WorldWideScience

Sample records for detailed nmr analysis

  1. NMR spectroscopy: a tool for conformational analysis

    International Nuclear Information System (INIS)

    Tormena, Claudio F.; Cormanich, Rodrigo A.; Rittner, Roberto; Freitas, Matheus P.

    2011-01-01

    The present review deals with the application of NMR data to the conformational analysis of simple organic compounds, together with other experimental methods like infrared spectroscopy and with theoretical calculations. Each sub-section describes the results for a group of compounds which belong to a given organic function like ketones, esters, etc. Studies of a single compound, even of special relevance, were excluded since the main goal of this review is to compare the results for a given function, where different substituents were used or small structural changes were introduced in the substrate, in an attempt to disclose their effects in the conformational equilibrium. Moreover, the huge amount of data available in the literature, on this research field, imposed some limitations which will be detailed in the Introduction, but it can be reminded in advance that these limitations include mostly the period when these results were published. (author)

  2. Metal alkyls programmed to generate metal alkylidenes by α-H abstraction: prognosis from NMR chemical shift† †Electronic supplementary information (ESI) available: Experimental and computational details, NMR spectra, results of NMR calculations and NCS analysis, graphical representation of shielding tensors, molecular orbital diagrams of selected compounds, optimized structures for all calculated species. See DOI: 10.1039/c7sc05039a

    Science.gov (United States)

    Gordon, Christopher P.; Yamamoto, Keishi; Searles, Keith; Shirase, Satoru

    2018-01-01

    Metal alkylidenes, which are key organometallic intermediates in reactions such as olefination or alkene and alkane metathesis, are typically generated from metal dialkyl compounds [M](CH2R)2 that show distinctively deshielded chemical shifts for their α-carbons. Experimental solid-state NMR measurements combined with DFT/ZORA calculations and a chemical shift tensor analysis reveal that this remarkable deshielding originates from an empty metal d-orbital oriented in the M–Cα–Cα′ plane, interacting with the Cα p-orbital lying in the same plane. This π-type interaction inscribes some alkylidene character into Cα that favors alkylidene generation via α-H abstraction. The extent of the deshielding and the anisotropy of the alkyl chemical shift tensors distinguishes [M](CH2R)2 compounds that form alkylidenes from those that do not, relating the reactivity to molecular orbitals of the respective molecules. The α-carbon chemical shifts and tensor orientations thus predict the reactivity of metal alkyl compounds towards alkylidene generation. PMID:29675237

  3. Teaching NMR spectra analysis with nmr.cheminfo.org.

    Science.gov (United States)

    Patiny, Luc; Bolaños, Alejandro; Castillo, Andrés M; Bernal, Andrés; Wist, Julien

    2018-06-01

    Teaching spectra analysis and structure elucidation requires students to get trained on real problems. This involves solving exercises of increasing complexity and when necessary using computational tools. Although desktop software packages exist for this purpose, nmr.cheminfo.org platform offers students an online alternative. It provides a set of exercises and tools to help solving them. Only a small number of exercises are currently available, but contributors are invited to submit new ones and suggest new types of problems. Copyright © 2018 John Wiley & Sons, Ltd.

  4. PVT Degradation Studies: NMR Analysis

    Energy Technology Data Exchange (ETDEWEB)

    Cho, Herman M. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Kouzes, Richard T. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

    2017-06-06

    Under certain environmental conditions, polyvinyl toluene (PVT) plastic scintillator has been observed to undergo internal fogging. Nuclear magnetic resonance spectroscopy has been used to elucidate the state of water inside the PVT. The deuterium NMR results show that water absorbed by PVT under warm, humid conditions enters several distinct environments, and when the PVT is transferred from incubation to ambient temperature and humidity the water is lost on a time scale of a few hours from these samples. Most of the deuterium NMR peaks can be assigned to bulk liquid water, but almost 35% of the detected signal intensity is contained in a resonance that resembles spectra of water contained in nanometer-scale pores in mesoporous carbon.

  5. Nanodisc-Targeted STD NMR Spectroscopy Reveals Atomic Details of Ligand Binding to Lipid Environments.

    Science.gov (United States)

    Muñoz-García, Juan C; Inacio Dos Reis, Rosana; Taylor, Richard J; Henry, Alistair J; Watts, Anthony

    2018-05-18

    Saturation transfer difference (STD) NMR spectroscopy is one of the most popular ligand-based NMR techniques for the study of protein-ligand interactions. This is due to its robustness and the fact that it is focused on the signals of the ligand, without any need for NMR information on the macromolecular target. This technique is most commonly applied to systems involving different types of ligands (e.g., small organic molecules, carbohydrates or lipids) and a protein as the target, in which the latter is selectively saturated. However, only a few examples have been reported where membrane mimetics are the macromolecular binding partners. Here, we have employed STD NMR spectroscopy to investigate the interactions of the neurotransmitter dopamine with mimetics of lipid bilayers, such as nanodiscs, by saturation of the latter. In particular, the interactions between dopamine and model lipid nanodiscs formed either from charged or zwitterionic lipids have been resolved at the atomic level. The results, in agreement with previous isothermal titration calorimetry studies, show that dopamine preferentially binds to negatively charged model membranes, but also provide detailed atomic insights into the mode of interaction of dopamine with membrane mimetics. Our findings provide relevant structural information for the design of lipid-based drug carriers of dopamine and its structural analogues and are of general applicability to other systems. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Detailed {sup 1}H and {sup 13}C NMR spectral data assignment for two dihydrobenzofuran neolignans

    Energy Technology Data Exchange (ETDEWEB)

    Medeiros, Talita C.T.; Dias, Herbert J.; Crotti, Antônio E.M., E-mail: millercrotti@ffclrp.usp.br [Universidade de São Paulo (USP), Ribeirão Preto, SP (Brazil). Faculdade de Filosofia, Ciências e Letras. Departamento de Química

    2016-07-01

    In this work we present a complete proton ({sup 1}H) and carbon 13 ({sup 13}C) nuclear magnetic resonance (NMR) spectral analysis of two synthetic dihydrofuran neolignans (±)-trans-dehydrodicoumarate dimethyl ester and (±)-trans-dehydrodiferulate dimethyl ester. Unequivocal assignments were achieved by 1 H NMR, proton decoupled {sup 13}C ({sup 13}C{"1H}) NMR spectra, gradient-selected correlation spectroscopy (gCOSY), J-resolved, gradient-selected heteronuclear multiple quantum coherence (gHMQC), gradient-selected heteronuclear multiple bond coherence (gHMBC) and nuclear Overhauser effect spectroscopy (NOESY) experiments. All hydrogen coupling constants were measured, clarifying all the hydrogen signals multiplicities. Computational methods were also used to simulate the {sup 1}H and {sup 13}C chemical shifts and showed good agreement with the trans configuration of the substituents at C{sub 7} and C{sub 8}. (author)

  7. Detailed 1H and 13C NMR spectral data assignment for two dihydrobenzofuran neolignans

    International Nuclear Information System (INIS)

    Medeiros, Talita C.T.; Dias, Herbert J.; Crotti, Antônio E.M.

    2016-01-01

    In this work we present a complete proton ( 1 H) and carbon 13 ( 13 C) nuclear magnetic resonance (NMR) spectral analysis of two synthetic dihydrofuran neolignans (±)-trans-dehydrodicoumarate dimethyl ester and (±)-trans-dehydrodiferulate dimethyl ester. Unequivocal assignments were achieved by 1 H NMR, proton decoupled 13 C ( 13 C{ 1 H}) NMR spectra, gradient-selected correlation spectroscopy (gCOSY), J-resolved, gradient-selected heteronuclear multiple quantum coherence (gHMQC), gradient-selected heteronuclear multiple bond coherence (gHMBC) and nuclear Overhauser effect spectroscopy (NOESY) experiments. All hydrogen coupling constants were measured, clarifying all the hydrogen signals multiplicities. Computational methods were also used to simulate the 1 H and 13 C chemical shifts and showed good agreement with the trans configuration of the substituents at C 7 and C 8 . (author)

  8. Detailed NMR investigation of cyclodextrin-perfluorinated surfactant interactions in aqueous media

    Energy Technology Data Exchange (ETDEWEB)

    Weiss-Errico, Mary Jo; O’Shea, Kevin E., E-mail: osheak@fiu.edu

    2017-05-05

    Highlights: • Perfluorochemicals (PFCs) are strongly encapsulated by cyclodextrins (CDs). • Competition studies confirm strong CD:PFC host-guest interactions. • {sup 19}F NMR Spectroscopy demonstrates association constants up to 10{sup 5} M{sup −1}. • Position of CD along PFC chain is elucidated from NMR results. • CD:PFC complex is not disturbed under a variety of water quality conditions. - Abstract: Perfluorochemicals (PFCs) are contaminants of serious concern because of their toxicological properties, widespread presence in drinking water sources, and incredible stability in the environment. To assess the potential application of α-, β-, and γ-cyclodextrins for PFC remediation, we investigated their complexation with linear fluorinated carboxylic acids, sulfonates, and a sulfonamide with carbon backbones ranging from C4-C9. {sup 19}F Nuclear Magnetic Resonance (NMR) spectroscopy studies demonstrated β-CD formed the strongest complexes with these PFCs. The polar head group had a modest influence, but for PFCs with backbones longer than six carbons, strong association constants are observed for 1:1 (K{sub 1:1} ∼ 10{sup 5} M{sup −1}) and 2:1 (K{sub 2:1} ∼ 10{sup 3} M{sup −1}) β-CD:PFC complexes. Excess β-CD can be used to complex 99.5% of the longer chain PFCs. Competition studies with adamantane-carboxylic acid and phenol confirmed the nature and persistence of the β-CD:PFC complex. Detailed analyses of the individual NMR chemical shifts and Job plots indicate the favored positions of the β-CD along the PFC chain. Solution pH, ionic strength, and the presence of humic acid have modest influence on the β-CD:PFC complexes. The strong encapsulation of PFCs by β-CD under a variety of water quality conditions demonstrates the tremendous potential of CD-based materials for the environmental remediation of PFCs.

  9. Detailed Astrometric Analysis of Pluto

    Science.gov (United States)

    ROSSI, GUSTAVO B.; Vieira-Martins, R.; Camargo, J. I.; Assafin, M.

    2013-05-01

    Abstract (2,250 Maximum Characters): Pluto is the main representant of the transneptunian objects (TNO's), presenting some peculiarities such as an atmosphere and a satellite system with 5 known moons: Charon, discovered in 1978, Nix and Hydra, in 2006, P4 in 2011 and P5 in 2012. Until the arrival of the New Horizons spacecraft to this system (july 2015), stellar occultations are the most efficient method, from the ground, to know physical and dinamical properties of this system. In 2010, it was evident a drift in declinations (about 20 mas/year) comparing to the ephemerides. This fact motivated us to remake the reductions and analysis of a great set of our observations at OPD/LNA, in a total of 15 years. The ephemerides and occultations results was then compared with the astrometric and photometric reductions of CCD images of Pluto (around 6500 images). Two corrections were used for a refinement of the data set: diferential chromatic refraction and photocenter. The first is due to the mean color of background stars beeing redder than the color of Pluto, resulting in a slightly different path of light through the atmosphere (that may cause a difference in position of 0.1”). It became more evident because Pluto is crossing the region of the galactic plane. The photocenter correction is based on two gaussians curves overlapped, with different hights and non-coincident centers, corresponding to Pluto and Charon (since they have less than 1” of angular separation). The objective is to separate these two gaussian curves from the observed one and find the right position of Pluto. The method is strongly dependent of the hight of each of the gaussian curves, related to the respective albedos of charon and Pluto. A detailed analysis of the astrometric results, as well a comparison with occultation results was made. Since Pluto has an orbital period of 248,9 years and our interval of observation is about 15 years, we have around 12% of its observed orbit and also, our

  10. CcpNmr AnalysisAssign: a flexible platform for integrated NMR analysis

    Energy Technology Data Exchange (ETDEWEB)

    Skinner, Simon P.; Fogh, Rasmus H. [University of Leicester, Department of Molecular and Cell Biology, Leicester Institute for Structural- and Chemical Biology (United Kingdom); Boucher, Wayne [University of Cambridge, Department of Biochemistry (United Kingdom); Ragan, Timothy J.; Mureddu, Luca G.; Vuister, Geerten W., E-mail: gv29@le.ac.uk [University of Leicester, Department of Molecular and Cell Biology, Leicester Institute for Structural- and Chemical Biology (United Kingdom)

    2016-10-15

    NMR spectroscopy is an indispensably powerful technique for the analysis of biomolecules under ambient conditions, both for structural- and functional studies. However, in practice the complexity of the technique has often frustrated its application by non-specialists. In this paper, we present CcpNmr version-3, the latest software release from the Collaborative Computational Project for NMR, for all aspects of NMR data analysis, including liquid- and solid-state NMR data. This software has been designed to be simple, functional and flexible, and aims to ensure that routine tasks can be performed in a straightforward manner. We have designed the software according to modern software engineering principles and leveraged the capabilities of modern graphics libraries to simplify a variety of data analysis tasks. We describe the process of backbone assignment as an example of the flexibility and simplicity of implementing workflows, as well as the toolkit used to create the necessary graphics for this workflow. The package can be downloaded from www.ccpn.ac.uk/v3-software/downloads http://www.ccpn.ac.uk/v3-software/downloads and is freely available to all non-profit organisations.

  11. CcpNmr AnalysisAssign: a flexible platform for integrated NMR analysis

    International Nuclear Information System (INIS)

    Skinner, Simon P.; Fogh, Rasmus H.; Boucher, Wayne; Ragan, Timothy J.; Mureddu, Luca G.; Vuister, Geerten W.

    2016-01-01

    NMR spectroscopy is an indispensably powerful technique for the analysis of biomolecules under ambient conditions, both for structural- and functional studies. However, in practice the complexity of the technique has often frustrated its application by non-specialists. In this paper, we present CcpNmr version-3, the latest software release from the Collaborative Computational Project for NMR, for all aspects of NMR data analysis, including liquid- and solid-state NMR data. This software has been designed to be simple, functional and flexible, and aims to ensure that routine tasks can be performed in a straightforward manner. We have designed the software according to modern software engineering principles and leveraged the capabilities of modern graphics libraries to simplify a variety of data analysis tasks. We describe the process of backbone assignment as an example of the flexibility and simplicity of implementing workflows, as well as the toolkit used to create the necessary graphics for this workflow. The package can be downloaded from www.ccpn.ac.uk/v3-software/downloads http://www.ccpn.ac.uk/v3-software/downloads and is freely available to all non-profit organisations.

  12. NMR

    International Nuclear Information System (INIS)

    Kneeland, J.B.; Lee, B.C.P.; Whalen, J.P.; Knowles, R.J.R.; Cahill, P.T.

    1984-01-01

    Although still quite new, NMR imaging has already emerged as a safe, noninvasive, painless, and effective diagnostic modality requiring no ionizing radiation. Also, NMR appears already to have established itself as the method of choice for the examination of the brain spinal cord (excluding herniated disks). Another area in which NMR excels is in the examination of the pelvis. The use of surface coils offers the promise of visualizing structures with resolution unobtainable by any other means. In addition, NMR, with its superb visualization of vascular structures and potential ability to measure flow, may soon revolutionize the diagnosis of cardiovascular disease. Finally, NMR, through biochemically and physiologically based T/sub 1/ and T/sub 2/ indices or through spectroscopy, may provide a means of monitoring therapeutic response so as to permit tailoring of treatment to the individual patient. In short, NMR is today probably at the same stage as the x-ray was in Roentgen's day

  13. Detailed Source-Specific Molecular Composition of Ambient Aerosol Organic Matter Using Ultrahigh Resolution Mass Spectrometry and 1H NMR

    Directory of Open Access Journals (Sweden)

    Amanda S. Willoughby

    2016-06-01

    Full Text Available Organic aerosols (OA are universally regarded as an important component of the atmosphere that have far-ranging impacts on climate forcing and human health. Many of these impacts are related to OA molecular characteristics. Despite the acknowledged importance, current uncertainties related to the source apportionment of molecular properties and environmental impacts make it difficult to confidently predict the net impacts of OA. Here we evaluate the specific molecular compounds as well as bulk structural properties of total suspended particulates in ambient OA collected from key emission sources (marine, biomass burning, and urban using ultrahigh resolution mass spectrometry (UHR-MS and proton nuclear magnetic resonance spectroscopy (1H NMR. UHR-MS and 1H NMR show that OA within each source is structurally diverse, and the molecular characteristics are described in detail. Principal component analysis (PCA revealed that (1 aromatic nitrogen species are distinguishing components for these biomass burning aerosols; (2 these urban aerosols are distinguished by having formulas with high O/C ratios and lesser aromatic and condensed aromatic formulas; and (3 these marine aerosols are distinguished by lipid-like compounds of likely marine biological origin. This study provides a unique qualitative approach for enhancing the chemical characterization of OA necessary for molecular source apportionment.

  14. PDBStat: a universal restraint converter and restraint analysis software package for protein NMR

    International Nuclear Information System (INIS)

    Tejero, Roberto; Snyder, David; Mao, Binchen; Aramini, James M.; Montelione, Gaetano T.

    2013-01-01

    The heterogeneous array of software tools used in the process of protein NMR structure determination presents organizational challenges in the structure determination and validation processes, and creates a learning curve that limits the broader use of protein NMR in biology. These challenges, including accurate use of data in different data formats required by software carrying out similar tasks, continue to confound the efforts of novices and experts alike. These important issues need to be addressed robustly in order to standardize protein NMR structure determination and validation. PDBStat is a C/C++ computer program originally developed as a universal coordinate and protein NMR restraint converter. Its primary function is to provide a user-friendly tool for interconverting between protein coordinate and protein NMR restraint data formats. It also provides an integrated set of computational methods for protein NMR restraint analysis and structure quality assessment, relabeling of prochiral atoms with correct IUPAC names, as well as multiple methods for analysis of the consistency of atomic positions indicated by their convergence across a protein NMR ensemble. In this paper we provide a detailed description of the PDBStat software, and highlight some of its valuable computational capabilities. As an example, we demonstrate the use of the PDBStat restraint converter for restrained CS-Rosetta structure generation calculations, and compare the resulting protein NMR structure models with those generated from the same NMR restraint data using more traditional structure determination methods. These results demonstrate the value of a universal restraint converter in allowing the use of multiple structure generation methods with the same restraint data for consensus analysis of protein NMR structures and the underlying restraint data

  15. PDBStat: a universal restraint converter and restraint analysis software package for protein NMR

    Energy Technology Data Exchange (ETDEWEB)

    Tejero, Roberto [Rutgers, The State University of New Jersey, Center for Advanced Biotechnology and Medicine (United States); Snyder, David [William Paterson University, Department of Chemistry (United States); Mao, Binchen; Aramini, James M.; Montelione, Gaetano T., E-mail: guy@cabm.rutgers.edu [Rutgers, The State University of New Jersey, Center for Advanced Biotechnology and Medicine (United States)

    2013-08-15

    The heterogeneous array of software tools used in the process of protein NMR structure determination presents organizational challenges in the structure determination and validation processes, and creates a learning curve that limits the broader use of protein NMR in biology. These challenges, including accurate use of data in different data formats required by software carrying out similar tasks, continue to confound the efforts of novices and experts alike. These important issues need to be addressed robustly in order to standardize protein NMR structure determination and validation. PDBStat is a C/C++ computer program originally developed as a universal coordinate and protein NMR restraint converter. Its primary function is to provide a user-friendly tool for interconverting between protein coordinate and protein NMR restraint data formats. It also provides an integrated set of computational methods for protein NMR restraint analysis and structure quality assessment, relabeling of prochiral atoms with correct IUPAC names, as well as multiple methods for analysis of the consistency of atomic positions indicated by their convergence across a protein NMR ensemble. In this paper we provide a detailed description of the PDBStat software, and highlight some of its valuable computational capabilities. As an example, we demonstrate the use of the PDBStat restraint converter for restrained CS-Rosetta structure generation calculations, and compare the resulting protein NMR structure models with those generated from the same NMR restraint data using more traditional structure determination methods. These results demonstrate the value of a universal restraint converter in allowing the use of multiple structure generation methods with the same restraint data for consensus analysis of protein NMR structures and the underlying restraint data.

