Structure Determination

    International Nuclear Information System (INIS)

    Cox, D. E.

    1999-01-01

    It is clear that high-resolution synchrotrons X-ray powder diffraction is a very powerful and convenient tool for material characterization and structure determination. Most investigations to date have been carried out under ambient conditions and have focused on structure solution and refinement. The application of high-resolution techniques to increasingly complex structures will certainly represent an important part of future studies, and it has been seen how ab initio solution of structures with perhaps 100 atoms in the asymmetric unit is within the realms of possibility. However, the ease with which temperature-dependence measurements can be made combined with improvements in the technology of position-sensitive detectors will undoubtedly stimulate precise in situ structural studies of phase transitions and related phenomena. One challenge in this area will be to develop high-resolution techniques for ultra-high pressure investigations in diamond anvil cells. This will require highly focused beams and very precise collimation in front of the cell down to dimensions of 50 (micro)m or less. Anomalous scattering offers many interesting possibilities as well. As a means of enhancing scattering contrast it has applications not only to the determination of cation distribution in mixed systems such as the superconducting oxides discussed in Section 9.5.3, but also to the location of specific cations in partially occupied sites, such as the extra-framework positions in zeolites, for example. Another possible application is to provide phasing information for ab initio structure solution. Finally, the precise determination of f as a function of energy through an absorption edge can provide useful information about cation oxidation states, particularly in conjunction with XANES data. In contrast to many experiments at a synchrotron facility, powder diffraction is a relatively simple and user-friendly technique, and most of the procedures and software for data analysis

  2. Determination of dynamic characteristics of multi-layer carbon plastic structures of high-resolution scanner

    Directory of Open Access Journals (Sweden)

    В. Н. Маслей

    2017-10-01

    Full Text Available The comparative analysis results for the numerical determination of the dynamic characteristics of multi-layer carbon-fiber plates of the space vehicle scanner design by various types of finite element approximation of the physico-mechanical properties of the composite material are presented. Using the topological structure of the construction of reinforcing layers material in the plate package plane, experimental data for the elastic and mass characteristics of homogeneous carbon-fiber fibers, equivalent structural and orthotropic stiffness and elastic characteristics of the material of composite plates are determined.

  3. Utilization of paramagnetic relaxation enhancements for high-resolution NMR structure determination of a soluble loop-rich protein with sparse NOE distance restraints

    International Nuclear Information System (INIS)

    Furuita, Kyoko; Kataoka, Saori; Sugiki, Toshihiko; Hattori, Yoshikazu; Kobayashi, Naohiro; Ikegami, Takahisa; Shiozaki, Kazuhiro; Fujiwara, Toshimichi; Kojima, Chojiro

    2015-01-01

    NMR structure determination of soluble proteins depends in large part on distance restraints derived from NOE. In this study, we examined the impact of paramagnetic relaxation enhancement (PRE)-derived distance restraints on protein structure determination. A high-resolution structure of the loop-rich soluble protein Sin1 could not be determined by conventional NOE-based procedures due to an insufficient number of NOE restraints. By using the 867 PRE-derived distance restraints obtained from the NOE-based structure determination procedure, a high-resolution structure of Sin1 could be successfully determined. The convergence and accuracy of the determined structure were improved by increasing the number of PRE-derived distance restraints. This study demonstrates that PRE-derived distance restraints are useful in the determination of a high-resolution structure of a soluble protein when the number of NOE constraints is insufficient

  4. Structure of high-resolution NMR spectra

    CERN Document Server

    Corio, PL

    2012-01-01

    Structure of High-Resolution NMR Spectra provides the principles, theories, and mathematical and physical concepts of high-resolution nuclear magnetic resonance spectra.The book presents the elementary theory of magnetic resonance; the quantum mechanical theory of angular momentum; the general theory of steady state spectra; and multiple quantum transitions, double resonance and spin echo experiments.Physicists, chemists, and researchers will find the book a valuable reference text.

  5. Fully convergent chemical synthesis of ester insulin: determination of the high resolution X-ray structure by racemic protein crystallography.

    Science.gov (United States)

    Avital-Shmilovici, Michal; Mandal, Kalyaneswar; Gates, Zachary P; Phillips, Nelson B; Weiss, Michael A; Kent, Stephen B H

    2013-02-27

    Efficient total synthesis of insulin is important to enable the application of medicinal chemistry to the optimization of the properties of this important protein molecule. Recently we described "ester insulin"--a novel form of insulin in which the function of the 35 residue C-peptide of proinsulin is replaced by a single covalent bond--as a key intermediate for the efficient total synthesis of insulin. Here we describe a fully convergent synthetic route to the ester insulin molecule from three unprotected peptide segments of approximately equal size. The synthetic ester insulin polypeptide chain folded much more rapidly than proinsulin, and at physiological pH. Both the D-protein and L-protein enantiomers of monomeric DKP ester insulin (i.e., [Asp(B10), Lys(B28), Pro(B29)]ester insulin) were prepared by total chemical synthesis. The atomic structure of the synthetic ester insulin molecule was determined by racemic protein X-ray crystallography to a resolution of 1.6 Å. Diffraction quality crystals were readily obtained from the racemic mixture of {D-DKP ester insulin + L-DKP ester insulin}, whereas crystals were not obtained from the L-ester insulin alone even after extensive trials. Both the D-protein and L-protein enantiomers of monomeric DKP ester insulin were assayed for receptor binding and in diabetic rats, before and after conversion by saponification to the corresponding DKP insulin enantiomers. L-DKP ester insulin bound weakly to the insulin receptor, while synthetic L-DKP insulin derived from the L-DKP ester insulin intermediate was fully active in binding to the insulin receptor. The D- and L-DKP ester insulins and D-DKP insulin were inactive in lowering blood glucose in diabetic rats, while synthetic L-DKP insulin was fully active in this biological assay. The structural basis of the lack of biological activity of ester insulin is discussed.

  6. High-resolution noise substitution to measure overfitting and validate resolution in 3D structure determination by single particle electron cryomicroscopy

    International Nuclear Information System (INIS)

    Chen, Shaoxia; McMullan, Greg; Faruqi, Abdul R.; Murshudov, Garib N.; Short, Judith M.; Scheres, Sjors H.W.; Henderson, Richard

    2013-01-01

    Three-dimensional (3D) structure determination by single particle electron cryomicroscopy (cryoEM) involves the calculation of an initial 3D model, followed by extensive iterative improvement of the orientation determination of the individual particle images and the resulting 3D map. Because there is much more noise than signal at high resolution in the images, this creates the possibility of noise reinforcement in the 3D map, which can give a false impression of the resolution attained. The balance between signal and noise in the final map at its limiting resolution depends on the image processing procedure and is not easily predicted. There is a growing awareness in the cryoEM community of how to avoid such over-fitting and over-estimation of resolution. Equally, there has been a reluctance to use the two principal methods of avoidance because they give lower resolution estimates, which some people believe are too pessimistic. Here we describe a simple test that is compatible with any image processing protocol. The test allows measurement of the amount of signal and the amount of noise from overfitting that is present in the final 3D map. We have applied the method to two different sets of cryoEM images of the enzyme beta-galactosidase using several image processing packages. Our procedure involves substituting the Fourier components of the initial particle image stack beyond a chosen resolution by either the Fourier components from an adjacent area of background, or by simple randomisation of the phases of the particle structure factors. This substituted noise thus has the same spectral power distribution as the original data. Comparison of the Fourier Shell Correlation (FSC) plots from the 3D map obtained using the experimental data with that from the same data with high-resolution noise (HR-noise) substituted allows an unambiguous measurement of the amount of overfitting and an accompanying resolution assessment. A simple formula can be used to calculate an

  7. High-resolution noise substitution to measure overfitting and validate resolution in 3D structure determination by single particle electron cryomicroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Shaoxia; McMullan, Greg; Faruqi, Abdul R.; Murshudov, Garib N.; Short, Judith M.; Scheres, Sjors H.W.; Henderson, Richard, E-mail: rh15@mrc-lmb.cam.ac.uk

    2013-12-15

    Three-dimensional (3D) structure determination by single particle electron cryomicroscopy (cryoEM) involves the calculation of an initial 3D model, followed by extensive iterative improvement of the orientation determination of the individual particle images and the resulting 3D map. Because there is much more noise than signal at high resolution in the images, this creates the possibility of noise reinforcement in the 3D map, which can give a false impression of the resolution attained. The balance between signal and noise in the final map at its limiting resolution depends on the image processing procedure and is not easily predicted. There is a growing awareness in the cryoEM community of how to avoid such over-fitting and over-estimation of resolution. Equally, there has been a reluctance to use the two principal methods of avoidance because they give lower resolution estimates, which some people believe are too pessimistic. Here we describe a simple test that is compatible with any image processing protocol. The test allows measurement of the amount of signal and the amount of noise from overfitting that is present in the final 3D map. We have applied the method to two different sets of cryoEM images of the enzyme beta-galactosidase using several image processing packages. Our procedure involves substituting the Fourier components of the initial particle image stack beyond a chosen resolution by either the Fourier components from an adjacent area of background, or by simple randomisation of the phases of the particle structure factors. This substituted noise thus has the same spectral power distribution as the original data. Comparison of the Fourier Shell Correlation (FSC) plots from the 3D map obtained using the experimental data with that from the same data with high-resolution noise (HR-noise) substituted allows an unambiguous measurement of the amount of overfitting and an accompanying resolution assessment. A simple formula can be used to calculate an

  8. High-resolution noise substitution to measure overfitting and validate resolution in 3D structure determination by single particle electron cryomicroscopy.

    Science.gov (United States)

    Chen, Shaoxia; McMullan, Greg; Faruqi, Abdul R; Murshudov, Garib N; Short, Judith M; Scheres, Sjors H W; Henderson, Richard

    2013-12-01

    Three-dimensional (3D) structure determination by single particle electron cryomicroscopy (cryoEM) involves the calculation of an initial 3D model, followed by extensive iterative improvement of the orientation determination of the individual particle images and the resulting 3D map. Because there is much more noise than signal at high resolution in the images, this creates the possibility of noise reinforcement in the 3D map, which can give a false impression of the resolution attained. The balance between signal and noise in the final map at its limiting resolution depends on the image processing procedure and is not easily predicted. There is a growing awareness in the cryoEM community of how to avoid such over-fitting and over-estimation of resolution. Equally, there has been a reluctance to use the two principal methods of avoidance because they give lower resolution estimates, which some people believe are too pessimistic. Here we describe a simple test that is compatible with any image processing protocol. The test allows measurement of the amount of signal and the amount of noise from overfitting that is present in the final 3D map. We have applied the method to two different sets of cryoEM images of the enzyme beta-galactosidase using several image processing packages. Our procedure involves substituting the Fourier components of the initial particle image stack beyond a chosen resolution by either the Fourier components from an adjacent area of background, or by simple randomisation of the phases of the particle structure factors. This substituted noise thus has the same spectral power distribution as the original data. Comparison of the Fourier Shell Correlation (FSC) plots from the 3D map obtained using the experimental data with that from the same data with high-resolution noise (HR-noise) substituted allows an unambiguous measurement of the amount of overfitting and an accompanying resolution assessment. A simple formula can be used to calculate an

  9. High resolution interface nanochemistry and structure

    International Nuclear Information System (INIS)

    1993-01-01

    A summary is given of results on nanospectroscopy etc. during the previous three years, divided into the following subsections: development of methods and instrumentation for interface/boundary chemical analysis, interface and boundary structure in ceramic matrix composites, quantitative composition measurements of thin films and inclusions, theoretical calculations for electron energy loss near edge fine structure and grain boundary structure, and small probe radiation effects in ceramics. Materials studied include SiC whisker-reinforced Si3N4, SiC, Si oxides, Si, Si oxynitride, other ceramics. Methods mentioned include field emission, EELS (electron energy loss spectroscopy), nanospectroscopy, electron nanoprobe, etc

  10. Multi element high resolution scintillator structure

    International Nuclear Information System (INIS)

    Cusano, D.A.

    1980-01-01

    A gamma camera scintillator structure, suitable for detecting high energy gamma photons which, in a single scintillator camera, would require a comparatively thick scintillator crystal, so resulting in unacceptable dispersion of light photons, comprises a collimator array of a high Z material with elongated, parallel wall channels with the scintillator material being disposed in one end of the channels so as to form an integrated collimator/scintillator structure. The collimator channel walls are preferably coated with light reflective material and further light reflective surfaces being translucent to gamma photons, may be provided in each channel. The scintillators may be single crystals or preferably comprise a phosphor dispersed in a thermosetting translucent matrix as disclosed in GB2012800A. The light detectors of the assembled camera may be photomultiplier tubes charge coupled devices or charge injection devices. (author)

  11. Structure Identification in High-Resolution Transmission Electron Microscopic Images

    DEFF Research Database (Denmark)

    Vestergaard, Jacob Schack; Kling, Jens; Dahl, Anders Bjorholm

    2014-01-01

    A connection between microscopic structure and macroscopic properties is expected for almost all material systems. High-resolution transmission electron microscopy is a technique offering insight into the atomic structure, but the analysis of large image series can be time consuming. The present ...

  12. Human enamel structure studied by high resolution electron microscopy

    International Nuclear Information System (INIS)

    Wen, S.L.

    1989-01-01

    Human enamel structural features are characterized by high resolution electron microscopy. The human enamel consists of polycrystals with a structure similar to Ca10(PO4)6(OH)2. This article describes the structural features of human enamel crystal at atomic and nanometer level. Besides the structural description, a great number of high resolution images are included. Research into the carious process in human enamel is very important for human beings. This article firstly describes the initiation of caries in enamel crystal at atomic and unit-cell level and secondly describes the further steps of caries with structural and chemical demineralization. The demineralization in fact, is the origin of caries in human enamel. The remineralization of carious areas in human enamel has drawn more and more attention as its potential application is realized. This process has been revealed by high resolution electron microscopy in detail in this article. On the other hand, the radiation effects on the structure of human enamel are also characterized by high resolution electron microscopy. In order to reveal this phenomenon clearly, a great number of electron micrographs have been shown, and a physical mechanism is proposed. 26 references

  13. High-resolution structure of the native histone octamer

    International Nuclear Information System (INIS)

    Wood, Christopher M.; Nicholson, James M.; Lambert, Stanley J.; Chantalat, Laurent; Reynolds, Colin D.; Baldwin, John P.

    2005-01-01

    The high-resolution (1.90 Å) model of the native histone octamer allows structural comparisons to be made with the nucleosome-core particle, along with an identification of a likely core-histone binding site. Crystals of native histone octamers (H2A–H2B)–(H4–H3)–(H3′–H4′)–(H2B′–H2A′) from chick erythrocytes in 2 M KCl, 1.35 M potassium phosphate pH 6.9 diffract X-rays to 1.90 Å resolution, yielding a structure with an R work value of 18.7% and an R free of 22.2%. The crystal space group is P6 5 , the asymmetric unit of which contains one complete octamer. This high-resolution model of the histone-core octamer allows further insight into intermolecular interactions, including water molecules, that dock the histone dimers to the tetramer in the nucleosome-core particle and have relevance to nucleosome remodelling. The three key areas analysed are the H2A′–H3–H4 molecular cluster (also H2A–H3′–H4′), the H4–H2B′ interaction (also H4′–H2B) and the H2A′–H4 β-sheet interaction (also H2A–H4′). The latter of these three regions is important to nucleosome remodelling by RNA polymerase II, as it is shown to be a likely core-histone binding site, and its disruption creates an instability in the nucleosome-core particle. A majority of the water molecules in the high-resolution octamer have positions that correlate to similar positions in the high-resolution nucleosome-core particle structure, suggesting that the high-resolution octamer model can be used for comparative studies with the high-resolution nucleosome-core particle

  14. Free radicals. High-resolution spectroscopy and molecular structure

    International Nuclear Information System (INIS)

    Hirota, E.

    1983-01-01

    High-resolution, high-sensitivity spectroscopy using CW laser and microwave sources has been applied to free radicals and transient molecules to establish their existence and to explore their properties in detail. The radicals studied were mainly generated by discharge-induced reactions. A few molecules are used as typical examples to illustrate the results so far obtained. The molecular and electronic structures of free radicals, intramolecular motions of large amplitudes in some labile molecules, and metastable electronic states of carbenes are given special emphasis. The significance of the present spectroscopic results in other related fields such as astronomy and atmospheric chemistry is stressed. 4 figures, 3 tables

  15. Determination of radium-226 by high-resolution alpha spectrometry

    International Nuclear Information System (INIS)

    Sill, C.W.

    1983-01-01

    Condition were determined under which high resolution and accurate and reliable results can be obtained. Refractory solids are dissolved completely by fusion with KF and Ba-133 tracer. The fluoride cake is then transposed with sulfuric acid to a pyrosulfate fusion. Radium is precipitated with barium by addition of lead perchlorate to a dilute HCl solution of the pyrosulfate cake. The resulting insoluble sulfates are dissolved in an alkaline solution of DTPA and the Ra and Ba sulfates are reprecipitated with acetic acid to produce very small crystals. The precipitate is mounted on 0.1-μm membrane filter and analyzed by alpha spectrometry. Water samples are partially evaporated and treated similarly. Resolution, almost as good as with actinides electrodeposited on polished steel plates, is about 60 keV full-width-half-maximum with 100 μg of barium on a 1-inch filter with a 450 mm 2 detector at 20% counting efficiency. Recovery is about 97%. One solid sample can be prepared for counting in less than 2 hours. Methods are discussed for ensuring reliability of the results. Severe contamination of the surface-barrier detector by polonium-210 and recoil products is discussed

  16. Determination of radium-226 by high-resolution alpha spectrometry

    International Nuclear Information System (INIS)

    Sill, C.W.

    1983-01-01

    The determination of radium-226 by alpha spectrometry has been investigated critically to determine experimental conditions under which high resolution and accurate and reliable results can be obtained. Refractory solids such as soils, ores, and tailings from uranium mills are dissolved completely by fusion with potassium fluoride in the presence of barium-133 tracer. The fluoride cake is then transposed with sulfuric acid to a pyrosulfate fusion with simultaneous volatilization of all silica and fluoride. Radium is precipitated with barium already present in the sample by addition of lead perchlorate to a dilute hydrochloric acid solution of the pyrosulfate cake. The resulting insoluble sulfates are dissolved in an alkaline solution of diethylenetriaminepentaacetic acid, and the radium and barium sulfates are reprecipitated with acetic acid. The precipitate is mounted on a membrane filter and analyzed by alpha spectrometry. Water samples are partially evaporated and treated similarly. Resolution of the subsequent alpha spectra is much better than has been achieved previously from barium sulfate, and is almost as good as is obtainable with actinides electrodeposited on polished steel plates. The resolution is about 60 keV full-width-half-maximum with 100 μg of barium on a 1-inch filter with a 450 mm 2 detector at 20% counting efficiency. Recovery is about 97% and accuracy is generally as good as the counting statistics obtained will permit. Grossly inaccurate results can be obtained under certain conditions when barium-133 tracer is used to determine the chemical yield of radium-226. Severe contamination of the surface-barrier detector by polonium-210 and by recoil products of the radium isotopes being counted is demonstrated, amd methods for virtual elimination of both problems are discussed

  17. Simultaneous Speciation, Structure, and Equilibrium Constant Determination in the Ni2+-EDTA-CN- Ternary System via High-Resolution Laboratory X-ray Absorption Fine Structure Spectroscopy and Theoretical Calculations.

    Science.gov (United States)

    Bajnóczi, Éva G; Németh, Zoltán; Vankó, György

    2017-11-20

    Even quite simple chemical systems can involve many components and chemical states, and sometimes it can be very difficult to differentiate them by their hardly separable physical-chemical properties. The Ni II -EDTA-CN - (EDTA = ethylenediaminetetraacetic acid) ternary system is a good example for this problem where, in spite of its fairly simple components and numerous investigations, several molecular combinations can exist, all of them not having been identified unambiguously yet. In order to achieve a detailed understanding of the reaction steps and chemical equilibria, methods are required in which the structural transitions in the different reaction steps can be followed via element-selective complex spectral feature sets. With the help of our recently developed von Hámos type high-resolution laboratory X-ray absorption spectrometer, both the structural variations and stability constants of the forming complexes were determined from the same measurement series, proving that X-ray absorption spectroscopy can be considered as a multifaced, table-top tool in coordination chemistry. Furthermore, with the help of theoretical calculations, independent structural evidence was also given for the formation of the [NiEDTA(CN)] 3- mixed complex.

  18. Topographic precursors and geological structures of deep-seated catastrophic landslides caused by typhoon Talas, determined from the analysis of high-resolution DEMs

    Science.gov (United States)

    Chigira, Masahiro; Tsou, Ching-Ying; Matsushi, Yuki

    2013-04-01

    Typhoon Talas crossed the Japanese Islands between 2 and 5 September 2011, causing more than 70 deep-seated catastrophic landslides in a Jurassic to Paleogene-Early Miocene accretion complex. Detailed examination of the topographic features of 10 large landslides before the event, recorded on DEMs with a resolution of 1 m (based on airborne laser scanner surveys), showed that all of the landslides had small scarplets near their future crowns prior to the slide, and one landslide had linear depressions along its future crown as precursor topographic features. These scarplets and linear depressions were caused by gravitational slope deformation that preceded the catastrophic failure. Strains, defined by the ratio of the length of a scarplet to the length of the whole slope (as measured along the slope line), ranged from 5% to 21%, and are the first reliable numerical data relating to the topographic precursor features of large and catastrophic landslides. Careful examination of aerial photographs from another four large landslides, for which no high-resolution DEMs were available, suggested that they also developed scarplets at their heads beforehand, which are not precisely quantified. Twelve of the 14 landslides we surveyed in the field had sliding surfaces with wedge-shaped discontinuities that consisted of faults, shear surfaces that formed during accretion, and bedding, suggesting that the buildup of pore pressure occurs readily in a gravitationally deformed rock body containing wedge-shaped discontinuities. Other types of gravitational deformation were also active; e.g., flexural toppling and buckling were each observed to have preceded one landslide.

  19. High-Resolution Reciprocal Space Mapping for Characterizing Deformation Structures

    DEFF Research Database (Denmark)

    Pantleon, Wolfgang; Wejdemann, Christian; Jakobsen, Bo

    2014-01-01

    With high-angular resolution three-dimensional X-ray diffraction (3DXRD), quantitative information is gained about dislocation structures in individual grains in the bulk of a macroscopic specimen by acquiring reciprocal space maps. In high-resolution 3D reciprocal space maps of tensile......-deformed copper, individual, almost dislocation-free subgrains are identified from high-intensity peaks and distinguished by their unique combination of orientation and elastic strain; dislocation walls manifest themselves as a smooth cloud of lower intensity. The elastic strain shows only minor variations within...... dynamics is followed in situ during varying loading conditions by reciprocal space mapping: during uninterrupted tensile deformation, formation of subgrains is observed concurrently with broadening of Bragg reflections shortly after the onset of plastic deformation. When the traction is terminated, stress...

  20. HCN Polymers: Toward Structure Comprehension Using High Resolution Mass Spectrometry

    Science.gov (United States)

    Bonnet, Jean-Yves; Thissen, Roland; Frisari, Ma; Vuitton, Veronique; Quirico, Eric; Le Roy, Léna; Fray, Nicolas; Cottin, Hervé; Horst, Sarah; Yelle, Roger

    A lot of solar system materials, including cometary ices and Titan aerosols, contain dark matter that can be interpreted as complex nitrogen bearing organic matter [1]. In laboratory experi-ments, HCN polymers are thus analogs of great interest. In fact they may be present in Titan atmosphere and in comet nuclei and then reprocessed as a CN distributed source [2], when ices began to sublimate and ejects from the nucleus organic matter grains [3]. The presence of HCN polymers is suggested because HCN molecule has been directly observed in 1P/Halley comet [4] and others. HCN polymers are also of prebiotic interest [5] as it can form amino acid under hydrolysis conditions. Even if they have been studied during the last decades, their chemical composition and structure are still poorly understood, and a great analytical effort has to be continued. In this way we present a high resolution mass spectrometry (HRMS) and a high resolution tandem mass spectrometry (MS/HRMS) analysis of HCN polymers. It was shown [6] that this is a suitable technique to elucidate composition and structure of the soluble part of tholins analogs of Titan's atmosphere aerosols. HCN polymers have never been studied by HRMS, thus we used a LTQ-Orbitrap XL high resolution mass spectrometer to analyse the HCN polymers. These are produced at LISA by direct polymerisation of pure liquid HCN, catalyzed by ammonia. HCN polymers have been completely dissolved in methanol and then injected in the mass spectrometer by ElectroSpray Ionization (ESI). This atmospheric pressure ionization process produces protonated or deprotonated ions, but it does not fragment molecules. Thus HRMS, allows a direct access to the stoechiometry of all the ionizable molecules present in the samples. Fragmentation analyses (MS/MS) of selected ions have also been performed. Thess analysis provide information about the different chemical fonctionnalities present in HCN poly-mers and also about their structure. Thus we are able to

  1. Determination of the usage factor of components after cyclic loading using high-resolution microstructural investigations

    International Nuclear Information System (INIS)

    Seibold, A.; Scheibe, A.; Assmann, H.D.

    1989-01-01

    The usage factor can be derived from the quantification of the structure changes and the allocation of the microstructural state to the fatigue curves of the component materials. Using the example of the low alloy fine grain structural steel 20 Mn Mo Ni 5 5 (annealed structure), the relationship between micro-structure and the number of load cycles is shown in the form of a calibration curve. By high resolution structural investigation, the usage factor can be determined to n = N/N B ≅ 0.5 under given vibration stress. Only a small volume sample is required for the electron microscope examination. (orig./DG) [de

  2. Structure recognition from high resolution images of ceramic composites

    Energy Technology Data Exchange (ETDEWEB)

    Ushizima, Daniela; Perciano, Talita; Krishnan, Harinarayan; Loring, Burlen; Bale, Hrishikesh; Parkinson, Dilworth; Sethian, James

    2015-01-05

    Fibers provide exceptional strength-to-weight ratio capabilities when woven into ceramic composites, transforming them into materials with exceptional resistance to high temperature, and high strength combined with improved fracture toughness. Microcracks are inevitable when the material is under strain, which can be imaged using synchrotron X-ray computed micro-tomography (mu-CT) for assessment of material mechanical toughness variation. An important part of this analysis is to recognize fibrillar features. This paper presents algorithms for detecting and quantifying composite cracks and fiber breaks from high-resolution image stacks. First, we propose recognition algorithms to identify the different structures of the composite, including matrix cracks and fibers breaks. Second, we introduce our package F3D for fast filtering of large 3D imagery, implemented in OpenCL to take advantage of graphic cards. Results show that our algorithms automatically identify micro-damage and that the GPU-based implementation introduced here takes minutes, being 17x faster than similar tools on a typical image file.

  3. Microwave structure of quiescent solar filaments at high resolution

    International Nuclear Information System (INIS)

    Gary, D.E.

    1986-01-01

    High resolution very low altitude maps of a quiescent filament at three frequencies are presented. The spatial resolution (approx. 15'' at 1.45 GHz, approx. 6'' at 4.9 GHz, and approx. 2'' at 15 GHz) is several times better than previously attained. At each frequency, the filament appears as a depression in the quiet Sun background. The depression is measurably wider and longer in extent than the corresponding H alpha filament at 1.45 GHz and 4.9 GHz, indicating that the depression is due in large part to a deficit in coronal density associated with the filament channel. In contrast, the shape of the radio depression at 15 CHz closely matches that of the H alpha filament. In addition, the 15 GHz map shows enhanced emission along both sides of the radio depression. A similar enhancement is seen in an observation of a second filament 4 days later, which suggests that the enhancement is a general feature of filaments. Possible causes of the enhanced emission are explored

  4. High-resolution X-ray crystal structure of bovine H-protein using the high-pressure cryocooling method

    International Nuclear Information System (INIS)

    Higashiura, Akifumi; Ohta, Kazunori; Masaki, Mika; Sato, Masaru; Inaka, Koji; Tanaka, Hiroaki; Nakagawa, Atsushi

    2013-01-01

    Using the high-pressure cryocooling method, the high-resolution X-ray crystal structure of bovine H-protein was determined at 0.86 Å resolution. This is the first ultra-high-resolution structure obtained from a high-pressure cryocooled crystal. Recently, many technical improvements in macromolecular X-ray crystallography have increased the number of structures deposited in the Protein Data Bank and improved the resolution limit of protein structures. Almost all high-resolution structures have been determined using a synchrotron radiation source in conjunction with cryocooling techniques, which are required in order to minimize radiation damage. However, optimization of cryoprotectant conditions is a time-consuming and difficult step. To overcome this problem, the high-pressure cryocooling method was developed (Kim et al., 2005 ▶) and successfully applied to many protein-structure analyses. In this report, using the high-pressure cryocooling method, the X-ray crystal structure of bovine H-protein was determined at 0.86 Å resolution. Structural comparisons between high- and ambient-pressure cryocooled crystals at ultra-high resolution illustrate the versatility of this technique. This is the first ultra-high-resolution X-ray structure obtained using the high-pressure cryocooling method

  5. High-Resolution Structural Monitoring of Ionospheric Absorption Events

    Science.gov (United States)

    2013-07-01

    7 riometry. Incorporation of an outrigger site, to enable treatment of the unknown structure of the celestial background and the effects of...riometry. Incorporation of an outrigger site, to enable treatment of the unknown structure of the celestial background and the effects of confusion...event captured with this system . Note that, even at this fairly coarse resolution, there is discrete structure that changes in position and strength

  6. High Resolution Studies of the Structure of the Solar Atmosphere

    Science.gov (United States)

    1993-08-04

    the variable emission from active regions", submitted to Solar Phys., August 1993. M. Karovska and F. Blundell, "The fine structure at the limb in a ...in a coronal hole", in preparation. 3.2 Conference Presentations M. Karovska , S. R. Habbal and F. Blundell, "Fine structure at the limb in a coronal...hole", 181st AAS Meeting, Phoenix, Arizona, January 1993. M. Karovska , "Exploring the dynamical structure at the limb in a coronal hole, 24th Solar

  7. High-resolution NMR structures of the domains of Saccharomyces cerevisiae Tho1

    International Nuclear Information System (INIS)

    Jacobsen, Julian O. B.; Allen, Mark D.; Freund, Stefan M. V.; Bycroft, Mark

    2016-01-01

    In this study, high-resolution structures of both the N-terminal DNA-binding SAP domain and the C-terminal RNA-binding domain of S. cerevisiae Tho1 have been determined. THO is a multi-protein complex involved in the formation of messenger ribonuclear particles (mRNPs) by coupling transcription with mRNA processing and export. THO is thought to be formed from five subunits, Tho2p, Hpr1p, Tex1p, Mft1p and Thp2p, and recent work has determined a low-resolution structure of the complex [Poulsen et al. (2014 ▸), PLoS One, 9, e103470]. A number of additional proteins are thought to be involved in the formation of mRNP in yeast, including Tho1, which has been shown to bind RNA in vitro and is recruited to actively transcribed chromatin in vivo in a THO-complex and RNA-dependent manner. Tho1 is known to contain a SAP domain at the N-terminus, but the ability to suppress the expression defects of the hpr1Δ mutant of THO was shown to reside in the RNA-binding C-terminal region. In this study, high-resolution structures of both the N-terminal DNA-binding SAP domain and C-terminal RNA-binding domain have been determined

  8. High-resolution NMR structures of the domains of Saccharomyces cerevisiae Tho1

    Energy Technology Data Exchange (ETDEWEB)

    Jacobsen, Julian O. B.; Allen, Mark D.; Freund, Stefan M. V.; Bycroft, Mark, E-mail: mxb@mrc-lmb.cam.ac.uk [MRC Laboratory of Molecular Biology, Hills Road, Cambridge CB2 0QH (United Kingdom)

    2016-05-23

    In this study, high-resolution structures of both the N-terminal DNA-binding SAP domain and the C-terminal RNA-binding domain of S. cerevisiae Tho1 have been determined. THO is a multi-protein complex involved in the formation of messenger ribonuclear particles (mRNPs) by coupling transcription with mRNA processing and export. THO is thought to be formed from five subunits, Tho2p, Hpr1p, Tex1p, Mft1p and Thp2p, and recent work has determined a low-resolution structure of the complex [Poulsen et al. (2014 ▸), PLoS One, 9, e103470]. A number of additional proteins are thought to be involved in the formation of mRNP in yeast, including Tho1, which has been shown to bind RNA in vitro and is recruited to actively transcribed chromatin in vivo in a THO-complex and RNA-dependent manner. Tho1 is known to contain a SAP domain at the N-terminus, but the ability to suppress the expression defects of the hpr1Δ mutant of THO was shown to reside in the RNA-binding C-terminal region. In this study, high-resolution structures of both the N-terminal DNA-binding SAP domain and C-terminal RNA-binding domain have been determined.

  9. Water polygons in high-resolution protein crystal structures.

    Science.gov (United States)

    Lee, Jonas; Kim, Sung-Hou

    2009-07-01

    We have analyzed the interstitial water (ISW) structures in 1500 protein crystal structures deposited in the Protein Data Bank that have greater than 1.5 A resolution with less than 90% sequence similarity with each other. We observed varieties of polygonal water structures composed of three to eight water molecules. These polygons may represent the time- and space-averaged structures of "stable" water oligomers present in liquid water, and their presence as well as relative population may be relevant in understanding physical properties of liquid water at a given temperature. On an average, 13% of ISWs are localized enough to be visible by X-ray diffraction. Of those, averages of 78% are water molecules in the first water layer on the protein surface. Of the localized ISWs beyond the first layer, almost half of them form water polygons such as trigons, tetragons, as well as expected pentagons, hexagons, higher polygons, partial dodecahedrons, and disordered networks. Most of the octagons and nanogons are formed by fusion of smaller polygons. The trigons are most commonly observed. We suggest that our observation provides an experimental basis for including these water polygon structures in correlating and predicting various water properties in liquid state.

  10. High resolution soil moisture radiometer. [large space structures

    Science.gov (United States)

    Wilheit, T. T.

    1978-01-01

    An electrically scanned pushbroom phased antenna array is described for a microwave radiometer which can provide agriculturally meaningful measurements of soil moisture. The antenna size of 100 meters at 1400 MHz or 230 meters at 611 MHz requires several shuttle launches and orbital assembly. Problems inherent to the size of the structure and specific instrument problems are discussed as well as the preliminary design.

  11. High Resolutions Studies of the Structure of the Solar Atmosphere

    Science.gov (United States)

    1992-06-30

    Regions", manuscript in preparation. M. Karovska , F. Blundell and S. R. Habbal, "Fine Scale Structure of the Solar Limb in a Coronal Hole", manuscript in...Astrophysical Observatory RIPORr MUMUR Smithsonian Institution AFOSR-TR- 2 0 9 1 MS 15 - 60 Garden Street Cambridge, 1; A 02138 SD. U sC,, i~ro AGENCY NAMI(S...visited the Solar and Stellar Physics Division for three months, and with Dr. Ruth Esser who has recently joined the Division as a physicist. 92

  12. High-resolution flow structure measurements in a rod bundle

    Energy Technology Data Exchange (ETDEWEB)

    Ylönen, A. T.

    2013-07-01

    Flow behaviour inside a rod bundle has been an active research topic since the early days of the nuclear power industry. Of particular interest in previous studies have been topics such as flow mixing, two-phase flow structure and mapping of two-phase flow transitions. The optimisation of fuel element design can only be achieved by truly understanding the nature of flow. The ultimate goal in this research is to enhance the heat transfer and increase the critical heat flux, which would improve the fuel economy. A better understanding of the flow would also improve nuclear safety as departure from nucleate boiling (DNB) can be predicted more accurately. The motivation for the current project (SUBFLOW) was to increase knowledge of the complex flow phenomena inside a rod bundle. A dedicated sub-channel flow test facility was designed and constructed at the Paul Scherrer Institut (PSI), Villigen, Switzerland. An adiabatic test loop has an up-scaled (1:2.6) vertical fuel rod bundle model with a 4 × 4 geometry. For the very first time, the wire-mesh sensor measurement technique was implemented in a rod bundle as two 64×64 conductivity wire-mesh sensors were installed in the upper part of the test section. The measurement technique enables one to study single- and two-phase flow behaviour with high spatial and temporal resolution. The research topics addressed in this thesis cover a wide range of flow conditions with and without a spacer grid in a rod bundle. The experimental campaign was started by studying natural mixing of a passive scalar to characterise the development of turbulent diffusion in an injection sub-channel and, later on, cross-mixing between adjacent sub-channels. The results were also used in comparison with the in-house CFD code PSI-Boil that is being developed at PSI. The code could estimate the mixing inside the sub-channel and the transition to cross-mixing with a good accuracy. As a natural transition, the SUBFLOW experiments were continued by

  13. High-resolution flow structure measurements in a rod bundle

    International Nuclear Information System (INIS)

    Ylönen, A. T.

    2013-01-01

    Flow behaviour inside a rod bundle has been an active research topic since the early days of the nuclear power industry. Of particular interest in previous studies have been topics such as flow mixing, two-phase flow structure and mapping of two-phase flow transitions. The optimisation of fuel element design can only be achieved by truly understanding the nature of flow. The ultimate goal in this research is to enhance the heat transfer and increase the critical heat flux, which would improve the fuel economy. A better understanding of the flow would also improve nuclear safety as departure from nucleate boiling (DNB) can be predicted more accurately. The motivation for the current project (SUBFLOW) was to increase knowledge of the complex flow phenomena inside a rod bundle. A dedicated sub-channel flow test facility was designed and constructed at the Paul Scherrer Institut (PSI), Villigen, Switzerland. An adiabatic test loop has an up-scaled (1:2.6) vertical fuel rod bundle model with a 4 × 4 geometry. For the very first time, the wire-mesh sensor measurement technique was implemented in a rod bundle as two 64×64 conductivity wire-mesh sensors were installed in the upper part of the test section. The measurement technique enables one to study single- and two-phase flow behaviour with high spatial and temporal resolution. The research topics addressed in this thesis cover a wide range of flow conditions with and without a spacer grid in a rod bundle. The experimental campaign was started by studying natural mixing of a passive scalar to characterise the development of turbulent diffusion in an injection sub-channel and, later on, cross-mixing between adjacent sub-channels. The results were also used in comparison with the in-house CFD code PSI-Boil that is being developed at PSI. The code could estimate the mixing inside the sub-channel and the transition to cross-mixing with a good accuracy. As a natural transition, the SUBFLOW experiments were continued by

  14. Advances in high-resolution imaging--techniques for three-dimensional imaging of cellular structures.

    Science.gov (United States)

    Lidke, Diane S; Lidke, Keith A

    2012-06-01

    A fundamental goal in biology is to determine how cellular organization is coupled to function. To achieve this goal, a better understanding of organelle composition and structure is needed. Although visualization of cellular organelles using fluorescence or electron microscopy (EM) has become a common tool for the cell biologist, recent advances are providing a clearer picture of the cell than ever before. In particular, advanced light-microscopy techniques are achieving resolutions below the diffraction limit and EM tomography provides high-resolution three-dimensional (3D) images of cellular structures. The ability to perform both fluorescence and electron microscopy on the same sample (correlative light and electron microscopy, CLEM) makes it possible to identify where a fluorescently labeled protein is located with respect to organelle structures visualized by EM. Here, we review the current state of the art in 3D biological imaging techniques with a focus on recent advances in electron microscopy and fluorescence super-resolution techniques.

  15. High-resolution structure of a retroviral protease folded as a monomer

    International Nuclear Information System (INIS)

    Gilski, Miroslaw; Kazmierczyk, Maciej; Krzywda, Szymon; Zábranská, Helena; Cooper, Seth; Popović, Zoran; Khatib, Firas; DiMaio, Frank; Thompson, James; Baker, David; Pichová, Iva; Jaskolski, Mariusz

    2011-01-01

    The crystal structure of Mason–Pfizer monkey virus protease folded as a monomer has been solved by molecular replacement using a model generated by players of the online game Foldit. The structure shows at high resolution the details of a retroviral protease folded as a monomer which can guide rational design of protease dimerization inhibitors as retroviral drugs. Mason–Pfizer monkey virus (M-PMV), a D-type retrovirus assembling in the cytoplasm, causes simian acquired immunodeficiency syndrome (SAIDS) in rhesus monkeys. Its pepsin-like aspartic protease (retropepsin) is an integral part of the expressed retroviral polyproteins. As in all retroviral life cycles, release and dimerization of the protease (PR) is strictly required for polyprotein processing and virion maturation. Biophysical and NMR studies have indicated that in the absence of substrates or inhibitors M-PMV PR should fold into a stable monomer, but the crystal structure of this protein could not be solved by molecular replacement despite countless attempts. Ultimately, a solution was obtained in mr-rosetta using a model constructed by players of the online protein-folding game Foldit. The structure indeed shows a monomeric protein, with the N- and C-termini completely disordered. On the other hand, the flap loop, which normally gates access to the active site of homodimeric retropepsins, is clearly traceable in the electron density. The flap has an unusual curled shape and a different orientation from both the open and closed states known from dimeric retropepsins. The overall fold of the protein follows the retropepsin canon, but the C α deviations are large and the active-site ‘DTG’ loop (here NTG) deviates up to 2.7 Å from the standard conformation. This structure of a monomeric retropepsin determined at high resolution (1.6 Å) provides important extra information for the design of dimerization inhibitors that might be developed as drugs for the treatment of retroviral infections

  16. High-resolution EELS investigation of the electronic structure of ilmenites

    NARCIS (Netherlands)

    Radtke, G.; Lazar, S.; Botton, G.A.

    2006-01-01

    The electronic structure of a series of compounds belonging to the ilmenite family is investigated using high resolution electron energy loss spectroscopy (EELS). The energy loss near edge structure (ELNES) of the O-K, Ti-L23 and transition metal L23 edges have been recorded in MnTiO3, FeTiO3,

  17. An Optimized, Grid Independent, Narrow Band Data Structure for High Resolution Level Sets

    DEFF Research Database (Denmark)

    Nielsen, Michael Bang; Museth, Ken

    2004-01-01

    enforced by the convex boundaries of an underlying cartesian computational grid. Here we present a novel very memory efficient narrow band data structure, dubbed the Sparse Grid, that enables the representation of grid independent high resolution level sets. The key features our new data structure are...

  18. In-situ investigations of structural changes during cyclic loading by high resolution reciprocal space mapping

    DEFF Research Database (Denmark)

    Diederichs, Annika M.; Thiel, Felix; Lienert, Ulrich

    2017-01-01

    dislocation structures can be identified using advanced electron microscopy and synchrotron techniques. A detailed characterization of the microstructure during cyclic loading by in-situ monitoring the internal structure within individual grains with high energy x-rays can help to understand and predict...... the materials behavior during cyclic deformation and to improve the material design. While monitoring macroscopic stress and strain during cyclic loading, reciprocal space maps of diffraction peaks from single grains are obtained with high resolution. High Resolution Reciprocal Space Mapping was applied...

  19. High-resolution X-ray crystal structure of bovine H-protein using the high-pressure cryocooling method.

    Science.gov (United States)

    Higashiura, Akifumi; Ohta, Kazunori; Masaki, Mika; Sato, Masaru; Inaka, Koji; Tanaka, Hiroaki; Nakagawa, Atsushi

    2013-11-01

    Recently, many technical improvements in macromolecular X-ray crystallography have increased the number of structures deposited in the Protein Data Bank and improved the resolution limit of protein structures. Almost all high-resolution structures have been determined using a synchrotron radiation source in conjunction with cryocooling techniques, which are required in order to minimize radiation damage. However, optimization of cryoprotectant conditions is a time-consuming and difficult step. To overcome this problem, the high-pressure cryocooling method was developed (Kim et al., 2005) and successfully applied to many protein-structure analyses. In this report, using the high-pressure cryocooling method, the X-ray crystal structure of bovine H-protein was determined at 0.86 Å resolution. Structural comparisons between high- and ambient-pressure cryocooled crystals at ultra-high resolution illustrate the versatility of this technique. This is the first ultra-high-resolution X-ray structure obtained using the high-pressure cryocooling method.

  20. Integration of High-Resolution Laser Displacement Sensors and 3D Printing for Structural Health Monitoring

    Directory of Open Access Journals (Sweden)

    Shu-Wei Chang

    2017-12-01

    Full Text Available This paper presents a novel experimental design for complex structural health monitoring (SHM studies achieved by integrating 3D printing technologies, high-resolution laser displacement sensors, and multiscale entropy SHM theory. A seven-story structure with a variety of composite bracing systems was constructed using a dual-material 3D printer. A wireless Bluetooth vibration speaker was used to excite the ground floor of the structure, and high-resolution laser displacement sensors (1-μm resolution were used to monitor the displacement history on different floors. Our results showed that the multiscale entropy SHM method could detect damage on the 3D-printed structures. The results of this study demonstrate that integrating 3D printing technologies and high-resolution laser displacement sensors enables the design of cheap, fast processing, complex, small-scale civil structures for future SHM studies. The novel experimental design proposed in this study provides a suitable platform for investigating the validity and sensitivity of SHM in different composite structures and damage conditions for real life applications in the future.

  1. Integration of High-Resolution Laser Displacement Sensors and 3D Printing for Structural Health Monitoring.

    Science.gov (United States)

    Chang, Shu-Wei; Lin, Tzu-Kang; Kuo, Shih-Yu; Huang, Ting-Hsuan

    2017-12-22

    This paper presents a novel experimental design for complex structural health monitoring (SHM) studies achieved by integrating 3D printing technologies, high-resolution laser displacement sensors, and multiscale entropy SHM theory. A seven-story structure with a variety of composite bracing systems was constructed using a dual-material 3D printer. A wireless Bluetooth vibration speaker was used to excite the ground floor of the structure, and high-resolution laser displacement sensors (1-μm resolution) were used to monitor the displacement history on different floors. Our results showed that the multiscale entropy SHM method could detect damage on the 3D-printed structures. The results of this study demonstrate that integrating 3D printing technologies and high-resolution laser displacement sensors enables the design of cheap, fast processing, complex, small-scale civil structures for future SHM studies. The novel experimental design proposed in this study provides a suitable platform for investigating the validity and sensitivity of SHM in different composite structures and damage conditions for real life applications in the future.

  2. The development of high-resolution spectroscopic methods and their use in atomic structure studies

    International Nuclear Information System (INIS)

    Poulsen, O.

    1984-01-01

    This thesis discusses work performed during the last nine years in the field of atomic spectroscopy. Several high-resolution techniques, ranging from quantum beats, level crossings, rf-laser double resonances to nonlinear field atom interactions, have been employed. In particular, these methods have been adopted and developed to deal with fast accelerated atomic or ionic beams, allowing studies of problems in atomic-structure theory. Fine- and hyperfine-structure determinations in the He I and Li I isoelectronic sequences, in 51 V I, and in 235 U I, II have permitted a detailed comparison with ab initio calculations, demonstrating the change in problems when going towards heavier elements or higher ionization stage. The last part of the thesis is concerned with the fundamental question of obtaining very high optical resolution in the interaction between a fast accelerated atom or ion beam and a laser field, this problem being the core in the continuing development of atomic spectroscopy necessary to challenge the more precise and sophisticated theories advanced. (Auth.)

  3. Determination of accurate 1H positions of an alanine tripeptide with anti-parallel and parallel β-sheet structures by high resolution 1H solid state NMR and GIPAW chemical shift calculation.

    Science.gov (United States)

    Yazawa, Koji; Suzuki, Furitsu; Nishiyama, Yusuke; Ohata, Takuya; Aoki, Akihiro; Nishimura, Katsuyuki; Kaji, Hironori; Shimizu, Tadashi; Asakura, Tetsuo

    2012-11-25

    The accurate (1)H positions of alanine tripeptide, A(3), with anti-parallel and parallel β-sheet structures could be determined by highly resolved (1)H DQMAS solid-state NMR spectra and (1)H chemical shift calculation with gauge-including projector augmented wave calculations.

  4. Design and development of high-resolution atomic beam fluorescence spectroscopy facility for isotope shift and hyperfine structure measurements

    International Nuclear Information System (INIS)

    Acharyulu, G.V.S.G.; Sankari, M.; Kiran Kumar, P.V.; Suryanarayana, M.V.

    2012-01-01

    A high-resolution atomic beam fluorescence spectroscopy facility for the determination of isotope shifts and hyperfine structure in atomic species has been designed and developed. A resistively heated graphite tube atomic beam source was designed, tested and integrated into a compact interaction chamber for atomic beam fluorescence experiments. The design of the laser-atom interaction chamber and the source has been modified in a phased manner so as to achieve sub-Doppler resolution. The system has been used to record the hyperfine spectrum of the D2 transitions of Rb and K isotopes. The spectral resolution achieved is ∼ 26 MHz and is adequate to carry out high resolution measurement of isotope shifts and hyperfine structure of various atomic species. The other major advantage of the source is that it requires very small amounts of sample for achieving very good signal to noise ratio. (author)

  5. The high-resolution extraterrestrial solar spectrum (QASUMEFTS determined from ground-based solar irradiance measurements

    Directory of Open Access Journals (Sweden)

    J. Gröbner

    2017-09-01

    Full Text Available A high-resolution extraterrestrial solar spectrum has been determined from ground-based measurements of direct solar spectral irradiance (SSI over the wavelength range from 300 to 500 nm using the Langley-plot technique. The measurements were obtained at the Izaña Atmospheric Research Centre from the Agencia Estatal de Meteorología, Tenerife, Spain, during the period 12 to 24 September 2016. This solar spectrum (QASUMEFTS was combined from medium-resolution (bandpass of 0.86 nm measurements of the QASUME (Quality Assurance of Spectral Ultraviolet Measurements in Europe spectroradiometer in the wavelength range from 300 to 500 nm and high-resolution measurements (0.025 nm from a Fourier transform spectroradiometer (FTS over the wavelength range from 305 to 380 nm. The Kitt Peak solar flux atlas was used to extend this high-resolution solar spectrum to 500 nm. The expanded uncertainties of this solar spectrum are 2 % between 310 and 500 nm and 4 % at 300 nm. The comparison of this solar spectrum with solar spectra measured in space (top of the atmosphere gave very good agreements in some cases, while in some other cases discrepancies of up to 5 % were observed. The QASUMEFTS solar spectrum represents a benchmark dataset with uncertainties lower than anything previously published. The metrological traceability of the measurements to the International System of Units (SI is assured by an unbroken chain of calibrations leading to the primary spectral irradiance standard of the Physikalisch-Technische Bundesanstalt in Germany.

  6. High-Resolution Printing of 3D Structures Using an Electrohydrodynamic Inkjet with Multiple Functional Inks.

    Science.gov (United States)

    An, Byeong Wan; Kim, Kukjoo; Lee, Heejoo; Kim, So-Yun; Shim, Yulhui; Lee, Dae-Young; Song, Jun Yeob; Park, Jang-Ung

    2015-08-05

    Electrohydrodynamic-inkjet-printed high-resolution complex 3D structures with multiple functional inks are demonstrated. Printed 3D structures can have a variety of fine patterns, such as vertical or helix-shaped pillars and straight or rounded walls, with high aspect ratios (greater than ≈50) and narrow diameters (≈0.7 μm). Furthermore, the formation of freestanding, bridge-like Ag wire structures on plastic substrates suggests substantial potentials as high-precision, flexible 3D interconnects. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. High resolution MR imaging of bladder cancer: new criteria for determining depth of wall invasion

    International Nuclear Information System (INIS)

    Suh, Chang Hae; Kressel, Herbert Y

    1993-01-01

    To establish new criteria to determine the depth of bladder cancer as well as to obtain the findings of each stage of bladder cancer we reviewed high resolution MR images of 18 bladder cancer patients including seven cases (26%) with superficial bladder wall invasion. All MR scans were done before biopsy or surgery. Multiple layers of the bladder wall (inner black, middle white, outer black) were demonstrated in 11 cases out of a total 18 cases. Thickening of the middle layer caused by tumor infiltration or edema of lamina propria was seen in 8 of 12 patients with stage T2 or greater, and was suggestive of superficial muscle invasion when multiple layers were demonstrated. Disruption of outer layer (as well as inner layer) and external protrusion of tumor itself were indicative of perivesical invasion. When multiple layers were not demonstrated, the depth of tumor invasion could not be judged. High resolution MR imaging can depict submucosal invasion, muscle invasion, and perivesical invasion secondary to bladder cancer

  8. 3D high-resolution two-photon crosslinked hydrogel structures for biological studies.

    Science.gov (United States)

    Brigo, Laura; Urciuolo, Anna; Giulitti, Stefano; Della Giustina, Gioia; Tromayer, Maximilian; Liska, Robert; Elvassore, Nicola; Brusatin, Giovanna

    2017-06-01

    Hydrogels are widely used as matrices for cell growth due to the their tuneable chemical and physical properties, which mimic the extracellular matrix of natural tissue. The microfabrication of hydrogels into arbitrarily complex 3D structures is becoming essential for numerous biological applications, and in particular for investigating the correlation between cell shape and cell function in a 3D environment. Micrometric and sub-micrometric resolution hydrogel scaffolds are required to deeply investigate molecular mechanisms behind cell-matrix interaction and downstream cellular processes. We report the design and development of high resolution 3D gelatin hydrogel woodpile structures by two-photon crosslinking. Hydrated structures of lateral linewidth down to 0.5µm, lateral and axial resolution down to a few µm are demonstrated. According to the processing parameters, different degrees of polymerization are obtained, resulting in hydrated scaffolds of variable swelling and deformation. The 3D hydrogels are biocompatible and promote cell adhesion and migration. Interestingly, according to the polymerization degree, 3D hydrogel woodpile structures show variable extent of cell adhesion and invasion. Human BJ cell lines show capability of deforming 3D micrometric resolved hydrogel structures. The design and development of high resolution 3D gelatin hydrogel woodpile structures by two-photon crosslinking is reported. Significantly, topological and mechanical conditions of polymerized gelatin structures were suitable for cell accommodation in the volume of the woodpiles, leading to a cell density per unit area comparable to the bare substrate. The fabricated structures, presenting micrometric features of high resolution, are actively deformed by cells, both in terms of cell invasion within rods and of cell attachment in-between contiguous woodpiles. Possible biological targets for this 3D approach are customized 3D tissue models, or studies of cell adhesion

  9. Homogenization-based topology optimization for high-resolution manufacturable micro-structures

    DEFF Research Database (Denmark)

    Groen, Jeroen Peter; Sigmund, Ole

    2018-01-01

    This paper presents a projection method to obtain high-resolution, manufacturable structures from efficient and coarse-scale, homogenization-based topology optimization results. The presented approach bridges coarse and fine scale, such that the complex periodic micro-structures can be represented...... by a smooth and continuous lattice on the fine mesh. A heuristic methodology allows control of the projected topology, such that a minimum length-scale on both solid and void features is ensured in the final result. Numerical examples show excellent behavior of the method, where performances of the projected...

  10. Evaluation of variability in high-resolution protein structures by global distance scoring

    Directory of Open Access Journals (Sweden)

    Risa Anzai

    2018-01-01

    Full Text Available Systematic analysis of the statistical and dynamical properties of proteins is critical to understanding cellular events. Extraction of biologically relevant information from a set of high-resolution structures is important because it can provide mechanistic details behind the functional properties of protein families, enabling rational comparison between families. Most of the current structural comparisons are pairwise-based, which hampers the global analysis of increasing contents in the Protein Data Bank. Additionally, pairing of protein structures introduces uncertainty with respect to reproducibility because it frequently accompanies other settings for superimposition. This study introduces intramolecular distance scoring for the global analysis of proteins, for each of which at least several high-resolution structures are available. As a pilot study, we have tested 300 human proteins and showed that the method is comprehensively used to overview advances in each protein and protein family at the atomic level. This method, together with the interpretation of the model calculations, provide new criteria for understanding specific structural variation in a protein, enabling global comparison of the variability in proteins from different species.

  11. Evaluation of variability in high-resolution protein structures by global distance scoring.

    Science.gov (United States)

    Anzai, Risa; Asami, Yoshiki; Inoue, Waka; Ueno, Hina; Yamada, Koya; Okada, Tetsuji

    2018-01-01

    Systematic analysis of the statistical and dynamical properties of proteins is critical to understanding cellular events. Extraction of biologically relevant information from a set of high-resolution structures is important because it can provide mechanistic details behind the functional properties of protein families, enabling rational comparison between families. Most of the current structural comparisons are pairwise-based, which hampers the global analysis of increasing contents in the Protein Data Bank. Additionally, pairing of protein structures introduces uncertainty with respect to reproducibility because it frequently accompanies other settings for superimposition. This study introduces intramolecular distance scoring for the global analysis of proteins, for each of which at least several high-resolution structures are available. As a pilot study, we have tested 300 human proteins and showed that the method is comprehensively used to overview advances in each protein and protein family at the atomic level. This method, together with the interpretation of the model calculations, provide new criteria for understanding specific structural variation in a protein, enabling global comparison of the variability in proteins from different species.

  12. Determination of the usage factor of components after cyclic loading by means of high-resolution microstructural examination

    International Nuclear Information System (INIS)

    Seibold, A.; Scheibe, A.; Assmann, H.D.

    1991-01-01

    Materials subjected to cyclic loading experience a change in the microstructure which may affect the service life. Quantification of the microstructural changes and allocation of the microstructural condition to the corresponding point on the fatigue curve for the component material allows the usage factor to be derived. Taking the low-alloy, fine-grained structural steel 20MnMoNi55 (quenched and tempered structure) as an example, the relationship between microstructure and number of load cycles can be represented in the form of a reference curve. High-resolution examination allows the usage factor to be determined up to η=N/N f ≅0.5 under the given cyclic loading. Only a small specimen volume is required for examination using a transmission electron microscope. It can be taken from the component without affecting the required minimum wall thickness. The location of the specimen must, however, be stipulated, e.g. the location of highest loading according to calculations. When removing the specimen, care must be taken to ensure that the micro-structure is not affected. If these requirements are observed, high-resolution microstructural examination provides a method for checking the usage factor of a component. (orig.)

  13. Determination of Polychlorinated Diben-p-dioxins and Dibenzofurans in Flue Gas by High Resolution Gas Chromatography Coupled with High Resolution Spectrometry

    International Nuclear Information System (INIS)

    Chen, T.; Yan, J. H.; Li, X. D.; Cen, K. F.

    2007-01-01

    In 1988 the first municipal solid waste (MSW) incinerator plant was built in Shenzhen, China. Since then Beijing, Shanghai and other big cities have built a few MSW incineration plants. MSW incineration has gradually been used in some cities of China due to its advantages such as significant volume reduction (about 90%), mass reduction (about 70%), and toxicity reduction of the waste and energy recovery. However, MSW incineration is sometimes considered to the general public as the secondary pollution source, because of concerns about is toxic combustion byproducts (TCBs). Polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) are the most toxic compounds among the TCBs. In this paper, PCDD/Fs in flue gas produced from a MSW incinerator were isokinetically withdrawn and collected in a multi component sampling train. Then the PCDD/Fs samples were extracted, concentrated and cleaned up step by step. Finally, the determination of PCDD/Fs was carried out by high-resolution gas chromatography coupled with high-resolution mass spectrometry (HRGC/HRMS). The two PCDD/Fs emission levels were the similar, which was 0.115 and 0.096ng TEQ/Nm3 although different sampling time. The PCDD/Fs emission levels were lower than the PCDD/Fs emission regulation in China (1.0 ng TEQ / Nm3) and close to the developed countries' regulations, i.e., 0.1ng TEQ/Nm3. 2,3,4,7,8-Pentachlorodibenzofuran (2,3,4,7,8-PeCDF) was the dominant congener of the total TEQ

  14. Examination of High Resolution Channel Topography to Determine Suitable Metrics to Characterize Morphological Complexity

    Science.gov (United States)

    Stewart, R. L.; Gaeuman, D.

    2015-12-01

    Complex bed morphology is deemed necessary to restore salmonid habitats, yet quantifiable metrics that capture channel complexity have remained elusive. This work utilizes high resolution topographic data from the 40 miles of the Trinity River of northern California to determine a suitable metric for characterizing morphological complexity at the reach scale. The study area is segregated into reaches defined by individual riffle pool units or aggregates of several consecutive units. Potential measures of complexity include rugosity and depth statistics such as standard deviation and interquartile range, yet previous research has shown these metrics are scale dependent and subject to sampling density-based bias. The effect of sampling density on the present analysis has been reduced by underrepresenting the high resolution topographic data as a 3'x 3' raster so that all areas are equally sampled. Standard rugosity, defined as the three-dimensional surface area divided by projected area, has been shown to be dependent on average depth. We therefore define R*, a empirically depth-corrected rugosity metric in which rugosity is corrected using an empirical relationship based on linear regression between the standard rugosity metric and average depth. By removing the dependence on depth using a regression based on the study reach, R* provides a measure reach scale complexity relative to the entire study area. The interquartile range of depths is also depth-dependent, so we defined a non-dimensional metric (IQR*) as the interquartile range dividing by median depth. These are calculated to develop rankings of channel complexity which, are found to closely agree with perceived channel complexity observed in the field. Current efforts combine these measures of morphological complexity with salmonid habitat suitability to evaluate the effects of channel complexity on the various life stages of salmonids. Future work will investigate the downstream sequencing of channel

  15. Quantifying vegetation distribution and structure using high resolution drone-based structure-from-motion photogrammetry

    Science.gov (United States)

    Zhang, J.; Okin, G.

    2017-12-01

    Vegetation is one of the most important driving factors of different ecosystem processes in drylands. The structure of vegetation controls the spatial distribution of moisture and heat in the canopy and the surrounding area. Also, the structure of vegetation influences both airflow and boundary layer resistance above the land surface. Multispectral satellite remote sensing has been widely used to monitor vegetation coverage and its change; however, it can only capture 2D images, which do not contain the vertical information of vegetation. In situ observation uses different methods to measure the structure of vegetation, and their results are accurate; however, these methods are laborious and time-consuming, and susceptible to undersampling in spatial heterogeneity. Drylands are sparsely covered by short plants, which allows the drone fly at a relatively low height to obtain ultra-high resolution images. Structure-from-motion (SfM) is a photogrammetric method that was proved to produce 3D model based on 2D images. Drone-based remote sensing can obtain the multiangle images for one object, which can be used to constructed 3D models of vegetation in drylands. Using these images detected by the drone, the orthomosaics and digital surface model (DSM) can be built. In this study, the drone-based remote sensing was conducted in Jornada Basin, New Mexico, in the spring of 2016 and 2017, and three derived vegetation parameters (i.e., canopy size, bare soil gap size, and plant height) were compared with those obtained with field measurement. The correlation coefficient of canopy size, bare soil gap size, and plant height between drone images and field data are 0.91, 0.96, and 0.84, respectively. The two-year averaged root-mean-square error (RMSE) of canopy size, bare soil gap size, and plant height between drone images and field data are 0.61 m, 1.21 m, and 0.25 cm, respectively. The two-year averaged measure error (ME) of canopy size, bare soil gap size, and plant height

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

    Science.gov (United States)

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

    2016-10-14

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

  17. An application of impediography to the high sensitivity and high resolution identification of structural damage

    International Nuclear Information System (INIS)

    Zhao, L; Yang, J; Semperlotti, F; Wang, K W

    2015-01-01

    In this study we explore the use of impediographic techniques to perform damage detection in plate-like metal structures. Impediography relies on the piezo-resistive coupling of the host structure to reconstruct high sensitivity and high resolution maps of the internal electrical conductivity. By exploiting localized strain perturbations generated via focused acoustic waves, the piezo-resistive coupling allows extracting a set of linearly independent boundary voltage data that drastically reduces the ill-conditioning of the inverse problem, therefore increasing the performance. The localized perturbation is achieved by leveraging the concept of frequency selective structure (FSS), that is a dynamically tailored structural element enabling the required acoustic focusing via vibration localization. Based on the FSS approach, the impediographic technique is numerically tested to investigate the performance of the combined approach for structural damage detection. The effects of practical implementation issues, such as limited perturbations and limited boundary data, are also explored. (paper)

  18. LTE modeling of inhomogeneous chromospheric structure using high-resolution limb observations

    Science.gov (United States)

    Lindsey, C.

    1987-01-01

    The paper discusses considerations relevant to LTE modeling of rough atmospheres. Particular attention is given to the application of recent high-resolution observations of the solar limb in the far-infrared and radio continuum to the modeling of chromospheric spicules. It is explained how the continuum limb observations can be combined with morphological knowledge of spicule structure to model the physical conditions in chromospheric spicules. This discussion forms the basis for a chromospheric model presented in a parallel publication based on observations ranging from 100 microns to 2.6 mm.

  19. Ultra high resolution tomography

    Energy Technology Data Exchange (ETDEWEB)

    Haddad, W.S.

    1994-11-15

    Recent work and results on ultra high resolution three dimensional imaging with soft x-rays will be presented. This work is aimed at determining microscopic three dimensional structure of biological and material specimens. Three dimensional reconstructed images of a microscopic test object will be presented; the reconstruction has a resolution on the order of 1000 A in all three dimensions. Preliminary work with biological samples will also be shown, and the experimental and numerical methods used will be discussed.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-02-15

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

  1. Structural characterization of suppressor lipids by high-resolution mass spectrometry

    DEFF Research Database (Denmark)

    Rovillos, Mary Joy; Pauling, Josch Konstantin; Hannibal-Bach, Hans Kristian

    2016-01-01

    RATIONALE: Suppressor lipids were originally identified in 1993 and reported to encompass six lipid classes that enable Saccharomyces cerevisiae to live without sphingolipids. Structural characterization, using non-mass spectrometric approaches, revealed that these suppressor lipids are very long...... chain fatty acid (VLCFA)-containing glycerophospholipids with polar head groups that are typically incorporated into sphingolipids. Here we report, for the first time, the structural characterization of the yeast suppressor lipids using high-resolution mass spectrometry. METHODS: Suppressor lipids were...... isolated by preparative chromatography and subjected to structural characterization using hybrid quadrupole time-of-flight and ion trap-orbitrap mass spectrometry. RESULTS: Our investigation recapitulates the overall structural features of the suppressor lipids and provides an in-depth characterization...

  2. [Determination of sulfur in plant using a high-resolution continuum source atomic absorption spectrometer].

    Science.gov (United States)

    Wang, Yu; Li, Jia-xi

    2009-05-01

    A method for the analysis of sulfur (S) in plant by molecular absorption of carbon monosulfide (CS) using a high-resolution continuum source atomic absorption spectrometer (CS AAS) with a fuel-rich air/acetylene flame has been devised. The strong CS absorption band was found around 258 nm. The half-widths of some absorption bands were of the order of picometers, the same as the common atomic absorption lines. The experimental procedure in this study provided optimized instrumental conditions (the ratio of acetylene to air, the burner height) and parameters, and researched the spectral interferences and chemical interferences. The influence of the organic solvents on the CS absorption signals and the different digestion procedures for the determination of sulfur were also investigated. The limit of detection achieved for sulfur was 14 mg x L(-1), using the CS wavelength of 257. 961 nm and a measurement time of 3 s. The accuracy and precision were verified by analysis of two plant standard reference materials. The major applications of this method have been used for the determination of sulfur in plant materials, such as leaves. Compared to the others, this method for the analysis of sulfur is rapid, easy and simple for sulfur determination in plant.

  3. The cyclopropene radical cation: Rovibrational level structure at low energies from high-resolution photoelectron spectra

    Energy Technology Data Exchange (ETDEWEB)

    Vasilatou, K.; Michaud, J. M.; Baykusheva, D.; Grassi, G.; Merkt, F. [Laboratorium für Physikalische Chemie, ETH Zürich, CH-8093 Zurich (Switzerland)

    2014-08-14

    The cyclopropene radical cation (c-C{sub 3}H{sub 4}{sup +}) is an important but poorly characterized three-membered-ring hydrocarbon. We report on a measurement of the high-resolution photoelectron and photoionization spectra of cyclopropene and several deuterated isotopomers, from which we have determined the rovibrational energy level structure of the X{sup ~+} {sup 2}B{sub 2} ground electronic state of c-C{sub 3}H{sub 4}{sup +} at low energies for the first time. The synthesis of the partially deuterated isotopomers always resulted in mixtures of several isotopomers, differing in their number of D atoms and in the location of these atoms, so that the photoelectron spectra of deuterated samples are superpositions of the spectra of several isotopomers. The rotationally resolved spectra indicate a C{sub 2v}-symmetric R{sub 0} structure for the ground electronic state of c-C{sub 3}H{sub 4}{sup +}. Two vibrational modes of c-C{sub 3}H{sub 4}{sup +} are found to have vibrational wave numbers below 300 cm{sup −1}, which is surprising for such a small cyclic hydrocarbon. The analysis of the isotopic shifts of the vibrational levels enabled the assignment of the lowest-frequency mode (fundamental wave number of ≈110 cm{sup −1} in c-C{sub 3}H{sub 4}{sup +}) to the CH{sub 2} torsional mode (ν{sub 8}{sup +}, A{sub 2} symmetry) and of the second-lowest-frequency mode (≈210 cm{sup −1} in c-C{sub 3}H{sub 4}{sup +}) to a mode combining a CH out-of-plane with a CH{sub 2} rocking motion (ν{sub 15}{sup +}, B{sub 2} symmetry). The potential energy along the CH{sub 2} torsional coordinate is flat near the equilibrium structure and leads to a pronounced anharmonicity.

  4. A High-resolution Atlas and Statistical Model of the Vocal Tract from Structural MRI.

    Science.gov (United States)

    Woo, Jonghye; Lee, Junghoon; Murano, Emi Z; Xing, Fangxu; Al-Talib, Meena; Stone, Maureen; Prince, Jerry L

    Magnetic resonance imaging (MRI) is an essential tool in the study of muscle anatomy and functional activity in the tongue. Objective assessment of similarities and differences in tongue structure and function has been performed using unnormalized data, but this is biased by the differences in size, shape, and orientation of the structures. To remedy this, we propose a methodology to build a 3D vocal tract atlas based on structural MRI volumes from twenty normal subjects. We first constructed high-resolution volumes from three orthogonal stacks. We then removed extraneous data so that all 3D volumes contained the same anatomy. We used an unbiased diffeomorphic groupwise registration using a cross-correlation similarity metric. Principal component analysis was applied to the deformation fields to create a statistical model from the atlas. Various evaluations and applications were carried out to show the behaviour and utility of the atlas.

  5. Valence band structure of binary chalcogenide vitreous semiconductors by high-resolution XPS

    International Nuclear Information System (INIS)

    Kozyukhin, S.; Golovchak, R.; Kovalskiy, A.; Shpotyuk, O.; Jain, H.

    2011-01-01

    High-resolution X-ray photoelectron spectroscopy (XPS) is used to study regularities in the formation of valence band electronic structure in binary As x Se 100−x , As x S 100−x , Ge x Se 100−x and Ge x S 100−x chalcogenide vitreous semiconductors. It is shown that the highest occupied energetic states in the valence band of these materials are formed by lone pair electrons of chalcogen atoms, which play dominant role in the formation of valence band electronic structure of chalcogen-rich glasses. A well-expressed contribution from chalcogen bonding p electrons and more deep s orbitals are also recorded in the experimental valence band XPS spectra. Compositional dependences of the observed bands are qualitatively analyzed from structural and compositional points of view.

  6. Valence band structure of binary chalcogenide vitreous semiconductors by high-resolution XPS

    Energy Technology Data Exchange (ETDEWEB)

    Kozyukhin, S., E-mail: sergkoz@igic.ras.ru [Russian Academy of Science, Institute of General and Inorganic Chemistry (Russian Federation); Golovchak, R. [Lviv Scientific Research Institute of Materials of SRC ' Carat' (Ukraine); Kovalskiy, A. [Lehigh University, Department of Materials Science and Engineering (United States); Shpotyuk, O. [Lviv Scientific Research Institute of Materials of SRC ' Carat' (Ukraine); Jain, H. [Lehigh University, Department of Materials Science and Engineering (United States)

    2011-04-15

    High-resolution X-ray photoelectron spectroscopy (XPS) is used to study regularities in the formation of valence band electronic structure in binary As{sub x}Se{sub 100-x}, As{sub x}S{sub 100-x}, Ge{sub x}Se{sub 100-x} and Ge{sub x}S{sub 100-x} chalcogenide vitreous semiconductors. It is shown that the highest occupied energetic states in the valence band of these materials are formed by lone pair electrons of chalcogen atoms, which play dominant role in the formation of valence band electronic structure of chalcogen-rich glasses. A well-expressed contribution from chalcogen bonding p electrons and more deep s orbitals are also recorded in the experimental valence band XPS spectra. Compositional dependences of the observed bands are qualitatively analyzed from structural and compositional points of view.

  7. Structural characterization of ether lipids from the archaeon Sulfolobus islandicus by high-resolution shotgun lipidomics

    DEFF Research Database (Denmark)

    Jensen, Sara Munk; Brandl, Martin; Treusch, Alexander H

    2015-01-01

    The molecular structures, biosynthetic pathways and physiological functions of membrane lipids produced by organisms in the domain Archaea are poorly characterized as compared with that of counterparts in Bacteria and Eukaryota. Here we report on the use of high-resolution shotgun lipidomics......-resolution Fourier transform mass spectrometry using an ion trap-orbitrap mass spectrometer. This analysis identified five clusters of molecular ions that matched ether lipids in the database with sub-ppm mass accuracy. To structurally characterize and validate the identities of the potential lipid species, we...... performed structural analysis using multistage activation on the ion trap-orbitrap instrument as well as tandem mass analysis using a quadrupole time-of-flight machine. Our analysis identified four ether lipid species previously reported in Archaea, and one ether lipid species that had not been described...

  8. Chronic hypersensitivity pneumonitis: high resolution computed tomography patterns and pulmonary function indices as prognostic determinants

    Energy Technology Data Exchange (ETDEWEB)

    Walsh, Simon L.F.; Devaraj, Anand; Hansell, David M. [Royal Brompton Hospital, Department of Radiology, London (United Kingdom); Sverzellati, Nicola [University of Parma, Department of Clinical Sciences, Section of Radiology, Parma (Italy); Wells, Athol U. [Royal Brompton Hospital, Interstitial Lung Diseases Unit, London (United Kingdom)

    2012-08-15

    To investigate high resolution computed tomography (HRCT) and pulmonary function indices (PFTs) for determining prognosis in patients with chronic fibrotic hypersensitivity pneumonitis (CHP). Case records, PFTs (FEV{sub 1}, FVC and DLco) and HRCTs of ninety-two patients with chronic hypersensitivity pneumonitis were evaluated. HRCT studies were scored by two observers for total disease extent, ground-glass opacification, fine and coarse reticulation, microcystic and macrocystic honeycombing, centrilobular emphysema and consolidation. Traction bronchiectasis within each pattern was graded. Using Cox proportional hazards regression models the prognostic strength of individual HRCT patterns and pulmonary function test variables were determined. There were forty two deaths during the study period. Increasing severity of traction bronchiectasis was the strongest predictor of mortality (HR 1.10, P < 0.001, 95%CI 1.04-1.16). Increasing global interstitial disease extent (HR 1.02, P = 0.02, 95%CI 1.00-1.03), microcystic honeycombing (HR 1.09, P = 0.019, 95%CI 1.01-1.17) and macrocystic honeycombing (HR 1.06, P < 0.01, 95%CI 1.01-1.10) were also independent predictors of mortality. In contrast, no individual PFT variable was predictive of mortality once HRCT patterns were accounted for. HRCT patterns, in particular, severity of traction bronchiectasis and extent of honeycombing are superior to pulmonary function tests for predicting mortality in patients with CHP. (orig.)

  9. Chronic hypersensitivity pneumonitis: high resolution computed tomography patterns and pulmonary function indices as prognostic determinants

    International Nuclear Information System (INIS)

    Walsh, Simon L.F.; Devaraj, Anand; Hansell, David M.; Sverzellati, Nicola; Wells, Athol U.

    2012-01-01

    To investigate high resolution computed tomography (HRCT) and pulmonary function indices (PFTs) for determining prognosis in patients with chronic fibrotic hypersensitivity pneumonitis (CHP). Case records, PFTs (FEV 1 , FVC and DLco) and HRCTs of ninety-two patients with chronic hypersensitivity pneumonitis were evaluated. HRCT studies were scored by two observers for total disease extent, ground-glass opacification, fine and coarse reticulation, microcystic and macrocystic honeycombing, centrilobular emphysema and consolidation. Traction bronchiectasis within each pattern was graded. Using Cox proportional hazards regression models the prognostic strength of individual HRCT patterns and pulmonary function test variables were determined. There were forty two deaths during the study period. Increasing severity of traction bronchiectasis was the strongest predictor of mortality (HR 1.10, P < 0.001, 95%CI 1.04-1.16). Increasing global interstitial disease extent (HR 1.02, P = 0.02, 95%CI 1.00-1.03), microcystic honeycombing (HR 1.09, P = 0.019, 95%CI 1.01-1.17) and macrocystic honeycombing (HR 1.06, P < 0.01, 95%CI 1.01-1.10) were also independent predictors of mortality. In contrast, no individual PFT variable was predictive of mortality once HRCT patterns were accounted for. HRCT patterns, in particular, severity of traction bronchiectasis and extent of honeycombing are superior to pulmonary function tests for predicting mortality in patients with CHP. (orig.)

  10. High-resolution polypeptide structure and dynamics in anisotropic environments: The gramicidin channel

    Energy Technology Data Exchange (ETDEWEB)

    Cross, T.A.; Lee, K.C.; Ketchem, R.R.; Hu, W.; Lazo, N.D.; Huo, S. [Florida State Univ., Tallahassee, FL (United States)

    1994-12-01

    To understand the details of macromolecular function, high-resolution structural and dynamic detail is essential. The polypeptide fold of the gramicidin channel has been effectively modeled for the past 20 years, yet the functional changes in conductance and channel lifetime associated with amino acid substitutions cannot be predicted. To accomplish this goal, high-resolution electrostatic modeling and the precise orientation of all dipoles are required. Furthermore, an enhanced knowledge of the complex molecular environment of this membrane-bound peptide is needed. An aqueous environment is relatively uniform and achiral. The membrane environment is very heterogenous and chiral. A knowledge of the interactions, specific and nonspecific, between peptide and lipid will aid in developing a better understanding of this environment. To accomplish this goal, it is necessary to study the peptide in an extended lipid bilayer, rather than in a vesicular or micellar form. These latter environments are likely to possess increased dynamics, increased water penetration, and distorted interactions between the polypeptide and membrane surface. To perform NMR studies on bilayer bound peptides, solid state NMR methods are required, and for specific site information, isotopic labels are incorporated using solid phase peptide synthesis.

  11. Determination of Pu isotopic composition and 241Am by high resolution gamma spectrometry on solid samples

    International Nuclear Information System (INIS)

    Sarkar, Arnab; Paul, Sumana; Aggarwal, Suresh K.; Tomar, Bhupendra S.

    2011-08-01

    The present report gives a detailed account of the development of non-destructive assay technique using high resolution gamma-ray spectrometry (HRGS) for determination of plutonium (Pu) isotopic composition and the 241 Am content in solid Pu samples. Energy range 120-420 keV was used in this study. The methodology involves in situ relative efficiency calibration during the measurement process itself, to reduce the errors and increase the reliability of the method. Twenty solid Pu samples of power reactor and research reactor grade were analyzed by this method and the results were compared with those obtained by thermal ionization mass spectrometry. The accuracy of the final results depends strongly upon the accuracy of the available nuclear data (decay constant, gamma abundance etc.). MATLAB based programme was written to perform the analysis. A counting time of 4 hour was chosen for achieving good statistics on the results for samples having 100-200 mg of Pu. The attainable accuracy is found to be 0.5-1% for the fissile isotopes ( 239 Pu + 241 Pu) and 5-10% for 241 Am content. (author)

  12. Analytical method by high resolution liquid chromatography for the determination of carbamazepine in human plasma

    International Nuclear Information System (INIS)

    Jimenez Aleman, Narda M; Calero Carbonell, Jorge E; Padron Yaquis, Alejandro S; Izquierdo Lozano, Julio C

    2007-01-01

    One of the requirements to develop the studies of bioavailability and bioequivalence is to have analytic methodologies validated for the work with samples in biological fluids. A method was developed by high resolution liquid chromatography for the determination of carbamazepine in human plasma. A mixture of hydrogen phosphate of sodium: acetonitrile (65:35) adjusted to pH= 3.3 with phosphoric acid, flow of 1.2 mL/min and ultraviolet detection at 210 nm, was used as mobile phase. Propylparabene was used as an internal standard. According to the established regulations for the validation of the methods in biological fluids, the following parameters were studied: stability of the samples, lineality, specificity, precision, accuracy and limit of detection and quantification. The method proved to be specific and sensitive with a detection and quantification limit of 0.9 and 1.0 ng, respectively. The method was lineal, precise and exact in the range of concentrations of 1. 07 at 12.67 μg/mL. The mean recovery was not statistically different from 100.0 %. The analito in the proposed biological matrix remained in the studied period. The methodology described in this work is applied in our case to the study that evaluates the bioavailability and bioequivalence of a Cuban formulation of carbamazepine in healthy volunteers. (Author)

  13. Determination of sulfur in food by high resolution continuum source flame molecular absorption spectrometry

    Science.gov (United States)

    Zambrzycka, Elżbieta; Godlewska-Żyłkiewicz, Beata

    2014-11-01

    In the present work, a fast, simple and sensitive analytical method for determination of sulfur in food and beverages by high resolution continuum source flame molecular absorption spectrometry was developed. The determination was performed via molecular absorption of carbon monosulfide, CS. Different CS rotational lines (257.959 nm, 258.033 nm, 258.055 nm), number of pixels and types of standard solution of sulfur, namely: sulfuric acid, sodium sulfate, ammonium sulfate, sodium sulfite, sodium sulfide, DL-cysteine, and L-cystine, were studied in terms of sensitivity, repeatability of results as well as limit of detection and limit of quantification. The best results were obtained for measurements of absorption of the CS molecule at 258.055 nm at the wavelength range covering 3 pixels and DL-cysteine in 0.2 mol L- 1 HNO3 solution as a calibration standard. Under optimized conditions the limit of detection and the limit of quantification achieved for sulfur were 10.9 mg L- 1 and 36.4 mg L- 1, respectively. The repeatability of the results expressed as relative standard deviation was typically beverage samples with added known amount of sulfur standard. The recovery of analyte from such samples was in the range of 93-105% with the repeatability in the range of 4.1-5.0%. The developed method was applied for the determination of sulfur in milk (194 ± 10 mg kg- 1), egg white (2188 ± 29 mg kg- 1), mineral water (31.0 ± 0.9 mg L- 1), white wine (260 ± 4 mg L- 1) and red wine (82 ± 2 mg L- 1), as well as in sample rich in ions, such as bitter mineral water (6900 ± 100 mg L- 1).

  14. Three dimensional imaging of damage in structural materials using high resolution micro-tomography

    Energy Technology Data Exchange (ETDEWEB)

    Buffiere, J.-Y. [GEMPPM UMR CNRS 5510, INSA Lyon, 20 Av. A. Einstein, 69621 Villeurbanne Cedex (France)]. E-mail: jean-yves.buffiere@insa-lyon.fr; Proudhon, H. [GEMPPM UMR CNRS 5510, INSA Lyon, 20 Av. A. Einstein, 69621 Villeurbanne Cedex (France); Ferrie, E. [GEMPPM UMR CNRS 5510, INSA Lyon, 20 Av. A. Einstein, 69621 Villeurbanne Cedex (France); Ludwig, W. [GEMPPM UMR CNRS 5510, INSA Lyon, 20 Av. A. Einstein, 69621 Villeurbanne Cedex (France); Maire, E. [GEMPPM UMR CNRS 5510, INSA Lyon, 20 Av. A. Einstein, 69621 Villeurbanne Cedex (France); Cloetens, P. [ESRF Grenoble (France)

    2005-08-15

    This paper presents recent results showing the ability of high resolution synchrotron X-ray micro-tomography to image damage initiation and development during mechanical loading of structural metallic materials. First, the initiation, growth and coalescence of porosities in the bulk of two metal matrix composites have been imaged at different stages of a tensile test. Quantitative data on damage development has been obtained and related to the nature of the composite matrix. Second, three dimensional images of fatigue crack have been obtained in situ for two different Al alloys submitted to fretting and/or uniaxial in situ fatigue. The analysis of those images shows the strong interaction of the cracks with the local microstructure and provides unique experimental data for modelling the behaviour of such short cracks.

  15. Three dimensional imaging of damage in structural materials using high resolution micro-tomography

    International Nuclear Information System (INIS)

    Buffiere, J.-Y.; Proudhon, H.; Ferrie, E.; Ludwig, W.; Maire, E.; Cloetens, P.

    2005-01-01

    This paper presents recent results showing the ability of high resolution synchrotron X-ray micro-tomography to image damage initiation and development during mechanical loading of structural metallic materials. First, the initiation, growth and coalescence of porosities in the bulk of two metal matrix composites have been imaged at different stages of a tensile test. Quantitative data on damage development has been obtained and related to the nature of the composite matrix. Second, three dimensional images of fatigue crack have been obtained in situ for two different Al alloys submitted to fretting and/or uniaxial in situ fatigue. The analysis of those images shows the strong interaction of the cracks with the local microstructure and provides unique experimental data for modelling the behaviour of such short cracks

  16. Determination of sulfur in food by high resolution continuum source flame molecular absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zambrzycka, Elżbieta; Godlewska-Żyłkiewicz, Beata, E-mail: bgodlew@uwb.edu.pl

    2014-11-01

    In the present work, a fast, simple and sensitive analytical method for determination of sulfur in food and beverages by high resolution continuum source flame molecular absorption spectrometry was developed. The determination was performed via molecular absorption of carbon monosulfide, CS. Different CS rotational lines (257.959 nm, 258.033 nm, 258.055 nm), number of pixels and types of standard solution of sulfur, namely: sulfuric acid, sodium sulfate, ammonium sulfate, sodium sulfite, sodium sulfide, DL-cysteine, and L-cystine, were studied in terms of sensitivity, repeatability of results as well as limit of detection and limit of quantification. The best results were obtained for measurements of absorption of the CS molecule at 258.055 nm at the wavelength range covering 3 pixels and DL-cysteine in 0.2 mol L{sup −1} HNO{sub 3} solution as a calibration standard. Under optimized conditions the limit of detection and the limit of quantification achieved for sulfur were 10.9 mg L{sup −1} and 36.4 mg L{sup −1}, respectively. The repeatability of the results expressed as relative standard deviation was typically < 5%. The accuracy of the method was tested by analysis of digested biological certified reference materials (soya bean flour, corn flour and herbs) and recovery experiment for beverage samples with added known amount of sulfur standard. The recovery of analyte from such samples was in the range of 93–105% with the repeatability in the range of 4.1–5.0%. The developed method was applied for the determination of sulfur in milk (194 ± 10 mg kg{sup −1}), egg white (2188 ± 29 mg kg{sup −1}), mineral water (31.0 ± 0.9 mg L{sup −1}), white wine (260 ± 4 mg L{sup −1}) and red wine (82 ± 2 mg L{sup −1}), as well as in sample rich in ions, such as bitter mineral water (6900 ± 100 mg L{sup −1}). - Highlights: • HR-CS FMAS technique was used for sulfur measurement via molecular absorption of carbon monosulfide, CS. • Organic DL

  17. Determination of lattice parameters, strain state and composition in semipolar III-nitrides using high resolution X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Frentrup, Martin, E-mail: frentrup@physik.tu-berlin.de; Wernicke, Tim; Stellmach, Joachim; Kneissl, Michael [Institute of Solid State Physics, Technische Universität Berlin, Hardenbergstr. 36, 10623 Berlin (Germany); Hatui, Nirupam; Bhattacharya, Arnab [Department of Condensed Matter Physics and Materials Science, Tata Institute of Fundamental Research, Homi Bhabha Road, Mumbai 400005 (India)

    2013-12-07

    In group-III-nitride heterostructures with semipolar or nonpolar crystal orientation, anisotropic lattice and thermal mismatch with the buffer or substrate lead to a complex distortion of the unit cells, e.g., by shearing of the lattice. This makes an accurate determination of lattice parameters, composition, and strain state under assumption of the hexagonal symmetry impossible. In this work, we present a procedure to accurately determine the lattice constants, strain state, and composition of semipolar heterostructures using high resolution X-ray diffraction. An analysis of the unit cell distortion shows that four independent lattice parameters are sufficient to describe this distortion. Assuming only small deviations from an ideal hexagonal structure, a linear expression for the interplanar distances d{sub hkl} is derived. It is used to determine the lattice parameters from high resolution X-ray diffraction 2ϑ-ω-scans of multiple on- and off-axis reflections via a weighted least-square fit. The strain and composition of ternary alloys are then evaluated by transforming the elastic parameters (using Hooke's law) from the natural crystal-fixed coordinate system to a layer-based system, given by the in-plane directions and the growth direction. We illustrate our procedure taking an example of (112{sup ¯}2) Al{sub κ}Ga{sub 1−κ}N epilayers with Al-contents over the entire composition range. We separately identify the in-plane and out-of-plane strains and discuss origins for the observed anisotropy.

  18. Using high-resolution radar images to determine vegetation cover for soil erosion assessments.

    Science.gov (United States)

    Bargiel, D; Herrmann, S; Jadczyszyn, J

    2013-07-30

    Healthy soils are crucial for human well-being. Because soils are threatened worldwide, politicians recognize the need for soil protection. For example, the European Commission has launched the Thematic Strategy for Soil Protection, which requests the European member states to identify high risk areas for soil degradation. Most states use the Universal Soil Loss Equation (USLE) to assess soil erosion risk at the national scale. The USLE includes different factors, one of them is the vegetation cover and management factor (C factor). Modern satellite-based radar sensors now provide highly accurate vegetation cover data, enabling opportunities to improve the accuracy of the C factor. The presented study proves the suitability for C factor determination based on a multi-temporal classification of high-resolution radar images. Further USLE factors were derived from existing data sources (meteorological data, soil maps, digital elevation model) to conduct an USLE-based soil erosion assessment. The resulting map illustrates a qualitative assessment for soil erosion risk within a plot of about 7*12 km in an agricultural region in Poland that is very susceptible to soil erosion processes. A high erosion risk of more than 10 tonnes per ha and year was assessed to occur on 13.6% (646 ha) of the agricultural areas within the investigated plot. Further 7.8% (372 ha) of agricultural land is threaten by a medium risk of 5-10 tonnes per ha and year. Such a spatial information about areas of high or medium soil erosion risk are crucial for the development of strategies for the protection of soils. Copyright © 2013 Elsevier Ltd. All rights reserved.

  19. Determination of the activity of pulmonary tuberculosis : the utility of high-resolution computed tomography

    International Nuclear Information System (INIS)

    Chung, Myung Hee; Lee, Hae Giu; Yu, Won Jong; Chung, Hong Jun; Yang, Bo Sung; Kwon, Soon Suck; Park, Seog Hee

    2000-01-01

    To evaluate the utility of high-resolution computed tomography (HRCT), as used to determine the activity of tuberculosis, and to analyze the HRCT findings in active and in inactive tuberculosis. We analyzed the HRCT findings of 100 patients (54 men, 46 women; average age, 54 years) who according to the results of chest radiography had pulmonary tuberculosis of undetermined activity. We assessed HRCT findings such as the presence of a centrilobular, macro-, or micronodule; consolidation, ground-glass opacity, cavity, interlobular septal thickening, irregular linear opacities, bronchial wall thickening, bronchovascular bundle distortion, bronchiectasis, atelectasis, and pericicatrical emphysema. We compared the ratio of the area of nodule and consolidation to that of whole lung, and compared the findings between active and inactive tuberculosis. Eleven of 100 patients were excluded because the final diagnosis was other than tuberculosis. In 59 patients, the presence of active pulmonary tuberculosis was proven by positive sputum smear and/or culture for mycobacterium tuberculosis. On the basis of the negative results of these tests, pulmonary tuberculosis was found to be inactive in 30 patients; serial chest radiographs indicated that their condition remained stable over a 6-month period. For HRCT, sensitivity was 96.6%, specificity 56.7%, positive predictive value 81.4%, negative predictive value 89.5%, and accuracy 83.1%. For active tuberculosis, the presence of centrilobular nodules, tree-in-bud, macronodules, cavity within the nodule, and consolidations was statistically significant, while for inactive tuberculosis, that of irregular linear opacities, micronodules, bronchiectasis, and cicatrization atectasis was similarly significant. The CT score for the area of nodules and consolidations was higher in active than in inactive tuberculosis, but only the nodule score showed statistical significance. HRCT can be a useful diagnostic tool for evaluating the activity

  20. A Color-Texture-Structure Descriptor for High-Resolution Satellite Image Classification

    Directory of Open Access Journals (Sweden)

    Huai Yu

    2016-03-01

    Full Text Available Scene classification plays an important role in understanding high-resolution satellite (HRS remotely sensed imagery. For remotely sensed scenes, both color information and texture information provide the discriminative ability in classification tasks. In recent years, substantial performance gains in HRS image classification have been reported in the literature. One branch of research combines multiple complementary features based on various aspects such as texture, color and structure. Two methods are commonly used to combine these features: early fusion and late fusion. In this paper, we propose combining the two methods under a tree of regions and present a new descriptor to encode color, texture and structure features using a hierarchical structure-Color Binary Partition Tree (CBPT, which we call the CTS descriptor. Specifically, we first build the hierarchical representation of HRS imagery using the CBPT. Then we quantize the texture and color features of dense regions. Next, we analyze and extract the co-occurrence patterns of regions based on the hierarchical structure. Finally, we encode local descriptors to obtain the final CTS descriptor and test its discriminative capability using object categorization and scene classification with HRS images. The proposed descriptor contains the spectral, textural and structural information of the HRS imagery and is also robust to changes in illuminant color, scale, orientation and contrast. The experimental results demonstrate that the proposed CTS descriptor achieves competitive classification results compared with state-of-the-art algorithms.

  1. High-resolution AFM structure of DNA G-wires in aqueous solution.

    Science.gov (United States)

    Bose, Krishnashish; Lech, Christopher J; Heddi, Brahim; Phan, Anh Tuân

    2018-05-17

    We investigate the self-assembly of short pieces of the Tetrahymena telomeric DNA sequence d[G 4 T 2 G 4 ] in physiologically relevant aqueous solution using atomic force microscopy (AFM). Wire-like structures (G-wires) of 3.0 nm height with well-defined surface periodic features were observed. Analysis of high-resolution AFM images allowed their classification based on the periodicity of these features. A major species is identified with periodic features of 4.3 nm displaying left-handed ridges or zigzag features on the molecular surface. A minor species shows primarily left-handed periodic features of 2.2 nm. In addition to 4.3 and 2.2 nm ridges, background features with periodicity of 0.9 nm are also observed. Using molecular modeling and simulation, we identify a molecular structure that can explain both the periodicity and handedness of the major G-wire species. Our results demonstrate the potential structural diversity of G-wire formation and provide valuable insight into the structure of higher-order intermolecular G-quadruplexes. Our results also demonstrate how AFM can be combined with simulation to gain insight into biomolecular structure.

  2. New approaches to high-resolution mapping of marine vertical structures.

    Science.gov (United States)

    Robert, Katleen; Huvenne, Veerle A I; Georgiopoulou, Aggeliki; Jones, Daniel O B; Marsh, Leigh; D O Carter, Gareth; Chaumillon, Leo

    2017-08-21

    Vertical walls in marine environments can harbour high biodiversity and provide natural protection from bottom-trawling activities. However, traditional mapping techniques are usually restricted to down-looking approaches which cannot adequately replicate their 3D structure. We combined sideways-looking multibeam echosounder (MBES) data from an AUV, forward-looking MBES data from ROVs and ROV-acquired videos to examine walls from Rockall Bank and Whittard Canyon, Northeast Atlantic. High-resolution 3D point clouds were extracted from each sonar dataset and structure from motion photogrammetry (SfM) was applied to recreate 3D representations of video transects along the walls. With these reconstructions, it was possible to interact with extensive sections of video footage and precisely position individuals. Terrain variables were derived on scales comparable to those experienced by megabenthic individuals. These were used to show differences in environmental conditions between observed and background locations as well as explain spatial patterns in ecological characteristics. In addition, since the SfM 3D reconstructions retained colours, they were employed to separate and quantify live coral colonies versus dead framework. The combination of these new technologies allows us, for the first time, to map the physical 3D structure of previously inaccessible habitats and demonstrates the complexity and importance of vertical structures.

  3. High-resolution synchrotron imaging shows that root hairs influence rhizosphere soil structure formation.

    Science.gov (United States)

    Koebernick, Nicolai; Daly, Keith R; Keyes, Samuel D; George, Timothy S; Brown, Lawrie K; Raffan, Annette; Cooper, Laura J; Naveed, Muhammad; Bengough, Anthony G; Sinclair, Ian; Hallett, Paul D; Roose, Tiina

    2017-10-01

    In this paper, we provide direct evidence of the importance of root hairs on pore structure development at the root-soil interface during the early stage of crop establishment. This was achieved by use of high-resolution (c. 5 μm) synchrotron radiation computed tomography (SRCT) to visualise both the structure of root hairs and the soil pore structure in plant-soil microcosms. Two contrasting genotypes of barley (Hordeum vulgare), with and without root hairs, were grown for 8 d in microcosms packed with sandy loam soil at 1.2 g cm -3 dry bulk density. Root hairs were visualised within air-filled pore spaces, but not in the fine-textured soil regions. We found that the genotype with root hairs significantly altered the porosity and connectivity of the detectable pore space (> 5 μm) in the rhizosphere, as compared with the no-hair mutants. Both genotypes showed decreasing pore space between 0.8 and 0.1 mm from the root surface. Interestingly the root-hair-bearing genotype had a significantly greater soil pore volume-fraction at the root-soil interface. Effects of pore structure on diffusion and permeability were estimated to be functionally insignificant under saturated conditions when simulated using image-based modelling. © 2017 The Authors. New Phytologist © 2017 New Phytologist Trust.

  4. Similarity of High-Resolution Tandem Mass Spectrometry Spectra of Structurally Related Micropollutants and Transformation Products

    Science.gov (United States)

    Schollée, Jennifer E.; Schymanski, Emma L.; Stravs, Michael A.; Gulde, Rebekka; Thomaidis, Nikolaos S.; Hollender, Juliane

    2017-12-01

    High-resolution tandem mass spectrometry (HRMS2) with electrospray ionization is frequently applied to study polar organic molecules such as micropollutants. Fragmentation provides structural information to confirm structures of known compounds or propose structures of unknown compounds. Similarity of HRMS2 spectra between structurally related compounds has been suggested to facilitate identification of unknown compounds. To test this hypothesis, the similarity of reference standard HRMS2 spectra was calculated for 243 pairs of micropollutants and their structurally related transformation products (TPs); for comparison, spectral similarity was also calculated for 219 pairs of unrelated compounds. Spectra were measured on Orbitrap and QTOF mass spectrometers and similarity was calculated with the dot product. The influence of different factors on spectral similarity [e.g., normalized collision energy (NCE), merging fragments from all NCEs, and shifting fragments by the mass difference of the pair] was considered. Spectral similarity increased at higher NCEs and highest similarity scores for related pairs were obtained with merged spectra including measured fragments and shifted fragments. Removal of the monoisotopic peak was critical to reduce false positives. Using a spectral similarity score threshold of 0.52, 40% of related pairs and 0% of unrelated pairs were above this value. Structural similarity was estimated with the Tanimoto coefficient and pairs with higher structural similarity generally had higher spectral similarity. Pairs where one or both compounds contained heteroatoms such as sulfur often resulted in dissimilar spectra. This work demonstrates that HRMS2 spectral similarity may indicate structural similarity and that spectral similarity can be used in the future to screen complex samples for related compounds such as micropollutants and TPs, assisting in the prioritization of non-target compounds. [Figure not available: see fulltext.

  5. A study on the determination of phosphorus in Th-U matrix by a high resolution spectroanalyser (ICP-AES)

    International Nuclear Information System (INIS)

    Save, Neeta; Kumar, Neeraj; Jaiswal, Rajesh; Ghosh, Seema; Malav, R.K.; Das, D.K.; Prakash, Amrit; Behere, P.G.; Afzal, Mohd

    2013-01-01

    Phosphorus is present as an impurity in Thoria and constitutes an important chemical specification of the Thoria based fuel. The present paper depicts the importance of determination of phosphorus, which forms an important quality control step during the fabrication of mixed oxide (Th-U)O 2 pellet. A high resolution spectroanalyser using ICP-AES has been used for the determination of Phosphorus in (ThO 2 -3.25%UO 2 ). (author)

  6. In situ determination of a rock mass modulus using a high resolution tiltmeter

    Energy Technology Data Exchange (ETDEWEB)

    Saleh, B.; Husein Malkawi, A.I. [University of Jordan, Amman (Jordan); Blum, P.A. [Universite Pierre et Marie Curie, 75 - Paris (France)

    1996-04-01

    A very sensitive, compact tiltmeter made of melted silica, developed for the measurement of small deformations of various civil engineering structures, was described. The instrument is capable of giving a continuous record and was used to establish a new approach to directly evaluating the in situ average elastic rock mass modulus. Such information is important in decision making during the design stages of large civil engineering works, such as dams, nuclear plant facilities, and underground structures. Five tiltmeters were installed on the facades of the Louvre in Paris to study the deformation induced by internal structural work and by the impact of the Paris metro traffic movement. The data was used to determine displacement using the Boussinesq equation. Results were consistent with typical elastic rock-mass modulus for the rock found in the museum`s foundations. 13 refs., 1 tab., 10 figs.

  7. Computationally-optimized bone mechanical modeling from high-resolution structural images.

    Directory of Open Access Journals (Sweden)

    Jeremy F Magland

    Full Text Available Image-based mechanical modeling of the complex micro-structure of human bone has shown promise as a non-invasive method for characterizing bone strength and fracture risk in vivo. In particular, elastic moduli obtained from image-derived micro-finite element (μFE simulations have been shown to correlate well with results obtained by mechanical testing of cadaveric bone. However, most existing large-scale finite-element simulation programs require significant computing resources, which hamper their use in common laboratory and clinical environments. In this work, we theoretically derive and computationally evaluate the resources needed to perform such simulations (in terms of computer memory and computation time, which are dependent on the number of finite elements in the image-derived bone model. A detailed description of our approach is provided, which is specifically optimized for μFE modeling of the complex three-dimensional architecture of trabecular bone. Our implementation includes domain decomposition for parallel computing, a novel stopping criterion, and a system for speeding up convergence by pre-iterating on coarser grids. The performance of the system is demonstrated on a dual quad-core Xeon 3.16 GHz CPUs equipped with 40 GB of RAM. Models of distal tibia derived from 3D in-vivo MR images in a patient comprising 200,000 elements required less than 30 seconds to converge (and 40 MB RAM. To illustrate the system's potential for large-scale μFE simulations, axial stiffness was estimated from high-resolution micro-CT images of a voxel array of 90 million elements comprising the human proximal femur in seven hours CPU time. In conclusion, the system described should enable image-based finite-element bone simulations in practical computation times on high-end desktop computers with applications to laboratory studies and clinical imaging.

  8. Structure and Evolution of Hawaii's Loihi Seamount from High-resolution Mapping

    Science.gov (United States)

    Clague, D. A.; Paduan, J. B.; Moyer, C. L.; Glazer, B. T.; Caress, D. W.; Yoerger, D.; Kaiser, C. L.

    2016-12-01

    Loihi Seamount has been mapped repeatedly using shipboard multibeam sonars with improving resolution over time. Simrad EM302 data with 25m resolution at the 950m summit and 90m at the 5000m base of the volcano were collected from Schmidt Ocean Institute's R/V Falkor in 2014. A contracted multibeam survey in 1997 employing a deep-towed vehicle has 7m resolution for the summit and upper north and south rift zones, but suffered from poor navigation. Woods Hole Oceanographic Institution's AUV Sentry surveyed most of the summit and low-T hydrothermal vents on the base of the south rift in 2013 and 2014. The 2m resolution of most data is more precise than the navigation. The 6 summit surveys were reprocessed using MB-System to remove abundant bad bottom picks and adjust the navigation to produce a spatially accurate map. The 3 summit pits, including Pele's Pit that formed in 1996, are complex collapse structures and nested inside a larger caldera that was modified by large landslides on the east and west summit flanks. The pits cut low shields that once formed a complex of overlapping summit shields, similar to Kilauea before the current caldera formed 1500 to 1790 CE. An 11m section of ash deposits crops out on the east rim of the summit along a caldera-bounding fault and is analogous to Kilauea where the caldera-bounding faults expose ash erupted as the present caldera formed. Most of the Loihi ash section is 3300 to 5880 yr BP, indicating that the larger caldera structure at Loihi is younger than 3300 yr BP. The landslides on the east and west edges of the summit are therefore younger 3300 yr BP. The uppermost south rift has several small pit craters between cones and pillow ridges, also analogous to Kilauea. Two cones near the deep low-T vents are steep pillow mounds with slopes of talus. High-resolution mapping reveals, for the first time, the many similarities between the structure and evolution of submarine Loihi Seamount and subaerial Kilauea Volcano.

  9. Unit cell determination of epitaxial thin films based on reciprocal space vectors by high-resolution X-ray diffractometry

    OpenAIRE

    Yang, Ping; Liu, Huajun; Chen, Zuhuang; Chen, Lang; Wang, John

    2013-01-01

    A new approach, based on reciprocal space vectors (RSVs), is developed to determine Bravais lattice types and accurate lattice parameters of epitaxial thin films by high-resolution X-ray diffractometry (HR-XRD). The lattice parameters of single crystal substrates are employed as references to correct the systematic experimental errors of RSVs of thin films. The general procedure is summarized, involving correction of RSVs, derivation of raw unit cell, subsequent conversion to the Niggli unit ...

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

    Science.gov (United States)

    2013-01-01

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

  11. Linear versus non-linear structural information limit in high-resolution transmission electron microscopy

    International Nuclear Information System (INIS)

    Van Aert, S.; Chen, J.H.; Van Dyck, D.

    2010-01-01

    A widely used performance criterion in high-resolution transmission electron microscopy (HRTEM) is the information limit. It corresponds to the inverse of the maximum spatial object frequency that is linearly transmitted with sufficient intensity from the exit plane of the object to the image plane and is limited due to partial temporal coherence. In practice, the information limit is often measured from a diffractogram or from Young's fringes assuming a weak phase object scattering beyond the inverse of the information limit. However, for an aberration corrected electron microscope, with an information limit in the sub-angstrom range, weak phase objects are no longer applicable since they do not scatter sufficiently in this range. Therefore, one relies on more strongly scattering objects such as crystals of heavy atoms observed along a low index zone axis. In that case, dynamical scattering becomes important such that the non-linear and linear interaction may be equally important. The non-linear interaction may then set the experimental cut-off frequency observed in a diffractogram. The goal of this paper is to quantify both the linear and the non-linear information transfer in terms of closed form analytical expressions. Whereas the cut-off frequency set by the linear transfer can be directly related with the attainable resolution, information from the non-linear transfer can only be extracted using quantitative, model-based methods. In contrast to the historic definition of the information limit depending on microscope parameters only, the expressions derived in this paper explicitly incorporate their dependence on the structure parameters as well. In order to emphasize this dependence and to distinguish from the usual information limit, the expressions derived for the inverse cut-off frequencies will be referred to as the linear and non-linear structural information limit. The present findings confirm the well-known result that partial temporal coherence has

  12. Characterizing the structural maturity of fault zones using high-resolution earthquake locations.

    Science.gov (United States)

    Perrin, C.; Waldhauser, F.; Scholz, C. H.

    2017-12-01

    We use high-resolution earthquake locations to characterize the three-dimensional structure of active faults in California and how it evolves with fault structural maturity. We investigate the distribution of aftershocks of several recent large earthquakes that occurred on immature faults (i.e., slow moving and small cumulative displacement), such as the 1992 (Mw7.3) Landers and 1999 (Mw7.1) Hector Mine events, and earthquakes that occurred on mature faults, such as the 1984 (Mw6.2) Morgan Hill and 2004 (Mw6.0) Parkfield events. Unlike previous studies which typically estimated the width of fault zones from the distribution of earthquakes perpendicular to the surface fault trace, we resolve fault zone widths with respect to the 3D fault surface estimated from principal component analysis of local seismicity. We find that the zone of brittle deformation around the fault core is narrower along mature faults compared to immature faults. We observe a rapid fall off of the number of events at a distance range of 70 - 100 m from the main fault surface of mature faults (140-200 m fault zone width), and 200-300 m from the fault surface of immature faults (400-600 m fault zone width). These observations are in good agreement with fault zone widths estimated from guided waves trapped in low velocity damage zones. The total width of the active zone of deformation surrounding the main fault plane reach 1.2 km and 2-4 km for mature and immature faults, respectively. The wider zone of deformation presumably reflects the increased heterogeneity in the stress field along complex and discontinuous faults strands that make up immature faults. In contrast, narrower deformation zones tend to align with well-defined fault planes of mature faults where most of the deformation is concentrated. Our results are in line with previous studies suggesting that surface fault traces become smoother, and thus fault zones simpler, as cumulative fault slip increases.

  13. CIRS High-Resolution Thermal Scans and the Structure of Saturn's B Ring

    Science.gov (United States)

    Brooks, S. M.; Spilker, L. J.; Showalter, M.; Pilorz, S.; Edgington, S. G.

    2017-12-01

    The flyby of Titan on November 29, 2016, sent the Cassini spacecraft on a trajectory that would take it within 10,000 kilometers of Saturn's F ring multiple times before a subsequent Titan encounter on April 22, 2017, would send it on ballistic trajectory carrying it between Saturn's cloud tops and the planet's D ring for several flybys. This geometry has proven beneficial for high-resolution studies of the rings, not just because of Cassini's proximity to the rings, but also because of the spacecraft's high elevation angle above the rings, which reduces the foreshortening that tends to degrade resolution in the ring plane. We will report on several observations of Saturn's main rings at the high spatial resolutions enabled by the end-of-mission geometry, particulary the B ring, with the Composite Infrared Spectrometer onboard Cassini during the F-ring and proximal orbits. CIRS' three infrared detectors cover a combined spectral range of 10 to 1400 cm-1 (1 mm down to 7 microns). We focus on data from Focal Plane 1, which covers the 10 to 600 cm-1 range (1 mm to 16 microns). The apodized spectral resolution of the instrument can be varied from 15 cm-1 to 0.5 cm-1 (Flasar et al. 2004). FP1's wavelength range makes it well-suited to sensing thermal emission from objects at temperatures typical of Saturn's rings. Correlating ring optical depth with temperatures retrieved from scans of the face of the rings exposed to direct solar illumination (the lit face) and the opposite (unlit) face suggests differences in ring structure or particle transport between the lit and unlit sides of the rings in different regions of the B ring. Lit side temperatures in the core of the B ring range between 82 and 87 K; temperatures on the unlit side of the core vary from 66 K up to 74 K. Ferrari and Reffet (2013) and Pilorz et al. (2015) published thorough analyses of the thermal throughput across this optically thick ring. We will discuss these recent CIRS rings observations and their

  14. High-resolution Anorectal Manometry for Identifying Defecatory Disorders and Rectal Structural Abnormalities in Women.

    Science.gov (United States)

    Prichard, David O; Lee, Taehee; Parthasarathy, Gopanandan; Fletcher, Joel G; Zinsmeister, Alan R; Bharucha, Adil E

    2017-03-01

    Contrary to conventional wisdom, the rectoanal gradient during evacuation is negative in many healthy people, undermining the utility of anorectal high-resolution manometry (HRM) for diagnosing defecatory disorders. We aimed to compare HRM and magnetic resonance imaging (MRI) for assessing rectal evacuation and structural abnormalities. We performed a retrospective analysis of 118 patients (all female; 51 with constipation, 48 with fecal incontinence, and 19 with rectal prolapse; age, 53 ± 1 years) assessed by HRM, the rectal balloon expulsion test (BET), and MRI at Mayo Clinic, Rochester, Minnesota, from February 2011 through March 2013. Thirty healthy asymptomatic women (age, 37 ± 2 years) served as controls. We used principal components analysis of HRM variables to identify rectoanal pressure patterns associated with rectal prolapse and phenotypes of patients with prolapse. Compared with patients with normal findings from the rectal BET, patients with an abnormal BET had lower median rectal pressure (36 vs 22 mm Hg, P = .002), a more negative median rectoanal gradient (-6 vs -29 mm Hg, P = .006) during evacuation, and a lower proportion of evacuation on the basis of MRI analysis (median of 40% vs 80%, P < .0001). A score derived from rectal pressure and anorectal descent during evacuation and a patulous anal canal was associated (P = .005) with large rectoceles (3 cm or larger). A principal component (PC) logistic model discriminated between patients with and without prolapse with 96% accuracy. Among patients with prolapse, there were 2 phenotypes, which were characterized by high (PC1) or low (PC2) anal pressures at rest and squeeze along with higher rectal and anal pressures (PC1) or a higher rectoanal gradient during evacuation (PC2). In a retrospective analysis of patients assessed by HRM, measurements of rectal evacuation by anorectal HRM, BET, and MRI were correlated. HRM alone and together with anorectal descent during evacuation may identify

  15. Determination of Chlorophenoxy Acid Methyl Esters and Other Chlorinated Herbicides by GC High-resolution QTOFMS and Soft lonization

    Directory of Open Access Journals (Sweden)

    Viorica Lopez-Avila

    2015-01-01

    Full Text Available Gas chromatography with quadrupole time-of-flight mass spectrometry (GC-QTOFMS and soft ionization generated by a rare-gas plasma is described here for the determination of various chlorophenoxy acid methyl esters and a few chlorinated herbicides. This plasma-based, wavelength-selectable ionization source, which can use Xe, Kr, Ar, Ne, or He as the plasma gas, enables ionization of GC-amenable compounds with ionization energies below 8.4, 10, 11.6, 16.5, or 22.4 eV, respectively. The advantages of soft ionization include enhanced molecular ions, reduced fragmentation, and reduced background noise as compared to electron ionization. In the study presented here for two plasma gases, we demonstrate that Kr plasma, which is softer than Ar plasma, yields molecular ions with a relative intensity >60% for 11 of the 16 test compounds. When using this “tunable” plasma to ionize the analytes, there is the possibility for selective ionization and less fragmentation, which may lead to increased sensitivity and may help structure elucidation, especially when using high-resolution mass spectrometry that generates accurate masses within a few parts per million (ppm mass errors. Data generated with the Ar plasma and real matrices such as a peppermint extract, a plum extract, and an orange peel extract, spiked with 16 test compounds, indicate that the test compounds can be detected at 1-10 pg/µL of extract, and compounds such as menthone, limonene, eucalyptol, pinene, caryophylene, and other C 15 H 24 isomers, which are present in the peppermint and the orange peel extracts at ppm to percent levels, do not appear to interfere with the determination of the chlorophenoxy acid methyl esters or the chlorinated herbicides, although there were matrix effects when the test compounds were spiked at 1-10 pg/µL of extract.

  16. High-Resolution Mapping of Chromatin Conformation in Cardiac Myocytes Reveals Structural Remodeling of the Epigenome in Heart Failure.

    Science.gov (United States)

    Rosa-Garrido, Manuel; Chapski, Douglas J; Schmitt, Anthony D; Kimball, Todd H; Karbassi, Elaheh; Monte, Emma; Balderas, Enrique; Pellegrini, Matteo; Shih, Tsai-Ting; Soehalim, Elizabeth; Liem, David; Ping, Peipei; Galjart, Niels J; Ren, Shuxun; Wang, Yibin; Ren, Bing; Vondriska, Thomas M

    2017-10-24

    Cardiovascular disease is associated with epigenomic changes in the heart; however, the endogenous structure of cardiac myocyte chromatin has never been determined. To investigate the mechanisms of epigenomic function in the heart, genome-wide chromatin conformation capture (Hi-C) and DNA sequencing were performed in adult cardiac myocytes following development of pressure overload-induced hypertrophy. Mice with cardiac-specific deletion of CTCF (a ubiquitous chromatin structural protein) were generated to explore the role of this protein in chromatin structure and cardiac phenotype. Transcriptome analyses by RNA-seq were conducted as a functional readout of the epigenomic structural changes. Depletion of CTCF was sufficient to induce heart failure in mice, and human patients with heart failure receiving mechanical unloading via left ventricular assist devices show increased CTCF abundance. Chromatin structural analyses revealed interactions within the cardiac myocyte genome at 5-kb resolution, enabling examination of intra- and interchromosomal events, and providing a resource for future cardiac epigenomic investigations. Pressure overload or CTCF depletion selectively altered boundary strength between topologically associating domains and A/B compartmentalization, measurements of genome accessibility. Heart failure involved decreased stability of chromatin interactions around disease-causing genes. In addition, pressure overload or CTCF depletion remodeled long-range interactions of cardiac enhancers, resulting in a significant decrease in local chromatin interactions around these functional elements. These findings provide a high-resolution chromatin architecture resource for cardiac epigenomic investigations and demonstrate that global structural remodeling of chromatin underpins heart failure. The newly identified principles of endogenous chromatin structure have key implications for epigenetic therapy. © 2017 The Authors.

  17. Test of a detection structure for a high-resolution vertex chamber

    International Nuclear Information System (INIS)

    Gruenewald, M.W.

    1988-01-01

    For the LEP experiment L3 a self-supporting detection structure in the TEC principle for the central vertex chamber was tested both with particles and with laser beams. The main topic of this thesis lied thereby on the determination of the coordinate of the particle passage along the signal-wire axis. Two different methods for the determination of this coordinate along the signal wire were studied. (orig./HSI) [de

  18. Evolution of dislocation structures following a change in loading conditions studied by in situ high resolution reciprocal space mapping

    DEFF Research Database (Denmark)

    Wejdemann, Christian

    or to a strain of 7% at a temperature of -196 ○C, and the samples were characterized by electron microscopy and mechanical tests. Transmission electron microscopy showed that the pre-deformation produced a characteristic dislocation cell structure consisting of regions with relatively high dislocation density...... the pre-deformation axis. In the X-ray diffraction experiments a technique was employed with which it is possible to obtain high-resolution reciprocal space maps from individual bulk grains. The high-resolution reciprocal space maps contain features related to the dislocation structure in the grains......: A spread-out ‘cloud’ of low intensity caused by diffraction from the dislocation walls and a number of sharp peaks of high intensity caused by diffraction from the individual subgrains. By acquiring reciprocal space maps at a number of different strain levels the evolution of the dislocation structures can...

  19. The Project Serapis: High Resolution Seismic Imagingof The Campi Flegrei Caldera Structure

    Science.gov (United States)

    Zollo, A.; Virieux, J.; Capuano, P.; Chiarabba, C.; de Franco, R.; Makris, J.; Michelini, A.; Musacchio, G.; Serapis Group

    During September 2001, an extended active seismic survey has been performed in the gulfs of Naples and Pozzuoli in the framework of the so called SERAPIS (SEismic Re- flection Acquisition Project for Imaging Structures). The project SERAPIS is aimed at the acquisition in the bays of Naples and Pozzuoli, on land and at the sea bottom (using sea bottom seismographs), of seismic signals emitted by a very dense network of airgun sources. The energization is performed through the syncronized implosion of bubbles produced by a battery of three to twelve, 16 liters airguns, mounted on the oceanographic vessel NADIR, owned by the french company IFREMER, which supported the project at no cost. The experiment has been designed to have 2D-3D acquisition lay-outs and its objective is the high resolution imaging of the main shal- low crustal discontinuities underneath the major neapolitan volcanic complexes. In particular some desired targets are the location and spatial definition of the magmatic feeding system of Campi Flegrei and the morphologic reconstruction of the interface separating the shallow volcano-alluvium sediments and the Mesozoic carbonates, re- cently detected and accurately imaged underneath Mt.Vesuvius volcano. A secondary but not less important objective is the denser re-sampling of areas in the Bay of Naples prospicient to Mt.Vesuvius, which have been investigated during the last marine sur- vey using the same vessel in 1997 (MareVes 97). Sixty, three-component stations have been installed on-land in the areas of Campi Flegrei, Mt.Vesuvius and on the islands of Ischia and Procida. In particular, the Mt.Vesuvius stations have been deployed along a 40 km long, SE-NW profile crossing the Campanian Plain toward the limestone out- crops. 72 sea bottom seismographs (OBS) have been installed in the gulfs of Naples and Pozzuoli by the University of Hamburg, with the logistic support of Geopro smbh and Geolab Italia. The OBS network geometry follows the main

  20. High-resolution structure of the recombinant sweet-tasting protein thaumatin I

    International Nuclear Information System (INIS)

    Masuda, Tetsuya; Ohta, Keisuke; Mikami, Bunzo; Kitabatake, Naofumi

    2011-01-01

    The structure of a recombinant form of the sweet-tasting protein thaumatin I was determined at 1.1 Å resolution and refined to an R work of 9.1% and an R free of 11.7%. Comparisons with plant thaumatin revealed the electron density of recombinant thaumatin I to be significantly improved, especially around Asn46 and Ser63. Thaumatin, an intensely sweet-tasting plant protein, elicits a sweet taste at a concentration of 50 nM. The crystal structure of a recombinant form of thaumatin I produced in the yeast Pichia pastoris has been determined to a resolution of 1.1 Å. The model was refined with anisotropic B parameters and riding H atoms. A comparison of the diffraction data and refinement statistics for recombinant thaumatin I with those for plant thaumatin I revealed no significant differences in the diffraction data. The R values for recombinant thaumatin I and plant thaumatin I (F o > 4σ) were 9.11% and 9.91%, respectively, indicating the final model to be of good quality. Notably, the electron-density maps around Asn46 and Ser63, which differ between thaumatin variants, were significantly improved. Furthermore, a number of H atoms became visible in an OMIT map and could be assigned. The high-quality structure of recombinant thaumatin with H atoms should provide details about sweetness determinants in thaumatin and provide valuable insights into the mechanism of its interaction with taste receptors

  1. High-resolution structures of Lactobacillus salivarius transketolase in the presence and absence of thiamine pyrophosphate.

    Science.gov (United States)

    Lukacik, Petra; Lobley, Carina M C; Bumann, Mario; Arena de Souza, Victoria; Owens, Raymond J; O'Toole, Paul W; Walsh, Martin A

    2015-10-01

    Probiotic bacterial strains have been shown to enhance the health of the host through a range of mechanisms including colonization, resistance against pathogens, secretion of antimicrobial compounds and modulation of the activity of the innate immune system. Lactobacillus salivarius UCC118 is a well characterized probiotic strain which survives intestinal transit and has many desirable host-interaction properties. Probiotic bacteria display a wide range of catabolic activities, which determine their competitiveness in vivo. Some lactobacilli are heterofermentative and can metabolize pentoses, using a pathway in which transketolase and transaldolase are key enzymes. L. salivarius UCC118 is capable of pentose utilization because it encodes the key enzymes on a megaplasmid. The crystal structures of the megaplasmid-encoded transketolase with and without the enzyme cofactor thiamine pyrophosphate have been determined. Comparisons with other known transketolase structures reveal a high degree of structural conservation in both the catalytic site and the overall conformation. This work extends structural knowledge of the transketolases to the industrially and commercially important Lactobacillus genus.

  2. Use of high-resolution satellite images for detection of geological structures related to Central Andes geothermal field, Chile.

    Science.gov (United States)

    Benavides-Rivas, C. L.; Soto-Pinto, C. A.; Arellano-Baeza, A. A.

    2014-12-01

    Central valley and the border with Argentina in the center, and in the fault system Liquiñe-Ofqui in the South of the country. High resolution images from the LANDSAT 8 satellite have been used to delineate the geological structures related to the potential geothermal reservoirs located at the northern end of the Southern Volcanic Zone of Chile. It was done by applying the lineament extraction technique, using the ADALGEO software, developed by [Soto et al., 2013]. These structures have been compared with the distribution of main geological structures obtained in the field. It was found that the lineament density increases in the areas of the major heat flux indicating that the lineament analysis could be a power tool for the detection of faults and joint zones associated to the geothermal fields. A lineament is generally defined as a straight or slightly curved feature in the landscape visible satellite image as an aligned sequence of pixel intensity contrast compared to the background. The system features extracted from satellite images is not identical to the geological lineaments that are generally determined by ground surveys, however, generally reflects the structure of faults and fractures in the crust. A temporal sequence of eight Landsat multispectral images of Central Andes geothermal field, located in VI region de Chile, was used to study changes in the configuration of the lineaments during 2011. The presence of minerals with silicification, epidotization, and albitization, which are typical for geothrmal reservoirs, was also identified, using their spectral characteristics, and subsequently corroborated in the field. Both lineament analysis and spectral analysis gave similar location of the reservoir, which increases reliability of the results.

  3. Lunar Prospector Orbit Determination Uncertainties Using the High Resolution Lunar Gravity Models

    Science.gov (United States)

    Carranza, Eric; Konopliv, Alex; Ryne, Mark

    1999-01-01

    The Lunar Prospector (LP) mission began on January 6, 1998, when the LP spacecraft was launched from Cape Canaveral, Florida. The objectives of the mission were to determine whether water ice exists at the lunar poles, generate a global compositional map of the lunar surface, detect lunar outgassing, and improve knowledge of the lunar magnetic and gravity fields. Orbit determination of LP performed at the Jet Propulsion Laboratory (JPL) is conducted as part of the principal science investigation of the lunar gravity field. This paper will describe the JPL effort in support of the LP Gravity Investigation. This support includes high precision orbit determination, gravity model validation, and data editing. A description of the mission and its trajectory will be provided first, followed by a discussion of the orbit determination estimation procedure and models. Accuracies will be examined in terms of orbit-to-orbit solution differences, as a function of oblateness model truncation, and inclination in the plane-of-sky. Long term predictions for several gravity fields will be compared to the reconstructed orbits to demonstrate the accuracy of the orbit determination and oblateness fields developed by the Principal Gravity Investigator.

  4. Fluorine determination in coal using high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis

    Energy Technology Data Exchange (ETDEWEB)

    Machado, Patrícia M.; Morés, Silvane; Pereira, Éderson R. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Welz, Bernhard, E-mail: w.bernardo@terra.com.br [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Carasek, Eduardo [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Andrade, Jailson B. de [Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil)

    2015-03-01

    The absorption of the calcium mono-fluoride (CaF) molecule has been employed in this study for the determination of fluorine in coal using direct solid sample analysis and high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS). The rotational line at 606.440 nm was used for measuring the molecular absorption in the gas phase. The pyrolysis and vaporization temperatures were 700 °C and 2100 °C, respectively. Different chemical modifiers have been studied, such as Pd and Ir as permanent modifiers, and Pd and the mixed Pd/Mg modifier in solution. The limit of detection and the characteristic mass were 0.3 and 0.1 ng F, respectively. One certified reference material (CRM) of coal (NIST 1635) and four CRMs with a non-certified value for F (SARM 18, SARM 20, BCR 40, BCR 180) were used to evaluate the accuracy and precision of the method, obtaining good agreement (104%) with the certified value and with the informed values (ranging from 90 to 103%). - Highlights: • High-resolution Graphite Furnace Molecular Absorption Spectrometry (HR-GF MAS) • Fluorine has been determined using HR-GF MAS of the CaF molecule. • The CaF molecule was generated in a graphite furnace at a temperature of 2100 °C • Coal samples have been analyzed using direct solid sample introduction. • Aqueous standard solutions have been used for calibration.

  5. Recognition of anesthetic barbiturates by a protein binding site: a high resolution structural analysis.

    Directory of Open Access Journals (Sweden)

    Simon Oakley

    Full Text Available Barbiturates potentiate GABA actions at the GABA(A receptor and act as central nervous system depressants that can induce effects ranging from sedation to general anesthesia. No structural information has been available about how barbiturates are recognized by their protein targets. For this reason, we tested whether these drugs were able to bind specifically to horse spleen apoferritin, a model protein that has previously been shown to bind many anesthetic agents with affinities that are closely correlated with anesthetic potency. Thiopental, pentobarbital, and phenobarbital were all found to bind to apoferritin with affinities ranging from 10-500 µM, approximately matching the concentrations required to produce anesthetic and GABAergic responses. X-ray crystal structures were determined for the complexes of apoferritin with thiopental and pentobarbital at resolutions of 1.9 and 2.0 Å, respectively. These structures reveal that the barbiturates bind to a cavity in the apoferritin shell that also binds haloalkanes, halogenated ethers, and propofol. Unlike these other general anesthetics, however, which rely entirely upon van der Waals interactions and the hydrophobic effect for recognition, the barbiturates are recognized in the apoferritin site using a mixture of both polar and nonpolar interactions. These results suggest that any protein binding site that is able to recognize and respond to the chemically and structurally diverse set of compounds used as general anesthetics is likely to include a versatile mixture of both polar and hydrophobic elements.

  6. Determination of strontium and lead isotope ratios of grains using high resolution inductively coupled plasma mass spectrometer with single collector

    International Nuclear Information System (INIS)

    Shinozaki, Miyuki; Ariyama, Kaoru; Kawasaki, Akira; Hirata, Takafumi

    2010-01-01

    A method for determining strontium and lead isotope ratios of grains was developed. The samples investigated in this study were rice, barley and wheat. The samples were digested with nitric acid and hydrogen peroxide, and heated in a heating block. Strontium and lead were separated from the matrix by adding an acid digested solution into a column packed with Sr resin, which has selectivity for the absorption of strontium and lead. Strontium and lead isotope ratios were determined using a high-resolution inductively coupled plasma mass spectrometer (HR-ICP-MS) with a single collector. The intraday relative standard deviations of 87 Sr/ 86 Sr and lead isotope ratios ( 204 Pb/ 206 Pb, 207 Pb/ 206 Pb, 208 Pb/ 206 Pb) by HR-ICP-MS measurements were < 0.06% and around 0.1%, respectively. This method enabled us to determine strontium and lead isotope ratios in two days. (author)

  7. Classification of wine by determination of bioactive phenolic compounds using high resolution mass spectrometry

    OpenAIRE

    Ivanova, Violeta; Dimovska, Violeta; Mitrev, Sasa; Gulaboski, Rubin; Bogeva, Elena; Petruseva, Dragana; Causon, Tim; Hann, Stephan

    2016-01-01

    In this project proposal, metabolomic fingerprinting of wine samples will be examined using high performance liquid chromatography combined with ion mobility quadruple time-of-flight mass spectrometry (HPLC–IMS-QTOF-MS) for the first time. Bioactive compounds in wines from various red and white varieties produced in Macedonia and Austria from different wine regions and different vintages will be determined for the first time using a non-targeted fingerprinting approach on this analytical plat...

  8. Structural elucidation of the Brucella melitensis M antigen by high-resolution NMR at 500 MHz

    International Nuclear Information System (INIS)

    Bundle, D.R.; Cherwonogrodzky, J.W.; Perry, M.B.

    1987-01-01

    The Brucella M antigen from the species type strain Brucella melitensis 16M has been identified as a component of the cell wall lipopolysaccharide (LPS). O polysaccharide liberated from this LPS by mild acid hydrolysis exhibited M activity in serological tests and was shown to be a homopolymer of 4-formamido-4,6-dideoxy-α-D-mannopyranosyl residues arranged in an oligosaccharide repeating unit as judged by sodium dodecyl sulfate-polyacrylamide gel electrophoresis of the native lipopolysaccharide. Structural analysis of the O polysaccharide by NMR methods was difficult due to apparent microheterogeneity of the repeating unit, which was in fact caused by the presence of rotational isomers of the N-formyl moiety. This problem was resolved by chemical modification of the polysaccharide to its amino and N-acetyl derivatives, the 500-MHz 1 H and 125-MHz 13 C NMR spectra of which could be analyzed in terms of a unique structure through application of pH-dependent β-shifts and two-dimensional techniques that included COSY, relayed COSY, and NOESY experiments together with heteronuclear C/H shift correlation spectroscopy. On the basis of these experiments and supported by methylation and periodate oxidation data, the structure of the M polysaccharide was determined as a linear polymer of unbranched pentasaccharide repeating units consisting of four 1,2-linked and one 1,3-lined 4,6-dideoxy-4-formamido-α-D-mannopyranosyl residues. The marked structural similarity of the M antigen and the A antigen, which is known to be a 1,2-linked homopolysaccharide of 4,6-dideoxy-4-formamido-α-D-mannopyranosyl units, accounts for cross-serological reactions of the two and the long-standing confusion surrounding the nature of their antigenic determinants

  9. Burn-Up Determination by High Resolution Gamma Spectrometry: Axial and Diametral Scanning Experiments

    Energy Technology Data Exchange (ETDEWEB)

    Forsyth, R S; Blackadder, W H; Ronqvist, N

    1967-02-15

    In the gamma spectrometric determination of burn-up the use of a single fission product as a monitor of the specimen fission rate is subject to errors caused by activity saturation or, in certain cases, fission product migration. Results are presented of experiments in which all the resolvable gamma peaks in the fission product spectrum have been used to calculate the fission rate; these results form a pattern which reflect errors in the literature values of the gamma branching ratios, fission yields etc., and also represent a series of empirical correction factors. Axial and diametral scanning experiments on a long-irradiated low-enrichment fuel element are also described and demonstrate that it is possible to differentiate between fissions in U-235 and in Pu-239 respectively by means of the ratios of the Ru-106 activity to the activities of the other fission products.

  10. Medical images of patients in voxel structures in high resolution for Monte Carlo simulation

    International Nuclear Information System (INIS)

    Boia, Leonardo S.; Menezes, Artur F.; Silva, Ademir X.

    2011-01-01

    This work aims to present a computational process of conversion of tomographic and MRI medical images from patients in voxel structures to an input file, which will be manipulated in Monte Carlo Simulation code for tumor's radiotherapic treatments. The problem's scenario inherent to the patient is simulated by such process, using the volume element (voxel) as a unit of computational tracing. The head's voxel structure geometry has voxels with volumetric dimensions around 1 mm 3 and a population of millions, which helps - in that way, for a realistic simulation and a decrease in image's digital process techniques for adjustments and equalizations. With such additional data from the code, a more critical analysis can be developed in order to determine the volume of the tumor, and the protection, beside the patients' medical images were borrowed by Clinicas Oncologicas Integradas (COI/RJ), joined to the previous performed planning. In order to execute this computational process, SAPDI computational system is used in a digital image process for optimization of data, conversion program Scan2MCNP, which manipulates, processes, and converts the medical images into voxel structures to input files and the graphic visualizer Moritz for the verification of image's geometry placing. (author)

  11. Medical images of patients in voxel structures in high resolution for Monte Carlo simulation

    Energy Technology Data Exchange (ETDEWEB)

    Boia, Leonardo S.; Menezes, Artur F.; Silva, Ademir X., E-mail: lboia@con.ufrj.b, E-mail: ademir@con.ufrj.b [Universidade Federal do Rio de Janeiro (PEN/COPPE/UFRJ), RJ (Brazil). Coordenacao dos Programas de Pos-Graduacao de Engenharia. Programa de Engenharia Nuclear; Salmon Junior, Helio A. [Clinicas Oncologicas Integradas (COI), Rio de Janeiro, RJ (Brazil)

    2011-07-01

    This work aims to present a computational process of conversion of tomographic and MRI medical images from patients in voxel structures to an input file, which will be manipulated in Monte Carlo Simulation code for tumor's radiotherapic treatments. The problem's scenario inherent to the patient is simulated by such process, using the volume element (voxel) as a unit of computational tracing. The head's voxel structure geometry has voxels with volumetric dimensions around 1 mm{sup 3} and a population of millions, which helps - in that way, for a realistic simulation and a decrease in image's digital process techniques for adjustments and equalizations. With such additional data from the code, a more critical analysis can be developed in order to determine the volume of the tumor, and the protection, beside the patients' medical images were borrowed by Clinicas Oncologicas Integradas (COI/RJ), joined to the previous performed planning. In order to execute this computational process, SAPDI computational system is used in a digital image process for optimization of data, conversion program Scan2MCNP, which manipulates, processes, and converts the medical images into voxel structures to input files and the graphic visualizer Moritz for the verification of image's geometry placing. (author)

  12. Electron diffraction and high-resolution transmission electron microscopy of the high temperature crystal structures of GexSb2Te3+x (x=1,2,3) phase change material

    NARCIS (Netherlands)

    Kooi, B.J.; de Hosson, J.T.M.

    2002-01-01

    The crystal structures of GeSb2Te4, Ge2Sb2Te5, and Ge3Sb2Te6 were determined using electron diffraction and high-resolution transmission electron microscopy. The structure determined for the former two crystals deviates from the ones proposed in the literature. These crystal structures were

  13. Investigating Mercury's South Polar Deposits: Arecibo Radar Observations and High-Resolution Determination of Illumination Conditions

    Science.gov (United States)

    Chabot, Nancy L.; Shread, Evangela E.; Harmon, John K.

    2018-02-01

    There is strong evidence that Mercury's polar deposits are water ice hosted in permanently shadowed regions. In this study, we present new Arecibo radar observations of Mercury's south pole, which reveal numerous radar-bright deposits and substantially increase the radar imaging coverage. We also use images from MESSENGER's full mission to determine the illumination conditions of Mercury's south polar region at the same spatial resolution as the north polar region, enabling comparisons between the two poles. The area of radar-bright deposits in Mercury's south is roughly double that found in the north, consistent with the larger permanently shadowed area in the older, cratered terrain at the south relative to the younger smooth plains at the north. Radar-bright features are strongly associated with regions of permanent shadow at both poles, consistent with water ice being the dominant component of the deposits. However, both of Mercury's polar regions show that roughly 50% of permanently shadowed regions lack radar-bright deposits, despite some of these locations having thermal environments that are conducive to the presence of water ice. The observed uneven distribution of water ice among Mercury's polar cold traps may suggest that the source of Mercury's water ice was not a steady, regular process but rather that the source was an episodic event, such as a recent, large impact on the innermost planet.

  14. Demonstrating the Uneven Importance of Fine-Scale Forest Structure on Snow Distributions using High Resolution Modeling

    Science.gov (United States)

    Broxton, P. D.; Harpold, A. A.; van Leeuwen, W.; Biederman, J. A.

    2016-12-01

    Quantifying the amount of snow in forested mountainous environments, as well as how it may change due to warming and forest disturbance, is critical given its importance for water supply and ecosystem health. Forest canopies affect snow accumulation and ablation in ways that are difficult to observe and model. Furthermore, fine-scale forest structure can accentuate or diminish the effects of forest-snow interactions. Despite decades of research demonstrating the importance of fine-scale forest structure (e.g. canopy edges and gaps) on snow, we still lack a comprehensive understanding of where and when forest structure has the largest impact on snowpack mass and energy budgets. Here, we use a hyper-resolution (1 meter spatial resolution) mass and energy balance snow model called the Snow Physics and Laser Mapping (SnowPALM) model along with LIDAR-derived forest structure to determine where spatial variability of fine-scale forest structure has the largest influence on large scale mass and energy budgets. SnowPALM was set up and calibrated at sites representing diverse climates in New Mexico, Arizona, and California. Then, we compared simulations at different model resolutions (i.e. 1, 10, and 100 m) to elucidate the effects of including versus not including information about fine scale canopy structure. These experiments were repeated for different prescribed topographies (i.e. flat, 30% slope north, and south-facing) at each site. Higher resolution simulations had more snow at lower canopy cover, with the opposite being true at high canopy cover. Furthermore, there is considerable scatter, indicating that different canopy arrangements can lead to different amounts of snow, even when the overall canopy coverage is the same. This modeling is contributing to the development of a high resolution machine learning algorithm called the Snow Water Artificial Network (SWANN) model to generate predictions of snow distributions over much larger domains, which has implications

  15. Structural characterizaiton and gas reactions of small metal particles by high-resolution, in-situ TEM and TED

    Science.gov (United States)

    1984-01-01

    The existing in-situ transmission electron microscopy (TEM) facility was improved by adding a separately pumped mini-specimen chamber. The chamber contains wire-evaporation sources for three metals and a specimen heater for moderate substrate temperatures. A sample introduction device was constructed, installed, and tested, facilitating rapid introduction of a specimen into the mini-chamber while maintaining the background pressure in that chamber in the 10(-9) millibar range. Small particles and clusters of Pd, grown by deposition from the vapor phase in an in-situ TEM facility on amorphous and crystalline support films of alumina and on ultra-thin carbon films, were analyzed by conventional high-resolution TEM and image analysis in terms of detectability, number density, and size distribution. The smallest particles that could be detected and counted contained no more than 6 atoms; size determinations could be made for particles 1 nm in diameter. The influence of various oxygen plasma treatments, annealing treatments, and of increasing the substrate temperature during deposition was investigated. The TEM technique was employed to demonstrate that under otherwise identica l conditions the lattice parameter of Pd particles in the 1 to 2 nm size range and supported in random orientation on ex-situ prepared mica films is expanded by some 3% when compared to 5 nm size particles. It is believed that this expansion is neither a small-particle diffraction effect nor due to pseudomorphism, but that it is due to a annealing-induced transformation of the small as-deposited particles with predominantly composite crystal structures into larger particles with true f.c.c. structure and thus inherently smaller lattice parameter.

  16. Structural Characterization of a Thrombin-Aptamer Complex by High Resolution Native Top-Down Mass Spectrometry

    Science.gov (United States)

    Zhang, Jiang; Loo, Rachel R. Ogorzalek; Loo, Joseph A.

    2017-09-01

    Native mass spectrometry (MS) with electrospray ionization (ESI) has evolved as an invaluable tool for the characterization of intact native proteins and non-covalently bound protein complexes. Here we report the structural characterization by high resolution native top-down MS of human thrombin and its complex with the Bock thrombin binding aptamer (TBA), a 15-nucleotide DNA with high specificity and affinity for thrombin. Accurate mass measurements revealed that the predominant form of native human α-thrombin contains a glycosylation mass of 2205 Da, corresponding to a sialylated symmetric biantennary oligosaccharide structure without fucosylation. Native MS showed that thrombin and TBA predominantly form a 1:1 complex under near physiological conditions (pH 6.8, 200 mM NH4OAc), but the binding stoichiometry is influenced by the solution ionic strength. In 20 mM ammonium acetate solution, up to two TBAs were bound to thrombin, whereas increasing the solution ionic strength destabilized the thrombin-TBA complex and 1 M NH4OAc nearly completely dissociated the complex. This observation is consistent with the mediation of thrombin-aptamer binding through electrostatic interactions and it is further consistent with the human thrombin structure that contains two anion binding sites on the surface. Electron capture dissociation (ECD) top-down MS of the thrombin-TBA complex performed with a high resolution 15 Tesla Fourier transform ion cyclotron resonance (FTICR) mass spectrometer showed the primary binding site to be at exosite I located near the N-terminal sequence of the heavy chain, consistent with crystallographic data. High resolution native top-down MS is complementary to traditional structural biology methods for structurally characterizing native proteins and protein-DNA complexes. [Figure not available: see fulltext.

  17. Absorbed dose estimates to structures of the brain and head using a high-resolution voxel-based head phantom

    International Nuclear Information System (INIS)

    Evans, Jeffrey F.; Blue, Thomas E.; Gupta, Nilendu

    2001-01-01

    The purpose of this article is to demonstrate the viability of using a high-resolution 3-D head phantom in Monte Carlo N-Particle (MCNP) for boron neutron capture therapy (BNCT) structure dosimetry. This work describes a high-resolution voxel-based model of a human head and its use for calculating absorbed doses to the structures of the brain. The Zubal head phantom is a 3-D model of a human head that can be displayed and manipulated on a computer. Several changes were made to the original head phantom which now contains over 29 critical structures of the brain and head. The modified phantom is a 85x109x120 lattice of voxels, where each voxel is 2.2x2.2x1.4 mm 3 . This model was translated into MCNP lattice format. As a proof of principle study, two MCNP absorbed dose calculations were made (left and right lateral irradiations) using a uniformly distributed neutron disk source with an 1/E energy spectrum. Additionally, the results of these two calculations were combined to estimate the absorbed doses from a bilateral irradiation. Radiobiologically equivalent (RBE) doses were calculated for all structures and were normalized to 12.8 Gy-Eq. For a left lateral irradiation, the left motor cortex receives the limiting RBE dose. For a bilateral irradiation, the insula cortices receive the limiting dose. Among the nonencephalic structures, the parotid glands receive RBE doses that were within 15% of the limiting dose

  18. High-resolution crystal structures of protein helices reconciled with three-centered hydrogen bonds and multipole electrostatics.

    Science.gov (United States)

    Kuster, Daniel J; Liu, Chengyu; Fang, Zheng; Ponder, Jay W; Marshall, Garland R

    2015-01-01

    Theoretical and experimental evidence for non-linear hydrogen bonds in protein helices is ubiquitous. In particular, amide three-centered hydrogen bonds are common features of helices in high-resolution crystal structures of proteins. These high-resolution structures (1.0 to 1.5 Å nominal crystallographic resolution) position backbone atoms without significant bias from modeling constraints and identify Φ = -62°, ψ = -43 as the consensus backbone torsional angles of protein helices. These torsional angles preserve the atomic positions of α-β carbons of the classic Pauling α-helix while allowing the amide carbonyls to form bifurcated hydrogen bonds as first suggested by Némethy et al. in 1967. Molecular dynamics simulations of a capped 12-residue oligoalanine in water with AMOEBA (Atomic Multipole Optimized Energetics for Biomolecular Applications), a second-generation force field that includes multipole electrostatics and polarizability, reproduces the experimentally observed high-resolution helical conformation and correctly reorients the amide-bond carbonyls into bifurcated hydrogen bonds. This simple modification of backbone torsional angles reconciles experimental and theoretical views to provide a unified view of amide three-centered hydrogen bonds as crucial components of protein helices. The reason why they have been overlooked by structural biologists depends on the small crankshaft-like changes in orientation of the amide bond that allows maintenance of the overall helical parameters (helix pitch (p) and residues per turn (n)). The Pauling 3.6(13) α-helix fits the high-resolution experimental data with the minor exception of the amide-carbonyl electron density, but the previously associated backbone torsional angles (Φ, Ψ) needed slight modification to be reconciled with three-atom centered H-bonds and multipole electrostatics. Thus, a new standard helix, the 3.6(13/10)-, Némethy- or N-helix, is proposed. Due to the use of constraints from

  19. High-resolution ultrasound biomicroscopy for monitoring ovarian structures in mice

    Directory of Open Access Journals (Sweden)

    Singh Jaswant

    2009-07-01

    Full Text Available Abstract Background Until recently, the limit of spatial resolution of ultrasound systems has prevented characterization of structures Methods Experiment 1 was a pilot study to develop methods of immobilization (physical restraint vs. general anesthesia and determine technical factors affecting ovarian images using ultrasound bio-microscopy in rats vs. mice. The hair coat was removed over the thoraco-lumber area using depilation cream, and a highly viscous acoustic gel was applied while the animals were maintained in sternal recumbency. In Experiment 2, changes in ovarian structures during the estrous cycle were monitored by twice daily ultrasonography in 10 mice for 2 estrous cycles. Results Ovarian images were not distinct in rats due to attenuation of ultrasound waves. Physical restraint, without general anesthesia, was insufficient for immobilization in mice. By placing the transducer face over the dorsal flank, the kidney was visualized initially as a point of reference. A routine of moving the transducer a few millimetres caudo-laterally from the kidney was established to quickly and consistently localize the ovaries; the total time to scan both ovaries in a mouse was about 10 minutes. By comparing vaginal cytology with non-anesthetized controls, repeated exposure to anesthesia did not affect the estrous cycle. Temporal changes in the number of follicles in 3 different size categories support the hypothesis that follicles ≥ 20 microns develop in a wave-like fashion. Conclusion The mouse is a suitable model for the study of ovarian dynamics using transcutaneous ultrasound bio-microscopy. Repeated general anesthesia for examination had no apparent effect on the estrous cycle, and preliminary results revealed a wave-like pattern of ovarian follicle development in mice.

  20. Median filters as a tool to determine dark noise thresholds in high resolution smartphone image sensors for scientific imaging

    Science.gov (United States)

    Igoe, Damien P.; Parisi, Alfio V.; Amar, Abdurazaq; Rummenie, Katherine J.

    2018-01-01

    An evaluation of the use of median filters in the reduction of dark noise in smartphone high resolution image sensors is presented. The Sony Xperia Z1 employed has a maximum image sensor resolution of 20.7 Mpixels, with each pixel having a side length of just over 1 μm. Due to the large number of photosites, this provides an image sensor with very high sensitivity but also makes them prone to noise effects such as hot-pixels. Similar to earlier research with older models of smartphone, no appreciable temperature effects were observed in the overall average pixel values for images taken in ambient temperatures between 5 °C and 25 °C. In this research, hot-pixels are defined as pixels with intensities above a specific threshold. The threshold is determined using the distribution of pixel values of a set of images with uniform statistical properties associated with the application of median-filters of increasing size. An image with uniform statistics was employed as a training set from 124 dark images, and the threshold was determined to be 9 digital numbers (DN). The threshold remained constant for multiple resolutions and did not appreciably change even after a year of extensive field use and exposure to solar ultraviolet radiation. Although the temperature effects' uniformity masked an increase in hot-pixel occurrences, the total number of occurrences represented less than 0.1% of the total image. Hot-pixels were removed by applying a median filter, with an optimum filter size of 7 × 7; similar trends were observed for four additional smartphone image sensors used for validation. Hot-pixels were also reduced by decreasing image resolution. The method outlined in this research provides a methodology to characterise the dark noise behavior of high resolution image sensors for use in scientific investigations, especially as pixel sizes decrease.

  1. High Resolution/High Fidelity Seismic Imaging and Parameter Estimation for Geological Structure and Material Characterization

    Energy Technology Data Exchange (ETDEWEB)

    Ru-Shan Wu; Xiao-Bi Xie

    2008-06-08

    Our proposed work on high resolution/high fidelity seismic imaging focused on three general areas: (1) development of new, more efficient, wave-equation-based propagators and imaging conditions, (2) developments towards amplitude-preserving imaging in the local angle domain, in particular, imaging methods that allow us to estimate the reflection as a function of angle at a layer boundary, and (3) studies of wave inversion for local parameter estimation. In this report we summarize the results and progress we made during the project period. The report is divided into three parts, totaling 10 chapters. The first part is on resolution analysis and its relation to directional illumination analysis. The second part, which is composed of 6 chapters, is on the main theme of our work, the true-reflection imaging. True-reflection imaging is an advanced imaging technology which aims at keeping the image amplitude proportional to the reflection strength of the local reflectors or to obtain the reflection coefficient as function of reflection-angle. There are many factors which may influence the image amplitude, such as geometrical spreading, transmission loss, path absorption, acquisition aperture effect, etc. However, we can group these into two categories: one is the propagator effect (geometric spreading, path losses); the other is the acquisition-aperture effect. We have made significant progress in both categories. We studied the effects of different terms in the true-amplitude one-way propagators, especially the terms including lateral velocity variation of the medium. We also demonstrate the improvements by optimizing the expansion coefficients in different terms. Our research also includes directional illumination analysis for both the one-way propagators and full-wave propagators. We developed the fast acquisition-aperture correction method in the local angle-domain, which is an important element in the true-reflection imaging. Other developments include the super

  2. Real time, high resolution studies of protein adsorption and structure at the solid-liquid interface using dual polarization interferometry

    International Nuclear Information System (INIS)

    Freeman, Neville J; Peel, Louise L; Swann, Marcus J; Cross, Graham H; Reeves, Andrew; Brand, Stuart; Lu, Jian R

    2004-01-01

    A novel method for the analysis of thin biological films, called dual polarization interferometry (DPI), is described. This high resolution (<1 A), laboratory-based technique allows the thickness and refractive index (density) of biological molecules adsorbing or reacting at the solid-liquid interface to be measured in real time (up to 10 measurements per second). Results from the adsorption of bovine serum albumin (BSA) on to a silicon oxynitride chip surface are presented to demonstrate how time dependent molecular behaviour can be examined using DPI. Mechanistic and structural information relating to the adsorption process is obtained as a function of the solution pH

  3. Mobile and embedded fast high resolution image stitching for long length rectangular monochromatic objects with periodic structure

    Science.gov (United States)

    Limonova, Elena; Tropin, Daniil; Savelyev, Boris; Mamay, Igor; Nikolaev, Dmitry

    2018-04-01

    In this paper we describe stitching protocol, which allows to obtain high resolution images of long length monochromatic objects with periodic structure. This protocol can be used for long length documents or human-induced objects in satellite images of uninhabitable regions like Arctic regions. The length of such objects can reach notable values, while modern camera sensors have limited resolution and are not able to provide good enough image of the whole object for further processing, e.g. using in OCR system. The idea of the proposed method is to acquire a video stream containing full object in high resolution and use image stitching. We expect the scanned object to have straight boundaries and periodic structure, which allow us to introduce regularization to the stitching problem and adapt algorithm for limited computational power of mobile and embedded CPUs. With the help of detected boundaries and structure we estimate homography between frames and use this information to reduce complexity of stitching. We demonstrate our algorithm on mobile device and show image processing speed of 2 fps on Samsung Exynos 5422 processor

  4. Lunar Circular Structure Classification from Chang 'e 2 High Resolution Lunar Images with Convolutional Neural Network

    Science.gov (United States)

    Zeng, X. G.; Liu, J. J.; Zuo, W.; Chen, W. L.; Liu, Y. X.