  16. Complete 1H NMR spectral analysis of ten chemical markers of Ginkgo biloba.

    Science.gov (United States)

    Napolitano, José G; Lankin, David C; Chen, Shao-Nong; Pauli, Guido F

    2012-08-01

    The complete and unambiguous (1)H NMR assignments of ten marker constituents of Ginkgo biloba are described. The comprehensive (1)H NMR profiles (fingerprints) of ginkgolide A, ginkgolide B, ginkgolide C, ginkgolide J, bilobalide, quercetin, kaempferol, isorhamnetin, isoquercetin, and rutin in DMSO-d(6) were obtained through the examination of 1D (1)H NMR and 2D (1)H,(1)H-COSY data, in combination with (1)H iterative full spin analysis (HiFSA). The computational analysis of discrete spin systems allowed a detailed characterization of all the (1)H NMR signals in terms of chemical shifts (δ(H)) and spin-spin coupling constants (J(HH)), regardless of signal overlap and higher order coupling effects. The capability of the HiFSA-generated (1)H fingerprints to reproduce experimental (1)H NMR spectra at different field strengths was also evaluated. As a result of this analysis, a revised set of (1)H NMR parameters for all ten phytoconstituents was assembled. Furthermore, precise (1)H NMR assignments of the sugar moieties of isoquercetin and rutin are reported for the first time. Copyright © 2012 John Wiley & Sons, Ltd.

  17. Crystallographically-based analysis of the NMR spectra of maghemite

    International Nuclear Information System (INIS)

    Spiers, K.M.; Cashion, J.D.

    2012-01-01

    All possible iron environments with respect to nearest neighbour vacancies in vacancy-ordered and vacancy-disordered maghemite have been evaluated and used as the foundation for a crystallographically-based analysis of the published NMR spectra of maghemite. The spectral components have been assigned to particular configurations and excellent agreement obtained in comparing predicted spectra with published spectra taken in applied magnetic fields. The broadness of the published NMR lines has been explained by calculations of the magnetic dipole fields at the various iron sites and consideration of the supertransferred hyperfine fields. - Highlights: ► Analysis of 57 Fe NMR of maghemite based on vacancy ordering and nearest neighbour vacancies. ► Assignment of NMR spectral components based on crystallographic analysis of unique iron sites. ► Strong agreement between predicted spectra and published spectra taken in applied magnetic fields. ► Maghemite NMR spectral broadening due to various iron sites and supertransferred hyperfine field.

  18. [Rapid analysis of suppositories by quantitative 1H NMR spectroscopy].

    Science.gov (United States)

    Abramovich, R A; Kovaleva, S A; Goriainov, S V; Vorob'ev, A N; Kalabin, G A

    2012-01-01

    Rapid analysis of suppositories with ibuprofen and arbidol by quantitative 1H NMR spectroscopy was performed. Optimal conditions for the analysis were developed. The results are useful for design of rapid methods for quality control of suppositories with different components

  19. NMR Analysis of Some Pentacycloundecanedione Derivatives

    African Journals Online (AJOL)

    NJD

    Although many authors have commented on the difficulty of ... coming these former difficulties. Cookson's dione 19,10 .... and 2.58 ppm) is the common factor and the positions of H-2. (2.94 ppm) .... Owing to advances in NMR technology, the.

  20. Nmrglue: an open source Python package for the analysis of multidimensional NMR data.

    Science.gov (United States)

    Helmus, Jonathan J; Jaroniec, Christopher P

    2013-04-01

    Nmrglue, an open source Python package for working with multidimensional NMR data, is described. When used in combination with other Python scientific libraries, nmrglue provides a highly flexible and robust environment for spectral processing, analysis and visualization and includes a number of common utilities such as linear prediction, peak picking and lineshape fitting. The package also enables existing NMR software programs to be readily tied together, currently facilitating the reading, writing and conversion of data stored in Bruker, Agilent/Varian, NMRPipe, Sparky, SIMPSON, and Rowland NMR Toolkit file formats. In addition to standard applications, the versatility offered by nmrglue makes the package particularly suitable for tasks that include manipulating raw spectrometer data files, automated quantitative analysis of multidimensional NMR spectra with irregular lineshapes such as those frequently encountered in the context of biomacromolecular solid-state NMR, and rapid implementation and development of unconventional data processing methods such as covariance NMR and other non-Fourier approaches. Detailed documentation, install files and source code for nmrglue are freely available at http://nmrglue.com. The source code can be redistributed and modified under the New BSD license.

  1. Nmrglue: an open source Python package for the analysis of multidimensional NMR data

    Energy Technology Data Exchange (ETDEWEB)

    Helmus, Jonathan J., E-mail: jjhelmus@gmail.com [Argonne National Laboratory, Environmental Science Division (United States); Jaroniec, Christopher P., E-mail: jaroniec@chemistry.ohio-state.edu [Ohio State University, Department of Chemistry and Biochemistry (United States)

    2013-04-15

    Nmrglue, an open source Python package for working with multidimensional NMR data, is described. When used in combination with other Python scientific libraries, nmrglue provides a highly flexible and robust environment for spectral processing, analysis and visualization and includes a number of common utilities such as linear prediction, peak picking and lineshape fitting. The package also enables existing NMR software programs to be readily tied together, currently facilitating the reading, writing and conversion of data stored in Bruker, Agilent/Varian, NMRPipe, Sparky, SIMPSON, and Rowland NMR Toolkit file formats. In addition to standard applications, the versatility offered by nmrglue makes the package particularly suitable for tasks that include manipulating raw spectrometer data files, automated quantitative analysis of multidimensional NMR spectra with irregular lineshapes such as those frequently encountered in the context of biomacromolecular solid-state NMR, and rapid implementation and development of unconventional data processing methods such as covariance NMR and other non-Fourier approaches. Detailed documentation, install files and source code for nmrglue are freely available at http://nmrglue.comhttp://nmrglue.com. The source code can be redistributed and modified under the New BSD license.

  2. Nmrglue: an open source Python package for the analysis of multidimensional NMR data

    International Nuclear Information System (INIS)

    Helmus, Jonathan J.; Jaroniec, Christopher P.

    2013-01-01

    Nmrglue, an open source Python package for working with multidimensional NMR data, is described. When used in combination with other Python scientific libraries, nmrglue provides a highly flexible and robust environment for spectral processing, analysis and visualization and includes a number of common utilities such as linear prediction, peak picking and lineshape fitting. The package also enables existing NMR software programs to be readily tied together, currently facilitating the reading, writing and conversion of data stored in Bruker, Agilent/Varian, NMRPipe, Sparky, SIMPSON, and Rowland NMR Toolkit file formats. In addition to standard applications, the versatility offered by nmrglue makes the package particularly suitable for tasks that include manipulating raw spectrometer data files, automated quantitative analysis of multidimensional NMR spectra with irregular lineshapes such as those frequently encountered in the context of biomacromolecular solid-state NMR, and rapid implementation and development of unconventional data processing methods such as covariance NMR and other non-Fourier approaches. Detailed documentation, install files and source code for nmrglue are freely available at http://nmrglue.comhttp://nmrglue.com. The source code can be redistributed and modified under the New BSD license.

  3. ImatraNMR: Novel software for batch integration and analysis of quantitative NMR spectra

    Science.gov (United States)

    Mäkelä, A. V.; Heikkilä, O.; Kilpeläinen, I.; Heikkinen, S.

    2011-08-01

    Quantitative NMR spectroscopy is a useful and important tool for analysis of various mixtures. Recently, in addition of traditional quantitative 1D 1H and 13C NMR methods, a variety of pulse sequences aimed for quantitative or semiquantitative analysis have been developed. To obtain actual usable results from quantitative spectra, they must be processed and analyzed with suitable software. Currently, there are many processing packages available from spectrometer manufacturers and third party developers, and most of them are capable of analyzing and integration of quantitative spectra. However, they are mainly aimed for processing single or few spectra, and are slow and difficult to use when large numbers of spectra and signals are being analyzed, even when using pre-saved integration areas or custom scripting features. In this article, we present a novel software, ImatraNMR, designed for batch analysis of quantitative spectra. In addition to capability of analyzing large number of spectra, it provides results in text and CSV formats, allowing further data-analysis using spreadsheet programs or general analysis programs, such as Matlab. The software is written with Java, and thus it should run in any platform capable of providing Java Runtime Environment version 1.6 or newer, however, currently it has only been tested with Windows and Linux (Ubuntu 10.04). The software is free for non-commercial use, and is provided with source code upon request.

  4. Comprehensive NMR analysis of compositional changes of black garlic during thermal processing.

    Science.gov (United States)

    Liang, Tingfu; Wei, Feifei; Lu, Yi; Kodani, Yoshinori; Nakada, Mitsuhiko; Miyakawa, Takuya; Tanokura, Masaru

    2015-01-21

    Black garlic is a processed food product obtained by subjecting whole raw garlic to thermal processing that causes chemical reactions, such as the Maillard reaction, which change the composition of the garlic. In this paper, we report a nuclear magnetic resonance (NMR)-based comprehensive analysis of raw garlic and black garlic extracts to determine the compositional changes resulting from thermal processing. (1)H NMR spectra with a detailed signal assignment showed that 38 components were altered by thermal processing of raw garlic. For example, the contents of 11 l-amino acids increased during the first step of thermal processing over 5 days and then decreased. Multivariate data analysis revealed changes in the contents of fructose, glucose, acetic acid, formic acid, pyroglutamic acid, cycloalliin, and 5-(hydroxymethyl)furfural (5-HMF). Our results provide comprehensive information on changes in NMR-detectable components during thermal processing of whole garlic.

  5. Calibrating Detailed Chemical Analysis of M dwarfs

    Science.gov (United States)

    Veyette, Mark; Muirhead, Philip Steven; Mann, Andrew; Brewer, John; Allard, France; Homeier, Derek

    2018-01-01

    The ability to perform detailed chemical analysis of Sun-like F-, G-, and K-type stars is a powerful tool with many applications including studying the chemical evolution of the Galaxy, assessing membership in stellar kinematic groups, and constraining planet formation theories. Unfortunately, complications in modeling cooler stellar atmospheres has hindered similar analysis of M-dwarf stars. Large surveys of FGK abundances play an important role in developing methods to measure the compositions of M dwarfs by providing benchmark FGK stars that have widely-separated M dwarf companions. These systems allow us to empirically calibrate metallicity-sensitive features in M dwarf spectra. However, current methods to measure metallicity in M dwarfs from moderate-resolution spectra are limited to measuring overall metallicity and largely rely on astrophysical abundance correlations in stellar populations. In this talk, I will discuss how large, homogeneous catalogs of precise FGK abundances are crucial to advancing chemical analysis of M dwarfs beyond overall metallicity to direct measurements of individual elemental abundances. I will present a new method to analyze high-resolution, NIR spectra of M dwarfs that employs an empirical calibration of synthetic M dwarf spectra to infer effective temperature, Fe abundance, and Ti abundance. This work is a step toward detailed chemical analysis of M dwarfs at a similar precision achieved for FGK stars.

  6. INFOS: spectrum fitting software for NMR analysis

    Energy Technology Data Exchange (ETDEWEB)

    Smith, Albert A., E-mail: alsi@nmr.phys.chem.ethz.ch [ETH Zürich, Physical Chemistry (Switzerland)

    2017-02-15

    Software for fitting of NMR spectra in MATLAB is presented. Spectra are fitted in the frequency domain, using Fourier transformed lineshapes, which are derived using the experimental acquisition and processing parameters. This yields more accurate fits compared to common fitting methods that use Lorentzian or Gaussian functions. Furthermore, a very time-efficient algorithm for calculating and fitting spectra has been developed. The software also performs initial peak picking, followed by subsequent fitting and refinement of the peak list, by iteratively adding and removing peaks to improve the overall fit. Estimation of error on fitting parameters is performed using a Monte-Carlo approach. Many fitting options allow the software to be flexible enough for a wide array of applications, while still being straightforward to set up with minimal user input.

  7. Quantitative analysis of protein-ligand interactions by NMR.

    Science.gov (United States)

    Furukawa, Ayako; Konuma, Tsuyoshi; Yanaka, Saeko; Sugase, Kenji

    2016-08-01

    Protein-ligand interactions have been commonly studied through static structures of the protein-ligand complex. Recently, however, there has been increasing interest in investigating the dynamics of protein-ligand interactions both for fundamental understanding of the underlying mechanisms and for drug development. NMR is a versatile and powerful tool, especially because it provides site-specific quantitative information. NMR has widely been used to determine the dissociation constant (KD), in particular, for relatively weak interactions. The simplest NMR method is a chemical-shift titration experiment, in which the chemical-shift changes of a protein in response to ligand titration are measured. There are other quantitative NMR methods, but they mostly apply only to interactions in the fast-exchange regime. These methods derive the dissociation constant from population-averaged NMR quantities of the free and bound states of a protein or ligand. In contrast, the recent advent of new relaxation-based experiments, including R2 relaxation dispersion and ZZ-exchange, has enabled us to obtain kinetic information on protein-ligand interactions in the intermediate- and slow-exchange regimes. Based on R2 dispersion or ZZ-exchange, methods that can determine the association rate, kon, dissociation rate, koff, and KD have been developed. In these approaches, R2 dispersion or ZZ-exchange curves are measured for multiple samples with different protein and/or ligand concentration ratios, and the relaxation data are fitted to theoretical kinetic models. It is critical to choose an appropriate kinetic model, such as the two- or three-state exchange model, to derive the correct kinetic information. The R2 dispersion and ZZ-exchange methods are suitable for the analysis of protein-ligand interactions with a micromolar or sub-micromolar dissociation constant but not for very weak interactions, which are typical in very fast exchange. This contrasts with the NMR methods that are used

  8. Covariance NMR Processing and Analysis for Protein Assignment.

    Science.gov (United States)

    Harden, Bradley J; Frueh, Dominique P

    2018-01-01

    During NMR resonance assignment it is often necessary to relate nuclei to one another indirectly, through their common correlations to other nuclei. Covariance NMR has emerged as a powerful technique to correlate such nuclei without relying on error-prone peak peaking. However, false-positive artifacts in covariance spectra have impeded a general application to proteins. We recently introduced pre- and postprocessing steps to reduce the prevalence of artifacts in covariance spectra, allowing for the calculation of a variety of 4D covariance maps obtained from diverse combinations of pairs of 3D spectra, and we have employed them to assign backbone and sidechain resonances in two large and challenging proteins. In this chapter, we present a detailed protocol describing how to (1) properly prepare existing 3D spectra for covariance, (2) understand and apply our processing script, and (3) navigate and interpret the resulting 4D spectra. We also provide solutions to a number of errors that may occur when using our script, and we offer practical advice when assigning difficult signals. We believe such 4D spectra, and covariance NMR in general, can play an integral role in the assignment of NMR signals.

  9. Computer compensation for NMR quantitative analysis of trace components

    International Nuclear Information System (INIS)

    Nakayama, T.; Fujiwara, Y.

    1981-01-01

    A computer program has been written that determines trace components and separates overlapping components in multicomponent NMR spectra. This program uses the Lorentzian curve as a theoretical curve of NMR spectra. The coefficients of the Lorentzian are determined by the method of least squares. Systematic errors such as baseline/phase distortion are compensated and random errors are smoothed by taking moving averages, so that there processes contribute substantially to decreasing the accumulation time of spectral data. The accuracy of quantitative analysis of trace components has been improved by two significant figures. This program was applied to determining the abundance of 13C and the saponification degree of PVA

  10. A global analysis of NMR distance constraints from the PDB

    International Nuclear Information System (INIS)

    Vranken, Wim

    2007-01-01

    Information obtained from Nuclear Magnetic Resonance (NMR) experiments is encoded as a set of constraint lists when calculating three-dimensional structures for a protein. With the amount of constraint data from the world wide Protein Data Bank (wwPDB) that is now available, it is possible to do a global, large-scale analysis using only information from the constraints, without taking the coordinate information into account. This article describes such an analysis of distance constraints from NOE data based on a set of 1834 NMR PDB entries containing 1909 protein chains. In order to best represent the quality and extent of the data that is currently deposited at the wwPDB, only the original data as deposited by the authors was used, and no attempt was made to 'clean up' and further interpret this information. Because the constraint lists provide a single set of data, and not an ensemble of structural solutions, they are easier to analyse and provide a reduced form of structural information that is relevant for NMR analysis only. The online resource resulting from this analysis makes it possible to check, for example, how often a particular contact occurs when assigning NOESY spectra, or to find out whether a particular sequence fragment is likely to be difficult to assign. In this respect it formalises information that scientists with experience in spectrum analysis are aware of but cannot necessarily quantify. The analysis described here illustrates the importance of depositing constraints (and all other possible NMR derived information) along with the structure coordinates, as this type of information can greatly assist the NMR community

  11. Quantitative produced water analysis using mobile 1H NMR

    International Nuclear Information System (INIS)

    Wagner, Lisabeth; Fridjonsson, Einar O; May, Eric F; Stanwix, Paul L; Graham, Brendan F; Carroll, Matthew R J; Johns, Michael L; Kalli, Chris

    2016-01-01

    Measurement of oil contamination of produced water is required in the oil and gas industry to the (ppm) level prior to discharge in order to meet typical environmental legislative requirements. Here we present the use of compact, mobile 1 H nuclear magnetic resonance (NMR) spectroscopy, in combination with solid phase extraction (SPE), to meet this metrology need. The NMR hardware employed featured a sufficiently homogeneous magnetic field, such that chemical shift differences could be used to unambiguously differentiate, and hence quantitatively detect, the required oil and solvent NMR signals. A solvent system consisting of 1% v/v chloroform in tetrachloroethylene was deployed, this provided a comparable 1 H NMR signal intensity for the oil and the solvent (chloroform) and hence an internal reference 1 H signal from the chloroform resulting in the measurement being effectively self-calibrating. The measurement process was applied to water contaminated with hexane or crude oil over the range 1–30 ppm. The results were validated against known solubility limits as well as infrared analysis and gas chromatography. (paper)

  12. Detailed inelastic analysis of an LMFBR pipeline

    International Nuclear Information System (INIS)

    Hibbitt, H.D.; Leung, E.K.; Ohalla, A.K.

    1982-01-01

    The paper describes detailed inelastic analyses of a large diameter, thin walled pipeline configuration typical of liquid metal cooled reactor primary piping, subject to thermal shock, with intermediate periods of creep hold time. Three such analyses are compared. Two of these analyses are performed with recently developed elements based on a combination of Fourier and polynomial interpolation to describe the deformation of the pipe. One of these two analyses includes continuous deformation of the pipe wall between each elbow and the adjacent straight pipe segments, while the other neglects such ''end effects'' on the elbow deformation. The third analysis is based on a modified axi-symmetric shell element for modeling the elbows (neglecting and effects). The results thus provide an assessment of the relative cost and importance of including consideration of end effects in modeling a realistic piping system, as well as providing a similar comparison between the two basic deforming section pipe models (Fourier/polynomial versus modified axi-symmetric shells)

  13. Automated NMR relaxation dispersion data analysis using NESSY

    Directory of Open Access Journals (Sweden)

    Gooley Paul R

    2011-10-01

    Full Text Available Abstract Background Proteins are dynamic molecules with motions ranging from picoseconds to longer than seconds. Many protein functions, however, appear to occur on the micro to millisecond timescale and therefore there has been intense research of the importance of these motions in catalysis and molecular interactions. Nuclear Magnetic Resonance (NMR relaxation dispersion experiments are used to measure motion of discrete nuclei within the micro to millisecond timescale. Information about conformational/chemical exchange, populations of exchanging states and chemical shift differences are extracted from these experiments. To ensure these parameters are correctly extracted, accurate and careful analysis of these experiments is necessary. Results The software introduced in this article is designed for the automatic analysis of relaxation dispersion data and the extraction of the parameters mentioned above. It is written in Python for multi platform use and highest performance. Experimental data can be fitted to different models using the Levenberg-Marquardt minimization algorithm and different statistical tests can be used to select the best model. To demonstrate the functionality of this program, synthetic data as well as NMR data were analyzed. Analysis of these data including the generation of plots and color coded structures can be performed with minimal user intervention and using standard procedures that are included in the program. Conclusions NESSY is easy to use open source software to analyze NMR relaxation data. The robustness and standard procedures are demonstrated in this article.