    2018-04-01

    Circular structures are widely distributed around the lunar surface. The most typical of them could be lunar impact crater, lunar dome, et.al. In this approach, we are trying to use the Convolutional Neural Network to classify the lunar circular structures from the lunar images.

  5. Structural Characterisation of Acetogenins from Annona muricata by Supercritical Fluid Chromatography Coupled to High-Resolution Tandem Mass Spectrometry.

    Science.gov (United States)

    Laboureur, Laurent; Bonneau, Natacha; Champy, Pierre; Brunelle, Alain; Touboul, David

    2017-11-01

    Acetogenins are plant polyketides known to be cytotoxic and proposed as antitumor candidates. They are also suspected to be alimentary neurotoxins. Their occurrence as complex mixtures renders their dereplication and structural identification difficult using liquid chromatography coupled to tandem mass spectrometry and efforts are required to improve the methodology. To develop a supercritical fluid chromatography (SFC) high-resolution tandem mass spectrometry method, involving lithium post-column cationisation, for the structural characterisation of Annonaceous acetogenins in crude extracts. The seeds of Annona muricata L. were extracted with methanol. Supercritical fluid chromatography of the extract, using a 2-ethylpyridine stationary phase column, was monitored using a high-resolution quadrupole time-of-flight mass spectrometer. Lithium iodide was added post-column in the make-up solvent. For comparison, the same extract was analysed using high-pressure liquid chromatography coupled to the same mass spectrometer, with a column based on solid core particles. Sensitivity was similar for both HPLC and SFC approaches. Retention behaviour and fragmentation pathways of three different isomer groups are described. A previously unknown group of acetogenins was also evidenced for the first time. The use of SFC-MS/MS allows the reduction of the time of analysis, of environmental impact and an increase in the chromatographic resolution, compared to liquid chromatography. This new methodology enlightened a new group of acetogenins, isomers of montanacin-D. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  6. High resolution (transformers.

    Science.gov (United States)

    Garcia-Souto, Jose A; Lamela-Rivera, Horacio

    2006-10-16

    A novel fiber-optic interferometric sensor is presented for vibrations measurements and analysis. In this approach, it is shown applied to the vibrations of electrical structures within power transformers. A main feature of the sensor is that an unambiguous optical phase measurement is performed using the direct detection of the interferometer output, without external modulation, for a more compact and stable implementation. High resolution of the interferometric measurement is obtained with this technique (transformers are also highlighted.

  7. The digital structural analysis of cadmium selenide crystals by a method of ion beam thinning for high resolution electron microscopy

    International Nuclear Information System (INIS)

    Kanaya, Koichi; Baba, Norio; Naka, Michiaki; Kitagawa, Yukihisa; Suzuki, Kunio

    1986-01-01

    A digital processing method using a scanning densitometer system for structural analysis of electron micrographs was successfully applied to a study of cadmium selenide crystals, which were prepared by an argon-ion beam thinning method. Based on Fourier techniques for structural analysis from a computer-generated diffractogram, it was demonstrated that when cadmium selenide crystals were sufficiently thin to display the higher order diffraction spots at a high resolution approaching the atomic level, they constitute an alternative hexagonal lattice of imperfect wurtzite phase from a superposition of individual harmonic images by the enhanced scattering amplitude and corrected phase. From the structural analysis data, a Fourier synthetic lattice image was reconstructed, representing the precise location and three-dimensional arrangement of each of the atoms in the unit cell. Extensively enhanced lattice defect images of dislocations and stacking faults were also derived and shown graphically. (author)

  8. Structure of Se-rich As-Se glasses by high-resolution x-ray photoelectron spectroscopy

    International Nuclear Information System (INIS)

    Golovchak, R.; Kovalskiy, A.; Miller, A. C.; Jain, H.; Shpotyuk, O.

    2007-01-01

    To establish the validity of various proposed structural models, we have investigated the structure of the binary As x Se 100-x chalcogenide glass family (x≤40) by high-resolution x-ray photoelectron spectroscopy. From the composition dependence of the valence band, the contributions to the density of states from the 4p lone pair electrons of Se and the 4p bonding states and 4s electrons of Se and As are identified in the top part of the band. The analysis of Se 3d and As 3d core-level spectra supports the so-called chain crossing model for the atomic structure of Se-rich As x Se 100-x bulk glasses. The results also indicate small deviations (∼3-8%) from this model, especially for glass compositions with short Se chains (25 40 Se 60 and of Se-Se-Se fragments in a glass with composition x=30 is established

  9. A first principles study of the binding of formic acid in catalase complementing high resolution X-ray structures

    International Nuclear Information System (INIS)

    Rovira, Carme; Alfonso-Prieto, Mercedes; Biarnes, Xevi; Carpena, Xavi; Fita, Ignacio; Loewen, Peter C.

    2006-01-01

    Density functional molecular dynamics simulations using a QM/MM approach are used to get insight into the binding modes of formic acid in catalase. Two ligand binding sites are found, named A and B, in agreement with recent high resolution structures of catalase with bound formic acid. In addition, the calculations show that the His56 residue is protonated and the ligand is present as a formate anion. The lowest energy minimum structure (A) corresponds to the ligand interacting with both the heme iron and the catalytic residues (His56 and Asn129). The second minimum energy structure (B) corresponds to the situation in which the ligand interacts solely with the catalytic residues. A mechanism for the process of formic acid binding in catalase is suggested

  10. Use of high-resolution satellite images for detection of geological structures related to Calerias geothermal field, Chile

    Science.gov (United States)

    Arellano-Baeza, A. A.; Urzua, L.

    2011-12-01

    Chile has enormous potential to use the geothermal resources for electric energy generation. The main geothermal fields are located in the Central Andean Volcanic Chain in the North, between the Central valley and the border with Argentina in the center, and in the fault system Liquiñe-Ofqui in the South of the country. High resolution images from the LANDSAT and ASTER satellites have been used to delineate the geological structures related to the Calerias geothermal field located at the northern end of the Southern Volcanic Zone of Chile. It was done by applying the lineament extraction technique developed by authors. These structures have been compared with the distribution of main geological structures obtained in the field. It was found that the lineament density increases in the areas of the major heat flux indicating that the lineament analysis could be a power tool for the detection of faults and joint zones associated to the geothermal fields.

  11. A first principles study of the binding of formic acid in catalase complementing high resolution X-ray structures

    Energy Technology Data Exchange (ETDEWEB)

    Rovira, Carme [Centre especial de Recerca en Quimica Teorica, Parc Cientific de Barcelona, Josep Samitier 1-5, 08028 Barcelona (Spain)], E-mail: crovira@pcb.ub.es; Alfonso-Prieto, Mercedes [Centre especial de Recerca en Quimica Teorica, Parc Cientific de Barcelona, Josep Samitier 1-5, 08028 Barcelona (Spain); Biarnes, Xevi [Centre especial de Recerca en Quimica Teorica, Parc Cientific de Barcelona, Josep Samitier 1-5, 08028 Barcelona (Spain); Carpena, Xavi [Consejo Superior de Investigaciones Cientificas y Parc Cientific de Barcelona (CSIC-PCB), Josep Samitier 1-5, 08028 Barcelona (Spain); Fita, Ignacio [Consejo Superior de Investigaciones Cientificas y Parc Cientific de Barcelona (CSIC-PCB), Josep Samitier 1-5, 08028 Barcelona (Spain); Loewen, Peter C. [Department of Microbiology, University of Manitoba, Winnipeg, Canada MB R3T 2N2 (Canada)

    2006-03-31

    Density functional molecular dynamics simulations using a QM/MM approach are used to get insight into the binding modes of formic acid in catalase. Two ligand binding sites are found, named A and B, in agreement with recent high resolution structures of catalase with bound formic acid. In addition, the calculations show that the His56 residue is protonated and the ligand is present as a formate anion. The lowest energy minimum structure (A) corresponds to the ligand interacting with both the heme iron and the catalytic residues (His56 and Asn129). The second minimum energy structure (B) corresponds to the situation in which the ligand interacts solely with the catalytic residues. A mechanism for the process of formic acid binding in catalase is suggested.

  12. Determination of sulfur in coal and ash slurry by high-resolution continuum source electrothermal molecular absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Nakadi, Flávio V.; Rosa, Lilian R.; Veiga, Márcia A.M.S. da, E-mail: mamsveiga@ffclrp.usp.br

    2013-10-01

    We propose a procedure for the determination of sulfur in coal slurries by high resolution continuum source electrothermal molecular absorption spectrometry. The slurry, whose concentration is 1 mg mL{sup −1}, was prepared by mixing 50 mg of the sample with 5% v/v nitric acid and 0.04% m/v Triton X-100 and was homogenized manually. It sustained good stability. The determination was performed via CS molecular absorption at 257.592 nm, and the optimized vaporization temperature was 2500 °C. The accuracy of the method was ensured by analysis of certified reference materials SRM 1632b (trace elements in coal) and SRM 1633b (coal fly ash) from the National Institute of Standards and Technology, using external calibration with aqueous standards prepared in the same medium and used as slurry. We achieved good agreement with the certified reference materials within 95% confidence interval, LOD of 0.01% w/w, and RSD of 6%, which confirms the potential of the proposed method. - Highlights: • HR-CS ET MAS as a technique to determine sulfur in coal and ash • Utilization of (coal and coal fly ash) slurry as a sample preparation • Simple and fast method, which uses external calibration with aqueous standards without chemical modifier.

  13. Ability of High-Resolution Manometry to Determine Feeding Method and to Predict Aspiration Pneumonia in Patients With Dysphagia.

    Science.gov (United States)

    Park, Chul-Hyun; Lee, Yong-Taek; Yi, Youbin; Lee, Jung-Sang; Park, Jung Ho; Yoon, Kyung Jae

    2017-07-01

    The introduction of high-resolution manometry (HRM) offered an improved method to objectively analyze the status of pharynx and esophagus. At present, HRM for patients with oropharyngeal dysphagia has been poorly studied. We aimed to determine feeding method and predict the development of aspiration pneumonia in patients with oropharyngeal dysphagia using HRM. We recruited 120 patients with dysphagia who underwent both HRM and videofluoroscopic swallow study. HRM was used to estimate pressure events from velopharynx (VP) to upper esophageal sphincter (UES). Feeding methods were determined to non-oral or oral feeding according to dysphagia severity. We prospectively followed patients to assess the development of aspiration pneumonia. VP maximal pressure and UES relaxation duration were independently associated with non-oral feeding. Non-oral feeding was determined based on optimal cutoff value of 105.0 mm Hg for VP maximal pressure (95.0% sensitivity and 70.0% specificity) and 0.45 s for UES relaxation duration (76.3% sensitivity and 57.5% specificity), respectively. During a mean follow-up of 18.8 months, 15.8% of patients developed aspiration pneumonia. On multivariate Cox regression analysis, VP maximal pressure (Pdysphagia.

  14. Possibilities of High Resolution Inductively Coupled Plasma Optical Emission Spectrometry in the Determination of Trace Elements in Environmental Materials

    Directory of Open Access Journals (Sweden)

    Nikolaya Velitchkova

    2013-01-01

    Full Text Available This paper presents new quantitative data for the spectral interferences obtained by high resolution 40.68 MHz radial viewing inductively coupled plasma optical emission spectrometry (HR-ICP-OES in the determination of Zn, Cd, Sb, Cu, Mn, Pb, Sn, Cr, U, and Ba in environmental materials in the presence of a complex matrix, containing Al, Ca, Fe, Mg, and Ti. The -concept for quantification of spectral interferences was used. The optimum line selection for trace analysis of a variety of multicomponent matrices requires the choice of prominent lines, which are free or negligibly influenced by line interference problems. The versatility of -concept as basic methodology was experimentally demonstrated in the determination of trace of elements in soil and drinking water. The detection limits are lower in comparison with corresponding threshold concentration levels for soil and drinking water in accordance with environmental regulations. This paper shows the possibilities of present day ICP-OES equipment in the direct determination of trace elements (without preconcentration of impurities in environmental samples.

  15. Structure Annotation and Quantification of Wheat Seed Oxidized Lipids by High-Resolution LC-MS/MS.

    Science.gov (United States)

    Riewe, David; Wiebach, Janine; Altmann, Thomas

    2017-10-01

    Lipid oxidation is a process ubiquitous in life, but the direct and comprehensive analysis of oxidized lipids has been limited by available analytical methods. We applied high-resolution liquid chromatography-mass spectrometry (LC-MS) and tandem mass spectrometry (MS/MS) to quantify oxidized lipids (glycerides, fatty acids, phospholipids, lysophospholipids, and galactolipids) and implemented a platform-independent high-throughput-amenable analysis pipeline for the high-confidence annotation and acyl composition analysis of oxidized lipids. Lipid contents of 90 different naturally aged wheat ( Triticum aestivum ) seed stocks were quantified in an untargeted high-resolution LC-MS experiment, resulting in 18,556 quantitative mass-to-charge ratio features. In a posthoc liquid chromatography-tandem mass spectrometry experiment, high-resolution MS/MS spectra (5 mD accuracy) were recorded for 8,957 out of 12,080 putatively monoisotopic features of the LC-MS data set. A total of 353 nonoxidized and 559 oxidized lipids with up to four additional oxygen atoms were annotated based on the accurate mass recordings (1.5 ppm tolerance) of the LC-MS data set and filtering procedures. MS/MS spectra available for 828 of these annotations were analyzed by translating experimentally known fragmentation rules of lipids into the fragmentation of oxidized lipids. This led to the identification of 259 nonoxidized and 365 oxidized lipids by both accurate mass and MS/MS spectra and to the determination of acyl compositions for 221 nonoxidized and 295 oxidized lipids. Analysis of 15-year aged wheat seeds revealed increased lipid oxidation and hydrolysis in seeds stored in ambient versus cold conditions. © 2017 The author(s). All Rights Reserved.

  16. High-resolution anatomy of the human brain stem using 7-T MRI: improved detection of inner structures and nerves?

    Energy Technology Data Exchange (ETDEWEB)

    Gizewski, Elke R. [Medical University Innsbruck, Department of Neuroradiology, Innsbruck (Austria); Maderwald, Stefan [University Duisburg-Essen, Erwin L. Hahn Institute for Magnetic Resonance Imaging, Essen (Germany); Linn, Jennifer; Bochmann, Katja [LMU Munich, Department of Neuroradiology, Munich (Germany); Dassinger, Benjamin [Medical University Innsbruck, Department of Neuroradiology, Innsbruck (Austria); Justus-Liebig-University Giessen, Department of Neuroradiology, Giessen (Germany); Forsting, Michael [University Hospital, University Duisburg-Essen, Departments of Diagnostic and Interventional Radiology and Neuroradiology, Essen (Germany); Ladd, Mark E. [University Duisburg-Essen, Erwin L. Hahn Institute for Magnetic Resonance Imaging, Essen (Germany); University Hospital, University Duisburg-Essen, Departments of Diagnostic and Interventional Radiology and Neuroradiology, Essen (Germany)

    2014-03-15

    The purpose of this paper is to assess the value of 7 Tesla (7 T) MRI for the depiction of brain stem and cranial nerve (CN) anatomy. Six volunteers were examined at 7 T using high-resolution SWI, MPRAGE, MP2RAGE, 3D SPACE T2, T2, and PD images to establish scanning parameters targeted at optimizing spatial resolution. Direct comparisons between 3 and 7 T were performed in two additional subjects using the finalized sequences (3 T: T2, PD, MPRAGE, SWAN; 7 T: 3D T2, MPRAGE, SWI, MP2RAGE). Artifacts and the depiction of structures were evaluated by two neuroradiologists using a standardized score sheet. Sequences could be established for high-resolution 7 T imaging even in caudal cranial areas. High in-plane resolution T2, PD, and SWI images provided depiction of inner brain stem structures such as pons fibers, raphe, reticular formation, nerve roots, and periaqueductal gray. MPRAGE and MP2RAGE provided clear depiction of the CNs. 3D T2 images improved depiction of inner brain structure in comparison to T2 images at 3 T. Although the 7-T SWI sequence provided improved contrast to some inner structures, extended areas were influenced by artifacts due to image disturbances from susceptibility differences. Seven-tesla imaging of basal brain areas is feasible and might have significant impact on detection and diagnosis in patients with specific diseases, e.g., trigeminal pain related to affection of the nerve root. Some inner brain stem structures can be depicted at 3 T, but certain sequences at 7 T, in particular 3D SPACE T2, are superior in producing anatomical in vivo images of deep brain stem structures. (orig.)

  17. High-resolution anatomy of the human brain stem using 7-T MRI: improved detection of inner structures and nerves?

    International Nuclear Information System (INIS)

    Gizewski, Elke R.; Maderwald, Stefan; Linn, Jennifer; Bochmann, Katja; Dassinger, Benjamin; Forsting, Michael; Ladd, Mark E.

    2014-01-01

    The purpose of this paper is to assess the value of 7 Tesla (7 T) MRI for the depiction of brain stem and cranial nerve (CN) anatomy. Six volunteers were examined at 7 T using high-resolution SWI, MPRAGE, MP2RAGE, 3D SPACE T2, T2, and PD images to establish scanning parameters targeted at optimizing spatial resolution. Direct comparisons between 3 and 7 T were performed in two additional subjects using the finalized sequences (3 T: T2, PD, MPRAGE, SWAN; 7 T: 3D T2, MPRAGE, SWI, MP2RAGE). Artifacts and the depiction of structures were evaluated by two neuroradiologists using a standardized score sheet. Sequences could be established for high-resolution 7 T imaging even in caudal cranial areas. High in-plane resolution T2, PD, and SWI images provided depiction of inner brain stem structures such as pons fibers, raphe, reticular formation, nerve roots, and periaqueductal gray. MPRAGE and MP2RAGE provided clear depiction of the CNs. 3D T2 images improved depiction of inner brain structure in comparison to T2 images at 3 T. Although the 7-T SWI sequence provided improved contrast to some inner structures, extended areas were influenced by artifacts due to image disturbances from susceptibility differences. Seven-tesla imaging of basal brain areas is feasible and might have significant impact on detection and diagnosis in patients with specific diseases, e.g., trigeminal pain related to affection of the nerve root. Some inner brain stem structures can be depicted at 3 T, but certain sequences at 7 T, in particular 3D SPACE T2, are superior in producing anatomical in vivo images of deep brain stem structures. (orig.)

  18. Determination of cobalt in biological samples by line-source and high-resolution continuum source graphite furnace atomic absorption spectrometry using solid sampling or alkaline treatment

    International Nuclear Information System (INIS)

    Ribeiro, Anderson Schwingel; Vieira, Mariana Antunes; Furtado da Silva, Alessandra; Borges, Daniel L. Gallindo; Welz, Bernhard; Heitmann, Uwe; Curtius, Adilson Jose

    2005-01-01

    Two procedures for the determination of Co in biological samples by graphite furnace atomic absorption spectrometry (GF AAS) were compared: solid sampling (SS) and alkaline treatment with tetramethylammonium hydroxide (TMAH) using two different instruments for the investigation: a conventional line-source (LS) atomic absorption spectrometer and a prototype high-resolution continuum source atomic absorption spectrometer. For the direct introduction of the solid samples, certified reference materials (CRM) were ground to a particle size ≤50 μm. Alkaline treatment was carried out by placing about 250 mg of the sample in polypropylene flasks, adding 2 mL of 25% m/v tetramethylammonium hydroxide and de-ionized water. Due to its unique capacity of providing a 3-D spectral plot, a high-resolution continuum source (HR-CS) graphite furnace atomic absorption spectrometry was used as a tool to evaluate potential spectral interferences, including background absorption for both sample introduction procedures, revealing that a continuous background preceded the atomic signal for pyrolysis temperatures lower than 700 deg. C. Molecular absorption bands with pronounced rotational fine structure appeared for atomization temperatures >1800 deg. C probably as a consequence of the formation of PO. After optimization had been carried out using high resolution continuum source atomic absorption spectrometry, the optimized conditions were adopted also for line-source atomic absorption spectrometry. Six biological certified reference materials were analyzed, with calibration against aqueous standards, resulting in agreement with the certified values (according to the t-test for a 95% confidence level) and in detection limits as low as 5 ng g -1

  19. High-resolution structure of TBP with TAF1 reveals anchoring patterns in transcriptional regulation.

    Science.gov (United States)

    Anandapadamanaban, Madhanagopal; Andresen, Cecilia; Helander, Sara; Ohyama, Yoshifumi; Siponen, Marina I; Lundström, Patrik; Kokubo, Tetsuro; Ikura, Mitsuhiko; Moche, Martin; Sunnerhagen, Maria

    2013-08-01

    The general transcription factor TFIID provides a regulatory platform for transcription initiation. Here we present the crystal structure (1.97 Å) and NMR analysis of yeast TAF1 N-terminal domains TAND1 and TAND2 bound to yeast TBP, together with mutational data. We find that yeast TAF1-TAND1, which in itself acts as a transcriptional activator, binds TBP's concave DNA-binding surface by presenting similar anchor residues to TBP as does Mot1 but from a distinct structural scaffold. Furthermore, we show how TAF1-TAND2 uses an aromatic and acidic anchoring pattern to bind a conserved TBP surface groove traversing the basic helix region, and we find highly similar TBP-binding motifs also presented by the structurally distinct TFIIA, Mot1 and Brf1 proteins. Our identification of these anchoring patterns, which can be easily disrupted or enhanced, provides insight into the competitive multiprotein TBP interplay critical to transcriptional regulation.

  20. High-resolution studies of the structure of the solar atmosphere using a new imaging algorithm

    Science.gov (United States)

    Karovska, Margarita; Habbal, Shadia Rifai

    1991-01-01

    The results of the application of a new image restoration algorithm developed by Ayers and Dainty (1988) to the multiwavelength EUV/Skylab observations of the solar atmosphere are presented. The application of the algorithm makes it possible to reach a resolution better than 5 arcsec, and thus study the structure of the quiet sun on that spatial scale. The results show evidence for discrete looplike structures in the network boundary, 5-10 arcsec in size, at temperatures of 100,000 K.

  1. Ultra-high resolution X-ray structures of two forms of human recombinant insulin at 100 K.

    Science.gov (United States)

    Lisgarten, David R; Palmer, Rex A; Lobley, Carina M C; Naylor, Claire E; Chowdhry, Babur Z; Al-Kurdi, Zakieh I; Badwan, Adnan A; Howlin, Brendan J; Gibbons, Nicholas C J; Saldanha, José W; Lisgarten, John N; Basak, Ajit K

    2017-08-01

    with the Insugen (I) structure. In the Intergen (II) structure there is no solvated propanol or acetate molecule. The electron density of Intergen (II), however, does also exhibit the three types of amino acid representations as in Insugen (I). These effects do not necessarily correspond between chains A and C or chains B and D in Intergen (II), or between corresponding residues in Insugen (I). The results of this comparison are reported. Graphical abstract Conformations of PheB25 and PheD25 in three insulin structures: implications for biological activity? Insulin residues PheB25 and PheD25 are considered to be important for insulin receptor binding and changes in biological activity occur when these residues are modified. In porcine insulin and Intergen (II) PheB25 adopts conformation B and PheD25 conformation D. However, unexpectedly PheB25 in Insugen (I) human recombinant insulin adopts two distinct conformations corresponding to B and D, Figure 1 and PheD25 adopts a single conformation corresponding to B not D, Figure 2. Conformations of this residue in the ultra-high resolution structure of Insugen (I) are therefore unique within this set. Figures were produced with Biovia, Discovery Studio 2016.

  2. GPCR engineering yields high-resolution structural insights into beta2-adrenergic receptor function

    DEFF Research Database (Denmark)

    Rosenbaum, Daniel M; Cherezov, Vadim; Hanson, Michael A

    2007-01-01

    The beta2-adrenergic receptor (beta2AR) is a well-studied prototype for heterotrimeric guanine nucleotide-binding protein (G protein)-coupled receptors (GPCRs) that respond to diffusible hormones and neurotransmitters. To overcome the structural flexibility of the beta2AR and to facilitate its cr...

  3. High-resolution structure of a retroviral protease folded as a monomer

    Czech Academy of Sciences Publication Activity Database

    Gilski, M.; Kazmierczyk, M.; Krzywda, S.; Zábranská, Helena; Cooper, S.; Popovic, Z.; Khatíb, F.; Dímaio, F.; Thompson, J.; Baker, D.; Pichová, Iva; Jaskolski, M.

    D67, č. 11 (2011), s. 907-914 ISSN 0907-4449 R&D Projects: GA MŠk 1M0508 Institutional research plan: CEZ:AV0Z40550506 Keywords : M-PMV protease * crystal structure * monomer * dimerization inhibitors Subject RIV: CE - Biochemistry Impact factor: 12.619, year: 2011

  4. High-resolution probing of inner core structure with seismic interferometry

    KAUST Repository

    Huang, Hsin-Hua; Lin, Fan-Chi; Tsai, Victor C.; Koper, Keith D.

    2015-01-01

    of the differential travel time residuals between the two phases reveals significant short-wavelength variation and implies the existence of strong structural variability in the deep Earth. A linear N-S trending anomaly across the middle of the U.S. may reflect

  5. High Resolution Ecosystem Structure, Biomass and Blue Carbon stocks in Mangrove Ecosystems- Methods and Applications of Lidar, radar Interferometry and High Resolution imagery

    Science.gov (United States)

    Lagomasino, D.; Fatoyinbo, T. E.; Lee, S. K.; Feliciano, E. A.; Simard, M.; Trettin, C.

    2016-12-01

    Earth's climate is determined by the exchange of radiant energy between the Sun, Earth and space. The absorbed solar radiation (ASR) fuels the climate system, providing the energy required for atmospheric and oceanic motions, while the system cools by emitting outgoing longwave (LW) radiation to space. A central objective of the Clouds and the Earth's Radiant Energy System (CERES) is to produce a long-term global climate data record of Earth's radiation budget along with the associated atmospheric and surface properties that influence it. CERES data products utilize a number of data sources, including broadband radiometers measuring incoming and reflected solar radiation and OLR, polar orbiting and geostationary spectral imagers, meteorological, aerosol and ozone assimilation data, and snow/sea-ice maps based on microwave radiometer data. Here we use simple diagnostic model of Earth's albedo and CERES Energy Balanced and Filled (EBAF) Ed4.0 data for March 2000-February 2016 to quantify interannual variations in SW TOA flux associated with surface albedo and atmospheric reflectance and transmittance variations. Surface albedo variations account for albedo and atmospheric reflectance/transmittance. Equatorward of 60-degree latitude, the atmospheric contribution exceeds that of the surface by at least an order-of-magnitude. In contrast, the surface and atmospheric variations contribute equally poleward of 60S and surface variations account for twice as much as the atmosphere poleward of 60N. However, as much as 40% of the total SW TOA flux variance poleward of 60N is explained by the covariance of surface albedo and atmospheric reflectance/transmittance, highlighting the tight coupling between sea-ice concentration and cloud properties over the Arctic Ocean.

  6. [Determination of hydroxyproline in liver tissue by hydrophilic interaction chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry].

    Science.gov (United States)

    Liu, Wei; Qi, Shenglan; Xu, Ying; Xiao, Zhun; Fu, Yadong; Chen, Jiamei; Yang, Tao; Liu, Ping

    2017-12-08

    A method for the determination of hydroxyproline (Hyp) in liver tissue of mice by hydrophilic interaction chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry (HILIC-HRMS) was developed. The liver tissue samples of normal mice and liver fibrosis mice induced by carbon tetrachloride were hydrolyzed by concentrated hydrochloric acid. After filtrated and diluted by solution, the diluent was separated on an Hypersil GOLD HILIC column (100 mm×2.1 mm, 3 μm). Water-acetonitrile (28:72, v/v)were used as the mobile phases with isocratic elution. Finally, the target analytes were detected in positive model by HRMS equipped with an electrospray ionization source. The linear range of hydroxyproline was from 0.78 to 100.00 μg/L with the correlation coefficient ( R 2 ) of 0.9983. The limit of quantification was 0.78 μg/L. By detecting the spiked samples, the recoveries were in the range of 97.4%-100.9% with the relative standard deviations (RSDs) between 1.4% and 2.0%. In addition, comparison of the measurement results by this method and the chloramine T method was proceeded. It was found that the linear correlation between the two methods was very good, and the Pearson correlation coefficient was 0.927. And this method had simpler operation procedure and higher accuracy than chloramine T method. This method can be used for the quick determination of hydroxyproline in liver tissue samples.

  7. Determination of 230Th/232Th and correct methods by High Resolution Inductively Coupled Plasma Mass Spectrometry

    International Nuclear Information System (INIS)

    Xie Shengkai; Guo Dongfa; Tan Jing; Zhang Yanhui; Huang Qiuhong; Gao Aiguo

    2013-01-01

    It is very important for the rapid and reliable determination of 230 Th/ 232 Th in the thorium-230 dating. A method of measuring 230 Th/ 232 Th in natural samples by high resolution inductively coupled plasma mass spectrometer (HR-ICP-MS) was developed on the base of our former work. The precise and accurate of natural 230 Th in geology samples is challenging, as the peak tailing to the high intensity of neighboring peak at 232 Th and the mass discrimination of the instrument. The peak tailing of 238 U to 236 U was used to decrease the peak tailing effect of 232 Th to 230 Th. The mass discrimination factor K between ture and measured isotope ratio was calculated after measuring different 230 Th/ 232 Th ratio solutions. Lab used standard samples was digested in mixed acids of HN0 3 -HF-HCI-HCl0 4 , and separated by the Bio-rad AG 1 × 8 Cl - resin. The measurement method of blank-standard-blank-sample procession was used to determinate the 230 Th/ 232 Th. The measured result of 230 Th/ 232 Th was at (7.29 ± 0.34) × 10 -6 , which agreed with the reference value of (7.33 ± 0.17) × 10 -6 . (authors)

  8. Determination of trace concentrations of chlorine in aqueous solutions by high-resolution continuum source graphite furnace molecular absorption spectrometry

    Science.gov (United States)

    Machyňák, Ľubomír; Čacho, František; Němeček, Martin; Beinrohr, Ernest

    2016-11-01

    Trace concentrations of total chlorine were determined by means of molecular absorption of indium mono-chloride (InCl) at 267.217 nm using high-resolution continuum source graphite furnace molecular absorption spectrometry. The effects of chemical modifiers and the amount of In on the sensitivity and accuracy were investigated. The optimum pyrolysis and vaporization temperatures were 600 °C and 1400 °C, respectively. The limit of detection and characteristic mass were found to be 0.10 ng and 0.21 ng, respectively. Potential non-spectral and spectral interferences were tested for various metals and non-metals at concentrations up to 50 mg L- 1 and for phosphoric, sulphuric and nitric acids. No spectral interferences were observed. Significant non-spectral interferences were observed with F, Br, and I at concentrations higher than 1 mg L- 1, 5 mg L- 1 and 25 mg L- 1, respectively, which is probably caused by formation of competitive indium halogen molecules. Higher concentrations of mineral acids depressed the signal owing to the formation of volatile HCl. The calibration curve was linear in the range between 0.3 and 10 ng with a correlation coefficient of R = 0.993. The elaborated method was used for the chlorine determination in various waters and a drug sample.

  9. High resolution, high sensitivity, dynamic distributed structural monitoring using optical frequency domain reflectometry

    Science.gov (United States)

    Kreger, Stephen T.; Sang, Alex K.; Garg, Naman; Michel, Julia

    2013-05-01

    Fiber-optic ultrasonic transducers are an important component of an active ultrasonic testing system for structural health monitoring. Fiber-optic transducers have several advantages such as small size, light weight, and immunity to electromagnetic interference that make them much more attractive than the current available piezoelectric transducers, especially as embedded and permanent transducers in active ultrasonic testing for structural health monitoring. In this paper, a distributed fiber-optic laser-ultrasound generation based on the ghost-mode of tilted fiber Bragg gratings is studied. The influences of the laser power and laser pulse duration on the laser-ultrasound generation are investigated. The results of this paper are helpful to understand the working principle of this laser-ultrasound method and improve the ultrasonic generation efficiency.

  10. Preservation of high resolution protein structure by cryo-electron microscopy of vitreous sections

    International Nuclear Information System (INIS)

    Sader, Kasim; Studer, Daniel; Zuber, Benoit; Gnaegi, Helmut; Trinick, John

    2009-01-01

    We have quantitated the degree of structural preservation in cryo-sections of a vitrified biological specimen. Previous studies have used sections of periodic specimens to assess the resolution present, but preservation before sectioning was not assessed and so the damage due particularly to cutting was not clear. In this study large single crystals of lysozyme were vitrified and from these X-ray diffraction patterns extending to better than 2.1 A were obtained. The crystals were high pressure frozen in 30% dextran, and cryo-sectioned using a diamond knife. In the best case, preservation to a resolution of 7.9 A was shown by electron diffraction, the first observation of sub-nanometre structural preservation in a vitreous section.

  11. High-resolution Crystal Structure of Dimeric VP40 From Sudan ebolavirus.

    Science.gov (United States)

    Clifton, Matthew C; Bruhn, Jessica F; Atkins, Kateri; Webb, Terry L; Baydo, Ruth O; Raymond, Amy; Lorimer, Donald D; Edwards, Thomas E; Myler, Peter J; Saphire, Erica Ollmann

    2015-10-01

    Ebolaviruses cause severe hemorrhagic fever. Central to the Ebola life cycle is the matrix protein VP40, which oligomerizes and drives viral budding. Here we present the crystal structure of the Sudan virus (SUDV) matrix protein. This structure is higher resolution (1.6 Å) than previously achievable. Despite differences in the protein purification, we find that it still forms a stable dimer in solution, as was noted for other Ebola VP40s. Although the N-terminal domain interface by which VP40 dimerizes is conserved between Ebola virus and SUDV, the C-terminal domain interface by which VP40 dimers may further assemble is significantly smaller in this SUDV assembly. © The Author 2015. Published by Oxford University Press on behalf of the Infectious Diseases Society of America. All rights reserved. For Permissions, please e-mail: journals.permissions@oup.com.

  12. HIGH RESOLUTION MICROTOMOGRAPHY FOR DENSITY AND SPATIAL INFORMATION ABOUT WOOD STRUCTURES.

    Energy Technology Data Exchange (ETDEWEB)

    ILLMAN,B.

    1999-07-22

    Microtomography has successfully been used to characterize loss of structural integrity of wood. Tomographic images were generated with the newly developed third generation x-ray computed microtomography (XCMT) instrument at the X27A beamline at the National Synchrotron Light Source (NSLS). The beamline is equipped with high-flux x-ray monochromator based on multilayer optics developed for this application. The sample is mounted on a translation stage with which to center the sample rotation, a rotation stage to perform the rotation during data collection and a motorized goniometer head for small alignment motions. The absorption image is recorded by a single-crystal scintillator, an optical microscope and a cooled CCD array detector. Data reconstruction has provided three-dimensional geometry of the heterogeneous wood matrix in microtomographic images. Wood is a heterogeneous material composed of long lignocellulose vessels. Although wood is a strong natural product, fungi have evolved chemical systems that weaken the strength properties of wood by degrading structural vessels. Tomographic images with a resolution of three microns were obtained nonintrusively to characterize the compromised structural integrity of wood. Computational tools developed by Lindquist et al (1996) applied to characterize the microstructure of the tomographic volumes.

  13. Understanding the structure of nanocatalysts with high resolution scanning/transmission electron microscopy

    International Nuclear Information System (INIS)

    Francis, L D; Rivas, J; José-Yacamán, M

    2014-01-01

    Nanomaterials including nanoparticles, nanowires and nanotubes play an important role in heterogeneous catalysis. Thanks to the rapid improvement of the electron microscopic techniques and with the advent of aberration corrected electron microscopy as well as theoretical methodologies, the potential effects induced by nanocatalysts are better understood than before by unravelling their atomic structure. A brief introduction to advanced electron microscopic techniques namely aberration corrected scanning transmission electron microscopy (Cs-STEM) is presented and subsequently two examples of nanocatalysts are considered in the present review. The first example will focus on the study of bimetallic/core-shell nanoalloys. In heterogeneous catalysis, catalysts containing two or more metals might show significantly different catalytic properties compared to the parent metals and thus are widely utilized in several catalytic reactions. Atom-by-atom insights of the nanoalloy based catalysts ex: Au-Pd will be described in the present review using a combination of advanced electron microscopic and spectroscopic techniques. A related example on the understanding of bimetallic clusters by HAADF-STEM will also be presented in addition to nanoparticles. In the second case understanding the structure of transition metal chalcogenide based nanocatalysts by HRTEM and aberration corrected STEM, for the case of MoS 2 will be discussed. MoS 2 -based catalysts serve as model catalysts and are employed in the hydrodesulphurisations (HDS) reactions in the removal of sulphur from gasoline and related petrochemical products. They have been studied in various forms including nanowires, nanotubes and nanoplates. Their structure, atomic insights and as a consequence elucidation of their corresponding catalytic activity are thus important

  14. High-resolution probing of inner core structure with seismic interferometry

    KAUST Repository

    Huang, Hsin-Hua

    2015-12-23

    © 2015. American Geophysical Union. All Rights Reserved. Increasing complexity of Earth\\'s inner core has been revealed in recent decades as the global distribution of seismic stations has improved. The uneven distribution of earthquakes, however, still causes a biased geographical sampling of the inner core. Recent developments in seismic interferometry, which allow for the retrieval of core-sensitive body waves propagating between two receivers, can significantly improve ray path coverage of the inner core. In this study, we apply such earthquake coda interferometry to 1846 USArray stations deployed across the U.S. from 2004 through 2013. Clear inner core phases PKIKP2 and PKIIKP2 are observed across the entire array. Spatial analysis of the differential travel time residuals between the two phases reveals significant short-wavelength variation and implies the existence of strong structural variability in the deep Earth. A linear N-S trending anomaly across the middle of the U.S. may reflect an asymmetric quasi-hemispherical structure deep within the inner core with boundaries of 99°W and 88°E.

  15. High-resolution structure of the antibiotic resistance protein NimA from Deinococcus radiodurans

    International Nuclear Information System (INIS)

    Leiros, Hanna-Kirsti S.; Tedesco, Consiglia; McSweeney, Seán M.

    2008-01-01

    In this paper, the 1.2 Å atomic resolution crystal structure of the 5-nitroimidazole antibiotic resistance protein NimA from Deinococcus radiodurans (DrNimA) is presented. Many anaerobic human pathogenic bacteria are treated using 5-nitroimidazole-based (5-Ni) antibiotics, a class of inactive prodrugs that contain a nitro group. The nitro group must be activated in an anaerobic one-electron reduction and is therefore dependent on the redox system in the target cells. Antibiotic resistance towards 5-Ni drugs is found to be related to the nim genes (nimA, nimB, nimC, nimD, nimE and nimF), which are proposed to encode a reductase that is responsible for converting the nitro group of the antibiotic into a nonbactericidal amine. A mechanism for the Nim enzyme has been proposed in which two-electron reduction of the nitro group leads to the generation of nontoxic derivatives and confers resistance against these antibiotics. The cofactor was found to be important in the mechanism and was found to be covalently linked to the reactive His71. In this paper, the 1.2 Å atomic resolution crystal structure of the 5-nitroimidazole antibiotic resistance protein NimA from Deinococcus radiodurans (DrNimA) is presented. A planar cofactor is clearly visible and well defined in the electron-density map adjacent to His71, the identification of the cofactor and its properties are discussed

  16. High-resolution x-ray spectroscopy of coherent bremsstrahlung fine structure

    International Nuclear Information System (INIS)

    Lund, M.W.

    1989-01-01

    The aim of this research was to provide experimental evidence for fine structure due to umklapp by distinct reciprocal lattice vectors in coherent bremsstrahlung spectra. The spontaneous emission of photons by relativistic electrons transversing thin crystals is made possible by recoil of the crystal, which absorbs momentum in multiples of ℎG where G is a reciprocal lattice vector. Previous work in the MeV-GeV beam energy range used detectors whose energy resolution was greater than 10%. By fitting a Johann wavelength dispersive spectrometer to a transmission electron microscope the author obtained coherent bremsstrahlung spectra of very high quality with energy resolution of 1%. Important to this result were also the fine angular collimation, small energy width of the electron beam in the microscope, and the accurate control of crystal orientation possible in a modern goniometer stage. The theory of the design of bent crystal x-ray spectrometers is extended to include effects of defocus and aberrations. The theory for diffraction from a stationary three dimensional grating due to a dipole radiator moving at relativistic speeds is derived as well as several other broadening mechanisms stemming from experimental variables. This dissertation provides the first experimental observations and corresponding theoretical background for the fine structure of coherent bremsstrahlung due to umklapp by different G-vectors in the same reciprocal lattice plane

  17. Fine structure of the isoscalar giant quadrupole resonance from high-resolution inelastic proton scattering experiments

    International Nuclear Information System (INIS)

    Shevchenko, A.

    2005-02-01

    In the present work the phenomenon of fine structure in the region of the isoscalar giant quadrupole resonance in a number of heavy and medium-heavy nuclei is systematically investigated for the first time. High energy-resolution inelastic proton scattering experiments were carried out in September-October 2001 and in October 2003 at the iThemba LABS cyclotron facility in South Africa with an incident proton energy of 200 MeV. The obtained data with the energy resolution of triangle E 58 Ni, 89 Y, 90 Zr, 120 Sn, 142 Nd, 166 Er, 208 Pb), thereby establishing the global character of this phenomenon. Fine structure can be described using characteristic energy scales, appearing as a result of the decay of collective modes towards the compound nucleus through a hierarchy of couplings to complex degrees of freedom. For the extraction of the characteristic energy scales from the spectra an entropy index method and a novel technique based on the wavelet analysis are utilized. The global analysis of available data shows the presence of three groups of scales, according to their values. To the first group belong the scales with the values around and below 100 keV, which were detected in all the nuclei studied. The second group contains intermediate scales in the range of 100 keV to 1 MeV. These scales show large variations depending on the nuclear structure of the nucleus. The largest scales above 1 MeV are classified to the third group, describing the global structure of the resonance (the width). The interpretation of the observed scales is realized via the comparison with microscopic model calculations including the coupling of the initial one-particle-one-hole excitations to more complex configurations. A qualitative agreement of the experimentally observed scales with those obtained from the theoretical predictions supports the suggestion of the origin of fine structure from the coupling to the two-particle-two-hole states. However, quantitatively, large deviations are

  18. High resolution 3-D shear wave velocity structure in South China from surface wave tomography

    Science.gov (United States)

    Ning, S.; Guo, Z.; Chen, Y. J.

    2017-12-01

    Using continuous data from a total of 638 seismic stations, including 484 from CEArray between 2008 and 2013 and 154 from SINOPROBE between 2014 and 2015, we perform both ambient noise and earthquake Rayleigh wave tomography across South China. Combining Rayleigh wave phase velocity between 6and 40s periods from ambient noise tomography and Rayleigh wave phase velocity between 20and 140s from teleseismic two-plane-wave tomography, we obtain phase velocity maps between 6 and140 s periods. We then invert Rayleigh wave phase velocity to construct a 3-D shear wave velocity structure of South China by Markov Chain Monte Carlo method. Similar to other inversion results, our results correspond topography well. Moreover, our results also reveal that velocity structure of the eastern South China in mantle depth is similar to eastern North China, the core of the western South China, Sichuan Block (SB),still exists thick lithosphere. However, owing to much more data employed and some data quality control techniques in this research, our results reveal more detailed structures. Along Qinling-Dabie Orogenic Belt (QDOB), North-South Gravity Lineament (NSGL) and the Sichuan-Yunnan Rhombic Block (SYRB), there are obvious high speed anomalies in depths of 10-20 km, which possibly imply ancient intrusions. Moreover, it seems that Tancheng-Lujiang Fault Zone (TLFZ) has already cut through QDOB, forming a deep fracture cutting through the crust of the whole China continent. Although SB still exists thick lithosphere, there are indications for thermal erosion. At the same time, the lithosphere of the central SYRB seems to be experiencing delamination process, obviously forming a barrier to prevent the hot Tibetan Plateau (TP) mantle material from flowing further southeast. Upwelling hot mantle material possibly triggered by this delamination process might be the cause of the Emeishan Large Igneous Province. There exists an intercontinental low velocity layer in the crust of the TP

  19. The determination of high-resolution spatio-temporal glacier motion fields from time-lapse sequences

    Science.gov (United States)

    Schwalbe, Ellen; Maas, Hans-Gerd

    2017-12-01

    This paper presents a comprehensive method for the determination of glacier surface motion vector fields at high spatial and temporal resolution. These vector fields can be derived from monocular terrestrial camera image sequences and are a valuable data source for glaciological analysis of the motion behaviour of glaciers. The measurement concepts for the acquisition of image sequences are presented, and an automated monoscopic image sequence processing chain is developed. Motion vector fields can be derived with high precision by applying automatic subpixel-accuracy image matching techniques on grey value patterns in the image sequences. Well-established matching techniques have been adapted to the special characteristics of the glacier data in order to achieve high reliability in automatic image sequence processing, including the handling of moving shadows as well as motion effects induced by small instabilities in the camera set-up. Suitable geo-referencing techniques were developed to transform image measurements into a reference coordinate system.The result of monoscopic image sequence analysis is a dense raster of glacier surface point trajectories for each image sequence. Each translation vector component in these trajectories can be determined with an accuracy of a few centimetres for points at a distance of several kilometres from the camera. Extensive practical validation experiments have shown that motion vector and trajectory fields derived from monocular image sequences can be used for the determination of high-resolution velocity fields of glaciers, including the analysis of tidal effects on glacier movement, the investigation of a glacier's motion behaviour during calving events, the determination of the position and migration of the grounding line and the detection of subglacial channels during glacier lake outburst floods.

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

    International Nuclear Information System (INIS)

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

    2004-01-01

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

  1. Kotai Antibody Builder: automated high-resolution structural modeling of antibodies.

    Science.gov (United States)

    Yamashita, Kazuo; Ikeda, Kazuyoshi; Amada, Karlou; Liang, Shide; Tsuchiya, Yuko; Nakamura, Haruki; Shirai, Hiroki; Standley, Daron M

    2014-11-15

    Kotai Antibody Builder is a Web service for tertiary structural modeling of antibody variable regions. It consists of three main steps: hybrid template selection by sequence alignment and canonical rules, 3D rendering of alignments and CDR-H3 loop modeling. For the last step, in addition to rule-based heuristics used to build the initial model, a refinement option is available that uses fragment assembly followed by knowledge-based scoring. Using targets from the Second Antibody Modeling Assessment, we demonstrate that Kotai Antibody Builder generates models with an overall accuracy equal to that of the best-performing semi-automated predictors using expert knowledge. Kotai Antibody Builder is available at http://kotaiab.org standley@ifrec.osaka-u.ac.jp. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please e-mail: journals.permissions@oup.com.

  2. The braingraph.org database of high resolution structural connectomes and the brain graph tools.

    Science.gov (United States)

    Kerepesi, Csaba; Szalkai, Balázs; Varga, Bálint; Grolmusz, Vince

    2017-10-01

    Based on the data of the NIH-funded Human Connectome Project, we have computed structural connectomes of 426 human subjects in five different resolutions of 83, 129, 234, 463 and 1015 nodes and several edge weights. The graphs are given in anatomically annotated GraphML format that facilitates better further processing and visualization. For 96 subjects, the anatomically classified sub-graphs can also be accessed, formed from the vertices corresponding to distinct lobes or even smaller regions of interests of the brain. For example, one can easily download and study the connectomes, restricted to the frontal lobes or just to the left precuneus of 96 subjects using the data. Partially directed connectomes of 423 subjects are also available for download. We also present a GitHub-deposited set of tools, called the Brain Graph Tools, for several processing tasks of the connectomes on the site http://braingraph.org.

  3. Determination of total sulfur in agricultural samples by high-resolution continuum source flame molecular absorption spectrometry.

    Science.gov (United States)

    Virgilio, Alex; Raposo, Jorge L; Cardoso, Arnaldo A; Nóbrega, Joaquim A; Gomes Neto, José A

    2011-03-23

    The usefulness of molecular absorption was investigated for the determination of total sulfur (S) in agricultural samples by high-resolution continuum source flame molecular absorption spectrometry. The lines for CS at 257.595, 257.958, and 258.056 nm and for SH at 323.658, 324.064, and 327.990 nm were evaluated. Figures of merit, such as linear dynamic range, sensitivity, linear correlation, characteristic concentration, limit of detection, and precision, were established. For selected CS lines, wavelength-integrated absorbance equivalent to 3 pixels, analytical curves in the 100-2500 mg L(-1) (257.595 nm), 250-2000 mg L(-1) (257.958 nm), and 250-5000 mg L(-1) (258.056 nm) ranges with a linear correlation coefficient better than 0.9980 were obtained. Results were in agreement at a 95% confidence level (paired t test) with those obtained by gravimetry. Recoveries of S in fungicide and fertilizer samples were within the 84-109% range, and the relative standard deviation (n=12) was typically <5%.

  4. Determination of boron isotope ratios by high-resolution continuum source molecular absorption spectrometry using graphite furnace vaporizers

    Science.gov (United States)

    Abad, Carlos; Florek, Stefan; Becker-Ross, Helmut; Huang, Mao-Dong; Heinrich, Hans-Joachim; Recknagel, Sebastian; Vogl, Jochen; Jakubowski, Norbert; Panne, Ulrich

    2017-10-01

    Boron isotope amount ratios n(10B)/n(11B) have been determined by monitoring the absorption spectrum of boron monohydride (BH) in a graphite furnace using high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS). Bands (0 → 0) and (1 → 1) for the electronic transition X1Σ+ → A1Π were evaluated around wavelengths 433.1 nm and 437.1 nm respectively. Clean and free of memory effect molecular spectra of BH were recorded. In order to eliminate the memory effect of boron, a combination of 2% (v/v) hydrogen gas in argon and 1% trifluoromethane in argon, an acid solution of calcium chloride and mannitol as chemical modifiers was used. Partial least square regression (PLS) for analysis of samples and reference materials were applied. For this, a spectral library with different isotopes ratios for PLS regression was built. Results obtained around the 433.1 nm and 437.1 nm spectral regions are metrologically compatible with those reported by mass spectrometric methods. Moreover, for the evaluated region of 437 nm, an accuracy of 0.15‰ is obtained as the average deviation from the isotope reference materials. Expanded uncertainties with a coverage factor of k = 2 range between 0.15 and 0.44‰. This accuracy and precision are compatible with those obtained by mass spectrometry for boron isotope ratio measurements.

  5. The determination of polycyclic aromatic hydrocarbons in human urine by high-resolution gas chromatography-mass spectrometry.

    Science.gov (United States)

    Cho, Sung-Hee; Lee, Sun-Kyung; Kim, Chong Hyeak

    2018-05-01

    Polycyclic aromatic hydrocarbons (PAHs), organic compounds formed by at least two condensed aromatic rings, are ubiquitous environmental pollutants that are produced by incomplete combustion of organic materials. PAHs have been classified as carcinogenIC to humans by the International Agency for Research on Cancer, because they can bind to DNA, causing mutations. Therefore, the levels of PAHs in human urine can be used as an indicator for potential carcinogenesis and cell mutation. An analytical method was developed for the accurate measurement of PAHs in urine using high-resolution gas chromatography-mass spectrometry. Urine samples were extracted by an Oasis HLB extraction cartridge after enzymatic hydrolysis with a β-glucuronidase/arylsulfatase cocktail. The 18 PAHs were separated using an Agilent DB-5 MS capillary column (30 m × 0.25 mm, 0.25 μm) and monitored by time-of-flight mass spectrometry. Under the optimized method, the linearity of calibration curves was >0.994. The limits of detection at a signal-to-noise ratio of 3 were 10-100 ng/L. The coefficients of variation were in the range of 0.4-9.0%. The present method was highly accurate for simultaneous determination of 18 PAHs in human urine and could be applied to monitoring and biomedical investigations to check exposure of PAHs. Copyright © 2017 John Wiley & Sons, Ltd.

  6. A high-resolution study of mesospheric fine structure with the Jicamarca MST radar

    Directory of Open Access Journals (Sweden)

    R. Sheth

    2006-07-01

    Full Text Available Correlation studies performed on data from recent mesospheric experiments conducted with the 50-MHz Jicamarca radar in May 2003 and July 2004 are reported. The study is based on signals detected from a combination of vertical and off-vertical beams. The nominal height resolution was 150 m and spectral estimates were obtained after ~1 min integration. Spectral widths and backscattered power generally show positive correlations at upper mesospheric heights in agreement with earlier findings (e.g., Fukao et al., 1980 that upper mesospheric echoes are dominated by isotropic Bragg scatter. In many instances in the upper mesosphere, a weakening of positive correlation away from layer centers (towards top and bottom boundaries was observed with the aid of improved height resolution. This finding supports the idea that layer edges are dominated by anisotropic turbulence. The data also suggests that negative correlations observed at lower mesospheric heights are caused by scattering from anisotropic structures rather than reflections from sharp vertical gradients in electron density.

  7. Ultra-high resolution four dimensional geodetic imaging of engineered structures for stability assessment

    Science.gov (United States)

    Bawden, Gerald W.; Bond, Sandra; Podoski, J. H.; Kreylos, O.; Kellogg, L. H.

    2012-01-01

    We used ground-based Tripod LiDAR (T-LiDAR) to assess the stability of two engineered structures: a bridge spanning the San Andreas fault following the M6.0 Parkfield earthquake in Central California and a newly built coastal breakwater located at the Kaumālapa`u Harbor Lana'i, Hawaii. In the 10 weeks following the earthquake, we found that the surface under the bridge shifted 7.1 cm with an additional 2.6 cm of motion in the subsequent 13 weeks, which deflected the bridge's northern I-beam support 4.3 cm and 2.1 respectively; the bridge integrity remained intact. T-LiDAR imagery was collected after the completion of armored breakwater with 817 35-ton interlocking concrete armor units, Core-Locs®, in the summers of 2007, 2008 and 2010. We found a wide range of motion of individual Core-Locs, from a few centimeters to >110 cm along the ocean side of the breakwater, with lesser movement along the harbor side.

  8. A high-resolution study of mesospheric fine structure with the Jicamarca MST radar

    Science.gov (United States)

    Sheth, R.; Kudeki, E.; Lehmacher, G.; Sarango, M.; Woodman, R.; Chau, J.; Guo, L.; Reyes, P.

    2006-07-01

    Correlation studies performed on data from recent mesospheric experiments conducted with the 50-MHz Jicamarca radar in May 2003 and July 2004 are reported. The study is based on signals detected from a combination of vertical and off-vertical beams. The nominal height resolution was 150 m and spectral estimates were obtained after ~1 min integration. Spectral widths and backscattered power generally show positive correlations at upper mesospheric heights in agreement with earlier findings (e.g., Fukao et al., 1980) that upper mesospheric echoes are dominated by isotropic Bragg scatter. In many instances in the upper mesosphere, a weakening of positive correlation away from layer centers (towards top and bottom boundaries) was observed with the aid of improved height resolution. This finding supports the idea that layer edges are dominated by anisotropic turbulence. The data also suggests that negative correlations observed at lower mesospheric heights are caused by scattering from anisotropic structures rather than reflections from sharp vertical gradients in electron density.

  9. High resolution structuring of emitter tips for the gaseous field ionization source

    International Nuclear Information System (INIS)

    Kubby, J.A.; Siegel, B.M.

    1986-01-01

    Extraction of a stable, high brightness ion beam from an apertured field ion emitter surface requires microfabrication procedures to sculpture the surface topography on both microscopic (100 --1000 nm) and near atomic (10 --100 nm) length scales. Structuring on a near atomic scale is required to confine and stabilize the ion beam by local enhancement of the surface electrostatic field and to orient that emission on the optical axis. Control of the emitter contour on a microscopic scale is required for manipulating the supply of neutral molecules to the ionization site and also affects beam stability. We have developed a method using ion milling for configuring surface contour on microscopic and near atomic length scales which utilizes the morphological changes occurring at ion bombarded surfaces as a result of erosion by sputtering. A SEM study of the microscopic emitter topographical development is compared to computer simulations of the kinematical wave equation which depicts the erosion process. In this way, prediction of configuration on a length scale large compared to the ion penetration depth has been established. TEM observations show the surface development on the length scale of ion penetration depth. Preliminary results using this microfabricated emitter in a gaseous field ion source to produce a hydrogen ion beam with high angular beam confinement are given. Requirements for surface topography that are essential to obtain stable high brightness ion beams are discussed

  10. Structural characterization and gas reactions of small metal particles by high-resolution TEM and TED

    Science.gov (United States)

    Heinemann, K.

    1985-01-01

    The interaction of 100 and 200 keV electron beams with amorphous alumina, titania, and aluminum nitride substrates and nanometer-size palladium particulate deposits was investigated for the two extreme cases of (1) large-area electron-beam flash-heating and (2) small-area high-intensity electron-beam irradiation. The former simulates a short-term heating effect with minimum electron irradiation exposure, the latter simulates high-dosage irradiation with minimum heating effect. All alumina and titania samples responded to the flash-heating treatment with significant recrystallization. However, the size, crystal structure, shape, and orientation of the grains depended on the type and thickness of the films and the thickness of the Pd deposit. High-dosage electron irradiation also readily crystallized the alumina substrate films but did not affect the titania films. The alumina recrystallization products were usually either all in the alpha phase, or they were a mixture of small grains in a number of low-temperature phases including gamma, delta, kappa, beta, theta-alumina. Palladium deposits reacted heavily with the alumina substrates during either treatment, but they were very little effected when supported on titania. Both treatments had the same, less prominent localized crystallization effect on aluminum nitride films.

  11. High resolution CSMT method for shallow structure; Senjo ochi ni okeru kobunkaino denjiho tansa

    Energy Technology Data Exchange (ETDEWEB)

    Yamane, K; Takasugi, S [GERD Geothermal Energy Research and Development Co. Ltd., Tokyo (Japan); Inazaki, S [Geological Survey of Japan, Tsukuba (Japan); Sasaki, Y

    1997-10-22

    Electromagnetic exploration methods and seismic reflection methods are conducted for the study of applicability of geophysical exploration to shallow layer geological survey. In the study, four north-south traverse lines are set in 400mtimes200m grassland. Tensor type CSMT methods are employed, a CSMT method using 96kHz-1kHz artificial magnetic fields and an MT method using 1kHz-10kHz natural magnetic fields, for the determination of resistivity distribution in the ground. Distributed in the site are a surface layer composed of gravel-containing sand and silt, andesitic fractured lava, and massive andesite, and the exploration reaches several tens of meters below the surface. The results of CSMT measurements are found to be in agreement with reflection profiles acquired simultaneously with these CSMT measurements. It is found, furthermore, that CSMT profiles help identify reflection waveforms in a domain where reflection is obscure. It is also found that electromagnetic methods are effective in fault logging because they are very sensitive to porosity, or the amount of pore water, which is higher in a domain with subsurface cracks than in the neighborhood without cracks. 1 ref., 4 figs.

  12. Joint inversion of high resolution S-wave velocity structure underneath North China Basin

    Science.gov (United States)

    Yang, C.; Li, G.; Niu, F.

    2017-12-01

    North China basin is one of earthquake prone areas in China. Many devastating earthquakes occurred in the last century and before, such as the 1937 M7.0 Heze Earthquake in Shandong province, the 1966 M7.2 Xingtai Earthquake and 1976 Tangshan Earthquake in Hebei province. Knowing the structure of the sediment cover is of great importance to predict strong ground motion caused by earthquakes. Unconsolidated sediments are loose materials, ranging from clay to sand to gravel. Earthquakes can liquefy unconsolidated sediments, thus knowing the distribution and thickness of the unconsolidated sediments has significant implication in seismic hazard analysis of the area. Quantitative estimates of the amount of extension of the North China basin is important to understand the thinning and evolution of the eastern North China craton and the underlying mechanism. In principle, the amount of lithospheric stretching can be estimated from sediment and crustal thickness. Therefore an accurate estimate of the sediment and crustal thickness of the area is also important in understanding regional tectonics. In this study, we jointly invert the Rayleigh wave phase-velocity dispersion and Z/H ratio data to construct a 3-D S-wave velocity model beneath North China area. We use 4-year ambient noise data recorded from 249 temporary stations, and 139 earthquake events to extract Rayleigh wave Z/H ratios. The Z/H ratios obtained from ambient noise data and earthquake data show a good agreement within the overlapped periods. The phase velocity dispersion curve was estimated from the same ambient noise data. The preliminary result shows a relatively low Z/H ratio and low velocity anomaly at the shallow part of sediment basins.

  13. Parallel computation of fluid-structural interactions using high resolution upwind schemes

    Science.gov (United States)

    Hu, Zongjun

    An efficient and accurate solver is developed to simulate the non-linear fluid-structural interactions in turbomachinery flutter flows. A new low diffusion E-CUSP scheme, Zha CUSP scheme, is developed to improve the efficiency and accuracy of the inviscid flux computation. The 3D unsteady Navier-Stokes equations with the Baldwin-Lomax turbulence model are solved using the finite volume method with the dual-time stepping scheme. The linearized equations are solved with Gauss-Seidel line iterations. The parallel computation is implemented using MPI protocol. The solver is validated with 2D cases for its turbulence modeling, parallel computation and unsteady calculation. The Zha CUSP scheme is validated with 2D cases, including a supersonic flat plate boundary layer, a transonic converging-diverging nozzle and a transonic inlet diffuser. The Zha CUSP2 scheme is tested with 3D cases, including a circular-to-rectangular nozzle, a subsonic compressor cascade and a transonic channel. The Zha CUSP schemes are proved to be accurate, robust and efficient in these tests. The steady and unsteady separation flows in a 3D stationary cascade under high incidence and three inlet Mach numbers are calculated to study the steady state separation flow patterns and their unsteady oscillation characteristics. The leading edge vortex shedding is the mechanism behind the unsteady characteristics of the high incidence separated flows. The separation flow characteristics is affected by the inlet Mach number. The blade aeroelasticity of a linear cascade with forced oscillating blades is studied using parallel computation. A simplified two-passage cascade with periodic boundary condition is first calculated under a medium frequency and a low incidence. The full scale cascade with 9 blades and two end walls is then studied more extensively under three oscillation frequencies and two incidence angles. The end wall influence and the blade stability are studied and compared under different

  14. Coupling physics and biogeochemistry thanks to high-resolution observations of the phytoplankton community structure in the northwestern Mediterranean Sea

    Science.gov (United States)

    Marrec, Pierre; Grégori, Gérald; Doglioli, Andrea M.; Dugenne, Mathilde; Della Penna, Alice; Bhairy, Nagib; Cariou, Thierry; Hélias Nunige, Sandra; Lahbib, Soumaya; Rougier, Gilles; Wagener, Thibaut; Thyssen, Melilotus

    2018-03-01

    Fine-scale physical structures and ocean dynamics strongly influence and regulate biogeochemical and ecological processes. These processes are particularly challenging to describe and understand because of their ephemeral nature. The OSCAHR (Observing Submesoscale Coupling At High Resolution) campaign was conducted in fall 2015 in which a fine-scale structure (1-10 km/1-10 days) in the northwestern Mediterranean Ligurian subbasin was pre-identified using both satellite and numerical modeling data. Along the ship track, various variables were measured at the surface (temperature, salinity, chlorophyll a and nutrient concentrations) with ADCP current velocity. We also deployed a new model of the CytoSense automated flow cytometer (AFCM) optimized for small and dim cells, for near real-time characterization of the surface phytoplankton community structure of surface waters with a spatial resolution of a few kilometers and an hourly temporal resolution. For the first time with this optimized version of the AFCM, we were able to fully resolve Prochlorococcus picocyanobacteria in addition to the easily distinguishable Synechococcus. The vertical physical dynamics and biogeochemical properties of the studied area were investigated by continuous high-resolution CTD profiles thanks to a moving vessel profiler (MVP) during the vessel underway associated with a high-resolution pumping system deployed during fixed stations allowing sampling of the water column at a fine resolution (below 1 m). The observed fine-scale feature presented a cyclonic structure with a relatively cold core surrounded by warmer waters. Surface waters were totally depleted in nitrate and phosphate. In addition to the doming of the isopycnals by the cyclonic circulation, an intense wind event induced Ekman pumping. The upwelled subsurface cold nutrient-rich water fertilized surface waters and was marked by an increase in Chl a concentration. Prochlorococcus and pico- and nano-eukaryotes were more

  15. Coupling physics and biogeochemistry thanks to high-resolution observations of the phytoplankton community structure in the northwestern Mediterranean Sea

    Directory of Open Access Journals (Sweden)

    P. Marrec

    2018-03-01

    Full Text Available Fine-scale physical structures and ocean dynamics strongly influence and regulate biogeochemical and ecological processes. These processes are particularly challenging to describe and understand because of their ephemeral nature. The OSCAHR (Observing Submesoscale Coupling At High Resolution campaign was conducted in fall 2015 in which a fine-scale structure (1–10 km∕1–10 days in the northwestern Mediterranean Ligurian subbasin was pre-identified using both satellite and numerical modeling data. Along the ship track, various variables were measured at the surface (temperature, salinity, chlorophyll a and nutrient concentrations with ADCP current velocity. We also deployed a new model of the CytoSense automated flow cytometer (AFCM optimized for small and dim cells, for near real-time characterization of the surface phytoplankton community structure of surface waters with a spatial resolution of a few kilometers and an hourly temporal resolution. For the first time with this optimized version of the AFCM, we were able to fully resolve Prochlorococcus picocyanobacteria in addition to the easily distinguishable Synechococcus. The vertical physical dynamics and biogeochemical properties of the studied area were investigated by continuous high-resolution CTD profiles thanks to a moving vessel profiler (MVP during the vessel underway associated with a high-resolution pumping system deployed during fixed stations allowing sampling of the water column at a fine resolution (below 1 m. The observed fine-scale feature presented a cyclonic structure with a relatively cold core surrounded by warmer waters. Surface waters were totally depleted in nitrate and phosphate. In addition to the doming of the isopycnals by the cyclonic circulation, an intense wind event induced Ekman pumping. The upwelled subsurface cold nutrient-rich water fertilized surface waters and was marked by an increase in Chl a concentration. Prochlorococcus and pico

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

    International Nuclear Information System (INIS)

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

    1993-01-01

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

  17. High-resolution structural characterization and magnetic properties of epitaxial Ce-doped yttrium iron garnet thin films

    Science.gov (United States)

    Li, Zhong; Vikram Singh, Amit; Rastogi, Ankur; Gazquez, Jaume; Borisevich, Albina Y.; Mishra, Rohan; Gupta, Arunava

    2017-07-01

    Thin films of magnetic garnet materials, e.g. yttrium iron garnet (Y3Fe5O12, YIG), are useful for a variety of applications including microwave integrated circuits and spintronics. Substitution of rare earth ions, such as cerium, is known to enhance the magneto-optic Kerr effect (MOKE) as compared to pure YIG. Thin films of Ce0.75Y2.25Fe5O12 (Ce:YIG) have been grown using the pulsed laser deposition (PLD) technique and their crystal structure examined using high resolution scanning transmission electron microscopy. Homogeneous substitution of Ce in YIG, without oxidation to form a separate CeO2 phase, can be realized in a narrow process window with resulting enhancement of the MOKE signal. The thermally generated signal due to spin Seebeck effect for the optimally doped Ce:YIG films has also been investigated.

  18. Structural evolution of a deformed Σ=9 (122) grain boundary in silicon. A high resolution electron microscopy study

    International Nuclear Information System (INIS)

    Putaux, Jean-Luc

    1991-01-01

    This research thesis addresses the study by high resolution electron microscopy of the evolution of a silicon bi-crystal under deformation at different temperatures. The author notably studied the structural evolution of the boundary as well as that of grains at the vicinity of the boundary. Two observation scales have been used: the evolution of sub-structures of dislocations induced by deformation in grains and in boundary, and the structure of all defects at an atomic scale. After a presentation of experimental tools (the necessary perfect quality of the electronic optics is outlined), the author recalls some descriptive aspects of grain boundaries (geometric network concepts to describe coinciding networks, concepts of delimiting boundaries and of structural unit to describe grain boundary atomic structure), recalls the characteristics of the studied bi-crystal, and the conditions under which it is deformed. He presents the structures of all perfectly coinciding boundaries, describes defects obtained by deformation at the vicinity of the boundary, describes the entry of dissociated dislocations into the boundaries, and discusses the characterization of boundary dislocations (the notion of Burgers vector is put into question again), and the atomic mechanism of displacement of dislocations in boundaries [fr

  19. Determination of silicon in biomass and products of pyrolysis process via high-resolution continuum source atomic absorption spectrometry.

    Science.gov (United States)

    Nakadi, Flávio V; Prodanov, Caroline; Boschetti, Wiliam; Vale, Maria Goreti R; Welz, Bernhard; de Andrade, Jailson B

    2018-03-01

    Thermochemical processes can convert the biomass into fuels, such as bio-oil. The biomass submitted to pyrolysis process, such as fibers, are generally rich in silicon, an element that can lead to damages in an engine when there is high concentration in a fuel. High-resolution continuum source atomic absorption spectrometry (HR-CS AAS) is an interesting alternative for Si determination in the products and byproducts of the pyrolysis process because, besides the flame (F) and graphite furnace (GF) atomizers, it has enhanced the application of direct analysis of solid samples (SS) within GF. This study aimed the development of methods to determine Si in biomass samples, their products and byproducts using HR-CS AAS. A high-resolution continuum source atomic absorption spectrometer contrAA 700 equipped with F and GF atomizers was used throughout the study. HR-CS F AAS (λ = 251.611nm, 1 detection pixel, N 2 O/C 2 H 2 flame) was used to evaluate Si content in biomass and ash, after a microwave-assisted acid digestion with HNO 3 and HF. HR-CS GF AAS (T pyr = 1400°C, T atom = 2650°C) has evaluated Si in pyrolysis water and bio-oil at 251.611nm, and in peach pit biomass and ash at 221.174nm using SS, both wavelengths with 1 detection pixel. Rhodium (300μg) was applied as permanent modifier and 10μgPd + 6μg Mg were pipetted onto the standards/samples at each analysis. Three different biomass samples were studied: palm tree fiber, coconut fiber and peach pit, and three certified reference materials (CRM) were used to verify the accuracy of the methods. The figures of merit were LOD 0.09-20mgkg -1 , and LOQ 0.3-20mgkg -1 , considering all the methods. There were no significant differences between the CRM certified values and the determined ones, using a Student t-test with a confidence interval of 95% (n = 5). Si concentration ranged from 0.11-0.92% mm -1 , 1.1-1.7mgkg -1 , 3.3-13mgkg -1 , and 0.41-1.4%mm -1 , in biomass, bio-oil, pyrolysis water and ash, respectively

  20. Feasibility of high-resolution continuum source molecular absorption spectrometry in flame and furnace for sulphur determination in petroleum products

    Science.gov (United States)

    Kowalewska, Zofia

    2011-07-01

    For the first time, high-resolution molecular absorption spectrometry with a high-intensity xenon lamp as radiation source has been applied for the determination of sulphur in crude oil and petroleum products. The samples were analysed as xylene solutions using vaporisation in acetylene-air flame or in an electrothermally heated graphite furnace. The sensitive rotational lines of the CS molecule, belonging to the ∆ν = 0 vibrational sequence within the electronic transition X 1∑ + → A 1П, were applied. For graphite furnace molecular absorption spectrometry, the Pd + Mg organic modifier was selected. Strong interactions with Pd atoms enable easier decomposition of sulphur-containing compounds, likely through the temporal formation of Pd xS y molecules. At the 258.056 nm line, with the wavelength range covering central pixel ± 5 pixels and with application of interactive background correction, the detection limit was 14 ng in graphite furnace molecular absorption spectrometry and 18 mg kg -1 in flame molecular absorption spectrometry. Meanwhile, application of 2-points background correction found a characteristic mass of 12 ng in graphite furnace molecular absorption spectrometry and a characteristic concentration of 104 mg kg -1 in flame molecular absorption spectrometry. The range of application of the proposed methods turned out to be significantly limited by the properties of the sulphur compounds of interest. In the case of volatile sulphur compounds, which can be present in light petroleum products, severe difficulties were encountered. On the contrary, heavy oils and residues from distillation as well as crude oil could be analysed using both flame and graphite furnace vaporisation. The good accuracy of the proposed methods for these samples was confirmed by their mutual consistency and the results from analysis of reference samples (certified reference materials and home reference materials with sulphur content determined by X-ray fluorescence

  1. Feasibility of high-resolution continuum source molecular absorption spectrometry in flame and furnace for sulphur determination in petroleum products

    Energy Technology Data Exchange (ETDEWEB)

    Kowalewska, Zofia, E-mail: zofia.kowalewska@obr.pl

    2011-07-15

    For the first time, high-resolution molecular absorption spectrometry with a high-intensity xenon lamp as radiation source has been applied for the determination of sulphur in crude oil and petroleum products. The samples were analysed as xylene solutions using vaporisation in acetylene-air flame or in an electrothermally heated graphite furnace. The sensitive rotational lines of the CS molecule, belonging to the {Delta}{nu} = 0 vibrational sequence within the electronic transition X{sup 1}{Sigma}{sup +} {yields} A{sup 1}{Pi}, were applied. For graphite furnace molecular absorption spectrometry, the Pd + Mg organic modifier was selected. Strong interactions with Pd atoms enable easier decomposition of sulphur-containing compounds, likely through the temporal formation of Pd{sub x}S{sub y} molecules. At the 258.056 nm line, with the wavelength range covering central pixel {+-} 5 pixels and with application of interactive background correction, the detection limit was 14 ng in graphite furnace molecular absorption spectrometry and 18 mg kg{sup -1} in flame molecular absorption spectrometry. Meanwhile, application of 2-points background correction found a characteristic mass of 12 ng in graphite furnace molecular absorption spectrometry and a characteristic concentration of 104 mg kg{sup -1} in flame molecular absorption spectrometry. The range of application of the proposed methods turned out to be significantly limited by the properties of the sulphur compounds of interest. In the case of volatile sulphur compounds, which can be present in light petroleum products, severe difficulties were encountered. On the contrary, heavy oils and residues from distillation as well as crude oil could be analysed using both flame and graphite furnace vaporisation. The good accuracy of the proposed methods for these samples was confirmed by their mutual consistency and the results from analysis of reference samples (certified reference materials and home reference materials with

  2. Determination of silicon and aluminum in silicon carbide nanocrystals by high-resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Dravecz, Gabriella; Bencs, László; Beke, Dávid; Gali, Adam

    2016-01-15

    The determination of Al contaminant and the main component Si in silicon carbide (SiC) nanocrystals with the size-distribution of 1-8nm dispersed in an aqueous solution was developed using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS-GFAAS). The vaporization/atomization processes were investigated in a transversally heated graphite atomizer by evaporating solution samples of Al and Si preserved in various media (HCl, HNO3). For Si, the best results were obtained by applying a mixture of 5µg Pd plus 5µg Mg, whereas for Al, 10µg Mg (each as nitrate solution) was dispensed with the samples, but the results obtained without modifier were found to be better. This way a maximum pyrolysis temperature of 1200°C for Si and 1300°C for Al could be used, and the optimum (compromise) atomization temperature was 2400°C for both analytes. The Si and Al contents of different sized SiC nanocrystals, dispersed in aqueous solutions, were determined against aqueous (external) calibration standards. The correlation coefficients (R values) of the calibrations were found to be 0.9963 for Si and 0.9991 for Al. The upper limit of the linear calibration range was 2mg/l Si and 0.25mg/l Al. The limit of detection was 3µg/l for Si and 0.5µg/l for Al. The characteristic mass (m0) was calculated to be 389pg Si and 6.4pg Al. The Si and Al content in the solution samples were found to be in the range of 1.0-1.7mg/l and 0.1-0.25mg/l, respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Conformational flexibility in the catalytic triad revealed by the high-resolution crystal structure of Streptomyces erythraeus trypsin in an unliganded state

    Energy Technology Data Exchange (ETDEWEB)

    Blankenship, Elise; Vukoti, Krishna [Case Western Reserve University, 10900 Euclid Avenue, Cleveland, OH 44106 (United States); Miyagi, Masaru, E-mail: mxm356@cwru.edu [Case Western Reserve University, 10900 Euclid Avenue, Cleveland, OH 44106 (United States); Case Western Reserve University, 10900 Euclid Avenue, Cleveland, OH 44106 (United States); Case Western Reserve University, 10900 Euclid Avenue, Cleveland, OH 44106 (United States); Lodowski, David T., E-mail: mxm356@cwru.edu [Case Western Reserve University, 10900 Euclid Avenue, Cleveland, OH 44106 (United States); Case Western Reserve University, 10900 Euclid Avenue, Cleveland, OH 44106 (United States)

    2014-03-01

    This work reports the first sub-angstrom resolution structure of S. erythraeus trypsin. The detailed model of a prototypical serine protease at a catalytically relevant pH with an unoccupied active site is presented and is compared with other high-resolution serine protease structures. With more than 500 crystal structures determined, serine proteases make up greater than one-third of all proteases structurally examined to date, making them among the best biochemically and structurally characterized enzymes. Despite the numerous crystallographic and biochemical studies of trypsin and related serine proteases, there are still considerable shortcomings in the understanding of their catalytic mechanism. Streptomyces erythraeus trypsin (SET) does not exhibit autolysis and crystallizes readily at physiological pH; hence, it is well suited for structural studies aimed at extending the understanding of the catalytic mechanism of serine proteases. While X-ray crystallographic structures of this enzyme have been reported, no coordinates have ever been made available in the Protein Data Bank. Based on this, and observations on the extreme stability and unique properties of this particular trypsin, it was decided to crystallize it and determine its structure. Here, the first sub-angstrom resolution structure of an unmodified, unliganded trypsin crystallized at physiological pH is reported. Detailed structural analysis reveals the geometry and structural rigidity of the catalytic triad in the unoccupied active site and comparison to related serine proteases provides a context for interpretation of biochemical studies of catalytic mechanism and activity.