  14. Quali- and quantitative analysis of commercial coffee by NMR

    International Nuclear Information System (INIS)

    Tavares, Leila Aley; Ferreira, Antonio Gilberto

    2006-01-01

    Coffee is one of the beverages most widely consumed in the world and the 'cafezinho' is normally prepared from a blend of roasted powder of two species, Coffea arabica and Coffea canephora. Each one exhibits differences in their taste and in the chemical composition, especially in the caffeine percentage. There are several procedures proposed in the literature for caffeine determination in different samples like soft drinks, coffee, medicines, etc but most of them need a sample workup which involves at least one step of purification. This work describes the quantitative analysis of caffeine using 1 H NMR and the identification of the major components in commercial coffee samples using 1D and 2D NMR techniques without any sample pre-treatment. (author)

  15. The fluorescence properties and NMR analysis of protopine and allocryptopine

    International Nuclear Information System (INIS)

    Kubala, Martin; Vacek, Jan; Popa, Igor; Janovska, Marika; Kosina, Pavel; Ulrichova, Jitka; Travnicek, Zdenek; Simanek, Vilim

    2011-01-01

    The fluorescence properties of protopine and allocryptopine in aqueous and organic environments are described for the first time. The fluorescence of alkaloids and their pH-dependent interconversion to cationic forms (transannular interaction) were studied using steady-state and time-resolved fluorescence techniques. For the analysis of tricyclic base and cis/trans tetracyclic cations of the alkaloids, NMR and X-ray crystallography were used. - Highlights: → We describe fundamental fluorescence characteristics of alkaloids protopine and allocryptopine. → We analyzed the pH-dependent transitions and cis/trans isomerization. → These two alkaloids can be better distinguished by their fluorescence decay characteristics. → The fluorescence parameters are related to the NMR and crystallographic structural data.

  16. Phosphorus-31 NMR analysis of gold plating baths

    Energy Technology Data Exchange (ETDEWEB)

    Smith, R.E.

    1992-03-01

    This report describes the nuclear magnetic resonance (NMR) analysis of gold plating baths in the Micro-Miniature Electronic Assembly department of Allied-Signal Inc., Kansas City Division (KCD). The baths were analyzed for phosphorylated components. In freshly prepared gold plating baths in this department the principle compound observed is aminotrimethyl-phosphonate, or ATMP. As the bath is used in production, the ATMP breaks down; and new compounds, aminodimethylphosphonate (ADMP), aminomonomethylphosphonate, (AMMP), and inorganic phosphate (H{sub 2}PO{sub 4}{sup {minus}}), are formed. The NMR method has been used for almost three years to monitor the concentrations of the ATMP and breakdown products. In a previous report, results from January through October 1988 were reported. In this report, results from November 1988 through January 1991 are given.

  17. LC-NMR coupling technology: recent advancements and applications in natural products analysis

    NARCIS (Netherlands)

    Exarchou, V.; Krucker, M.; Beek, van T.A.; Vervoort, J.J.M.; Gerothanassis, I.P.; Albert, K.

    2005-01-01

    An overview of recent advances in nuclear magnetic resonance (NMR) coupled with separation technologies and their application in natural product analysis is given and discussed. The different modes of LC-NMR operation are described, as well as how technical improvements assist in establishing LC-NMR

  18. Combined chemometric analysis of (1)H NMR, (13)C NMR and stable isotope data to differentiate organic and conventional milk.

    Science.gov (United States)

    Erich, Sarah; Schill, Sandra; Annweiler, Eva; Waiblinger, Hans-Ulrich; Kuballa, Thomas; Lachenmeier, Dirk W; Monakhova, Yulia B

    2015-12-01

    The increased sales of organically produced food create a strong need for analytical methods, which could authenticate organic and conventional products. Combined chemometric analysis of (1)H NMR-, (13)C NMR-spectroscopy data, stable-isotope data (IRMS) and α-linolenic acid content (gas chromatography) was used to differentiate organic and conventional milk. In total 85 raw, pasteurized and ultra-heat treated (UHT) milk samples (52 organic and 33 conventional) were collected between August 2013 and May 2014. The carbon isotope ratios of milk protein and milk fat as well as the α-linolenic acid content of these samples were determined. Additionally, the milk fat was analyzed by (1)H and (13)C NMR spectroscopy. The chemometric analysis of combined data (IRMS, GC, NMR) resulted in more precise authentication of German raw and retail milk with a considerably increased classification rate of 95% compared to 81% for NMR and 90% for IRMS using linear discriminate analysis. Copyright © 2015 Elsevier Ltd. All rights reserved.

  19. OPIC Greenhouse Gas Emissions Analysis Details

    Data.gov (United States)

    Overseas Private Investment Corporation — Summary project inventory with independent analysis to quantify the greenhouse gas ("GHG") emissions directly attributable to projects to which the Overseas Private...

  20. Chemometric analysis of ESIMS and NMR data from Piper species

    Energy Technology Data Exchange (ETDEWEB)

    Yamaguchi, Lydia F.; Freitas, Giovana C.; Yoshida, Nidia C.; Silva, Renata A.; Gaia, Anderson M.; Silva, Adalberto M.; Kato, Massuo J.; Emerenciano, Vicente de P., E-mail: majokato@iq.usp.br [Departamento de Quimica Fundamental, Instituto de Quimica, Universidade de Sao Paulo, SP (Brazil); Scotti, Marcus T. [Centro de Ciencias Aplicadas e Educacao (Campus IV), Universidade Federal da Paraiba, Rio Tinto, PB (Brazil); Guimaraes, Elsie F. [Instituto de Pesquisas Jardim Botanico do Rio de Janeiro, RJ (Brazil); Floh, Eny I.S. [Departamento de Botanica, Instituto de Biociencias, Sao Paulo, SP (Brazil); Colombo, Carlos A.; Siqueira, Walter J. [Centro de Genetica Biologia Molecular e Fitoquimica, Instituto Agronomico de Campinas, SP (Brazil)

    2011-09-15

    The metabolomic profiling based on the application of multivariate analysis (principal component analysis, PCA) of positive mode electrospray ionization mass spectrometric (ESIMS) and {sup 1}H nuclear magnetic resonance (NMR) data of crude extracts highlighted some species characterized by lignans (P. solmsianum, P. truncatum and P. cernuum), neolignans (P. regnellii) and chromenes (P. gaudichaudianum). A specific analysis focusing on species having pendant and globular inflorescences (P. caldense, P. carniconnectivum, P. bowiei and P. permucronatum) or amides-producing species indicated higher potential of the methodology in determining similarities and establishing priorities for further phytochemical investigation. Such intraspecific analysis applied to analyzed seedling leaves of the P. solmsianum, P. regnellii and P. gaudichaudianum species revealed the production of dillapiole and apiole instead of lignans, neolignans or prenylated benzoic acid, produced by the adult leaves, respectively. In case of amides-producing species, a similar profile was observed regardless the developmental stage. (author)

  1. Chemometric analysis of ESIMS and NMR data from Piper species

    International Nuclear Information System (INIS)

    Yamaguchi, Lydia F.; Freitas, Giovana C.; Yoshida, Nidia C.; Silva, Renata A.; Gaia, Anderson M.; Silva, Adalberto M.; Kato, Massuo J.; Emerenciano, Vicente de P.; Scotti, Marcus T.; Guimaraes, Elsie F.; Floh, Eny I.S.; Colombo, Carlos A.; Siqueira, Walter J.

    2011-01-01

    The metabolomic profiling based on the application of multivariate analysis (principal component analysis, PCA) of positive mode electrospray ionization mass spectrometric (ESIMS) and 1 H nuclear magnetic resonance (NMR) data of crude extracts highlighted some species characterized by lignans (P. solmsianum, P. truncatum and P. cernuum), neolignans (P. regnellii) and chromenes (P. gaudichaudianum). A specific analysis focusing on species having pendant and globular inflorescences (P. caldense, P. carniconnectivum, P. bowiei and P. permucronatum) or amides-producing species indicated higher potential of the methodology in determining similarities and establishing priorities for further phytochemical investigation. Such intraspecific analysis applied to analyzed seedling leaves of the P. solmsianum, P. regnellii and P. gaudichaudianum species revealed the production of dillapiole and apiole instead of lignans, neolignans or prenylated benzoic acid, produced by the adult leaves, respectively. In case of amides-producing species, a similar profile was observed regardless the developmental stage. (author)

  2. The PEC reactor. Safety analysis: Detailed reports

    Energy Technology Data Exchange (ETDEWEB)

    1988-01-01

    In the safety-analysis of the PEC Brasimone reactor (Italy), attention was focused on the role of plant-incident analysis during the design stage and the conclusions reached. The analysis regarded the following: thermohydraulic incidents at full power; incidents with the reactor shut down; reactivity incidents; core local faults; analysis of fuel-handling incidents; engineered safeguards and passive safety features; coolant leakage and sodium fires; research and development studies on the seismic behaviour of the PEC fast reactor; generalized sodium fire; severe accidents, accident sequences with shudown; reference accident. Both the theoretical and experimental analyses demonstrated the adequacy of the design of the PEC fast reactor, aimed at minimizing the consequences of a hypothetical disruptive core accident with mechanical energy release. It was shown that the containment barriers were sized correctly and that the residual heat from a disassembled core would be removed. The re-evaluation of the source term emphasized the conservative nature of the hypotheses assumed in the preliminary safety analysis for calculating the risk to the public.

  3. Detailed heart rate variability analysis in athletes.

    Science.gov (United States)

    Kiss, Orsolya; Sydó, Nóra; Vargha, Péter; Vágó, Hajnalka; Czimbalmos, Csilla; Édes, Eszter; Zima, Endre; Apponyi, Györgyi; Merkely, Gergő; Sydó, Tibor; Becker, Dávid; Allison, Thomas G; Merkely, Béla

    2016-08-01

    Heart rate variability (HRV) analysis has been used to evaluate patients with various cardiovascular diseases. While the vast majority of HRV studies have focused on pathological states, our study focuses on the less explored area of HRV analysis across different training intensity and sports. We aimed to measure HRV in healthy elite and masters athletes and compare to healthy, but non-athletic controls. Time-domain HRV analysis was applied in 138 athletes (male 110, age 28.4 ± 8.3) and 100 controls (male 56, age 28.3 ± 6.9) during Holter monitoring (21.3 ± 3.0 h). All studied parameters were higher in elite athletes compared to controls [SDNN (CI) 225.3 (216.2-234.5) vs 158.6 (150.2-167.1) ms; SDNN Index (CI) 99.6 (95.6-103.7) vs 72.4 (68.7-76.2) ms; pNN50 (CI) 24.2 (22.2-26.3) vs 14.4 (12.7-16.3) %; RMSSD (CI) 71.8 (67.6-76.2) vs 50.8 (46.9-54.8) ms; p HRV values than controls, but no significant differences were found between elite athletes and masters athletes. Some parameters were higher in canoeists-kayakers and bicyclists than runners. Lower cut-off values in elite athletes were SDNN: 147.4 ms, SDNN Index: 66.6 ms, pNN50: 9.7 %, RMSSD: 37.9 ms. Autonomic regulation in elite athletes described with HRV is significantly different than in healthy controls. Sports modality and level of performance, but not age- or sex-influenced HRV. Our study provides athletic normal HRV values. Further investigations are needed to determine its role in risk stratification, optimization of training, or identifying overtraining.

  4. Assessment of 1H NMR-based metabolomics analysis for normalization of urinary metals against creatinine.

    Science.gov (United States)

    Cassiède, Marc; Nair, Sindhu; Dueck, Meghan; Mino, James; McKay, Ryan; Mercier, Pascal; Quémerais, Bernadette; Lacy, Paige

    2017-01-01

    Proton nuclear magnetic resonance ( 1 H NMR, or NMR) spectroscopy and inductively coupled plasma-mass spectrometry (ICP-MS) are commonly used for metabolomics and metal analysis in urine samples. However, creatinine quantification by NMR for the purpose of normalization of urinary metals has not been validated. We assessed the validity of using NMR analysis for creatinine quantification in human urine samples in order to allow normalization of urinary metal concentrations. NMR and ICP-MS techniques were used to measure metabolite and metal concentrations in urine samples from 10 healthy subjects. For metabolite analysis, two magnetic field strengths (600 and 700MHz) were utilized. In addition, creatinine concentrations were determined by using the Jaffe method. Creatinine levels were strongly correlated (R 2 =0.99) between NMR and Jaffe methods. The NMR spectra were deconvoluted with a target database containing 151 metabolites that are present in urine. A total of 50 metabolites showed good correlation (R 2 =0.7-1.0) at 600 and 700MHz. Metal concentrations determined after NMR-measured creatinine normalization were comparable to previous reports. NMR analysis provided robust urinary creatinine quantification, and was sufficient for normalization of urinary metal concentrations. We found that NMR-measured creatinine-normalized urinary metal concentrations in our control subjects were similar to general population levels in Canada and the United Kingdom. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. Detailed Analysis of ECMWF Surface Pressure Data

    Science.gov (United States)

    Fagiolini, E.; Schmidt, T.; Schwarz, G.; Zenner, L.

    2012-04-01

    Investigations of temporal variations within the gravity field of the Earth led us to the analysis of common surface pressure data products delivered by ECMWF. We looked into the characteristics of global as well as spatially and temporally confined phenomena being visible in the data. In particular, we were interested in the overall data quality, the local and temporal signal-to-noise ratio of surface pressure data sets, and the identification of irregular data. To this end, we analyzed a time series of a full year of surface pressure operational analysis data and their nominal standard deviations. The use of pressure data on a Gaussian grid data allowed us to remain close to the internal computations at ECMWF during data assimilation. Thus, we circumvented potential interpolation effects that would otherwise occur in cylindrical projections of conventional map products. The results obtained by us demonstrate the identification of a few distinct outliers, data quality effects over land or water and along coastlines as well as neighborhood effects of samples within and outside of the tropics. Small scale neighborhood effects depend on their geographical direction, sampling distance, land or water, and local time. In addition, one notices large scale seasonal effects that are latitude and longitude dependent. As a consequence, we obtain a cause-and-effect survey of pressure data peculiarities. One can then use background corrected pressure data to analyze seasonal effects within given latitude belts. Here time series of pressure data allow the tracking of high and low pressure areas together with the identification of their actual extent, velocity and life time. This information is vital to overall mass transport calculations and the determination of temporally varying gravity fields. However, one has to note that the satellite and ground-based instruments and the assimilation software being used for the pressure calculations will not remain the same over the years

  6. Detailed NMR, Including 1,1-ADEQUATE, and Anticancer Studies of Compounds from the Echinoderm Colobometra perspinosa

    Directory of Open Access Journals (Sweden)

    Catherine H. Liptrot

    2009-11-01

    Full Text Available From the dichloromethane/methanol extract of the crinoid Colobometra perspinosa, collected south east of Richards Island (Bedara, Family Islands, Central Great Barrier Reef, Australia, 3-(1'-hydroxypropyl-1,6,8-trihydroxy-9,10-anthraquinone [one of the two stereoisomers of rhodoptilometrin, (1], 3-propyl-1,6,8-trihydroxy-9,10-anthraquinone (3, 2-[(phenylacetylamino]ethanesulfonic acid (4, and 4-hydroxybutanoic acid (5 were isolated. Comparison of 1H- and 13C-NMR data for rhodoptilometrin (1 with those reported in the literature showed significant differences for some resonances associated with rings A and C. In an attempt to provide accurately assigned 1H- and 13C-NMR data, as well as to confirm the structure of 1, a thorough NMR investigation of this compound was undertaken. Measurements included: concentration dependent 13C, 1D selective NOE, HSQC, HMBC and 1,1-ADEQUATE. The NMR data for 4 and 5 are reported here for the first time, as is their occurrence from the marine environment. The in vitro anticancer activity of the original extract was found to be associated with 1, 3 and 5.

  7. Functional Analysis of the Nitrogen Metabolite Repression Regulator Gene nmrA in Aspergillus flavus

    Directory of Open Access Journals (Sweden)

    Xiaoyun Han

    2016-11-01

    Full Text Available In Aspergillus nidulans, the nitrogen metabolite repression regulator NmrA plays a major role in regulating the activity of the GATA transcription factor AreA during nitrogen metabolism. However, the function of nmrA in Aspergillus flavus has notbeen previously studied. Here, we report the identification and functional analysis of nmrA in A. flavus. Our work showed that the amino acid sequences of NmrA are highly conserved among Aspergillus species and that A. flavus NmrA protein contains a canonical Rossmann fold motif. Deletion of nmrA slowed the growth of A. flavus but significantly increased conidiation and sclerotia production. Moreover, seed infection experiments indicated that nmrA is required for the invasive virulence of A. flavus. In addition, the ΔnmrA mutant showed increased sensitivity to rapamycin and methyl methanesulfonate, suggesting that nmrA could be responsive to target of rapamycin signaling and DNA damage. Furthermore, quantitative real-time reverse transcription polymerase chain reaction analysis suggested that nmrA might interact with other nitrogen regulatory and catabolic genes. Our study provides a better understanding of nitrogen metabolite repression and the nitrogen metabolism network in fungi.

  8. Isotopomer analysis of lipid biosynthesis by high resolution mass spectrometry and NMR

    Energy Technology Data Exchange (ETDEWEB)

    Lane, Andrew N., E-mail: anlane01@louisville.edu [JG Brown Cancer Center, 529 S. Jackson Street, Louisville, KY 40202 (United States); Center for Regulatory and Environmental Analytical Metabolomics (CREAM), University of Louisville, Louisville, KY (United States); Fan, Teresa W.-M. [JG Brown Cancer Center, 529 S. Jackson Street, Louisville, KY 40202 (United States); Center for Regulatory and Environmental Analytical Metabolomics (CREAM), University of Louisville, Louisville, KY (United States); Department of Chemistry, University of Louisville, Louisville, KY 40292 (United States); Xie, Zhengzhi; Moseley, Hunter N.B.; Higashi, Richard M. [Center for Regulatory and Environmental Analytical Metabolomics (CREAM), University of Louisville, Louisville, KY (United States); Department of Chemistry, University of Louisville, Louisville, KY 40292 (United States)

    2009-10-05

    We have coupled 2D-NMR and infusion FT-ICR-MS with computer-assisted assignment to profile {sup 13}C-isotopologues of glycerophospholipids (GPL) directly in crude cell extracts, resulting in very high information throughput of >3000 isobaric molecules in a few minutes. A mass accuracy of better than 1 ppm combined with a resolution of 100,000 at the measured m/z was required to distinguish isotopomers from other GPL structures. Isotopologue analysis of GPLs extracted from LCC2 breast cancer cells grown on [U-{sup 13}C]-glucose provided a rich trove of information about the biosynthesis and turnover of the GPLs. The isotopologue intensity ratios from the FT-ICR-MS were accurate to {approx}1% or better based on natural abundance background, and depended on the signal-to-nose ratio. The time course of incorporation of {sup 13}C from [U-{sup 13}C]-glucose into a particular phosphatidylcholine was analyzed in detail, to provide a quantitative measure of the sizes of glycerol, acetyl CoA and total GPL pools in growing LCC2 cells. Independent and complementary analysis of the positional {sup 13}C enrichment in the glycerol and fatty acyl chains obtained from high resolution 2D NMR was used to verify key aspects of the model. This technology enables simple and rapid sample preparation, has rapid analysis, and is generally applicable to unfractionated GPLs of almost any head group, and to mixtures of other classes of metabolites.

  9. Isotopomer analysis of lipid biosynthesis by high resolution mass spectrometry and NMR

    International Nuclear Information System (INIS)

    Lane, Andrew N.; Fan, Teresa W.-M.; Xie, Zhengzhi; Moseley, Hunter N.B.; Higashi, Richard M.

    2009-01-01

    We have coupled 2D-NMR and infusion FT-ICR-MS with computer-assisted assignment to profile 13 C-isotopologues of glycerophospholipids (GPL) directly in crude cell extracts, resulting in very high information throughput of >3000 isobaric molecules in a few minutes. A mass accuracy of better than 1 ppm combined with a resolution of 100,000 at the measured m/z was required to distinguish isotopomers from other GPL structures. Isotopologue analysis of GPLs extracted from LCC2 breast cancer cells grown on [U- 13 C]-glucose provided a rich trove of information about the biosynthesis and turnover of the GPLs. The isotopologue intensity ratios from the FT-ICR-MS were accurate to ∼1% or better based on natural abundance background, and depended on the signal-to-nose ratio. The time course of incorporation of 13 C from [U- 13 C]-glucose into a particular phosphatidylcholine was analyzed in detail, to provide a quantitative measure of the sizes of glycerol, acetyl CoA and total GPL pools in growing LCC2 cells. Independent and complementary analysis of the positional 13 C enrichment in the glycerol and fatty acyl chains obtained from high resolution 2D NMR was used to verify key aspects of the model. This technology enables simple and rapid sample preparation, has rapid analysis, and is generally applicable to unfractionated GPLs of almost any head group, and to mixtures of other classes of metabolites.

  10. On the structure of amorphous calcium carbonate--a detailed study by solid-state NMR spectroscopy.

    Science.gov (United States)

    Nebel, Holger; Neumann, Markus; Mayer, Christian; Epple, Matthias

    2008-09-01

    The calcium carbonate phases calcite, aragonite, vaterite, monohydrocalcite (calcium carbonate monohydrate), and ikaite (calcium carbonate hexahydrate) were studied by solid-state NMR spectroscopy ( (1)H and (13)C). Further model compounds were sodium hydrogencarbonate, potassium hydrogencarbonate, and calcium hydroxide. With the help of these data, the structure of synthetically prepared additive-free amorphous calcium carbonate (ACC) was analyzed. ACC contains molecular water (as H 2O), a small amount of mobile hydroxide, and no hydrogencarbonate. This supports the concept of ACC as a transient precursor in the formation of calcium carbonate biominerals.

  11. Reliability of ^1^H NMR analysis for assessment of lipid oxidation at frying temperatures

    Science.gov (United States)

    The reliability of a method using ^1^H NMR analysis for assessment of oil oxidation at a frying temperature was examined. During heating and frying at 180 °C, changes of soybean oil signals in the ^1^H NMR spectrum including olefinic (5.16-5.30 ppm), bisallylic (2.70-2.88 ppm), and allylic (1.94-2.1...

  12. Whole-core analysis by 13C NMR

    International Nuclear Information System (INIS)

    Vinegar, H.J.; Tutunjian, P.N.; Edelstein, W.A.; Roemer, P.B.

    1991-01-01

    This paper reports on a whole-core nuclear magnetic resonance (NMR) system that was used to obtain natural abundance 13 C spectra. The system enables rapid, nondestructive measurements of bulk volume of movable oil, aliphatic/aromatic ratio, oil viscosity, and organic vs. carbonate carbon. 13 C NMR can be used in cores where the 1 H NMR spectrum is too broad to resolve oil and water resonances separately. A 5 1/4-in. 13 C/ 1 H NMR coil was installed on a General Electric (GE) CSI-2T NMR imager/spectrometer. With a 4-in.-OD whole core, good 13 C signal/noise ratio (SNR) is obtained within minutes, while 1 H spectra are obtained in seconds. NMR measurements have been made of the 13 C and 1 H density of crude oils with a wide range of API gravities. For light- and medium-gravity oils, the 13 C and 1 H signal per unit volume is constant within about 3.5%. For heavy crudes, the 13 C and 1 H density measured by NMR is reduced by the shortening of spin-spin relaxation time. 13 C and 1 H NMR spin-lattice relaxation times were measured on a suite of Cannon viscosity standards, crude oils (4 to 60 degrees API), and alkanes (C 5 through C 16 ) with viscosities at 77 degrees F ranging from 0.5 cp to 2.5 x 10 7 cp. The 13 C and 1 H relaxation times show a similar correlation with viscosity from which oil viscosity can be estimated accurately for viscosities up to 100 cp. The 13 C surface relaxation rate for oils on water-wet rocks is very low. Nonproton decoupled 13 C NMR is shown to be insensitive to kerogen; thus, 13 C NMR measures only the movable hydrocarbon content of the cores. In carbonates, the 13 C spectrum also contains a carbonate powder pattern useful in quantifying inorganic carbon and distinguishing organic from carbonate carbon

  13. NMR/MS Translator for the Enhanced Simultaneous Analysis of Metabolomics Mixtures by NMR Spectroscopy and Mass Spectrometry: Application to Human Urine.

    Science.gov (United States)

    Bingol, Kerem; Brüschweiler, Rafael

    2015-06-05

    A novel metabolite identification strategy is presented for the combined NMR/MS analysis of complex metabolite mixtures. The approach first identifies metabolite candidates from 1D or 2D NMR spectra by NMR database query, which is followed by the determination of the masses (m/z) of their possible ions, adducts, fragments, and characteristic isotope distributions. The expected m/z ratios are then compared with the MS(1) spectrum for the direct assignment of those signals of the mass spectrum that contain information about the same metabolites as the NMR spectra. In this way, the mass spectrum can be assigned with very high confidence, and it provides at the same time validation of the NMR-derived metabolites. The method was first demonstrated on a model mixture, and it was then applied to human urine collected from a pool of healthy individuals. A number of metabolites could be detected that had not been reported previously, further extending the list of known urine metabolites. The new analysis approach, which is termed NMR/MS Translator, is fully automated and takes only a few seconds on a computer workstation. NMR/MS Translator synergistically uses the power of NMR and MS, enhancing the accuracy and efficiency of the identification of those metabolites compiled in databases.

  14. Complete 1H NMR spectral analysis of ten chemical markers of Ginkgo biloba

    OpenAIRE

    Napolitano, José G.; Lankin, David C.; Chen, Shao-Nong; Pauli, Guido F.

    2012-01-01

    The complete and unambiguous 1H NMR assignments of ten marker constituents of Ginkgo biloba are described. The comprehensive 1H NMR profiles (fingerprints) of ginkgolide A, ginkgolide B, ginkgolide C, ginkgolide J, bilobalide, quercetin, kaempferol, isorhamnetin, isoquercetin, and rutin in DMSO-d6 were obtained through the examination of 1D 1H NMR and 2D 1H,1H-COSY data, in combination with 1H iterative Full Spin Analysis (HiFSA). The computational analysis of discrete spin systems allowed a ...

  15. Variable-temperature NMR and conformational analysis of Oenothein B

    International Nuclear Information System (INIS)

    Santos, Suzana C.; Carvalho, Ariadne G.; Fortes, Gilmara A.C.; Ferri, Pedro H.; Oliveira, Anselmo E. de

    2014-01-01

    Oenothein B is a dimeric hydrolyzable tannin with a wide range of biological activities, such as antitumour, anti-inflammatory and antiviral. Its nuclear magnetic resonance (NMR) at room temperature show duplications and broadening of signals. Experiments of 1D and 2D NMR at lower temperatures were useful for the complete NMR assignments of all hydrogens and carbons. The 3D structure of the most stable conformer was determined for the first time by nuclear Overhauser effect spectroscopy (NOESY) experiment (-20 deg C) and density functional theory (DFT)(B3LYP/6-31G)/ polarizable continuum model (PCM) quantum chemical calculations. The favoured conformation showed a highly compacted geometry and a lack of symmetry, in which the two valoneoyl groups showed distinct conformational parameters and stabilities. (author)

  16. Variable-temperature NMR and conformational analysis of Oenothein B

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Suzana C.; Carvalho, Ariadne G.; Fortes, Gilmara A.C.; Ferri, Pedro H.; Oliveira, Anselmo E. de, [Universidade Federal de Goias (UFGO), Goiania, GO (Brazil). Instituto de Quimica

    2014-02-15

    Oenothein B is a dimeric hydrolyzable tannin with a wide range of biological activities, such as antitumour, anti-inflammatory and antiviral. Its nuclear magnetic resonance (NMR) at room temperature show duplications and broadening of signals. Experiments of 1D and 2D NMR at lower temperatures were useful for the complete NMR assignments of all hydrogens and carbons. The 3D structure of the most stable conformer was determined for the first time by nuclear Overhauser effect spectroscopy (NOESY) experiment (-20 deg C) and density functional theory (DFT)(B3LYP/6-31G)/ polarizable continuum model (PCM) quantum chemical calculations. The favoured conformation showed a highly compacted geometry and a lack of symmetry, in which the two valoneoyl groups showed distinct conformational parameters and stabilities. (author)

  17. NMR analysis of silk for the interpretation of ancient history

    International Nuclear Information System (INIS)

    Chujo, Riichiro

    1998-01-01

    The aim of this paper is the characterization of archaeological silk with the aid of nuclear magnetic resonance (NMR). In this paper the nucleus is confined to 13C as a stable isotope carbon which is the most basic element in organic compounds. Among the stable carbon isotopes 12C is the most abundant but it has no magnetic moment and the natural abundance of 13C is only 1.108% and this isotope is frequently used in NMR due to its non-zero magnetic moment

  18. Tritium NMR in the analysis of tritiated compounds

    International Nuclear Information System (INIS)

    Kaspersen, F.M.; Funke, C.W.; Vader, Jan; Wagenaars, G.N.

    1993-01-01

    An overview is given of the possibilities of 3 H NMR in the characterisation of 3 H-labelled compounds. This technique gives information on the identity of the tritiated compounds, the position of the tritium, the distribution of the label and even the radiochemical purity of the labelled products. (author)

  19. Statistical models and NMR analysis of polymer microstructure

    Science.gov (United States)

    Statistical models can be used in conjunction with NMR spectroscopy to study polymer microstructure and polymerization mechanisms. Thus, Bernoullian, Markovian, and enantiomorphic-site models are well known. Many additional models have been formulated over the years for additional situations. Typica...

  20. Analysis of organophosphorus pesticides using FT-NMR

    International Nuclear Information System (INIS)

    Miyata, Yoshihiko; Takahashi, Yoshikazu; Ando, Hiroaki

    1988-01-01

    A rapid and highly selective method of the identification of 23 kinds of organophosphorus pesticides was develop by using 31 P FT-NMR with 1 H complete decoupling method. Chemical shifts referenced by 85 % H 3 PO 4 were within -4 to 100 ppm, and there was no overlapping among the organophosphorus pesticides used in this experiment. (author)

  1. Implementation of picoSpin Benchtop NMR Instruments into Organic Chemistry Teaching Laboratories through Spectral Analysis of Fischer Esterification Products

    Science.gov (United States)

    Yearty, Kasey L.; Sharp, Joseph T.; Meehan, Emma K.; Wallace, Doyle R.; Jackson, Douglas M.; Morrison, Richard W.

    2017-01-01

    [Superscript 1]H NMR analysis is an important analytical technique presented in introductory organic chemistry courses. NMR instrument access is limited for undergraduate organic chemistry students due to the size of the instrument, price of NMR solvents, and the maintenance level required for instrument upkeep. The University of Georgia Chemistry…

  2. Comparative 1H NMR-based metabonomic analysis of HIV-1 sera

    International Nuclear Information System (INIS)

    Philippeos, C.; Steffens, F. E.; Meyer, D.

    2009-01-01

    1 H NMR spectroscopy of sera from HIV-1 infected and uninfected individuals was performed on 300 and 600 MHz instruments. The resultant spectra were automatically data reduced to 90 and 180 integral segments of equal length. Analysis of variance identified significant differences between the sample groups, especially for the samples analyzed on 600 MHz and reduced to fewer segments. Linear discriminant analysis correctly classified 100% of the samples analyzed on the 300 MHz NMR (reduced to 180 segments); an increase in instrument sensitivity resulted in lower percentages of correctly classified samples. Multinomial logistic regression (MLR) resulted in 100% correct classification of all samples from both instruments. Thus 1 H-NMR metabonomics on either instrument distinguishes HIV-positive individuals using or not using anti retroviral therapy, but the sensitivity of the instrument impacts on data reduction. Furthermore, MLR is a novel multivariate statistical technique for improved classification of biological data analyzed in NMR

  3. Comparative {sup 1}H NMR-based metabonomic analysis of HIV-1 sera

    Energy Technology Data Exchange (ETDEWEB)

    Philippeos, C. [University of Johannesburg, Department of Biochemistry (South Africa); Steffens, F. E. [University of Pretoria, Department of Statistics (South Africa); Meyer, D. [University of Pretoria, Department of Biochemistry (South Africa)], E-mail: debra.meyer@up.ac.za

    2009-07-15

    {sup 1}H NMR spectroscopy of sera from HIV-1 infected and uninfected individuals was performed on 300 and 600 MHz instruments. The resultant spectra were automatically data reduced to 90 and 180 integral segments of equal length. Analysis of variance identified significant differences between the sample groups, especially for the samples analyzed on 600 MHz and reduced to fewer segments. Linear discriminant analysis correctly classified 100% of the samples analyzed on the 300 MHz NMR (reduced to 180 segments); an increase in instrument sensitivity resulted in lower percentages of correctly classified samples. Multinomial logistic regression (MLR) resulted in 100% correct classification of all samples from both instruments. Thus {sup 1}H-NMR metabonomics on either instrument distinguishes HIV-positive individuals using or not using anti retroviral therapy, but the sensitivity of the instrument impacts on data reduction. Furthermore, MLR is a novel multivariate statistical technique for improved classification of biological data analyzed in NMR.

  4. Two-dimensional NMR spectroscopy strongly enhances soil organic matter composition analysis

    Science.gov (United States)

    Soucemarianadin, Laure; Erhagen, Björn; Öquist, Mats; Nilsson, Mats; Hedenström, Mattias; Schleucher, Jürgen

    2016-04-01

    Soil organic matter (SOM) is the largest terrestrial carbon pool and strongly affects soil properties. With climate change, understanding SOM processes and turnover and how they could be affected by increasing temperatures becomes critical. This is particularly key for organic soils as they represent a huge carbon pool in very sensitive ecosystems, like boreal ecosystems and peatlands. Nevertheless, characterization of SOM molecular composition, which is essential to elucidate soil carbon processes, is not easily achieved, and further advancements in that area are greatly needed. Solid-state one-dimensional (1D) 13C nuclear magnetic resonance (NMR) spectroscopy is often used to characterize its molecular composition, but only provides data on a few major functional groups, which regroup many different molecular fragments. For instance, in the carbohydrates region, signals of all monosaccharides present in many different polymers overlap. This overlap thwarts attempts to identify molecular moieties, resulting in insufficient information to characterize SOM composition. Here we show that two-dimensional (2D) liquid-state 1H-13C NMR spectra provided much richer data on the composition of boreal plant litter and organic surface soil. The 2D spectra indeed resolved overlaps observed in 1D 13C spectra and displayed signals from hundreds of identifiable molecular groups. For example, in the aromatics region, signals from individual lignin units could be recognized. It was hence possible to follow the fate of specific structural moieties in soils. We observed differences between litter and soil samples, and were able to relate them to the decomposition of identifiable moieties. Sample preparation and data acquisition were both simple and fast. Further, using multivariate data analysis, we aimed at linking the detailed chemical fingerprints of SOM to turnover rates in a soil incubation experiment. With the multivariate models, we were able to identify specific molecular

  5. Analysis of local influences in structural details of the bridges

    Directory of Open Access Journals (Sweden)

    Adam RUDZIK

    2015-03-01

    Full Text Available The article analyses the problems of local influences in structural details of bridges as the critical locations, whose damages or excessive force may directly affect the safety of users. These analyses are shown on selected examples. Presented is the example of local changes in the forms of proper vibrations in the node of the truss bridge that can be used in expert issues concerning the causes of damages. The second example are the changes in stresses in the stay cable anchorage element including the nonlinear material models. Models of this type can be successfully used by engineers as they allow for analysis of selected structural details without the need for detailed mapping of the entire structure, but only a selected section.

  6. NMR imaging: A 'chemical' microscope for coal analysis

    International Nuclear Information System (INIS)

    French, D.C.; Dieckman, S.L.; Gopalsami, N.; Botto, R.E.

    1991-01-01

    This paper presents a new three-dimensional (3-D) nuclear magnetic resonance (NMR) imaging technique for spatially mapping proton distributions in whole coals and solvent-swollen coal samples. The technique is based on a 3-D back-projection protocol for data acquisition, and a reconstruction technique based on 3-D Radon transform inversion. In principle, the 3-D methodology provides higher spatial resolution of solid materials than is possible with conventional slice-selection protocols. The applicability of 3-D NMR imaging has been demonstrated by mapping the maceral phases in Utah Blind Canyon (APCS number-sign 6) coal and the distribution of mobile phases in Utah coal swollen with deuterated and protic pyridine. 7 refs., 5 figs

  7. Application of NMR Spectroscopy in the Analysis of Petroleum Derivatives and Products

    Directory of Open Access Journals (Sweden)

    Parlov Vuković, J.

    2012-11-01

    Full Text Available Complex chemical composition and physical properties of oil and fuel make their complete cha racterization very difficult. Components present in oil and oil products differ in structure, size, po larity and functionality. The presence and structure of specific hydrocarbons in final products depend on the processing procedure and type of the fuel. In order to predict or improve fuel pro perties it is necessary to determine its composition. Thus, new and more sophisticated analytical methods and procedures are constantly being developed. NMR spectroscopy plays a significant role in analysis and identification of complex hydrocarbon mixtures of petroleum and petroleum products. In this review, we describe the application of NMR spectroscopy for analyzing gasoline and diesel fuels. Hence, by using NMR spectroscopy it is possible to determine gasoline composition and presence of benzene and oxygenates, as well as some important physical characteristics of gasoli ne such as the research octane number. An application of different NMR techniques made it pos sible to characterize diesel fuels and middle oil distillates from various refineries. Data so obtained can be used in combination with statistical methods to predict fuel properties and to monitor pro- duction processes in the petroleum industry. NMR spectroscopy has proven useful in analysis of FAME which has recently been used as an ecologically acceptable alternative fuel. Furthermore, techniques such as CP/MAS for characterization of solid state oil-geochemical samples are inclu- ded. Also, possibilities of using NMR spectroscopy in the analysis of polymeric additives are di- scussed.