  4. Conformational flexibility in the catalytic triad revealed by the high-resolution crystal structure of Streptomyces erythraeus trypsin in an unliganded state

    International Nuclear Information System (INIS)

    Blankenship, Elise; Vukoti, Krishna; Miyagi, Masaru; Lodowski, David T.

    2014-01-01

    This work reports the first sub-angstrom resolution structure of S. erythraeus trypsin. The detailed model of a prototypical serine protease at a catalytically relevant pH with an unoccupied active site is presented and is compared with other high-resolution serine protease structures. With more than 500 crystal structures determined, serine proteases make up greater than one-third of all proteases structurally examined to date, making them among the best biochemically and structurally characterized enzymes. Despite the numerous crystallographic and biochemical studies of trypsin and related serine proteases, there are still considerable shortcomings in the understanding of their catalytic mechanism. Streptomyces erythraeus trypsin (SET) does not exhibit autolysis and crystallizes readily at physiological pH; hence, it is well suited for structural studies aimed at extending the understanding of the catalytic mechanism of serine proteases. While X-ray crystallographic structures of this enzyme have been reported, no coordinates have ever been made available in the Protein Data Bank. Based on this, and observations on the extreme stability and unique properties of this particular trypsin, it was decided to crystallize it and determine its structure. Here, the first sub-angstrom resolution structure of an unmodified, unliganded trypsin crystallized at physiological pH is reported. Detailed structural analysis reveals the geometry and structural rigidity of the catalytic triad in the unoccupied active site and comparison to related serine proteases provides a context for interpretation of biochemical studies of catalytic mechanism and activity

  5. HIGH-RESOLUTION HELIOSEISMIC IMAGING OF SUBSURFACE STRUCTURES AND FLOWS OF A SOLAR ACTIVE REGION OBSERVED BY HINODE

    International Nuclear Information System (INIS)

    Zhao Junwei; Kosovichev, Alexander G.; Sekii, Takashi

    2010-01-01

    We analyze a solar active region observed by the Hinode Ca II H line using the time-distance helioseismology technique, and infer wave-speed perturbation structures and flow fields beneath the active region with a high spatial resolution. The general subsurface wave-speed structure is similar to the previous results obtained from Solar and Heliospheric Observatory/Michelson Doppler Imager observations. The general subsurface flow structure is also similar, and the downward flows beneath the sunspot and the mass circulations around the sunspot are clearly resolved. Below the sunspot, some organized divergent flow cells are observed, and these structures may indicate the existence of mesoscale convective motions. Near the light bridge inside the sunspot, hotter plasma is found beneath, and flows divergent from this area are observed. The Hinode data also allow us to investigate potential uncertainties caused by the use of phase-speed filter for short travel distances. Comparing the measurements with and without the phase-speed filtering, we find out that inside the sunspot, mean acoustic travel times are in basic agreement, but the values are underestimated by a factor of 20%-40% inside the sunspot umbra for measurements with the filtering. The initial acoustic tomography results from Hinode show a great potential of using high-resolution observations for probing the internal structure and dynamics of sunspots.

  6. High-resolution 3-D S-wave Tomography of upper crust structures in Yilan Plain from Ambient Seismic Noise

    Science.gov (United States)

    Chen, Kai-Xun; Chen, Po-Fei; Liang, Wen-Tzong; Chen, Li-Wei; Gung, YuanCheng

    2015-04-01

    The Yilan Plain (YP) in NE Taiwan locates on the western YP of the Okinawa Trough and displays high geothermal gradients with abundant hot springs, likely resulting from magmatism associated with the back-arc spreading as attested by the offshore volcanic island (Kueishantao). YP features NS distinctive characteristics that the South YP exhibits thin top sedimentary layer, high on-land seismicity and significant SE movements, relative those of the northern counterpart. A dense network (~2.5 km station interval) of 89 Texan instruments was deployed in Aug. 2014, covering most of the YP and its vicinity. The ray path coverage density of each 0.015 degree cells are greater than 150 km that could provide the robustness assessment of tomographic results. We analyze ambient noise signals to invert a high-resolution 3D S-wave model for shallow velocity structures in and around YP. The aim is to investigate the velocity anomalies corresponding to geothermal resources and the NS geological distinctions aforementioned. We apply the Welch's method to generate empirical Rayleigh wave Green's functions between two stations records of continuous vertical components. The group velocities of thus derived functions are then obtained by the multiple-filter analysis technique measured at the frequency range between 0.25 and 1 Hz. Finally, we implement a wavelet-based multi-scale parameterization technique to construct 3D model of S-wave velocity. Our first month results exhibit low velocity in the plain, corresponding existing sediments, those of whole YP show low velocity offshore YP and those of high-resolution south YP reveal stark velocity contrast across the Sanshin fault. Key words: ambient seismic noises, Welch's method, S-wave, Yilan Plain

  7. Structure and chemistry of epitaxial ceria thin films on yttria-stabilized zirconia substrates, studied by high resolution electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Sinclair, Robert, E-mail: bobsinc@stanford.edu [Department of Materials Science and Engineering, Stanford University, Stanford, CA 94305 (United States); Lee, Sang Chul, E-mail: sclee99@stanford.edu [Department of Materials Science and Engineering, Stanford University, Stanford, CA 94305 (United States); Shi, Yezhou; Chueh, William C. [Department of Materials Science and Engineering, Stanford University, Stanford, CA 94305 (United States); Stanford Synchrotron Radiation Lightsource, SLAC National Accelerator Laboratory, Menlo Park, CA 94025 (United States); Stanford Institute for Materials and Energy Sciences, SLAC National Accelerator Laboratory, Menlo Park, CA 94025 (United States)

    2017-05-15

    We have applied aberration-corrected transmission electron microscopy (TEM) imaging and electron energy loss spectroscopy (EELS) to study the structure and chemistry of epitaxial ceria thin films, grown by pulsed laser deposition onto (001) yttria-stabilized zirconia (YSZ) substrates. There are few observable defects apart from the expected mismatch interfacial dislocations and so the films would be expected to have good potential for applications. Under high electron beam dose rate (above about 6000 e{sup -}/Å{sup 2}s) domains of an ordered structure appear and these are interpreted as being created by oxygen vacancy ordering. The ordered structure does not appear at lower lose rates (ca. 2600 e{sup -}/Å{sup 2}s) and can be removed by imaging under 1 mbar oxygen gas in an environmental TEM. EELS confirms that there is both oxygen deficiency and the associated increase in Ce{sup 3+} versus Ce{sup 4+} cations in the ordered domains. In situ high resolution TEM recordings show the formation of the ordered domains as well as atomic migration along the ceria thin film (001) surface. - Highlights: • The local structure and chemistry of ceria can be studied by TEM combined with EELS. • At lower electron, there are no observable changes in the ceria thin films. • At higher dose rates, an ordered phase is created due to oxygen vacancy ordering. • In situ HRTEM shows the oxygen vacancy ordering and the movement of surface atoms.

  8. The determination of cadmium, lead and vanadium by high resolution ICP-MS in Antarctic snow samples

    Energy Technology Data Exchange (ETDEWEB)

    Lanza, F. [Joh. Gutenberg Univ., Mainz (Germany). Inst. fuer Anorganische und Analytische Chemie; Trincherini, P. [European Union Joint Research Centre, Ispra, VA (Italy). Inst. of Environment

    2000-02-01

    Double focusing ICP-MS was successfully used in this research for the direct determination of the cadmium, lead and vanadium content of a set of Antarctic samples collected during the 11. Italian Expedition to Antarctica. For cadmium and lead measurements the low resolution mode was chosen since it ensured the highest ion sensitivity and it allowed the highest detection limits to be attained; in the case of vanadium the high resolution mode was used to solve the isobaric interference. As far as vanadium and cadmium are concerned by GFAAS coupled with different preconcentration procedures. The vanadium, cadmium and lead content measured in a riverine water reference material (SRLS-3) was found in agreement with the certified values. [Italian] Si e' utilizzato uno spettrometro ICP-MS a doppia focalizzazione per la determinazione diretta di cadmio, piombo e vanadio in una serie di campioni di neve antartica superficiale raccolta durante l'undicesima spedizione italiana in Antartide. Per le determinazioni di cadmio e piombo si e' scelta la procedura a bassa risoluzione, che ha garantito la piu' elevata sensibilita' ed ha permesso di ottenere limiti di determinazione migliori; nel caso del vanadio si e' utilizzata la procedura ad alta risoluzione che ha permesso di risolvere problemi di interferenza isobarica. Per quanto riguarda cadmio e vanadio, i risultati delle determinazioni mediante ICP-MS sono risultati in buon accordo con quelli ottenuti mediante GFAAS accoppiata a diverse procedure di preconcentrazione. Il contenuto di cadmio, piombo e vanadio misurato con le procedure sviluppate in un campione certificato di acqua di fiume (SRLS-3) e' risultato in accordo con i valori certificati.

  9. Hydrophilic interaction liquid chromatography coupled to high-resolution mass spectrometry to determine artificial sweeteners in environmental waters.

    Science.gov (United States)

    Salas, Daniela; Borrull, Francesc; Fontanals, Núria; Marcé, Rosa Maria

    2015-06-01

    Artificial sweeteners are food additives employed as sugar substitutes which are now considered to be emerging organic contaminants. In the present study, a method is developed for the determination of a group of artificial sweeteners in environmental waters. Considering the polar and hydrophilic character of these compounds, hydrophilic interaction liquid chromatography is proposed for their separation as an alternative to traditional reversed-phase liquid chromatography. Two stationary phases with different chemistry were compared for this purpose. For the detection of the analytes, high-resolution mass spectrometry (Orbitrap) was employed to take advantage of its benefits in terms of reliable quantification and confirmation for the measurement of accurate masses. Solid-phase extraction was chosen as the sample treatment, in which the extract in a mixture of NH4OH:MeOH:ACN (1:4:15) was directly injected into the chromatographic system, simplifying the analytical procedure. The optimized method was validated on river and waste water samples. For example, in the case of effluent water samples, limits of detection ranged from 0.002 to 0.7 μg/L and limits of quantification ranged from 0.004 to 1.5 μg/L. Apparent (whole method) recoveries ranged from 57 to 74% with intra-day precision (%RSD, n = 5) ranging from 6 to 25%. The method was successfully applied to water samples from different rivers in Catalonia and different waste water treatment plants in Tarragona. Acesulfame, cyclamate, saccharine and sucralose were found in several samples.

  10. Determination of 137Cs activity in soil from Qatar using high-resolution gamma-ray spectrometry

    International Nuclear Information System (INIS)

    Al-Sulaiti, Huda; Nasir, Tabassum; Al Mugren, K.S.; Alkhomashi, N.; Al-Dahan, N.; Al-Dosari, M.; Bradley, D.A.; Bukhari, S.; Matthews, M.; Regan, P.H.; Santawamaitre, T.; Malain, D.; Habib, A.; Al-Dosari, Hanan; Al Sadig, Ibrahim

    2016-01-01

    With interest in establishing baseline concentrations of 137 Cs in soil from the Qatarian peninsula, we focus on determination of the activity concentrations in 129 soil samples collected across the State of Qatar prior to the 2011 Fukushima Dai-ichi nuclear power plant accident. As such, the data provides the basis of a reference map for the detection of releases of this fission product. The activity concentrations were measured via high-resolution gamma-ray spectrometry using a hyper-pure germanium detector enclosed in a copper-lined passive lead shield that was situated in a low-background environment. The activity concentrations ranged from 0.21 to 15.41 Bq/kg, with a median value of 1 Bq/kg, the greatest activity concentration being observed in a sample obtained from northern Qatar. Although it cannot be confirmed, it is expected that this contamination is mainly due to releases from the Chernobyl accident of 26 April 1986, there being a lack of data from Qatar before the accident. The values are typically within but are sometimes lower than the range indicated by data from other countries in the region. The lower values than those of others is suggested to be due to variation in soil characteristics as well as metrological factors at the time of deposition. - Highlights: • A baseline for the radionuclide 137 Cs in soil samples collected from Qatar was established. • 129 soil samples collected across the landscape. • Samples were collected before the most recent accident “the 2011 Fukushima Dai-ichi NNP accident”. • The highest activity concentration was found to be 15.41±0.67 Stat. and 0.11 Syst. • The relatively high concentrations can be attributed to rain washout.

  11. Determination of total mercury for marine environmental monitoring studies by solid sampling continuum source high resolution atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mandjukov, Petko; Orani, Anna Maria; Han, Eunmi; Vassileva, Emilia, E-mail: e.vasileva-veleva@iaea.org

    2015-01-01

    The most critical step in almost all commonly used analytical procedures for Hg determination is the sample preparation due to its extreme volatility. One of the possible solutions of this problem is the application of methods for direct analysis of solid samples. The possibilities for solid sampling high resolution continuum source atomic absorption spectrometry (HR CS AAS) determination of total mercury in various marine environmental samples e.g. sediments and biota are object of the present study. The instrumental parameters were optimized in order to obtain reproducible and interference free analytical signal. A calibration technique based on the use of solid standard certified reference materials similar to the nature of the analyzed sample was developed and applied to various CRMs and real samples. This technique allows simple and reliable evaluation of the uncertainty of the result and the metrological characteristics of the method. A validation approach in line with the requirements of ISO 17025 standard and Eurachem guidelines was followed. With this in mind, selectivity, working range (0.06 to 25 ng for biota and 0.025 to 4 ng for sediment samples, expressed as total Hg) linearity (confirmed by Student's t-test), bias (1.6–4.3%), repeatability (4–9%), reproducibility (9–11%), and absolute limit of detection (0.025 ng for sediment, 0.096 ng for marine biota) were systematically assessed using solid CRMs. The relative expanded uncertainty was estimated at 15% for sediment sample and 8.5% for marine biota sample (k = 2). Demonstration of traceability of measurement results is also presented. The potential of the proposed analytical procedure, based on solid sampling HR CS AAS technique was demonstrated by direct analysis of sea sediments form the Caribbean region and various CRMs. Overall, the use of solid sampling HR CS AAS permits obtaining significant advantages for the determination of this complex analyte in marine samples, such as

  12. Rapid Determination of Lymphogranuloma Venereum Serovars of Chlamydia trachomatis by Quantitative High-Resolution Melt Analysis (HRMA)

    Science.gov (United States)

    Stevens, Matthew P.; Garland, Suzanne M.; Zaia, Angelo M.; Tabrizi, Sepehr N.

    2012-01-01

    A quantitative high-resolution melt analysis assay was developed to differentiate lymphogranuloma venereum-causing serovars of Chlamydia trachomatis (L1 to L3) from other C. trachomatis serovars (D to K). The detection limit of this assay is approximately 10 copies per reaction, comparable to the limits of other quantitative-PCR-based methods. PMID:22933594

  13. High resolution crystal structure of PedB: a structural basis for the classification of pediocin-like immunity proteins

    Directory of Open Access Journals (Sweden)

    Cha Sun-Shin

    2007-05-01

    Full Text Available Abstract Background Pediocin-like bacteriocins, ribosomally-synthesized antimicrobial peptides, are generally coexpressed with cognate immunity proteins in order to protect the bacteriocin-producer from its own bacteriocin. As a step for understanding the mode of action of immunity proteins, we determined the crystal structure of PedB, a pediocin-like immunity protein conferring immunity to pediocin PP-1. Results The 1.6 Å crystal structure of PedB reveals that PedB consists of an antiparallel four-helix bundle with a flexible C-terminal end. PedB shows structural similarity to an immunity protein against enterocin A (EntA-im but some disparity to an immunity protein against carnobacteriocin B2 (ImB2 in both the C-terminal conformation and the local structure constructed by α3, α4, and their connecting loop. Structure-inspired mutational studies reveal that deletion of the last seven residues of the C-terminus of PedB almost abolished its immunity activity. Conclusion The fact that PedB, EntA-im, and ImB2 share a four-helix bundle structure strongly suggests the structural conservation of this motif in the pediocin-like immunity proteins. The significant difference in the core structure and the C-terminal conformation provides a structural basis for the classification of pediocin-like immunity proteins. Our mutational study using C-terminal-shortened PedBs and the investigation of primary sequence of the C-terminal region, propose that several polar or charged residues in the extreme C-terminus of PedB which is crucial for the immunity are involved in the specific recognition of pediocin PP-1.

  14. Determination of total mercury for marine environmental monitoring studies by solid sampling continuum source high resolution atomic absorption spectrometry

    Science.gov (United States)

    Mandjukov, Petko; Orani, Anna Maria; Han, Eunmi; Vassileva, Emilia

    2015-01-01

    The most critical step in almost all commonly used analytical procedures for Hg determination is the sample preparation due to its extreme volatility. One of the possible solutions of this problem is the application of methods for direct analysis of solid samples. The possibilities for solid sampling high resolution continuum source atomic absorption spectrometry (HR CS AAS) determination of total mercury in various marine environmental samples e.g. sediments and biota are object of the present study. The instrumental parameters were optimized in order to obtain reproducible and interference free analytical signal. A calibration technique based on the use of solid standard certified reference materials similar to the nature of the analyzed sample was developed and applied to various CRMs and real samples. This technique allows simple and reliable evaluation of the uncertainty of the result and the metrological characteristics of the method. A validation approach in line with the requirements of ISO 17025 standard and Eurachem guidelines was followed. With this in mind, selectivity, working range (0.06 to 25 ng for biota and 0.025 to 4 ng for sediment samples, expressed as total Hg) linearity (confirmed by Student's t-test), bias (1.6-4.3%), repeatability (4-9%), reproducibility (9-11%), and absolute limit of detection (0.025 ng for sediment, 0.096 ng for marine biota) were systematically assessed using solid CRMs. The relative expanded uncertainty was estimated at 15% for sediment sample and 8.5% for marine biota sample (k = 2). Demonstration of traceability of measurement results is also presented. The potential of the proposed analytical procedure, based on solid sampling HR CS AAS technique was demonstrated by direct analysis of sea sediments form the Caribbean region and various CRMs. Overall, the use of solid sampling HR CS AAS permits obtaining significant advantages for the determination of this complex analyte in marine samples, such as straightforward

  15. Changes in structural lung disease in cystic fibrosis children over 4 years as evaluated by high-resolution computed tomography

    Energy Technology Data Exchange (ETDEWEB)

    Carpio, Carlos; Alvarez-Sala, Rodolfo; Prados, Concepcion [University Hospital La Paz, La Paz Hospital Research Institute, Department of Respiratory Medicine, Madrid (Spain); Albi, Gustavo [Nino de Jesus Children' s Hospital, Department of Radiology, Madrid (Spain); Rayon-Aledo, Jose Carlos; Caballero, Paloma [University Hospital La Princesa, Department of Radiology, Madrid (Spain); Giron, Rosa [University Hospital La Princesa, Department of Respiratory Medicine, Madrid (Spain)

    2015-12-15

    To compare the worsening of structural lung disease on high-resolution computed tomography (HRCT) with changes in spirometry results in cystic fibrosis (CF) patients, and analyse factors associated with the worsening of structural lung disease over time. A total of 31 CF subjects (mean age 11.03 ± 3.67 years old) were prospectively evaluated by two HRCT and spirometry tests performed 4 years apart. HRCT abnormalities were scored using the Bhalla scoring system. Comparisons between changes on HRCT and spirometry were made for all patients, and also for groups categorized by age, sex, genotypic alterations and lung obstruction. The mean HRCT Bhalla scoring, forced expiratory volume in 1 s (FEV{sub 1} %pred.) and forced vital capacity (FVC %pred.) were 7.92 ± 3.59, 87.76 ± 20.52 and 96.54 ± 15.12, respectively. There was a significant deterioration in the Bhalla score (p < 0.01) and in certain categories: severity of bronchiectasis, peribronchial thickening, mucous plugging and bronchial divisions. Females had a more pronounced worsening of the Bhalla score than males (p = 0.048). No change over time was found in FEV{sub 1} and FVC. Only sex was associated with a deterioration in HRCT. HRCT Bhalla scoring changes statistically significantly over 4 years, but spirometry results do not. Worsening on HRCT is more evident in females. (orig.)

  16. Changes in structural lung disease in cystic fibrosis children over 4 years as evaluated by high-resolution computed tomography

    International Nuclear Information System (INIS)

    Carpio, Carlos; Alvarez-Sala, Rodolfo; Prados, Concepcion; Albi, Gustavo; Rayon-Aledo, Jose Carlos; Caballero, Paloma; Giron, Rosa

    2015-01-01

    To compare the worsening of structural lung disease on high-resolution computed tomography (HRCT) with changes in spirometry results in cystic fibrosis (CF) patients, and analyse factors associated with the worsening of structural lung disease over time. A total of 31 CF subjects (mean age 11.03 ± 3.67 years old) were prospectively evaluated by two HRCT and spirometry tests performed 4 years apart. HRCT abnormalities were scored using the Bhalla scoring system. Comparisons between changes on HRCT and spirometry were made for all patients, and also for groups categorized by age, sex, genotypic alterations and lung obstruction. The mean HRCT Bhalla scoring, forced expiratory volume in 1 s (FEV 1 %pred.) and forced vital capacity (FVC %pred.) were 7.92 ± 3.59, 87.76 ± 20.52 and 96.54 ± 15.12, respectively. There was a significant deterioration in the Bhalla score (p < 0.01) and in certain categories: severity of bronchiectasis, peribronchial thickening, mucous plugging and bronchial divisions. Females had a more pronounced worsening of the Bhalla score than males (p = 0.048). No change over time was found in FEV 1 and FVC. Only sex was associated with a deterioration in HRCT. HRCT Bhalla scoring changes statistically significantly over 4 years, but spirometry results do not. Worsening on HRCT is more evident in females. (orig.)

  17. High resolution bone material property assignment yields robust subject specific finite element models of complex thin bone structures.

    Science.gov (United States)

    Pakdel, Amirreza; Fialkov, Jeffrey; Whyne, Cari M

    2016-06-14

    Accurate finite element (FE) modeling of complex skeletal anatomy requires high resolution in both meshing and the heterogeneous mapping of material properties onto the generated mesh. This study introduces Node-based elastic Modulus Assignment with Partial-volume correction (NMAP) as a new approach for FE material property assignment to thin bone structures. The NMAP approach incorporates point spread function based deblurring of CT images, partial-volume correction of CT image voxel intensities and anisotropic interpolation and mapping of CT intensity assignment to FE mesh nodes. The NMAP procedure combined with a derived craniomaxillo-facial skeleton (CMFS) specific density-isotropic elastic modulus relationship was applied to produce specimen-specific FE models of 6 cadaveric heads. The NMAP procedure successfully generated models of the complex thin bone structures with surface elastic moduli reflective of cortical bone material properties. The specimen-specific CMFS FE models were able to accurately predict experimental strains measured under in vitro temporalis and masseter muscle loading (r=0.93, slope=1.01, n=5). The strength of this correlation represents a robust validation for CMFS FE modeling that can be used to better understand load transfer in this complex musculoskeletal system. The developed methodology offers a systematic process-flow able to address the complexity of the CMFS that can be further applied to create high-fidelity models of any musculoskeletal anatomy. Copyright © 2016 Elsevier Ltd. All rights reserved.

  18. High-resolution crystal structures of Drosophila melanogaster angiotensin-converting enzyme in complex with novel inhibitors and antihypertensive drugs.

    Science.gov (United States)

    Akif, Mohd; Georgiadis, Dimitris; Mahajan, Aman; Dive, Vincent; Sturrock, Edward D; Isaac, R Elwyn; Acharya, K Ravi

    2010-07-16

    Angiotensin I-converting enzyme (ACE), one of the central components of the renin-angiotensin system, is a key therapeutic target for the treatment of hypertension and cardiovascular disorders. Human somatic ACE (sACE) has two homologous domains (N and C). The N- and C-domain catalytic sites have different activities toward various substrates. Moreover, some of the undesirable side effects of the currently available and widely used ACE inhibitors may arise from their targeting both domains leading to defects in other pathways. In addition, structural studies have shown that although both these domains have much in common at the inhibitor binding site, there are significant differences and these are greater at the peptide binding sites than regions distal to the active site. As a model system, we have used an ACE homologue from Drosophila melanogaster (AnCE, a single domain protein with ACE activity) to study ACE inhibitor binding. In an extensive study, we present high-resolution structures for native AnCE and in complex with six known antihypertensive drugs, a novel C-domain sACE specific inhibitor, lisW-S, and two sACE domain-specific phosphinic peptidyl inhibitors, RXPA380 and RXP407 (i.e., nine structures). These structures show detailed binding features of the inhibitors and highlight subtle changes in the orientation of side chains at different binding pockets in the active site in comparison with the active site of N- and C-domains of sACE. This study provides information about the structure-activity relationships that could be utilized for designing new inhibitors with improved domain selectivity for sACE. 2010 Elsevier Ltd. All rights reserved.

  19. Determination of the resonance parameters for 232Th from high resolution transmission and capture measurements at GELINA

    International Nuclear Information System (INIS)

    Brusegan, A.; Schillebeeckx, P.; Lobo, G.; Borella, A.; Volev, K.; Janeva, N.

    2003-01-01

    To deduce the resonance parameters for 232 Th in the resolved resonance region, high resolution transmission and capture measurements are being performed. The measurements are performed at the Time-Of-Flight facility GELINA. A comparison of experimental data resulting from capture (top) and transmission (bottom) are shown. The transmission measurements are performed at a 50 m flight path. The neutron are detected with a 0.25' thick lithium glass (NE912) placed in an Al sphere and viewed by a 5' EMI KQB photomultiplier orthogonal to the neutron beam axis. The injection of a stabilised light pulse in the detector during the measurements provided an efficient tool to control to better than 1% the gain of the entire electronics. The experimental set-up includes a sample-changer, placed at 23 m from the neutron source, which is driven by the acquisition system. The determination of the flight path length, was based on transmission of the 6.673 eV resonance of 238 U. We summarise, for the different energy regions of interest, the scheduled measurement conditions: the operation frequency of the accelerator and the target thickness. A simultaneous analysis of the data using REFIT will result in the resonance parameters from 0 to 4 keV. We show the result of a resonance shape analysis for the resonances at 21.8 and 23.5 eV. The resulting resonance parameters are important for the energy calibration and normalisation of the capture measurements in both the resolved and unresolved resonance region. The capture measurements are completed and were performed at a 60 m flight path. The sample consisted of a metallic natural thorium disc of 8 cm diameter and 1.0 mm thick, corresponding to a thickness of 3.176 10 -3 at/b. The neutron flux was measured with an ionisation chamber loaded with three back-to-back layers of about 40 μg/cm 2 10 B. The gamma rays, originating from the 232 Th(n,γ) reaction, were detected by four C 6 D 6 -based liquid scintillators (NE230) placed

  20. High-Resolution Photoionization, Photoelectron and Photodissociation Studies. Determination of Accurate Energetic and Spectroscopic Database for Combustion Radicals and Molecules

    Energy Technology Data Exchange (ETDEWEB)

    Ng, Cheuk-Yiu [Univ. of California, Davis, CA (United States)

    2016-04-25

    The main goal of this research program was to obtain accurate thermochemical and spectroscopic data, such as ionization energies (IEs), 0 K bond dissociation energies, 0 K heats of formation, and spectroscopic constants for radicals and molecules and their ions of relevance to combustion chemistry. Two unique, generally applicable vacuum ultraviolet (VUV) laser photoion-photoelectron apparatuses have been developed in our group, which have used for high-resolution photoionization, photoelectron, and photodissociation studies for many small molecules of combustion relevance.

  1. Using Unmanned Aerial Vehicles (UAV for High-Resolution Reconstruction of Topography: The Structure from Motion Approach on Coastal Environments

    Directory of Open Access Journals (Sweden)

    Francesco Mancini

    2013-12-01

    Full Text Available The availability of high-resolution Digital Surface Models of coastal environments is of increasing interest for scientists involved in the study of the coastal system processes. Among the range of terrestrial and aerial methods available to produce such a dataset, this study tests the utility of the Structure from Motion (SfM approach to low-altitude aerial imageries collected by Unmanned Aerial Vehicle (UAV. The SfM image-based approach was selected whilst searching for a rapid, inexpensive, and highly automated method, able to produce 3D information from unstructured aerial images. In particular, it was used to generate a dense point cloud and successively a high-resolution Digital Surface Models (DSM of a beach dune system in Marina di Ravenna (Italy. The quality of the elevation dataset produced by the UAV-SfM was initially evaluated by comparison with point cloud generated by a Terrestrial Laser Scanning (TLS surveys. Such a comparison served to highlight an average difference in the vertical values of 0.05 m (RMS = 0.19 m. However, although the points cloud comparison is the best approach to investigate the absolute or relative correspondence between UAV and TLS methods, the assessment of geomorphic features is usually based on multi-temporal surfaces analysis, where an interpolation process is required. DSMs were therefore generated from UAV and TLS points clouds and vertical absolute accuracies assessed by comparison with a Global Navigation Satellite System (GNSS survey. The vertical comparison of UAV and TLS DSMs with respect to GNSS measurements pointed out an average distance at cm-level (RMS = 0.011 m. The successive point by point direct comparison between UAV and TLS elevations show a very small average distance, 0.015 m, with RMS = 0.220 m. Larger values are encountered in areas where sudden changes in topography are present. The UAV-based approach was demonstrated to be a straightforward one and accuracy of the vertical dataset

  2. High-Resolution Inkjet-Printed Oxide Thin-Film Transistors with a Self-Aligned Fine Channel Bank Structure.

    Science.gov (United States)

    Zhang, Qing; Shao, Shuangshuang; Chen, Zheng; Pecunia, Vincenzo; Xia, Kai; Zhao, Jianwen; Cui, Zheng

    2018-05-09

    A self-aligned inkjet printing process has been developed to construct small channel metal oxide (a-IGZO) thin-film transistors (TFTs) with independent bottom gates on transparent glass substrates. Poly(methylsilsesquioxane) was used to pattern hydrophobic banks on the transparent substrate instead of commonly used self-assembled octadecyltrichlorosilane. Photolithographic exposure from backside using bottom-gate electrodes as mask formed hydrophilic channel areas for the TFTs. IGZO ink was selectively deposited by an inkjet printer in the hydrophilic channel region and confined by the hydrophobic bank structure, resulting in the precise deposition of semiconductor layers just above the gate electrodes. Inkjet-printed IGZO TFTs with independent gate electrodes of 10 μm width have been demonstrated, avoiding completely printed channel beyond the broad of the gate electrodes. The TFTs showed on/off ratios of 10 8 , maximum mobility of 3.3 cm 2 V -1 s -1 , negligible hysteresis, and good uniformity. This method is conductive to minimizing the area of printed TFTs so as to the development of high-resolution printing displays.

  3. High-Resolution Tracking Asymmetric Lithium Insertion and Extraction and Local Structure Ordering in SnS2.

    Science.gov (United States)

    Gao, Peng; Wang, Liping; Zhang, Yu-Yang; Huang, Yuan; Liao, Lei; Sutter, Peter; Liu, Kaihui; Yu, Dapeng; Wang, En-Ge

    2016-09-14

    In the rechargeable lithium ion batteries, the rate capability and energy efficiency are largely governed by the lithium ion transport dynamics and phase transition pathways in electrodes. Real-time and atomic-scale tracking of fully reversible lithium insertion and extraction processes in electrodes, which would ultimately lead to mechanistic understanding of how the electrodes function and why they fail, is highly desirable but very challenging. Here, we track lithium insertion and extraction in the van der Waals interactions dominated SnS2 by in situ high-resolution TEM method. We find that the lithium insertion occurs via a fast two-phase reaction to form expanded and defective LiSnS2, while the lithium extraction initially involves heterogeneous nucleation of intermediate superstructure Li0.5SnS2 domains with a 1-4 nm size. Density functional theory calculations indicate that the Li0.5SnS2 is kinetically favored and structurally stable. The asymmetric reaction pathways may supply enlightening insights into the mechanistic understanding of the underlying electrochemistry in the layered electrode materials and also suggest possible alternatives to the accepted explanation of the origins of voltage hysteresis in the intercalation electrode materials.

  4. Mapping Urban Tree Canopy Coverage and Structure using Data Fusion of High Resolution Satellite Imagery and Aerial Lidar

    Science.gov (United States)

    Elmes, A.; Rogan, J.; Williams, C. A.; Martin, D. G.; Ratick, S.; Nowak, D.

    2015-12-01

    Urban tree canopy (UTC) coverage is a critical component of sustainable urban areas. Trees provide a number of important ecosystem services, including air pollution mitigation, water runoff control, and aesthetic and cultural values. Critically, urban trees also act to mitigate the urban heat island (UHI) effect by shading impervious surfaces and via evaporative cooling. The cooling effect of urban trees can be seen locally, with individual trees reducing home HVAC costs, and at a citywide scale, reducing the extent and magnitude of an urban areas UHI. In order to accurately model the ecosystem services of a given urban forest, it is essential to map in detail the condition and composition of these trees at a fine scale, capturing individual tree crowns and their vertical structure. This paper presents methods for delineating UTC and measuring canopy structure at fine spatial resolution (body of methods, relying on a data fusion method to combine the information contained in high resolution WorldView-3 satellite imagery and aerial lidar data using an object-based image classification approach. The study area, Worcester, MA, has recently undergone a large-scale tree removal and reforestation program, following a pest eradication effort. Therefore, the urban canopy in this location provides a wide mix of tree age class and functional type, ideal for illustrating the effectiveness of the proposed methods. Early results show that the object-based classifier is indeed capable of identifying individual tree crowns, while continued research will focus on extracting crown structural characteristics using lidar-derived metrics. Ultimately, the resulting fine resolution UTC map will be compared with previously created UTC maps of the same area but for earlier dates, producing a canopy change map corresponding to the Worcester area tree removal and replanting effort.

  5. Intensive structural investigation of R{sub 2}Fe{sub 17-x}M{sub x} intermetallic compounds using high resolution powder neutron diffractometer

    Energy Technology Data Exchange (ETDEWEB)

    Mujamilah,; Ridwan, [Materials Science Research Center, National Atomic Energy Agency of Indonesia, Jakarta (Indonesia)

    1998-10-01

    The crystallographic and magnetic structure of R{sub 2}Fe{sub 17-x}M{sub x} intermetallic compounds system were refined by Rietveld analyses of the high resolution neutron powder diffraction data. The analyses results show that the substituent atoms were not distributed randomly over the Fe sites, but preferentially occupied some Fe sites. More further, it was also found that the substituent atoms which atomic radius smaller than Fe tend to avoid the 6c site at low concentration while the larger substituent atom tend to replace the Fe atom at this 6c site corresponding to their concentration. From these crystallographic data, it was suggested that the change of magnetic ordering temperature Tc, is not mainly determined by the change of short bond distance between this `dumb-bell` atoms, but it was also influenced by the nearest coordinated atoms to this site. (author)

  6. Ultra high-resolution gene centric genomic structural analysis of a non-syndromic congenital heart defect, Tetralogy of Fallot.

    Directory of Open Access Journals (Sweden)

    Douglas C Bittel

    Full Text Available Tetralogy of Fallot (TOF is one of the most common severe congenital heart malformations. Great progress has been made in identifying key genes that regulate heart development, yet approximately 70% of TOF cases are sporadic and nonsyndromic with no known genetic cause. We created an ultra high-resolution gene centric comparative genomic hybridization (gcCGH microarray based on 591 genes with a validated association with cardiovascular development or function. We used our gcCGH array to analyze the genomic structure of 34 infants with sporadic TOF without a deletion on chromosome 22q11.2 (n male = 20; n female = 14; age range of 2 to 10 months. Using our custom-made gcCGH microarray platform, we identified a total of 613 copy number variations (CNVs ranging in size from 78 base pairs to 19.5 Mb. We identified 16 subjects with 33 CNVs that contained 13 different genes which are known to be directly associated with heart development. Additionally, there were 79 genes from the broader list of genes that were partially or completely contained in a CNV. All 34 individuals examined had at least one CNV involving these 79 genes. Furthermore, we had available whole genome exon arrays from right ventricular tissue in 13 of our subjects. We analyzed these for correlations between copy number and gene expression level. Surprisingly, we could detect only one clear association between CNVs and expression (GSTT1 for any of the 591 focal genes on the gcCGH array. The expression levels of GSTT1 were correlated with copy number in all cases examined (r = 0.95, p = 0.001. We identified a large number of small CNVs in genes with varying associations with heart development. Our results illustrate the complexity of human genome structural variation and underscore the need for multifactorial assessment of potential genetic/genomic factors that contribute to congenital heart defects.

  7. High resolution structure of the ba3 cytochrome c oxidase from Thermus thermophilus in a lipidic environment.

    Directory of Open Access Journals (Sweden)

    Theresa Tiefenbrunn

    Full Text Available The fundamental chemistry underpinning aerobic life on Earth involves reduction of dioxygen to water with concomitant proton translocation. This process is catalyzed by members of the heme-copper oxidase (HCO superfamily. Despite the availability of crystal structures for all types of HCO, the mode of action for this enzyme is not understood at the atomic level, namely how vectorial H(+ and e(- transport are coupled. Toward addressing this problem, we report wild type and A120F mutant structures of the ba(3-type cytochrome c oxidase from Thermus thermophilus at 1.8 Å resolution. The enzyme has been crystallized from the lipidic cubic phase, which mimics the biological membrane environment. The structures reveal 20 ordered lipid molecules that occupy binding sites on the protein surface or mediate crystal packing interfaces. The interior of the protein encloses 53 water molecules, including 3 trapped in the designated K-path of proton transfer and 8 in a cluster seen also in A-type enzymes that likely functions in egress of product water and proton translocation. The hydrophobic O(2-uptake channel, connecting the active site to the lipid bilayer, contains a single water molecule nearest the Cu(B atom but otherwise exhibits no residual electron density. The active site contains strong electron density for a pair of bonded atoms bridging the heme Fe(a3 and Cu(B atoms that is best modeled as peroxide. The structure of ba(3-oxidase reveals new information about the positioning of the enzyme within the membrane and the nature of its interactions with lipid molecules. The atomic resolution details provide insight into the mechanisms of electron transfer, oxygen diffusion into the active site, reduction of oxygen to water, and pumping of protons across the membrane. The development of a robust system for production of ba(3-oxidase crystals diffracting to high resolution, together with an established expression system for generating mutants, opens the

  8. High resolution crustal structure for the region between the Chilenia and Cuyania terrane above the Pampean flat slab of Argentina from local receiver function and petrological analyses

    Science.gov (United States)

    Ammirati, J. B.; Alvarado, P. M.; Pérez, S. B.; Beck, S. L.; Porter, R. C.; Zandt, G.

    2015-12-01

    Jean-Baptiste Ammirati 1,Sofía Perez 1, Patricia Alvarado 1, Susan L. Beck 2, Ryan Porter 3 and George Zandt 2(1) CIGEOBIO-CONICET, Universidad Nacional de San Juan, Argentina (2) The University of Arizona, USA (3) Northern Arizona University, USA At ~31ºS, The subduction of the Nazca plate under the South American plate presents along-strike variations of its dip angle referred to the Chilean-Pampean flat slab. Geological observations suggest that the regional crustal structure is inherited from the accretion of different terranes at Ordovician times and later reactivated during Andean compression since Miocene. Geophysical observations confirmed that the structure is extending in depth with décollement levels that accommodate crustal shortening in the region. In order to get a better insight on the shallow tectonics we computed high frequency local receiver functions from slab seismicity (~100 km depth). Local earthquakes present a higher frequency content that permits a better vertical resolution. Using a common conversion point (CCP) stacking method we obtained cross sections showing high-resolution crustal structure in the western part of the Pampean flat slab region, at the transition between the Precordillera and the Frontal Cordillera. Our results show a well-defined structure and their lateral extent for both units down to 80 km depth. In good agreement with previous studies, our higher resolution images better identify very shallow discontinuities putting more constraints on the relationships with the regional structural geology. Recent petrological analyses combined with RF high-resolution structure also allow us to better understand the regional crustal composition. Interestingly, we are able to observe a shifting structure beneath the Uspallata-Calingasta Valley, highlighting the differences in terms of crustal structure between the Precordillera and the Frontal Cordillera. Previously determined focal mechanisms in the region match well this

  9. Factors Determining the Inter-observer Variability and Diagnostic Accuracy of High-resolution Manometry for Esophageal Motility Disorders.

    Science.gov (United States)

    Kim, Ji Hyun; Kim, Sung Eun; Cho, Yu Kyung; Lim, Chul-Hyun; Park, Moo In; Hwang, Jin Won; Jang, Jae-Sik; Oh, Minkyung

    2018-01-30

    Although high-resolution manometry (HRM) has the advantage of visual intuitiveness, its diagnostic validity remains under debate. The aim of this study was to evaluate the diagnostic accuracy of HRM for esophageal motility disorders. Six staff members and 8 trainees were recruited for the study. In total, 40 patients enrolled in manometry studies at 3 institutes were selected. Captured images of 10 representative swallows and a single swallow in analyzing mode in both high-resolution pressure topography (HRPT) and conventional line tracing formats were provided with calculated metrics. Assessments of esophageal motility disorders showed fair agreement for HRPT and moderate agreement for conventional line tracing (κ = 0.40 and 0.58, respectively). With the HRPT format, the k value was higher in category A (esophagogastric junction [EGJ] relaxation abnormality) than in categories B (major body peristalsis abnormalities with intact EGJ relaxation) and C (minor body peristalsis abnormalities or normal body peristalsis with intact EGJ relaxation). The overall exact diagnostic accuracy for the HRPT format was 58.8% and rater's position was an independent factor for exact diagnostic accuracy. The diagnostic accuracy for major disorders was 63.4% with the HRPT format. The frequency of major discrepancies was higher for category B disorders than for category A disorders (38.4% vs 15.4%; P < 0.001). The interpreter's experience significantly affected the exact diagnostic accuracy of HRM for esophageal motility disorders. The diagnostic accuracy for major disorders was higher for achalasia than distal esophageal spasm and jackhammer esophagus.

  10. High resolution ultrasonic densitometer

    International Nuclear Information System (INIS)

    Dress, W.B.

    1983-01-01

    The velocity of torsional stress pulses in an ultrasonic waveguide of non-circular cross section is affected by the temperature and density of the surrounding medium. Measurement of the transit times of acoustic echoes from the ends of a sensor section are interpreted as level, density, and temperature of the fluid environment surrounding that section. This paper examines methods of making these measurements to obtain high resolution, temperature-corrected absolute and relative density and level determinations of the fluid. Possible applications include on-line process monitoring, a hand-held density probe for battery charge state indication, and precise inventory control for such diverse fluids as uranium salt solutions in accountability storage and gasoline in service station storage tanks

  11. High-Resolution Aeromagnetic Survey over the Yucatan Peninsula - Implications for Chicxulub Impact, Secondary Craters and Regional Crustal Structures

    Science.gov (United States)

    Fucugauchi, J. U.; Lopez-Loera, H.; Rebolledo-Vieyra, M.

    2011-12-01

    We present the initial results of a low-altitude high-resolution aeromagnetic study over the Yucatan peninsula. Area surveyed extends from 86W to 91W and 18N to 21N, covering the peninsula and adjacent continental margin of Gulf of Mexico and Caribbean Sea. Aeromagnetic surveys are integrated into a regional map, and regional and residual anomalies are separated using spectral and least-squares methods. For the study, aeromagnetic field was reduced to the pole and several data filtering techniques were used, including first and second vertical derivatives, analytical signal, and upward and downward analytical continuations. The region is characterized by large amplitude broad elongated magnetic anomalies oriented north-south in the northern sector of the continental shelf, and northwest-southeast and northeast-southwest over the western and eastern sides of the peninsula, respectively. Major regional anomalies extend from the continental shelf into the peninsula, whereas other anomaly trends in the central northern sector, at northeast limit of Chicxulub crater, are restricted to the shelf. Largest anomaly on the east extends over the Holbox fracture zone. At its southern end, south of Chetumal a parallel trend extends over the Rio Hondo fault zone between Quintana Roo and Belize. On the western peninsula the anomaly is characterized by two parallel trends offset between Yucatan and Campeche. The central zone of Chicxulub is characterized by a semi-circular anomaly pattern, surrounded by long wavelength small amplitude anomalies extending to the east on the peninsula and shelf, isolated from the regional broad anomalies. To the south of Chicxulub anomaly, there is an elongated low with a central high extending southward from the terrace zone inside the crater rim. The elongated magnetic anomaly correlates with a broad gravity low, which is apparent south of the concentric zone of anomalies. To the north of Chicxulub anomaly, a magnetic high inside the crater is

  12. High-Resolution Crystal Structure of a Silver(I)-RNA Hybrid Duplex Containing Watson-Crick-like C-Silver(I)-C Metallo-Base Pairs.

    Science.gov (United States)

    Kondo, Jiro; Tada, Yoshinari; Dairaku, Takenori; Saneyoshi, Hisao; Okamoto, Itaru; Tanaka, Yoshiyuki; Ono, Akira

    2015-11-02

    Metallo-base pairs have been extensively studied for applications in nucleic acid-based nanodevices and genetic code expansion. Metallo-base pairs composed of natural nucleobases are attractive because nanodevices containing natural metallo-base pairs can be easily prepared from commercially available sources. Previously, we have reported a crystal structure of a DNA duplex containing T-Hg(II)-T base pairs. Herein, we have determined a high-resolution crystal structure of the second natural metallo-base pair between pyrimidine bases C-Ag(I)-C formed in an RNA duplex. One Ag(I) occupies the center between two cytosines and forms a C-Ag(I)-C base pair through N3-Ag(I)-N3 linear coordination. The C-Ag(I)-C base pair formation does not disturb the standard A-form conformation of RNA. Since the C-Ag(I)-C base pair is structurally similar to the canonical Watson-Crick base pairs, it can be a useful building block for structure-based design and fabrication of nucleic acid-based nanodevices. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Unambiguous determination of H-atom positions: comparing results from neutron and high-resolution X-ray crystallography.

    Science.gov (United States)

    Gardberg, Anna S; Del Castillo, Alexis Rae; Weiss, Kevin L; Meilleur, Flora; Blakeley, Matthew P; Myles, Dean A A

    2010-05-01

    The locations of H atoms in biological structures can be difficult to determine using X-ray diffraction methods. Neutron diffraction offers a relatively greater scattering magnitude from H and D atoms. Here, 1.65 A resolution neutron diffraction studies of fully perdeuterated and selectively CH(3)-protonated perdeuterated crystals of Pyrococcus furiosus rubredoxin (D-rubredoxin and HD-rubredoxin, respectively) at room temperature (RT) are described, as well as 1.1 A resolution X-ray diffraction studies of the same protein at both RT and 100 K. The two techniques are quantitatively compared in terms of their power to directly provide atomic positions for D atoms and analyze the role played by atomic thermal motion by computing the sigma level at the D-atom coordinate in simulated-annealing composite D-OMIT maps. It is shown that 1.65 A resolution RT neutron data for perdeuterated rubredoxin are approximately 8 times more likely overall to provide high-confidence positions for D atoms than 1.1 A resolution X-ray data at 100 K or RT. At or above the 1.0sigma level, the joint X-ray/neutron (XN) structures define 342/378 (90%) and 291/365 (80%) of the D-atom positions for D-rubredoxin and HD-rubredoxin, respectively. The X-ray-only 1.1 A resolution 100 K structures determine only 19/388 (5%) and 8/388 (2%) of the D-atom positions above the 1.0sigma level for D-rubredoxin and HD-rubredoxin, respectively. Furthermore, the improved model obtained from joint XN refinement yielded improved electron-density maps, permitting the location of more D atoms than electron-density maps from models refined against X-ray data only.

  14. Preliminary Determination of Natural Radioactivity Levels of the State of Qatar using High-Resolution Gamma-ray Spectrometry

    International Nuclear Information System (INIS)

    Al-Sulaiti, H.A.; Regan, P.H.; Bradley, D.A.; Matthews, M.; Santawamaitre, T.; Malain, D.

    2009-01-01

    The State of Qatar is a peninsula with a total area of 11,437 km 2 which lies over a geological formation comprising a sequence of limestone, chalk, clay and gypsum. Establishing a baseline for the radioactivity concentration in Qatar's soil is the main purpose behind the present study. The project is focused on obtaining measurements of representative soil samples from various areas in Qatar to establish concentrations of the 235 U, 238 U and 232 Th natural decay chains and also the long-lived naturally occurring radionuclide 40 K. The 235 U, 238 U, 232 Th and 40 K concentrations have been measured via high-resolution gamma-ray spectrometry using a hyper-pure germanium detector situated in a low-background environment with a copper inner-plated passive lead shield. A wide range of different gamma-ray energy transitions lines arising from the multiple decay products from the 235 U, 238 U and 232 Th decay chains have been analyzed separately to obtain more statistically significant overall results

  15. High Resolution Elevation Contours

    Data.gov (United States)

    Minnesota Department of Natural Resources — This dataset contains contours generated from high resolution data sources such as LiDAR. Generally speaking this data is 2 foot or less contour interval.

  16. High resolution spiral CT for determining the malignant potential of solitary pulmonary nodules: refining and testing the test

    Energy Technology Data Exchange (ETDEWEB)

    Harders, Stefan Walbom; Madsen, Hans Henrik; Rasmussen, Finn (Dept. of Radiology, Aarhus Univ. Hospital, Aarhus (Denmark)), Email: stefhard@rm.dk; Rasmussen, Torben Riis (Dept. of Pulmonology, Aarhus Univ. Hospital, Aarhus (Denmark)); Hager, Henrik (Dept. of Pathology, Aarhus Univ. Hospital, Aarhus (Denmark))

    2011-05-15

    Background A solitary pulmonary nodule (SPN) may represent early stage lung cancer. Lung cancer is a devastating disease with an overall 5-year mortality rate of approximately 84% but with early detection and surgery as low as 47%. Currently a contrast-enhanced multiple-row detector CT (MDCT) scan is the first examination when evaluating patients with suspected lung cancer. Purpose To apply an additional high resolution CT (HRCT) to SPNs to test whether certain morphological characteristics are associated with malignancy, to assess the diagnostic accuracy of HRCT in the characterization of SPNs, and to address the reproducibility of all measures. Material and Method Two hundred and thirteen participants with SPNs were included in a follow-up study. Blinded HRCT images were assessed with regard to margin risk categories (MRCs), calcification patterns and certain other characteristics and overall malignancy potential ratings (MPRs) were given. Morphological characteristics were tested against reference standard and ROC methodology was applied to assess diagnostic accuracy. Reproducibility was measured with Kappa statistics and 95% confidence intervals were computed for all results. Histopathology (90%) and CT follow-up (10%) were used as reference standard. Results MRCs (P < 0.001), calcification patterns (P = 0.003), and pleural retraction (P < 0.001) were all statistically significantly associated to malignancy. Reproducibility was moderate to substantial. Sensitivity, specificity, and overall diagnostic accuracy of HRCT were 98%, 23% and 87%, respectively. Reproducibility was substantial. Conclusion Statistically significant associations between SPN MRCs, calcification patterns, pleural retraction and malignancy were found. HRCT yielded a very high sensitivity and a somewhat lower specificity for malignancy. Reproducibility was high

  17. High resolution spiral CT for determining the malignant potential of solitary pulmonary nodules: refining and testing the test

    International Nuclear Information System (INIS)

    Harders, Stefan Walbom; Madsen, Hans Henrik; Rasmussen, Finn; Rasmussen, Torben Riis; Hager, Henrik

    2011-01-01

    Background A solitary pulmonary nodule (SPN) may represent early stage lung cancer. Lung cancer is a devastating disease with an overall 5-year mortality rate of approximately 84% but with early detection and surgery as low as 47%. Currently a contrast-enhanced multiple-row detector CT (MDCT) scan is the first examination when evaluating patients with suspected lung cancer. Purpose To apply an additional high resolution CT (HRCT) to SPNs to test whether certain morphological characteristics are associated with malignancy, to assess the diagnostic accuracy of HRCT in the characterization of SPNs, and to address the reproducibility of all measures. Material and Method Two hundred and thirteen participants with SPNs were included in a follow-up study. Blinded HRCT images were assessed with regard to margin risk categories (MRCs), calcification patterns and certain other characteristics and overall malignancy potential ratings (MPRs) were given. Morphological characteristics were tested against reference standard and ROC methodology was applied to assess diagnostic accuracy. Reproducibility was measured with Kappa statistics and 95% confidence intervals were computed for all results. Histopathology (90%) and CT follow-up (10%) were used as reference standard. Results MRCs (P < 0.001), calcification patterns (P = 0.003), and pleural retraction (P < 0.001) were all statistically significantly associated to malignancy. Reproducibility was moderate to substantial. Sensitivity, specificity, and overall diagnostic accuracy of HRCT were 98%, 23% and 87%, respectively. Reproducibility was substantial. Conclusion Statistically significant associations between SPN MRCs, calcification patterns, pleural retraction and malignancy were found. HRCT yielded a very high sensitivity and a somewhat lower specificity for malignancy. Reproducibility was high

  18. Determination of BMAA and three alkaloid cyanotoxins in lake water using dansyl chloride derivatization and high-resolution mass spectrometry.

    Science.gov (United States)

    Roy-Lachapelle, Audrey; Solliec, Morgan; Sauvé, Sébastien

    2015-07-01

    A new analytical method was developed for the detection of alkaloid cyanotoxins in harmful algal blooms. The detection of the nonproteinogenic amino acid β-N-methylamino-L-alanine (BMAA) and two of its conformation isomers, 2,4-diaminobutyric acid (DAB) and N-(2-aminoethyl) glycine (AEG), as well as three alkaloid cyanotoxins, anatoxin-a (ANA-a), cylindrospermopsin (CYN), and saxitoxin (STX), is presented. The use of a chemical derivatization with dansyl chloride (DNS) allows easier separation with reversed phase liquid chromatography. Detection with high-resolution mass spectrometry (HRMS) with the Q-Exactive enables high selectivity with specific fragmentation as well as exact mass detection, reducing considerably the possibilities of isobaric interferences. Previous to analysis, a solid phase extraction (SPE) step is used for purification and preconcentration. After DNS derivatization, samples are submitted to ultra high-performance liquid chromatography coupled with heated electrospray ionisation and the Q-Exactive mass spectrometer (UHPLC-HESI-HRMS). With an internal calibration using isotopically-labeled DAB-D3, the method was validated with good linearity (R (2)  > 0.998), and method limits of detection and quantification (MLD and MLQ) for target compounds ranged from 0.007 to 0.01 μg L(-1) and from 0.02 to 0.04 μg L(-1), respectively. Accuracy and within-day/between-days variation coefficients were below 15%. SPE recovery values ranged between 86 and 103%, and matrix effects recovery values ranged between 75 and 96%. The developed analytical method was successfully validated with 12 different lakes samples, and concentrations were found ranging between 0.009 and 0.3 μg L(-1) except for STX which was not found in any sample.

  19. Direct determination of acrylamide in food by gas chromatography-high-resolution time-of-flight mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Dunovska, Lenka [Institute of Chemical Technology, Department of Food Chemistry and Analysis, Technicka 3, 166 28 Prague 6 (Czech Republic); Cajka, Tomas [Institute of Chemical Technology, Department of Food Chemistry and Analysis, Technicka 3, 166 28 Prague 6 (Czech Republic); Hajslova, Jana [Institute of Chemical Technology, Department of Food Chemistry and Analysis, Technicka 3, 166 28 Prague 6 (Czech Republic)]. E-mail: jana.hajslova@vscht.cz; Holadova, Katerina [Institute of Chemical Technology, Department of Food Chemistry and Analysis, Technicka 3, 166 28 Prague 6 (Czech Republic)

    2006-09-25

    Simple and rapid gas chromatographic (GC) method employing a high-resolution time-of-flight mass analyzer that enables direct analysis (no derivatization) of acrylamide in various heat-processed foodstuffs has been developed and validated. Co-isolation of acrylamide precursors such as sugars and asparagine, constituting the risk of results overestimation due to additional formation of analyte in hot GC injector, is avoided by the extraction with n-propanol followed by solvent exchange to acetonitrile (MeCN). Introduction of a novel purification strategy, dispersive solid phase extraction, based on addition of primary-secondary amine (PSA) sorbent into deffated extract in MeCN, provides a significant reduction of some abundant matrix co-extracts (mainly free fatty acids). Isotope dilution technique (d{sub 3}-acrylamide as an internal standard) is employed for compensation of potential target analyte losses and/or matrix-inducted chromatographic response enhancement. Limits of quantifications (LOQs) ranged between 15 and 40 {mu}g kg{sup -1} and recoveries were between 97 and 108% depending on the examined food matrix. The repeatability of measurements (expressed as relative standard deviation, R.S.D.) was as low as 1.9% for potato crisps containing acrylamide at a level of 1 mg kg{sup -1}. Slightly higher values (R.S.D. < 4.0%) were achieved for breakfast cereals and crisp bread with approximately 10 times lower content of this processing contaminant. Trueness of results generated by this new method was demonstrated via FAPAS[reg] (Food Analysis Performance Assessment Scheme) interlaboratory proficiency tests.

  20. [Uncertainty evaluation of the determination of toxic equivalent quantity of polychlorinated dibenzo-p-dioxins and dibenzofurans in soil by isotope dilution high resolution gas chromatography and high resolution mass spectrometry].

    Science.gov (United States)

    Du, Bing; Liu Aimin; Huang, Yeru

    2014-09-01

    Polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) in soil samples were analyzed by isotope dilution method with high resolution gas chromatography and high resolution mass spectrometry (ID-HRGC/HRMS), and the toxic equivalent quantity (TEQ) were calculated. The impacts of major source of measurement uncertainty are discussed, and the combined relative standard uncertainties were calculated for each 2, 3, 7, 8 substituted con- gener. Furthermore, the concentration, combined uncertainty and expanded uncertainty for TEQ of PCDD/Fs in a soil sample in I-TEF, WHO-1998-TEF and WHO-2005-TEF schemes are provided as an example. I-TEF, WHO-1998-TEF and WHO-2005-TEF are the evaluation schemes of toxic equivalent factor (TEF), and are all currently used to describe 2,3,7,8 sub- stituted relative potencies.

  1. Determination of sulfur in bovine serum albumin and L-cysteine using high-resolution continuum source molecular absorption spectrometry of the CS molecule

    Science.gov (United States)

    Andrade-Carpente, Eva; Peña-Vázquez, Elena; Bermejo-Barrera, Pilar

    2016-08-01

    In this study, the content of sulfur in bovine serum albumin and L-cysteine was determined using high-resolution continuum source molecular absorption spectrometry of the CS molecule, generated in a reducing air-acetylene flame. Flame conditions (height above the burner, measurement time) were optimized using a 3.0% (v/v) sulfuric acid solution. A microwave lab station (Ethos Plus MW) was used for the digestion of both compounds. During the digestion step, sulfur was converted to sulfate previous to the determination. Good repeatability (4-10%) and analytical recovery (91-106%) was obtained.

  2. A new approach for the determination of sulphur in food samples by high-resolution continuum source flame atomic absorption spectrometer.

    Science.gov (United States)

    Ozbek, N; Baysal, A

    2015-02-01

    The new approach for the determination of sulphur in foods was developed, and the sulphur concentrations of various fresh and dried food samples determined using a high-resolution continuum source flame atomic absorption spectrometer with an air/acetylene flame. The proposed method was optimised and the validated using standard reference materials, and certified values were found to be within the 95% confidence interval. The sulphur content of foods ranged from less than the LOD to 1.5mgg(-1). The method is accurate, fast, simple and sensitive. Copyright © 2014 Elsevier Ltd. All rights reserved.

  3. Tunneling Splittings in Vibronic Structure of CH_3F^+ ( X^2E): Studied by High Resolution Photoelectron Spectra and AB Initio Theoretical Method

    Science.gov (United States)

    Mo, Yuxiang; Gao, Shuming; Dai, Zuyang; Li, Hua

    2013-06-01

    We report a combined experimental and theoretical study on the vibronic structure of CH_3F^+. The results show that the tunneling splittings of vibrational energy levels occur in CH_3F^+ due to the Jahn-Teller effect. Experimentally, we have measured a high resolution ZEKE spectrum of CH_3F up to 3500 cm^-^1 above the ground state. Theoretically, we performed an ab initio calculation based on the diabatic model. The adiabatic potential energy surfaces (APES) of CH_3F^+ have been calculated at the MRCI/CAS/avq(t)z level and expressed by Taylor expansions with normal coordinates as variables. The energy gradients for the lower and upper APES, the derivative couplings between them and also the energies of the APES have been used to determine the coefficients in the Taylor expansion. The spin-vibronic energy levels have been calculated by accounting all six vibrational modes and their couplings. The experimental ZEKE spectra were assigned based on the theoretical calculations. W. Domcke, D. R. Yarkony, and H. Köpple (Eds.), Conical Intersections: Eletronic Structure, Dynamics and Spectroscopy (World Scientific, Singapore, 2004). M. S. Schuurman, D. E. Weinberg, and D. R. Yarkony, J. Chem. Phys. 127, 104309 (2007).

  4. High-Resolution Mapping of Chromatin Conformation in Cardiac Myocytes Reveals Structural Remodeling of the Epigenome in Heart Failure

    NARCIS (Netherlands)

    M. Rosa-Garrido (Manuel); Chapski, D.J. (Douglas J.); Schmitt, A.D. (Anthony D.); Kimball, T.H. (Todd H.); Karbassi, E. (Elaheh); Monte, E. (Emma); Balderas, E. (Enrique); Pellegrini, M. (Matteo); Shih, T.-T. (Tsai-Ting); Soehalim, E. (Elizabeth); D.A. Liem (David); Ping, P. (Peipei); N.J. Galjart (Niels); Ren, S. (Shuxun); Wang, Y. (Yibin); Ren, B. (Bing); Vondriska, T.M. (Thomas M.)

    2017-01-01

    textabstractBACKGROUND: Cardiovascular disease is associated with epigenomic changes in the heart; however, the endogenous structure of cardiac myocyte chromatin has never been determined.METHODS: To investigate the mechanisms of epigenomic function in the heart, genome-wide chromatin conformation

  5. High-resolution crystal structure of Streptococcus pyogenes β-NAD{sup +} glycohydrolase in complex with its endogenous inhibitor IFS reveals a highly water-rich interface

    Energy Technology Data Exchange (ETDEWEB)

    Yoon, Ji Young; An, Doo Ri; Yoon, Hye-Jin [Seoul National University, Seoul 151-747 (Korea, Republic of); Kim, Hyoun Sook [Seoul National University, Seoul 151-747 (Korea, Republic of); Seoul National University, Seoul 151-742 (Korea, Republic of); Lee, Sang Jae [Seoul National University, Seoul 151-742 (Korea, Republic of); Im, Ha Na; Jang, Jun Young [Seoul National University, Seoul 151-747 (Korea, Republic of); Suh, Se Won, E-mail: sewonsuh@snu.ac.kr [Seoul National University, Seoul 151-747 (Korea, Republic of); Seoul National University, Seoul 151-747 (Korea, Republic of)

    2013-11-01

    The crystal structure of the complex between the C-terminal domain of Streptococcus pyogenes β-NAD{sup +} glycohydrolase and an endogenous inhibitor for SPN was determined at 1.70 Å. It reveals that the interface between the two proteins is highly rich in water molecules. One of the virulence factors produced by Streptococcus pyogenes is β-NAD{sup +} glycohydrolase (SPN). S. pyogenes injects SPN into the cytosol of an infected host cell using the cytolysin-mediated translocation pathway. As SPN is toxic to bacterial cells themselves, S. pyogenes possesses the ifs gene that encodes an endogenous inhibitor for SPN (IFS). IFS is localized intracellularly and forms a complex with SPN. This intracellular complex must be dissociated during export through the cell envelope. To provide a structural basis for understanding the interactions between SPN and IFS, the complex was overexpressed between the mature SPN (residues 38–451) and the full-length IFS (residues 1–161), but it could not be crystallized. Therefore, limited proteolysis was used to isolate a crystallizable SPN{sub ct}–IFS complex, which consists of the SPN C-terminal domain (SPN{sub ct}; residues 193–451) and the full-length IFS. Its crystal structure has been determined by single anomalous diffraction and the model refined at 1.70 Å resolution. Interestingly, our high-resolution structure of the complex reveals that the interface between SPN{sub ct} and IFS is highly rich in water molecules and many of the interactions are water-mediated. The wet interface may facilitate the dissociation of the complex for translocation across the cell envelope.

  6. High-resolution crystal structure of Streptococcus pyogenes β-NAD+ glycohydrolase in complex with its endogenous inhibitor IFS reveals a highly water-rich interface

    International Nuclear Information System (INIS)

    Yoon, Ji Young; An, Doo Ri; Yoon, Hye-Jin; Kim, Hyoun Sook; Lee, Sang Jae; Im, Ha Na; Jang, Jun Young; Suh, Se Won

    2013-01-01

    The crystal structure of the complex between the C-terminal domain of Streptococcus pyogenes β-NAD + glycohydrolase and an endogenous inhibitor for SPN was determined at 1.70 Å. It reveals that the interface between the two proteins is highly rich in water molecules. One of the virulence factors produced by Streptococcus pyogenes is β-NAD + glycohydrolase (SPN). S. pyogenes injects SPN into the cytosol of an infected host cell using the cytolysin-mediated translocation pathway. As SPN is toxic to bacterial cells themselves, S. pyogenes possesses the ifs gene that encodes an endogenous inhibitor for SPN (IFS). IFS is localized intracellularly and forms a complex with SPN. This intracellular complex must be dissociated during export through the cell envelope. To provide a structural basis for understanding the interactions between SPN and IFS, the complex was overexpressed between the mature SPN (residues 38–451) and the full-length IFS (residues 1–161), but it could not be crystallized. Therefore, limited proteolysis was used to isolate a crystallizable SPN ct –IFS complex, which consists of the SPN C-terminal domain (SPN ct ; residues 193–451) and the full-length IFS. Its crystal structure has been determined by single anomalous diffraction and the model refined at 1.70 Å resolution. Interestingly, our high-resolution structure of the complex reveals that the interface between SPN ct and IFS is highly rich in water molecules and many of the interactions are water-mediated. The wet interface may facilitate the dissociation of the complex for translocation across the cell envelope

  7. Determining the Accuracy of Paleomagnetic Remanence and High-Resolution Chronostratigraphy for Sedimentary Rocks using Rock Magnetics

    Science.gov (United States)

    Kodama, K. P.

    2017-12-01

    The talk will consider two broad topics in rock magnetism and paleomagnetism: the accuracy of paleomagnetic remanence and the use of rock magnetics to measure geologic time in sedimentary sequences. The accuracy of the inclination recorded by sedimentary rocks is crucial to paleogeographic reconstructions. Laboratory compaction experiments show that inclination shallows on the order of 10˚-15˚. Corrections to the inclination can be made using the effects of compaction on the directional distribution of secular variation recorded by sediments or the anisotropy of the magnetic grains carrying the ancient remanence. A summary of all the compaction correction studies as of 2012 shows that 85% of sedimentary rocks studied have enjoyed some amount of inclination shallowing. Future work should also consider the effect of grain-scale strain on paleomagnetic remanence. High resolution chronostratigraphy can be assigned to a sedimentary sequence using rock magnetics to detect astronomically-forced climate cycles. The power of the technique is relatively quick, non-destructive measurements, the objective identification of the cycles compared to facies interpretations, and the sensitivity of rock magnetics to subtle changes in sedimentary source. An example of this technique comes from using rock magnetics to identify astronomically-forced climate cycles in three globally distributed occurrences of the Shuram carbon isotope excursion. The Shuram excursion may record the oxidation of the world ocean in the Ediacaran, just before the Cambrian explosion of metazoans. Using rock magnetic cyclostratigraphy, the excursion is shown to have the same duration (8-9 Myr) in southern California, south China and south Australia. Magnetostratigraphy of the rocks carrying the excursion in California and Australia shows a reversed to normal geomagnetic field polarity transition at the excursion's nadir, thus supporting the synchroneity of the excursion globally. Both results point to a

  8. High-resolution He beam scattering as a tool for the investigation of the structural and dynamical properties of surface soliton dislocations

    International Nuclear Information System (INIS)

    El-Batanouny, M.; Martini, K.M.

    1986-01-01

    We discuss the applicability of high-resolution-He-beam/surface scattering to the investigation of the structural and dynamic properties of soliton-like surface misfit dislocations and associated phase transitions. We present evidence, based on recent He diffraction measurements, for the existence of double-sine-Gordon soliton-like dislocations on the reconstructed Au(111) surface. 18 refs., 3 figs., 1 tab

  9. High resolution solar observations

    International Nuclear Information System (INIS)

    Title, A.

    1985-01-01

    Currently there is a world-wide effort to develop optical technology required for large diffraction limited telescopes that must operate with high optical fluxes. These developments can be used to significantly improve high resolution solar telescopes both on the ground and in space. When looking at the problem of high resolution observations it is essential to keep in mind that a diffraction limited telescope is an interferometer. Even a 30 cm aperture telescope, which is small for high resolution observations, is a big interferometer. Meter class and above diffraction limited telescopes can be expected to be very unforgiving of inattention to details. Unfortunately, even when an earth based telescope has perfect optics there are still problems with the quality of its optical path. The optical path includes not only the interior of the telescope, but also the immediate interface between the telescope and the atmosphere, and finally the atmosphere itself

  10. Determination of 241Am in sediments by isotope dilution high resolution inductively coupled plasma mass spectrometry (ID HR ICP-MS).

    Science.gov (United States)

    Agarande, M; Benzoubir, S; Bouisset, P; Calmet, D

    2001-08-01

    Trace levels (pg kg(-1)) of 241Am in sediments were determined by isotope dilution high resolution inductively coupled plasma mass spectrometry (ID HR ICP-MS) using a microconcentric nebulizer. 241Am was isolated from major elements like Ca and Fe by different selective precipitations. In further steps. Am was first separated from other transuranic elements and purified by anion exchange and extraction chromatography prior to the mass spectrometric measurements. The ID HR ICP-MS results are compared with isotope dilution alpha spectrometry.

  11. Dislocation density and Burgers vector population in fiber-textured Ni thin films determined by high-resolution X-ray line profile analysis

    DEFF Research Database (Denmark)

    Csiszár, Gábor; Pantleon, Karen; Alimadadi, Hossein

    2012-01-01

    distribution are determined by high-resolution X-ray diffraction line profile analysis. The substructure parameters are correlated with the strength of the films by using the combined Taylor and Hall-Petch relations. The convolutional multiple whole profile method is used to obtain the substructure parameters......Nanocrystalline Ni thin films have been produced by direct current electrodeposition with different additives and current density in order to obtain 〈100〉, 〈111〉 and 〈211〉 major fiber textures. The dislocation density, the Burgers vector population and the coherently scattering domain size...

  12. Identification and accurate quantification of structurally related peptide impurities in synthetic human C-peptide by liquid chromatography-high resolution mass spectrometry.

    Science.gov (United States)

    Li, Ming; Josephs, Ralf D; Daireaux, Adeline; Choteau, Tiphaine; Westwood, Steven; Wielgosz, Robert I; Li, Hongmei

    2018-06-04

    Peptides are an increasingly important group of biomarkers and pharmaceuticals. The accurate purity characterization of peptide calibrators is critical for the development of reference measurement systems for laboratory medicine and quality control of pharmaceuticals. The peptides used for these purposes are increasingly produced through peptide synthesis. Various approaches (for example mass balance, amino acid analysis, qNMR, and nitrogen determination) can be applied to accurately value assign the purity of peptide calibrators. However, all purity assessment approaches require a correction for structurally related peptide impurities in order to avoid biases. Liquid chromatography coupled to high resolution mass spectrometry (LC-hrMS) has become the key technique for the identification and accurate quantification of structurally related peptide impurities in intact peptide calibrator materials. In this study, LC-hrMS-based methods were developed and validated in-house for the identification and quantification of structurally related peptide impurities in a synthetic human C-peptide (hCP) material, which served as a study material for an international comparison looking at the competencies of laboratories to perform peptide purity mass fraction assignments. More than 65 impurities were identified, confirmed, and accurately quantified by using LC-hrMS. The total mass fraction of all structurally related peptide impurities in the hCP study material was estimated to be 83.3 mg/g with an associated expanded uncertainty of 3.0 mg/g (k = 2). The calibration hierarchy concept used for the quantification of individual impurities is described in detail. Graphical abstract ᅟ.

  13. High resolution X-ray structures of mouse major urinary protein nasal isoform in complex with pheromones

    Energy Technology Data Exchange (ETDEWEB)

    Perez-Miller, Samantha; Zou, Qin; Novotny, Milos V.; Hurley, Thomas D. (Indiana-Med); (Indiana)

    2010-09-07

    In mice, the major urinary proteins (MUP) play a key role in pheromonal communication by binding and transporting semiochemicals. MUP-IV is the only isoform known to be expressed in the vomeronasal mucosa. In comparison with the MUP isoforms that are abundantly excreted in the urine, MUP-IV is highly specific for the male mouse pheromone 2-sec-butyl-4,5-dihydrothiazole (SBT). To examine the structural basis of this ligand preference, we determined the X-ray crystal structure of MUP-IV bound to three mouse pheromones: SBT, 2,5-dimethylpyrazine, and 2-heptanone. We also obtained the structure of MUP-IV with 2-ethylhexanol bound in the cavity. These four structures show that relative to the major excreted MUP isoforms, three amino acid substitutions within the binding calyx impact ligand coordination. The F103 for A along with F54 for L result in a smaller cavity, potentially creating a more closely packed environment for the ligand. The E118 for G substitution introduces a charged group into a hydrophobic environment. The sidechain of E118 is observed to hydrogen bond to polar groups on all four ligands with nearly the same geometry as seen for the water-mediated hydrogen bond network in the MUP-I and MUP-II crystal structures. These differences in cavity size and interactions between the protein and ligand are likely to contribute to the observed specificity of MUP-IV.

  14. A postprocessing method based on high-resolution spectral estimation for FDTD calculation of phononic band structures

    Energy Technology Data Exchange (ETDEWEB)

    Su Xiaoxing, E-mail: xxsu@bjtu.edu.c [School of Electronic and Information Engineering, Beijing Jiaotong University, Beijing 100044 (China); Li Jianbao; Wang Yuesheng [Institute of Engineering Mechanics, Beijing Jiaotong University, Beijing 100044 (China)

    2010-05-15

    If the energy bands of a phononic crystal are calculated by the finite difference time domain (FDTD) method combined with the fast Fourier transform (FFT), good estimation of the eigenfrequencies can only be ensured by the postprocessing of sufficiently long time series generated by a large number of FDTD iterations. In this paper, a postprocessing method based on the high-resolution spectral estimation via the Yule-Walker method is proposed to overcome this difficulty. Numerical simulation results for three-dimensional acoustic and two-dimensional elastic systems show that, compared with the classic FFT-based postprocessing method, the proposed method can give much better estimation of the eigenfrequencies when the FDTD is run with relatively few iterations.