  8. Automics: an integrated platform for NMR-based metabonomics spectral processing and data analysis

    Directory of Open Access Journals (Sweden)

    Qu Lijia

    2009-03-01

    Full Text Available Abstract Background Spectral processing and post-experimental data analysis are the major tasks in NMR-based metabonomics studies. While there are commercial and free licensed software tools available to assist these tasks, researchers usually have to use multiple software packages for their studies because software packages generally focus on specific tasks. It would be beneficial to have a highly integrated platform, in which these tasks can be completed within one package. Moreover, with open source architecture, newly proposed algorithms or methods for spectral processing and data analysis can be implemented much more easily and accessed freely by the public. Results In this paper, we report an open source software tool, Automics, which is specifically designed for NMR-based metabonomics studies. Automics is a highly integrated platform that provides functions covering almost all the stages of NMR-based metabonomics studies. Automics provides high throughput automatic modules with most recently proposed algorithms and powerful manual modules for 1D NMR spectral processing. In addition to spectral processing functions, powerful features for data organization, data pre-processing, and data analysis have been implemented. Nine statistical methods can be applied to analyses including: feature selection (Fisher's criterion, data reduction (PCA, LDA, ULDA, unsupervised clustering (K-Mean and supervised regression and classification (PLS/PLS-DA, KNN, SIMCA, SVM. Moreover, Automics has a user-friendly graphical interface for visualizing NMR spectra and data analysis results. The functional ability of Automics is demonstrated with an analysis of a type 2 diabetes metabolic profile. Conclusion Automics facilitates high throughput 1D NMR spectral processing and high dimensional data analysis for NMR-based metabonomics applications. Using Automics, users can complete spectral processing and data analysis within one software package in most cases

  9. Automics: an integrated platform for NMR-based metabonomics spectral processing and data analysis.

    Science.gov (United States)

    Wang, Tao; Shao, Kang; Chu, Qinying; Ren, Yanfei; Mu, Yiming; Qu, Lijia; He, Jie; Jin, Changwen; Xia, Bin

    2009-03-16

    Spectral processing and post-experimental data analysis are the major tasks in NMR-based metabonomics studies. While there are commercial and free licensed software tools available to assist these tasks, researchers usually have to use multiple software packages for their studies because software packages generally focus on specific tasks. It would be beneficial to have a highly integrated platform, in which these tasks can be completed within one package. Moreover, with open source architecture, newly proposed algorithms or methods for spectral processing and data analysis can be implemented much more easily and accessed freely by the public. In this paper, we report an open source software tool, Automics, which is specifically designed for NMR-based metabonomics studies. Automics is a highly integrated platform that provides functions covering almost all the stages of NMR-based metabonomics studies. Automics provides high throughput automatic modules with most recently proposed algorithms and powerful manual modules for 1D NMR spectral processing. In addition to spectral processing functions, powerful features for data organization, data pre-processing, and data analysis have been implemented. Nine statistical methods can be applied to analyses including: feature selection (Fisher's criterion), data reduction (PCA, LDA, ULDA), unsupervised clustering (K-Mean) and supervised regression and classification (PLS/PLS-DA, KNN, SIMCA, SVM). Moreover, Automics has a user-friendly graphical interface for visualizing NMR spectra and data analysis results. The functional ability of Automics is demonstrated with an analysis of a type 2 diabetes metabolic profile. Automics facilitates high throughput 1D NMR spectral processing and high dimensional data analysis for NMR-based metabonomics applications. Using Automics, users can complete spectral processing and data analysis within one software package in most cases. Moreover, with its open source architecture, interested

  10. Graphical analysis of NMR structural quality and interactive contact map of NOE assignments in ARIA

    Directory of Open Access Journals (Sweden)

    Malliavin Thérèse E

    2008-06-01

    Full Text Available Abstract Background The Ambiguous Restraints for Iterative Assignment (ARIA approach is widely used for NMR structure determination. It is based on simultaneously calculating structures and assigning NOE through an iterative protocol. The final solution consists of a set of conformers and a list of most probable assignments for the input NOE peak list. Results ARIA was extended with a series of graphical tools to facilitate a detailed analysis of the intermediate and final results of the ARIA protocol. These additional features provide (i an interactive contact map, serving as a tool for the analysis of assignments, and (ii graphical representations of structure quality scores and restraint statistics. The interactive contact map between residues can be clicked to obtain information about the restraints and their contributions. Profiles of quality scores are plotted along the protein sequence, and contact maps provide information of the agreement with the data on a residue pair level. Conclusion The graphical tools and outputs described here significantly extend the validation and analysis possibilities of NOE assignments given by ARIA as well as the analysis of the quality of the final structure ensemble. These tools are included in the latest version of ARIA, which is available at http://aria.pasteur.fr. The Web site also contains an installation guide, a user manual and example calculations.

  11. Cask crush pad analysis using detailed and simplified analysis methods

    International Nuclear Information System (INIS)

    Uldrich, E.D.; Hawkes, B.D.

    1997-01-01

    A crush pad has been designed and analyzed to absorb the kinetic energy of a hypothetically dropped spent nuclear fuel shipping cask into a 44-ft. deep cask unloading pool at the Fluorinel and Storage Facility (FAST). This facility, located at the Idaho Chemical Processing Plant (ICPP) at the Idaho national Engineering and Environmental Laboratory (INEEL), is a US Department of Energy site. The basis for this study is an analysis by Uldrich and Hawkes. The purpose of this analysis was to evaluate various hypothetical cask drop orientations to ensure that the crush pad design was adequate and the cask deceleration at impact was less than 100 g. It is demonstrated herein that a large spent fuel shipping cask, when dropped onto a foam crush pad, can be analyzed by either hand methods or by sophisticated dynamic finite element analysis using computer codes such as ABAQUS. Results from the two methods are compared to evaluate accuracy of the simplified hand analysis approach

  12. Structural analysis of the carbohydrate chains of glycoproteins by 500-MHz 1H-NMR spectroscopy

    International Nuclear Information System (INIS)

    Mutsaers, J.H.G.M.

    1986-01-01

    This thesis deals with the structural analysis by 500-MHz 1 H-NMR spectroscopy of carbohydrate chains obtained from glycoproteins. In the chapters 1 to 6 the structural analysis of N-glycosidically linked carbohydrate chains is described. The chapters 7 to 10 describe the structural analysis of O-glycosidically linked carbohydrate chains. 381 refs.; 44 figs.; 24 tabs.; 7 schemes

  13. NMR-based approach to the analysis of radiopharmaceuticals: radiochemical purity, specific activity, and radioactive concentration values by proton and tritium NMR spectroscopy.

    Science.gov (United States)

    Schenk, David J; Dormer, Peter G; Hesk, David; Pollack, Scott R; Lavey, Carolee Flader

    2015-06-15

    Compounds containing tritium are widely used across the drug discovery and development landscape. These materials are widely utilized because they can be efficiently synthesized and produced at high specific activity. Results from internally calibrated (3)H and (1)H nuclear magnetic resonance (NMR) spectroscopy suggests that at least in some cases, this calibrated approach could supplement or potentially replace radio-high-performance liquid chromatography for radiochemical purity, dilution and scintillation counting for the measurement of radioactivity per volume, and liquid chromatography/mass spectrometry analysis for the determination of specific activity. In summary, the NMR-derived values agreed with those from the standard approaches to within 1% to 9% for solution count and specific activity. Additionally, the NMR-derived values for radiochemical purity deviated by less than 5%. A benefit of this method is that these values may be calculated at the same time that (3)H NMR analysis provides the location and distribution of tritium atoms within the molecule. Presented and discussed here is the application of this method, advantages and disadvantages of the approach, and a rationale for utilizing internally calibrated (1)H and (3)H NMR spectroscopy for specific activity, radioactive concentration, and radiochemical purity whenever acquiring (3)H NMR for tritium location. Copyright © 2015 John Wiley & Sons, Ltd.

  14. CASD-NMR 2: robust and accurate unsupervised analysis of raw NOESY spectra and protein structure determination with UNIO

    International Nuclear Information System (INIS)

    Guerry, Paul; Duong, Viet Dung; Herrmann, Torsten

    2015-01-01

    UNIO is a comprehensive software suite for protein NMR structure determination that enables full automation of all NMR data analysis steps involved—including signal identification in NMR spectra, sequence-specific backbone and side-chain resonance assignment, NOE assignment and structure calculation. Within the framework of the second round of the community-wide stringent blind NMR structure determination challenge (CASD-NMR 2), we participated in two categories of CASD-NMR 2, namely using either raw NMR spectra or unrefined NOE peak lists as input. A total of 15 resulting NMR structure bundles were submitted for 9 out of 10 blind protein targets. All submitted UNIO structures accurately coincided with the corresponding blind targets as documented by an average backbone root mean-square deviation to the reference proteins of only 1.2 Å. Also, the precision of the UNIO structure bundles was virtually identical to the ensemble of reference structures. By assessing the quality of all UNIO structures submitted to the two categories, we find throughout that only the UNIO–ATNOS/CANDID approach using raw NMR spectra consistently yielded structure bundles of high quality for direct deposition in the Protein Data Bank. In conclusion, the results obtained in CASD-NMR 2 are another vital proof for robust, accurate and unsupervised NMR data analysis by UNIO for real-world applications

  15. KUJIRA, a package of integrated modules for systematic and interactive analysis of NMR data directed to high-throughput NMR structure studies

    International Nuclear Information System (INIS)

    Kobayashi, Naohiro; Iwahara, Junji; Koshiba, Seizo; Tomizawa, Tadashi; Tochio, Naoya; Guentert, Peter; Kigawa, Takanori; Yokoyama, Shigeyuki

    2007-01-01

    The recent expansion of structural genomics has increased the demands for quick and accurate protein structure determination by NMR spectroscopy. The conventional strategy without an automated protocol can no longer satisfy the needs of high-throughput application to a large number of proteins, with each data set including many NMR spectra, chemical shifts, NOE assignments, and calculated structures. We have developed the new software KUJIRA, a package of integrated modules for the systematic and interactive analysis of NMR data, which is designed to reduce the tediousness of organizing and manipulating a large number of NMR data sets. In combination with CYANA, the program for automated NOE assignment and structure determination, we have established a robust and highly optimized strategy for comprehensive protein structure analysis. An application of KUJIRA in accordance with our new strategy was carried out by a non-expert in NMR structure analysis, demonstrating that the accurate assignment of the chemical shifts and a high-quality structure of a small protein can be completed in a few weeks. The high completeness of the chemical shift assignment and the NOE assignment achieved by the systematic analysis using KUJIRA and CYANA led, in practice, to increased reliability of the determined structure

  16. Mixture analysis by long-range J-resolved 2D NMR

    International Nuclear Information System (INIS)

    Ha, S.T.K.; Lee, R.W.K.; Wilkins, C.L.

    1987-01-01

    In most spectroscopic qualitative analyses chromatographic separations are done before identification. Unfortunately, this general approach has suffered from a number of shortcomings. Off-line chromatographic separation followed by spectroscopic analysis is time consuming and inefficient and on-line analysis suffers from mismatch of the material flow requirements between chromatographic columns and spectroscopic instruments. An alternative mixture identification procedure solely based upon use of edited 13 C NMR spectra and a 13 C NMR chemical shift data base is reported. This approach has been demonstrated in the analyses of several mixtures, including a mixture of amino acids and some isomers. In all cases, identifications of components of these mixtures are successful

  17. Analysis of the structural quality of the CASD-NMR 2013 entries

    Energy Technology Data Exchange (ETDEWEB)

    Ragan, Timothy J.; Fogh, Rasmus H. [University of Leicester, Department of Biochemistry, School of Biological Sciences (United Kingdom); Tejero, Roberto [Universidad de Valencia, Departamento de Química Física (Spain); Vranken, Wim [Vrije Universiteit Brussel, Structural Biology Brussels (Belgium); Montelione, Gaetano T. [Rutgers, The State University of New Jersey, Center for Advanced Biotechnology and Medicine, Department of Molecular Biology and Biochemistry, and Northeast Structural Genomics Consortium (United States); Rosato, Antonio [University of Florence, Magnetic Resonance Center, Department of Chemistry (Italy); Vuister, Geerten W., E-mail: gv29@le.ac.uk [University of Leicester, Department of Biochemistry, School of Biological Sciences (United Kingdom)

    2015-08-15

    We performed a comprehensive structure validation of both automated and manually generated structures of the 10 targets of the CASD-NMR-2013 effort. We established that automated structure determination protocols are capable of reliably producing structures of comparable accuracy and quality to those generated by a skilled researcher, at least for small, single domain proteins such as the ten targets tested. The most robust results appear to be obtained when NOESY peak lists are used either as the primary input data or to augment chemical shift data without the need to manually filter such lists. A detailed analysis of the long-range NOE restraints generated by the different programs from the same data showed a surprisingly low degree of overlap. Additionally, we found that there was no significant correlation between the extent of the NOE restraint overlap and the accuracy of the structure. This result was surprising given the importance of NOE data in producing good quality structures. We suggest that this could be explained by the information redundancy present in NOEs between atoms contained within a fixed covalent network.

  18. Thermal and structural analysis of a cryogenic conduction cooling system for a HTS NMR magnet

    Energy Technology Data Exchange (ETDEWEB)

    In, Se Hwan; Hong, Yong Jun; Yeom, Han Kil; Ko, Hyo Bong; Park, Seong Je [Korea Institute of Machinery and Materials, Daejeon (Korea, Republic of)

    2016-03-15

    The superconducting NMR magnets have used cryogen such as liquid helium for their cooling. The conduction cooling method using cryocoolers, however, makes the cryogenic cooling system for NMR magnets more compact and user-friendly than the cryogen cooling method. This paper describes the thermal and structural analysis of a cryogenic conduction cooling system for a 400 MHz HTS NMR magnet, focusing on the magnet assembly. The highly thermo-conductive cooling plates between HTS double pancake coils are used to transfer the heat generated in coils, namely Joule heating at lap splice joints, to thermal link blocks and finally the cryocooler. The conduction cooling structure of the HTS magnet assembly preliminarily designed is verified by thermal and structural analysis. The orthotropic thermal properties of the HTS coil, thermal contact resistance and radiation heat load are considered in the thermal analysis. The thermal analysis confirms the uniform temperature distribution for the present thermal design of the NMR magnet within 0.2 K. The mechanical stress and the displacement by the electromagnetic force and the thermal contraction are checked to verify structural stability. The structural analysis indicates that the mechanical stress on each component of the magnet is less than its material yield strength and the displacement is acceptable in comparison with the magnet dimension.

  19. Simultaneous analysis of amino acid and organic acid by NMR spectrometry, 2

    International Nuclear Information System (INIS)

    Koda, Naoya; Yamaguchi, Shuichi; Mori, Takeshi.

    1987-01-01

    Analysis of urine from patients with inborn error of metabolism were studied by 1 H-nuclear magnetic resonance (NMR) spectrometry. Diseases studied were as follows; phenylketonuria, biotin responsive multiple carboxylase deficiency, non-ketotic hyperglycinemia, 3-ketothiolase deficiency, alkaptonuria, methylmalonic acidemia, isovaleric acidemia, glutaric aciduria, argininosuccinic aciduria and hyperornithinemia. In each disease, specific metabolites in urine were recognized by NMR spectrometry. This method is accomplished within 10 minutes with non-treated small volume of urine and will be successfully available for the screening and/or diagnosis of inherited metabolic diseases of amino acid and organic acid. (author)

  20. Detailed analysis of the KAERI nTOF facility

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Jong Woon; Lee, Young Ouk [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

    2016-06-15

    A project for building a neutron time-of-flight (nTOF) facility is progressing. We expect that the construction will start in early 2016. Before that, a detailed simulation based on the current architectural drawings was performed to optimize the performance of our facility. Currently, several parts had been modified or changed from the original design to reflect requirements such as the layout of the electron beam line, shape of the vacuum chamber producing a neutron beam, and the underground layout of the nTOF facility. Detailed analysis for these modifications has been done with MCNP simulation. An overview of our photo-neutron source and KAERI nTOF facility were introduced. The numerical simulations for heat deposition, source term, and radiation shielding of KAERI nTOF facility were performed and the results are discussed. We are expecting that the construction of the KAERI nTOF facility will start in early 2016, and these results will be used as basic data.

  1. Analysis of human muscle extracts by proton NMR

    International Nuclear Information System (INIS)

    Venkatasubramanian, P.N.; Barany, M.; Arus, C.

    1986-01-01

    Perchloric acid extracts were prepared from pooled human muscle biopsies from patients diagnosed with scoliosis (SCOL) and cerebral palsy (CP). After neutralization with KOH and removal of perchlorate, the extracts were concentrated by freeze drying and dissolved in 2 H 2 O to contain 120 O.D. units at 280 nm per 0.5 ml. 1 H NMR spectroscopy was performed with the 5 mm probe of a Varian XL300 instrument. Creatine, lactate, carnosine, and choline were the major resonances in the one-dimensional spectra of both extracts. With creatine as reference, 2.5-fold more lactate was found in SCOL than in CP, and a much smaller difference was also found in their carnosine content. Two-dimensional COSY comparison revealed several differences between the two extracts. Taurine, N-acetyl glutamate, glycerophosphoryl choline (or phosphoryl choline) and an unidentified spot were present only in the extract from SCOL but not in that from CP. On the other hand, aspartate, hydroxy-proline, carnitine and glycerophosphoryl ethanolamine were only present in CP but absent in SCOL. Alanine, cysteine, lysine and arginine appeared in both extracts without an apparent intensity difference

  2. Implementation of the NMR CHEmical Shift Covariance Analysis (CHESCA): A Chemical Biologist's Approach to Allostery.

    Science.gov (United States)

    Boulton, Stephen; Selvaratnam, Rajeevan; Ahmed, Rashik; Melacini, Giuseppe

    2018-01-01

    Mapping allosteric sites is emerging as one of the central challenges in physiology, pathology, and pharmacology. Nuclear Magnetic Resonance (NMR) spectroscopy is ideally suited to map allosteric sites, given its ability to sense at atomic resolution the dynamics underlying allostery. Here, we focus specifically on the NMR CHEmical Shift Covariance Analysis (CHESCA), in which allosteric systems are interrogated through a targeted library of perturbations (e.g., mutations and/or analogs of the allosteric effector ligand). The atomic resolution readout for the response to such perturbation library is provided by NMR chemical shifts. These are then subject to statistical correlation and covariance analyses resulting in clusters of allosterically coupled residues that exhibit concerted responses to the common set of perturbations. This chapter provides a description of how each step in the CHESCA is implemented, starting from the selection of the perturbation library and ending with an overview of different clustering options.

  3. A simple protocol for NMR analysis of the enantiomeric purity of chiral hydroxylamines.

    Science.gov (United States)

    Tickell, David A; Mahon, Mary F; Bull, Steven D; James, Tony D

    2013-02-15

    A practically simple three-component chiral derivatization protocol for determining the enantiopurity of chiral hydroxylamines by (1)H NMR spectroscopic analysis is described, involving their treatment with 2-formylphenylboronic acid and enantiopure BINOL to afford a mixture of diastereomeric nitrono-boronate esters whose ratio is an accurate reflection of the enantiopurity of the parent hydroxylamine.

  4. Detailed analysis of the scope of the modified Firsov model

    International Nuclear Information System (INIS)

    Cruz, S.A.; Vargas-Aburto, C.; Brice, D.K.; Alonso, E.V.; Armour, D.G.

    1983-01-01

    A detailed and systematic analysis of the scope of the Firsov model as modified by Cheshire when no adjustable parameters are included in the calculations of the low-velocity electronic-stopping cross section is presented. For this purpose we summarize and extend our previously reported [Radiat. Eff. Lett. 43, 79 (1979); Nucl. Instrum. Methods 170, 205 (1980)] preliminary results on the role of all computational degrees of freedom that influence the outcome of the calculations, namely, (a) inclusion of trajectory, (b) accuracy of wave functions and speed of atomic electrons, (c) motion of Firsov's plane, and (d) consideration of experimental conditions. We find that the Firsov theory is accurate only within a factor of 2; therefore, at least a scale factor is necessary in order to get reasonable agreement with experiment

  5. Detail analysis of fusion neutronics benchmark experiment on beryllium

    International Nuclear Information System (INIS)

    Konno, Chikara; Ochiai, Kentaro; Takakura, Kosuke; Ohnishi, Seiki; Kondo, Keitaro; Wada, Masayuki; Sato, Satoshi

    2010-01-01

    Our previous analysis of the integral experiments (in situ and TOF experiments) on beryllium with DT neutrons at JAEA/FNS pointed out two problems by using MCNP4C and the latest nuclear data libraries; one was a strange larger neutron peak around 12 MeV appearing in the TOF experiment analysis with JEFF-3.1 and the other was an overestimation on law energy neutrons in the in situ experiment analyses with all the nuclear data libraries. We investigated reasons for these problems in detail. It was found out that the official ACE file MCJEFF3.1 of JEFF-3.1 had an inconsistency with the original JEFF-3.1, which caused the strange larger neutron peak around 12 MeV in the TOF experiment analysis. We also found out that the calculated thermal neutron peak was probably too large in the in situ experiment. On trial we examined influence of the thermal neutron scattering law data of beryllium metal in ENDF/B-VI. The result pointed out that the coherent elastic scattering cross-section data in the thermal neutron scattering law data of beryllium metal were probably too large.

  6. Conformational analysis of amide extractants by NMR in organic phase

    International Nuclear Information System (INIS)

    Berthon, C.

    1993-08-01

    This study deals with nuclear fuel reprocessing. We have essentially used NMR spectroscopy. We want to understand which kind of conformational parameters control selectivity and efficiency of amide extractant. The symmetric monoamides used are DOBA (C 3 H 7 CON (CH 2 CH(C 2 H 5 ) C 4 H 9 ) 2 ), DOiBA ((CH 3 ) 2 CCHON (CH 2 CH(C 2 H 5 )C 4 H 9 ) 2 ) and DOTA ((CH 3 ) 3 CCH 2 CON(CH 2 CH(C 2 H 5 )C 4 H 9 ) 2 ). Each gives two quasi equivalent conformers (cis and trans) in organic phases. The selected malonamide DMDBTDMA ((C 4 H 9 (CH 3 )NCO) 2 CHC 14 H 29 ) has four conformers because of its twice disymmetric amide functions. Weak interactions between monoamides which yield to dimer formation. The malonamide also gives dimers but forms aggregates too. Nitric acid extraction is due to the competitive formation of six species L, L 2 , L 2 (HNO 3 ), L(HNO 3 ), L(HNO 3 ) 2 , L(HNO 3 ) 3 (L: monoamide). Complexation between lanthanides (III) and monoamides yields to the stoichiometries L 3 Ln(NO 3 ) 3 and L 2 Ln(NO 3 ) 3 . Their ratio depend of steric hindrance on the carbonyl and the metal ionic radius. The same thing is observed of Pu 4+ and Th 4+ extraction in non acidic media. L 2 An(NO 3 ) 4 is the main stoichiometric except for the Th 4+ - DOBA system where the species (DOBA) 3 Th(NO 3 ) 4 appear. Exchange rates between the ligand and the complex are pointed out. The monoamide conformations obtained with lanthanide and plutonium nitrate can explain the difference in extracting power of this molecule between An 4+ and Ln 3+ . (author). 162 refs., 87 figs., 44 tabs., 7 annexes

  7. Analysis of Fatigue Crack Growth in Ship Structural Details

    Directory of Open Access Journals (Sweden)

    Leheta Heba W.

    2016-04-01

    Full Text Available Fatigue failure avoidance is a goal that can be achieved only if the fatigue design is an integral part of the original design program. The purpose of fatigue design is to ensure that the structure has adequate fatigue life. Calculated fatigue life can form the basis for meaningful and efficient inspection programs during fabrication and throughout the life of the ship. The main objective of this paper is to develop an add-on program for the analysis of fatigue crack growth in ship structural details. The developed program will be an add-on script in a pre-existing package. A crack propagation in a tanker side connection is analyzed by using the developed program based on linear elastic fracture mechanics (LEFM and finite element method (FEM. The basic idea of the developed application is that a finite element model of this side connection will be first analyzed by using ABAQUS and from the results of this analysis the location of the highest stresses will be revealed. At this location, an initial crack will be introduced to the finite element model and from the results of the new crack model the direction of the crack propagation and the values of the stress intensity factors, will be known. By using the calculated direction of propagation a new segment will be added to the crack and then the model is analyzed again. The last step will be repeated until the calculated stress intensity factors reach the critical value.

  8. Detailed 3-D nuclear analysis of ITER outboard blanket modules

    International Nuclear Information System (INIS)

    Bohm, Tim; Davis, Andrew; Sawan, Mohamed; Marriott, Edward; Wilson, Paul; Ulrickson, Michael; Bullock, James

    2015-01-01

    Highlights: • Nuclear analysis was performed on detailed CAD models placed in a 40 degree model of ITER. • The regions examined include BM09, the upper ELM coil region (BM11–13), the neutral beam (NB) region (BM13–16), and BM18. • The results show that VV nuclear heating exceeds limits in the NB and upper ELM coil regions. • The results also show that the level of He production in parts of BM18 exceeds limits. • These calculations are being used to modify the design of the ITER blanket modules. - Abstract: In the ITER design, the blanket modules (BM) provide thermal and nuclear shielding for the vacuum vessel (VV), magnets, and other components. We used the CAD based DAG-MCNP5 transport code to analyze detailed models inserted into a 40 degree partially homogenized ITER global model. The regions analyzed include BM09, BM16 near the heating neutral beam injection (HNB) region, BM11–13 near the upper ELM coil region, and BM18. For the BM16 HNB region, the VV nuclear heating behind the NB region exceeds the design limit by up to 80%. For the BM11–13 region, the nuclear heating of the VV exceeds the design limit by up to 45%. For BM18, the results show that He production does not meet the limit necessary for re-welding. The results presented in this work are being used by the ITER Organization Blanket and Tokamak Integration groups to modify the BM design in the cases where limits are exceeded.

  9. Detailed 3-D nuclear analysis of ITER outboard blanket modules

    Energy Technology Data Exchange (ETDEWEB)

    Bohm, Tim, E-mail: tdbohm@wisc.edu [Fusion Technology Institute, University of Wisconsin-Madison, Madison, WI (United States); Davis, Andrew; Sawan, Mohamed; Marriott, Edward; Wilson, Paul [Fusion Technology Institute, University of Wisconsin-Madison, Madison, WI (United States); Ulrickson, Michael; Bullock, James [Formerly, Fusion Technology, Sandia National Laboratories, Albuquerque, NM (United States)

    2015-10-15

    Highlights: • Nuclear analysis was performed on detailed CAD models placed in a 40 degree model of ITER. • The regions examined include BM09, the upper ELM coil region (BM11–13), the neutral beam (NB) region (BM13–16), and BM18. • The results show that VV nuclear heating exceeds limits in the NB and upper ELM coil regions. • The results also show that the level of He production in parts of BM18 exceeds limits. • These calculations are being used to modify the design of the ITER blanket modules. - Abstract: In the ITER design, the blanket modules (BM) provide thermal and nuclear shielding for the vacuum vessel (VV), magnets, and other components. We used the CAD based DAG-MCNP5 transport code to analyze detailed models inserted into a 40 degree partially homogenized ITER global model. The regions analyzed include BM09, BM16 near the heating neutral beam injection (HNB) region, BM11–13 near the upper ELM coil region, and BM18. For the BM16 HNB region, the VV nuclear heating behind the NB region exceeds the design limit by up to 80%. For the BM11–13 region, the nuclear heating of the VV exceeds the design limit by up to 45%. For BM18, the results show that He production does not meet the limit necessary for re-welding. The results presented in this work are being used by the ITER Organization Blanket and Tokamak Integration groups to modify the BM design in the cases where limits are exceeded.

  10. 1H-NMR METABONOMICS ANALYSIS OF SERA DIFFERENTIATES BETWEEN MAMMARY TUMOR-BEARING MICE AND HEALTHY CONTROLS

    Science.gov (United States)

    Global analysis of 1H-NMR spectra of serum is an appealing approach for the rapid detection of cancer. To evaluate the usefulness of this method in distinguishing between mammary tumor-bearing mice and healthy controls, we conducted 1H-NMR metabonomic analyses on serum samples ob...

  11. Interlaboratory Comparison Test as an Evaluation of Applicability of an Alternative Edible Oil Analysis by 1H NMR Spectroscopy.

    Science.gov (United States)

    Zailer, Elina; Holzgrabe, Ulrike; Diehl, Bernd W K

    2017-11-01

    A proton (1H) NMR spectroscopic method was established for the quality assessment of vegetable oils. To date, several research studies have been published demonstrating the high potential of the NMR technique in lipid analysis. An interlaboratory comparison was organized with the following main objectives: (1) to evaluate an alternative analysis of edible oils by using 1H NMR spectroscopy; and (2) to determine the robustness and reproducibility of the method. Five different edible oil samples were analyzed by evaluating 15 signals (free fatty acids, peroxides, aldehydes, double bonds, and linoleic and linolenic acids) in each spectrum. A total of 21 NMR data sets were obtained from 17 international participant laboratories. The performance of each laboratory was assessed by their z-scores. The test was successfully passed by 90.5% of the participants. Results showed that NMR spectroscopy is a robust alternative method for edible oil analysis.

  12. Patterns of Communication through Interpreters: A Detailed Sociolinguistic Analysis

    Science.gov (United States)

    Aranguri, Cesar; Davidson, Brad; Ramirez, Robert

    2006-01-01

    BACKGROUND Numerous articles have detailed how the presence of an interpreter leads to less satisfactory communication with physicians; few have studied how actual communication takes place through an interpreter in a clinical setting. OBJECTIVE Record and analyze physician-interpreter-patient interactions. DESIGN Primary care physicians with high-volume Hispanic practices were recruited for a communication study. Dyslipidemic Hispanic patients, either monolingual Spanish or bilingual Spanish-English, were recruited on the day of a normally scheduled appointment and, once consented, recorded without a researcher present in the room. Separate postvisit interviews were conducted with the patient and the physician. All interactions were fully transcribed and analyzed. PARTICIPANTS Sixteen patients were recorded interacting with 9 physicians. Thirteen patients used an interpreter with 8 physicians, and 3 patients spoke Spanish with the 1 bilingual physician. APPROACH Transcript analysis based on sociolinguistic and discourse analytic techniques, including but not limited to time speaking, analysis of questions asked and answered, and the loss of semantic information. RESULTS Speech was significantly reduced and revised by the interpreter, resulting in an alteration of linguistic features such as content, meaning, reinforcement/validation, repetition, and affect. In addition, visits that included an interpreter had virtually no rapport-building “small talk,” which typically enables the physician to gain comprehensive patient history, learn clinically relevant information, and increase emotional engagement in treatment. CONCLUSIONS The presence of an interpreter increases the difficulty of achieving good physician-patient communication. Physicians and interpreters should be trained in the process of communication and interpretation, to minimize conversational loss and maximize the information and relational exchange with interpreted patients. PMID:16808747

  13. A Content Analysis of Officer Perceptions of Detailing.

    Science.gov (United States)

    1981-03-01

    answer was "No Way"! Told me needs of service were in Philippine Island CNSG WESTPAC as OPS, three year tour. I wrote letter saying O.K. Was detailed as...off to them as it has to be least preferred of all tasks...personnel detailer. 2 I regret the tardiness of this reply - New Zealand is a long way

  14. An integrated workflow for robust alignment and simplified quantitative analysis of NMR spectrometry data.

    Science.gov (United States)

    Vu, Trung N; Valkenborg, Dirk; Smets, Koen; Verwaest, Kim A; Dommisse, Roger; Lemière, Filip; Verschoren, Alain; Goethals, Bart; Laukens, Kris

    2011-10-20

    Nuclear magnetic resonance spectroscopy (NMR) is a powerful technique to reveal and compare quantitative metabolic profiles of biological tissues. However, chemical and physical sample variations make the analysis of the data challenging, and typically require the application of a number of preprocessing steps prior to data interpretation. For example, noise reduction, normalization, baseline correction, peak picking, spectrum alignment and statistical analysis are indispensable components in any NMR analysis pipeline. We introduce a novel suite of informatics tools for the quantitative analysis of NMR metabolomic profile data. The core of the processing cascade is a novel peak alignment algorithm, called hierarchical Cluster-based Peak Alignment (CluPA). The algorithm aligns a target spectrum to the reference spectrum in a top-down fashion by building a hierarchical cluster tree from peak lists of reference and target spectra and then dividing the spectra into smaller segments based on the most distant clusters of the tree. To reduce the computational time to estimate the spectral misalignment, the method makes use of Fast Fourier Transformation (FFT) cross-correlation. Since the method returns a high-quality alignment, we can propose a simple methodology to study the variability of the NMR spectra. For each aligned NMR data point the ratio of the between-group and within-group sum of squares (BW-ratio) is calculated to quantify the difference in variability between and within predefined groups of NMR spectra. This differential analysis is related to the calculation of the F-statistic or a one-way ANOVA, but without distributional assumptions. Statistical inference based on the BW-ratio is achieved by bootstrapping the null distribution from the experimental data. The workflow performance was evaluated using a previously published dataset. Correlation maps, spectral and grey scale plots show clear improvements in comparison to other methods, and the down

  15. An integrated workflow for robust alignment and simplified quantitative analysis of NMR spectrometry data

    Directory of Open Access Journals (Sweden)

    Dommisse Roger

    2011-10-01

    Full Text Available Abstract Background Nuclear magnetic resonance spectroscopy (NMR is a powerful technique to reveal and compare quantitative metabolic profiles of biological tissues. However, chemical and physical sample variations make the analysis of the data challenging, and typically require the application of a number of preprocessing steps prior to data interpretation. For example, noise reduction, normalization, baseline correction, peak picking, spectrum alignment and statistical analysis are indispensable components in any NMR analysis pipeline. Results We introduce a novel suite of informatics tools for the quantitative analysis of NMR metabolomic profile data. The core of the processing cascade is a novel peak alignment algorithm, called hierarchical Cluster-based Peak Alignment (CluPA. The algorithm aligns a target spectrum to the reference spectrum in a top-down fashion by building a hierarchical cluster tree from peak lists of reference and target spectra and then dividing the spectra into smaller segments based on the most distant clusters of the tree. To reduce the computational time to estimate the spectral misalignment, the method makes use of Fast Fourier Transformation (FFT cross-correlation. Since the method returns a high-quality alignment, we can propose a simple methodology to study the variability of the NMR spectra. For each aligned NMR data point the ratio of the between-group and within-group sum of squares (BW-ratio is calculated to quantify the difference in variability between and within predefined groups of NMR spectra. This differential analysis is related to the calculation of the F-statistic or a one-way ANOVA, but without distributional assumptions. Statistical inference based on the BW-ratio is achieved by bootstrapping the null distribution from the experimental data. Conclusions The workflow performance was evaluated using a previously published dataset. Correlation maps, spectral and grey scale plots show clear

  16. Conformational analysis of capsaicin using 13C, 15N MAS NMR, GIAO DFT and GA calculations

    Science.gov (United States)

    Siudem, Paweł; Paradowska, Katarzyna; Bukowicki, Jarosław

    2017-10-01

    Capsaicin produced by plants from genus Capsicum exerts multiple pharmacological effects and has found applications in food and pharmaceutical industry. The alkaloid was studied by a combined approach: solid-state NMR, GA conformational search and GIAO DFT methods. The 13C CPMAS NMR spectra were recorded using variable contact time and dipolar dephasing experiments. The results of cross-polarization (CP) kinetics, such as TCP values and long T1ρH (100-200 ms), indicated that the capsaicin molecule is fairly mobile, especially at the end of the aliphatic chain. The15N MAS NMR spectrum showed one narrow signal at -255 ppm. Genetic algorithm (GA) search with multi modal optimization was used to find low-energy conformations of capsaicin. Theoretical GIAO DFT calculations were performed using different basis sets to characterize five selected conformations. 13C CPMAS NMR was used as a validation method and the experimental chemical shifts were compared with those calculated for selected stable conformers. Conformational analysis suggests that the side chain can be bent or extended. A comparison of the experimental and the calculated chemical shifts indicates that solid capsaicin does not have the same structure as those established by PWXRD.

  17. NMR and modelling techniques in structural and conformation analysis

    Energy Technology Data Exchange (ETDEWEB)

    Abraham, R J [Liverpool Univ. (United Kingdom)

    1994-12-31

    The use of Lanthanide Induced Shifts (L.I.S.) and modelling techniques in conformational analysis is presented. The use of Co{sup III} porphyrins as shift reagents is discussed, with examples of their use in the conformational analysis of some heterocyclic amines. (author) 13 refs., 9 figs.

  18. MetaboLab - advanced NMR data processing and analysis for metabolomics

    Directory of Open Access Journals (Sweden)

    Günther Ulrich L

    2011-09-01

    Full Text Available Abstract Background Despite wide-spread use of Nuclear Magnetic Resonance (NMR in metabolomics for the analysis of biological samples there is a lack of graphically driven, publicly available software to process large one and two-dimensional NMR data sets for statistical analysis. Results Here we present MetaboLab, a MATLAB based software package that facilitates NMR data processing by providing automated algorithms for processing series of spectra in a reproducible fashion. A graphical user interface provides easy access to all steps of data processing via a script builder to generate MATLAB scripts, providing an option to alter code manually. The analysis of two-dimensional spectra (1H,13C-HSQC spectra is facilitated by the use of a spectral library derived from publicly available databases which can be extended readily. The software allows to display specific metabolites in small regions of interest where signals can be picked. To facilitate the analysis of series of two-dimensional spectra, different spectra can be overlaid and assignments can be transferred between spectra. The software includes mechanisms to account for overlapping signals by highlighting neighboring and ambiguous assignments. Conclusions The MetaboLab software is an integrated software package for NMR data processing and analysis, closely linked to the previously developed NMRLab software. It includes tools for batch processing and gives access to a wealth of algorithms available in the MATLAB framework. Algorithms within MetaboLab help to optimize the flow of metabolomics data preparation for statistical analysis. The combination of an intuitive graphical user interface along with advanced data processing algorithms facilitates the use of MetaboLab in a broader metabolomics context.

  19. Detailed analysis of radon flux studies at Australian uranium projects

    International Nuclear Information System (INIS)

    Mudd, Gavin M.

    2005-01-01

    The release of radon gas and radon progeny from uranium projects is a major issue during operation as well as for the design of rehabilitation works. In Australia, there have been a number of premining radon flux studies as part of the environmental investigation and potential development of recent uranium projects. There is also an increasing amount of operational data on radon fluxes and loads from various aspects of projects, such as tailings, waste rock and mills. Thus there exists much useful measured data which can be used to assess the design radon flux and load targets for rehabilitation. The main projects for which radon data exists includes Ranger, Olympic Dam, Beverley, Honeymoon, Jabiluka, Yeelirrie, Lake Way, Koongarra, Moline, Coronation Hill, Rockhole, Nabarlek, Rum Jungle, Port Pirie and Ben Lomond. To date, much of this data has not been systematically evaluated. The need to compile and assess this data is twofold. Firstly, to assess the loads released from uranium production as an input into life-cycle analyses of the nuclear fuel cycle, such as those undertaken by UNSCEAR and industry groups. Secondly, there is a need to set suitable design standards for radon flux for the rehabilitation of former and current uranium projects. This paper will present such a detailed compilation of radon fluxes and loads which can then be used as the basis for both life-cycle analyses as well as setting appropriate site-specific rehabilitation criteria for radon. The implications for former and current projects is then discussed as well as future data needs. Ultimately, there is a critical need for thorough baseline surveys prior to mining to ensure accurate assessments of changes to radon fluxes and loads. The data and analysis presented is considered applicable to all uranium projects in Australia, as well as being a useful model for considering such issues internationally

  20. Detailed thermodynamic analysis of a diffusion-absorption refrigeration cycle

    International Nuclear Information System (INIS)

    Taieb, Ahmed; Mejbri, Khalifa; Bellagi, Ahmed

    2016-01-01

    This paper proposes an advanced simulation model for a Diffusion-Absorption Refrigerator DAR using ammonia/water/hydrogen as working fluids, and developed to describe and predict the behavior of the device under different operating conditions. The system is supposed to be cooled with ambient air and actuated with solar hot water available at 200 °C. The DAR is first simulated for a set of basic data; a COP of 0.126 associated to a cooling capacity of 22.3 W are found. Basing on the obtained results an exergetic analysis of the system is performed which shows that the rectifier contribution to the exergy destruction is the most important with 34%. In a second step, the thermal capacities of all heat exchangers of the DAR are evaluated and the mathematical model so modified that the calculated capacities are now used as input data. A parametric study of the cycle is then carried out. The COP is found to exhibit a maximum when the heat supplied to the boiler or to the bubble pump is varied. Similar behavior is observed for variable submergence ratio. It is further noted that the COP is very sensitive to the ambient air temperature and to the absorber efficiency. - Highlights: • A detailed model of a Diffusion Absorption is developed and simulated. • Irreversibility of each component of the cycle is examined. • A modified model based on thermal capacity of components of the DAR is elaborated. • System performance is calculated over a series of practical operating conditions.

  1. Human Factors Considerations in New Nuclear Power Plants: Detailed Analysis.

    Energy Technology Data Exchange (ETDEWEB)

    OHara,J.; Higgins, J.; Brown, W.; Fink, R.