  15. A postprocessing method based on high-resolution spectral estimation for FDTD calculation of phononic band structures

    International Nuclear Information System (INIS)

    Su Xiaoxing; Li Jianbao; Wang Yuesheng

    2010-01-01

    If the energy bands of a phononic crystal are calculated by the finite difference time domain (FDTD) method combined with the fast Fourier transform (FFT), good estimation of the eigenfrequencies can only be ensured by the postprocessing of sufficiently long time series generated by a large number of FDTD iterations. In this paper, a postprocessing method based on the high-resolution spectral estimation via the Yule-Walker method is proposed to overcome this difficulty. Numerical simulation results for three-dimensional acoustic and two-dimensional elastic systems show that, compared with the classic FFT-based postprocessing method, the proposed method can give much better estimation of the eigenfrequencies when the FDTD is run with relatively few iterations.

  16. Strontium mono-chloride — A new molecule for the determination of chlorine using high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis

    Energy Technology Data Exchange (ETDEWEB)

    Pereira, Éderson R. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Welz, Bernhard, E-mail: w.bernardo@terra.com.br [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Lopez, Alfredo H.D.; Gois, Jefferson S. de; Caramori, Giovanni F. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Borges, Daniel L.G.; Carasek, Eduardo [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Andrade, Jailson B. de [Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil)

    2014-12-01

    A new method has been developed for the determination of chlorine in biological reference materials using high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) of the strontium mono-chloride (SrCl) molecule and direct solid sample analysis. The use of the SrCl molecule for high-temperature MAS was not described up to now in the literature. Preliminary time-dependent density functional theory calculations of the SrCl structure were carried out in order to obtain reasonable estimates of the absorption spectrum of the target molecule. The calculations, which were carried out at BHandHLyp/def2-QZVP level of theory, proved a very accurate and inexpensive way to get information about the spectrum of the SrCl molecule, which enabled us to perform the Cl determination with good sensitivity and specificity. The molecular absorption of the SrCl molecule has been measured using the wavelength at 635.862 nm, and zirconium and palladium have been evaluated as the chemical modifiers in order to increase the sensitivity of the gaseous SrCl molecule generated in the graphite furnace. The pyrolysis and vaporization temperatures were 600 °C and 2300 °C, respectively. Accuracy and precision of the method have been evaluated using biological certified reference materials of both animal and plant origins, showing good agreement with the informed and certified values. Limit of detection and characteristic mass were 1.0 and 2.2 ng, respectively. The results found using HR-CS GF MAS were in agreement (95% confidence level) compared to those obtained by electrothermal vaporization-inductively coupled plasma mass spectrometry. - Highlights: • The spectrum of the SrCl molecule was calculated on a theoretical basis and found very close to the predicted wavelength. • It is the first time that the spectrum of the SrCl molecule is described and used analytically for the determination of Cl. • No spectral interferences were observed as the

  17. Investigation of spectral interferences in the determination of lead in fertilizers and limestone samples using high-resolution continuum source graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Borges, Aline R. [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq — INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Becker, Emilene M.; François, Luciane L.; Jesus, Alexandre de [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Vale, Maria Goreti R. [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq — INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Welz, Bernhard [Instituto Nacional de Ciência e Tecnologia do CNPq — INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Dessuy, Morgana B., E-mail: mbdessuy@ufrgs.br [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Andrade, Jailson B. de [Instituto Nacional de Ciência e Tecnologia do CNPq — INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil)

    2014-11-01

    In the present work, spectral interferences on the determination of lead in fertilizer and limestone samples were investigated using high-resolution continuum source graphite furnace atomic absorption spectrometry at the main analytical lines: 217.001 and 283.306 nm. For these investigations, samples were introduced into the furnace as slurry together with a mixture of Pd and Mg as chemical modifier. Spectral interferences were observed for some samples at both analytical lines. In order to verify whether a wet digestion procedure would avoid these interferences, a reference method for wet digestion of fertilizers was employed as an alternative sample preparation procedure. However, the same interferences were also observed in the digested samples. In order to identify and eliminate the fine-structured background using a least-squares background correction, reference spectra were generated using the combination of different species. The use of the latter technique allowed the elimination of spectral interferences for most of the investigated samples, making possible the determination of lead in fertilizer and limestone samples free of interferences. The best results were found using a reference spectrum of NH{sub 4}H{sub 2}PO{sub 4} at 217.001 nm, and a mixture of H{sub 2}SO{sub 4} + Ca and HNO{sub 3} + Ca at the 283.306 nm line. The accuracy of the method was evaluated using a certified reference material “Trace Elements in Multi-Nutrient Fertilizer”. Similar results were obtained using line source graphite furnace atomic absorption spectrometry with Zeeman-effect background correction, indicating that the latter technique was also capable to correct the spectral interferences, at least in part. - Highlights: • Spectral interferences on the determination of lead in fertilizers and limestone. • The analytical lines at 217.001 nm and 283.306 nm using HR-CS GF AAS. • Various combinations of compounds were used to create reference spectra. • LSBC

  18. Ultra-high resolution protein crystallography

    International Nuclear Information System (INIS)

    Takeda, Kazuki; Hirano, Yu; Miki, Kunio

    2010-01-01

    Many protein structures have been determined by X-ray crystallography and deposited with the Protein Data Bank. However, these structures at usual resolution (1.5< d<3.0 A) are insufficient in their precision and quantity for elucidating the molecular mechanism of protein functions directly from structural information. Several studies at ultra-high resolution (d<0.8 A) have been performed with synchrotron radiation in the last decade. The highest resolution of the protein crystals was achieved at 0.54 A resolution for a small protein, crambin. In such high resolution crystals, almost all of hydrogen atoms of proteins and some hydrogen atoms of bound water molecules are experimentally observed. In addition, outer-shell electrons of proteins can be analyzed by the multipole refinement procedure. However, the influence of X-rays should be precisely estimated in order to derive meaningful information from the crystallographic results. In this review, we summarize refinement procedures, current status and perspectives for ultra high resolution protein crystallography. (author)

  19. High resolution NMR theory and chemical applications

    CERN Document Server

    Becker, Edwin D

    1999-01-01

    High Resolution NMR provides a broad treatment of the principles and theory of nuclear magnetic resonance (NMR) as it is used in the chemical sciences. It is written at an "intermediate" level, with mathematics used to augment, rather than replace, clear verbal descriptions of the phenomena. The book is intended to allow a graduate student, advanced undergraduate, or researcher to understand NMR at a fundamental level, and to see illustrations of the applications of NMR to the determination of the structure of small organic molecules and macromolecules, including proteins. Emphasis is on the study of NMR in liquids, but the treatment also includes high resolution NMR in the solid state and the principles of NMR imaging and localized spectroscopy. Careful attention is given to developing and interrelating four approaches - steady state energy levels, the rotating vector picture, the density matrix, and the product operator formalism. The presentation is based on the assumption that the reader has an acquaintan...

  20. High-resolution electron microscopic evidence for the filamentous structure of the cyst wall in Giardia muris and Giardia duodenalis.

    Science.gov (United States)

    Erlandsen, S L; Bemrick, W J; Pawley, J

    1989-10-01

    High-resolution morphological studies of the cyst wall of Giardia spp. were performed using low-voltage scanning electron microscopy (LVSEM) and transmission electron microscopy (TEM). The cyst wall was composed of membranous and filamentous layers. The membranous layer consisted of an inner and an outer cyst membrane separated by a thin layer of cytoplasm. The filamentous layer contained individual filaments that ranged from 7 to 20 nm in diameter when measured by LVSEM, formed a dense meshwork with branches or interconnections, and were occasionally arranged on the surface in whorled patterns. Cysts of Giardia muris from mice, Giardia duodenalis from dogs, pigs, voles, beavers, muskrats, and humans, and Giardia psittaci from a bird (parakeet), possessed an essentially identical wall composed of filaments. Inducement of excystation in viable Giardia cysts produced a dramatic increase in the interfilament spacing over an entire cyst, but none was observed in heat-killed or chemically fixed control cysts. These results demonstrated that the cyst wall of Giardia spp. was composed of a complex arrangement of filaments, presumably formed during the process of encystment.

  1. Optimization of a method by liquid chromatography of high resolution to determine residues of ethilenthiourea in samples of tomato

    International Nuclear Information System (INIS)

    Mora, D.; Rodriguez, O.M.

    2002-01-01

    A method was optimized to determine the present residues of ethilenthiourea in samples of tomatoes. The method consisted of three stages: a extraction of ultrasonic bath with methanol; a cleaning of the extract through a glass column of 11 mm of diameter stuffed with 2,5 g of neutral aluminium's mixture and activated coal (97,5:2,5) and 2,5 g of pure-neutral aluminium, it is dissolved with 250 ml of methanol. The third stage was of quantification by HPLC in a C 18 ' column with a methanol and water mixture (90:10) like a mobile phase to an flow of 2,0 ml/min. and with UV detection to 232 nm. The retention's time under theses conditions was of 2,15 minutes. The merit's parameters of the method were determined, proving and lineal sphere between 1,0 and 28,0 (g/ml of ETU; some quantification and detection limits have been calculated by the method of Hubaux and Vos (22) of 0,153 and 0,306 mg/ml respectively and a recuperation of 84%. (Author) [es

  2. High-resolution crystal structure of a polyextreme GH43 glycosidase from Halothermothrix orenii with α-l-arabinofuranosidase activity

    International Nuclear Information System (INIS)

    Hassan, Noor; Kori, Lokesh D.; Gandini, Rosaria; Patel, Bharat K. C.; Divne, Christina; Tan, Tien Chye

    2015-01-01

    The crystal structure of the H. orenii glycosidase was determined by molecular replacement and refined at 1.10 Å resolution. A gene from the heterotrophic, halothermophilic marine bacterium Halothermothrix orenii has been cloned and overexpressed in Escherichia coli. This gene encodes the only glycoside hydrolase of family 43 (GH43) produced by H. orenii. The crystal structure of the H. orenii glycosidase was determined by molecular replacement and refined at 1.10 Å resolution. As for other GH43 members, the enzyme folds as a five-bladed β-propeller. The structure features a metal-binding site on the propeller axis, near the active site. Based on thermal denaturation data, the H. orenii glycosidase depends on divalent cations in combination with high salt for optimal thermal stability against unfolding. A maximum melting temperature of 76°C was observed in the presence of 4 M NaCl and Mn 2+ at pH 6.5. The gene encoding the H. orenii GH43 enzyme has previously been annotated as a putative α-l-arabinofuranosidase. Activity was detected with p-nitrophenyl-α-l-arabinofuranoside as a substrate, and therefore the name HoAraf43 was suggested for the enzyme. In agreement with the conditions for optimal thermal stability against unfolding, the highest arabinofuranosidase activity was obtained in the presence of 4 M NaCl and Mn 2+ at pH 6.5, giving a specific activity of 20–36 µmol min −1 mg −1 . The active site is structurally distinct from those of other GH43 members, including arabinanases, arabinofuranosidases and xylanases. This probably reflects the special requirements for degrading the unique biomass available in highly saline aqueous ecosystems, such as halophilic algae and halophytes. The amino-acid distribution of HoAraf43 has similarities to those of mesophiles, thermophiles and halophiles, but also has unique features, for example more hydrophobic amino acids on the surface and fewer buried charged residues

  3. High-resolution crystal structure of a polyextreme GH43 glycosidase from Halothermothrix orenii with α-l-arabinofuranosidase activity

    Energy Technology Data Exchange (ETDEWEB)

    Hassan, Noor [KTH Royal Institute of Technology, Stockholm (Sweden); Karolinska Institutet, Stockholm (Sweden); Kori, Lokesh D. [Griffith University, Brisbane, QLD 4111 (Australia); Baylor College of Medicine, Houston, TX 77030 (United States); Gandini, Rosaria [KTH Royal Institute of Technology, Stockholm (Sweden); Karolinska Institutet, Stockholm (Sweden); Patel, Bharat K. C. [Griffith University, Brisbane, QLD 4111 (Australia); Divne, Christina; Tan, Tien Chye, E-mail: tantc@kth.se [KTH Royal Institute of Technology, Stockholm (Sweden); Karolinska Institutet, Stockholm (Sweden)

    2015-02-19

    The crystal structure of the H. orenii glycosidase was determined by molecular replacement and refined at 1.10 Å resolution. A gene from the heterotrophic, halothermophilic marine bacterium Halothermothrix orenii has been cloned and overexpressed in Escherichia coli. This gene encodes the only glycoside hydrolase of family 43 (GH43) produced by H. orenii. The crystal structure of the H. orenii glycosidase was determined by molecular replacement and refined at 1.10 Å resolution. As for other GH43 members, the enzyme folds as a five-bladed β-propeller. The structure features a metal-binding site on the propeller axis, near the active site. Based on thermal denaturation data, the H. orenii glycosidase depends on divalent cations in combination with high salt for optimal thermal stability against unfolding. A maximum melting temperature of 76°C was observed in the presence of 4 M NaCl and Mn{sup 2+} at pH 6.5. The gene encoding the H. orenii GH43 enzyme has previously been annotated as a putative α-l-arabinofuranosidase. Activity was detected with p-nitrophenyl-α-l-arabinofuranoside as a substrate, and therefore the name HoAraf43 was suggested for the enzyme. In agreement with the conditions for optimal thermal stability against unfolding, the highest arabinofuranosidase activity was obtained in the presence of 4 M NaCl and Mn{sup 2+} at pH 6.5, giving a specific activity of 20–36 µmol min{sup −1} mg{sup −1}. The active site is structurally distinct from those of other GH43 members, including arabinanases, arabinofuranosidases and xylanases. This probably reflects the special requirements for degrading the unique biomass available in highly saline aqueous ecosystems, such as halophilic algae and halophytes. The amino-acid distribution of HoAraf43 has similarities to those of mesophiles, thermophiles and halophiles, but also has unique features, for example more hydrophobic amino acids on the surface and fewer buried charged residues.

  4. Comparison of laser fluorimetry, high resolution gamma-ray spectrometry and neutron activation analysis techniques for determination of uranium content in soil samples

    International Nuclear Information System (INIS)

    Ghods, A.; Asgharizadeh, F.; Salimi, B.; Abbasi, A.

    2004-01-01

    Much more concern is given nowadays for exposure of the world population to natural radiation especially to uranium since 57% of that exposure is due to radon-222, which is a member of uranium decay series. Most of the methods used for uranium determination is low concentration require either tedious separation and preconcentration or the accessibility to special instrumentation for detection of uranium at this low level. this study compares three techniques and methods for uranium analysis among different soil sample with variable uranium contents. Two of these techniques, neutron activation analysis and high resolution gamma-ray spectrometry , are non-destructive while the other, laser fluorimetry is done via chemical extraction of uranium. Analysis of standard materials is done also to control the quality and accuracy of the work. In spite of having quite variable ranges of detection limit, results obtained by high resolution gamma-ray spectrometry based on the assumption of having secular equilibrium between uranium and its daughters, which causes deviation whenever this condition was missed. For samples with reasonable uranium content, neutron activation analysis would be a rapid and reliable technique, while for low uranium content laser fluorimetry would be the most appropriate and accurate technique

  5. Atrazine determination and some of their degradation products in soils and water by means of liquid chromatography of high resolution

    International Nuclear Information System (INIS)

    Olarte, Israel; Guerrero, Jairo Arturo; Fuentes, Cilia

    1999-01-01

    This study describes the validation of the analytical method for the simultaneous determination of atrazine (AT) and its metabolites deisopropylatrazine (DIA) and deetylatrazine (DEA) in irrigation water and agricultural soil. Field samples were collected in a cornfield located in Saldana, (Tolima, Colombia) and treated with 2.9 kg. a.i/ha of atrazine. Samples were collected for three months starting after herbicide treatment. The quantitative determination of the compounds of interest was carried out by HPLC with UV detection in a lichrospher RP-18 column of 125 x 4 mm, 5 , using a gradient of acetonitrile-water as mobile phase. The compounds were extracted from the water matrix and concentrated using solid phase extraction (SPE). From the soil matrix the compounds were extracted with methanol followed by a clean up with dichloromethane and buffer phosphate 0.01 M, pH 10.0. Calibration curves were linear over a concentration range of 6 /L- 30 /L in water and 30 /kg - 200 /kg in soil. The method is specific and sensitive with a detection limit of 0.6 /L for DIA, 0.7 /L for DIA and AT in water, 2.0 /kg for DIA, 2.3 /kg for DIA and AT in soil. Recovery experiments were performed with irrigation water samples yielding average recoveries between 80-100% and performed on soil samples yielding average recoveries between 45-65%. DIA and DEA were not detected in neither water nor soil field samples, but atrazine was found in water after the first month following herbicide application at a concentration level of 5,8 /L, and in soil AT a concentration level of 97 /kg - at the second month, no atrazine was found in water but 42 /kg were detected in soil

  6. High resolution data acquisition

    Science.gov (United States)

    Thornton, Glenn W.; Fuller, Kenneth R.

    1993-01-01

    A high resolution event interval timing system measures short time intervals such as occur in high energy physics or laser ranging. Timing is provided from a clock (38) pulse train (37) and analog circuitry (44) for generating a triangular wave (46) synchronously with the pulse train (37). The triangular wave (46) has an amplitude and slope functionally related to the time elapsed during each clock pulse in the train. A converter (18, 32) forms a first digital value of the amplitude and slope of the triangle wave at the start of the event interval and a second digital value of the amplitude and slope of the triangle wave at the end of the event interval. A counter (26) counts the clock pulse train (37) during the interval to form a gross event interval time. A computer (52) then combines the gross event interval time and the first and second digital values to output a high resolution value for the event interval.

  7. Metabolism of clofibric acid in zebrafish embryos (Danio rerio) as determined by liquid chromatography-high resolution-mass spectrometry.

    Science.gov (United States)

    Brox, Stephan; Seiwert, Bettina; Haase, Nora; Küster, Eberhard; Reemtsma, Thorsten

    2016-01-01

    The zebrafish embryo (ZFE) is increasingly used in ecotoxicology research but detailed knowledge of its metabolic potential is still limited. This study focuses on the xenobiotic metabolism of ZFE at different life-stages using the pharmaceutical compound clofibric acid as study compound. Liquid chromatography with quadrupole-time-of-flight mass spectrometry (LC-QToF-MS) is used to detect and to identify the transformation products (TPs). In screening experiments, a total of 18 TPs was detected and structure proposals were elaborated for 17 TPs, formed by phase I and phase II metabolism. Biotransformation of clofibric acid by the ZFE involves conjugation with sulfate or glucuronic acid, and, reported here for the first time, with carnitine, taurine, and aminomethanesulfonic acid. Further yet unknown cyclization products were identified using non-target screening that may represent a new detoxification pathway. Sulfate containing TPs occurred already after 3h of exposure (7hpf), and from 48h of exposure (52hpf) onwards, all TPs were detected. The detection of these TPs indicates the activity of phase I and phase II enzymes already at early life-stages. Additionally, the excretion of one TP into the exposure medium was observed. The results of this study outline the high metabolic potential of the ZFE with respect to the transformation of xenobiotics. Similarities but also differences to other test systems were observed. Biotransformation of test chemicals in toxicity testing with ZFE may therefore need further consideration. Copyright © 2016 Elsevier Inc. All rights reserved.

  8. High resolution crystal structure of the Grb2 SH2 domain with a phosphopeptide derived from CD28.

    Directory of Open Access Journals (Sweden)

    Kunitake Higo

    Full Text Available Src homology 2 (SH2 domains play a critical role in cellular signal transduction. They bind to peptides containing phosphotyrosine (pY with various specificities that depend on the flanking amino-acid residues. The SH2 domain of growth-factor receptor-bound protein 2 (Grb2 specifically recognizes pY-X-N-X, whereas the SH2 domains in phosphatidylinositol 3-kinase (PI3K recognize pY-X-X-M. Binding of the pY site in CD28 (pY-M-N-M by PI3K and Grb2 through their SH2 domains is a key step that triggers the CD28 signal transduction for T cell activation and differentiation. In this study, we determined the crystal structure of the Grb2 SH2 domain in complex with a pY-containing peptide derived from CD28 at 1.35 Å resolution. The peptide was found to adopt a twisted U-type conformation, similar to, but distinct from type-I β-turn. In all previously reported crystal structures, the peptide bound to the Grb2 SH2 domains adopts a type-I β-turn conformation, except those with a proline residue at the pY+3 position. Molecular modeling also suggests that the same peptide bound to PI3K might adopt a very different conformation.

  9. High resolution crystal structure of the Grb2 SH2 domain with a phosphopeptide derived from CD28.

    Science.gov (United States)

    Higo, Kunitake; Ikura, Teikichi; Oda, Masayuki; Morii, Hisayuki; Takahashi, Jun; Abe, Ryo; Ito, Nobutoshi

    2013-01-01

    Src homology 2 (SH2) domains play a critical role in cellular signal transduction. They bind to peptides containing phosphotyrosine (pY) with various specificities that depend on the flanking amino-acid residues. The SH2 domain of growth-factor receptor-bound protein 2 (Grb2) specifically recognizes pY-X-N-X, whereas the SH2 domains in phosphatidylinositol 3-kinase (PI3K) recognize pY-X-X-M. Binding of the pY site in CD28 (pY-M-N-M) by PI3K and Grb2 through their SH2 domains is a key step that triggers the CD28 signal transduction for T cell activation and differentiation. In this study, we determined the crystal structure of the Grb2 SH2 domain in complex with a pY-containing peptide derived from CD28 at 1.35 Å resolution. The peptide was found to adopt a twisted U-type conformation, similar to, but distinct from type-I β-turn. In all previously reported crystal structures, the peptide bound to the Grb2 SH2 domains adopts a type-I β-turn conformation, except those with a proline residue at the pY+3 position. Molecular modeling also suggests that the same peptide bound to PI3K might adopt a very different conformation.

  10. Determination of the natural radioactivity levels in north west of Dukhan, Qatar using high-resolution gamma-ray spectrometry

    International Nuclear Information System (INIS)

    Al-Sulaiti, Huda; Nasir, Tabassum; Al Mugren, K.S.; Alkhomashi, N.; Al-Dahan, N.; Al-Dosari, M.; Bradley, D.A.; Bukhari, S.; Matthews, M.; Regan, P.H.; Santawamaitre, T.; Malain, D.; Habib, A.

    2012-01-01

    This study is aimed at the determination of the activity concentrations of naturally occuring and technologically enhanced levels of radiation in 34 representative soil samples that have been collected from an inshore oil field area which was found to have, in a previous study, the highest observed value of 226 Ra concentration among 129 soil samples. The activity concentrations of 238 U and 226 Ra have been inferred from gamma-ray transitions associated with their decay progenies and measured using a hyper-pure germanium detector. Details of the sample preparation and the gamma-ray spectroscopic analysis techniques are presented, together with the values of the activity concentrations associated with the naturally occuring radionuclide chains for all the samples collected from NW Dukhan. Discrete-line, gamma-ray energy transitions from spectral lines ranging in energy from ∼100 keV up to 2.6 MeV have been associated with characteristic decays of the various decay products within the 235.8 U and 232 Th radioactive decay chains. These data have been analyzed, under the assumption of secular equilibrium for the U and Th decay chains. Details of the sample preparation and the gamma-ray spectroscopic analysis techniques are presented. The weighted mean value of the activity concentrations of 226 Ra in one of the samples was found to be around a factor of 2 higher than the values obtained in the previous study and approximately a factor of 10 higher than the accepted worldwide average value of 35 Bq/kg. The weighted mean values of the activity concentrations of 232 Th and 40 K were also deduced and found to be within the worldwide average values of 30 and 400 Bq/kg, respectively. Our previous study reported a value of 201.9±1.5 Stat. ±13 Syst. Bq/kg for 226 Ra in one sample and further investigation in the current work determined a measured value for 226 Ra of 342.00±1.9 Stat. ±25 Syst. Bq/kg in a sample taken from the same locality. This is significantly higher

  11. Determination of the natural radioactivity levels in north west of Dukhan, Qatar using high-resolution gamma-ray spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Al-Sulaiti, Huda [Centre for Nuclear and Radiation Physics, Department of Physics, University of Surrey, Guildford GU2 7XH (United Kingdom); Radiation Protection and Chemicals Department, Ministry of Environment, P.O. Box 7634, Doha (Qatar); Nasir, Tabassum [Centre for Nuclear and Radiation Physics, Department of Physics, University of Surrey, Guildford GU2 7XH (United Kingdom); Department of Physics, Gomal University, D.I. Khan (Pakistan); Al Mugren, K S [Centre for Nuclear and Radiation Physics, Department of Physics, University of Surrey, Guildford GU2 7XH (United Kingdom); Physics Department, Faculty of Sciences, Princess Nora Bint Abdul Rahman University, Riyadh (Saudi Arabia); Alkhomashi, N [King Abdulaziz City of Science and Technology (KACST), P.O. Box 6086, Riyadh 11442 (Saudi Arabia); Al-Dahan, N [Centre for Nuclear and Radiation Physics, Department of Physics, University of Surrey, Guildford GU2 7XH (United Kingdom); Department of Physics, College of Science, University of Kerbala, Kerbala (Iraq); Al-Dosari, M [Radiation Protection and Chemicals Department, Ministry of Environment, P.O. Box 7634, Doha (Qatar); Bradley, D A [Centre for Nuclear and Radiation Physics, Department of Physics, University of Surrey, Guildford GU2 7XH (United Kingdom); Bukhari, S [Information Systems Management Department, Ministry of Environment, P.O. Box 7634, Doha (Qatar); Matthews, M [Centre of Environmental Health Engineering, Department of Civil Engineering, University of Surrey, Guildford GU2 7XH (United Kingdom); Regan, P H [Centre for Nuclear and Radiation Physics, Department of Physics, University of Surrey, Guildford GU2 7XH (United Kingdom); Santawamaitre, T [Radiation Protection and Chemicals Department, Ministry of Environment, P.O. Box 7634, Doha (Qatar); Malain, D; Habib, A [Centre for Nuclear and Radiation Physics, Department of Physics, University of Surrey, Guildford GU2 7XH (United Kingdom)

    2012-07-15

    This study is aimed at the determination of the activity concentrations of naturally occuring and technologically enhanced levels of radiation in 34 representative soil samples that have been collected from an inshore oil field area which was found to have, in a previous study, the highest observed value of {sup 226}Ra concentration among 129 soil samples. The activity concentrations of {sup 238}U and {sup 226}Ra have been inferred from gamma-ray transitions associated with their decay progenies and measured using a hyper-pure germanium detector. Details of the sample preparation and the gamma-ray spectroscopic analysis techniques are presented, together with the values of the activity concentrations associated with the naturally occuring radionuclide chains for all the samples collected from NW Dukhan. Discrete-line, gamma-ray energy transitions from spectral lines ranging in energy from {approx}100 keV up to 2.6 MeV have been associated with characteristic decays of the various decay products within the {sup 235.8}U and {sup 232}Th radioactive decay chains. These data have been analyzed, under the assumption of secular equilibrium for the U and Th decay chains. Details of the sample preparation and the gamma-ray spectroscopic analysis techniques are presented. The weighted mean value of the activity concentrations of {sup 226}Ra in one of the samples was found to be around a factor of 2 higher than the values obtained in the previous study and approximately a factor of 10 higher than the accepted worldwide average value of 35 Bq/kg. The weighted mean values of the activity concentrations of {sup 232}Th and {sup 40}K were also deduced and found to be within the worldwide average values of 30 and 400 Bq/kg, respectively. Our previous study reported a value of 201.9{+-}1.5{sub Stat.}{+-}13{sub Syst.} Bq/kg for {sup 226}Ra in one sample and further investigation in the current work determined a measured value for {sup 226}Ra of 342.00{+-}1.9{sub Stat.}{+-}25{sub Syst

  12. ANL high resolution injector

    International Nuclear Information System (INIS)

    Minehara, E.; Kutschera, W.; Hartog, P.D.; Billquist, P.

    1985-01-01

    The ANL (Argonne National Laboratory) high-resolution injector has been installed to obtain higher mass resolution and higher preacceleration, and to utilize effectively the full mass range of ATLAS (Argonne Tandem Linac Accelerator System). Preliminary results of the first beam test are reported briefly. The design and performance, in particular a high-mass-resolution magnet with aberration compensation, are discussed. 7 refs., 5 figs., 2 tabs

  13. Determination of polycyclic aromatic hydrocarbons and their nitrated derivatives in Diesel soot by gas chromatography and high resolution mass spectrometry

    International Nuclear Information System (INIS)

    Remberg, G.

    1998-11-01

    Periodical monitoring of the exposure levels towards chemical hazards is an important issue of occupational safety and health. Some constituents of diesel exhaust emissions, like polycyclic aromatic hydrocarbons and their nitrated derivatives, have attracted special attention due to their carcinogenic and partly mutagenic properties. Therefore, the present work focused on the development of new methodical aspects for the determination of these substances in diesel particulate matter. In the first stage of this study the essential gas chromatographic and mass spectrometric characteristics of 51 authentic PAH and NPAH single standards have been investigated. A retention index system on DB-5 type capillary columns has been established in order to facilitate the identification of these target compounds in complex matrices. Before choosing proper MID quantification ions the full scan (+)EI- and ECNCI-mass spectra of all standards were acquired. The GC-(+)EI-MS detection limits of three NPAH were determined with different mass spectrometric modes (i.e. LR/full scan, LR/MID and HR/MID), being in the range of a few picograms in the latter mode. The use of large volume injection in conjunction with a PTV for PAH/NPAH trace analysis was studied and optimized for an injection volume of up to nine microliters. Extraction of diesel soot with dichloromethane was performed in accordance with US EPA method 3545 by means of accelerated solvent extraction, which takes significantly less than one hour. Gas chromatographic investigations on such extracts with various detectors of different selectivity (i.e. FID, LRMS and HRMS) showed the exclusive capability of high mass spectral resolution (about R ∼10000) to differentiate between analytes and matrix components. On the basis of these preliminary results an operating procedure was proposed. Its key-elements are accelerated solvent extraction of the sample and analysis of the resulting solution by means of GC-(+)EI-HRMS followed by

  14. Determination of trace elements in Ethiopian, Vietnamese, and Japanese women using high-resolution IC-PMS.

    Science.gov (United States)

    Tekeste, Zinaye; Amare, Bemnet; Asfaw, Fanaye; Fantahun, Bereket; van Nguyen, Nhien; Nishikawa, Takeshi; Yabutani, Tomoki; Okayasu, Takako; Ota, Fusao; Kassu, Afework

    2015-10-01

    Humans and other living organisms require small quantities of trace elements throughout life. Both insufficient and excessive intakes of trace elements can have negative consequences. However, there is little information on serum level of trace elements in different populations. This study examines serum levels of trace elements in Ethiopian, Japanese, and Vietnamese women. Random samples of healthy women who were referred for routine hospital laboratory examinations in the cities of Hanoi, Sapporo, and Gondar were invited to participate in the study. Serum levels of magnesium, zinc, copper, iron, selenium, and calcium were determined using an inductively coupled plasma mass spectrometer. Furthermore, body mass index of each study participant was determined. The mean ± SD serum concentrations of zinc (μg/dL), copper (μg/dL), iron (μg/dL), selenium (μg/dL) and calcium (mg/dL), respectively, were 76.51 ± 39.16, 152.20 ± 55.37, 385.68 ± 217.95, 9.15 ± 4.21, and 14.18 ± 3.91 in Ethiopian women; 111.49 ± 52.92, 105.86 ± 26.02, 155.09 ± 94.83, 14.11 ± 3.41, and 11.66 ± 2.51 in Vietnamese women; and 60.69 ± 9.76, 107 ± 156, 268 ± 128, 8.33 ± 3.65, and 11.18 ± 0.68 in Japanese participants. Ethiopian women had significantly higher level of serum calcium than Vietnamese and Japanese women (both P Vietnamese women was higher than in women from Japan, the difference was not statistically significant (P > 0.05). Furthermore, compared with Japanese women, Ethiopian women had significantly high iron and copper concentrations (P Vietnamese than Ethiopian women. The study revealed a remarkable difference in serum concentrations of trace elements in women from different countries, implying differences in trace elements in the food or soil. Copyright © 2015 Elsevier Inc. All rights reserved.

  15. Direct determination of 3-chloropropanol esters in edible vegetable oils using high resolution mass spectrometry (HRMS-Orbitrap).

    Science.gov (United States)

    Graziani, Giulia; Gaspari, Anna; Chianese, Donato; Conte, Lanfranco; Ritieni, Alberto

    2017-11-01

    A series of refined edible oils derived from mixed seeds, peanuts, corn, sunflower and palm obtained from the local supermarket were analyzed for their content of 3-MCPD esters. A direct analytical method for the determination of 3-monochloropropane-1,2-diol esters (3-MCPD esters) was applied to investigate the major MCPD esters found in common edible oils; in particular seven types of monoesters and eleven types of diesters were detected. The limits of detection (LODs) for monoesters and diesters of 3-MCPD were in the range of 0.079-12.678 µg kg -1 and 0.033-18.610 µg kg -1 in edible oils, and the ranges of limits of quantitation (LOQs) were 0.979-38.035 µg kg -1 and 0.100-55 µg kg -1 , respectively. The recoveries of 3-MCPD esters from oil samples were in the range of 80-100%, with RSD ranging between 1.9 and 11.8%. The concentration levels of total 3-MCPD diesters in vegetable oil samples were in the range from 0.106 up to 3.444 μg g -1 whereas total monoesters ranged from 0.005 up to 1.606 μg g -1 .

  16. Determination of gold and cobalt dopants in advanced materials based on tin oxide by slurry sampling high-resolution continuum source graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    Filatova, Daria G.; Eskina, Vasilina V.; Baranovskaya, Vasilisa B.; Vladimirova, Svetlana A.; Gaskov, Alexander M.; Rumyantseva, Marina N.; Karpov, Yuri A.

    2018-02-01

    A novel approach is developed for the determination of Co and Au dopants in advanced materials based on tin oxide using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS) with direct slurry sampling. Sodium carboxylmethylcellulose (Na-CMC) is an effective stabilizer for diluted suspensions. Use Na-CMC allows to transfer the analytes into graphite furnace completely and reproducibly. The relative standard deviation obtained by HR CS GFAAS was not higher than 4%. Accuracy was proven by means inductively coupled plasma mass spectrometry (ICP-MS) in solutions after decomposition as a comparative technique. To determine Au and Co in the volume of SnO2, the acid decomposition conditions (HCl, HF) of the samples were suggested by means of an autoclave in a microwave oven.

  17. A method for volume determination of the orbit and its contents by high resolution axial tomography and quantitative digital image analysis.

    Science.gov (United States)

    Cooper, W C

    1985-01-01

    The various congenital and acquired conditions which alter orbital volume are reviewed. Previous investigative work to determine orbital capacity is summarized. Since these studies were confined to postmortem evaluations, the need for a technique to measure orbital volume in the living state is presented. A method for volume determination of the orbit and its contents by high-resolution axial tomography and quantitative digital image analysis is reported. This procedure has proven to be accurate (the discrepancy between direct and computed measurements ranged from 0.2% to 4%) and reproducible (greater than 98%). The application of this method to representative clinical problems is presented and discussed. The establishment of a diagnostic system versatile enough to expand the usefulness of computerized axial tomography and polytomography should add a new dimension to ophthalmic investigation and treatment.

  18. Software-aided approach to investigate peptide structure and metabolic susceptibility of amide bonds in peptide drugs based on high resolution mass spectrometry.

    Directory of Open Access Journals (Sweden)

    Tatiana Radchenko

    Full Text Available Interest in using peptide molecules as therapeutic agents due to high selectivity and efficacy is increasing within the pharmaceutical industry. However, most peptide-derived drugs cannot be administered orally because of low bioavailability and instability in the gastrointestinal tract due to protease activity. Therefore, structural modifications peptides are required to improve their stability. For this purpose, several in-silico software tools have been developed such as PeptideCutter or PoPS, which aim to predict peptide cleavage sites for different proteases. Moreover, several databases exist where this information is collected and stored from public sources such as MEROPS and ExPASy ENZYME databases. These tools can help design a peptide drug with increased stability against proteolysis, though they are limited to natural amino acids or cannot process cyclic peptides, for example. We worked to develop a new methodology to analyze peptide structure and amide bond metabolic stability based on the peptide structure (linear/cyclic, natural/unnatural amino acids. This approach used liquid chromatography / high resolution, mass spectrometry to obtain the analytical data from in vitro incubations. We collected experimental data for a set (linear/cyclic, natural/unnatural amino acids of fourteen peptide drugs and four substrate peptides incubated with different proteolytic media: trypsin, chymotrypsin, pepsin, pancreatic elastase, dipeptidyl peptidase-4 and neprilysin. Mass spectrometry data was analyzed to find metabolites and determine their structures, then all the results were stored in a chemically aware manner, which allows us to compute the peptide bond susceptibility by using a frequency analysis of the metabolic-liable bonds. In total 132 metabolites were found from the various in vitro conditions tested resulting in 77 distinct cleavage sites. The most frequent observed cleavage sites agreed with those reported in the literature. The

  19. High resolution CT of the chest

    Energy Technology Data Exchange (ETDEWEB)

    Barneveld Binkhuysen, F H [Eemland Hospital (Netherlands), Dept. of Radiology

    1996-12-31

    Compared to conventional CT high resolution CT (HRCT) shows several extra anatomical structures which might effect both diagnosis and therapy. The extra anatomical structures were discussed briefly in this article. (18 refs.).

  20. Comparison of three techniques for evaluating skin erythemal response for determination of sun protection factors of sunscreens: high resolution laser Doppler imaging, colorimetry and visual scoring.

    Science.gov (United States)

    Wilhelm, K P; Kaspar, K; Funkel, O

    2001-04-01

    Sun protection factor (SPF) measurement is based on the determination of the minimal erythema dose (MED). The ratio of doses required to induce a minimal erythema between product-treated and untreated skin is defined as SPF. The aim of this study was to validate the conventionally used visual scoring with two non-invasive methods: high resolution laser Doppler imaging (HR-LDI) and colorimetry. Another goal was to check whether suberythemal reactions could be detected by means of HR-LDI measurements. Four sunscreens were selected. The measurements were made on the back of 10 subjects. A solar simulator SU 5000 (m.u.t., Wedel, Germany) served as radiation source. For the visual assessment, the erythema was defined according to COLIPA as the first perceptible, clearly defined unambiguous redness of the skin. For the colorimetric determination of the erythema, a Chromameter CR 300 (Minolta, Osaka, Japan) was used. The threshold for the colorimetry was chosen according to the COLIPA recommendation as an increase of the redness parameter delta a* = 2.5. For the non-contact perfusion measurements of skin blood flow, a two-dimensional high resolution laser Doppler imager (HR-LDI) (Lisca, Linköping, Sweden) was used. For the HR-LDI measurements, an optimal threshold perfusion needed to be established. For the HR-LDI measurements basal perfusion +1 standard deviation of all basal measurements was found to be a reliable threshold perfusion corresponding to the minimal erythema. Smaller thresholds, which would be necessary for detection of suberythemal responses, did not provide unambiguous data. All three methods, visual scoring, colorimetry and HR-LDI, produced similar SPFs for the test products with a variability of colorimetry are suitable, reliable and observer-independent methods for MED determination. However, they do not provide greater sensitivity and thus do not result in lower UV dose requirements for testing.

  1. Fission-product yields for thermal-neutron fission of 243Cm determined from measurements with a high-resolution low-energy germanium gamma-ray detector

    International Nuclear Information System (INIS)

    Merriman, L.D.

    1984-04-01

    Cumulative fission-product yields have been determined for 13 gamma rays emitted during the decay of 12 fission products created by thermal-neutron fission of 243 Cm. A high-resolution low-energy germanium detector was used to measure the pulse-height spectra of gamma rays emitted from a 77-nanogram sample of 243 Cm after the sample had been irradiated by thermal neutrons. Analysis of the data resulted in the identification and matching of gamma-ray energies and half-lives to individual radioisotopes. From these results, 12 cumulative fission product yields were deduced for radionuclides with half-lives between 4.2 min and 84.2 min. 7 references

  2. Installation of high-resolution ERDA in UTTAC at the University of Tsukuba: Determination of the energy resolution and the detection limit for hydrogen

    Energy Technology Data Exchange (ETDEWEB)

    Sekiba, D., E-mail: sekiba@tac.tsukuba.ac.jp [Institute of Applied Physics, University of Tsukuba, Tennodai 1-1-1, Tsukuba, Ibaraki 305-8573 (Japan); University of Tsukuba, Tandem Accelerator Complex (UTTAC), Tennodai 1-1-1, Tsukuba, Ibaraki 305-8577 (Japan); Chito, K.; Harayama, I. [Institute of Applied Physics, University of Tsukuba, Tennodai 1-1-1, Tsukuba, Ibaraki 305-8573 (Japan); Watahiki, Y.; Ishii, S. [University of Tsukuba, Tandem Accelerator Complex (UTTAC), Tennodai 1-1-1, Tsukuba, Ibaraki 305-8577 (Japan); Ozeki, K. [Department of Mechanical Engineering, Ibaraki University, Nakanarusawa 4-12-1, Hitachi, Ibaraki 316-8511 (Japan)

    2017-06-15

    A newly developed high-resolution elastic recoil detection analysis (HERDA) system installed at the 1 MV Tandetron in UTTAC at the University of Tsukuba is introduced. The effective solid angle of detector, energy resolution and detection limit for hydrogen are, for the first time, determined quantitatively by the measurements on an a-C:H (and D) film deposited on a Si substrate. In the case of a 500 keV {sup 16}O{sup +} as the incident beam, an energy resolution of ∼0.45 keV and a detection limit of ∼3.8 × 10{sup 20} atoms/cm{sup 3} (∼0.18 at.%) with a data acquisition time of ∼310 s are derived.

  3. Rapid determination of 18 glucocorticoids in serum using reusable on-line SPE polymeric monolithic column coupled with LC-quadrupole/orbitrap high-resolution mass spectrometer.

    Science.gov (United States)

    Li, Hui; Ai, Lianfeng; Fan, Sufang; Wang, Yan; Sun, Dianxing

    2017-10-15

    A simple, rapid and sensitive method for the simultaneous determination of 18 glucocorticoids in serum was developed by coupling on-line solid-phase extraction (SPE) polymeric monolithic column to a liquid chromatography-quadrupole/orbitrap high-resolution mass spectrometer. A simple poly(ethylene glycol dimethacrylate) monolith column (10mm×2.1mm i.d.) was fabricated, and the morphology, surface area and extraction performance of the monolithic column were characterized. Serum samples were extracted by acetonitrile (ACN). Then, online SPE was achieved on the synthesized monolithic column using a 10mmol/L ammonium acetate solution as the loading solvent. After the transfer from the monolith into analytical column (Capcell Pak ADME column) using ACN, the adsorbed analytes were separated on the analytical column and detected with a high-resolution hybrid quadrupole/orbitrap mass spectrometer with full scan/ddMS 2 scan mode Under optimized conditions, the method was linear with target linear correlation coefficient (R 2 ) higher than 0.995. Detection limits were in range of 0.1-0.6ng/mL, and the quantification limits were 0.3-1.5ng/mL. The recovery was between 71.9% and 89.2% in three spike levels with precision (n=5) of 5.40-12.1%. The serum sample was directly analyzed after a simple extraction procedure, and the on-line SPE and determination were achieved within only 16min. The method was used to analyze the dynamic contents variation of cortisone and hydrocortisone in serum before and after the surgery. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. High-resolution structure of the M14-type cytosolic carboxypeptidase from Burkholderia cenocepacia refined exploiting PDB-REDO strategies

    Energy Technology Data Exchange (ETDEWEB)

    Rimsa, Vadim; Eadsforth, Thomas C. [University of Dundee, Dundee DD1 5EH, Scotland (United Kingdom); Joosten, Robbie P. [Netherlands Cancer Institute, Plesmanlaan 121, 1066 CX Amsterdam (Netherlands); Hunter, William N., E-mail: w.n.hunter@dundee.ac.uk [University of Dundee, Dundee DD1 5EH, Scotland (United Kingdom)

    2014-02-01

    The structure of a bacterial M14-family carboxypeptidase determined exploiting microfocus synchrotron radiation and highly automated refinement protocols reveals its potential to act as a polyglutamylase. A potential cytosolic metallocarboxypeptidase from Burkholderia cenocepacia has been crystallized and a synchrotron-radiation microfocus beamline allowed the acquisition of diffraction data to 1.9 Å resolution. The asymmetric unit comprises a tetramer containing over 1500 amino acids, and the high-throughput automated protocols embedded in PDB-REDO were coupled with model–map inspections in refinement. This approach has highlighted the value of such protocols for efficient analyses. The subunit is constructed from two domains. The N-terminal domain has previously only been observed in cytosolic carboxypeptidase (CCP) proteins. The C-terminal domain, which carries the Zn{sup 2+}-containing active site, serves to classify this protein as a member of the M14D subfamily of carboxypeptidases. Although eukaryotic CCPs possess deglutamylase activity and are implicated in processing modified tubulin, the function and substrates of the bacterial family members remain unknown. The B. cenocepacia protein did not display deglutamylase activity towards a furylacryloyl glutamate derivative, a potential substrate. Residues previously shown to coordinate the divalent cation and that contribute to peptide-bond cleavage in related enzymes such as bovine carboxypeptidase are conserved. The location of a conserved basic patch in the active site adjacent to the catalytic Zn{sup 2+}, where an acetate ion is identified, suggests recognition of the carboxy-terminus in a similar fashion to other carboxypeptidases. However, there are significant differences that indicate the recognition of substrates with different properties. Of note is the presence of a lysine in the S1′ recognition subsite that suggests specificity towards an acidic substrate.

  5. High-resolution structure of the M14-type cytosolic carboxypeptidase from Burkholderia cenocepacia refined exploiting PDB-REDO strategies

    International Nuclear Information System (INIS)

    Rimsa, Vadim; Eadsforth, Thomas C.; Joosten, Robbie P.; Hunter, William N.

    2014-01-01

    The structure of a bacterial M14-family carboxypeptidase determined exploiting microfocus synchrotron radiation and highly automated refinement protocols reveals its potential to act as a polyglutamylase. A potential cytosolic metallocarboxypeptidase from Burkholderia cenocepacia has been crystallized and a synchrotron-radiation microfocus beamline allowed the acquisition of diffraction data to 1.9 Å resolution. The asymmetric unit comprises a tetramer containing over 1500 amino acids, and the high-throughput automated protocols embedded in PDB-REDO were coupled with model–map inspections in refinement. This approach has highlighted the value of such protocols for efficient analyses. The subunit is constructed from two domains. The N-terminal domain has previously only been observed in cytosolic carboxypeptidase (CCP) proteins. The C-terminal domain, which carries the Zn 2+ -containing active site, serves to classify this protein as a member of the M14D subfamily of carboxypeptidases. Although eukaryotic CCPs possess deglutamylase activity and are implicated in processing modified tubulin, the function and substrates of the bacterial family members remain unknown. The B. cenocepacia protein did not display deglutamylase activity towards a furylacryloyl glutamate derivative, a potential substrate. Residues previously shown to coordinate the divalent cation and that contribute to peptide-bond cleavage in related enzymes such as bovine carboxypeptidase are conserved. The location of a conserved basic patch in the active site adjacent to the catalytic Zn 2+ , where an acetate ion is identified, suggests recognition of the carboxy-terminus in a similar fashion to other carboxypeptidases. However, there are significant differences that indicate the recognition of substrates with different properties. Of note is the presence of a lysine in the S1′ recognition subsite that suggests specificity towards an acidic substrate

  6. Crystal structure and defects of Zr4Co4Si7( V-phase) investigated by high resolution transmission electron microscope

    International Nuclear Information System (INIS)

    Mao, J.F.; Ye, H.Q.; Ning, X.G.; He, L.L.; Yang, D.Z.

    1997-01-01

    The results of high resolution transmission electron microscope (HRTEM) observation and image simulation show that Zr 4 Co 4 Si 7 possesses the same structure type of Zr 4 Co 4 Ge 7 . Adding of Fe or Ni into the Zr 4 Co 4 Si 7 compound, except that the dimensions changed slightly, does not change the lattice type and coordination in the crystal structure, maintaining the V-phase structure. Also, twins with coherent boundaries and with partially coherent at interfaces are observed. The image conditions of Zr 4 Co 4 Si 7 and the structure differences between Zr 4 Co 4 Si 7 and tetrahedral close-packed phases are also discussed. copyright 1997 Materials Research Society

  7. Ozone-induced dissociation on a traveling wave high-resolution mass spectrometer for determination of double-bond position in lipids.

    Science.gov (United States)

    Vu, Ngoc; Brown, Jeffery; Giles, Kevin; Zhang, Qibin

    2017-09-15

    The position of C=C within fatty acyl chains affects the biological function of lipids. Ozone-induced dissociation mass spectrometry (OzID-MS) has great potential in determination of lipid double-bond position, but has generally been implemented on low-resolution ion trap mass spectrometers. In addition, most of the OzID-MS experiments carried out so far were focused on the sodiated adducts of lipids; fragmentation of the most commonly observed protonated ions generated in LC/MS-based lipidomics workflow has been less explored. Ozone generated in line from an ozone generator was connected to the trap and transfer gas supply line of a Synapt G2 high-resolution mass spectrometer. Protonated ions of different phosphatidylcholines (PC) were generated by electrospray ionization through direct infusion. Different parameters, including traveling wave height and velocity, trap entrance and DC potential, were adjusted to maximize the OzID efficiency. sn-positional isomers and cis/trans isomers of lipids were compared for their reactivity with ozone. Traveling wave height and velocity were tuned to prolong the encounter time between lipid ions and ozone, and resulted in improved OzID efficiency, as did increasing trapping region DC and entrance potential. Under optimized settings, at least 1000 times enhancement in OzID efficiency was achieved compared to that under default settings for monounsaturated PC standards. Monounsaturated C=C in the sn-2 PC isomer reacted faster with ozone than the sn-1 isomer. Similarly, the C=C in trans PC reacted faster than in cis PC. This is the first implementation of OzID in the trap and transfer region of a traveling wave enabled high-resolution mass spectrometer. The OzID reaction efficiency is significantly improved by slowing down ions in the trap region for their prolonged interaction with ozone. This will facilitate application of high-resolution OzID-MS in lipidomics. Copyright © 2017 John Wiley & Sons, Ltd.

  8. Solution NMR structure determination of proteins revisited

    International Nuclear Information System (INIS)

    Billeter, Martin; Wagner, Gerhard; Wuethrich, Kurt

    2008-01-01

    This 'Perspective' bears on the present state of protein structure determination by NMR in solution. The focus is on a comparison of the infrastructure available for NMR structure determination when compared to protein crystal structure determination by X-ray diffraction. The main conclusion emerges that the unique potential of NMR to generate high resolution data also on dynamics, interactions and conformational equilibria has contributed to a lack of standard procedures for structure determination which would be readily amenable to improved efficiency by automation. To spark renewed discussion on the topic of NMR structure determination of proteins, procedural steps with high potential for improvement are identified

  9. Study of the structure of the particles of channel black of phase-contrasting electron microscopy of high resolution

    Energy Technology Data Exchange (ETDEWEB)

    Varlakov, V.P.; Fialkov, A.S.; Smirnov, B.N.

    1981-01-01

    The structure of channel black, DG-100, in the initial and graphitized states has been studied by phase-contrasting electron microscopy with a direct resolution of the carbon layers. An individual carbon layer is the main structural element of carbon black. The structure of channel black in the graphitized state looks like a hollow closed polyhedron made up of bundles of continuous carbon layers which can bend and become deformed to a great extent, testifying to the polymeric nature of the structure of channel black. The authors give an interpretation of the roentgen values of the 'dimensions of crystallites' in channel black.

  10. Restoring defect structures in 3C-SiC/Si (001) from spherical aberration-corrected high-resolution transmission electron microscope images by means of deconvolution processing.

    Science.gov (United States)

    Wen, C; Wan, W; Li, F H; Tang, D

    2015-04-01

    The [110] cross-sectional samples of 3C-SiC/Si (001) were observed with a spherical aberration-corrected 300 kV high-resolution transmission electron microscope. Two images taken not close to the Scherzer focus condition and not representing the projected structures intuitively were utilized for performing the deconvolution. The principle and procedure of image deconvolution and atomic sort recognition are summarized. The defect structure restoration together with the recognition of Si and C atoms from the experimental images has been illustrated. The structure maps of an intrinsic stacking fault in the area of SiC, and of Lomer and 60° shuffle dislocations at the interface have been obtained at atomic level. Copyright © 2015 Elsevier Ltd. All rights reserved.

  11. The mechanism of vault opening from the high resolution structure of the N-terminal repeats of MVP.

    Science.gov (United States)

    Querol-Audí, Jordi; Casañas, Arnau; Usón, Isabel; Luque, Daniel; Castón, José R; Fita, Ignasi; Verdaguer, Nuria

    2009-11-04

    Vaults are ubiquitous ribonucleoprotein complexes involved in a diversity of cellular processes, including multidrug resistance, transport mechanisms and signal transmission. The vault particle shows a barrel-shaped structure organized in two identical moieties, each consisting of 39 copies of the major vault protein MVP. Earlier data indicated that vault halves can dissociate at acidic pH. The crystal structure of the vault particle solved at 8 A resolution, together with the 2.1-A structure of the seven N-terminal domains (R1-R7) of MVP, reveal the interactions governing vault association and provide an explanation for a reversible dissociation induced by low pH. The structural comparison with the recently published 3.5 A model shows major discrepancies, both in the main chain tracing and in the side chain assignment of the two terminal domains R1 and R2.

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

    Science.gov (United States)

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

    2015-04-14

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

  13. Use of slurry sampling for the direct determination of zinc in yogurt by high resolution-continuum source flame atomic absorption spectrometry.

    Science.gov (United States)

    Brandao, Geovani C; de Jesus, Raildo M; da Silva, Erik G P; Ferreira, Sergio L C

    2010-06-15

    This paper presents an analytical procedure for the direct determination of zinc in yogurt employing sampling slurry and high resolution-continuum source flame atomic absorption spectrometry (HR-CS FAAS). The step optimization established the experimental conditions of: 2.0molL(-1) hydrochloric acid, a sonication time of 20min and a sample mass of 1.0g for a slurry volume of 25mL. This method allows the determination of zinc with a limit of quantification of 0.32microgg(-1). The precision expressed as relative standard deviation (RSD) were 0.82 and 2.08% for yogurt samples containing zinc concentrations of 4.85 and 2.49microgg(-1), respectively. The accuracy was confirmed by the analysis of a certified reference material of non-fat milk powder furnished by the National Institute of Standard and Technology. The proposed method was applied for the determination of zinc in seven yogurt samples. The zinc content was varied from 2.19 to 4.85microgg(-1). These results agreed with those reported in the literature. The samples were also analyzed after acid digestion and zinc determination by FAAS. No statistical difference was observed between the results obtained by both of the procedures performed.

  14. Determination of sulfur in human hair using high resolution continuum source graphite furnace molecular absorption spectrometry and its correlation with total protein and albumin

    Science.gov (United States)

    Ozbek, Nil; Baysal, Asli

    2017-04-01

    Human hair is a valuable contributor for biological monitoring. It is an information storage point to assess the effects of environmental, nutritional or occupational sources on the body. Human proteins, amino acids or other compounds are among the key components to find the sources of different effects or disorders in the human body. Sulfur is a significant one of these compounds, and it has great affinity to some metals and compounds. This property of the sulfur affects the human health positively or negatively. In this manuscript, sulfur was determined in hair samples of autistic and age-match control group children via molecular absorption of CS using a high-resolution continuum source graphite furnace atomic absorption spectrometer. For this purpose, hair samples were appropriately washed and dried at 75 °C. Then samples were dissolved in microwave digestion using HNO3 for sulfur determination. Extraction was performed with HCl hydrolysation by incubation for 24 h at 110 °C for total protein and albumin determination. The validity of the method for the sulfur determination was tested using hair standard reference materials. The results were in the uncertainty limits of the certified values at 95% confidence level. Finally correlation of sulfur levels of autistic children's hair with their total protein and albumin levels were done.

  15. High-resolution NMR structure of the antimicrobial peptide protegrin-2 in the presence of DPC micelles

    Energy Technology Data Exchange (ETDEWEB)

    Usachev, K. S., E-mail: k.usachev@kpfu.ru; Efimov, S. V.; Kolosova, O. A.; Filippov, A. V.; Klochkov, V. V. [Kazan Federal University (Russian Federation)

    2015-04-15

    PG-1 adopts a dimeric structure in dodecylphosphocholine (DPC) micelles, and a channel is formed by the association of several dimers but the molecular mechanisms of the membrane damage by non-α-helical peptides are still unknown. The formation of the PG-1 dimer is important for pore formation in the lipid bilayer, since the dimer can be regarded as the primary unit for assembly into the ordered aggregates. It was supposed that only 12 residues (RGGRL-CYCRR-RFCVC-V) are needed to endow protegrin molecules with strong antibacterial activity and that at least four additional residues are needed to add potent antifungal properties. Thus, the 16-residue protegrin (PG-2) represents the minimal structure needed for broad-spectrum antimicrobial activity encompassing bacteria and fungi. As the peptide conformation and peptide-to-membrane binding properties are very sensitive to single amino acid substitutions, the solution structure of PG-2 in solution and in a membrane mimicking environment are crucial. In order to find evidence if the oligomerization state of PG-1 in a lipid environment will be the same or not for another protegrins, we investigate in the present work the PG-2 NMR solution structure in the presence of perdeuterated DPC micelles. The NMR study reported in the present work indicates that PG-2 form a well-defined structure (PDB: 2MUH) composed of a two-stranded antiparallel β-sheet when it binds to DPC micelles.

  16. Analyses of the temporal and spatial structures of heavy rainfall from a catalog of high-resolution radar rainfall fields

    DEFF Research Database (Denmark)

    Thorndahl, Søren; Smith, James A.; Baeck, Mary Lynn

    2014-01-01

    that relate to size, structure and evolution of heavy rainfall. Extreme rainfall is also linked with severe weather (tornados, large hail and damaging wind). The diurnal cycle of rainfall for heavy rain days is characterized by an early peak in the largest rainfall rates, an afternoon-evening peak in rain...

  17. High-resolution crystal structure of an engineered human beta2-adrenergic G protein-coupled receptor

    DEFF Research Database (Denmark)

    Cherezov, Vadim; Rosenbaum, Daniel M; Hanson, Michael A

    2007-01-01

    Heterotrimeric guanine nucleotide-binding protein (G protein)-coupled receptors constitute the largest family of eukaryotic signal transduction proteins that communicate across the membrane. We report the crystal structure of a human beta2-adrenergic receptor-T4 lysozyme fusion protein bound to t...

  18. Determination of fusarium mycotoxins in wheat, maize and animal feed using on-line clean-up with high resolution mass spectrometry.

    Science.gov (United States)

    Ates, E; Mittendorf, K; Stroka, J; Senyuva, H

    2013-01-01

    An automated method involving on-line clean-up and analytical separation in a single run using TurboFlow™ reversed phase liquid chromatography coupled to a high resolution mass spectrometer has been developed for the simultaneous determination of deoxynivalenol, T2 toxin, HT2 toxin, zearalenone and fumonisins B1 and B2 in maize, wheat and animal feed. Detection was performed in full scan mode at a resolution of R = 100,000 full width at half maximum with high energy collision cell dissociation for the determination of fragment ions with a mass accuracy below 5 ppm. The extract from homogenised samples, after blending with a 0.1% aqueous mixture of 0.1% formic acid/acetonitrile (43:57) for 45 min, was injected directly onto the TurboFlow™ (TLX) column for automated on-line clean-up followed by analytical separation and accurate mass detection. The TurboFlow™ column enabled specific binding of target mycotoxins, whereas higher molecular weight compounds, like fats, proteins and other interferences with different chemical properties, were removed to waste. Single laboratory method validation was performed by spiking blank materials with mycotoxin standards. The recovery and repeatability was determined by spiking at three concentration levels (50, 100 and 200% of legislative limits) with six replicates. Average recovery, relative standard deviation and intermediate precision values were 71 to 120%, 1 to 19% and 4 to 19%, respectively. The method accuracy was confirmed with certified reference materials and participation in proficiency testing.

  19. Determination of phospholipids in soybean lecithin samples via the phosphorus monoxide molecule by high-resolution continuum source graphite furnace molecular absorption spectrometry.

    Science.gov (United States)

    Pires, Laís N; Brandão, Geovani C; Teixeira, Leonardo S G

    2017-06-15

    This paper presents a method for determining phospholipids in soybean lecithin samples by phosphorus determination using high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) via molecular absorption of phosphorus monoxide. Samples were diluted in methyl isobutyl ketone. The best conditions were found to be 213.561nm with a pyrolysis temperature of 1300°C, a volatilization temperature of 2300°C and Mg as a chemical modifier. To increase the analytical sensitivity, measurement of the absorbance signal was obtained by summing molecular transition lines for PO surrounding 213nm: 213.561, 213.526, 213.617 and 213.637nm. The limit of detection was 2.35mgg -1 and the precision, evaluated as relative standard deviation (RSD), was 2.47% (n=10) for a sample containing 2.2% (w/v) phosphorus. The developed method was applied for the analysis of commercial samples of soybean lecithin. The determined concentrations of phospholipids in the samples varied between 38.1 and 45% (w/v). Copyright © 2017 Elsevier Ltd. All rights reserved.

  20. CaI and SrI molecules for iodine determination by high-resolution continuum source graphite furnace molecular absorption spectrometry: Greener molecules for practical application.

    Science.gov (United States)

    Zanatta, Melina Borges Teixeira; Nakadi, Flávio Venâncio; da Veiga, Márcia Andreia Mesquita Silva

    2018-03-01

    A new method to determine iodine in drug samples by high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) has been developed. The method measures the molecular absorption of a diatomic molecule, CaI or SrI (less toxic molecule-forming reagents), at 638.904 or 677.692nm, respectively, and uses a mixture containing 5μg of Pd and 0.5μg of Mg as chemical modifier. The method employs pyrolysis temperatures of 1000 and 800°C and vaporization temperatures of 2300 and 2400°C for CaI and SrI, respectively. The optimized amounts of Ca and Sr as molecule-forming reagents are 100 and 150µg, respectively. On the basis of interference studies, even small chlorine concentrations reduce CaI and SrI absorbance significantly. The developed method was used to analyze different commercial drug samples, namely thyroid hormone pills with three different iodine amounts (15.88, 31.77, and 47.66µg) and one liquid drug with 1% m v -1 active iodine in their compositions. The results agreed with the values informed by the manufacturers (95% confidence level) regardless of whether CaI or SrI was determined. Therefore, the developed method is useful for iodine determination on the basis of CaI or SrI molecular absorption. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Ultra-High Resolution Ion Mobility Separations Utilizing Traveling Waves in a 13 m Serpentine Path Length Structures for Lossless Ion Manipulations Module

    Energy Technology Data Exchange (ETDEWEB)

    Deng, Liulin; Ibrahim, Yehia M.; Hamid, Ahmed M.; Garimella, Sandilya V. B.; Webb, Ian K.; Zheng, Xueyun; Prost, Spencer A.; Sandoval, Jeremy A.; Norheim, Randolph V.; Anderson, Gordon A.; Tolmachev, Aleksey V.; Baker, Erin S.; Smith, Richard D.

    2016-09-20

    We report the development and initial evaluation of a 13-m path length Structures for Lossless Manipulations (SLIM) module for achieving high resolution separations using traveling waves (TW) with ion mobility (IM) spectrometry. The TW SLIM module was fabricated using two mirror-image printed circuit boards with appropriately configured RF, DC and TW electrodes and positioned with a 2.75-mm inter-surface gap. Ions were effective confined between the surfaces by RF-generated pseudopotential fields and moved losslessly through a serpentine path including 44 “U” turns using TWs. The ion mobility resolution was characterized at different pressures, gaps between the SLIM surfaces, TW and RF parameters. After initial optimization the SLIM IM-MS module provided about 5-fold higher resolution separations than present commercially available drift tube or traveling wave IM-MS platforms. Peak capacity and peak generation rates achieved were 246 and 370 s-1, respectively, at a TW speed of 148 m/s. The high resolution achieved in the TW SLIM IM-MS enabled e.g., isomeric sugars (Lacto-N-fucopentaose I and Lacto-N-fucopentaose II) to be baseline resolved, and peptides from a albumin tryptic digest much better resolved than with existing commercial IM-MS platforms. The present work also provides a foundation for the development of much higher resolution SLIM devices based upon both considerably longer path lengths and multi-pass designs.

  2. Temperature-salinity structure of the AMOC in high-resolution ocean simulations and in CMIP5 models

    Science.gov (United States)

    Wang, F.; Xu, X.; Chassignet, E.

    2017-12-01

    On average, the CMIP5 models represent the AMOC structure, water properties, Heat transport and Freshwater transport reasonably well. For temperature, CMIP5 models exhibit a colder northward upper limb and a warmer southward lower limb. the temperature contrast induces weaker heat transport than observation. For salinity, CMIP5 models exhibit saltier southward lower limb, thus contributes to weaker column freshwater transport. Models have large spread, among them, AMOC strength contributes to Heat transport but not freshwater transport. AMOC structure (the overturning depth) contributes to transport-weighted temperature not transport-weighted salinity in southward lower limb. The salinity contrast in upper and lower limb contributes to freshwater transport, but temperature contrast do not contribute to heat transport.

  3. The high-resolution structure of the Centaurus A nucleus at 2.3 and 8.4 GHz

    International Nuclear Information System (INIS)

    Meier, D.L.; Preston, R.A.; Morabito, D.D.

    1989-01-01

    VLBI observations of the nucleus of Centaurus A have been made at two frequencies with an array of five Australian radio telescopes as part of the Southern Hemisphere VLBI Experiment. Observations were made at 2.3 GHz with all five antennas, while only two were employed at 8.4 GHz. At 2.3 GHz seven tracks in the (u,v) plane with coverage of 6-8 hr each were obtained, yielding significant information on the structure of the nuclear jet. At 8.4 GHz a compact unresolved core was detected as well. It is found that the source consists of the compact self-absorbed core, a jet containing a set of three knots extending from 100 to 160 mas from the core, and a very long, narrow component elongated along the same position angle as the knots. The allowable range for the position angle of the jet is 51 + or - 3 deg, in agreement with that of the radio and X-ray structure on arcsecond and arcminute scales. The jet has brightened at 2.3 GHz by about 4 Jy, a factor of nearly 3, since the early 1970s, 1.8 Jy of which has occurred in the last 2 yr with no discernable changes in structure. 21 refs

  4. High Resolution 3D Experimental Investigation of Flow Structures and Turbulence Statistics in the Viscous and Buffer Layer

    Science.gov (United States)

    Sheng, Jian; Malkiel, Edwin; Katz, Joseph

    2006-11-01

    Digital Holographic Microscopy is implemented to perform 3D velocity measurement in the near-wall region of a turbulent boundary layer in a square channel over a smooth wall at Reτ=1,400. The measurements are performed at a resolution of ˜1μm over a sample volume of 1.5x2x1.5mm (x^+=50, y^+=60, z^+=50), sufficient for resolving buffer layer structures and for measuring the instantaneous wall shear stress distributions from velocity gradients in the sublayer. The data provides detailed statistics on the spatial distribution of both wall shear stress components along with the characteristic flow structures, including streamwise counter-rotating vortex pairs, multiple streamwise vortices, and rare hairpins. Conditional sampling identifies characteristic length scales of 70 wall units in spanwise and 10 wall units in wall-normal direction. In the region of high stress, the conditionally averaged flow consists of a stagnation-like sweeping motion induced by a counter rotating pair of streamwise vortices. Regions with low stress are associated with ejection motion, also generated by pairs of counter-rotating vortices. Statistics on the local strain and geometric alignment between strain and vorticity shows that the high shear generating vortices are inclined at 45 to streamwise direction, indicating that vortices are being stretched. Results of on-going analysis examines statistics of helicity, strain and impacts of near-wall structures.

  5. Investigation of artifacts caused by deuterium background correction in the determination of phosphorus by electrothermal atomization using high-resolution continuum source atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Dessuy, Morgana B.; Vale, Maria Goreti R.; Lepri, Fabio G.; Borges, Daniel L.G.; Welz, Bernhard; Silva, Marcia M.; Heitmann, Uwe

    2008-01-01

    The artifacts created in the measurement of phosphorus at the 213.6-nm non-resonance line by electrothermal atomic absorption spectrometry using line source atomic absorption spectrometry (LS AAS) and deuterium lamp background correction (D 2 BC) have been investigated using high-resolution continuum source atomic absorption spectrometry (HR-CS AAS). The absorbance signals and the analytical curves obtained by LS AAS without and with D 2 BC, and with HR-CS AAS without and with automatic correction for continuous background absorption, and also with least-squares background correction for molecular absorption with rotational fine structure were compared. The molecular absorption due to the suboxide PO that exhibits pronounced fine structure could not be corrected by the D 2 BC system, causing significant overcorrection. Among the investigated chemical modifiers, NaF, La, Pd and Pd + Ca, the Pd modifier resulted in the best agreement of the results obtained with LS AAS and HR-CS AAS. However, a 15% to 100% higher sensitivity, expressed as slope of the analytical curve, was obtained for LS AAS compared to HR-CS AAS, depending on the modifier. Although no final proof could be found, the most likely explanation is that this artifact is caused by a yet unidentified phosphorus species that causes a spectrally continuous absorption, which is corrected without problems by HR-CS AAS, but which is not recognized and corrected by the D 2 BC system of LS AAS

  6. Structure and hydrocarbon potential of the Nuussuaq basin: acquisition and interpretation of high-resolution multichannel seismic data

    Energy Technology Data Exchange (ETDEWEB)

    Marcussen, C.; Skaarup, N.; Chalmers, J.A.

    2002-07-01

    Data acquisition of project NuussuaqSeis2000 (GEUS2000G survey) was very successful. Due to very favourable weather and ice conditions, 2743 km of good quality data were acquired, nearly 20% more than originally planned. High concentrations of icebergs prevented acquisition of data in the eastern part of Uummannaq Fjord and east of Svartenhuk Halvoe. Data from project NuussuaqSeis 2000 have therefore considerably increased the seismic coverage in the region. Interpretation of the new data has given information on the size and geometry of the individual fault blocks in areas with Cretaceous sediments. Furthermore the new data confirm that the seeps in the Vaigat region are structurally controlled and mainly occur in the block-faulted area north of the Disko gneiss ridge. Data from the GEUS2000G survey confirm the overall structural interpretation published in Chalmers et al. (1999). The interpretation of the structural style in western Vaigat is confirmed as being substantially correct, although the fault patterns have been shown to be much more complex than realised previously, from either the onshore data or from the single line GGU/95-06. The main area of revision has been in eastern Vaigat, but even there the essentials of the Chalmers et al. (1999) interpretation remain. In the area north of Nuussuaq in Uummannaq Fjord and Illorssuit Sund the fault trend is more N-S than in Vaigat, but also here the complexity in the fault pattern prohibites a correlation for too long distances. The general fault pattern from the structural interpretation of Chalmers et al. (1999) remains valid in this area as well. Some of the data acquired under project NuussuaqSeis2000 are highly relevant for an assessment of the petroleum prospectivity of the Disko-Nuussuaq region, and the data and their interpretation will be included in the next revised GEUS Note to the Bureau of Minerals and Petroleum on this matter. The new data and the interpretations are particularly important for

  7. Determination of copper and mercury in phosphate fertilizers employing direct solid sampling analysis and high resolution continuum source graphite furnace atomic absorption spectrometry

    Science.gov (United States)

    de Oliveira Souza, Sidnei; François, Luciane Luiza; Borges, Aline Rocha; Vale, Maria Goreti Rodrigues; Araujo, Rennan Geovanny Oliveira

    2015-12-01

    The present study proposes the determination of copper and mercury in phosphate fertilizers by direct solid sampling analysis (SS) employing high resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS). For Cu determination, two analytical lines were used: 327.3960 nm and 249.2146 nm. Hg determination was carried out on the line 253.6521 nm and 100 μg KMnO4 was used as chemical modifier. The optimal pyrolysis temperature for Cu determination was 1300 °C. Atomization temperatures for Cu and Hg were 2400 and 1100 °C, respectively. External calibration with aqueous standard solutions was adopted for both elements. The limits of quantification (LoQs) and characteristic mass (m0) obtained for Cu determination were 0.4 μg g- 1 and 1.12 ng, respectively, on line 249.2146 nm, and 64 μg g- 1 and 25 pg on 327.3960 nm. For mercury, LoQ and m0 were 4.8 ng g- 1 and 39 pg, respectively. The accuracy of the proposed methods was confirmed by the analysis of standard reference material (SRM) of Trace Elements in Multi-Nutrient Fertilizer (SRM NIST 695). The precision expressed as relative standard deviation (RSD), was better than 8.2% for Hg and 7.7% for the Cu (n = 5), considered satisfactory for microanalysis in solid sample. Four fertilizer samples acquired in commercial establishments in the city of Salvador, Bahia, Brazil, were analyzed. The optimized analytical methods were simple, fast, accurate, precise and free of spectral interferences for the determination of Cu and Hg in phosphate fertilizer samples by SS-HR-CS GF AAS, avoiding the dissolution of the sample, the use of harmful reagents and the generation of residues.

  8. High-resolution deep sequencing reveals biodiversity, population structure, and persistence of HIV-1 quasispecies within host ecosystems

    Directory of Open Access Journals (Sweden)

    Yin Li

    2012-12-01

    Full Text Available Abstract Background Deep sequencing provides the basis for analysis of biodiversity of taxonomically similar organisms in an environment. While extensively applied to microbiome studies, population genetics studies of viruses are limited. To define the scope of HIV-1 population biodiversity within infected individuals, a suite of phylogenetic and population genetic algorithms was applied to HIV-1 envelope hypervariable domain 3 (Env V3 within peripheral blood mononuclear cells from a group of perinatally HIV-1 subtype B infected, therapy-naïve children. Results Biodiversity of HIV-1 Env V3 quasispecies ranged from about 70 to 270 unique sequence clusters across individuals. Viral population structure was organized into a limited number of clusters that included the dominant variants combined with multiple clusters of low frequency variants. Next generation viral quasispecies evolved from low frequency variants at earlier time points through multiple non-synonymous changes in lineages within the evolutionary landscape. Minor V3 variants detected as long as four years after infection co-localized in phylogenetic reconstructions with early transmitting viruses or with subsequent plasma virus circulating two years later. Conclusions Deep sequencing defines HIV-1 population complexity and structure, reveals the ebb and flow of dominant and rare viral variants in the host ecosystem, and identifies an evolutionary record of low-frequency cell-associated viral V3 variants that persist for years. Bioinformatics pipeline developed for HIV-1 can be applied for biodiversity studies of virome populations in human, animal, or plant ecosystems.