    2008-02-14

    This Nuclear Regulatory Commission (NRC) sponsored study has identified human-performance issues in new and advanced nuclear power plants. To identify the issues, current industry developments and trends were evaluated in the areas of reactor technology, instrumentation and control technology, human-system integration technology, and human factors engineering (HFE) methods and tools. The issues were organized into seven high-level HFE topic areas: Role of Personnel and Automation, Staffing and Training, Normal Operations Management, Disturbance and Emergency Management, Maintenance and Change Management, Plant Design and Construction, and HFE Methods and Tools. The issues where then prioritized into four categories using a 'Phenomena Identification and Ranking Table' methodology based on evaluations provided by 14 independent subject matter experts. The subject matter experts were knowledgeable in a variety of disciplines. Vendors, utilities, research organizations and regulators all participated. Twenty issues were categorized into the top priority category. This Brookhaven National Laboratory (BNL) technical report provides the detailed methodology, issue analysis, and results. A summary of the results of this study can be found in NUREG/CR-6947. The research performed for this project has identified a large number of human-performance issues for new control stations and new nuclear power plant designs. The information gathered in this project can serve as input to the development of a long-term strategy and plan for addressing human performance in these areas through regulatory research. Addressing human-performance issues will provide the technical basis from which regulatory review guidance can be developed to meet these challenges. The availability of this review guidance will help set clear expectations for how the NRC staff will evaluate new designs, reduce regulatory uncertainty, and provide a well-defined path to new nuclear power plant

  2. The application of NMR-based milk metabolite analysis in milk authenticity identification.

    Science.gov (United States)

    Li, Qiangqiang; Yu, Zunbo; Zhu, Dan; Meng, Xianghe; Pang, Xiumei; Liu, Yue; Frew, Russell; Chen, He; Chen, Gang

    2017-07-01

    Milk is an important food component in the human diet and is a target for fraud, including many unsafe practices. For example, the unscrupulous adulteration of soymilk into bovine and goat milk or of bovine milk into goat milk in order to gain profit without declaration is a health risk, as the adulterant source and sanitary history are unknown. A robust and fit-for-purpose technique is required to enforce market surveillance and hence protect consumer health. Nuclear magnetic resonance (NMR) is a powerful technique for characterization of food products based on measuring the profile of metabolites. In this study, 1D NMR in conjunction with multivariate chemometrics as well as 2D NMR was applied to differentiate milk types and to identify milk adulteration. Ten metabolites were found which differed among milk types, hence providing characteristic markers for identifying the milk. These metabolites were used to establish mathematical models for milk type differentiation. The limit of quantification (LOQ) of adulteration was 2% (v/v) for soymilk in bovine milk, 2% (v/v) for soymilk in goat milk and 5% (v/v) for bovine milk in goat milk, with relative standard deviation (RSD) less than 10%, which can meet the needs of daily inspection. The NMR method described here is effective for milk authenticity identification, and the study demonstrates that the NMR-based milk metabolite analysis approach provides a means of detecting adulteration at expected levels and can be used for dairy quality monitoring. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

  3. Metabolomic differentiation of maca (Lepidium meyenii) accessions cultivated under different conditions using NMR and chemometric analysis.

    Science.gov (United States)

    Zhao, Jianping; Avula, Bharathi; Chan, Michael; Clément, Céline; Kreuzer, Michael; Khan, Ikhlas A

    2012-01-01

    To gain insights on the effects of color type, cultivation history, and growing site on the composition alterations of maca (Lepidium meyenii Walpers) hypocotyls, NMR profiling combined with chemometric analysis was applied to investigate the metabolite variability in different maca accessions. Maca hypocotyls with different colors (yellow, pink, violet, and lead-colored) cultivated at different geographic sites and different areas were examined for differences in metabolite expression. Differentiations of the maca accessions grown under the different cultivation conditions were determined by principle component analyses (PCAs) which were performed on the datasets derived from their ¹H NMR spectra. A total of 16 metabolites were identified by NMR analysis, and the changes in metabolite levels in relation to the color types and growing conditions of maca hypocotyls were evaluated using univariate statistical analysis. In addition, the changes of the correlation pattern among the metabolites identified in the maca accessions planted at the two different sites were examined. The results from both multivariate and univariate analysis indicated that the planting site was the major determining factor with regards to metabolite variations in maca hypocotyls, while the color of maca accession seems to be of minor importance in this respect. © Georg Thieme Verlag KG Stuttgart · New York.

  4. Quantifying NMR relaxation correlation and exchange in articular cartilage with time domain analysis

    Science.gov (United States)

    Mailhiot, Sarah E.; Zong, Fangrong; Maneval, James E.; June, Ronald K.; Galvosas, Petrik; Seymour, Joseph D.

    2018-02-01

    Measured nuclear magnetic resonance (NMR) transverse relaxation data in articular cartilage has been shown to be multi-exponential and correlated to the health of the tissue. The observed relaxation rates are dependent on experimental parameters such as solvent, data acquisition methods, data analysis methods, and alignment to the magnetic field. In this study, we show that diffusive exchange occurs in porcine articular cartilage and impacts the observed relaxation rates in T1-T2 correlation experiments. By using time domain analysis of T2-T2 exchange spectroscopy, the diffusive exchange time can be quantified by measurements that use a single mixing time. Measured characteristic times for exchange are commensurate with T1 in this material and so impacts the observed T1 behavior. The approach used here allows for reliable quantification of NMR relaxation behavior in cartilage in the presence of diffusive fluid exchange between two environments.

  5. Conformational analysis of oxa-thio-azolydines through NMR

    International Nuclear Information System (INIS)

    Val, Amelia Maria Gomes do; Guimaraes, Afonso Celso

    1997-01-01

    This work presents the conformational analysis of some selected oxa-thio-azolidines. As the chemical properties of such compounds do not depend only upon the chemical structure, but also upon the conformational state which they may present, special emphasis is given to this phenomenon, which can elucidate the compounds properties

  6. Polymer Molecular Weight Analysis by [Superscript 1]H NMR Spectroscopy

    Science.gov (United States)

    Izunobi, Josephat U.; Higginbotham, Clement L.

    2011-01-01

    The measurement and analysis of molecular weight and molecular weight distribution remain matters of fundamental importance for the characterization and physical properties of polymers. Gel permeation chromatography (GPC) is the most routinely used method for the molecular weight determination of polymers whereas matrix-assisted laser…

  7. NMR-based urine analysis in rats: prediction of proximal tubule kidney toxicity and phospholipidosis.

    Science.gov (United States)

    Lienemann, Kai; Plötz, Thomas; Pestel, Sabine

    2008-01-01

    The aim of safety pharmacology is early detection of compound-induced side-effects. NMR-based urine analysis followed by multivariate data analysis (metabonomics) identifies efficiently differences between toxic and non-toxic compounds; but in most cases multiple administrations of the test compound are necessary. We tested the feasibility of detecting proximal tubule kidney toxicity and phospholipidosis with metabonomics techniques after single compound administration as an early safety pharmacology approach. Rats were treated orally, intravenously, inhalatively or intraperitoneally with different test compounds. Urine was collected at 0-8 h and 8-24 h after compound administration, and (1)H NMR-patterns were recorded from the samples. Variation of post-processing and feature extraction methods led to different views on the data. Support Vector Machines were trained on these different data sets and then aggregated as experts in an Ensemble. Finally, validity was monitored with a cross-validation study using a training, validation, and test data set. Proximal tubule kidney toxicity could be predicted with reasonable total classification accuracy (85%), specificity (88%) and sensitivity (78%). In comparison to alternative histological studies, results were obtained quicker, compound need was reduced, and very importantly fewer animals were needed. In contrast, the induction of phospholipidosis by the test compounds could not be predicted using NMR-based urine analysis or the previously published biomarker PAG. NMR-based urine analysis was shown to effectively predict proximal tubule kidney toxicity after single compound administration in rats. Thus, this experimental design allows early detection of toxicity risks with relatively low amounts of compound in a reasonably short period of time.

  8. Chemical tagging of chlorinated phenols for their facile detection and analysis by NMR spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Valdez, Carlos A. [Lawrence Livermore National Laboratory (LLNL), Livermore, CA (United States); Leif, Roald N. [Lawrence Livermore National Laboratory (LLNL), Livermore, CA (United States)

    2015-03-22

    A derivatization method that employs diethyl (bromodifluoromethyl) phosphonate (DBDFP) to efficiently tag the endocrine disruptor pentachlorophenol (PCP) and other chlorinated phenols (CPs) along with their reliable detection and analysis by NMR is presented. The method accomplishes the efficient alkylation of the hydroxyl group in CPs with the difluoromethyl (CF2H) moiety in extremely rapid fashion (5 min), at room temperature and in an environmentally benign manner. The approach proved successful in difluoromethylating a panel of 18 chlorinated phenols, yielding derivatives that displayed unique 1H, 19F NMR spectra allowing for the clear discrimination between isomerically related CPs. Due to its biphasic nature, the derivatization can be applied to both aqueous and organic mixtures where the analysis of CPs is required. Furthermore, the methodology demonstrates that PCP along with other CPs can be selectively derivatized in the presence of other various aliphatic alcohols, underscoring the superiority of the approach over other general derivatization methods that indiscriminately modify all analytes in a given sample. The present work demonstrates the first application of NMR on the qualitative analysis of these highly toxic and environmentally persistent species.

  9. A route to quantitative 13C NMR analysis of multicomponent polyesters

    DEFF Research Database (Denmark)

    Hvilsted, S.

    1991-01-01

    A protocol for quantitative sequential 13C NMR analysis is developed for polyesters composed of trimethylol propane (TMP), neopentyl glycol (NPG), and adipic and isophthalic acids. TMP centred, structural models with methyl adipate and isophthalate branches in all possible combinations...

  10. Numerical analysis of boosting scheme for scalable NMR quantum computation

    International Nuclear Information System (INIS)

    SaiToh, Akira; Kitagawa, Masahiro

    2005-01-01

    Among initialization schemes for ensemble quantum computation beginning at thermal equilibrium, the scheme proposed by Schulman and Vazirani [in Proceedings of the 31st ACM Symposium on Theory of Computing (STOC'99) (ACM Press, New York, 1999), pp. 322-329] is known for the simple quantum circuit to redistribute the biases (polarizations) of qubits and small time complexity. However, our numerical simulation shows that the number of qubits initialized by the scheme is rather smaller than expected from the von Neumann entropy because of an increase in the sum of the binary entropies of individual qubits, which indicates a growth in the total classical correlation. This result--namely, that there is such a significant growth in the total binary entropy--disagrees with that of their analysis

  11. Analysis of the extracts of Isatis tinctoria by new analytical approaches of HPLC, MS and NMR.

    Science.gov (United States)

    Zhou, Jue; Qu, Fan

    2011-01-01

    The methods of extraction, separation and analysis of alkaloids and indole glucosinolates (GLs) ofIsatis tinctoria were reviewed. Different analytical approaches such as High-pressure Liquid Chromatography (HPLC), Liquid Chromatography with Electrospray Ionization Mass Spectrometry (LC/ESI/MS), Electrospray Ionization Time-Of-Flight Mass Spectrometry (ESI-TOF-MS), and Nuclear Magnetic Resonance (NMR) were used to validate and identity of these constituents. These methods provide rapid separation, identification and quantitative measurements of alkaloids and GLs of Isatis tinctoria. By connection with different detectors to HPLC such as PDA, ELSD, ESI- and APCI-MS in positive and negative ion modes, complicated compounds could be detected with at least two independent detection modes. The molecular formula can be derived in a second step of ESI-TOF-MS data. But for some constituents, UV and MS cannot provide sufficient structure identification. After peak purification, NMR by semi-preparative HPLC can be used as a complementary method.

  12. Reproducibility of NMR Analysis of Urine Samples: Impact of Sample Preparation, Storage Conditions, and Animal Health Status

    OpenAIRE

    Schreier, Christina; Kremer, Werner; Huber, Fritz; Neumann, Sindy; Pagel, Philipp; Lienemann, Kai; Pestel, Sabine

    2013-01-01

    Introduction. Spectroscopic analysis of urine samples from laboratory animals can be used to predict the efficacy and side effects of drugs. This employs methods combining 1H NMR spectroscopy with quantification of biomarkers or with multivariate data analysis. The most critical steps in data evaluation are analytical reproducibility of NMR data (collection, storage, and processing) and the health status of the animals, which may influence urine pH and osmolarity. Methods. We treated rats wit...

  13. Quantitative analysis of deuterium using the isotopic effect on quaternary {sup 13}C NMR chemical shifts

    Energy Technology Data Exchange (ETDEWEB)

    Darwish, Tamim A., E-mail: tamim.darwish@ansto.gov.au [National Deuteration Facility, Australian Nuclear Science and Technology Organisation, Locked Bag 21, Kirrawee DC, NSW 2232 (Australia); Yepuri, Nageshwar Rao; Holden, Peter J. [National Deuteration Facility, Australian Nuclear Science and Technology Organisation, Locked Bag 21, Kirrawee DC, NSW 2232 (Australia); James, Michael [Australian Synchrotron, 800 Blackburn Road, Clayton, Victoria 3168 (Australia)

    2016-07-13

    Quantitative analysis of specifically deuterated compounds can be achieved by a number of conventional methods, such as mass spectroscopy, or by quantifying the residual {sup 1}H NMR signals compared to signals from internal standards. However, site specific quantification using these methods becomes challenging when dealing with non-specifically or randomly deuterated compounds that are produced by metal catalyzed hydrothermal reactions in D{sub 2}O, one of the most convenient deuteration methods. In this study, deuterium-induced NMR isotope shifts of quaternary {sup 13}C resonances neighboring deuterated sites have been utilized to quantify the degree of isotope labeling of molecular sites in non-specifically deuterated molecules. By probing {sup 13}C NMR signals while decoupling both proton and deuterium nuclei, it is possible to resolve {sup 13}C resonances of the different isotopologues based on the isotopic shifts and the degree of deuteration of the carbon atoms. We demonstrate that in different isotopologues, the same quaternary carbon, neighboring partially deuterated carbon atoms, are affected to an equal extent by relaxation. Decoupling both nuclei ({sup 1}H, {sup 2}H) resolves closely separated quaternary {sup 13}C signals of the different isotopologues, and allows their accurate integration and quantification under short relaxation delays (D1 = 1 s) and hence fast accumulative spectral acquisition. We have performed a number of approaches to quantify the deuterium content at different specific sites to demonstrate a convenient and generic analysis method for use in randomly deuterated molecules, or in cases of specifically deuterated molecules where back-exchange processes may take place during work up. - Graphical abstract: The relative intensities of quaternary {sup 13}C {"1H,"2H} resonances are equal despite the different relaxation delays, allowing the relative abundance of the different deuterated isotopologues to be calculated using NMR fast

  14. Synergistic effect of the simultaneous chemometric analysis of {sup 1}H NMR spectroscopic and stable isotope (SNIF-NMR, {sup 18}O, {sup 13}C) data: Application to wine analysis

    Energy Technology Data Exchange (ETDEWEB)

    Monakhova, Yulia B., E-mail: yul-monakhova@mail.ru [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, Karlsruhe 76187 (Germany); Bruker Biospin GmbH, Silberstreifen, Rheinstetten 76287 (Germany); Department of Chemistry, Saratov State University, Astrakhanskaya Street 83, Saratov 410012 (Russian Federation); Godelmann, Rolf [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, Karlsruhe 76187 (Germany); Hermann, Armin [Landesuntersuchungsamt -Institut für Lebensmittelchemie und Arzneimittelprüfung, Emy-Roeder-Straße 1, Mainz 55129 (Germany); Kuballa, Thomas [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, Karlsruhe 76187 (Germany); Cannet, Claire; Schäfer, Hartmut; Spraul, Manfred [Bruker Biospin GmbH, Silberstreifen, Rheinstetten 76287 (Germany); Rutledge, Douglas N. [AgroParisTech, UMR 1145, Ingénierie Procédés Aliments, 16 rue Claude Bernard, Paris F-75005 (France)

    2014-06-23

    Highlights: • {sup 1}H NMR profilings of 718 wines were fused with stable isotope analysis data (SNIF-NMR, {sup 18}O, {sup 13}C). • The best improvement was obtained for prediction of the geographical origin of wine. • Certain enhancement was also obtained for the year of vintage (from 88 to 97% for {sup 1}H NMR to 99% for the fused data). • Independent component analysis was used as an alternative chemometric tool for classification. - Abstract: It is known that {sup 1}H NMR spectroscopy represents a good tool for predicting the grape variety, the geographical origin, and the year of vintage of wine. In the present study we have shown that classification models can be improved when {sup 1}H NMR profiles are fused with stable isotope (SNIF-NMR, {sup 18}O, {sup 13}C) data. Variable selection based on clustering of latent variables was performed on {sup 1}H NMR data. Afterwards, the combined data of 718 wine samples from Germany were analyzed using linear discriminant analysis (LDA), partial least squares-discriminant analysis (PLS-DA), factorial discriminant analysis (FDA) and independent components analysis (ICA). Moreover, several specialized multiblock methods (common components and specific weights analysis (ComDim), consensus PCA and consensus PLS-DA) were applied to the data. The best improvement in comparison with {sup 1}H NMR data was obtained for prediction of the geographical origin (up to 100% for the fused data, whereas stable isotope data resulted only in 60–70% correct prediction and {sup 1}H NMR data alone in 82–89% respectively). Certain enhancement was obtained also for the year of vintage (from 88 to 97% for {sup 1}H NMR to 99% for the fused data), whereas in case of grape varieties improved models were not obtained. The combination of {sup 1}H NMR data with stable isotope data improves efficiency of classification models for geographical origin and vintage of wine and can be potentially used for other food products as well.

  15. NMR-CT scanner

    International Nuclear Information System (INIS)

    Kose, Katsumi; Sato, Kozo; Sugimoto, Hiroshi; Sato, Masataka.

    1983-01-01

    A brief explanation is made on the imaging methods for a practical diagnostic NMR-CT scanner : A whole-body NMR-CT scanner utilizing a resistive magnet has been developed by Toshiba in cooperation with the Institute for Solid State Physics, the University of Tokyo. Typical NMR-CT images of volunteers and patients obtained in the clinical experiments using this device are presented. Detailed specifications are also shown about the practical NMR-CTs which are to be put on the market after obtaining the government approval. (author)

  16. Fractional order analysis of Sephadex gel structures: NMR measurements reflecting anomalous diffusion

    Science.gov (United States)

    Magin, Richard L.; Akpa, Belinda S.; Neuberger, Thomas; Webb, Andrew G.

    2011-12-01

    We report the appearance of anomalous water diffusion in hydrophilic Sephadex gels observed using pulse field gradient (PFG) nuclear magnetic resonance (NMR). The NMR diffusion data was collected using a Varian 14.1 Tesla imaging system with a home-built RF saddle coil. A fractional order analysis of the data was used to characterize heterogeneity in the gels for the dynamics of water diffusion in this restricted environment. Several recent studies of anomalous diffusion have used the stretched exponential function to model the decay of the NMR signal, i.e., exp[-( bD) α], where D is the apparent diffusion constant, b is determined the experimental conditions (gradient pulse separation, durations and strength), and α is a measure of structural complexity. In this work, we consider a different case where the spatial Laplacian in the Bloch-Torrey equation is generalized to a fractional order model of diffusivity via a complexity parameter, β, a space constant, μ, and a diffusion coefficient, D. This treatment reverts to the classical result for the integer order case. The fractional order decay model was fit to the diffusion-weighted signal attenuation for a range of b-values (0 < b < 4000 s mm -2). Throughout this range of b values, the parameters β, μ and D, were found to correlate with the porosity and tortuosity of the gel structure.