  9. Design and analysis of a cross-type structured-illumination confocal microscope for high speed and high resolution

    International Nuclear Information System (INIS)

    Kim, Young-Duk; Ahn, MyoungKi; Kim, Taejoong; Gweon, DaeGab; Yoo, Hongki

    2012-01-01

    There have been many studies about a super resolution microscope for many years. A super resolution microscope can detect the physical phenomena or morphology of a biological sample more precisely than conventional microscopes. The structured-illumination microscope (SIM) is one of the technologies that demonstrate super resolution. However, the conventional SIM requires more time to obtain one resolution-enhanced image than other super resolution microscopes. More specifically, the conventional SIM uses three images with a 120° phase difference for each direction and three different directions are image-processed to make one resolution enhancement by increasing the optical transfer function in three directions. In this paper, we present a novel cross structured-illumination confocal microscope (CSICM) that takes the advantage of the technology of both SIM and the confocal microscope. The CSICM uses only two directions with three phase difference images, for a total of six images. By reducing the number of images that must be obtained, the total image acquisition time and image reconstruction time in obtaining the final output images can be decreased, and the confocal microscope provides axial information of the sample automatically. We demonstrate our method of cross illumination and evaluate the performance of the CSICM and compare it to the conventional SIM and the confocal microscope. (paper)

  10. Investigation of chemical modifiers for sulfur determination in diesel fuel samples by high-resolution continuum source graphite furnace molecular absorption spectrometry using direct analysis

    Energy Technology Data Exchange (ETDEWEB)

    Huber, Charles S. [Instituto Federal Sul-rio-grandense, Câmpus Pelotas, Pelotas, RS (Brazil); Universidade Federal do Rio Grande do Sul, Instituto de Química, Porto Alegre, RS (Brazil); Vale, Maria Goreti R. [Universidade Federal do Rio Grande do Sul, Instituto de Química, Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Welz, Bernhard [Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Universidade Federal de Santa Catarina, Departamento de Química, Florianópolis, SC (Brazil); Andrade, Jailson B. [Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Dessuy, Morgana B., E-mail: mbdessuy@ufrgs.br [Universidade Federal do Rio Grande do Sul, Instituto de Química, Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil)

    2015-06-01

    High-resolution continuum source graphite furnace molecular absorption spectrometry has been applied for sulfur determination in diesel fuel. The sharp rotational lines of the carbon monosulfide molecule (formed during the vaporization step) were used to measure the absorbance. The analytical line at 258.056 nm was monitored using the sum of three pixels. Different chemical modifiers were investigated and the mixture of palladium and magnesium was used as chemical modifier in combination with iridium as permanent modifier. L-Cysteine was chosen as sulfur standard and the calibration was done against aqueous standard solutions. The proposed method was applied for the analyses of four diesel samples: two S10 samples and two S500 samples. The trueness of the method was checked with a certified reference material (CRM) of sulfur in diesel fuel (NIST 2724b). Accurate results, for samples and CRM, were achieved after a dilution with propan-1-ol. The following figures of merit were obtained: characteristic mass of 17 ± 3 ng, limit of detection and limit of quantification of 1.4 mg kg{sup −1} and 4.7 mg kg{sup −1}, respectively. - Highlights: • Ir, Ru and Zr were investigated as permanent modifiers. • Ca, Mg, Pd and Pd/Mg were investigated as modifiers in solution. • Indirect determination of sulfur monitoring the molecular absorbance of the CS • Direct analysis of diesel samples using a dilution in propan-1-ol.

  11. Dilute-and-shoot coupled to nanoflow liquid chromatography high resolution mass spectrometry for the determination of drugs of abuse and sport drugs in human urine.

    Science.gov (United States)

    Alcántara-Durán, Jaime; Moreno-González, David; Beneito-Cambra, Miriam; García-Reyes, Juan F

    2018-05-15

    In this work, a sensitive nanoflow liquid chromatography high-resolution mass spectrometry screening method has been developed for the determination of multiclass drugs of abuse and sport drugs in human urine. 81 drugs belonging to different multiclass pharmaceuticals were targeted. The method is based on the use of a nanoLC column (75 µm × 150 mm, 3 µm particle size and 100 Å pore) with the nanospray emitter tip integrated so that dead volumes are significantly minimized. Data acquisition method included both full-scan and all ion fragmentation experiments using an Orbitrap analyser (Q-Exactive) operated in the positive ionization mode. To increase laboratory throughput, a dilute-and-shoot methodology has been tested and proposed, based solely on direct urine dilution without further sample workup. Matrix effects were evaluated, showing a negligible effect for all studied compounds when a dilution 1:50 was implemented. Despite this high-dilution factor, limits of quantification were still satisfactory, with values below 5 µg L -1 in most cases, being lower than their minimum required performance limits correspond established by the World Anti-Doping Agency. Therefore, the use of the dilute-and-shoot method with the enhanced sensitivity provided by nanoflow LC setup could be useful tool for the determination of studied compounds in drug testing, thus increasing laboratory performance, because a minimum sample treatment steps are required. Copyright © 2018 Elsevier B.V. All rights reserved.

  12. Determination of bromide in aqueous solutions via the TlBr molecule using high-resolution continuum source graphite furnace molecular absorption spectrometry

    Science.gov (United States)

    Cacho, Frantisek; Machynak, Lubomir; Nemecek, Martin; Beinrohr, Ernest

    2018-06-01

    The paper describes the determination of bromide by evaluating the molecular absorption of thallium mono-bromide (TlBr) at the rotational line at 342.9815 nm by making use a high-resolution continuum source graphite furnace atomic absorption spectrometer. The effects of variables such as the wavelength, graphite furnace program, amount of Tl and the use of a modifier were investigated and optimized. Various chemical modifiers have been studied, such as Pd, Mg, Ag and a mixture of Pd/Mg. It was found that best results were obtained by using Ag which prevents losses of bromide during pyrolysis step through precipitation of bromide as AgBr. In this way, a maximum pyrolysis temperature of 400 °C could be used. The optimum molecule forming temperature was found to be 900 °C. Bromide concentrations in various water samples (CRM, bottled drinking water and tap water) were determined. The quantification was made by both linear calibration and standard addition techniques. The results were matched well those of the reference method. The calibration curve was linear in the range between 1 and 1000 ng Br with a correlation coefficient R = 0.999. The limit of detection and characteristic mass of the method were 0.3 ng and 4.4 ng of Br.

  13. Determination of Chlorine in Milk via Molecular Absorption of SrCl Using High-Resolution Continuum Source Graphite Furnace Atomic Absorption Spectrometry.

    Science.gov (United States)

    Ozbek, Nil; Akman, Suleyman

    2016-07-20

    Total chlorine in milk was determined via the molecular absorption of diatomic strontium monochloride at 635.862 nm using high-resolution continuum source graphite furnace atomic absorption spectrometry. The effects of coating the graphite furnace, using different modifiers, amount of molecule-forming element, and different calibrants were investigated and optimized. Chlorine concentrations in milk samples were determined in a Zr-coated graphite furnace using 25 μg of Sr as the molecule-forming reagent and applying a pyrolysis temperature of 600 °C and a molecule-forming temperature of 2300 °C. Linearity was maintained up to 500 μg mL(-1) of Cl. The method was tested by analyzing a certified reference wastewater. The results were in the uncertainty limits of the certified value. The limit of detection of the method was 1.76 μg mL(-1). The chlorine concentrations in various cow milk samples taken from the market were found in the range of 588-1472 mg L(-1).

  14. Investigation of chemical modifiers for the direct determination of arsenic in fish oil using high-resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Pereira, Éderson R; de Almeida, Tarcísio S; Borges, Daniel L G; Carasek, Eduardo; Welz, Bernhard; Feldmann, Jörg; Campo Menoyo, Javier Del

    2016-04-01

    High-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) has been applied for the development of a method for the determination of total As in fish oil samples using direct analysis. The method does not use any sample pretreatment, besides dilution with 1-propanole, in order to decrease the oil viscosity. The stability and sensitivity of As were evaluated using ruthenium and iridium as permanent chemical modifiers and palladium added in solution over the sample. The best results were obtained with ruthenium as the permanent modifier and palladium in solution added to samples and standard solutions. Under these conditions, aqueous standard solutions could be used for calibration for the fish oil samples diluted with 1-propanole. The pyrolysis and atomization temperatures were 1400 °C and 2300 °C, respectively, and the limit of detection and characteristic mass were 30 pg and 43 pg, respectively. Accuracy and precision of the method have been evaluated using microwave-assisted acid digestion of the samples with subsequent determination by HR-CS GF AAS and ICP-MS; the results were in agreement (95% confidence level) with those of the proposed method. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. Micro-sampling method based on high-resolution continuum source graphite furnace atomic absorption spectrometry for calcium determination in blood and mitochondrial suspensions.

    Science.gov (United States)

    Gómez-Nieto, Beatriz; Gismera, Mª Jesús; Sevilla, Mª Teresa; Satrústegui, Jorgina; Procopio, Jesús R

    2017-08-01

    A micro-sampling and straightforward method based on high resolution continuum source atomic absorption spectrometry (HR-CS AAS) was developed to determine extracellular and intracellular Ca in samples of interest in clinical and biomedical analysis. Solid sampling platforms were used to introduce the micro-samples into the graphite furnace atomizer. The secondary absorption line for Ca, located at 239.856nm, was selected to carry out the measurements. Experimental parameters such as pyrolysis and atomization temperatures and the amount of sample introduced for the measurements were optimized. Calibration was performed using aqueous standards and the approach to measure at the wings of the absorption lines was employed for the expansion of the linear response range. The limit of detection was of 0.02mgL -1 Ca (0.39ng Ca) and the upper limit of linear range was increased up to 8.0mgL -1 Ca (160ng Ca). The proposed method was used to determine Ca in mitochondrial suspensions and whole blood samples with successful results. Adequate recoveries (within 91-107%) were obtained in the tests performed for validation purposes. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Rapid determination of 99Tc in environmental samples by high resolution ICP-MS coupled with on-line flow injection system

    International Nuclear Information System (INIS)

    Kim, C.K.; Kim, C.S.; Rho, B.H.; Lee, J.I.

    2002-01-01

    High resolution inductively coupled plasma mass spectrometry coupled with an on-line flow injection system (FI-HR-ICP-MS) was applied to determine the ultra-trace level 99 Tc in soil. The flow injection system (PrepLab TM ) was composed of two TEVA-Spec R resins, reduced remarkably the sample amounts and the analysis time, compared to the conventional analytical methods. In the flow injection system, Mo and Ru were sufficiently eliminated by using the flow injection system, with the decontamination factors of 1.6 x 10 4 and 9.9 x 10 5 , respectively. With the present method, it was possible to determine ultra-low level of 99 Tc in 3∼6 soil at 3-5 hours of analysis time per sample. The relative standard deviation for each sample was less than 4%. The detection limits for 99 Tc was 85 fg x ml -1 (0.05 mBq x ml -1 ), which was calculated from the three times standard deviation of the count rate of the blank. (author)

  17. Internal structure of InP/ZnS nanocrystals unraveled by high-resolution soft X-ray photoelectron spectroscopy.

    Science.gov (United States)

    Huang, Kai; Demadrille, Renaud; Silly, Mathieu G; Sirotti, Fausto; Reiss, Peter; Renault, Olivier

    2010-08-24

    High-energy resolution photoelectron spectroscopy (DeltaE InP/ZnS core/shell nanocrystals synthesized using a single-step procedure (core and shell precursors added at the same time), a homogeneously alloyed InPZnS core structure is evidenced by quantitative analysis of their In3d(5/2) spectra recorded at variable excitation energy. When using a two-step method (core InP nanocrystal synthesis followed by subsequent ZnS shell growth), XPS analysis reveals a graded core/shell interface. We demonstrate the existence of In-S and S(x)-In-P(1-x) bonding states in both types of InP/ZnS nanocrystals, which allows a refined view on the underlying reaction mechanisms.

  18. High-resolution structure of AKR1a4 in the apo form and its interaction with ligands

    International Nuclear Information System (INIS)

    Faucher, Frédérick; Jia, Zongchao

    2012-01-01

    Despite its high affinity for NADPH, AKR1a4 crystallized in the apo form, which is very rare for aldo-keto reductase enzymes. Aldo-keto reductase 1a4 (AKR1a4; EC 1.1.1.2) is the mouse orthologue of human aldehyde reductase (AKR1a1), the founding member of the AKR family. As an NADPH-dependent enzyme, AKR1a4 catalyses the conversion of d-glucuronate to l-gulonate. AKR1a4 is involved in ascorbate biosynthesis in mice, but has also recently been found to interact with SMAR1, providing a novel mechanism of ROS regulation by ATM. Here, the crystal structure of AKR1a4 in its apo form at 1.64 Å resolution as well as the characterization of the binding of AKR1a4 to NADPH and P44, a peptide derived from SMAR1, is presented

  19. Ultrasound-assisted single-drop microextraction for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Almeida, Jorge S.; Anunciação, Taiana A.; Brandão, Geovani C.; Dantas, Alailson F.; Lemos, Valfredo A.

    2015-01-01

    This work presents an ultrasound-assisted single-drop microextraction procedure for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry. Some initial tests showed that the best extraction efficiency was obtained when using ultrasound instead of mechanical agitation, indicating that acoustic cavitation improved the extraction process. Nitric, hydrochloric and acetic acids were evaluated for use in the extraction process, and HNO 3 gave the best results. A two-level full-factorial design was applied to investigate the best conditions for the extraction of Cd from the oil samples. The influences of the sonication amplitude, time and temperature of the extraction were evaluated. The results of the design revealed that all of the variables had a significant effect on the experimental results. Afterward, a Box–Behnken design was applied to determine the optimum conditions for the determination of cadmium in vegetable oil samples. According to a multivariate study, the optimum conditions were as follows: sonication amplitude of 60%, extraction time of 15 min, extraction temperature of 46 °C and 0.1 mol L −1 HNO 3 as the extractor solution. Under optimized conditions, the developed method allows for the determination of Cd in oil samples with a limit of quantification of 7.0 ng kg −1 . Addition and recovery experiments were performed in vegetable oil samples to evaluate the accuracy of the method, and the recoveries obtained varied from 90% to 115%. The samples were also analyzed after the acid digestion procedure, and the paired t-test (95% confidence level) did not show significant differences from the proposed method. - Highlights: • The determination of cadmium in vegetable oils was developed using UA-SDME. • HR-CS ET-AAS was employed as a detection technique with direct drop sampling. • The procedure allowed for a reduction in the consumption of reagents and samples

  20. Ultrasound-assisted single-drop microextraction for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Almeida, Jorge S.; Anunciação, Taiana A. [Departamento de Química Analítica, Instituto de Química, Universidade Federal da Bahia, Campus Universitário de Ondina, Salvador, Bahia 40170-280 (Brazil); Brandão, Geovani C. [Departamento de Química Analítica, Instituto de Química, Universidade Federal da Bahia, Campus Universitário de Ondina, Salvador, Bahia 40170-280 (Brazil); INCT de Energia e Ambiente, Instituto de Química, Universidade Federal da Bahia, Campus Universitário de Ondina, Salvador, Bahia 40170-280 (Brazil); Dantas, Alailson F. [Departamento de Química Analítica, Instituto de Química, Universidade Federal da Bahia, Campus Universitário de Ondina, Salvador, Bahia 40170-280 (Brazil); Lemos, Valfredo A. [Laboratório de Química Analítica (LQA), Universidade Estadual do Sudoeste da Bahia, Campus de Jequié, Jequié, Bahia 45506-191 (Brazil); and others

    2015-05-01

    This work presents an ultrasound-assisted single-drop microextraction procedure for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry. Some initial tests showed that the best extraction efficiency was obtained when using ultrasound instead of mechanical agitation, indicating that acoustic cavitation improved the extraction process. Nitric, hydrochloric and acetic acids were evaluated for use in the extraction process, and HNO{sub 3} gave the best results. A two-level full-factorial design was applied to investigate the best conditions for the extraction of Cd from the oil samples. The influences of the sonication amplitude, time and temperature of the extraction were evaluated. The results of the design revealed that all of the variables had a significant effect on the experimental results. Afterward, a Box–Behnken design was applied to determine the optimum conditions for the determination of cadmium in vegetable oil samples. According to a multivariate study, the optimum conditions were as follows: sonication amplitude of 60%, extraction time of 15 min, extraction temperature of 46 °C and 0.1 mol L{sup −1} HNO{sub 3} as the extractor solution. Under optimized conditions, the developed method allows for the determination of Cd in oil samples with a limit of quantification of 7.0 ng kg{sup −1}. Addition and recovery experiments were performed in vegetable oil samples to evaluate the accuracy of the method, and the recoveries obtained varied from 90% to 115%. The samples were also analyzed after the acid digestion procedure, and the paired t-test (95% confidence level) did not show significant differences from the proposed method. - Highlights: • The determination of cadmium in vegetable oils was developed using UA-SDME. • HR-CS ET-AAS was employed as a detection technique with direct drop sampling. • The procedure allowed for a reduction in the consumption of reagents and

  1. High resolution studies of barium Rydberg states

    International Nuclear Information System (INIS)

    Eliel, E.R.

    1982-01-01

    The subtle structure of Rydberg states of barium with orbital angular momentum 0, 1, 2 and 3 is investigated. Some aspects of atomic theory for a configuration with two valence electrons are reviewed. The Multi Channel Quantum Defect Theory (MQDT) is concisely introduced as a convenient way to describe interactions between Rydberg series. Three high-resolution UV studies are presented. The first two, presenting results on a transition in indium and europium serve as an illustration of the frequency doubling technique. The third study is of hyperfine structure and isotope shifts in low-lying p states in Sr and Ba. An extensive study of the 6snp and 6snf Rydberg states of barium is presented with particular emphasis on the 6snf states. It is shown that the level structure cannot be fully explained with the model introduced earlier. Rather an effective two-body spin-orbit interaction has to be introduced to account for the observed splittings, illustrating that high resolution studies on Rydberg states offer an unique opportunity to determine the importance of such effects. Finally, the 6sns and 6snd series are considered. The hyperfine induced isotope shift in the simple excitation spectra to 6sns 1 S 0 is discussed and attention is paid to series perturbers. It is shown that level mixing parameters can easily be extracted from the experimental data. (Auth.)

  2. High resolution spectroscopic mapping imaging applied in situ to multilayer structures for stratigraphic identification of painted art objects

    Science.gov (United States)

    Karagiannis, Georgios Th.

    2016-04-01

    The development of non-destructive techniques is a reality in the field of conservation science. These techniques are usually not so accurate, as the analytical micro-sampling techniques, however, the proper development of soft-computing techniques can improve their accuracy. In this work, we propose a real-time fast acquisition spectroscopic mapping imaging system that operates from the ultraviolet to mid infrared (UV/Vis/nIR/mIR) area of the electromagnetic spectrum and it is supported by a set of soft-computing methods to identify the materials that exist in a stratigraphic structure of paint layers. Particularly, the system acquires spectra in diffuse-reflectance mode, scanning in a Region-Of-Interest (ROI), and having wavelength range from 200 up to 5000 nm. Also, a fuzzy c-means clustering algorithm, i.e., the particular soft-computing algorithm, produces the mapping images. The evaluation of the method was tested on a byzantine painted icon.

  3. High-resolution positron Q-value measurements and nuclear-structure studies far from the stability line. Progress report

    International Nuclear Information System (INIS)

    Avignone, F.T. III.

    1981-01-01

    Extensive data analysis and theoretical analysis has been done to complete the extensive decay scheme investigation of 206 208 Fr and the level structures of 206 208 Rn. A final version of a journal article is presented in preprint form. Extensive Monte Carlo calculations have been made to correct the end point energies of positron spectra taken with intrinsic Ge detectors for annihilation radiation interferences. These calculations were tested using the decay of 82 Sr which has previously measured positron branches. This technique was applied to the positron spectra collected at the on-line UNISOR isotope separator. The reactions used were 60 Ni( 20 Ne;p2n) 77 Rb and 60 Ni( 20 Ne;pn) 78 Rb. Values for 5, γ-β + coincidence positron end point energies are given for the decay of 77 Rb. The implied Q-value is 5.075 +- 0.010 MeV. A complete paper on the calculated corrections is presented. A flow chart of a more complete program which accounts for positrons scattering out of the detector and for bremsstralung radiation is also presented. End-point energies of four β + branches in 77 Rb are given as well as a proposed energy level scheme of 75 Kr based on γ-γ coincidence data taken at UNISOR

  4. High resolution LiDAR measurements reveal fine internal structure and variability of sediment-carrying coastal plume

    Science.gov (United States)

    Zavialov, P. O.; Pelevin, V. V.; Belyaev, N. A.; Izhitskiy, A. S.; Konovalov, B. V.; Krementskiy, V. V.; Goncharenko, I. V.; Osadchiev, A. A.; Soloviev, D. M.; Garcia, C. A. E.; Pereira, E. S.; Sartorato, L.; Moller, O. O.

    2018-05-01

    We report results of a field survey conducted in the buoyant, sediment-carrying coastal plume generated by the discharge from the Patos Lagoon, the World's largest choked lagoon. The concentration of total suspended matter (TSM) and organic matter (as represented by total organic carbon, TOC) were mapped using an ultraviolet fluorescent LiDAR, which allowed for extensive data coverage (total of 79,387 simultaneous determinations of TSM and TOC) during 3 consecutive days. These observations were accompanied by hydrographic measurements from the ship and at a mooring station. We first describe synoptic variability of the plume, which responded energetically to wind forcing. We then analyze the TSM, TOC and hydrographic data jointly and develop a simple approach to estimate the rates of suspended matter removal from the upper layer due to gravitational settling and turbulent mixing based on relative changes in TSM and TOC concentrations. Four distinct regions within the plume exhibiting different dynamics of suspended and dissolved constituents were identified on this basis.

  5. Determination of mercury in airborne particulate matter collected on glass fiber filters using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sampling

    Energy Technology Data Exchange (ETDEWEB)

    Araujo, Rennan G.O., E-mail: rgoa01@terra.com.br [Laboratorio de Quimica Analitica Ambiental, Departamento de Quimica, Universidade Federal de Sergipe, Campus Sao Cristovao, 49.100-000, Sao Cristovao, SE (Brazil); Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil); Vignola, Fabiola; Castilho, Ivan N.B. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil); Borges, Daniel L.G.; Welz, Bernhard [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900, Florianopolis, SC (Brazil); Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Vale, Maria Goreti R. [Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Instituto de Quimica, Universidade Federal do Rio Grande do Sul, 91501-970 Porto Alegre, RS (Brazil); Smichowski, Patricia [Comision Nacional de Energia Atomica (CNEA) and Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET), Buenos Aires (Argentina); Ferreira, Sergio L.C. [Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Instituto de Quimica, Universidade Federal da Bahia, 40170-290, Salvador, BA (Brazil); Becker-Ross, Helmut [Leibniz-Institut fuer Analytische Wissenschaften-ISAS-e.V., Department Berlin, 12489 Berlin (Germany)

    2011-05-15

    A study has been undertaken to assess the capability of high-resolution continuum source graphite furnace atomic absorption spectrometry for the determination of mercury in airborne particulate matter (APM) collected on glass fiber filters using direct solid sampling. The main Hg absorption line at 253.652 nm was used for all determinations. The certified reference material NIST SRM 1648 (Urban Particulate Matter) was used to check the accuracy of the method, and good agreement was obtained between published and determined values. The characteristic mass was 22 pg Hg. The limit of detection (3{sigma}), based on ten atomizations of an unexposed filter, was 40 ng g{sup -1}, corresponding to 0.12 ng m{sup -3} in the air for a typical air volume of 1440 m{sup 3} collected within 24 h. The limit of quantification was 150 ng g{sup -1}, equivalent to 0.41 ng m{sup -3} in the air. The repeatability of measurements was better than 17% RSD (n = 5). Mercury concentrations found in filter samples loaded with APM collected in Buenos Aires, Argentina, were between < 40 ng g{sup -1} and 381 {+-} 24 ng g{sup -1}. These values correspond to a mercury concentration in the air between < 0.12 ng m{sup -3} and 1.47 {+-} 0.09 ng m{sup -3}. The proposed procedure was found to be simple, fast and reliable, and suitable as a screening procedure for the determination of mercury in APM samples.

  6. Direct determination of chromium in infant formulas employing high-resolution continuum source electrothermal atomic absorption spectrometry and solid sample analysis.

    Science.gov (United States)

    Silva, Arlene S; Brandao, Geovani C; Matos, Geraldo D; Ferreira, Sergio L C

    2015-11-01

    The present work proposed an analytical method for the direct determination of chromium in infant formulas employing the high-resolution continuum source electrothermal atomic absorption spectrometry combined with the solid sample analysis (SS-HR-CS ET AAS). Sample masses up to 2.0mg were directly weighted on a solid sampling platform and introduced into the graphite tube. In order to minimize the formation of carbonaceous residues and to improve the contact of the modifier solution with the solid sample, a volume of 10 µL of a solution containing 6% (v/v) H2O2, 20% (v/v) ethanol and 1% (v/v) HNO3 was added. The pyrolysis and atomization temperatures established were 1600 and 2400 °C, respectively, using magnesium as chemical modifier. The calibration technique was evaluated by comparing the slopes of calibration curves established using aqueous and solid standards. This test revealed that chromium can be determined employing the external calibration technique using aqueous standards. Under these conditions, the method developed allows the direct determination of chromium with limit of quantification of 11.5 ng g(-1), precision expressed as relative standard deviation (RSD) in the range of 4.0-17.9% (n=3) and a characteristic mass of 1.2 pg of chromium. The accuracy was confirmed by analysis of a certified reference material of tomato leaves furnished by National Institute of Standards and Technology. The method proposed was applied for the determination of chromium in five different infant formula samples. The chromium content found varied in the range of 33.9-58.1 ng g(-1) (n=3). These samples were also analyzed employing ICP-MS. A statistical test demonstrated that there is no significant difference between the results found by two methods. The chromium concentrations achieved are lower than the maximum limit permissible for chromium in foods by Brazilian Legislation. Copyright © 2015. Published by Elsevier B.V.

  7. Ultrasound-assisted single-drop microextraction for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Almeida, Jorge S.; Anunciação, Taiana A.; Brandão, Geovani C.; Dantas, Alailson F.; Lemos, Valfredo A.; Teixeira, Leonardo S. G.

    2015-05-01

    This work presents an ultrasound-assisted single-drop microextraction procedure for the determination of cadmium in vegetable oils using high-resolution continuum source electrothermal atomic absorption spectrometry. Some initial tests showed that the best extraction efficiency was obtained when using ultrasound instead of mechanical agitation, indicating that acoustic cavitation improved the extraction process. Nitric, hydrochloric and acetic acids were evaluated for use in the extraction process, and HNO3 gave the best results. A two-level full-factorial design was applied to investigate the best conditions for the extraction of Cd from the oil samples. The influences of the sonication amplitude, time and temperature of the extraction were evaluated. The results of the design revealed that all of the variables had a significant effect on the experimental results. Afterward, a Box-Behnken design was applied to determine the optimum conditions for the determination of cadmium in vegetable oil samples. According to a multivariate study, the optimum conditions were as follows: sonication amplitude of 60%, extraction time of 15 min, extraction temperature of 46 °C and 0.1 mol L- 1 HNO3 as the extractor solution. Under optimized conditions, the developed method allows for the determination of Cd in oil samples with a limit of quantification of 7.0 ng kg- 1. Addition and recovery experiments were performed in vegetable oil samples to evaluate the accuracy of the method, and the recoveries obtained varied from 90% to 115%. The samples were also analyzed after the acid digestion procedure, and the paired t-test (95% confidence level) did not show significant differences from the proposed method.

  8. Nuclear structure studies using the high resolution spectrometer at the Los Alamos Clinton P. Anderson Meson Physics Facility: Progress report, [1986-1987

    International Nuclear Information System (INIS)

    Hoffmann, G.W.

    1986-12-01

    A major part of the work done this past year was associated with research conducted at the Los Alamos Clinton P. Anderson Meson Physics Facility (LAMPF) using the High Resolution Spectrometer (HRS) and the External Proton Beam (EPB). The research focussed on (1) providing p + nucleus data which test nonrelativistic and relativistic models of the medium energy proton + nucleus interaction, (2) providing (p,p) and (p,n) data which are to be analyzed to provide new nuclear structure information (both ground state and excited state), (3) providing nucleon + nucleon data to aid in the systematic study of the fundamental nucleon-nucleon interaction, (4) developing and improving the pA models themselves, and (5) initiating new experimental programs whose goals are to search for new phenomena in nuclear physics

  9. Glacio-tectonic thrust and deformation structures in the Vejle Fjord, Denmark revealed by high-resolution subbottom-profile data

    DEFF Research Database (Denmark)

    Andresen, Katrine Juul; Boldreel, Lars Ole; Wahlgreen, Katrine Bak

    Surface geomorphological features and partial cliff exposures up till now represent the predominant source of information of glaciation related deformation in Denmark. In this study we apply high-resolution marine reflection seismic data from the Vejle Fjord area, supported by gravity and Rumohr...... coring, to document intense glacio-tectonic deformation in the shallow subsurface of Denmark. The subbottom profiler seismic data have a peak frequency around 13 kHz and a vertical resolution in the order of 10-20 cm. The data reveal several variations of glacio-tectonic deformation structures, primarily...... movements from outcrops and shallow cores. The subbottom profiler data provides larger (longer and deeper) sectional views on for instance deformation and deposition complexes related to ice progressions and retreats and thus represents a very good supplement and valuable input to field mapping and outcrops...

  10. High Resolution and Differential PIXE combined with RBS, EBS and AFM analysis of magnesium titanate (MgTiO3) multilayer structures

    International Nuclear Information System (INIS)

    Reis, M.A.; Alves, L.C.; Barradas, N.P.; Chaves, P.C.; Nunes, B.; Taborda, A.; Surendran, K.P.; Wu, A.; Vilarinho, P.M.; Alves, E.

    2010-01-01

    Thorough structural characterization of deep laying thin film, including the inference of interdiffusion profiles is frequently a complex problem. The use of RBS/PIXE holistic approaches, already shown to represent a powerful method, sometimes faces difficulties if standard experimental procedures are used. In this work, following a series of 4 He Rutherford backscattering and 1 H elastic backscattering experiments, carried out to study the influence of SrTiO 3 as a possible cladding layer between Pt/TiO 2 /SiO 2 /(1 0 0)Si substrates and MgTiO 3 films, a simple holistic RBS-PIXE is shown to be not enough for the solution of such a problem. Establishing of the Sr depth profile, was only possible after AFM, High-Resolution EDS PIXE and differential PIXE analysis were carried out. Results, problems faced and conclusions obtained are presented.

  11. A Method for Simultaneous Determination of 20 Fusarium Toxins in Cereals by High-Resolution Liquid Chromatography-Orbitrap Mass Spectrometry with a Pentafluorophenyl Column

    Science.gov (United States)

    Tamura, Masayoshi; Mochizuki, Naoki; Nagatomi, Yasushi; Harayama, Koichi; Toriba, Akira; Hayakawa, Kazuichi

    2015-01-01

    A high-resolution liquid chromatography-Orbitrap mass spectrometry (LC-Orbitrap MS) method was developed for simultaneous determination of 20 Fusarium toxins (nivalenol, fusarenon-X, deoxynivalenol, 3-acetyl deoxynivalenol, 15-acetyl deoxynivalenol, HT-2 toxin, T-2 toxin, neosolaniol, diacetoxyscirpenol, fumonisin B1, fumonisin B2, fumonisin B3, fumonisin A1, fumonisin A2, fumonisin A3, zearalenone, α-zearalenol, β-zearalenol, α-zearalanol, and β-zearalanol) in cereals. The separation of 20 Fusarium toxins with good peak shapes was achieved using a pentafluorophenyl column, and Orbitrap MS was able to detect accurately from cereal matrix components within ±0.77 ppm. The samples were prepared using a QuEChERS kit for extraction and a multifunctional cartridge for purification. The linearity, repeatability, and recovery of the method were >0.9964, 0.8%–14.7%, and 71%–106%, respectively. Using this method, an analysis of 34 commercially available cereals detected the presence of deoxynivalenol, 15-acetyl deoxynivalenol, fumonisin B1, fumonisin B2, fumonisin B3, fumonisn A1, fumonisin A2, fumonisin A3, and zearalenone in corn samples with high concentration and frequency. Trichothecenes was detected from wheat samples with high frequency; in particular, the concentration of deoxynivalenol was high. Conversely, α-zearalenol, β-zearalenol, α-zearalanol, and β-zearalanol were not detected in any of the samples. PMID:26008230

  12. Determination of Triazine Herbicides in Drinking Water by Dispersive Micro Solid Phase Extraction with Ultrahigh-Performance Liquid Chromatography-High-Resolution Mass Spectrometric Detection.

    Science.gov (United States)

    Chen, Dawei; Zhang, Yiping; Miao, Hong; Zhao, Yunfeng; Wu, Yongning

    2015-11-11

    A novel dispersive micro solid phase extraction (DMSPE) method based on a polymer cation exchange material (PCX) was applied to the simultaneous determination of the 30 triazine herbicides in drinking water with ultrahigh-performance liquid chromatography-high-resolution mass spectrometric detection. Drinking water samples were acidified with formic acid, and then triazines were adsorbed by the PCX sorbent. Subsequently, the analytes were eluted with ammonium hydroxide/acetonitrile. The chromatographic separation was performed on an HSS T3 column using water (4 mM ammonium formate and 0.1% formic acid) and acetonitrile (0.1% formic acid) as the mobile phase. The method achieved LODs of 0.2-30.0 ng/L for the 30 triazines, with recoveries in the range of 70.5-112.1%, and the precision of the method was better than 12.7%. These results indicated that the proposed method had the advantages of convenience and high efficiency when applied to the analysis of the 30 triazines in drinking water.

  13. Evaluation of solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for direct determination of chromium in medicinal plants

    International Nuclear Information System (INIS)

    Virgilio, Alex; Nóbrega, Joaquim A.; Rêgo, Jardes F.; Neto, José A. Gomes

    2012-01-01

    A method for Cr determination in medicinal plants using direct solid sampling graphite furnace high-resolution continuum source atomic absorption spectrometry was developed. Modifiers were dispensable. Pyrolysis and atomization temperatures were 1500 °C and 2400 °C, respectively. Slopes of calibration curves (50–750 pg Cr, R 2 > 0.999) using aqueous and solid standards coincides in 96%, indicated feasibility of aqueous calibration for solid sampling of medicinal plants. Accuracy was checked by analysis of four plant certified reference materials. Results were in agreement at 95% confidence level with certified and non-certified values. Ten samples of medicinal plants were analyzed and Cr contents were in the 1.3–17.7 μg g −1 Cr range. The highest RSD (n = 5) was 15.4% for the sample Melissa officinalis containing 13.9 ± 2.1 μg g −1 Cr. The limit of detection was 3.3 ng g −1 Cr. - Highlights: ► Direct solid sampling is first time employed for Cr in plant materials. ► Calibration curves with liquids and solids are coincident. ► Microanalysis of plants for Cr is validated by reference materials. ► The proposed HR-CS GF AAS method is environmental friendly.

  14. Evaluation of solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for direct determination of chromium in medicinal plants

    Energy Technology Data Exchange (ETDEWEB)

    Virgilio, Alex; Nobrega, Joaquim A. [Department of Chemistry, Federal University of Sao Carlos, Post Office Box 676, 13560-970, Sao Carlos-SP (Brazil); Rego, Jardes F. [Department of Analytical Chemistry, Institute of Chemistry, Sao Paulo State University-UNESP, Post Office Box 355, 14801-970, Araraquara-SP (Brazil); Neto, Jose A. Gomes, E-mail: anchieta@iq.unesp.br [Department of Analytical Chemistry, Institute of Chemistry, Sao Paulo State University-UNESP, Post Office Box 355, 14801-970, Araraquara-SP (Brazil)

    2012-12-01

    A method for Cr determination in medicinal plants using direct solid sampling graphite furnace high-resolution continuum source atomic absorption spectrometry was developed. Modifiers were dispensable. Pyrolysis and atomization temperatures were 1500 Degree-Sign C and 2400 Degree-Sign C, respectively. Slopes of calibration curves (50-750 pg Cr, R{sup 2} > 0.999) using aqueous and solid standards coincides in 96%, indicated feasibility of aqueous calibration for solid sampling of medicinal plants. Accuracy was checked by analysis of four plant certified reference materials. Results were in agreement at 95% confidence level with certified and non-certified values. Ten samples of medicinal plants were analyzed and Cr contents were in the 1.3-17.7 {mu}g g{sup -1} Cr range. The highest RSD (n = 5) was 15.4% for the sample Melissa officinalis containing 13.9 {+-} 2.1 {mu}g g{sup -1} Cr. The limit of detection was 3.3 ng g{sup -1} Cr. - Highlights: Black-Right-Pointing-Pointer Direct solid sampling is first time employed for Cr in plant materials. Black-Right-Pointing-Pointer Calibration curves with liquids and solids are coincident. Black-Right-Pointing-Pointer Microanalysis of plants for Cr is validated by reference materials. Black-Right-Pointing-Pointer The proposed HR-CS GF AAS method is environmental friendly.

  15. Determination of the activity concentration levels of the artificial radionuclide137Cs in soil samples collected from Qatar using high-resolution gamma-ray spectrometry

    Science.gov (United States)

    Al-Sulaiti, Huda; Nasir, Tabassum; Al Mugren, K. S.; Alkhomashi, N.; Al-Dahan, N.; Al-Dosari, M.; Bradley, D. A.; Bukhari, S.; Regan, P. H.; Santawamaitre, T.; Malain, D.; Habib, A.; Al-Dosari, Hanan; Daar, Eman

    2016-09-01

    The goal of this study was to establish the first baseline measurements for radioactivity concentration of the artificial radionuclide 137Cs in soil samples collected from the Qatarian peninsula. The work focused on the determination of the activity concentrations levels of man-made radiation in 129 soil samples collected across the landscape of the State of Qatar. All the samples were collected before the most recent accident in Japan, “the 2011 Fukushima Dai-ichi nuclear power plant accident”. The activity concentrations have been measured via high-resolution gamma-ray spectrometry using a hyper-pure germanium detector situated in a low-background environment with a copper inner-plated passive lead shield. A radiological map showing the activity concentrations of 137Cs is presented in this work. The concentration wasfound to range from 0.21 to 15.41 Bq/kg. The highest activity concentration of 137Cs was observed in sample no. 26 in North of Qatar. The mean value was found to be around 2.15 ± 0.27 Bq/kg. These values lie within the expected range relative to the countries in the region. It is expected that this contamination is mainly due to the Chernobyl accident on 26 April 1986, but this conclusion cannot be confirmed because of the lack of data before this accident.

  16. Development and validation of a QuEChERS method coupled to liquid chromatography and high resolution mass spectrometry to determine pyrrolizidine and tropane alkaloids in honey.

    Science.gov (United States)

    Martinello, Marianna; Borin, Alice; Stella, Roberto; Bovo, Davide; Biancotto, Giancarlo; Gallina, Albino; Mutinelli, Franco

    2017-11-01

    Awareness about pyrrolizidine alkaloids (PAs) and tropane alkaloids (TAs) in food was recently raised by the European Food Safety Authority stressing the lack of data and gaps of knowledge required to improve the risk assessment strategy. The present study aimed at the elaboration and validation of a method to determine PAs and TAs in honey. QuEChERS sample treatment and liquid chromatography coupled to hybrid high resolution mass spectrometry, were used. The method resulted in good linearity (R 2 >0.99) and low limits of detection and quantification, ranging from 0.04 to 0.2µgkg -1 and from 0.1 to 0.7µgkg -1 respectively. Recoveries ranged from 92.3 to 114.8% with repeatability lying between 0.9 and 15.1% and reproducibility between 1.1 and 15.6%. These performances demonstrate the selectivity and sensitivity of the method for simultaneous trace detection and quantification of PAs and TAs in honey, verified through the analysis of forty commercial samples. Copyright © 2017 Elsevier Ltd. All rights reserved.

  17. Fast sequential multi-element determination of major and minor elements in environmental samples and drinking waters by high-resolution continuum source flame atomic absorption spectrometry.

    Science.gov (United States)

    Gómez-Nieto, Beatriz; Gismera, Ma Jesús; Sevilla, Ma Teresa; Procopio, Jesús R

    2015-01-07

    The fast sequential multi-element determination of 11 elements present at different concentration levels in environmental samples and drinking waters has been investigated using high-resolution continuum source flame atomic absorption spectrometry. The main lines for Cu (324.754 nm), Zn (213.857 nm), Cd (228.802 nm), Ni (232.003 nm) and Pb (217.001 nm), main and secondary absorption lines for Mn (279.482 and 279.827 nm), Fe (248.327, 248.514 and 302.064 nm) and Ca (422.673 and 239.856 nm), secondary lines with different sensitivities for Na (589.592 and 330.237 nm) and K (769.897 and 404.414 nm) and a secondary line for Mg (202.582 nm) have been chosen to perform the analysis. A flow injection system has been used for sample introduction so sample consumption has been reduced up to less than 1 mL per element, measured in triplicate. Furthermore, the use of multiplets for Fe and the side pixel registration approach for Mg have been studied in order to reduce sensitivity and extend the linear working range. The figures of merit have been calculated and the proposed method was applied to determine these elements in a pine needles reference material (SRM 1575a), drinking and natural waters and soil extracts. Recoveries of analytes added at different concentration levels to water samples and extracts of soils were within 88-115% interval. In this way, the fast sequential multi-element determination of major and minor elements can be carried out, in triplicate, with successful results without requiring additional dilutions of samples or several different strategies for sample preparation using about 8-9 mL of sample. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. Abstracts of International Conference on Experimental and Computing Methods in High Resolution Diffraction Applied for Structure Characterization of Modern Materials - HREDAMM

    International Nuclear Information System (INIS)

    2004-01-01

    The conference addressed all aspects of high resolution diffraction. The topics of meeting include advanced experimental diffraction methods and computer data analysis for characterization of modern materials as well as the progress and new achievements in high resolution diffraction (X-ray, electrons, neutrons). Application of these methods for characterization of modern materials are widely presented among the invited, oral and poster contributions

  19. Method validation for high resolution sector field inductively coupled plasma mass spectrometry determination of the emerging contaminants in the open ocean: Rare earth elements as a case study

    Science.gov (United States)

    Wysocka, Irena; Vassileva, Emilia

    2017-02-01

    Analytical procedure for the determination of fourteen rare earth elements (REEs) in the seawater samples has been developed and validated. The elements (La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) at ultra-trace level were measured by high resolution sector field inductively coupled plasma mass spectrometry (HR ICP-SFMS) after off-line analytes pre-concentration and matrix separation. The sample pre-treatment was carried out by commercially available automated system seaFAST-pico™, which is a low-pressure ion chromatography technique, based on solid phase extraction principles. Efficient elimination of seawater matrix and up to 50-fold pre-concentration of REEs enabled their accurate and precise quantification at ng L- 1 level. A validation approach in line with the requirements of ISO/IEC 17025 standard and Eurachem guidelines were followed. With this in mind, selectivity, working range, linearity, recovery (from 92% to 102%), repeatability (1%-4%), intermediate precision (2%-6%), limits of detection (0.001-0.08 ng L- 1) were systematically assessed. The total uncertainty associated to each result was estimated and the main sources of uncertainty sorted out. All major contributions to the combined uncertainty of the obtained results were identified and propagated together, following the ISO/GUM guidelines. The relative expanded uncertainty was estimated at range from 10.4% to 11.6% (k = 2). Demonstration of traceability of measurement results was also presented. Due to the low limits of detection, this method enables the determination of ultra-low levels of REEs in the open seawater as well as small variations in their concentrations. The potential of the proposed analytical procedure, based on combination of seaFAST-pico™ for sample preparation and HR ICP-SFMS, was demonstrated by direct analysis of seawater form different regions of the world.

  20. Aortic and Cardiac Structure and Function Using High-Resolution Echocardiography and Optical Coherence Tomography in a Mouse Model of Marfan Syndrome.

    Directory of Open Access Journals (Sweden)

    Ling Lee

    Full Text Available Marfan syndrome (MFS is an autosomal-dominant disorder of connective tissue caused by mutations in the fibrillin-1 (FBN1 gene. Mortality is often due to aortic dissection and rupture. We investigated the structural and functional properties of the heart and aorta in a [Fbn1C1039G/+] MFS mouse using high-resolution ultrasound (echo and optical coherence tomography (OCT. Echo was performed on 6- and 12-month old wild type (WT and MFS mice (n = 8. In vivo pulse wave velocity (PWV, aortic root diameter, ejection fraction, stroke volume, left ventricular (LV wall thickness, LV mass and mitral valve early and atrial velocities (E/A ratio were measured by high resolution echocardiography. OCT was performed on 12-month old WT and MFS fixed mouse hearts to measure ventricular volume and mass. The PWV was significantly increased in 6-mo MFS vs. WT (366.6 ± 19.9 vs. 205.2 ± 18.1 cm/s; p = 0.003 and 12-mo MFS vs. WT (459.5 ± 42.3 vs. 205.3 ± 30.3 cm/s; p< 0.0001. PWV increased with age in MFS mice only. We also found a significantly enlarged aortic root and decreased E/A ratio in MFS mice compared with WT for both age groups. The [Fbn1C1039G/+] mouse model of MFS replicates many of the anomalies of Marfan patients including significant aortic dilation, central aortic stiffness, LV systolic and diastolic dysfunction. This is the first demonstration of the direct measurement in vivo of pulse wave velocity non-invasively in the aortic arch of MFS mice, a robust measure of aortic stiffness and a critical clinical parameter for the assessment of pathology in the Marfan syndrome.

  1. High-Resolution Digital Elevation Modeling from TLS and UAV Campaign Reveals Structural Complexity at the 2014/2015 Holuhraun Eruption Site, Iceland

    Directory of Open Access Journals (Sweden)

    Daniel Müller

    2017-07-01

    Full Text Available Fissure eruptions are commonly linked to magma dikes at depth and are associated with elastic and inelastic surface deformation. Elastic deformation is well described by subsidence occurring above the dike plane and uplift and lateral widening occurring perpendicular to the dike plane. Inelastic deformation is associated with the formation of a graben, which is bordered by graben parallel faults that might express as sets of fractures at the surface. Additionally, secondary structures, such as push-ups, bends and step overs, yield information about the deforming domain. However, once these structures are formed during fissure eruptions, they are rarely preserved in nature, due to the effects of rapid erosion, sediment coverage or overprinting by other faulting events. Therefore, simple normal fault displacements are commonly assumed at dikes. At the 2014/2015 Holuhraun eruption sites (Iceland, increasing evidence suggests that developing fractures exhibited variations in their displacement modes. In an attempt to investigate these variations, a fieldwork mapping project combining Terrestrial Laser Scanning (TLS and Unmanned Aerial Vehicle (UAV-based aerophoto analysis was undertaken. Using these data, we generated local high-resolution Digital Elevation Models (DEMs and a structural map that facilitated the identification of kinematic indicators and the assessment of the observed structures. We identified 315 fracture segments from these satellite data. We measured the strike directions of single segments, including the amount of opening and opening angles, which indicate that many of the measured fractures show transtensional dislocations. Of these, ~81% exhibit a significant left-lateral component and only ~17% exhibit a right-lateral component. Here, we demonstrate that the local complexities in these fracture traces and geometries are closely related to variations in their transtensional opening directions. Moreover, we identified local

  2. Isolation of dissolved organic matter from permafrost soil and freshwater environments of the Kolyma River basin, east Siberia, for high resolution structural analysis

    Science.gov (United States)

    Dubinenkov, I. V.; Perminova, I. V.; Bulygina, E. B.; Holmes, R. M.; Davydov, S.; Mann, P. J.; Vonk, J.; Zimov, S. A.

    2010-12-01

    The Arctic and Subarctic ecosystems are known to be the most vulnerable with respect to climate change. Hence, research on carbon cycling in the Arctic region is very important for understanding the current climatic trends and their consequences. The Kolyma River watershed is one of the Arctic Ocean’s largest. It is dominated by continuous permafrost which is underlain with rich organic soils susceptible to increased fluvial transport. The thaw of permafrost enhanced due to global warming might provide additional large source of organic carbon to the Kolyma River and to the Arctic Ocean as a whole. For estimating the contribution of this source to the total pool of organic carbon, specific structural features of permafrost dissolved organic matter (DOM) as opposed to the waterborne DOM of the Kolyma River should be identified and monitored. The objective of this work was to isolate a representive set of the DOM samples from permafrost soil and freshwater environments of the Kolyma River basin suitable for further structural analysis using high resolution Fourier Transform Ion Cyclotron Resonance Mass Spectroscopy (FTICR-MS) and 1H NMR spectroscopy. The isolation protocol of DOM used in this study has been developed by Dittmar et al, 2008 for sampling marine DOM for NMR studies. It is based on the solid phase extraction of DOM from seawater using PPL Varian Bond Elute cartridges Those cartridges were shown to possess the highest efficiency in DOM isolation from marine water. Prior to discharge through the cartridge, a water sample was filtered through 0.45 μm filter for separation of particulate matter and acidified to pH 2 using HCl. About 50mg of DOM could be sequestered from aqueous phase using one cartridge. Sorption extent was monitored by measurements of DOC concentration and UV-vis spectra at the inlet and outlet of the cartridge. It was determined that from 60 to 65% of the total DOC could be extracted from the tested samples of freshwater. As a result

  3. Raman spectroscopy adds complementary detail to the high-resolution x-ray crystal structure of photosynthetic PsbP from Spinacia oleracea.

    Directory of Open Access Journals (Sweden)

    Vladimir Kopecky

    Full Text Available Raman microscopy permits structural analysis of protein crystals in situ in hanging drops, allowing for comparison with Raman measurements in solution. Nevertheless, the two methods sometimes reveal subtle differences in structure that are often ascribed to the water layer surrounding the protein. The novel method of drop-coating deposition Raman spectropscopy (DCDR exploits an intermediate phase that, although nominally "dry," has been shown to preserve protein structural features present in solution. The potential of this new approach to bridge the structural gap between proteins in solution and in crystals is explored here with extrinsic protein PsbP of photosystem II from Spinacia oleracea. In the high-resolution (1.98 Å x-ray crystal structure of PsbP reported here, several segments of the protein chain are present but unresolved. Analysis of the three kinds of Raman spectra of PsbP suggests that most of the subtle differences can indeed be attributed to the water envelope, which is shown here to have a similar Raman intensity in glassy and crystal states. Using molecular dynamics simulations cross-validated by Raman solution data, two unresolved segments of the PsbP crystal structure were modeled as loops, and the amino terminus was inferred to contain an additional beta segment. The complete PsbP structure was compared with that of the PsbP-like protein CyanoP, which plays a more peripheral role in photosystem II function. The comparison suggests possible interaction surfaces of PsbP with higher-plant photosystem II. This work provides the first complete structural picture of this key protein, and it represents the first systematic comparison of Raman data from solution, glassy, and crystalline states of a protein.

  4. Retrievals of ethane from ground-based high-resolution FTIR solar observations with updated line parameters: determination of the optimum strategy for the Jungfraujoch station.

    Science.gov (United States)

    Bader, W.; Perrin, A.; Jacquemart, D.; Sudo, K.; Yashiro, H.; Gauss, M.; Demoulin, P.; Servais, C.; Mahieu, E.

    2012-04-01

    of methyl chloride (CH3Cl) in the 3.4 μm region (Bray et al., 2011) will be quantified. The ethane a priori volume mixing ratio (VMR) profile and associated covariance are based on synthetic data from the chemical transport model (CTM) of the University of Oslo. In this contribution, we will present updated ethane total and tropospheric column retrievals, using the SFIT-2 algorithm (v3.91) and high-resolution Fourier Transform Infrared (FTIR) solar absorption observations recorded with a Bruker 120HR instrument, at the high altitude research station of the Jungfraujoch (46.5° N, 8° E, 3580 m asl), within the framework of the Network for the Detection of Atmospheric Composition Change (NDACC, visit http://www.ndacc.org). We will characterize three microwindows encompassing the strongest ethane features after careful selection of a priori VMR profiles, spectroscopic parameters, accounting at best for all interfering species. We will then present the retrieval strategy representative of the best combination of those three characterized micro-windows in order to minimize the fitting residuals while maximizing the information content, the precision and the reliability of the retrieved product. The long-term C2H6 column time series will be produced using the Jungfraujoch observational database. Comparisons with synthetic data produced by two chemical transport model (CHASER and the one of the University of Oslo) will also be presented and analyzed, aiming at the determination and interpretation of long-term trends and interannual variations of ethane at Northern mid-latitudes. Acknowledgments The University of Liège involvement has primarily been supported by the PRODEX program funded by the Belgian Federal Science Policy Office, Brussels and by the Swiss GAW-CH program. E. Mahieu is Research Associate with the F.R.S. - FNRS. The FRS-FNRS and the Fédération Wallonie-Bruxelles are further acknowledged for observational activities support. We thank the International

  5. Automated method for relating regional pulmonary structure and function: integration of dynamic multislice CT and thin-slice high-resolution CT

    Science.gov (United States)

    Tajik, Jehangir K.; Kugelmass, Steven D.; Hoffman, Eric A.

    1993-07-01

    We have developed a method utilizing x-ray CT for relating pulmonary perfusion to global and regional anatomy, allowing for detailed study of structure to function relationships. A thick slice, high temporal resolution mode is used to follow a bolus contrast agent for blood flow evaluation and is fused with a high spatial resolution, thin slice mode to obtain structure- function detail. To aid analysis of blood flow, we have developed a software module, for our image analysis package (VIDA), to produce the combined structure-function image. Color coded images representing blood flow, mean transit time, regional tissue content, regional blood volume, regional air content, etc. are generated and imbedded in the high resolution volume image. A text file containing these values along with a voxel's 3-D coordinates is also generated. User input can be minimized to identifying the location of the pulmonary artery from which the input function to a blood flow model is derived. Any flow model utilizing one input and one output function can be easily added to a user selectable list. We present examples from our physiologic based research findings to demonstrate the strengths of combining dynamic CT and HRCT relative to other scanning modalities to uniquely characterize pulmonary normal and pathophysiology.

  6. Characterization of the Navy Fan Channel-to-Lobe Transition: Geomorphology, Gradient, and Structure Imaged through High-Resolution AUV Bathymetry

    Science.gov (United States)

    Carvajal, C.; Paull, C. K.; Caress, D. W.; Anderson, K.; Lundsten, E. M.; Gwiazda, R.; Fildani, A.; Dykstra, M.; McGann, M.; Maier, K. L.; Herguera, J. C.

    2016-12-01

    Channel to lobe transition zones (CLTZ) are elusive sectors of the seafloor. They record complex interactions between sediment-gravity flows, flow confinement, and gradient that can result in contrasting geomorphologies. If present, structural controls can add additional intricacies. We illustrate such complexities in the Navy Fan CLTZ offshore California/Mexico using AUV-collected high-resolution (1x1x0.25 m) bathymetry and chirp profiles. The AUV bathymetry images the fine scale details of the seafloor, otherwise unresolved in surface-ship-mounted multibeam bathymetry. Three morphological areas standout that in a direction transverse to sediment transport are: 1) An unconfined area with variable but overall steep gradients (0.5o-1.7o), and considerable erosion shown by numerous large scours that truncate underlying strata. These scours are elongate (turbidity currents due to high gradients, which resulted from relief along the San Clemente Fault and probably from differential seafloor aggradation. In the moderate confinement area, the smoother and gentler seafloor may be related to more efficient sediment dispersal able to transfer/deposit sediment to heal structural relief (though not completely) while avoiding significant local aggradation, hence preventing major gradient build up. In the faulted area, the steep and prominent structure reroutes the sediments. The findings of this study have broad application to any seafloor areas with rapid changes of gradient.

  7. Determination of steroid hormones and their metabolite in several types of meat samples by ultra high performance liquid chromatography-Orbitrap high resolution mass spectrometry.

    Science.gov (United States)

    López-García, Marina; Romero-González, Roberto; Garrido Frenich, Antonia

    2018-03-09

    A new analytical method based on ultra-high performance liquid chromatography (UHPLC) coupled to Orbitrap high resolution mass spectrometry (Orbitrap-HRMS) has been developed for the determination of steroid hormones (hydrocortisone, cortisone, progesterone, prednisone, prednisolone, testosterone, melengesterol acetate, hydrocortisone-21-acetate, cortisone-21-acetate, testosterone propionate, 17α-methyltestosterone, 6α-methylprednisolone and medroxyprogesterone) and their metabolite (17α-hydroxyprogesterone) in three meat samples (chicken, pork and beef). Two different extraction approaches were tested (QuEChERS "quick, easy, cheap, effective, rugged and safe" and "dilute and shoot"), observing that the QuEChERS method provided the best results in terms of recovery. A clean-up step was applied comparing several sorbents, obtaining the best results when florisil and aluminum oxide were used. The optimized method was validated, obtaining suitable results for all validation parameters in the three meat matrices evaluated. Recovery values ranged from 70% to 103% (except for prednisone in beef samples), meanwhile repeatability and reproducibility were obtained at values lower than 18% and 21%, respectively. The limit of quantification (LOQ) was established for most of the compounds at 1.0 μg/kg, except for testosterone in chicken and hydrocortisone-21-acetate and cortisone-21-acetate in pork at 2.0 μg/kg. Decision limit (CCα) and detection capability (CCβ) values ranged from 1.0-2.7 μg/kg and 1.9-5.5 μg/kg, respectively, in the three matrices. Finally, thirty one meat samples were analyzed and two hormones, progesterone and hydrocortisone, were detected in a beef and pork sample at 1.7 and 2.8 μg/kg respectively. Copyright © 2018 Elsevier B.V. All rights reserved.

  8. [Determination of 11 mycotoxins in baked foods and raw materials by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high-resolution mass spectrometry].

    Science.gov (United States)

    Li, Rong; He, Chunmei; Yang, Luqi; Wang, Yong; Zhang, Pengjie; Gao, Yongqing

    2017-08-08

    A method for the determination of 11 mycotoxins in baked foods and raw materials by ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high-resolution mass spectrometry (UPLC-HRMS) is reported in this paper. The samples were extracted with 20 mL 90% (v/v) acetonitrile aqueous solution containing 1% (v/v) formic acid, and the extracts were salted out by 2.0 g MgSO 4 and 0.5 g NaCl, cleaned up by 300 mg C18. The analytes were carried out on a CORTECS C18 column (100 mm×2.1 mm, 1.6 μ m) by gradient elution with 2 mmol/L ammonium acetate with 0.1% (v/v) formic acid aqueous solution and 2 mmol/L ammonium acetate methanol with 0.1% (v/v) formic acid. The results showed that the 11 mycotoxins had good linear relationships in their respective mass concentration ranges. The correlation coefficients were not less than 0.9960 and the limits of quantitation (LOQs) were from 0.15 to 20.00 μ g/kg. The recoveries of the 11 mycotoxins in bread ranged from 64.38% to 122.61% with the relative standard deviations (RSDs) from 1.52% to 12.99% at three spiked levels ( n =6). The method is demonstrated to be simple, fast, highly sensitive, reliable and it is effective to detect common mycotoxins in baked foods and raw materials.

  9. Determination of Pb (Lead, Cd (Cadmium, Cr (Chromium, Cu (Copper, and Ni (Nickel in Chinese tea with high-resolution continuum source graphite furnace atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Wen-Si Zhong

    2016-01-01

    Full Text Available The contents of lead, cadmium, chromium, copper, and nickel were determined in 25 tea samples from China, including green, yellow, white, oolong, black, Pu'er, and jasmine tea products, using high-resolution continuum source graphite furnace atomic absorption spectrometry. The methods used for sample preparation, digestion, and quantificational analysis were established, generating satisfactory analytical precisions (represented by relative standard deviations ranging from 0.6% to 2.5% and recoveries (98.91–101.32%. The lead contents in tea leaves were 0.48–10.57 mg/kg, and 80% of these values were below the maximum values stated by the guidelines in China. The contents of cadmium and chromium ranged from 0.01 mg/kg to 0.39 mg/kg and from 0.27 mg/kg to 2.45 mg/kg, respectively, remaining in compliance with the limits stipulated by China's Ministry of Agriculture. The copper contents were 7.73–63.71 mg/kg; only 64% of these values complied with the standards stipulated by the Ministry of Agriculture. The nickel contents ranged from 2.70 mg/kg to 13.41 mg/kg. Consequently, more attention must be paid to the risks of heavy metal contamination in tea. The quantitative method established in this work lays a foundation for preventing heavy metal toxicity in human from drinking tea and will help establish regulations to control the contents of heavy metals in tea.

  10. Probing the electronic structure and Au–C chemical bonding in AuC2− and AuC2 using high-resolution photoelectron spectroscopy

    International Nuclear Information System (INIS)

    León, Iker; Yang, Zheng; Wang, Lai-Sheng

    2014-01-01

    We report photoelectron spectroscopy (PES) and high-resolution PE imaging of AuC 2 − at a wide range of photon energies. The ground state of AuC 2 − is found to be linear (C ∞v , 1 Σ + ) with a …8π 4 4δ 4 17σ 2 9π 4 18σ 2 valence configuration. Detachments from all the five valence orbitals of the ground state of AuC 2 − are observed at 193 nm. High-resolution PE images are obtained in the energy range from 830 to 330 nm, revealing complicated vibronic structures from electron detachment of the 18σ, 9π, and 17σ orbitals. Detachment from the 18σ orbital results in the 2 Σ + ground state of neutral AuC 2 , which, however, is bent due to strong vibronic coupling with the nearby 2 Π state from detachment of a 9π electron. The 2 Σ + – 2 Π vibronic and spin-orbit coupling results in complicated vibronic structures for the 2 Σ + and 2 Π 3/2 states with extensive bending excitations. The electron affinity of AuC 2 is measured accurately to be 3.2192(7) eV with a ground state bending frequency of 195(6) cm −1 . The first excited state ( 2 A′) of AuC 2 , corresponding to the 2 Π 3/2 state at the linear geometry, is only 0.0021 eV above the ground state ( 2 A′) and has a bending frequency of 207(6) cm −1 . The 2 Π 1/2 state, 0.2291 eV above the ground state, is linear with little geometry change relative to the anion ground state. The detachment of the 17σ orbital also results in complicated vibronic structures, suggesting again a bent state due to possible vibronic coupling with the lower 2 Π state. The spectrum at 193 nm shows the presence of a minor species with less than 2% intensity relative to the ground state of AuC 2 − . High-resolution data of the minor species reveal several vibrational progressions in the Au–C stretching mode, which are assigned to be from the metastable 3 Π 2,1,0 spin-orbit excited states of AuC 2 − to the 2 Π 3/2,1/2 spin-orbit states of neutral AuC 2 . The spin-orbit splittings of the 3 Π and 2

  11. High-resolution ultrasonic spectroscopy

    Directory of Open Access Journals (Sweden)

    V. Buckin

    2018-03-01

    Full Text Available High-resolution ultrasonic spectroscopy (HR-US is an analytical technique for direct and non-destructive monitoring of molecular and micro-structural transformations in liquids and semi-solid materials. It is based on precision measurements of ultrasonic velocity and attenuation in analysed samples. The application areas of HR-US in research, product development, and quality and process control include analysis of conformational transitions of polymers, ligand binding, molecular self-assembly and aggregation, crystallisation, gelation, characterisation of phase transitions and phase diagrams, and monitoring of chemical and biochemical reactions. The technique does not require optical markers or optical transparency. The HR-US measurements can be performed in small sample volumes (down to droplet size, over broad temperature range, at ambient and elevated pressures, and in various measuring regimes such as automatic temperature ramps, titrations and measurements in flow.

  12. Application of laser ablation-ICP-MS to determine high-resolution elemental profiles across the Cretaceous/Paleogene boundary at Agost (Spain)

    NARCIS (Netherlands)

    Sosa-Montes de Oca, Claudia; de Lange, Gert J.|info:eu-repo/dai/nl/073930962; Martínez-Ruiz, Francisca; Rodríguez-Tovar, Francisco J.

    2018-01-01

    A high-resolution analysis of the distribution of major and trace elements across a Cretaceous/Paleogene boundary (KPgB) was done using Laser Ablation-Inductivity Coupled Plasma-Mass Spectrometry (LA-ICP-MS) and was compared with traditional distinct sampling and analysis. At the Agost site (SE

  13. Simultaneous determination of cadmium, iron and tin in canned foods using high-resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Leao, Danilo J; Junior, Mario M S; Brandao, Geovani C; Ferreira, Sergio L C

    2016-06-01

    A method was established to simultaneously determine cadmium, iron and tin in canned-food samples using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS). The quantification step has been performed using the primary line (228.802nm) for cadmium and the adjacent secondary lines (228.725nm and 228.668nm) for iron and tin, respectively. The selected chemical modifier was an acid solution that contained a mixture of 0.1% (w/v) Pd and 0.05% (w/v) Mg. The absorbance signals were measured based on the peak area using 3 pixels for cadmium and 5 pixels for iron and tin. Under these conditions, cadmium, iron and tin have been determined in canned-food samples using the external calibration technique based on aqueous standards, where the limits of quantification were 2.10ngg(-1) for cadmium, 1.95mgkg(-1) for iron and 3.00mgkg(-1) for tin, and the characteristic masses were 1.0pg for cadmium, 0.9ng for iron and 1.1ng for tin. The precision was evaluated using two solutions of each metal ion, and the results, which were expressed as the relative standard deviation (RSD%), were 3.4-6.8%. The method accuracy for cadmium and iron was confirmed by analyzing a certified reference material of apple leaves (NIST 1515), which was supplied by NIST. However, for tin, the accuracy was confirmed by comparing the results of the proposed method and another analytical technique (inductively coupled plasma optical emission spectrometry). The proposed procedure was applied to determine cadmium, iron and tin in canned samples of peeled tomato and sardine. Eleven samples were analyzed, and the analyte concentrations were 3.57-62.9ngg(-1), 2.68-31.48mgkg(-1) and 4.06-122.0mgkg(-1) for cadmium, iron and tin, respectively. In all analyzed samples, the cadmium and tin contents were lower than the permissible maximum levels for these metals in canned foods in the Brazilian legislation. Copyright © 2016. Published by Elsevier B.V.

  14. Determination of chlorine in food samples via the AlCl molecule using high-resolution continuum source molecular absorption spectrometry in a graphite furnace

    Energy Technology Data Exchange (ETDEWEB)

    Fechetia, Miriam; Tognon, Andre Luiz; Veiga, Marcia A.M.S. da, E-mail: mamsveiga@ffclrp.usp.br

    2012-05-15

    Determination of chlorine using the molecular absorption of aluminum mono-chloride (AlCl) at the 261.418 nm wavelength was accomplished by high-resolution continuum source molecular absorption spectrometry using a transversely heated graphite tube furnace with an integrated platform. For the analysis, 10 {mu}L of the sample followed by 10 {mu}L of a solution containing Al-Ag-Sr modifier, (1 g L{sup -1} each), were directly injected onto the platform. A spectral interference due to the use of Al-Ag-Sr as mixed modifier was easily corrected by the least-squares algorithm present in the spectrometer software. The pyrolysis and vaporization temperatures were 500 Degree-Sign C and 2200 Degree-Sign C, respectively. To evaluate the feasibility of a simple procedure for the determination of chlorine in food samples present in our daily lives, two different digestion methods were applied, namely (A) an acid digestion method using HNO{sub 3} only at room temperature, and (B) a digestion method with Ag, HNO{sub 3} and H{sub 2}O{sub 2}, where chlorine is precipitated as a low-solubility salt (AgCl), which is then dissolved with ammonia solution. The experimental results obtained with method B were in good agreement with the certified values and demonstrated that the proposed method is more accurate than method A. This is because the formation of silver chloride prevented analyte losses by volatilization. The limit of detection (LOD, 3{sigma}/s) for Cl in methods A and B was 18 {mu}g g{sup -1} and 9 {mu}g g{sup -1}, respectively, 1.7 and 3.3 times lower compared to published work using inductively coupled plasma optical emission spectrometry, and absolute LODs were 2.4 and 1.2 ng, respectively. - Highlights: Black-Right-Pointing-Pointer HR-CS MAS as technique for Cl determination via AlCl molecule Black-Right-Pointing-Pointer Spectral interference was corrected by the least-squares algorithm. Black-Right-Pointing-Pointer Chorine precipitation as AgCl prevents Cl losses during

  15. Structural characterization of epitaxial YBa2Cu3O7 thin films on step-edge substrates by means of high-resolution electron microscopy

    International Nuclear Information System (INIS)

    Jia, C.L.; Kabius, B.; Urban, K.

    1993-01-01

    The microstructure of YBa 2 Cu 3 O 7 films epitaxially grown on step-edge (0 0 1) SrTiO 3 and LaAlO 3 substrates has been characterized by means of high-resolution electron microscopy. The results indicate a relationship between the microstructure of the film across a step and the angle the step makes with the substrate plane. On a steep, high-angle step, the film grows with its c-axis perpendicular to that of the film on substrate surface so that two grain boundaries are formed. In the upper grain boundary, on the average, a (0 1 3) habit plane alternates with a (1 0 3) habit plane. This alternating structure is caused by twinning in the orthorhombic structure. The lower boundaries consist of a chain of (0 1 3)(0 1 3) and (0 1 0)(0 0 1) type segments exhibiting a tendency to tilt the whole habit plane toward the a-b plane of the flank film. Dislocations, stacking faults and misfit strains were also observed in or close to the boundaries. (orig.)

  16. Monitoring post-fire changes in species composition and stand structure in boreal forests using high-resolution, 3-D aerial drone data and Landsat

    Science.gov (United States)

    Alonzo, M.; Morton, D. C.; Cook, B.; Andersen, H. E.; Mack, M. C.

    2017-12-01

    The growing frequency and severity of boreal forest fires has important consequences for fire carbon emissions and ecosystem composition. Severe fires are typically associated with high degrees of both canopy and soil organic layer (SOL) consumption, particularly in black spruce stands. Complete canopy consumption can decrease the likelihood of spruce regeneration due to reduced viability of the aerial seedbank. Deeper burning of the SOL increases fire emissions and can expose mineral soil that promotes colonization by broadleaf species. There is mounting evidence that a disturbance-driven shift from spruce to broadleaf forests may indicate an ecological state change with feedbacks to regional and global climate. If post-fire successional dynamics can be characterized at an ecosystem scale using remote sensing data, we will be better equipped to constrain carbon and energy fluxes from SOL losses and albedo changes. In this study, we used Landsat time series, very high-resolution structure-from-motion (SFM) drone imagery, and field measurements to investigate post-fire regrowth 13 years after the 2004 Taylor Complex (TC) fires in interior Alaska. Twenty-seven TC plots span a gradient of moisture conditions and burn severity as estimated by loss of SOL. A range of variables potentially governing seedling species dominance (e.g., moisture status, distance to seed sources) have been collected systematically over the years following fire. In July 2017, we additionally collected drone imagery over 25 of the TC plots. We processed these highly overlapped, nadir-view and oblique angle photos into extremely dense (>700 pts/m2) RGB-colored point clouds using SFM techniques. With these point clouds and high resolution orthomosaics, we estimated: 1) snag heights and biomass, 2) remnant snag fine branching, and 3) species and structure of shrubs and groundcover that have regrown since fire. We additionally assembled a dense Landsat time series arranged by day-of-year to monitor

  17. High Resolution Crystal Structures of Streptococcus pneumoniae Nicotinamidase with Trapped Intermediates Provide Insights into Catalytic Mechanism and Inhibition by Aldehydes∥,‡

    Science.gov (United States)

    French, Jarrod B.; Cen, Yana; Sauve, Anthony A.; Ealick, Steven E.

    2010-01-01

    Nicotinamidases are salvage enzymes that convert nicotinamide to nicotinic acid. These enzymes are essential for the recycling of nicotinamide into NAD+ in most prokaryotes, most single cell and multicellular eukaryotes, but not in mammals. The significance of these enzymes for nicotinamide salvage and for NAD+ homeostasis has increased interest in nicotinamidases as possible antibiotic targets. Nicotinamidases are also regulators of intracellular nicotinamide concentrations, thereby regulating signaling of downstream NAD+ consuming enzymes, such as the NAD+-dependent deacetylases (sirtuins). Here, we report several high resolution crystal structures of the nicotinamidase from Streptococcus pneumoniae (SpNic) in unliganded and ligand-bound forms. The structure of the C136S mutant in complex with nicotinamide provides details about substrate binding while a trapped nicotinoyl-thioester complexed with SpNic reveals the structure of the proposed thioester reaction intermediate. Examination of the active site of SpNic reveals several important features including a metal ion that coordinates the substrate and the catalytically relevant water molecule, and an oxyanion hole which both orients the substrate and offsets the negative charge that builds up during catalysis. Structures of this enzyme with bound nicotinaldehyde inhibitors elucidate the mechanism of inhibition and provide further details about the catalytic mechanism. In addition, we provide a biochemical analysis of the identity and role of the metal ion that orients the ligand in the active site and activates the water molecule responsible for hydrolysis of the substrate. These data provide structural evidence for several proposed reaction intermediates and allow for a more complete understanding of the catalytic mechanism of this enzyme. PMID:20853856

  18. High-resolution crystal structures of Streptococcus pneumoniae nicotinamidase with trapped intermediates provide insights into the catalytic mechanism and inhibition by aldehydes .

    Science.gov (United States)

    French, Jarrod B; Cen, Yana; Sauve, Anthony A; Ealick, Steven E

    2010-10-12

    Nicotinamidases are salvage enzymes that convert nicotinamide to nicotinic acid. These enzymes are essential for the recycling of nicotinamide into NAD(+) in most prokaryotes and most single-cell and multicellular eukaryotes, but not in mammals. The significance of these enzymes for nicotinamide salvage and for NAD(+) homeostasis has stimulated interest in nicotinamidases as possible antibiotic targets. Nicotinamidases are also regulators of intracellular nicotinamide concentrations, thereby regulating signaling of downstream NAD(+)-consuming enzymes, such as the NAD(+)-dependent deacetylases (sirtuins). Here, we report several high-resolution crystal structures of the nicotinamidase from Streptococcus pneumoniae (SpNic) in unliganded and ligand-bound forms. The structure of the C136S mutant in complex with nicotinamide provides details about substrate binding, while a trapped nicotinoyl thioester in a complex with SpNic reveals the structure of the proposed thioester reaction intermediate. Examination of the active site of SpNic reveals several important features, including a metal ion that coordinates the substrate and the catalytically relevant water molecule and an oxyanion hole that both orients the substrate and offsets the negative charge that builds up during catalysis. Structures of this enzyme with bound nicotinaldehyde inhibitors elucidate the mechanism of inhibition and provide further details about the catalytic mechanism. In addition, we provide a biochemical analysis of the identity and role of the metal ion that orients the ligand in the active site and activates the water molecule responsible for hydrolysis of the substrate. These data provide structural evidence of several proposed reaction intermediates and allow for a more complete understanding of the catalytic mechanism of this enzyme.

  19. High-Resolution Crystal Structures of Streptococcus pneumoniae Nicotinamidase with Trapped Intermediates Provide Insights into the Catalytic Mechanism and Inhibition by Aldehydes

    Energy Technology Data Exchange (ETDEWEB)

    French, Jarrod B.; Cen, Yana; Sauve, Anthony A.; Ealick, Steven E. (Cornell); (Weill-Med)

    2010-11-11

    Nicotinamidases are salvage enzymes that convert nicotinamide to nicotinic acid. These enzymes are essential for the recycling of nicotinamide into NAD{sup +} in most prokaryotes and most single-cell and multicellular eukaryotes, but not in mammals. The significance of these enzymes for nicotinamide salvage and for NAD{sup +} homeostasis has stimulated interest in nicotinamidases as possible antibiotic targets. Nicotinamidases are also regulators of intracellular nicotinamide concentrations, thereby regulating signaling of downstream NAD{sup +}-consuming enzymes, such as the NAD{sup +}-dependent deacetylases (sirtuins). Here, we report several high-resolution crystal structures of the nicotinamidase from Streptococcus pneumoniae (SpNic) in unliganded and ligand-bound forms. The structure of the C136S mutant in complex with nicotinamide provides details about substrate binding, while a trapped nicotinoyl thioester in a complex with SpNic reveals the structure of the proposed thioester reaction intermediate. Examination of the active site of SpNic reveals several important features, including a metal ion that coordinates the substrate and the catalytically relevant water molecule and an oxyanion hole that both orients the substrate and offsets the negative charge that builds up during catalysis. Structures of this enzyme with bound nicotinaldehyde inhibitors elucidate the mechanism of inhibition and provide further details about the catalytic mechanism. In addition, we provide a biochemical analysis of the identity and role of the metal ion that orients the ligand in the active site and activates the water molecule responsible for hydrolysis of the substrate. These data provide structural evidence of several proposed reaction intermediates and allow for a more complete understanding of the catalytic mechanism of this enzyme.

  20. Determination of fluorine in copper concentrate via high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis - Comparison of three target molecules.

    Science.gov (United States)

    Cadorim, Heloisa R; de Gois, Jefferson S; Borges, Aline R; Vale, Maria Goreti R; Welz, Bernhard; Gleisner, Heike; Ott, Christina

    2018-01-01

    The chemical composition of complex inorganic materials, such as copper concentrate, may influence the economics of their further processing because most smelters, and particularly the producers of high-purity electrolyte copper, have strict limitations for the permissible concentration of impurities. These components might be harmful to the quality of the products, impair the production process and be hazardous to the environment. The goal of the present work is the development of a method for the determination of fluorine in copper concentrate using high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis. The molecular absorption of the diatomic molecule CaF was measured at 606.440nm. The molecule CaF was generated by the addition of 200µg Ca as the molecule-forming reagent; the optimized pyrolysis and vaporization temperatures were 900°C and 2400°C, respectively. The characteristic mass and limit of detection were 0.5ng and 3ng, respectively. Calibration curves were established using aqueous standard solutions containing the major components Cu, Fe, S and the minor component Ag in optimized concentrations. The accuracy of the method was verified using certified reference materials. Fourteen copper concentrate samples from Chile and Australia were analyzed to confirm the applicability of the method to real samples; the concentration of fluorine ranged from 34 to 5676mgkg -1 . The samples were also analyzed independently at Analytik Jena by different operators, using the same equipment, but different target molecules, InF and GaF, and different operating conditions; but with a few exceptions, the results agreed quite well. The results obtained at Analytik Jena using the GaF molecule and our results obtained with CaF, with one exception, were also in agreement with the values informed by the supplier of the samples, which were obtained using ion selective electrode potentiometry after alkaline fusion. A comparison will

  1. High resolution satellite imagery : from spies to pipeline management

    Energy Technology Data Exchange (ETDEWEB)

    Adam, S. [Canadian Geomatic Solutions Ltd., Calgary, AB (Canada); Farrell, M. [TransCanada Transmission, Calgary, AB (Canada)

    2000-07-01

    The launch of Space Imaging's IKONOS satellite in September 1999 has opened the door for corridor applications. The technology has been successfully implemented by TransCanada PipeLines in mapping over 1500 km of their mainline. IKONOS is the world's first commercial high resolution satellite which collects data at 1-meter black/white and 4-meter multi-spectral. Its use is regulated by the U.S. government. It is the best source of high resolution satellite image data. Other sources include the Indian Space Agency's IRS-1 C/D satellite and the Russian SPIN-2 which provides less reliable coverage. In addition, two more high resolution satellites may be launched this year to provide imagery every day of the year. IKONOS scenes as narrow as 5 km can be purchased. TransCanada conducted a pilot study to determine if high resolution satellite imagery is as effective as ortho-photos for identifying population structures within a buffer of TransCanada's east line right-of-way. The study examined three unique segments where residential, commercial, industrial and public features were compared. It was determined that IKONOS imagery is as good as digital ortho-photos for updating structures from low to very high density areas. The satellite imagery was also logistically easier than ortho-photos to acquire. This will be even more evident when the IKONOS image archives begins to grow. 4 tabs., 3 figs.

  2. Accurate evaluation of subband structure in a carrier accumulation layer at an n-type InAs surface: LDF calculation combined with high-resolution photoelectron spectroscopy

    Directory of Open Access Journals (Sweden)

    Takeshi Inaoka

    2012-12-01

    Full Text Available Adsorption on an n-type InAs surface often induces a gradual formation of a carrier-accumulation layer at the surface. By means of high-resolution photoelectron spectroscopy (PES, Betti et al. made a systematic observation of subbands in the accumulation layer in the formation process. Incorporating a highly nonparabolic (NP dispersion of the conduction band into the local-density-functional (LDF formalism, we examine the subband structure in the accumulation-layer formation process. Combining the LDF calculation with the PES experiment, we make an accurate evaluation of the accumulated-carrier density, the subband-edge energies, and the subband energy dispersion at each formation stage. Our theoretical calculation can reproduce the three observed subbands quantitatively. The subband dispersion, which deviates downward from that of the projected bulk conduction band with an increase in wave number, becomes significantly weaker in the formation process. Accurate evaluation of the NP subband dispersion at each formation stage is indispensable in making a quantitative analysis of collective electronic excitations and transport properties in the subbands.

  3. Nuclear structure studies using the high resolution spectrometer at the Los Alamos Clinton P. Anderson Meson Physics Facility: Annual progress report, [1987-1988

    International Nuclear Information System (INIS)

    1987-09-01

    This document constitutes the (1987 to 1988) progress report for the ongoing medium energy nuclear physics research program supported by the US Department of Energy with the University of Texas at Austin. A major part of the work has been and will continue to be associated with research done at the Los Alamos Clinton P. Anderson Meson Physics Facility (LAMPF) using the High Resolution Spectrometer (HRS), the External Proton Beam (EPB), and the new Neutron Time of Flight Facility (NTOF). Other research is done at the Fermi National Accelerator Laboratory (FNAL). The research focuses on (1) providing proton + nucleus data which test nonrelativistic and relativistic models of the medium energy proton + nucleus interaction, (2) providing (p,p) and (p,n) data which are to be analyzed to provide new nuclear structure information (both ground state and excited state), (3) providing nucleon + nucleon data to aid in the systematic study of the fundamental nucleon-nucleon interaction, (4) developing and improving the proton + nucleus theoretical models themselves, and (5) initiating new experimental programs whose goals are to search for new phenomena in nuclear physics. 182 refs., 71 figs., 5 tabs

  4. High-resolution extreme ultraviolet spectroscopy of G191-B2B: structure of the stellar photosphere and the surrounding interstellar medium

    Science.gov (United States)

    Barstow, M. A.; Cruddace, R. G.; Kowalski, M. P.; Bannister, N. P.; Yentis, D.; Lapington, J. S.; Tandy, J. A.; Hubeny, I.; Schuh, S.; Dreizler, S.; Barbee, T. W.

    2005-10-01

    We have continued our detailed analysis of the high-resolution (R= 4000) spectroscopic observation of the DA white dwarf G191-B2B, obtained by the Joint Astrophysical Plasmadynamic Experiment (J-PEX) normal incidence sounding rocket-borne telescope, comparing the observed data with theoretical predictions for both homogeneous and stratified atmosphere structures. We find that the former models give the best agreement over the narrow waveband covered by J-PEX, in conflict with what is expected from previous studies of the lower resolution but broader wavelength coverage Extreme Ultraviolet Explorer spectra. We discuss the possible limitations of the atomic data and our understanding of the stellar atmospheres that might give rise to this inconsistency. In our earlier study, we obtained an unusually high ionization fraction for the ionized HeII present along the line of sight to the star. In the present paper, we obtain a better fit when we assume, as suggested by Space Telescope Imaging Spectrograph results, that this HeII resides in two separate components. When one of these is assigned to the local interstellar cloud, the implied He ionization fraction is consistent with measurements along other lines of sight. However, the resolving power and signal-to-noise available from the instrument configuration used in this first successful J-PEX flight are not sufficient to clearly identify and prove the existence of the two components.

  5. An Automated Technique for Generating Georectified Mosaics from Ultra-High Resolution Unmanned Aerial Vehicle (UAV Imagery, Based on Structure from Motion (SfM Point Clouds

    Directory of Open Access Journals (Sweden)

    Christopher Watson

    2012-05-01

    Full Text Available Unmanned Aerial Vehicles (UAVs are an exciting new remote sensing tool capable of acquiring high resolution spatial data. Remote sensing with UAVs has the potential to provide imagery at an unprecedented spatial and temporal resolution. The small footprint of UAV imagery, however, makes it necessary to develop automated techniques to geometrically rectify and mosaic the imagery such that larger areas can be monitored. In this paper, we present a technique for geometric correction and mosaicking of UAV photography using feature matching and Structure from Motion (SfM photogrammetric techniques. Images are processed to create three dimensional point clouds, initially in an arbitrary model space. The point clouds are transformed into a real-world coordinate system using either a direct georeferencing technique that uses estimated camera positions or via a Ground Control Point (GCP technique that uses automatically identified GCPs within the point cloud. The point cloud is then used to generate a Digital Terrain Model (DTM required for rectification of the images. Subsequent georeferenced images are then joined together to form a mosaic of the study area. The absolute spatial accuracy of the direct technique was found to be 65–120 cm whilst the GCP technique achieves an accuracy of approximately 10–15 cm.

  6. Azimuthally anisotropic hydride lens structures in Zircaloy 4 nuclear fuel cladding: High-resolution neutron radiography imaging and BISON finite element analysis

    Science.gov (United States)

    Lin, Jun-Li; Zhong, Weicheng; Bilheux, Hassina Z.; Heuser, Brent J.

    2017-12-01

    High-resolution neutron radiography has been used to image bulk circumferential hydride lens particles in unirradiated Zircaloy 4 tubing cross section specimens. Zircaloy 4 is a common light water nuclear reactor (LWR) fuel cladding; hydrogen pickup, hydride formation, and the concomitant effect on the mechanical response are important for LWR applications. Ring cross section specimens with three hydrogen concentrations (460, 950, and 2830 parts per million by weight) and an as-received reference specimen were imaged. Azimuthally anisotropic hydride lens particles were observed at 950 and 2830 wppm. The BISON finite element analysis nuclear fuel performance code was used to model the system elastic response induced by hydride volumetric dilatation. The compressive hoop stress within the lens structure becomes azimuthally anisotropic at high hydrogen concentrations or high hydride phase fraction. This compressive stress anisotropy matches the observed lens anisotropy, implicating the effect of stress on hydride formation as the cause of the observed lens azimuthal asymmetry. The cause and effect relation between compressive stress and hydride lens anisotropy represents an indirect validation of a key BISON output, the evolved hoop stress associated with hydride formation.

  7. Novel strategy for the determination of illegal adulterants in health foods and herbal medicines using high-performance liquid chromatography with high-resolution mass spectrometry.

    Science.gov (United States)

    Wang, Zhe; Wu, Caisheng; Wang, Gangli; Zhang, Qingsheng; Zhang, Jinlan

    2015-03-01

    The detection, confirmation, and quantification of multiple illegal adulterants in health foods and herbal medicines by using a single analytical method are a challenge. This paper reports on a new strategy to meet this challenge by employing high-performance liquid chromatography coupled with high-resolution mass spectrometry and a mass spectral tree similarity filter technique. This analytical method can rapidly collect high-resolution, high-accuracy, optionally multistage mass data for compounds in samples. After a preliminary screening by retention time and high-resolution mass spectral data, known illegal adulterants can be detected. The mass spectral tree similarity filter technique has been applied to rapidly confirm these adulterants and simultaneously discover unknown ones. By using full-scan mass spectra as stem and data-dependent subsequent stage mass spectra to form branches, mass spectrometry data from detected compounds are converted into mass spectral trees. The known or unknown illegal adulterants in the samples are confirmed or discovered based on the similarity between their mass spectral trees and those of the references in a library, and they are finally quantified against standard curves. This new strategy has been tested by using 50 samples, and the illegal adulterants were rapidly and effectively detected, confirmed and quantified. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. High resolution hadron calorimetry

    International Nuclear Information System (INIS)

    Wigmans, R.

    1987-01-01

    The components that contribute to the signal of a hadron calorimeter and the factors that affect its performance are discussed, concentrating on two aspects; energy resolution and signal linearity. Both are decisively dependent on the relative response to the electromagnetic and the non-electromagnetic shower components, the e/h signal ratio, which should be equal to 1.0 for optimal performance. The factors that determine the value of this ratio are examined. The calorimeter performance is crucially determined by its response to the abundantly present soft neutrons in the shower. The presence of a considerable fraction of hydrogen atoms in the active medium is essential for achieving the best possible results. Firstly, this allows one to tune e/h to the desired value by choosing the appropriate sampling fraction. And secondly, the efficient neutron detection via recoil protons in the readout medium itself reduces considerably the effect of fluctuations in binding energy losses at the nuclear level, which dominate the intrinsic energy resolution. Signal equalization, or compensation (e/h = 1.0) does not seem to be a property unique to 238 U, but can also be achieved with lead and probably even iron absorbers. 21 refs.; 19 figs

  9. 4D imaging and quantification of pore structure modifications inside natural building stones by means of high resolution X-ray CT.

    Science.gov (United States)

    Dewanckele, J; De Kock, T; Boone, M A; Cnudde, V; Brabant, L; Boone, M N; Fronteau, G; Van Hoorebeke, L; Jacobs, P

    2012-02-01

    Weathering processes have been studied in detail for many natural building stones. The most commonly used analytical techniques in these studies are thin-section petrography, SEM, XRD and XRF. Most of these techniques are valuable for chemical and mineralogical analysis of the weathering patterns. However, to obtain crucial quantitative information on structural evolutions like porosity changes and growth of weathering crusts in function of time, non-destructive techniques become necessary. In this study, a Belgian historical calcareous sandstone, the Lede stone, was exposed to gaseous SO(2) under wet surface conditions according to the European Standard NBN EN 13919 (2003). Before, during and after the strong acid test, high resolution X-ray tomography has been performed to visualize gypsum crust formation to yield a better insight into the effects of gaseous SO(2) on the pore modification in 3D. The tomographic scans were taken at the Centre for X-ray Tomography at Ghent University (UGCT). With the aid of image analysis, partial porosity changes were calculated in different stadia of the process. Increasing porosity has been observed visually and quantitatively below the new superficial formed layer of gypsum crystals. In some cases micro-cracks and dissolution zones were detected on the grain boundaries of quartz. By using Morpho+, an in-house developed image analysis program, radial porosity, partial porosity, ratio of open and closed porosity and equivalent diameter of individual pore structures have been calculated. The results obtained in this study are promising for a better understanding of gypsum weathering mechanisms, porosity changes and patterns on natural building stones in four dimensions. Copyright © 2011 Elsevier B.V. All rights reserved.

  10. High-Resolution Nuclear Magnetic Resonance Determination of Transfer RNA Tertiary Base Pairs in Solution. 2. Species Containing a Large Variable Loop

    NARCIS (Netherlands)

    HURD, RE; ROBILLARD, GT; REID, BR

    1977-01-01

    The number of base pairs in the solution structure of several class III D3VN tRNA species from E. coli has been determined by analyzing the number of low-field (-15 to -11 ppm) proton resonances in their nuclear magnetic resonance spectra at 360 MHz. Contrary to previous reports indicating the

  11. Structure from motion, a low cost, very high resolution method for surveying glaciers using GoPros and opportunistic helicopter flights

    Science.gov (United States)

    Girod, L.; Nuth, C.; Schellenberger, T.

    2014-12-01

    The capability of structure from motion techniques to survey glaciers with a very high spatial and temporal resolution is a promising tool for better understanding the dynamic changes of glaciers. Modern software and computing power allow us to produce accurate data sets from low cost surveys, thus improving the observational capabilities on a wider range of glaciers and glacial processes. In particular, highly accurate glacier volume change monitoring and 3D movement computations will be possible Taking advantage of the helicopter flight needed to survey the ice stakes on Kronenbreen, NW Svalbard, we acquired high resolution photogrammetric data over the well-studied Midre Lovénbreen in September 2013. GoPro Hero 2 cameras were attached to the landing gear of the helicopter, acquiring two images per second. A C/A code based GPS was used for registering the stereoscopic model. Camera clock calibration is obtained through fitting together the shapes of the flight given by both the GPS logger and the relative orientation of the images. A DEM and an ortho-image are generated at 30cm resolution from 300 images collected. The comparison with a 2005 LiDAR DEM (5 meters resolution) shows an absolute error in the direct registration of about 6±3m in 3D which could be easily reduced to 1,5±1m by using fine point cloud alignment algorithms on stable ground. Due to the different nature of the acquisition method, it was not possible to use tie point based co-registration. A combination of the DEM and ortho-image is shown with the point cloud in figure below. A second photogrammetric data set will be acquired in September 2014 to survey the annual volume change and movement. These measurements will then be compared to the annual resolution glaciological stake mass balance and velocity measurements to assess the precision of the method to monitor at an annual resolution.

  12. Simultaneous observations of structure function parameter of refractive index using a high-resolution radar and the DataHawk small airborne measurement system

    Science.gov (United States)

    Scipión, Danny E.; Lawrence, Dale A.; Milla, Marco A.; Woodman, Ronald F.; Lume, Diego A.; Balsley, Ben B.

    2016-09-01

    The SOUSY (SOUnding SYstem) radar was relocated to the Jicamarca Radio Observatory (JRO) near Lima, Peru, in 2000, where the radar controller and acquisition system were upgraded with state-of-the-art parts to take full advantage of its potential for high-resolution atmospheric sounding. Due to its broad bandwidth (4 MHz), it is able to characterize clear-air backscattering with high range resolution (37.5 m). A campaign conducted at JRO in July 2014 aimed to characterize the lower troposphere with a high temporal resolution (8.1 Hz) using the DataHawk (DH) small unmanned aircraft system, which provides in situ atmospheric measurements at scales as small as 1 m in the lower troposphere and can be GPS-guided to obtain measurements within the beam of the radar. This was a unique opportunity to make coincident observations by both systems and to directly compare their in situ and remotely sensed parameters. Because SOUSY only points vertically, it is only possible to retrieve vertical radar profiles caused by changes in the refractive index within the resolution volume. Turbulent variations due to scattering are described by the structure function parameter of refractive index Cn2. Profiles of Cn2 from the DH are obtained by combining pressure, temperature, and relative humidity measurements along the helical trajectory and integrated at the same scale as the radar range resolution. Excellent agreement is observed between the Cn2 estimates obtained from the DH and SOUSY in the overlapping measurement regime from 1200 m up to 4200 m above sea level, and this correspondence provides the first accurate calibration of the SOUSY radar for measuring Cn2.

  13. Simultaneous observations of structure function parameter of refractive index using a high-resolution radar and the DataHawk small airborne measurement system

    Directory of Open Access Journals (Sweden)

    D. E. Scipión

    2016-09-01

    Full Text Available The SOUSY (SOUnding SYstem radar was relocated to the Jicamarca Radio Observatory (JRO near Lima, Peru, in 2000, where the radar controller and acquisition system were upgraded with state-of-the-art parts to take full advantage of its potential for high-resolution atmospheric sounding. Due to its broad bandwidth (4 MHz, it is able to characterize clear-air backscattering with high range resolution (37.5 m. A campaign conducted at JRO in July 2014 aimed to characterize the lower troposphere with a high temporal resolution (8.1 Hz using the DataHawk (DH small unmanned aircraft system, which provides in situ atmospheric measurements at scales as small as 1 m in the lower troposphere and can be GPS-guided to obtain measurements within the beam of the radar. This was a unique opportunity to make coincident observations by both systems and to directly compare their in situ and remotely sensed parameters. Because SOUSY only points vertically, it is only possible to retrieve vertical radar profiles caused by changes in the refractive index within the resolution volume. Turbulent variations due to scattering are described by the structure function parameter of refractive index Cn2. Profiles of Cn2 from the DH are obtained by combining pressure, temperature, and relative humidity measurements along the helical trajectory and integrated at the same scale as the radar range resolution. Excellent agreement is observed between the Cn2 estimates obtained from the DH and SOUSY in the overlapping measurement regime from 1200 m up to 4200 m above sea level, and this correspondence provides the first accurate calibration of the SOUSY radar for measuring Cn2.

  14. Combining structure-from-motion derived point clouds from satellites and unmanned aircraft systems images with ground-truth data to create high-resolution digital elevation models

    Science.gov (United States)

    Palaseanu, M.; Thatcher, C.; Danielson, J.; Gesch, D. B.; Poppenga, S.; Kottermair, M.; Jalandoni, A.; Carlson, E.

    2016-12-01

    Coastal topographic and bathymetric (topobathymetric) data with high spatial resolution (1-meter or better) and high vertical accuracy are needed to assess the vulnerability of Pacific Islands to climate change impacts, including sea level rise. According to the Intergovernmental Panel on Climate Change reports, low-lying atolls in the Pacific Ocean are extremely vulnerable to king tide events, storm surge, tsunamis, and sea-level rise. The lack of coastal topobathymetric data has been identified as a critical data gap for climate vulnerability and adaptation efforts in the Republic of the Marshall Islands (RMI). For Majuro Atoll, home to the largest city of RMI, the only elevation dataset currently available is the Shuttle Radar Topography Mission data which has a 30-meter spatial resolution and 16-meter vertical accuracy (expressed as linear error at 90%). To generate high-resolution digital elevation models (DEMs) in the RMI, elevation information and photographic imagery have been collected from field surveys using GNSS/total station and unmanned aerial vehicles for Structure-from-Motion (SfM) point cloud generation. Digital Globe WorldView II imagery was processed to create SfM point clouds to fill in gaps in the point cloud derived from the higher resolution UAS photos. The combined point cloud data is filtered and classified to bare-earth and georeferenced using the GNSS data acquired on roads and along survey transects perpendicular to the coast. A total station was used to collect elevation data under tree canopies where heavy vegetation cover blocked the view of GNSS satellites. A subset of the GPS / total station data was set aside for error assessment of the resulting DEM.

  15. Close-range airborne Structure-from-Motion Photogrammetry for high-resolution beach morphometric surveys: Examples from an embayed rotating beach

    Science.gov (United States)

    Brunier, Guillaume; Fleury, Jules; Anthony, Edward J.; Gardel, Antoine; Dussouillez, Philippe

    2016-05-01

    The field of photogrammetry has seen significant new developments essentially related to the emergence of new computer-based applications that have fostered the growth of the workflow technique called Structure-from-Motion (SfM). Low-cost, user-friendly SfM photogrammetry offers interesting new perspectives in coastal and other fields of geomorphology requiring high-resolution topographic data. The technique enables the construction of topographic products such as digital surface models (DSMs) and orthophotographs, and combines the advantages of the reproducibility of GPS surveys and the high density and accuracy of airborne LiDAR, but at very advantageous cost compared to the latter. Three SfM-based photogrammetric experiments were conducted on the embayed beach of Montjoly in Cayenne, French Guiana, between October 2013 and 2014, in order to map morphological changes and quantify sediment budgets. The beach is affected by a process of rotation induced by the alongshore migration of mud banks from the mouths of the Amazon River that generate spatial and temporal changes in wave refraction and incident wave angles, thus generating the reversals in longshore drift that characterise this process. Sub-vertical aerial photographs of the beach were acquired from a microlight aircraft that flew alongshore at low elevation (275 m). The flight plan included several parallel flight axes with an overlap of 85% between pictures in the lengthwise direction and 50% between paths. Targets of 40 × 40 cm, georeferenced by RTK-DGPS, were placed on the beach, spaced 100 m apart. These targets served in optimizing the model and in producing georeferenced 3D products. RTK-GPS measurements of random points and cross-shore profiles were used to validate the photogrammetry results and assess their accuracy. We produced dense point clouds with 150 to 200 points/m², from which we generated DSMs and orthophotos with respective resolutions of 10 cm and 5 cm. Compared to the GPS control

  16. High-Resolution Mass Spectrometers

    Science.gov (United States)

    Marshall, Alan G.; Hendrickson, Christopher L.

    2008-07-01

    Over the past decade, mass spectrometry has been revolutionized by access to instruments of increasingly high mass-resolving power. For small molecules up to ˜400 Da (e.g., drugs, metabolites, and various natural organic mixtures ranging from foods to petroleum), it is possible to determine elemental compositions (CcHhNnOoSsPp…) of thousands of chemical components simultaneously from accurate mass measurements (the same can be done up to 1000 Da if additional information is included). At higher mass, it becomes possible to identify proteins (including posttranslational modifications) from proteolytic peptides, as well as lipids, glycoconjugates, and other biological components. At even higher mass (˜100,000 Da or higher), it is possible to characterize posttranslational modifications of intact proteins and to map the binding surfaces of large biomolecule complexes. Here we review the principles and techniques of the highest-resolution analytical mass spectrometers (time-of-flight and Fourier transform ion cyclotron resonance and orbitrap mass analyzers) and describe some representative high-resolution applications.

  17. Organic solvent and temperature-enhanced ion chromatography-high resolution mass spectrometry for the determination of low molecular weight organic and inorganic anions

    International Nuclear Information System (INIS)

    Gilchrist, Elizabeth S.; Nesterenko, Pavel N.; Smith, Norman W.; Barron, Leon P.

    2015-01-01

    Highlights: • IC selectivity at high contents of organic solvent in eluent and elevated temperature is studied. • Solvent-enhanced IC coupled to high resolution MS is beneficial for sensitive detection of ions. • The first application of IC-HRMS to the detection of low explosives in fingermarks is shown. - Abstract: There has recently been increased interest in coupling ion chromatography (IC) to high resolution mass spectrometry (HRMS) to enable highly sensitive and selective analysis. Herein, the first comprehensive study focusing on the direct coupling of suppressed IC to HRMS without the need for post-suppressor organic solvent modification is presented. Chromatographic selectivity and added HRMS sensitivity offered by organic solvent-modified IC eluents on a modern hyper-crosslinked polymeric anion-exchange resin (IonPac AS18) are shown using isocratic eluents containing 5–50 mM hydroxide with 0–80% methanol or acetonitrile for a range of low molecular weight anions (<165 Da). Comprehensive experiments on IC thermodynamics over a temperature range between 20–45 °C with the eluent containing up to 60% of acetonitrile or methanol revealed markedly different retention behaviour and selectivity for the selected analytes on the same polymer based ion-exchange resin. Optimised sensitivity with HRMS was achieved with as low as 30–40% organic eluent content. Analytical performance characteristics are presented and compared with other IC-MS based works. This study also presents the first application of IC-HRMS to forensic detection of trace low-order anionic explosive residues in latent human fingermarks

  18. Organic solvent and temperature-enhanced ion chromatography-high resolution mass spectrometry for the determination of low molecular weight organic and inorganic anions

    Energy Technology Data Exchange (ETDEWEB)

    Gilchrist, Elizabeth S. [Analytical & Environmental Science Division, Department of Forensic & Analytical Science, King’s College London, 150 Stamford Street, London, SE1 9NH (United Kingdom); Nesterenko, Pavel N. [Australian Centre for Research on Separation Science, School of Physical Sciences, University of Tasmania, Private Bag 75, Hobart 7001 (Australia); Smith, Norman W. [Analytical & Environmental Science Division, Department of Forensic & Analytical Science, King’s College London, 150 Stamford Street, London, SE1 9NH (United Kingdom); Barron, Leon P., E-mail: leon.barron@kcl.ac.uk [Analytical & Environmental Science Division, Department of Forensic & Analytical Science, King’s College London, 150 Stamford Street, London, SE1 9NH (United Kingdom)

    2015-03-20

    Highlights: • IC selectivity at high contents of organic solvent in eluent and elevated temperature is studied. • Solvent-enhanced IC coupled to high resolution MS is beneficial for sensitive detection of ions. • The first application of IC-HRMS to the detection of low explosives in fingermarks is shown. - Abstract: There has recently been increased interest in coupling ion chromatography (IC) to high resolution mass spectrometry (HRMS) to enable highly sensitive and selective analysis. Herein, the first comprehensive study focusing on the direct coupling of suppressed IC to HRMS without the need for post-suppressor organic solvent modification is presented. Chromatographic selectivity and added HRMS sensitivity offered by organic solvent-modified IC eluents on a modern hyper-crosslinked polymeric anion-exchange resin (IonPac AS18) are shown using isocratic eluents containing 5–50 mM hydroxide with 0–80% methanol or acetonitrile for a range of low molecular weight anions (<165 Da). Comprehensive experiments on IC thermodynamics over a temperature range between 20–45 °C with the eluent containing up to 60% of acetonitrile or methanol revealed markedly different retention behaviour and selectivity for the selected analytes on the same polymer based ion-exchange resin. Optimised sensitivity with HRMS was achieved with as low as 30–40% organic eluent content. Analytical performance characteristics are presented and compared with other IC-MS based works. This study also presents the first application of IC-HRMS to forensic detection of trace low-order anionic explosive residues in latent human fingermarks.

  19. High resolution Neutron and Synchrotron Powder Diffraction

    International Nuclear Information System (INIS)

    Hewat, A.W.

    1986-01-01

    The use of high-resolution powder diffraction has grown rapidly in the past years, with the development of Rietveld (1967) methods of data analysis and new high-resolution diffractometers and multidetectors. The number of publications in this area has increased from a handful per year until 1973 to 150 per year in 1984, with a ten-year total of over 1000. These papers cover a wide area of solid state-chemistry, physics and materials science, and have been grouped under 20 subject headings, ranging from catalysts to zeolites, and from battery electrode materials to pre-stressed superconducting wires. In 1985 two new high-resolution diffractometers are being commissioned, one at the SNS laboratory near Oxford, and one at the ILL in Grenoble. In different ways these machines represent perhaps the ultimate that can be achieved with neutrons and will permit refinement of complex structures with about 250 parameters and unit cell volumes of about 2500 Angstrom/sp3/. The new European Synchotron Facility will complement the Grenoble neutron diffractometers, and extend the role of high-resolution powder diffraction to the direct solution of crystal structures, pioneered in Sweden

  20. Berkeley High-Resolution Ball

    International Nuclear Information System (INIS)

    Diamond, R.M.

    1984-10-01

    Criteria for a high-resolution γ-ray system are discussed. Desirable properties are high resolution, good response function, and moderate solid angle so as to achieve not only double- but triple-coincidences with good statistics. The Berkeley High-Resolution Ball involved the first use of bismuth germanate (BGO) for anti-Compton shield for Ge detectors. The resulting compact shield permitted rather close packing of 21 detectors around a target. In addition, a small central BGO ball gives the total γ-ray energy and multiplicity, as well as the angular pattern of the γ rays. The 21-detector array is nearly complete, and the central ball has been designed, but not yet constructed. First results taken with 9 detector modules are shown for the nucleus 156 Er. The complex decay scheme indicates a transition from collective rotation (prolate shape) to single- particle states (possibly oblate) near spin 30 h, and has other interesting features

  1. Contradictions about Fine Structures in Meson Spectra and Proposed High-Resolution Hadron Spectrometer Using 'Interactive' Solid-State Hydrogen Target

    International Nuclear Information System (INIS)

    Maglich, Bogdan C.

    2004-01-01

    High resolution has been discouraged in meson spectrometry for 4 decades by the Doctrine of Experiments Incompatible with Theory (DEIT). DEIT a priori rejects narrow hadron resonances on the paradigm that only broad hadron peaks, Γ≥ 100 MeV, can exist -- in spite of the accumulated evidence to the contrary. The facts are: Mesons 2 orders of magnitude narrower than 'allowed' for hadrons, have been confirmed; a new one was announced at this conference. Narrow meson structures have been repeatedly reported at high momentum transfer, vertical bar t vertical bar >0.2, while they are absent at the low transfer, vertical bar t vertical bar ∼0.01, where 99% of the experiments are performed. Modification of meson mass and width as a function of the density of nuclear matter in which they are produced, have been recently reported.We postulate for meson spectra: (1) Intrinsic ('true') width, Γ, is different from the observable ('apparent') width, Γ': Γ< Γ' (2) Γ of all meson states are narrow and can be observed only at or near the maximum vertical bar t vertical bar reachable in the reaction, and (3) Γ of all meson resonances are subject to broadening as vertical bar t vertical bar decreases. Since both Γ' and the production σ are inversely proportional to vertical bar t vertical ar, most of the observed spectra are produced at the lowest vertical bar t vertical bar <0.01 and thus the peaks appear broad. We have conceptually designed a novel type hadron spectrometer with an order of magnitude better resolution (0.1 MeV). It would operate at 2 orders of magnitude higher vertical bar t vertical bar (0.3< vertical bar t vertical bar <1 (GeV/c)2, than most experiments to date (vertical bar t vertical bar <0.01). Mesons in the mass region 0.5 < Mx<5 GeV would be produced in πP→PX (baryons in PP→PP*) in a 'solid state hydrogen target' consisting of an array of plastic scintillator fibers, CH; collisions with C are electronically rejected. Missing mass of P is

  2. High-resolution resonant magnetic x-ray scattering on TbNi2B2C: Determination of the modulation wave vector in the orthorhombic phase

    International Nuclear Information System (INIS)

    Song, C.; Wermeille, D.; Goldman, A. I.; Canfield, P. C.; Rhee, J. Y.; Harmon, B. N.

    2001-01-01

    Resonant magnetic x-ray scattering measurements have been performed on a single crystal of TbNi 2 B 2 C to uniquely determine the modulation wave vector in the low-temperature orthorhombic phase. Below the transition temperature of 14.4(±0.1)K, two magnetic satellite peaks develop, centered on (h00) orth charge reflections. Our study shows that the longitudinal modulation of the magnetic moment is along the longer basal plane axes of the orthorhombic phase. Power law fits to the temperature dependence of the structural distortion, a/b-1, and the magnetic scattering intensity result in the same exponent, β, and transition temperature evidencing explicitly that the structural phase transition is magneto-elastic in origin

  3. A multi-sample based method for identifying common CNVs in normal human genomic structure using high-resolution aCGH data.

    Directory of Open Access Journals (Sweden)

    Chihyun Park

    Full Text Available BACKGROUND: It is difficult to identify copy number variations (CNV in normal human genomic data due to noise and non-linear relationships between different genomic regions and signal intensity. A high-resolution array comparative genomic hybridization (aCGH containing 42 million probes, which is very large compared to previous arrays, was recently published. Most existing CNV detection algorithms do not work well because of noise associated with the large amount of input data and because most of the current methods were not designed to analyze normal human samples. Normal human genome analysis often requires a joint approach across multiple samples. However, the majority of existing methods can only identify CNVs from a single sample. METHODOLOGY AND PRINCIPAL FINDINGS: We developed a multi-sample-based genomic variations detector (MGVD that uses segmentation to identify common breakpoints across multiple samples and a k-means-based clustering strategy. Unlike previous methods, MGVD simultaneously considers multiple samples with different genomic intensities and identifies CNVs and CNV zones (CNVZs; CNVZ is a more precise measure of the location of a genomic variant than the CNV region (CNVR. CONCLUSIONS AND SIGNIFICANCE: We designed a specialized algorithm to detect common CNVs from extremely high-resolution multi-sample aCGH data. MGVD showed high sensitivity and a low false discovery rate for a simulated data set, and outperformed most current methods when real, high-resolution HapMap datasets were analyzed. MGVD also had the fastest runtime compared to the other algorithms evaluated when actual, high-resolution aCGH data were analyzed. The CNVZs identified by MGVD can be used in association studies for revealing relationships between phenotypes and genomic aberrations. Our algorithm was developed with standard C++ and is available in Linux and MS Windows format in the STL library. It is freely available at: http://embio.yonsei.ac.kr/~Park/mgvd.php.

  4. High resolution metric imaging payload

    Science.gov (United States)

    Delclaud, Y.

    2017-11-01

    Alcatel Space Industries has become Europe's leader in the field of high and very high resolution optical payloads, in the frame work of earth observation system able to provide military government with metric images from space. This leadership allowed ALCATEL to propose for the export market, within a French collaboration frame, a complete space based system for metric observation.

  5. A novel method for the determination of mercury and selenium in shark tissue using high-resolution inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Paul, Mitchell C.; Toia, Robert F.; Nagy-Felsobuki, Ellak I. von

    2003-01-01

    A method for measuring Hg and Se in shark tissue by high-resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) has been developed. Using a matrix of 4% (v/v) aqueous methanol, the spray chamber and transfer tubing memory effects of Hg were significantly reduced. The methanol matrix was able to effectively wash out Hg (10 ppb) and return the signal to blank level in approximately 5 min. This enabled accurate and concomitant measurements of Hg and Se with detection limits (3σ blank signal, n=10) of 26 and 4 ppt, respectively. The recoveries of Hg and Se based on the CRM were 88 and 83%, respectively. The concentrations of Hg and Se in the (liver, muscle, kidney) of a hammerhead shark (dry weight) were (2.65±0.85, 7.09±1.32, 4.43±1.36) and (17.3±4.1, 1.28±0.29, 24.1±5.2) mg kg -1 (where the expanded uncertainty uses a k=2 value) respectively. Multi-elemental semi-quantitative analysis of a hammerhead shark liver, muscle and kidney revealed high levels of Cd, Zn and As

  6. Study of High-Resolution Spectroscopy of Plutonium. Part I. Contribution to the Classification of the Arc Spectrum. Part II. Determination of the Magnetic Moment of 239Pu

    International Nuclear Information System (INIS)

    Gerstenkorn, S.

    1962-01-01

    The study of the hyperfine structure and isotope shift enabled the positions of the first five levels of the multiplet 7 F 0-6 belonging to the fundamental configuration 5f 6 7s 2 to be determined. The classification of the arc spectrum begun in this way led to 25 odd levels, the number of classified lines (70) representing about 30 p. 100 of the light emitted by this hollow cathode in the visible. In addition, the isotope shifts of many lines and the data given by the King furnace show that the first levels of the configuration 5f 5 6d7s 2 are also low less than 8000 cm -1 above the fundamental level 7 F 0 . The proximity of the configuration f 6 s 2 and f 5 ds 2 shows that the bonding energies of the 5f and 6d electrons are of the same order of magnitude and this fact must be responsible for the multiple valences belonging to plutonium. From the hyperfine structure of spark lines (Pu II) the interval factor a 7 for the electron was deduced giving for the calculated nuclear moment of 239 Pu a value of +0.21 ±0.06 μ N . The position of the hyperfine components show that the nuclear moment is positive, although the theoretical value given by B. R. Mottelson and S. Nillson is negative and equal to -0.1 μ N . (author) [fr

  7. Structural Masquerade of Plesiomonas shigelloides Strain CNCTC 78/89 O-Antigen-High-Resolution Magic Angle Spinning NMR Reveals the Modified d-galactan I of Klebsiella pneumoniae.

    Science.gov (United States)

    Ucieklak, Karolina; Koj, Sabina; Pawelczyk, Damian; Niedziela, Tomasz

    2017-11-29

    The high-resolution magic angle spinning nuclear magnetic resonance spectroscopy (HR-MAS NMR) analysis of Plesiomonas shigelloides 78/89 lipopolysaccharide directly on bacteria revealed the characteristic structural features of the O -acetylated polysaccharide in the NMR spectra. The O -antigen profiles were unique, yet the pattern of signals in the, spectra along with their ¹H, 13 C chemical shift values, resembled these of d-galactan I of Klebsiella pneumoniae . The isolated O- specific polysaccharide (O-PS) of P. shigelloides strain CNCTC 78/89 was investigated by ¹H and 13 C NMR spectroscopy, mass spectrometry and chemical methods. The analyses demonstrated that the P. shigelloides 78/89 O- PS is composed of →3)-α-d-Gal p -(1→3)-β-d-Gal f 2OAc-(1→ disaccharide repeating units. The O- acetylation was incomplete and resulted in a microheterogeneity of the O- antigen. This O- acetylation generates additional antigenic determinants within the O- antigen, forms a new chemotype, and contributes to the epitopes recognized by the O- serotype specific antibodies. The serological cross-reactivities further confirmed the inter-specific structural similarity of these O- antigens.

  8. Recent applications of gas chromatography with high-resolution mass spectrometry.

    Science.gov (United States)

    Špánik, Ivan; Machyňáková, Andrea

    2018-01-01

    Gas chromatography coupled to high-resolution mass spectrometry is a powerful analytical method that combines excellent separation power of gas chromatography with improved identification based on an accurate mass measurement. These features designate gas chromatography with high-resolution mass spectrometry as the first choice for identification and structure elucidation of unknown volatile and semi-volatile organic compounds. Gas chromatography with high-resolution mass spectrometry quantitative analyses was previously focused on the determination of dioxins and related compounds using magnetic sector type analyzers, a standing requirement of many international standards. The introduction of a quadrupole high-resolution time-of-flight mass analyzer broadened interest in this method and novel applications were developed, especially for multi-target screening purposes. This review is focused on the development and the most interesting applications of gas chromatography coupled to high-resolution mass spectrometry towards analysis of environmental matrices, biological fluids, and food safety since 2010. The main attention is paid to various approaches and applications of gas chromatography coupled to high-resolution mass spectrometry for non-target screening to identify contaminants and to characterize the chemical composition of environmental, food, and biological samples. The most interesting quantitative applications, where a significant contribution of gas chromatography with high-resolution mass spectrometry over the currently used methods is expected, will be discussed as well. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Liquid chromatography-high resolution mass spectrometry (LC-HRMS) determination of stimulants, anorectic drugs and phosphodiesterase 5 inhibitors (PDE5I) in food supplements.

    Science.gov (United States)

    Strano-Rossi, Sabina; Odoardi, Sara; Castrignanò, Erika; Serpelloni, Giovanni; Chiarotti, Marcello

    2015-03-15

    The paper describes a liquid chromatography/high resolution mass spectrometry LC/HRMS method for the simultaneous identification and quantification of stimulants (ephedrines, caffeine, anorectic drugs such as phentermine, phendimetrazine, phenmetrazine, fenfluramine, benfluorex, mephentermine, fencanfamine, sibutramine) and PDE5I (sildenafil, vardenafil and tadalafil) in food supplements using a benchtop Orbitrap mass spectrometer. The mass detector, with a nominal resolving power of 100,000 (FWHM at m/z 200), operated in full scan mode in ESI positive ionization mode. Analytes were identified by retention times, accurate masses and correspondence of experimental and calculated isotopic patterns. The limits of detection (LOD) obtained varied from 1 to 25 ng g(-1) and limits of quantification (LOQ) were 50 ng g(-1) for all compounds. The method was linear for all the analytes in the ranges from 50 to 2000 ng g(-1), giving correlation coefficients>0.99. Accuracy (intended as %E) and repeatability (% CV) were always lower than 15%. The method was applied to the analysis of 36 dietary supplements, revealing the presence of ephedrine and/or pseudoephedrine in four of them, caffeine in eight of them and sildenafil in four of them. In one case, ephedrine was not reported on the label of the dietary supplement, as well as for caffeine in other two cases. A further confirmation of the analytes identity in positive samples was obtained through in-source fragmentation and comparison of the obtained fragments and their relative abundances with those from certified standards. As the acquisition mode is full scan, it would be also possible to re-process a previously acquired datafile for the investigation of untargeted analytes. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Development of a High-Resolution Laser Absorption Spectroscopy Method with Application to the Determination of Absolute Concentration of Gaseous Elemental Mercury in Air.

    Science.gov (United States)

    Srivastava, Abneesh; Hodges, Joseph T

    2018-05-07

    Isotope dilution-cold-vapor-inductively coupled plasma mass spectrometry (ID-CV-ICPMS) has become the primary standard for measurement of gaseous elemental mercury (GEM) mass concentration. However, quantitative mass spectrometry is challenging for several reasons including (1) the need for isotopic spiking with a standard reference material, (2) the requirement for bias-free passive sampling protocols, (3) the need for stable mass spectrometry interface design, and (4) the time and cost involved for gas sampling, sample processing, and instrument calibration. Here, we introduce a high-resolution laser absorption spectroscopy method that eliminates the need for sample-specific calibration standards or detailed analysis of sample treatment losses. This technique involves a tunable, single-frequency laser absorption spectrometer that measures isotopically resolved spectra of elemental mercury (Hg) spectra of 6 1 S 0 ← 6 3 P 1 intercombination transition near λ = 253.7 nm. Measured spectra are accurately modeled from first-principles using the Beer-Lambert law and Voigt line profiles combined with literature values for line positions, line shape parameters, and the spontaneous emission Einstein coefficient to obtain GEM mass concentration values. We present application of this method for the measurement of the equilibrium concentration of mercury vapor near room temperature. Three closed systems are considered: two-phase mixtures of liquid Hg and its vapor and binary two-phase mixtures of Hg-air and Hg-N 2 near atmospheric pressure. Within the experimental relative standard uncertainty, 0.9-1.5% congruent values of the equilibrium Hg vapor concentration are obtained for the Hg-only, Hg-air, Hg-N 2 systems, in confirmation with thermodynamic predictions. We also discuss detection limits and the potential of the present technique to serve as an absolute primary standard for measurements of gas-phase mercury concentration and isotopic composition.

  11. High-resolution structure of the Shigella type-III secretion needle by solid-state NMR and cryo-electron microscopy

    Science.gov (United States)

    Demers, Jean-Philippe; Habenstein, Birgit; Loquet, Antoine; Kumar Vasa, Suresh; Giller, Karin; Becker, Stefan; Baker, David; Lange, Adam; Sgourakis, Nikolaos G.

    2014-09-01

    We introduce a general hybrid approach for determining the structures of supramolecular assemblies. Cryo-electron microscopy (cryo-EM) data define the overall envelope of the assembly and rigid-body orientation of the subunits while solid-state nuclear magnetic resonance (ssNMR) chemical shifts and distance constraints define the local secondary structure, protein fold and inter-subunit interactions. Finally, Rosetta structure calculations provide a general framework to integrate the different sources of structural information. Combining a 7.7-Å cryo-EM density map and 996 ssNMR distance constraints, the structure of the type-III secretion system needle of Shigella flexneri is determined to a precision of 0.4 Å. The calculated structures are cross-validated using an independent data set of 691 ssNMR constraints and scanning transmission electron microscopy measurements. The hybrid model resolves the conformation of the non-conserved N terminus, which occupies a protrusion in the cryo-EM density, and reveals conserved pore residues forming a continuous pattern of electrostatic interactions, thereby suggesting a mechanism for effector protein translocation.

  12. Structural Insight on the Mechanism of Regulation of the MarR Family of Proteins: High-Resolution Crystal Structure of a Transcriptional Repressor from Methanobacterium thermoautotrophicum

    Energy Technology Data Exchange (ETDEWEB)

    Saridakis, Vivian; Shahinas, Dea; Xu, Xiaohui; Christendat, Dinesh (York); (Toronto); (CG)

    2008-03-31

    Transcriptional regulators belonging to the MarR family are characterized by a winged-helix DNA binding domain. These transcriptional regulators regulate the efflux and influx of phenolic agents in bacteria and archaea. In Escherichia coli, MarR regulates the multiple antibiotic resistance operon and its inactivation produces a multiple antibiotic resistance phenotype. In some organisms, active efflux of drug compounds will produce a drug resistance phenotype, whereas in other organisms, active influx of chlorinated hydrocarbons results in their rapid degradation. Although proteins in the MarR family are regulators of important biological processes, their mechanism of action is not well understood and structural information about how phenolic agents regulate the activity of these proteins is lacking. This article presents the three-dimensional structure of a protein of the MarR family, MTH313, in its apo form and in complex with salicylate, a known inactivator. A comparison of these two structures indicates that the mechanism of regulation involves a large conformational change in the DNA binding lobe. Electrophoretic mobility shift assay and biophysical analyses further suggest that salicylate inactivates MTH313 and prevents it from binding to its promoter region.

  13. Investigation of the feasibility to use Zeeman-effect background correction for the graphite furnace determination of phosphorus using high-resolution continuum source atomic absorption spectrometry as a diagnostic tool

    Energy Technology Data Exchange (ETDEWEB)

    Lepri, Fabio G. [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900 Florianopolis, SC (Brazil); Welz, Bernhard, E-mail: w.bernardo@terra.com.b [Departamento de Quimica, Universidade Federal de Santa Catarina, 88040-900 Florianopolis, SC (Brazil); Dessuy, Morgana B.; Vale, Maria Goreti R. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves, 9500, 91501-970 Porto Alegre-RS (Brazil); Bohrer, Denise [Departamento de Quimica, Universidade Federal de Santa Maria, 97110-905 Santa Maria, RS (Brazil); Loos-Vollebregt, Margaretha T.C. de [Delft University of Technology, Faculty of Applied Sciences, Analytical Biotechnology, Julianalaan 137, 2628 BL Delft (Netherlands); Department of Analytical Chemistry, Ghent University, Krijgslaan 281 - S12, B-9000 Ghent (Belgium); Mao Donghuang; Becker-Ross, Helmut [ISAS, Institute for Analytical Sciences, Department of Interface Spectroscopy, Albert-Einstein Str. 9, 12489 Berlin (Germany)

    2010-01-15

    The determination of phosphorus by graphite furnace atomic absorption spectrometry at the non-resonance line at 213.6 nm, and the capability of Zeeman-effect background correction (Z-BC) to deal with the fine-structured background absorption due to the PO molecule have been investigated in the presence of selected chemical modifiers. Two line source atomic absorption spectrometers, one with a longitudinally heated and the other with a transversely heated graphite tube atomizer have been used in this study, as well as two prototype high-resolution continuum source atomic absorption spectrometers, one of which had a longitudinally arranged magnet at the furnace. It has been found that Z-BC is capable correcting very well the background caused by the PO molecule, and also that of the NO molecule, which has been encountered when the Pd + Ca mixed modifier was used. Both spectra exhibited some Zeeman splitting, which, however, did not cause any artifacts or correction errors. The practical significance of this study is to confirm that accurate results can be obtained for the determination of phosphorus using Z-BC. The best sensitivity with a characteristic mass of m{sub 0} = 11 ng P has been obtained with the pure Pd modifier, which also caused the lowest background level. The characteristic mass obtained with the mixed Pd+Ca modifier depended on the equipment used and was between m{sub 0} = 9 ng P and m{sub 0} = 15 ng P, and the background signal was higher. The major problem of Z-BC remains the relatively restricted linear working range.

  14. High-resolution intravital microscopy.

    Directory of Open Access Journals (Sweden)

    Volker Andresen

    Full Text Available Cellular communication constitutes a fundamental mechanism of life, for instance by permitting transfer of information through synapses in the nervous system and by leading to activation of cells during the course of immune responses. Monitoring cell-cell interactions within living adult organisms is crucial in order to draw conclusions on their behavior with respect to the fate of cells, tissues and organs. Until now, there is no technology available that enables dynamic imaging deep within the tissue of living adult organisms at sub-cellular resolution, i.e. detection at the level of few protein molecules. Here we present a novel approach called multi-beam striped-illumination which applies for the first time the principle and advantages of structured-illumination, spatial modulation of the excitation pattern, to laser-scanning-microscopy. We use this approach in two-photon-microscopy--the most adequate optical deep-tissue imaging-technique. As compared to standard two-photon-microscopy, it achieves significant contrast enhancement and up to 3-fold improved axial resolution (optical sectioning while photobleaching, photodamage and acquisition speed are similar. Its imaging depth is comparable to multifocal two-photon-microscopy and only slightly less than in standard single-beam two-photon-microscopy. Precisely, our studies within mouse lymph nodes demonstrated 216% improved axial and 23% improved lateral resolutions at a depth of 80 µm below the surface. Thus, we are for the first time able to visualize the dynamic interactions between B cells and immune complex deposits on follicular dendritic cells within germinal centers (GCs of live mice. These interactions play a decisive role in the process of clonal selection, leading to affinity maturation of the humoral immune response. This novel high-resolution intravital microscopy method has a huge potential for numerous applications in neurosciences, immunology, cancer research and

  15. High-Resolution Intravital Microscopy

    Science.gov (United States)

    Andresen, Volker; Pollok, Karolin; Rinnenthal, Jan-Leo; Oehme, Laura; Günther, Robert; Spiecker, Heinrich; Radbruch, Helena; Gerhard, Jenny; Sporbert, Anje; Cseresnyes, Zoltan; Hauser, Anja E.; Niesner, Raluca

    2012-01-01

    Cellular communication constitutes a fundamental mechanism of life, for instance by permitting transfer of information through synapses in the nervous system and by leading to activation of cells during the course of immune responses. Monitoring cell-cell interactions within living adult organisms is crucial in order to draw conclusions on their behavior with respect to the fate of cells, tissues and organs. Until now, there is no technology available that enables dynamic imaging deep within the tissue of living adult organisms at sub-cellular resolution, i.e. detection at the level of few protein molecules. Here we present a novel approach called multi-beam striped-illumination which applies for the first time the principle and advantages of structured-illumination, spatial modulation of the excitation pattern, to laser-scanning-microscopy. We use this approach in two-photon-microscopy - the most adequate optical deep-tissue imaging-technique. As compared to standard two-photon-microscopy, it achieves significant contrast enhancement and up to 3-fold improved axial resolution (optical sectioning) while photobleaching, photodamage and acquisition speed are similar. Its imaging depth is comparable to multifocal two-photon-microscopy and only slightly less than in standard single-beam two-photon-microscopy. Precisely, our studies within mouse lymph nodes demonstrated 216% improved axial and 23% improved lateral resolutions at a depth of 80 µm below the surface. Thus, we are for the first time able to visualize the dynamic interactions between B cells and immune complex deposits on follicular dendritic cells within germinal centers (GCs) of live mice. These interactions play a decisive role in the process of clonal selection, leading to affinity maturation of the humoral immune response. This novel high-resolution intravital microscopy method has a huge potential for numerous applications in neurosciences, immunology, cancer research and developmental biology

  16. High-resolution crystal structure reveals a HEPN domain at the C-terminal region of S. cerevisiae RNA endonuclease Swt1

    International Nuclear Information System (INIS)

    Peng, Shuxia; Zhou, Ke; Wang, Wenjia; Gao, Zengqiang; Dong, Yuhui; Liu, Quansheng

    2014-01-01

    Highlights: • Crystal structure of the C-terminal (CT) domain of Swt1 was determined at 2.3 Å. • Structure of the CT domain was identified as HEPN domain superfamily member. • Low-resolution envelope of Swt1 full-length in solution was analyzed by SAXS. • The middle and CT domains gave good fit to SAXS structural model. - Abstract: Swt1 is an RNA endonuclease that plays an important role in quality control of nuclear messenger ribonucleoprotein particles (mRNPs) in eukaryotes; however, its structural details remain to be elucidated. Here, we report the crystal structure of the C-terminal (CT) domain of Swt1 from Saccharomyces cerevisiae, which shares common characteristics of higher eukaryotes and prokaryotes nucleotide binding (HEPN) domain superfamily. To study in detail the full-length protein structure, we analyzed the low-resolution architecture of Swt1 in solution using small angle X-ray scattering (SAXS) method. Both the CT domain and middle domain exhibited a good fit upon superimposing onto the molecular envelope of Swt1. Our study provides the necessary structural information for detailed analysis of the functional role of Swt1, and its importance in the process of nuclear mRNP surveillance

  17. Enantioselective determination of (R)-zopiclone and (S)-zopiclone (eszopiclone) in human hair by micropulverized extraction and chiral liquid chromatography/high resolution mass spectrometry.

    Science.gov (United States)

    Miyaguchi, Hajime; Kuwayama, Kenji

    2017-10-13

    Zopiclone and its (S)-enantiomer (eszopiclone) are commonly prescribed for insomnia. Despite the high demand for enantioselective differentiation, the chiral analysis of zopiclone in hair has not been reported. In this study, a method for the enantioselective quantification of zopiclone in human hair was developed. The extraction medium and duration were optimized using real eszopiclone-positive hair samples. Specifically, micropulverized extraction with 3.0M ammonium phosphate buffer (pH 8.4) involving salting-out assisted liquid-liquid extraction with acetonitrile was utilized to minimize the degradation of zopiclone and for rapid and facile operation. On the other hand, recovery of the conventional solid-liquid extraction involved overnight soaking in 3.0M ammonium phosphate buffer (pH 8.4) was only 0.58±0.12% of the maximum recovery achieved by the present method due to the decomposition in the phosphate buffer. An excellent chiral separation (Rs=5.0) was achieved using a chiral stationary phase comprising cellulose tris(3,5-dichlorophenylcarbamate) and a volatile mobile phase of 10mM ammonium carbonate (pH 8.0)-acetonitrile (25:75, v/v). Detection was carried out using liquid chromatography/high resolution mass spectrometry (LC/HRMS) with electrospray ionization. A Q Exactive mass spectrometer equipped with a quadrupole-Orbitrap analyzer was used for detection. The concentration of 0.50pg/mg was defined as the lowest limit of quantification using 5mg of hair sample. Using the developed approach, the concentration of eszopiclone in hair after a single 2-mg dose was found to be 441pg/mg, which was higher than all the reported values regarding a single administration of zopiclone. After daily administration of racemic zopiclone (3.75mg/day), the concentrations of (R)-enantiomer and (S)-enantiomer in the black hair were 5.30-8.31ng/mg and 7.96-12.8ng/mg, respectively, and the concentration of the (S)-enantiomer was always higher than that of the (R

  18. Spatial attributes of the four-helix bundle group of bacteriocins – The high-resolution structure of BacSp222 in solution

    KAUST Repository

    Nowakowski, Michał

    2017-11-01

    BacSp222 is a multifunctional bacteriocin produced by Staphylococcus pseudintermedius strain 222, an opportunistic pathogen of domestic animals. At micromolar concentrations, BacSp222 kills Gram-positive bacteria and is cytotoxic toward mammalian cells, while at nanomolar doses, it acts as an immunomodulatory factor, enhancing nitric oxide release in macrophage-like cell lines. The bacteriocin is a cationic, N-terminally formylated, 50-amino-acid-long linear peptide that is rich in tryptophan residues.In this study, the solution structure of BacSp222 was determined and compared to the currently known structures of similar bacteriocins. BacSp222 was isolated from a liquid culture medium in a uniformly 13C- and 15N-labeled form, and NMR data were collected. The structure was calculated based on NMR-derived constraints and consists of a rigid and tightly packed globular bundle of four alpha-helices separated by three short turns.Although the amino acid sequence of BacSp222 has no significant similarity to any known peptide or protein, a 3D structure similarity search indicates a close relation to other four-helix bundle-motif bacteriocins, such as aureocin A53, lacticin Q and enterocins 7A/7B. Assuming similar functions, biology, structure and physicochemical properties, we propose to distinguish the four-helix bundle bacteriocins as a new Type A in subclass IId of bacteriocins, containing linear, non-pediocin-like peptides.

  19. High resolution 148Nd(3He, ny) two proton stripping reaction and the structure of the O2+ state in 150Sm

    International Nuclear Information System (INIS)

    Sharpey-Schafer, J.F.; Dinoko, T.S.; Herbert, M.S.; Orce, J.N.; Papka, P.; Kheswa, B.V.; Ndayishimye, J.; Bvumbi, S.P.; Jones, P.M.; Bucher, T.D.; Lawrie, E.A.; Lawrie, J.J.; Negi, D.; Shirinda, O.; Wiedeking, M.; Vymers, P.; Easton, J.L.; Noncolela, S.P.; Sithole, P.; Khumalo, N.; Majola, S.N.T.; Stankiewicz, M.A.

    2014-01-01

    The challenge of achieving high resolution in binary reactions involving an outgoing high energy neutron is solved by detecting the γ-ray decay of populated excited states in an array of escape suppressed HPGe detectors in coincidence with fast neutrons detected in a wall of scintillator detectors 2 m down beam of the target. The selectivity of the arrangement is of the order of 1 in 1000. The time-of-flight difference is sufficient to separate fast neutrons from direct reactions from a large background of statistical neutrons from fusion-evaporation reactions. Our interest is in the wavefunction of the 0 2 + state at 740 keV in the N=88 nucleus 150 Sm which, with the 0 2 + state in 100 Ru, are the only two excited states observed in 2β2ν double β-decay. (authors)

  20. Cryo-EM Structure Determination Using Segmented Helical Image Reconstruction.

    Science.gov (United States)

    Fromm, S A; Sachse, C

    2016-01-01

    Treating helices as single-particle-like segments followed by helical image reconstruction has become the method of choice for high-resolution structure determination of well-ordered helical viruses as well as flexible filaments. In this review, we will illustrate how the combination of latest hardware developments with optimized image processing routines have led to a series of near-atomic resolution structures of helical assemblies. Originally, the treatment of helices as a sequence of segments followed by Fourier-Bessel reconstruction revealed the potential to determine near-atomic resolution structures from helical specimens. In the meantime, real-space image processing of helices in a stack of single particles was developed and enabled the structure determination of specimens that resisted classical Fourier helical reconstruction and also facilitated high-resolution structure determination. Despite the progress in real-space analysis, the combination of Fourier and real-space processing is still commonly used to better estimate the symmetry parameters as the imposition of the correct helical symmetry is essential for high-resolution structure determination. Recent hardware advancement by the introduction of direct electron detectors has significantly enhanced the image quality and together with improved image processing procedures has made segmented helical reconstruction a very productive cryo-EM structure determination method. © 2016 Elsevier Inc. All rights reserved.

  1. High-Resolution MRI in Rectal Cancer

    International Nuclear Information System (INIS)

    Dieguez, Adriana

    2010-01-01

    High-resolution MRI is the best method of assessing the relation of the rectal tumor with the potential circumferential resection margin (CRM). Therefore it is currently considered the method of choice for local staging of rectal cancer. The primary surgery of rectal cancer is total mesorectal excision (TME), which plane of dissection is formed by the mesorectal fascia surrounding mesorectal fat and rectum. This fascia will determine the circumferential margin of resection. At the same time, high resolution MRI allows adequate pre-operative identification of important prognostic risk factors, improving the selection and indication of therapy for each patient. This information includes, besides the circumferential margin of resection, tumor and lymph node staging, extramural vascular invasion and the description of lower rectal tumors. All these should be described in detail in the report, being part of the discussion in the multidisciplinary team, the place where the decisions involving the patient with rectal cancer will take place. The aim of this study is to provide the information necessary to understand the use of high resolution MRI in the identification of prognostic risk factors in rectal cancer. The technical requirements and standardized report for this study will be describe, as well as the anatomical landmarks of importance for the total mesorectal excision (TME), as we have said is the surgery of choice for rectal cancer. (authors) [es

  2. Ultrahigh and High Resolution Structures and Mutational Analysis of Monomeric Streptococcus pyogenes SpeB Reveal a Functional Role for the Glycine-rich C-terminal Loop

    Energy Technology Data Exchange (ETDEWEB)

    González-Páez, Gonzalo E.; Wolan, Dennis W. (Scripps)

    2012-09-05

    Cysteine protease SpeB is secreted from Streptococcus pyogenes and has been studied as a potential virulence factor since its identification almost 70 years ago. Here, we report the crystal structures of apo mature SpeB to 1.06 {angstrom} resolution as well as complexes with the general cysteine protease inhibitor trans-epoxysuccinyl-L-leucylamido(4-guanidino)butane and a novel substrate mimetic peptide inhibitor. These structures uncover conformational changes associated with maturation of SpeB from the inactive zymogen to its active form and identify the residues required for substrate binding. With the use of a newly developed fluorogenic tripeptide substrate to measure SpeB activity, we determined IC{sub 50} values for trans-epoxysuccinyl-L-leucylamido(4-guanidino)butane and our new peptide inhibitor and the effects of mutations within the C-terminal active site loop. The structures and mutational analysis suggest that the conformational movements of the glycine-rich C-terminal loop are important for the recognition and recruitment of biological substrates and release of hydrolyzed products.

  3. Validation and optimization of a chromatographic method for the quantitative and qualitative determination of cocaine and heroin through liquid chromatography of high resolution

    International Nuclear Information System (INIS)

    Montero Aguilar, A.L.

    1997-01-01

    A (HPLC) chromatographic method was optimized in this work, for the determination of cocaine and heroin in seizures, through the application of the factorial and the simplex design. It applied the developed methodology in the determination of the content of cocaine and of heroin in nine different samples. The application of this methodology in abuse drugs seizures samples, turned out analytically satisfactory for the time of analysis and the veracity of the results. It also complements efficiently the qualitative analysis of cocaine and heroin, that the Laboratory of Physical and Chemical Investigations of the Department of Forensic Sciences of the Agency of Judicial Investigation carries out. (S. Grainger) [es

  4. Solid-phase extraction and separation procedure for trace aluminum in water samples and its determination by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS).

    Science.gov (United States)

    Ciftci, Harun; Er, Cigdem

    2013-03-01

    In the present study, a separation/preconcentration procedure for determination of aluminum in water samples has been developed by using a new atomic absorption spectrometer concept with a high-intensity xenon short-arc lamp as continuum radiation source, a high-resolution double-echelle monochromator, and a charge-coupled device array detector. Sample solution pH, sample volume, flow rate of sample solution, volume, and concentration of eluent for solid-phase extraction of Al chelates with 4-[(dicyanomethyl)diazenyl] benzoic acid on polymeric resin (Duolite XAD-761) have been investigated. The adsorbed aluminum on resin was eluted with 5 mL of 2 mol L(-1) HNO(3) and its concentration was determined by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). Under the optimal conditions, limit of detection obtained with HR-CS FAAS and Line Source FAAS (LS-FAAS) were 0.49 μg L(-1) and 3.91 μg L(-1), respectively. The accuracy of the procedure was confirmed by analyzing certified materials (NIST SRM 1643e, Trace elements in water) and spiked real samples. The developed procedure was successfully applied to water samples.

  5. Fine-structural distribution of MMP-2 and MMP-9 activities in the rat skeletal muscle upon training: a study by high-resolution in situ zymography.

    Science.gov (United States)

    Yeghiazaryan, Marine; Żybura-Broda, Katarzyna; Cabaj, Anna; Włodarczyk, Jakub; Sławińska, Urszula; Rylski, Marcin; Wilczyński, Grzegorz M

    2012-07-01

    Matrix metalloproteinases (MMPs) are key regulators of extracellular matrix remodeling, but have also important intracellular targets. The purpose of this study was to examine the activity and subcellular localization of the gelatinases MMP-2 and MMP-9 in skeletal muscle of control and physically trained rats. In control hind limb muscle, the activity of the gelatinases was barely detectable. In contrast, after 5 days of intense exercise, in Soleus (Sol), but not Extensor digitorum longus (EDL) muscle, significant upregulation of gelatinolytic activity in myofibers was observed mainly in the nuclei, as assessed by high resolution in situ zymography. The nuclei of quiescent satellite cells did not contain the activity. Within the myonuclei, the gelatinolytic activity colocalized with an activated RNA Polymerase II. Also in Sol, but not in EDL, there were few foci of mononuclear cells with strongly positive cytoplasm, associated with apparent necrotic myofibers. These cells were identified as activated satellite cells/myoblasts. No extracellular gelatinase activity was observed. Gel zymography combined with subcellular fractionation revealed training-related upregulation of active MMP-2 in the nuclear fraction, and increase of active MMP-9 in the cytoplasmic fraction of Sol. Using RT-PCR, selective increase in MMP-9 mRNA was observed. We conclude that training activates nuclear MMP-2, and increases expression and activity of cytoplasmic MMP-9 in Sol, but not in EDL. Our results suggest that the gelatinases are involved in muscle adaptation to training, and that MMP-2 may play a novel role in myonuclear functions.

  6. Use of high resolution satellite images for tracking of changes in the lineament structure, caused by earthquakes, situated nearly the Pacific coast of the North and South America.

    Science.gov (United States)

    Arellano-Baeza, A. A.; Garcia, R. V.; Trejo-Soto, M.

    The Pacific coast of the North and South America is one of the most seismically and volcanically active regions in the world forming part of the so-called Ring of Fire More than 10 earthquakes with the Richter scale magnitude 4 5 were analyzed They were located in the regions with small seasonal variations and limited vegetation to facilitate the tracking of features associated with the seismic activity only High resolution Aster satellite images were used to extract the principal lineaments using The Lineament Extraction and Stripes Statistic Analysis LESSA software package It was found that the number and orientation of lineaments changed significantly about one month before an earthquake approximately and a few months later the system returns to its initial state This effect increases with the earthquake magnitude and it is much more easily detectable in case of convergent plate boundaries for example Nasca and South American plates The results obtained open the possibility to develop a methodology able to evaluate the seismic risk in the regions with similar geological conditions

  7. Determination of mycophenolic acid in mest products using mixed mode reversed phase-anion exchange clean-up and liquid chromatography-high-resolution mass spectrometry

    DEFF Research Database (Denmark)

    Sørensen, Louise Marie; Nielsen, Kristian Fog; Jacobsen, Thomas

    2008-01-01

    A method for determination of mycophenolic acid (MPA) in dry-cured ham, fermented sausage and liver pate is described. MPA was extracted from meat with bicarbonate-acetonitrile, further cleaned-up by mixed mode reversed phase-anion exchange and detected using a LC-MS system with electrospray...

  8. High-resolution structural studies of ultra-thin magnetic, transition metal overlayers and two-dimensional transition metal oxides using synchrotron radiation

    International Nuclear Information System (INIS)

    Kellar, S.A.; Lawrence Berkeley National Lab., CA

    1997-05-01

    This thesis report the surface-structure determination of three, ultra-thin magnetic transition-metal films, Fe/Au(100), Mn/Ni(100), and Mn/Cu(100) using Angle-Resolved Photoemission Extended Fine Structure (ARPEFS) and photoelectron holography. These structural studies are the first to use non-s initial states in the ARPEFS procedure. This thesis also reports an ARPEFS surface-structure determination of a two-dimensional transition-metal oxide, [(1 x 1)O/W(110)] x 12. The authors have analyzed the ARPFES signal from the Au 4f 7/5 core level of the Au(1 ML)/Fe(15 ML)/Au(100) system. The analysis shows that the Fe grows layer by layer with one monolayer of gold, acting as a surfactant, remaining on top of the growing Fe layers. These surface gold atoms sit in the four-fold hollow site, 1.67 ± 0.02 A above the iron surface. The grown Fe layer is very much like the bulk, bcc iron, with an interlayer spacing of 1.43 ± 0.03 A. Analysis of the Mn 3p ARPEFS signals from c(2 x 2)Mn/Ni(100) and c(2 x 2)Mn/Cu(100) shows that the Mn forms highly corrugated surface alloys. The corrugation of the Mn/Ni(100) and Mn/Cu(100) systems are 0.24 ± 0.02 A and 0.30 ± 0.04 A respectively. In both cases the Mn is sticking above the plane of the surface substrate atoms. For the Mn/Ni(100) system the first layer Ni is contracted 4% from the bulk value. The Mn/Cu(100) system shows bulk spacing for the substrate Cu. Photoelectron holography shows that the Mn/Ni interface is very abrupt with very little Mn leaking into the second layer, while the Mn/Cu(100) case has a significant amount of Mn leaking into the second layer. A new, five-element electrostatic electron lens was developed for hemispherical electron-energy analyzers. This lens system can be operated at constant transverse or constants angular magnification, and has been optimized for use with the very small photon-spot sizes. Improvements to the hemispherical electron-energy analyzer are also discussed

  9. High-resolution structural studies of ultra-thin magnetic, transition metal overlayers and two-dimensional transition metal oxides using synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Kellar, S.A. [Univ. of California, Berkeley, CA (United States). Dept. of Chemistry]|[Lawrence Berkeley National Lab., CA (United States). Advanced Light Source Div.

    1997-05-01

    This thesis report the surface-structure determination of three, ultra-thin magnetic transition-metal films, Fe/Au(100), Mn/Ni(100), and Mn/Cu(100) using Angle-Resolved Photoemission Extended Fine Structure (ARPEFS) and photoelectron holography. These structural studies are the first to use non-s initial states in the ARPEFS procedure. This thesis also reports an ARPEFS surface-structure determination of a two-dimensional transition-metal oxide, [(1 x 1)O/W(110)] x 12. The authors have analyzed the ARPFES signal from the Au 4f{sub 7/5} core level of the Au(1 ML)/Fe(15 ML)/Au(100) system. The analysis shows that the Fe grows layer by layer with one monolayer of gold, acting as a surfactant, remaining on top of the growing Fe layers. These surface gold atoms sit in the four-fold hollow site, 1.67 {+-} 0.02 A above the iron surface. The grown Fe layer is very much like the bulk, bcc iron, with an interlayer spacing of 1.43 {+-} 0.03 A. Analysis of the Mn 3p ARPEFS signals from c(2 x 2)Mn/Ni(100) and c(2 x 2)Mn/Cu(100) shows that the Mn forms highly corrugated surface alloys. The corrugation of the Mn/Ni(100) and Mn/Cu(100) systems are 0.24 {+-} 0.02 A and 0.30 {+-} 0.04 A respectively. In both cases the Mn is sticking above the plane of the surface substrate atoms. For the Mn/Ni(100) system the first layer Ni is contracted 4% from the bulk value. The Mn/Cu(100) system shows bulk spacing for the substrate Cu. Photoelectron holography shows that the Mn/Ni interface is very abrupt with very little Mn leaking into the second layer, while the Mn/Cu(100) case has a significant amount of Mn leaking into the second layer. A new, five-element electrostatic electron lens was developed for hemispherical electron-energy analyzers. This lens system can be operated at constant transverse or constants angular magnification, and has been optimized for use with the very small photon-spot sizes. Improvements to the hemispherical electron-energy analyzer are also discussed.

  10. Innovative method of direct determination of the content of paraffins, naphthenes, aromatics and sulfur compounds by capillary high-resolution gas chromatography

    Directory of Open Access Journals (Sweden)

    R. Baizhumanova

    2012-03-01

    Full Text Available Based on determination of individual Hydrocarbon (paraffins, naphthenes, aromatics and Sulphur components of fuels and their mixture on the thin bonded of absorber (the stationary phase is a 100-metre silica capillary column, containing 0.5μm film thickness of bonded dimethylpolysiloxane phase by means of the selective solvents (mobile phase combined with technique of ionization of separated compounds by Flame Ionization Detector (FID and Sulphur Chemiluminescence Detector (SCD.

  11. Spatial and temporal changes in household structure locations using high-resolution satellite imagery for population assessment: an analysis in southern Zambia, 2006-2011

    Directory of Open Access Journals (Sweden)

    Timothy Shields

    2016-05-01

    Full Text Available Satellite imagery is increasingly available at high spatial resolution and can be used for various purposes in public health research and programme implementation. Comparing a census generated from two satellite images of the same region in rural southern Zambia obtained four and a half years apart identified patterns of household locations and change over time. The length of time that a satellite image-based census is accurate determines its utility. Households were enumerated manually from satellite images obtained in 2006 and 2011 of the same area. Spatial statistics were used to describe clustering, cluster detection, and spatial variation in the location of households. A total of 3821 household locations were enumerated in 2006 and 4256 in 2011, a net change of 435 houses (11.4% increase. Comparison of the images indicated that 971 (25.4% structures were added and 536 (14.0% removed. Further analysis suggested similar household clustering in the two images and no substantial difference in concentration of households across the study area. Cluster detection analysis identified a small area where significantly more household structures were removed than expected; however, the amount of change was of limited practical significance. These findings suggest that random sampling of households for study participation would not induce geographic bias if based on a 4.5-year-old image in this region. Application of spatial statistical methods provides insights into the population distribution changes between two time periods and can be helpful in assessing the accuracy of satellite imagery.

  12. A High-Resolution Crystal Structure of a Psychrohalophilic α-Carbonic Anhydrase from Photobacterium profundum Reveals a Unique Dimer Interface.

    Directory of Open Access Journals (Sweden)

    Vijayakumar Somalinga

    Full Text Available Bacterial α-carbonic anhydrases (α-CA are zinc containing metalloenzymes that catalyze the rapid interconversion of CO2 to bicarbonate and a proton. We report the first crystal structure of a pyschrohalophilic α-CA from a deep-sea bacterium, Photobacterium profundum. Size exclusion chromatography of the purified P. profundum α-CA (PprCA reveals that the protein is a heterogeneous mix of monomers and dimers. Furthermore, an "in-gel" carbonic anhydrase activity assay, also known as protonography, revealed two distinct bands corresponding to monomeric and dimeric forms of PprCA that are catalytically active. The crystal structure of PprCA was determined in its native form and reveals a highly conserved "knot-topology" that is characteristic of α-CA's. Similar to other bacterial α-CA's, PprCA also crystallized as a dimer. Furthermore, dimer interface analysis revealed the presence of a chloride ion (Cl- in the interface which is unique to PprCA and has not been observed in any other α-CA's characterized so far. Molecular dynamics simulation and chloride ion occupancy analysis shows 100% occupancy for the Cl- ion in the dimer interface. Zinc coordinating triple histidine residues, substrate binding hydrophobic patch residues, and the hydrophilic proton wire residues are highly conserved in PprCA and are identical to other well-studied α-CA's.

  13. A new technique for obtaining high-resolution pore pressure records in thick claystone aquitards and its use to determine in situ compressibility

    Science.gov (United States)

    Smith, Laura A.; van der Kamp, Garth; Jim Hendry, M.

    2013-02-01

    Laboratory tests are commonly used to determine properties (vertical compressibility, α; specific storage, SS; and vertical hydraulic conductivity, Kv) of claystone aquitards; however, whether data representative of in situ conditions can be obtained from disturbed samples is questionable. Here, we present a method to determine the in situ α and SS of a thick sequence of Cretaceous aged claystone by estimating the loading efficiency (γ) of a formation from pore pressure responses to barometric pressure fluctuations. We installed 10 vibrating wire pressure transducers at different depths (25-325 m below ground) in a thick claystone aquitard by placing them directly within the cement-bentonite grout. Two years of continuous transducer records using this method appeared to provide pore pressure data with a resolution of better than one part in 105, equivalent to millimeter of hydraulic head change. Pore pressure responses to barometric pressure changes, earth tides, and precipitation events can be clearly identified, and the barometric responses can be easily analyzed. The resulting values of γ (0.6-0.93), α (2.5 × 10-7 to 2.2 × 10-6 kPa-1), and SS (2.6 × 10-5 to 4.5 × 10-6 m-1) all decrease with depth. The results are comparable with the limited existing data for in situ estimates of SS and are as much as an order of magnitude smaller than laboratory estimates of SS for similar aquitard deposits. Our findings suggest that the fully grouted transducer method can provide an accurate and reliable means to monitor pore pressure changes and to determine in situ parameters for bedrock aquitard systems.

  14. An enhanced method to determine the Young’s modulus of technical single fibres by means of high resolution digital image correlation

    Science.gov (United States)

    Huether, Jonas; Rupp, Peter; Kohlschreiber, Ina; André Weidenmann, Kay

    2018-04-01

    To obtain mechanical tensile properties of materials it is customary to equip the specimen directly with a device to measure strain and Young’s modulus correctly and only within the measuring length defined by the standards. Whereas a variety of tools such as extensometers, strain gauges and optical systems are available for specimens on coupon level, no market-ready tools to measure strains of single fibres during single fibre tensile tests are available. Although there is a standard for single fibre testing, the procedures described there are only capable of measuring strains of the whole testing setup rather than the strain of the fibre. Without a direct strain measurement on the specimen, the compliance of the test rig itself influences the determination of the Young’s modulus. This work aims to fill this gap by establishing an enhanced method to measure strains directly on the tested fibre and thus provide accurate values for Young’s modulus. It is demonstrated that by applying and then optically tracking fluorescing polymeric beads on single glass fibres, Young’s modulus is determined directly and with high repeatability, without a need to measure at different measuring lengths or compensating for the system compliance. Employing this method to glass fibres, a Young’s modulus of approximately 82.5 GPa was determined, which is in the range of values obtained by applying a conventional procedure. This enhanced measuring technology achieves high accuracy and repeatability while reducing scatter of the data. It was demonstrated that the fluorescing beads do not affect the fibre properties.

  15. Depth determination of low-energy photon emitter deposits in tissue by means of high-resolution X-ray spectrometry

    International Nuclear Information System (INIS)

    Schlueter, W.

    1982-01-01

    A method has been developed for ascertaining the depth of low-energy photon emitters deposited in wounds. It is based on the determination of the energy-dependent absorption of the emitted photons by the tissue separating source and detector. The method is applicable to counting for low-energy photon-emitting nuclides that can be characterized by more than one quantum energy. Attenuation coefficients were given for lard, beef, and five tissue- equivalent materials. For spectrometry, a planar Ge(Li) detector proved most suitable. (author)

  16. High Resolution Thermometry for EXACT

    Science.gov (United States)

    Panek, J. S.; Nash, A. E.; Larson, M.; Mulders, N.

    2000-01-01

    High Resolution Thermometers (HRTs) based on SQUID detection of the magnetization of a paramagnetic salt or a metal alloy has been commonly used for sub-nano Kelvin temperature resolution in low temperature physics experiments. The main applications to date have been for temperature ranges near the lambda point of He-4 (2.177 K). These thermometers made use of materials such as Cu(NH4)2Br4 *2H2O, GdCl3, or PdFe. None of these materials are suitable for EXACT, which will explore the region of the He-3/He-4 tricritical point at 0.87 K. The experiment requirements and properties of several candidate paramagnetic materials will be presented, as well as preliminary test results.

  17. Linking structure and vibrational mode coupling using high-resolution infrared spectroscopy: A comparison of gauche and trans 1-chloro-2-fluoroethane

    Science.gov (United States)

    Miller, C. Cameron; Stone, Stephen C.; Philips, Laura A.

    1995-01-01

    The high-resolution infrared spectrum of 1-chloro-2-fluoroethane in a molecular beam was collected over the 2975-2994 cm-1 spectral region. The spectral region of 2975-2981 cm-1 contains a symmetric C-H stretching vibrational band of the gauche conformer containing the 35Cl isotope. The spectral region of 2985-2994 cm-1 contains three vibrational bands of the trans conformer. Two of the three bands are assigned as an antisymmetric C-H stretch of each of the two different chlorine isotopes. The third band is assigned as a symmetric C-H stretch of the 35Cl isotope. The gauche conformer of 1-chloro-2-fluoroethane showed doublet patterns similar to those previously observed in 1,2-difluoroethane. The model for 1,2-difluoroethane is further refined in the present work. These refinements suggest that the coupling dark state in 1,2-difluoroethane is composed of 1 quantum C-H bend, 1 quantum C-C stretch, and 12 quanta of torsion. For 1-chloro-2-fluoroethane the dark state could not be identified due to a small data set. The trans conformer of 1-chloro-2-fluoroethane showed no evidence of mode coupling in the three vibrational bands. Including 2-fluoroethanol in this series of molecules, the extent of vibrational mode coupling did not correlate with the density of states available for coupling. Therefore, density of states alone is insufficient to explain the observed trend. A correlation was observed between the degree of intramolecular interaction and vibrational mode coupling.

  18. High-resolution STIR for 3-T MRI of the posterior fossa: visualization of the lower cranial nerves and arteriovenous structures related to neurovascular compression.

    Science.gov (United States)

    Hiwatashi, Akio; Yoshiura, Takashi; Yamashita, Koji; Kamano, Hironori; Honda, Hiroshi

    2012-09-01

    Preoperative evaluation of small vessels without contrast material is sometimes difficult in patients with neurovascular compression disease. The purpose of this retrospective study was to evaluate whether 3D STIR MRI could simultaneously depict the lower cranial nerves--fifth through twelfth--and the blood vessels in the posterior fossa. The posterior fossae of 47 adults (26 women, 21 men) without gross pathologic changes were imaged with 3D STIR and turbo spin-echo heavily T2-weighted MRI sequences and with contrast-enhanced turbo field-echo MR angiography (MRA). Visualization of the cranial nerves on STIR images was graded on a 4-point scale and compared with visualization on T2-weighted images. Visualization of the arteries on STIR images was evaluated according to the segments in each artery and compared with that on MRA images. Visualization of the veins on STIR images was also compared with that on MRA images. Statistical analysis was performed with the Mann-Whitney U test. There were no significant differences between STIR and T2-weighted images with respect to visualization of the cranial nerves (p > 0.05). Identified on STIR and MRA images were 94 superior cerebellar arteries, 81 anteroinferior cerebellar arteries, and 79 posteroinferior cerebellar arteries. All veins evaluated were seen on STIR and MRA images. There were no significant differences between STIR and MRA images with respect to visualization of arteries and veins (p > 0.05). High-resolution STIR is a feasible method for simultaneous evaluation of the lower cranial nerves and the vessels in the posterior fossa without the use of contrast material.

  19. High resolution tomographic instrument development

    International Nuclear Information System (INIS)

    1992-01-01

    Our recent work has concentrated on the development of high-resolution PET instrumentation reflecting in part the growing importance of PET in nuclear medicine imaging. We have developed a number of positron imaging instruments and have the distinction that every instrument has been placed in operation and has had an extensive history of application for basic research and clinical study. The present program is a logical continuation of these earlier successes. PCR-I, a single ring positron tomograph was the first demonstration of analog coding using BGO. It employed 4 mm detectors and is currently being used for a wide range of biological studies. These are of immense importance in guiding the direction for future instruments. In particular, PCR-II, a volume sensitive positron tomograph with 3 mm spatial resolution has benefited greatly from the studies using PCR-I. PCR-II is currently in the final stages of assembly and testing and will shortly be placed in operation for imaging phantoms, animals and ultimately humans. Perhaps the most important finding resulting from our previous study is that resolution and sensitivity must be carefully balanced to achieve a practical high resolution system. PCR-II has been designed to have the detection characteristics required to achieve 3 mm resolution in human brain under practical imaging situations. The development of algorithms by the group headed by Dr. Chesler is based on a long history of prior study including his joint work with Drs. Pelc and Reiderer and Stearns. This body of expertise will be applied to the processing of data from PCR-II when it becomes operational

  20. High resolution tomographic instrument development

    Energy Technology Data Exchange (ETDEWEB)

    1992-08-01

    Our recent work has concentrated on the development of high-resolution PET instrumentation reflecting in part the growing importance of PET in nuclear medicine imaging. We have developed a number of positron imaging instruments and have the distinction that every instrument has been placed in operation and has had an extensive history of application for basic research and clinical study. The present program is a logical continuation of these earlier successes. PCR-I, a single ring positron tomograph was the first demonstration of analog coding using BGO. It employed 4 mm detectors and is currently being used for a wide range of biological studies. These are of immense importance in guiding the direction for future instruments. In particular, PCR-II, a volume sensitive positron tomograph with 3 mm spatial resolution has benefited greatly from the studies using PCR-I. PCR-II is currently in the final stages of assembly and testing and will shortly be placed in operation for imaging phantoms, animals and ultimately humans. Perhaps the most important finding resulting from our previous study is that resolution and sensitivity must be carefully balanced to achieve a practical high resolution system. PCR-II has been designed to have the detection characteristics required to achieve 3 mm resolution in human brain under practical imaging situations. The development of algorithms by the group headed by Dr. Chesler is based on a long history of prior study including his joint work with Drs. Pelc and Reiderer and Stearns. This body of expertise will be applied to the processing of data from PCR-II when it becomes operational.

  1. High resolution tomographic instrument development

    Energy Technology Data Exchange (ETDEWEB)

    1992-01-01

    Our recent work has concentrated on the development of high-resolution PET instrumentation reflecting in part the growing importance of PET in nuclear medicine imaging. We have developed a number of positron imaging instruments and have the distinction that every instrument has been placed in operation and has had an extensive history of application for basic research and clinical study. The present program is a logical continuation of these earlier successes. PCR-I, a single ring positron tomograph was the first demonstration of analog coding using BGO. It employed 4 mm detectors and is currently being used for a wide range of biological studies. These are of immense importance in guiding the direction for future instruments. In particular, PCR-II, a volume sensitive positron tomograph with 3 mm spatial resolution has benefited greatly from the studies using PCR-I. PCR-II is currently in the final stages of assembly and testing and will shortly be placed in operation for imaging phantoms, animals and ultimately humans. Perhaps the most important finding resulting from our previous study is that resolution and sensitivity must be carefully balanced to achieve a practical high resolution system. PCR-II has been designed to have the detection characteristics required to achieve 3 mm resolution in human brain under practical imaging situations. The development of algorithms by the group headed by Dr. Chesler is based on a long history of prior study including his joint work with Drs. Pelc and Reiderer and Stearns. This body of expertise will be applied to the processing of data from PCR-II when it becomes operational.

  2. Validation of an analytical method based on the high-resolution continuum source flame atomic absorption spectrometry for the fast-sequential determination of several hazardous/priority hazardous metals in soil.

    Science.gov (United States)

    Frentiu, Tiberiu; Ponta, Michaela; Hategan, Raluca

    2013-03-01

    The aim of this paper was the validation of a new analytical method based on the high-resolution continuum source flame atomic absorption spectrometry for the fast-sequential determination of several hazardous/priority hazardous metals (Ag, Cd, Co, Cr, Cu, Ni, Pb and Zn) in soil after microwave assisted digestion in aqua regia. Determinations were performed on the ContrAA 300 (Analytik Jena) air-acetylene flame spectrometer equipped with xenon short-arc lamp as a continuum radiation source for all elements, double monochromator consisting of a prism pre-monocromator and an echelle grating monochromator, and charge coupled device as detector. For validation a method-performance study was conducted involving the establishment of the analytical performance of the new method (limits of detection and quantification, precision and accuracy). Moreover, the Bland and Altman statistical method was used in analyzing the agreement between the proposed assay and inductively coupled plasma optical emission spectrometry as standardized method for the multielemental determination in soil. The limits of detection in soil sample (3σ criterion) in the high-resolution continuum source flame atomic absorption spectrometry method were (mg/kg): 0.18 (Ag), 0.14 (Cd), 0.36 (Co), 0.25 (Cr), 0.09 (Cu), 1.0 (Ni), 1.4 (Pb) and 0.18 (Zn), close to those in inductively coupled plasma optical emission spectrometry: 0.12 (Ag), 0.05 (Cd), 0.15 (Co), 1.4 (Cr), 0.15 (Cu), 2.5 (Ni), 2.5 (Pb) and 0.04 (Zn). Accuracy was checked by analyzing 4 certified reference materials and a good agreement for 95% confidence interval was found in both methods, with recoveries in the range of 94-106% in atomic absorption and 97-103% in optical emission. Repeatability found by analyzing real soil samples was in the range 1.6-5.2% in atomic absorption, similar with that of 1.9-6.1% in optical emission spectrometry. The Bland and Altman method showed no statistical significant difference between the two spectrometric

  3. Simultaneous determination of Cd and Fe in beans and soil of different regions of Brazil using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sampling.

    Science.gov (United States)

    dos Santos, Lisia M G; Welz, Bernhard; Araujo, Rennan G O; Jacob, Silvana do C; Vale, Maria Goreti R; Martens, Andreas; Gonzaga Martens, Irland B; Becker-Ross, Helmut

    2009-11-11

    A fast routine screening method for the simultaneous determination of cadmium and iron in bean and soil samples is proposed, using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sampling. The primary absorption line at 228.802 nm has been used for the determination of cadmium, and an adjacent secondary line, at 228.726 nm, for iron. Fourteen bean samples and 10 soil samples from nine states all over Brazil have been analyzed. The limits of detection (3 sigma, n = 10) were 2.0 microg kg(-1) for Cd and 4.5 mg kg(-1) for Fe. The relative standard deviation ranged from 4 to 7% for Cd and from 5 to 28% for Fe, which is usually acceptable for a screening method. The accuracy of the method has been confirmed by the analysis of two certified reference materials; the results were in agreement with the certified values at a 95% confidence interval.

  4. High resolution chronology of late Cretaceous-early Tertiary events determined from 21,000 yr orbital-climatic cycles in marine sediments

    Science.gov (United States)

    Herbert, Timothy D.; Dhondt, Steven

    1988-01-01

    A number of South Atlantic sites cored by the Deep Sea Drilling Project (DSDP) recovered late Cretaceous and early Tertiary sediments with alternating light-dark, high-low carbonate content. The sedimentary oscillations were turned into time series by digitizing color photographs of core segments at a resolution of about 5 points/cm. Spectral analysis of these records indicates prominent periodicity at 25 to 35 cm in the Cretaceous intervals, and about 15 cm in the early Tertiary sediments. The absolute period of the cycles that is determined from paleomagnetic calibration at two sites is 20,000 to 25,000 yr, and almost certainly corresponds to the period of the earth's precessional cycle. These sequences therefore contain an internal chronometer to measure events across the K/T extinction boundary at this scale of resolution. The orbital metronome was used to address several related questions: the position of the K/T boundary within magnetic chron 29R, the fluxes of biogenic and detrital material to the deep sea immediately before and after the K/T event, the duration of the Sr anomaly, and the level of background climatic variability in the latest Cretaceous time. The carbonate/color cycles that were analyzed contain primary records of ocean carbonate productivity and chemistry, as evidenced by bioturbational mixing of adjacent beds and the weak lithification of the rhythmic sequences. It was concluded that sedimentary sequences that contain orbital cyclicity are capable of providing resolution of dramatic events in earth history with much greater precision than obtainable through radiometric methods. The data show no evidence for a gradual climatic deterioration prior to the K/T extinction event, and argue for a geologically rapid revolution at this horizon.

  5. An off-line automated preconcentration system with ethylenediaminetriacetate chelating resin for the determination of trace metals in seawater by high-resolution inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Minami, Tomoharu; Konagaya, Wataru; Zheng, Linjie; Takano, Shotaro; Sasaki, Masanobu; Murata, Rena; Nakaguchi, Yuzuru; Sohrin, Yoshiki

    2015-01-07

    A novel automated off-line preconcentration system for trace metals (Al, Mn, Fe, Co, Ni, Cu, Zn, Cd, and Pb) in seawater was developed by improving a commercially available solid-phase extraction system SPE-100 (Hiranuma Sangyo). The utilized chelating resin was NOBIAS Chelate-PA1 (Hitachi High-Technologies) with ethylenediaminetriacetic acid and iminodiacetic acid functional groups. Parts of the 8-way valve made of alumina and zirconia in the original SPE-100 system were replaced with parts made of polychlorotrifluoroethylene in order to reduce contamination of trace metals. The eluent pass was altered for the back flush elution of trace metals. We optimized the cleaning procedures for the chelating resin column and flow lines of the preconcentration system, and developed a preconcentration procedure, which required less labor and led to a superior performance compared to manual preconcentration (Sohrin et al.). The nine trace metals were simultaneously and quantitatively preconcentrated from ∼120 g of seawater, eluted with ∼15 g of 1M HNO3, and determined by HR-ICP-MS using the calibration curve method. The single-step preconcentration removed more than 99.998% of Na, K, Mg, Ca, and Sr from seawater. The procedural blanks and detection limits were lower than the lowest concentrations in seawater for Mn, Ni, Cu, and Pb, while they were as low as the lowest concentrations in seawater for Al, Fe, Co, Zn, and Cd. The accuracy and precision of this method were confirmed by the analysis of reference seawater samples (CASS-5, NASS-5, GEOTRACES GS, and GD) and seawater samples for vertical distribution in the western North Pacific Ocean. Copyright © 2014 Elsevier B.V. All rights reserved.

  6. Laboratory of High resolution gamma spectrometry

    International Nuclear Information System (INIS)

    Mendez G, A.; Giber F, J.; Rivas C, I.; Reyes A, B.

    1992-01-01

    The Department of Nuclear Experimentation of the Nuclear Systems Management requests the collaboration of the Engineering unit for the supervision of the execution of the work of the High resolution Gamma spectrometry and low bottom laboratory, using the hut of the sub critic reactor of the Nuclear Center of Mexico. This laboratory has the purpose of determining the activity of special materials irradiated in nuclear power plants. In this report the architecture development, concepts, materials and diagrams for the realization of this type of work are presented. (Author)

  7. High resolution neutron spectroscopy for helium isotopes

    International Nuclear Information System (INIS)

    Abdel-Wahab, M.S.; Klages, H.O.; Schmalz, G.; Haesner, B.H.; Kecskemeti, J.; Schwarz, P.; Wilczynski, J.

    1992-01-01

    A high resolution fast neutron time-of-flight spectrometer is described, neutron time-of-flight spectra are taken using a specially designed TDC in connection to an on-line computer. The high time-of-flight resolution of 5 ps/m enabled the study of the total cross section of 4 He for neutrons near the 3/2 + resonance in the 5 He nucleus. The resonance parameters were determined by a single level Breit-Winger fit to the data. (orig.)

  8. OBSERVING THE FINE STRUCTURE OF LOOPS THROUGH HIGH-RESOLUTION SPECTROSCOPIC OBSERVATIONS OF CORONAL RAIN WITH THE CRISP INSTRUMENT AT THE SWEDISH SOLAR TELESCOPE

    International Nuclear Information System (INIS)

    Antolin, P.; Rouppe van der Voort, L.

    2012-01-01

    Observed in cool chromospheric lines, such as Hα or Ca II H, coronal rain corresponds to cool and dense plasma falling from coronal heights. Considered as a peculiar sporadic phenomenon of active regions, it has not received much attention since its discovery more than 40 years ago. Yet, it has been shown recently that a close relationship exists between this phenomenon and the coronal heating mechanism. Indeed, numerical simulations have shown that this phenomenon is most likely due to a loss of thermal equilibrium ensuing from a heating mechanism acting mostly toward the footpoints of loops. We present here one of the first high-resolution spectroscopic observations of coronal rain, performed with the CRisp Imaging Spectro Polarimeter (CRISP) instrument at the Swedish Solar Telescope. This work constitutes the first attempt to assess the importance of coronal rain in the understanding of the coronal magnetic field in active regions. With the present resolution, coronal rain is observed to literally invade the entire field of view. A large statistical set is obtained in which dynamics (total velocities and accelerations), shapes (lengths and widths), trajectories (angles of fall of the blobs), and thermodynamic properties (temperatures) of the condensations are derived. Specifically, we find that coronal rain is composed of small and dense chromospheric cores with average widths and lengths of ∼310 km and ∼710 km, respectively, average temperatures below 7000 K, displaying a broad distribution of falling speeds with an average of ∼70 km s –1 , and accelerations largely below the effective gravity along loops. Through estimates of the ion-neutral coupling in the blobs we show that coronal rain acts as a tracer of the coronal magnetic field, thus supporting the multi-strand loop scenario, and acts as a probe of the local thermodynamic conditions in loops. We further elucidate its potential in coronal heating. We find that the cooling in neighboring strands

  9. Disclosure of domain structure in cubic CaxZr1-xO2-x, 0x15 ≤ x ≤ 0x20, by Talbot image enhancement of high-resolution electron micrographs

    International Nuclear Information System (INIS)

    Rossell, H.J.; Wilson, I.J.; Sellar, J.R.

    1991-01-01

    High-resolution electron microscope images have been recorded of several cystalline samples of calcia-stabilized zirconia (Ca-CSZ) and of the fluorite-related superstructure phase φ 1 (CaZr 4 O 9 ). The contrast of the CSZ images has been enhanced markedly by the light-optical Talbot self-imaging technique. Is is demonstrated that the CSZ crystals contain a coherent dispersion of microdomains approximately 30 A in diameter, and that the structure of the microdomains is that of φ 1 . (orig.)

  10. High-Resolution Solid-State NMR Spectroscopy: Characterization of Polymorphism in Cimetidine, a Pharmaceutical Compound

    Science.gov (United States)

    Pacilio, Julia E.; Tokarski, John T.; Quiñones, Rosalynn; Iuliucci, Robbie J.

    2014-01-01

    High-resolution solid-state NMR (SSNMR) spectroscopy has many advantages as a tool to characterize solid-phase material that finds applications in polymer chemistry, nanotechnology, materials science, biomolecular structure determination, and others, including the pharmaceutical industry. The technology associated with achieving high resolution…

  11. Determinants of capital structure.

    Science.gov (United States)

    McCue, M J; Ozcan, Y A

    1992-01-01

    This study analyzes the determinants of hospital capital structure in a new market setting that are created by the financial pressures of prospective payment and the intense price competition among hospitals. Using California data, the study found hospital system affiliation, bed size, growth rate in revenues, operating risk, and asset structure affected both short- and long-term debt borrowings. In addition, percentage of uncompensated care, profitability, and payer mix influenced short-term borrowings while market conditions and ownership affected long-term borrowings. Most significant of all is the finding that smaller hospitals tend to borrow more, possibly because they cannot generate funds internally.

  12. High-resolution Al L2,3-edge x-ray absorption near edge structure spectra of Al-containing crystals and glasses: coordination number and bonding information from edge components

    International Nuclear Information System (INIS)

    Weigel, C; Calas, G; Cormier, L; Galoisy, L; Henderson, G S

    2008-01-01

    High-resolution Al L 2,3 -edge x-ray absorption near edge structure (XANES) spectra have been measured in selected materials containing aluminium in 4-, 5- and 6-coordination. A shift of 1.5 eV is observed between the onset of [4] Al and [6] Al L 2,3 -edge XANES, in agreement with the magnitude of the shift observed at the Al K-edge. The differences in the position and shape of low-energy components of Al L 2,3 -edge XANES spectra provide a unique fingerprint of the geometry of the Al site and of the nature of Al-O chemical bond. The high resolution allows the calculation of electronic parameters such as the spin-orbit coupling and exchange energy using intermediate coupling theory. The electron-hole exchange energy decreases in tetrahedral as compared to octahedral symmetry, in relation with the increased screening of the core hole in the former. Al L 2,3 -edge XANES spectra confirm a major structural difference between glassy and crystalline NaAlSi 2 O 6 , with Al in 4- and 6-coordination, respectively, Al coordination remaining unchanged in NaAl 1-x Fe x Si 2 O 6 glasses, as Fe is substituted for Al

  13. Raman Spectroscopy Adds Complementary Detail to the High-Resolution X-Ray Crystal Structure of Photosynthetic PsbP from Spinacia oleracea

    Czech Academy of Sciences Publication Activity Database

    Kopecký, V. Jr.; Kohoutová, Jaroslava; Lapkouski, Mikalai; Hofbauerová, Kateřina; Sovová, Žofie; Ettrichová, Olga; Gonzalez-Perez, S.; Dulebo, A.; Kaftan, D.; Kutá-Smatanová, Ivana; Reveuelta, J. L.; Arellano, J. B.; Carey, J.; Ettrich, Rüdiger

    2012-01-01

    Roč. 7, č. 10 (2012), s. 46694-46694 E-ISSN 1932-6203 Institutional research plan: CEZ:AV0Z60870520; CEZ:AV0Z50200510 Keywords : secondary-structure-analysis * oxygen-evolving complexO * plant photosystem-II * moleculars-dynamics * assisted crystallography * angstrom resolution * protein-structure * amide-I * conformation * biomolecules Subject RIV: BO - Biophysics; EE - Microbiology, Virology (MBU-M) Impact factor: 3.730, year: 2012

  14. Principles of high resolution NMR in solids

    CERN Document Server

    Mehring, Michael

    1983-01-01

    The field of Nuclear Magnetic Resonance (NMR) has developed at a fascinating pace during the last decade. It always has been an extremely valuable tool to the organic chemist by supplying molecular "finger print" spectra at the atomic level. Unfortunately the high resolution achievable in liquid solutions could not be obtained in solids and physicists and physical chemists had to live with unresolved lines open to a wealth of curve fitting procedures and a vast amount of speculations. High resolution NMR in solids seemed to be a paradoxon. Broad structure­ less lines are usually encountered when dealing with NMR in solids. Only with the recent advent of mUltiple pulse, magic angle, cross-polarization, two-dimen­ sional and multiple-quantum spectroscopy and other techniques during the last decade it became possible to resolve finer details of nuclear spin interactions in solids. I have felt that graduate students, researchers and others beginning to get involved with these techniques needed a book which trea...

  15. Determination of the detection limit and decision threshold for ionizing radiation measurements. Part 3: Fundamentals and application to counting measurements by high resolution gamma spectrometry, without the influence of sample treatment

    International Nuclear Information System (INIS)

    2000-01-01

    This part of ISO 11929 addresses the field of ionizing radiation measurements in which events (in particular pulses) are counted by high resolution gamma spectrometry registrating a pulse-heights distribution (acquisition of a multichannel spectrum), for example on samples. It considers exclusively the random character of radioactive decay and of pulse counting and ignores all other influences (e.g. arising from sample treatment, weighing, enrichment or the instability of the test setup). It assumes that the distance of neighbouring peaks of gamma lines is not smaller than four times the full width half maximum (FWHM) of gamma line and that the background near to gamma line is nearly a straight line. Otherwise ISO 11929-1 or ISO 11929-2 should be used. ISO 11929 consists of the following parts, under the general title Determination of the detection limit and decision threshold for ionizing radiation measurements: Part 1: Fundamentals and application to counting measurements without the influence of sample treatment; Part 2: Fundamentals and application to counting measurements with the influence of sample treatment; Part 3: Fundamentals and application to counting measurements by high resolution gamma spectrometry, without the influence of sample treatment; Part 4: Fundamentals and application to measurements by use of linear scale analogue ratemeters, without the influence of sample treatment. This part of ISO 11929 was prepared in parallel with other International Standards prepared by WG2 (now WG 17): ISO 11932:1996, Activity measurements of solid materials considered for recycling, re-use or disposal as nonradioactive waste, and ISO 11929-1, ISO 11929-2 and ISO 11929-4, and is, consequently, complementary to these documents

  16. Development of a high-resolution soft x-ray (30--1500 eV) beamline at the Advanced Light Source and its use for the study of angle-resolved photoemission extended fine structure

    International Nuclear Information System (INIS)

    Huff, W.R.A.

    1996-02-01

    ALS Bending magnet beamline 9.3.2 is for high resolution spectroscopy, with circularly polarized light. Fixed included-angle SGM uses three gratings for 30--1500 eV photons; circular polarization is produced by an aperture for selecting the beam above or below the horizontal plane. Photocurrent from upper and lower jaws of entrance slit sets a piezoelectric drive feedback loop on the vertically deflecting mirror for stable beam. End station has a movable platform. With photomeission data from Stanford, structure of c(2x2)P/Fe(100) was determined using angle-resolved photoemission extended fine structure (ARPEFS). Multiple-scattering spherical-wave (MSSW) calculations indicate that P atoms adsorb in fourfold hollow sites 1.02A above the first Fe layer. Self-consistent-field Xα scattered wave calculation confirm that the Fe 1 -Fe 2 space is contracted for S/Fe but not for P/Fe; comparison is made to atomic N and O on Fe(100). Final-state effects on ARPEFS curves used literature data from the S 1s and 2p core levels of c(2x2)S/Ni(001); a generalized Ramsauer-Townsend splitting is present in the 1s but not 2p data. An approximate method for analyzing ARPEFS data from a non-s initial state using only the higher-ell partial wave was tested successfully. ARPEFS data from clean surfaces were collected normal to Ni(111) (3p core levels) and 5 degree off-normal from Cu(111)(3s, 3p). Fourier transforms (FT) resemble adsorbate systems, showing backscattering signals from atoms up to 4 layers below emitters. 3p FTs show scattering from 6 nearest neighbors in the same crystal layer as the emitters. MSSW calulation indicate that Cu 3p photoemission is mostly d-wave. FTs also indicate double-scattering and single-scattering from laterally distant atoms; calculations indicate that the signal is dominated by photoemission from the first 2 crystal layers

  17. High-resolution X-ray television and high-resolution video recorders

    International Nuclear Information System (INIS)

    Haendle, J.; Horbaschek, H.; Alexandrescu, M.

    1977-01-01

    The improved transmission properties of the high-resolution X-ray television chain described here make it possible to transmit more information per television image. The resolution in the fluoroscopic image, which is visually determined, depends on the dose rate and the inertia of the television pick-up tube. This connection is discussed. In the last few years, video recorders have been increasingly used in X-ray diagnostics. The video recorder is a further quality-limiting element in X-ray television. The development of function patterns of high-resolution magnetic video recorders shows that this quality drop may be largely overcome. The influence of electrical band width and number of lines on the resolution in the X-ray television image stored is explained in more detail. (orig.) [de

  18. Spatial attributes of the four-helix bundle group of bacteriocins – The high-resolution structure of BacSp222 in solution

    KAUST Repository

    Nowakowski, Michał; Jaremko, Łukasz; Wladyka, Benedykt; Dubin, Grzegorz; Ejchart, Andrzej; Mak, Paweł

    2017-01-01

    collected. The structure was calculated based on NMR-derived constraints and consists of a rigid and tightly packed globular bundle of four alpha-helices separated by three short turns.Although the amino acid sequence of BacSp222 has no significant

  19. Structure analysis of OmpC, one of the major proteins in the outer membrane of E. coli, by high resolution electron microscopy

    International Nuclear Information System (INIS)

    Chang, C.F.

    1983-07-01

    This dissertation is concerned with the structure analysis of a pore-forming membrane protein, OmpC, which is one of the major proteins in the outer membrane of Escherichia coli. In order to obtain structural information it was necessary to develop a suitable technique for preparing two-dimensional crystalline arrays of this membrane protein in an unfixed, unstained and hydrated condition. Electron micrographs were recorded at exposures of less than 5 electrons/A 2 in order to avoid severe radiation damage. The resulting images were crystallographically averaged, in order to overcome the statistical limitations associated with the low electron exposures. The resulting images, which extend to a resolution of approx. 13.5 A, lend themselves to a natural interpretation that is consistent with the mass density of protein, water and lipid, prior data from 2-D and 3-D structure studies of negatively stained specimens at approx. = 20 A resolution, and published spectroscopic data on the peptide chain secondary structure

  20. Chemical structure changes in coals after low-temperature oxidation and demineralization by acid treatment as revealed by high resolution solid state 13C NMR

    International Nuclear Information System (INIS)

    Tekely, P.; Nicole, D.; Delpuech, J.-J.; Totino, E.; Muller, J.F.

    1987-01-01

    13 C CP/MAS NMR has been used for characterization of chemical structure changes in coals after low-temperature oxidation and prolonged demineralization by acid treatment. In both cases the changes take place mainly in the aliphatic part of coal molecules. 21 refs.; 3 figs.; 2 tabs

  1. Structural changes of Bi1.8Sr2(Ca1-xYx)Cu2.2Oz ceramics with yttrium content studied by electron diffraction and high-resolution electron microscopy

    Science.gov (United States)

    Onozuka, Takashi; Iwabuchi, Yoshihiro; Fukase, Tetsuo; Sato, Hiroshi; Mitchell, Terence E.

    1991-06-01

    The mode of the incommensurate modulation in the b direction of the Bi1.8Sr2(Ca1-xYx)Cu2.2Oz (0.05high-resolution lattice imaging. The change of period of the long-period structure with x is found to be basically due to the mixing ratio of domains of two modulation periods with b=4.5b0 and 5b0 or 4.5b0 and 4b0, thus creating periods of b=4.75b0-4.0b0. The fundamental orthorhombic lattice has dimensions of a~=b~=b0 (0.54 nm) and c~=c0 (3.1 nm). The change of the mixing mode from one to the other mentioned above occurs just in the yttrium concentration range, 0.45high-resolution lattice images. These images are reproduced well by a multislice computer-simulation technique.

  2. Structural characterization and gas reactions of small metal particles by high resolution in-situ TEM (Transmission Electron Microscopy) and TED (Transmission Electron Diffraction)

    Science.gov (United States)

    Heinemann, K.

    1987-01-01

    The detection and size analysis of small metal particles supported on amorphous substrates becomes increasingly difficult when the particle size approaches that of the phase contrast background structures of the support. An approach of digital image analysis, involving Fourier transformation of the original image, filtering, and image reconstruction was studied with respect to the likelihood of unambiguously detecting particles of less than 1 nm diameter on amorphous substrates from a single electron micrograph.

  3. Online coupling of high-resolution chromatography with extreme UV photon activation tandem mass spectrometry: Application to the structural investigation of complex glycans by dissociative photoionization

    International Nuclear Information System (INIS)

    Ropartz, David; Giuliani, Alexandre; Fanuel, Mathieu; Hervé, Cécile; Czjzek, Mirjam; Rogniaux, Hélène

    2016-01-01

    The activation of ions by extreme-energy photons (XUV) produced by a synchrotron radiation beamline is a powerful method for characterizing complex glycans using tandem mass spectrometry (MS). As previously described, this activation method leads to rich fragmentation spectra with many structurally valuable cross-ring cleavages while maintaining labile modifications on the glycan structures. However, until now, the tandem MS event was too long to be compatible with liquid chromatography elution times. In this work, the duty cycle of the activation and detection of fragments was shortened, and the background signal on the spectra was drastically reduced. Both improvements allowed, for the first time, the successful coupling of a UHPLC system to XUV-activated tandem MS. The approach was used to characterize a complex mixture of oligo-porphyrans, which are a class of highly sulfated oligosaccharides, in a fully automated way. Due to an enhanced dynamic range and an increased sensitivity, some hypothetical structures of low abundance have been unequivocally confirmed in this study and others have been revised. Some previously undescribed species of oligo-porphyrans that exhibit lateral branching have been fully resolved. This work contributes to the scarce knowledge of the structure of porphyrans in red algae and pushes the current capacities of XUV-activation tandem MS by demonstrating the possibility of a direct coupling with UHPLC. This study will considerably broaden the applicability and practicality of this method in many fields of analytical biology. - Highlights: • For the first time, XUV photon activation tandem MS was coupled to UHPLC. • The approach was used to characterize a complex mixture of biomolecules. • The MSMS duty cycle was compatible with elution times of UHPLC without compromised. • Minor species were characterized with an enhanced sensitivity and dynamic range. • These results broaden the application of the technique in many field of

  4. High resolution positron q-value measurements and nuclear structure studies far from the stability line. Progress report, 1983-1984

    International Nuclear Information System (INIS)

    Avignone, F.T. III.

    1984-01-01

    Results of studies of the beta-delayed proton spectra of 147 Dy and 149 Er are presented, and a preliminary report on measuring the masses of 77 Kr and 75 Kr is given. Studies on the beta decay of 76 Rb and the level structure of 76 Kr and a search for axions from the 1.1155 MeV transition of 65 Cu are briefly described

  5. High-resolution crystal structures of the photoreceptor glyceraldehyde 3-phosphate dehydrogenase (GAPDH) with three and four-bound NAD molecules

    Science.gov (United States)

    Baker, Bo Y; Shi, Wuxian; Wang, Benlian; Palczewski, Krzysztof

    2014-01-01

    Glyceraldehyde-3-phosphate dehydrogenase (GAPDH) catalyzes the oxidative phosphorylation of d-glyceraldehyde 3-phosphate (G3P) into 1,3-diphosphoglycerate (BGP) in the presence of the NAD cofactor. GAPDH is an important drug target because of its central role in glycolysis, and nonglycolytic processes such as nuclear RNA transport, DNA replication/repair, membrane fusion and cellular apoptosis. Recent studies found that GAPDH participates in the development of diabetic retinopathy and its progression after the cessation of hyperglycemia. Here, we report two structures for native bovine photoreceptor GAPDH as a homotetramer with differing occupancy by NAD, bGAPDH(NAD)4, and bGAPDH(NAD)3. The bGAPDH(NAD)4 was solved at 1.52 Å, the highest resolution for GAPDH. Structural comparison of the bGAPDH(NAD)4 and bGAPDH(NAD)3 models revealed novel details of conformational changes induced by cofactor binding, including a loop region (residues 54–56). Structure analysis of bGAPDH confirmed the importance of Phe34 in NAD binding, and demonstrated that Phe34 was stabilized in the presence of NAD but displayed greater mobility in its absence. The oxidative state of the active site Cys149 residue is regulated by NAD binding, because this residue was found oxidized in the absence of dinucleotide. The distance between Cys149 and His176 decreased upon NAD binding and Cys149 remained in a reduced state when NAD was bound. These findings provide an important structural step for understanding the mechanism of GAPDH activity in vision and its pathological role in retinopathies. PMID:25176140

  6. Online coupling of high-resolution chromatography with extreme UV photon activation tandem mass spectrometry: Application to the structural investigation of complex glycans by dissociative photoionization

    Energy Technology Data Exchange (ETDEWEB)

    Ropartz, David, E-mail: David.Ropartz@nantes.inra.fr [INRA, UR1268 Biopolymers Interactions Assemblies F-44316 Nantes (France); Giuliani, Alexandre [Synchrotron SOLEIL, L' Orme des Merisiers, F-91190 Gif-sur-Yvette (France); UAR 1008 CEPIA, INRA, F-44316 Nantes (France); Fanuel, Mathieu [INRA, UR1268 Biopolymers Interactions Assemblies F-44316 Nantes (France); Hervé, Cécile; Czjzek, Mirjam [Sorbonne Universités, Université Pierre et Marie Curie, Paris VI, CNRS, Integrative Biology of Marine Models, UMR 8227, Station Biologique, Place George Teissier, F29688 Roscoff Cedex (France); Rogniaux, Hélène [INRA, UR1268 Biopolymers Interactions Assemblies F-44316 Nantes (France)

    2016-08-24

    The activation of ions by extreme-energy photons (XUV) produced by a synchrotron radiation beamline is a powerful method for characterizing complex glycans using tandem mass spectrometry (MS). As previously described, this activation method leads to rich fragmentation spectra with many structurally valuable cross-ring cleavages while maintaining labile modifications on the glycan structures. However, until now, the tandem MS event was too long to be compatible with liquid chromatography elution times. In this work, the duty cycle of the activation and detection of fragments was shortened, and the background signal on the spectra was drastically reduced. Both improvements allowed, for the first time, the successful coupling of a UHPLC system to XUV-activated tandem MS. The approach was used to characterize a complex mixture of oligo-porphyrans, which are a class of highly sulfated oligosaccharides, in a fully automated way. Due to an enhanced dynamic range and an increased sensitivity, some hypothetical structures of low abundance have been unequivocally confirmed in this study and others have been revised. Some previously undescribed species of oligo-porphyrans that exhibit lateral branching have been fully resolved. This work contributes to the scarce knowledge of the structure of porphyrans in red algae and pushes the current capacities of XUV-activation tandem MS by demonstrating the possibility of a direct coupling with UHPLC. This study will considerably broaden the applicability and practicality of this method in many fields of analytical biology. - Highlights: • For the first time, XUV photon activation tandem MS was coupled to UHPLC. • The approach was used to characterize a complex mixture of biomolecules. • The MSMS duty cycle was compatible with elution times of UHPLC without compromised. • Minor species were characterized with an enhanced sensitivity and dynamic range. • These results broaden the application of the technique in many field of

  7. Structure and microstructure of Ni-Mn-Ga single crystal exhibiting magnetic shape memory effect analysed by high resolution X-ray diffraction

    Czech Academy of Sciences Publication Activity Database

    Heczko, Oleg; Cejpek, P.; Drahokoupil, Jan; Holý, V.

    2016-01-01

    Roč. 115, Aug (2016), s. 250-258 ISSN 1359-6454 R&D Projects: GA ČR GA13-30397S; GA ČR GA15-00262S Institutional support: RVO:68378271 Keywords : magnetic field-induced strain * magnetic shape memory effect * X-ray diffraction * structure of Ni-Mn-Ga Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 5.301, year: 2016

  8. High-Resolution Imaging of Dense Gas Structure and Kinematics in Nearby Molecular Clouds with the CARMA Large Area Star Formation Survey

    Science.gov (United States)

    Storm, Shaye

    This thesis utilizes new observations of dense gas in molecular clouds to develop an empirical framework for how clouds form structures which evolve into young cores and stars. Previous observations show the general turbulent and hierarchical nature of clouds. However, current understanding of the star formation pathway is limited by existing data that do not combine angular resolution needed to resolve individual cores with area coverage required to capture entire star-forming regions and with tracers that can resolve gas motions. The original contributions of this thesis to astrophysical research are the creation and analysis of the largest-area high-angular-resolution maps of dense gas in molecular clouds to-date, and the development of a non-binary dendrogram algorithm to quantify the hierarchical nature and three-dimensional morphology of cloud structure. I first describe the CARMA Large Area Star Formation Survey, which provides spectrally imaged N2H+, HCO+, and HCN (J = 1→0) emission across diverse regions of the Perseus and Serpens Molecular Clouds. I then present a detailed analysis of the Barnard 1 and L1451 regions in Perseus. A non-binary dendrogram analysis of Barnard 1 N2H emission and all L1451 emission shows that the most hierarchically complex gas corresponds with sub-regions actively forming young stars. I estimate the typical depth of molecular emission in each region using the spatial and kinematic properties of dendrogram-identified structures. Barnard 1 appears to be a sheet-like region at the largest scales with filamentary substructure, while the L1451 region is composed of more spatially distinct ellipsoidal structures. I then do a uniform comparison of the hierarchical structure and young stellar content of all five regions. The more evolved regions with the most young stellar objects (YSOs) and strongest emission have formed the most hierarchical levels. However, all regions show similar mean branching properties at each level

  9. Enhancement of catalytic activity of enzymes by heating in anhydrous organic solvents: 3D structure of a modified serine proteinase at high resolution.

    Science.gov (United States)

    Sharma, S; Tyagi, R; Gupta, M N; Singh, T P

    2001-01-01

    For the first time, it is demonstrated that exposure of an enzyme to anhydrous organic solvents at optimized high temperature enhances its catalytic power through local changes at the binding region. Six enzymes, namely, proteinase K, wheat germ acid phosphatase, alpha-amylase, beta-glucosidase, chymotrypsin and trypsin were exposed to acetonitrile at 70 degrees C for three hr. The activities of these enzymes were found to be considerably enhanced. In order to understand the basis of this change in the activity of these enzymes, proteinase K was analyzed in detail using X-ray diffraction method. The overall structure of the enzyme was found to be similar to the native structure in aqueous environment. The hydrogen bonding system of the catalytic triad remained intact after the treatment. However, the water structure in the substrate binding site underwent some rearrangement as some of the water molecules were either displaced or completely absent. The most striking observation concerning the water structure was the complete deletion of the water molecule which occupied the position at the so-called oxyanion hole in the active site of the native enzyme. Three acetonitrile molecules were found in the present structure. All the acetonitrile molecules were located in the recognition site. Interlinked through water molecules, the sites occupied by acetonitrile molecules were independent of water molecules. The acetonitrile molecules are involved in extensive interactions with the protein atoms. The methyl group of one of the acetonitrile molecules (CCN1) interacts simultaneously with the hydrophobic side chains of Leu 96, Ile 107 and Leu 133. The development of such a hydrophobic environment at the recognition site introduced a striking conformation change in Ile 107 by rotating its side chain about C alpha-C beta bond by 180 degrees to bring about the delta-methyl group within the range of attractive van der Waals interactions with the methyl group of CCN1. A similar

  10. High-resolution imaging of solar system objects

    International Nuclear Information System (INIS)

    Goldberg, B.A.

    1988-01-01

    The strategy of this investigation has been to develop new high-resolution imaging capabilities and to apply them to extended observing programs. These programs have included Io's neutral sodium cloud and comets. The Io observing program was carried out at Table Mountain Observatory (1976 to 1981), providing a framework interpreting Voyager measurements of the Io torus, and serving as an important reference for studying asymmetries and time variabilities in the Jovian magnetosphere. Comet observations made with the 3.6 m Canada-France-Hawaii Telescope and 1.6 m AMOS telescope (1984 to 1987) provide basis for studying early coma development in Halley, the kinematics of its nucleus, and the internal and external structure of the nucleus. Images of GZ from the ICE encounter period form the basis for unique comparisons with in situ magnetic field and dust impact measurements to determine the ion tail and dust coma structure, respectively

  11. Exploring the structure of fucosylated chondroitin sulfate through bottom-up nuclear magnetic resonance and electrospray ionization-high-resolution mass spectrometry approaches.

    Science.gov (United States)

    Santos, Gustavo Rc; Porto, Ana Co; Soares, Paulo Ag; Vilanova, Eduardo; Mourão, Paulo As

    2017-07-01

    Fucosylated chondroitin sulfate (FCS) from sea cucumbers is composed of a chondroitin sulfate (CS) central core and branches of sulfated fucose. The structure of this complex glycosaminoglycan is usually investigated via nuclear magnetic resonance (NMR) analyses of the intact molecule, ergo through a top-down approach, which often yield spectra with intricate sets of signals. Here we employed a bottom-up approach to analyze the FCSs from the sea cucumbers Isostichopus badionotus and Ludwigothurea grisea from their basic constituents, viz. CS cores and sulfated fucose branches, obtained via systematic fragmentation through mild acid hydrolysis. Oligosaccharides derived from the central CS core were analyzed via NMR spectroscopy and the disaccharides produced using chondroitin sulfate lyase via SAX-HPLC. The CS cores from the two species were similar, showing only slight differences in the proportions of 4- or 6-monosulfated and 4,6-disulfated β-d-GalNAc. Sulfated fucose units released from the FCSs were analyzed via NMR and ESI-HRMS spectroscopies. The fucose units from each species presented extensive qualitative differences, but quantitative assessments of these units were hindered, mostly because of their extensive desulfation during the hydrolysis. The bottom-up analysis performed here has proved useful to explore the structure of FCS through a sum-of-the-parts approach in a qualitative manner. We further demonstrate that under specific acidification conditions particular fucose branches can be removed preferentially from FCS. Preparation of derivatives enriched with particular fucose branches could be useful for studies on "structure vs. biological function" of FCS. © The Author 2017. Published by Oxford University Press. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

  12. Information Extraction of High Resolution Remote Sensing Images Based on the Calculation of Optimal Segmentation Parameters

    Science.gov (United States)

    Zhu, Hongchun; Cai, Lijie; Liu, Haiying; Huang, Wei

    2016-01-01

    Multi-scale image segmentation and the selection of optimal segmentation parameters are the key processes in the object-oriented information extraction of high-resolution remote sensing images. The accuracy of remote sensing special subject information depends on this extraction. On the basis of WorldView-2 high-resolution data, the optimal segmentation parameters methodof object-oriented image segmentation and high-resolution image information extraction, the following processes were conducted in this study. Firstly, the best combination of the bands and weights was determined for the information extraction of high-resolution remote sensing image. An improved weighted mean-variance method was proposed andused to calculatethe optimal segmentation scale. Thereafter, the best shape factor parameter and compact factor parameters were computed with the use of the control variables and the combination of the heterogeneity and homogeneity indexes. Different types of image segmentation parameters were obtained according to the surface features. The high-resolution remote sensing images were multi-scale segmented with the optimal segmentation parameters. Ahierarchical network structure was established by setting the information extraction rules to achieve object-oriented information extraction. This study presents an effective and practical method that can explain expert input judgment by reproducible quantitative measurements. Furthermore the results of this procedure may be incorporated into a classification scheme. PMID:27362762

  13. Determination of polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans, and dioxin-like polychlorinated biphenyls in human serum using programmable-temperature vaporization gas chromatography with high-resolution mass spectrometry.

    Science.gov (United States)

    Zhang, Lei; Zhong, Yuxin; Liu, Xin; Bao, Yan; Zhao, Yunfeng; Wu, Yongning; Cai, Zongwei; Li, Jingguang

    2017-09-01

    The determination of polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans, and dioxin-like polychlorinated biphenyls in blood from a non-occupational population is essential for the investigation of adverse health effects from these pollutants. In this study, a sensitive method based on programmable-temperature vaporization with large-volume injection coupled with gas chromatography with high-resolution mass spectrometry was developed to determine these pollutants in 1-2 mL of human serum samples. Various key parameters of programmable-temperature vaporization injector, including vent temperature, vent time, vent flow, transfer temperature and transfer time were optimized by factorial design. The accuracy and precision as well as applicability were assessed by determining polychlorinated dibenzo-p-dioxins, polychlorinated dibenzofurans, and dioxin-like polychlorinated biphenyls in calibration standard solutions, standard reference materials and real human serum samples from non-occupational population. The method detection limits of polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans, and dioxin-like polychlorinated biphenyls were 1.5-9.0 and 0.005-0.02 ng/kg wet weight, respectively. By comparing with typically splitless injection, the application of programmable-temperature vaporization injector could effectively lead to higher detectable rate of polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans, and dioxin-like polychlorinated biphenyls in 1-2 mL of human serum samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. High resolution integral holography using Fourier ptychographic approach.

    Science.gov (United States)

    Li, Zhaohui; Zhang, Jianqi; Wang, Xiaorui; Liu, Delian

    2014-12-29

    An innovative approach is proposed for calculating high resolution computer generated integral holograms by using the Fourier Ptychographic (FP) algorithm. The approach initializes a high resolution complex hologram with a random guess, and then stitches together low resolution multi-view images, synthesized from the elemental images captured by integral imaging (II), to recover the high resolution hologram through an iterative retrieval with FP constrains. This paper begins with an analysis of the principle of hologram synthesis from multi-projections, followed by an accurate determination of the constrains required in the Fourier ptychographic integral-holography (FPIH). Next, the procedure of the approach is described in detail. Finally, optical reconstructions are performed and the results are demonstrated. Theoretical analysis and experiments show that our proposed approach can reconstruct 3D scenes with high resolution.

  15. High-resolution structural and functional assessments of cerebral microvasculature using 3D Gas ΔR2*-mMRA.

    Science.gov (United States)

    Huang, Chien-Hsiang; Chen, Chiao-Chi V; Siow, Tiing-Yee; Hsu, Sheng-Hsiou S; Hsu, Yi-Hua; Jaw, Fu-Shan; Chang, Chen

    2013-01-01

    The ability to evaluate the cerebral microvascular structure and function is crucial for investigating pathological processes in brain disorders. Previous angiographic methods based on blood oxygen level-dependent (BOLD) contrast offer appropriate visualization of the cerebral vasculature, but these methods remain to be optimized in order to extract more comprehensive information. This study aimed to integrate the advantages of BOLD MRI in both structural and functional vascular assessments. The BOLD contrast was manipulated by a carbogen challenge, and signal changes in gradient-echo images were computed to generate ΔR2* maps. Simultaneously, a functional index representing the regional cerebral blood volume was derived by normalizing the ΔR2* values of a given region to those of vein-filled voxels of the sinus. This method is named 3D gas ΔR2*-mMRA (microscopic MRA). The advantages of using 3D gas ΔR2*-mMRA to observe the microvasculature include the ability to distinguish air-tissue interfaces, a high vessel-to-tissue contrast, and not being affected by damage to the blood-brain barrier. A stroke model was used to demonstrate the ability of 3D gas ΔR2*-mMRA to provide information about poststroke revascularization at 3 days after reperfusion. However, this technique has some limitations that cannot be overcome and hence should be considered when it is applied, such as magnifying vessel sizes and predominantly revealing venous vessels.

  16. Investigation into the Formation, Structure, and Evolution of an EF4 Tornado in East China Using a High-Resolution Numerical Simulation

    Science.gov (United States)

    Yao, Dan; Xue, Haile; Yin, Jinfang; Sun, Jisong; Liang, Xudong; Guo, Jianping

    2018-04-01

    Devastating tornadoes in China have received growing attention in recent years, but little is known about their formation, structure, and evolution on the tornadic scale. Most of these tornadoes develop within the East Asian monsoon regime, in an environment quite different from tornadoes in the U.S. In this study, we used an idealized, highresolution (25-m grid spacing) numerical simulation to investigate the deadly EF4 (Enhanced Fujita scale category 4) tornado that occurred on 23 June 2016 and claimed 99 lives in Yancheng, Jiangsu Province. A tornadic supercell developed in the simulation that had striking similarities to radar observations. The violent tornado in Funing County was reproduced, exceeding EF4 (74 m s-1), consistent with the on-site damage survey. It was accompanied by a funnel cloud that extended to the surface, and exhibited a double-helix vorticity structure. The signal of tornado genesis was found first at the cloud base in the pressure perturbation field, and then developed both upward and downward in terms of maximum vertical velocity overlapping with the intense vertical vorticity centers. The tornado's demise was found to accompany strong downdrafts overlapping with the intense vorticity centers. One of the interesting findings of this work is that a violent surface vortex was able to be generated and maintained, even though the simulation employed a free-slip lower boundary condition. The success of this simulation, despite using an idealized numerical approach, provides a means to investigate more historical tornadoes in China.

  17. The combination of structural parameters and areal bone mineral density improves relation to proximal femur strength. An in vitro study with high resolution peripheral quantitative computed tomography

    DEFF Research Database (Denmark)

    Hansen, Stinus; Beck Nielsen, Jens-Erik; Ahrberg, Fabian

    2011-01-01

    , volumetric BMD (vBMD), and microarchitectural parameters were obtained. In addition, aBMD by dual-energy X-ray absorptiometry (DXA) was performed at conventional hip regions and maximal compressive strength (MCS) was determined in a side-impact biomechanical test. Twelve cervical and 19 trochanteric...... fractures were confirmed. Geometry, vBMD, microarchitecture, and aBMD correlated significantly with MCS, with Spearman's correlation coefficients up to 0.77, 0.89, 0.90, and 0.85 (P ...

  18. Investigation of InN layers grown by MOCVD using analytical and high resolution TEM: The structure, band gap, role of the buffer layers

    International Nuclear Information System (INIS)

    Ruterana, P.; Abouzaid, M.; Gloux, F.; Maciej, W.; Doualan, J.L.; Drago, M.; Schmidtling, T.; Pohl, U.W.; Richter, W.

    2006-01-01

    In this work we investigate the microstructure of InN layers grown by MOCVD on different buffer layers using TEM (InN, GaN). The large mismatch between the various lattices (InN, sapphire or GaN) leads to particular interface structures. Our local analysis allows to show that at atomic scale, the material has the InN lattice parameters and that no metallic In precipitates are present, meaning that the PL emission below 0.8 eV is a genuine property of the InN semiconductor. It is also shown that the N polar layers, which exhibit a 2D growth, have poorer PL emission than In polar layers. (copyright 2006 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  19. High resolution measurements supported by electronic structure calculations of two naphthalene derivatives: [1,5]- and [1,6]-naphthyridine—Estimation of the zero point inertial defect for planar polycyclic aromatic compounds

    Energy Technology Data Exchange (ETDEWEB)

    Gruet, S., E-mail: sebastien.gruet@synchrotron-soleil.fr, E-mail: manuel.goubet@univ-lille1.fr; Pirali, O. [AILES Beamline, Synchrotron SOLEIL, Saint-Aubin, 91192 Gif-sur-Yvette (France); Institut des Sciences Moléculaires d’Orsay, UMR 8214 CNRS – Université Paris Sud, 91405 Orsay Cedex (France); Goubet, M., E-mail: sebastien.gruet@synchrotron-soleil.fr, E-mail: manuel.goubet@univ-lille1.fr [Laboratoire de Physique des Lasers, Atomes et Molécules, UMR 8523 CNRS – Université Lille 1, 59655 Villeneuve d’Ascq Cedex (France)

    2014-06-21

    Polycyclic aromatic hydrocarbons (PAHs) molecules are suspected to be present in the interstellar medium and to participate to the broad and unresolved emissions features, the so-called unidentified infrared bands. In the laboratory, very few studies report the rotationally resolved structure of such important class of molecules. In the present work, both experimental and theoretical approaches provide the first accurate determination of the rotational energy levels of two diazanaphthalene: [1,5]- and [1,6]-naphthyridine. [1,6]-naphthyridine has been studied at high resolution, in the microwave (MW) region using a Fourier transform microwave spectrometer and in the far-infrared (FIR) region using synchrotron-based Fourier transform spectroscopy. The very accurate set of ground state (GS) constants deduced from the analysis of the MW spectrum allowed the analysis of the most intense modes in the FIR (ν{sub 38}-GS centered at about 483 cm{sup −1} and ν{sub 34}-GS centered at about 842 cm{sup −1}). In contrast with [1,6]-naphthyridine, pure rotation spectroscopy of [1,5]-naphthyridine cannot be performed for symmetry reasons so the combined study of the two intense FIR modes (ν{sub 22}-GS centered at about 166 cm{sup −1} and ν{sub 18}-GS centered at about 818 cm{sup −1}) provided the GS and the excited states constants. Although the analysis of the very dense rotational patterns for such large molecules remains very challenging, relatively accurate anharmonic density functional theory calculations appeared as a highly relevant supporting tool to the analysis for both molecules. In addition, the good agreement between the experimental and calculated infrared spectrum shows that the present theoretical approach should provide useful data for the astrophysical models. Moreover, inertial defects calculated in the GS (Δ{sub GS}) of both molecules exhibit slightly negative values as previously observed for planar species of this molecular family. We adjusted

  20. Section on High Resolution Optical Imaging (HROI)

    Data.gov (United States)

    Federal Laboratory Consortium — The Section on High Resolution Optical Imaging (HROI) develops novel technologies for studying biological processes at unprecedented speed and resolution. Research...

  1. High resolution positron Q-value measurements and nuclear structure studies far from the stability line. Progress report, July 1, 1979-June 30, 1980

    International Nuclear Information System (INIS)

    Avignone, F.T. III.

    1980-01-01

    This document represents a progress report and renewal proposal for the contract DEAS 09 79 ER10434 between the USDOE and USC. During the time from 1 July 1979 to 1 March 1980, the large 35% intrinsic Ge detector was purchased and tested, and the new hyperpure Ge detector for positron end-point-energy measurements was designed and fabricated by ORTEC. It was delivered just prior to January 1, 1980. Measurements using this special equipment began in January 1980. During this period, a new effort in the measurement of short nuclear lifetimes was completed, and nuclear structure measurements of 206 Rn nd 208 Rn were completed. The results of these efforts are described in the text. A search for the Post Doctoral Research Associate was started last summer and the position will be filled on or about 1 March 1980. The first experiments to measure positron end-point-energies were proposed to the ORIC scheduling committee, and measurements will begin in March 1980. Theoretical efforts describe accurately the interference of annihilation radiation with positron end-point-energy measurements were begun

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-11-15

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

  3. Structure and dynamics of alpha-tocopherol in model membranes and in solution: a broad-line and high-resolution NMR study

    International Nuclear Information System (INIS)

    Ekiel, I.H.; Hughes, L.; Burton, G.W.; Jovall, P.A.; Ingold, K.U.; Smith, I.C.

    1988-01-01

    Nuclear magnetic resonance has been applied to study the conformational dynamics of alpha-tocopherol (vitamin E) in solution and in model membranes. In nonviscous solution, 1 H nuclear magnetic resonance (NMR) showed that alpha-tocopherol is in rapid equilibrium between two or more puckered conformers of its heterocyclic ring. The most likely conformers to be so involved are the two half-chair forms. Deuterium NMR spectra of specifically deuteriated alpha-tocopherol in multilamellar dispersions of egg phosphatidylcholine, measured in the liquid-crystalline state, were characteristic of axially symmetric motional averaging. The orientation of the rotational axis within the molecular framework was determined. Studies on oriented multilamellar membranes revealed that this axis is perpendicular to the surface of the membrane. The profile of quadrupolar splittings along the hydrophobic tail does not have a plateau, in contrast to that of the fatty acyl chains of the membrane lipids. Longitudinal relaxation times (T1) were short. The presence of a minimum in their temperature dependence shows that molecular motion with an effective correlation time tau eff approximately equal to 3 X 10(-9)s is responsible for relaxation. However, the temperatures and absolute values of the minima depend on the position of the deuterium in the molecule, demonstrating that tau eff represents a complex blend of motions

  4. Forward modelling of global gravity fields with 3D density structures and an application to the high-resolution ( 2 km) gravity fields of the Moon

    Science.gov (United States)

    Šprlák, M.; Han, S.-C.; Featherstone, W. E.

    2017-12-01

    Rigorous modelling of the spherical gravitational potential spectra from the volumetric density and geometry of an attracting body is discussed. Firstly, we derive mathematical formulas for the spatial analysis of spherical harmonic coefficients. Secondly, we present a numerically efficient algorithm for rigorous forward modelling. We consider the finite-amplitude topographic modelling methods as special cases, with additional postulates on the volumetric density and geometry. Thirdly, we implement our algorithm in the form of computer programs and test their correctness with respect to the finite-amplitude topography routines. For this purpose, synthetic and realistic numerical experiments, applied to the gravitational field and geometry of the Moon, are performed. We also investigate the optimal choice of input parameters for the finite-amplitude modelling methods. Fourth, we exploit the rigorous forward modelling for the determination of the spherical gravitational potential spectra inferred by lunar crustal models with uniform, laterally variable, radially variable, and spatially (3D) variable bulk density. Also, we analyse these four different crustal models in terms of their spectral characteristics and band-limited radial gravitation. We demonstrate applicability of the rigorous forward modelling using currently available computational resources up to degree and order 2519 of the spherical harmonic expansion, which corresponds to a resolution of 2.2 km on the surface of the Moon. Computer codes, a user manual and scripts developed for the purposes of this study are publicly available to potential users.

  5. Simultaneous determination of mushroom toxins α-amanitin, β-amanitin and muscarine in human urine by solid-phase extraction and ultra-high-performance liquid chromatography coupled with ultra-high-resolution TOF mass spectrometry.

    Science.gov (United States)

    Tomková, Jana; Ondra, Peter; Válka, Ivo

    2015-06-01

    This paper presents a method for the simultaneous determination of α-amanitin, β-amanitin and muscarine in human urine by solid-phase extraction (SPE) and ultra-high-performance liquid chromatography coupled with ultra-high-resolution TOF mass spectrometry. The method can be used for a diagnostics of mushroom poisonings. Different SPE cartridges were tested for sample preparation, namely hydrophilic modified reversed-phase (Oasis HLB) and polymeric weak cation phase (Strata X-CW). The latter gave better results and therefore it was chosen for the subsequent method optimization and partial validation. In the course of validation, limits of detection, linearity, intraday and interday precisions and recoveries were evaluated. The obtained LOD values of α-amanitin and β-amanitin were 1ng/mL and of muscarine 0.09ng/mL. The intraday and interday precisions of human urine spiked with α-amanitin (10ng/mL), β-amanitin (10ng/mL) and muscarine (1ng/mL) ranged from 6% to 10% and from 7% to 13%, respectively. The developed method was proved to be a relevant tool for the simultaneous determination of the studied mushroom toxins in human urine after mushroom poisoning. Copyright © 2015 Elsevier Ireland Ltd. All rights reserved.

  6. Halloysite nanotubes as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction for the determination of bismuth in water samples using high-resolution continuum source graphite-furnace atomic absorption spectrometry

    Science.gov (United States)

    Krawczyk-Coda, Magdalena

    2017-03-01

    In this research, a simple, accurate, and inexpensive preconcentration procedure was developed for the determination of bismuth in water samples, using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS). During the preconcentration step, halloysite nanotubes (HNTs) were used as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction (USA DMSPE). The influence of the pH of the sample solution, amount of HNTs, and extraction time, as well as of the main parameters of HR CS GFAAS, on absorbance was investigated. The limit of detection was 0.005 μg L- 1. The preconcentration factor achieved for bismuth was 32. The relative standard deviation (RSD) was 4%. The accuracy of this method was validated by analyses of NIST SRM 1643e (Trace elements in water) and TMDA-54.5 (A high level fortified sample for trace elements) certified reference materials. The measured bismuth contents in these certified reference materials were in satisfactory agreement with the certified values according to the t-test for a 95% confidence level. The proposed method has been successfully applied to the determination of bismuth in five different real water samples (seawater, lake water, river water, stream water and rain water).

  7. Cobalt internal standard for Ni to assist the simultaneous determination of Mo and Ni in plant materials by high-resolution continuum source graphite furnace atomic absorption spectrometry employing direct solid sample analysis.

    Science.gov (United States)

    de Babos, Diego Victor; Bechlin, Marcos André; Barros, Ariane Isis; Ferreira, Edilene Cristina; Gomes Neto, José Anchieta; de Oliveira, Silvana Ruella

    2016-05-15

    A new method is proposed for the simultaneous determination of Mo and Ni in plant materials by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS), employing direct solid sample analysis (DSS) and internal standardization (IS). Cobalt was used as internal standard to minimize matrix effects during Ni determinations, enabling the use of aqueous standards for calibration. Correlation coefficients for the calibration curves were typically better than 0.9937. The performance of the method was checked by analysis of six plant certified reference materials, and the results for Mo and Ni were in agreement with the certified values (95% confidence level, t-test). Analysis was made of different types of plant materials used as renewable sources of energy, including sugarcane leaves, banana tree fiber, soybean straw, coffee pods, orange bagasse, peanut hulls, and sugarcane bagasse. The concentrations found for Mo and Ni ranged from 0.08 to 0.63 ng mg(-1) and from 0.41 to 6.92 ng mg(-1), respectively. Precision (RSD) varied from 2.1% to 11% for Mo and from 3.7% to 10% for Ni. Limits of quantification of 0.055 and 0.074 ng were obtained for Mo and Ni, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. Seismic imaging of esker structures from a combination of high-resolution broadband multicomponent streamer and wireless sensors, Turku-Finland

    Science.gov (United States)

    Maries, Georgiana; Ahokangas, Elina; Mäkinen, Joni; Pasanen, Antti; Malehmir, Alireza

    2015-04-01

    information down to the bedrock, 50-80 m depth, using a diving-wave travel-time tomographic inversion method. The reflection data processing was challenging due to the large velocity contrasts between the dry sediments and the saturated ones. A careful velocity analysis was the key-processing step apart from filtering source-generated noise. The seismic refraction and reflection sections correlate well with the existing borehole information. Depth to the bedrock from the boreholes matches well the high velocity zones. A zone of low velocity associated with a flat reflection at about 20 m depth below the topography shows a good correspondence with the groundwater table. A major morphologically undetectable kettle hole (MUKH) is clearly observed in the reflection data as a concave reflectivity zone, with indication of normal faulting. The deposits show alternating coarse- and fine-grained sediments with channel structures representing subaqueous fans. An esker core is defined from a zone of reflectivity from coarser-grained materials overlaid by proximal fan sediments of the main aquifer. Acknowledgments: Formas (http://www.trust-geoinfra.se), Turku Region Water Ltd., University of Turku, GTK

  9. Development of AMS high resolution injector system

    International Nuclear Information System (INIS)

    Bao Yiwen; Guan Xialing; Hu Yueming

    2008-01-01

    The Beijing HI-13 tandem accelerator AMS high resolution injector system was developed. The high resolution energy achromatic system consists of an electrostatic analyzer and a magnetic analyzer, which mass resolution can reach 600 and transmission is better than 80%. (authors)

  10. High Resolution Scanning Ion Microscopy

    NARCIS (Netherlands)

    Castaldo, V.

    2011-01-01

    The structure of the thesis is the following. The first chapter is an introduction to scanning microscopy, where the path that led to the Focused Ion Beam (FIB) is described and the main differences between electrons and ion beams are highlighted. Chapter 2 is what is normally referred to (which I

  11. High-resolution electron microscopy and its applications.

    Science.gov (United States)

    Li, F H

    1987-12-01

    A review of research on high-resolution electron microscopy (HREM) carried out at the Institute of Physics, the Chinese Academy of Sciences, is presented. Apart from the direct observation of crystal and quasicrystal defects for some alloys, oxides, minerals, etc., and the structure determination for some minute crystals, an approximate image-contrast theory named pseudo-weak-phase object approximation (PWPOA), which shows the image contrast change with crystal thickness, is described. Within the framework of PWPOA, the image contrast of lithium ions in the crystal of R-Li2Ti3O7 has been observed. The usefulness of diffraction analysis techniques such as the direct method and Patterson method in HREM is discussed. Image deconvolution and resolution enhancement for weak-phase objects by use of the direct method are illustrated. In addition, preliminary results of image restoration for thick crystals are given.

  12. Structural changes of Bi sub 1. 8 Sr sub 2 (Ca sub 1 minus x Y sub x )Cu sub 2. 2 O sub z ceramics with yttrium content studied by electron diffraction and high-resolution electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Onozuka, T.; Iwabuchi, Y.; Fukase, T. (Institute for Materials Research, Tohoku University, Sendai 980, Japan (JP)); Sato, H. (School of Materials Engineering, Purdue University, West Lafayette, Indiana 47907 (USA)); Mitchell, T.E. (Los Alamos National Laboratory, Los Alamos, New Mexico 87545 (USA))

    1991-06-01

    The mode of the incommensurate modulation in the {ital b} direction of the Bi{sub 1.8}Sr{sub 2}(Ca{sub 1{minus}{ital x}}Y{sub {ital x}})Cu{sub 2.2}O{sub {ital z}} (0.05{lt}{ital x}{lt}0.75) system is investigated by means of electron diffraction and high-resolution lattice imaging. The change of period of the long-period structure with {ital x} is found to be basically due to the mixing ratio of domains of two modulation periods with {ital b}=4.5{ital b}{sub 0} and 5{ital b}{sub 0} or 4.5{ital b}{sub 0} and 4{ital b}{sub 0}, thus creating periods of {ital b}=4.75{ital b}{sub 0--}4.0{ital b}{sub 0}. The fundamental orthorhombic lattice has dimensions of {ital a}{congruent}{ital b}{congruent}{ital b}{sub 0} (0.54 nm) and {ital c}{congruent}{ital c}{sub 0} (3.1 nm). The change of the mixing mode from one to the other mentioned above occurs just in the yttrium concentration range, 0.45{lt}{ital x}{lt}0.65, which also corresponds to the superconductor (metallic)-to-semiconductor transition boundary. The mixing modes of the domains are directly recorded as a contrast modulation with half periods, 4.5{ital b}{sub 0}/2 and 5{ital b}{sub 0}/2 or 4.5{ital b}{sub 0}/2 and 4{ital b}{sub 0}/2 in high-resolution lattice images. These images are reproduced well by a multislice computer-simulation technique.

  13. Trace elements determination in high salinity petroleum produced formation water by high-resolution continuum source graphite furnace atomic absorption spectrometry after matrix separation using Chelex-100 Registered-Sign resin

    Energy Technology Data Exchange (ETDEWEB)

    Freire, Aline Soares [Departamento de Geoquimica, Universidade Federal Fluminense, Outeiro Sao Joao Batista s/n, Centro, Niteroi/RJ, 24020-150 (Brazil); Departamento de Quimica Analitica, Universidade Federal do Rio de Janeiro Av. Athos da Silveira Ramos 149, Centro de Tecnologia, Bloco A, Cidade Universitaria, Rio de Janeiro/RJ, 21941-909 (Brazil); Santelli, Ricardo Erthal, E-mail: santelli@iq.ufrj.br [Departamento de Geoquimica, Universidade Federal Fluminense, Outeiro Sao Joao Batista s/n, Centro, Niteroi/RJ, 24020-150 (Brazil); Departamento de Quimica Analitica, Universidade Federal do Rio de Janeiro Av. Athos da Silveira Ramos 149, Centro de Tecnologia, Bloco A, Cidade Universitaria, Rio de Janeiro/RJ, 21941-909 (Brazil)

    2012-05-15

    This study describes a procedure used for the determination of trace metals (Co, Cu, Mn, Ni and Pb) in high salinity petroleum produced formation water (PFW) employing high-resolution continuum source graphite furnace atomic absorption spectrometry for detection and Chelex-100 Registered-Sign resin for matrix elimination and analytes preconcentration. Using 15.0 mL of PFW for the separation/preconcentration, detection limits of 0.006, 0.07, 0.03, 0.08 and 0.02 {mu}g L{sup -1} were obtained for Co, Cu, Mn, Ni and Pb, respectively. The accuracy of the proposed method was evaluated by analyzing three seawater certified reference materials and by recovery tests, and the data indicate that the methodology can be successfully applied to this kind of samples. The precision values, expressed as relative standard deviation (% RSD, n = 10) for 2.0 {mu}g L{sup -1}, were found to be 3.5, 4.0, 9.0, 5.3 and 5.9 for Co, Cu, Mn, Ni and Pb, respectively. The proposed procedure was applied for the determination of these metals in medium and high salinity PFW samples obtained from Brazilian offshore petroleum exploration platforms. - Highlights: Black-Right-Pointing-Pointer Petroleum-produced formation water were analyzed for Co, Cu, Mn, Ni and Pb determination. Black-Right-Pointing-Pointer In batch analyte preconcentration/matrix separation using Chelex-100 Registered-Sign was used. Black-Right-Pointing-Pointer Detection limits between 0.006 and 0.08 {mu}g L{sup -1} were found by using HR-CS-GFAAS. Black-Right-Pointing-Pointer Trace elements characterization is possible using the developed method. Black-Right-Pointing-Pointer Maximum trace element concentrations found could support future Brazilian directives.

  14. Slurry sampling high-resolution continuum source electrothermal atomic absorption spectrometry for direct beryllium determination in soil and sediment samples after elimination of SiO interference by least-squares background correction.

    Science.gov (United States)

    Husáková, Lenka; Urbanová, Iva; Šafránková, Michaela; Šídová, Tereza

    2017-12-01

    In this work a simple, efficient, and environmentally-friendly method is proposed for determination of Be in soil and sediment samples employing slurry sampling and high-resolution continuum source electrothermal atomic absorption spectrometry (HR-CS-ETAAS). The spectral effects originating from SiO species were identified and successfully corrected by means of a mathematical correction algorithm. Fractional factorial design has been employed to assess the parameters affecting the analytical results and especially to help in the development of the slurry preparation and optimization of measuring conditions. The effects of seven analytical variables including particle size, concentration of glycerol and HNO 3 for stabilization and analyte extraction, respectively, the effect of ultrasonic agitation for slurry homogenization, concentration of chemical modifier, pyrolysis and atomization temperature were investigated by a 2 7-3 replicate (n = 3) design. Using the optimized experimental conditions, the proposed method allowed the determination of Be with a detection limit being 0.016mgkg -1 and characteristic mass 1.3pg. Optimum results were obtained after preparing the slurries by weighing 100mg of a sample with particle size < 54µm and adding 25mL of 20% w/w glycerol. The use of 1μg Rh and 50μg citric acid was found satisfactory for the analyte stabilization. Accurate data were obtained with the use of matrix-free calibration. The accuracy of the method was confirmed by analysis of two certified reference materials (NIST SRM 2702 Inorganics in Marine Sediment and IGI BIL-1 Baikal Bottom Silt) and by comparison of the results obtained for ten real samples by slurry sampling with those determined after microwave-assisted extraction by inductively coupled plasma time of flight mass spectrometry (TOF-ICP-MS). The reported method has a precision better than 7%. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. High resolution NMR in zeolites

    Energy Technology Data Exchange (ETDEWEB)

    Diaz, Anix [INTEVEP, Filial de Petroleos de Venezuela, SA, Caracas (Venezuela). Dept. de Analisis y Evalucion

    1992-12-31

    In this work {sup 29} Si and {sup 27} Al NMR spectroscopy was used to study various types of zeolites. The corresponding spectra were used to measure the Si/Al ratios, to follow chemical modifications ind