  17. Experimental and NMR theoretical methodology applied to geometric analysis of the bioactive clerodane trans-dehydrocrotonin

    Energy Technology Data Exchange (ETDEWEB)

    Soares, Breno Almeida; Firme, Caio Lima, E-mail: firme.caio@gmail.com, E-mail: caiofirme@quimica.ufrn.br [Universidade Federal do Rio Grande do Norte (UFRN), Natal, RN (Brazil). Instituto de Quimica; Maciel, Maria Aparecida Medeiros [Universidade Potiguar, Natal, RN (Brazil). Programa de Pos-graduacao em Biotecnologia; Kaiser, Carlos R. [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil). Instituto de Quimica; Schilling, Eduardo; Bortoluzzi, Adailton J. [Universidade Federal de Santa Catarina (UFSC), Florianopolis, SC (Brazil). Departamento de Quimica

    2014-04-15

    trans-Dehydrocrotonin (t-DCTN) a bioactive 19-nor-diterpenoid clerodane type isolated from Croton cajucara Benth, is one of the most investigated clerodane in the current literature. In this work, a new approach joining X-ray diffraction data, nuclear magnetic resonance (NMR) data and theoretical calculations was applied to the thorough characterization of t-DCTN. For that, the geometry of t-DCTN was reevaluated by X-ray diffraction as well as {sup 1}H and {sup 13}C NMR data, whose geometrical parameters where compared to those obtained from B3LYP/6-311G++(d,p) level of theory. From the evaluation of both calculated and experimental values of {sup 1}H and {sup 13}C NMR chemical shifts and spin-spin coupling constants, it was found very good correlations between theoretical and experimental magnetic properties of t-DCTN. Additionally, the delocalization indexes between hydrogen atoms correlated accurately with theoretical and experimental spin-spin coupling constants. An additional topological analysis from quantum theory of atoms in molecules (QTAIM) showed intramolecular interactions for t-DCTN. (author)

  18. Experimental and NMR theoretical methodology applied to geometric analysis of the bioactive clerodane trans-dehydrocrotonin

    International Nuclear Information System (INIS)

    Soares, Breno Almeida; Firme, Caio Lima; Maciel, Maria Aparecida Medeiros; Kaiser, Carlos R.; Schilling, Eduardo; Bortoluzzi, Adailton J.

    2014-01-01

    trans-Dehydrocrotonin (t-DCTN) a bioactive 19-nor-diterpenoid clerodane type isolated from Croton cajucara Benth, is one of the most investigated clerodane in the current literature. In this work, a new approach joining X-ray diffraction data, nuclear magnetic resonance (NMR) data and theoretical calculations was applied to the thorough characterization of t-DCTN. For that, the geometry of t-DCTN was reevaluated by X-ray diffraction as well as 1 H and 13 C NMR data, whose geometrical parameters where compared to those obtained from B3LYP/6-311G++(d,p) level of theory. From the evaluation of both calculated and experimental values of 1 H and 13 C NMR chemical shifts and spin-spin coupling constants, it was found very good correlations between theoretical and experimental magnetic properties of t-DCTN. Additionally, the delocalization indexes between hydrogen atoms correlated accurately with theoretical and experimental spin-spin coupling constants. An additional topological analysis from quantum theory of atoms in molecules (QTAIM) showed intramolecular interactions for t-DCTN. (author)

  19. Exploring high-resolution magic angle spinning (HR-MAS) NMR spectroscopy for metabonomic analysis of apples.

    Science.gov (United States)

    Vermathen, Martina; Marzorati, Mattia; Vermathen, Peter

    2012-01-01

    Classical liquid-state high-resolution (HR) NMR spectroscopy has proved a powerful tool in the metabonomic analysis of liquid food samples like fruit juices. In this paper the application of (1)H high-resolution magic angle spinning (HR-MAS) NMR spectroscopy to apple tissue is presented probing its potential for metabonomic studies. The (1)H HR-MAS NMR spectra are discussed in terms of the chemical composition of apple tissue and compared to liquid-state NMR spectra of apple juice. Differences indicate that specific metabolic changes are induced by juice preparation. The feasibility of HR-MAS NMR-based multivariate analysis is demonstrated by a study distinguishing three different apple cultivars by principal component analysis (PCA). Preliminary results are shown from subsequent studies comparing three different cultivation methods by means of PCA and partial least squares discriminant analysis (PLS-DA) of the HR-MAS NMR data. The compounds responsible for discriminating organically grown apples are discussed. Finally, an outlook of our ongoing work is given including a longitudinal study on apples.

  20. Molecular and Silica-Supported Molybdenum Alkyne Metathesis Catalysts: Influence of Electronics and Dynamics on Activity Revealed by Kinetics, Solid-State NMR, and Chemical Shift Analysis.

    Science.gov (United States)

    Estes, Deven P; Gordon, Christopher P; Fedorov, Alexey; Liao, Wei-Chih; Ehrhorn, Henrike; Bittner, Celine; Zier, Manuel Luca; Bockfeld, Dirk; Chan, Ka Wing; Eisenstein, Odile; Raynaud, Christophe; Tamm, Matthias; Copéret, Christophe

    2017-12-06

    Molybdenum-based molecular alkylidyne complexes of the type [MesC≡Mo{OC(CH 3 ) 3-x (CF 3 ) x } 3 ] (MoF 0 , x = 0; MoF 3 , x = 1; MoF 6 , x = 2; MoF 9 , x = 3; Mes = 2,4,6-trimethylphenyl) and their silica-supported analogues are prepared and characterized at the molecular level, in particular by solid-state NMR, and their alkyne metathesis catalytic activity is evaluated. The 13 C NMR chemical shift of the alkylidyne carbon increases with increasing number of fluorine atoms on the alkoxide ligands for both molecular and supported catalysts but with more shielded values for the supported complexes. The activity of these catalysts increases in the order MoF 0 molecular and supported species. Detailed solid-state NMR analysis of molecular and silica-supported metal alkylidyne catalysts coupled with DFT/ZORA calculations rationalize the NMR spectroscopic signatures and discernible activity trends at the frontier orbital level: (1) increasing the number of fluorine atoms lowers the energy of the π*(M≡C) orbital, explaining the more deshielded chemical shift values; it also leads to an increased electrophilicity and higher reactivity for catalysts up to MoF 6 , prior to a sharp decrease in reactivity for MoF 9 due to the formation of stable metallacyclobutadiene intermediates; (2) the silica-supported catalysts are less active than their molecular analogues because they are less electrophilic and dynamic, as revealed by their 13 C NMR chemical shift tensors.

  1. A chiral aluminum solvating agent (CASA) for 1H NMR chiral analysis of alcohols at low temperature.

    Science.gov (United States)

    Seo, Min-Seob; Jang, Sumin; Kim, Hyunwoo

    2018-03-16

    A chiral aluminum solvating agent (CASA) was demonstrated to be a general and efficient reagent for 1H NMR chiral analysis of alcohols. The sodium salt of the CASA (CASA-Na) showed a complete baseline peak separation of the hydroxyl group for various chiral alcohols including primary, secondary, and tertiary alcohols with alkyl and aryl substituents in CD3CN. Due to the weak intermolecular interaction, 1H NMR measurement at low temperature (-40 to 10 °C) was required.

  2. Characterization of solid polymer dispersions of active pharmaceutical ingredients by 19F MAS NMR and factor analysis

    Czech Academy of Sciences Publication Activity Database

    Urbanová, Martina; Brus, Jiří; Šeděnková, Ivana; Policianová, Olivia; Kobera, Libor

    2013-01-01

    Roč. 100, 1 January (2013), s. 59-66 ISSN 1386-1425 R&D Projects: GA ČR GPP106/11/P426; GA MŠk 2B08021 Institutional research plan: CEZ:AV0Z40500505 Institutional support: RVO:61389013 Keywords : solid-state NMR * factor analysis * 19F MAS NMR Subject RIV: FR - Pharmacology ; Medidal Chemistry Impact factor: 2.129, year: 2013

  3. Carbon-13 NMR of flavinoids

    International Nuclear Information System (INIS)

    Agrawal, P.K.

    1989-01-01

    The present book has been written with the objective of introducing the organic chemists with the conceptual and experimental basis required for interpretation of 13 C NMR spectra of a flavonoid and to a discussion of general usefulness of the technique in solving flavonoid structural problem. After a brief general introduction to the essential aspects of flavonoids and 13 C NMR spectroscopy, considerable emphasis has been placed in chapter 2 on the various experimental methods and the interpretation of spectral details which enable individual resonance lines to be associated with the appropriate carbons in a molecule. The whole bulk of the literature, published on 13 C NMR of flavonoids in the major journals upto 1986 alongwith some recent references of 1987 has been classified in several categories such as: flavonoids, isflavonoids, other flavonoids, flavonoid glycosides, chalconoids and flavanoids. Each category constitutes a chapter. Finally the last chapter is devoted largely to a discussion for the differentiation of various categories and subcategories of flavonoids and for the establishment of aromatic substitution pattern in these compounds. It should be emphasized that the book is a data book and only concerned with the actual analysis of 13 C NMR spectra, thus a reasonable familiarity with basic instrumentation of 13 C NMR and general pattern of nuclear chemical shifts has been assumed. (author). refs.; figs.; tabs

  4. Cutting costs through detailed probabilistic fire risk analysis

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Luiz; Huser, Asmund; Vianna, Savio [Det Norske Veritas PRINCIPIA, Rio de Janeiro, RJ (Brazil)

    2004-07-01

    A new procedure for calculation of fire risks to offshore installations has been developed. The purposes of the procedure are to calculate the escalation and impairment frequencies to be applied in quantitative risk analyses, to optimize Passive Fire Protection (PFP) arrangement, and to optimize other fire mitigation means. The novelties of the procedure are that it uses state of the art Computational Fluid Dynamics (CFD) models to simulate fires and radiation, as well as the use of a probabilistic approach to decide the dimensioning fire loads. A CFD model of an actual platform was used to investigate the dynamic properties of a large set of jet fires, resulting in detailed knowledge of the important parameters that decide the severity of offshore fires. These results are applied to design the procedure. Potential increase in safety is further obtained for those conditions where simplified tools may have failed to predict abnormal heat loads due to geometrical effects. Using a field example it is indicated that the probabilistic approach can give significant reductions in PFP coverage with corresponding cost savings, still keeping the risk at acceptable level. (author)

  5. Task analysis: a detailed example of stepping up from JSA

    International Nuclear Information System (INIS)

    Banks, W.W.; Paramore, B.A.; Buys, J.R.

    1984-10-01

    This paper discusses a pilot task analysis of operations in a proposed facility for the cutting and packaging of radioactively contaminated gloveboxes, for long-term storage or burial. The objective was to demonstrate how task analysis may be used as a tool for planning and risk management. Two specific products were generated - preliminary operating procedures and training requirements. The task data base, procedures list and training requirements developed were intended as first order categorizations. The analysis was limited to tasks that will be performed within the boundaries of the operational facility and the associated load-out area. The analysis documents tasks to be performed by D and D (Decontamination and Decommissioning) Workers. However, the analysis included all tasks identified as an integral part of glovebox processing within the facility. Thus tasks involving Radiation Protection Technicians (RPTs) are included. Based on hazard assessments, it is planned that at least two RPTs will be assigned full-time to the facility, so they may be considered part of its crew. Similarly, supervisory/administrative tasks are included where they were determined to be directly part of process sequences, such as obtaining appropriate certification. 11 tables

  6. Theoretical NMR and conformational analysis of solvated oximes for organophosphates-inhibited acetylcholinesterase reactivation

    Science.gov (United States)

    da Silva, Jorge Alberto Valle; Modesto-Costa, Lucas; de Koning, Martijn C.; Borges, Itamar; França, Tanos Celmar Costa

    2018-01-01

    In this work, quaternary and non-quaternary oximes designed to bind at the peripheral site of acetylcholinesterase previously inhibited by organophosphates were investigated theoretically. Some of those oximes have a large number of degrees of freedom, thus requiring an accurate method to obtain molecular geometries. For this reason, the density functional theory (DFT) was employed to refine their molecular geometries after conformational analysis and to compare their 1H and 13C nuclear magnetic resonance (NMR) theoretical signals in gas-phase and in solvent. A good agreement with experimental data was achieved and the same theoretical approach was employed to obtain the geometries in water environment for further studies.

  7. Tannin structural elucidation and quantitative ³¹P NMR analysis. 2. Hydrolyzable tannins and proanthocyanidins.

    Science.gov (United States)

    Melone, Federica; Saladino, Raffaele; Lange, Heiko; Crestini, Claudia

    2013-10-02

    An unprecedented analytical method that allows simultaneous structural and quantitative characterization of all functional groups present in tannins is reported. In situ labeling of all labile H groups (aliphatic and phenolic hydroxyls and carboxylic acids) with a phosphorus-containing reagent (Cl-TMDP) followed by quantitative ³¹P NMR acquisition constitutes a novel fast and reliable analytical tool for the analysis of tannins and proanthocyanidins with significant implications for the fields of food and feed analyses, tannery, and the development of natural polyphenolics containing products.

  8. DFT molecular modeling and NMR conformational analysis of a new longipinenetriolone diester

    Science.gov (United States)

    Cerda-García-Rojas, Carlos M.; Guerra-Ramírez, Diana; Román-Marín, Luisa U.; Hernández-Hernández, Juan D.; Joseph-Nathan, Pedro

    2006-05-01

    The structure and conformational behavior of the new natural compound (4 R,5 S,7 S,8 R,9 S,10 R,11 R)-longipin-2-en-7,8,9-triol-1-one 7-angelate-9-isovalerate (1) isolated from Stevia eupatoria, were studied by molecular modeling and NMR spectroscopy. A Monte Carlo search followed by DFT calculations at the B3LYP/6-31G* level provided the theoretical conformations of the sesquiterpene framework, which were in full agreement with results derived from the 1H- 1H coupling constant analysis.

  9. Detailed analysis of turbulent flows in air curtains

    NARCIS (Netherlands)

    Jaramillo, Julian E.; Perez-Segarra, Carlos D.; Lehmkuhl, Oriol; Castro, Jesus

    2011-01-01

    In order to prevent entrainment, an air curtain should provide a jet with low turbulence level, and enough momentum to counteract pressure differences across the opening. Consequently, the analysis of the discharge plenum should be taken into consideration. Hence, the main object of this paper is to

  10. The need for detailed gender-specific occupational safety analysis.

    Science.gov (United States)

    Cruz Rios, Fernanda; Chong, Wai K; Grau, David

    2017-09-01

    The female work in population is growing in the United States, therefore the occupational health and safety entities must start to analyze gender-specific data related to every industry, especially to nontraditional occupations. Women working in nontraditional jobs are often exposed to extreme workplace hazards. These women have their safety and health threatened because there are no adequate policies to mitigate gender-specific risks such as discrimination and harassment. Employers tend to aggravate this situation because they often fail to provide proper reporting infrastructure and support. According to past studies, women suffered from workplace injuries and illnesses that were less prominent among men. Statistics also confirmed that men and women faced different levels of risks in distinct work environments. For example, the rates of workplace violence and murders by personal acquaintances were significantly higher among women. In this paper, the authors analyze prior public data on fatal and nonfatal injuries to understand why we need to differentiate genders when analyzing occupational safety and health issues. The analyses confirmed that women dealt with unique workplace hazards compared to men. It is urgent that public agencies, such as the U.S. Department of Labor, record gender-specific data in details and by occupations and industries. The reader will become aware of the current lack - and need - of data and knowledge about injuries and illnesses separated by gender and industry. Finally, safety and health researchers are encouraged to investigate the gender-specific data in all industries and occupations, as soon as they become available. Copyright © 2017 National Safety Council and Elsevier Ltd. All rights reserved.

  11. Lightning climatology in the Congo Basin: detailed analysis

    Science.gov (United States)

    Soula, Serge; Kigotsi, Jean; Georgis, Jean-François; Barthe, Christelle

    2016-04-01

    The lightning climatology of the Congo Basin including several countries of Central Africa is analyzed in detail for the first time. It is based on World Wide Lightning Location Network (WWLLN) data for the period from 2005 to 2013. A comparison of these data with the Lightning Imaging Sensor (LIS) data for the same period shows the WWLLN detection efficiency (DE) in the region increases from about 1.70 % in the beginning of the period to 5.90 % in 2013, relative to LIS data, but not uniformly over the whole 2750 km × 2750 km area. Both the annual flash density and the number of stormy days show sharp maximum values localized in eastern of Democratic Republic of Congo (DRC) and west of Kivu Lake, regardless of the reference year and the period of the year. These maxima reach 12.86 fl km-2 and 189 days, respectively, in 2013, and correspond with a very active region located at the rear of the Virunga mountain range characterised with summits that can reach 3000 m. The presence of this range plays a role in the thunderstorm development along the year. The estimation of this local maximum of the lightning density by taking into account the DE, leads to a value consistent with that of the global climatology by Christian et al. (2003) and other authors. Thus, a mean maximum value of about 157 fl km-2 y-1 is found for the annual lightning density. The zonal distribution of the lightning flashes exhibits a maximum between 1°S and 2°S and about 56 % of the flashes located below the equator in the 10°S - 10°N interval. The diurnal evolution of the flash rate has a maximum between 1400 and 1700 UTC, according to the reference year, in agreement with previous works in other regions of the world.

  12. NMR analysis of male fathead minnow urinary metabolites: A potential approach for studying impacts of chemical exposures

    Energy Technology Data Exchange (ETDEWEB)

    Ekman, D.R. [Ecosystems Research Division, U.S. EPA, 960 College Station Road, Athens, GA 30605 (United States)], E-mail: ekman.drew@epa.gov; Teng, Q. [Ecosystems Research Division, U.S. EPA, 960 College Station Road, Athens, GA 30605 (United States); Jensen, K.M.; Martinovic, D.; Villeneuve, D.L.; Ankley, G.T. [Mid-Continent Ecology Division, U.S. EPA, 6201 Congdon Boulevard, Duluth, MN 55804 (United States); Collette, T.W. [Ecosystems Research Division, U.S. EPA, 960 College Station Road, Athens, GA 30605 (United States)

    2007-11-30

    The potential for profiling metabolites in urine from male fathead minnows (Pimephales promelas) to assess chemical exposures was explored using nuclear magnetic resonance (NMR) spectroscopy. Both one-dimensional (1D) and two-dimensional (2D) NMR spectroscopy was used for the assignment of metabolites in urine from unexposed fish. Because fathead minnow urine is dilute, we lyophilized these samples prior to analysis. Furthermore, 1D {sup 1}H NMR spectra of unlyophilized urine from unexposed male fathead minnow and Sprague-Dawley rat were acquired to qualitatively compare rat and fish metabolite profiles and to provide an estimate of the total urinary metabolite pool concentration difference. As a small proof-of-concept study, lyophilized urine samples from male fathead minnows exposed to three different concentrations of the antiandrogen vinclozolin were analyzed by 1D {sup 1}H NMR to assess exposure-induced changes. Through a combination of principal components analysis (PCA) and measurements of {sup 1}H NMR peak intensities, several metabolites were identified as changing with statistical significance in response to exposure. Among those changes occurring in response to exposure to the highest concentration (450 {mu}g/L) of vinclozolin were large increases in taurine, lactate, acetate, and formate. These increases coincided with a marked decrease in hippurate, a combination potentially indicative of hepatotoxicity. The results of these investigations clearly demonstrate the potential utility of an NMR-based approach for assessing chemical exposures in male fathead minnow, using urine collected from individual fish.

  13. NMR analysis of male fathead minnow urinary metabolites: A potential approach for studying impacts of chemical exposures

    International Nuclear Information System (INIS)

    Ekman, D.R.; Teng, Q.; Jensen, K.M.; Martinovic, D.; Villeneuve, D.L.; Ankley, G.T.; Collette, T.W.

    2007-01-01

    The potential for profiling metabolites in urine from male fathead minnows (Pimephales promelas) to assess chemical exposures was explored using nuclear magnetic resonance (NMR) spectroscopy. Both one-dimensional (1D) and two-dimensional (2D) NMR spectroscopy was used for the assignment of metabolites in urine from unexposed fish. Because fathead minnow urine is dilute, we lyophilized these samples prior to analysis. Furthermore, 1D 1 H NMR spectra of unlyophilized urine from unexposed male fathead minnow and Sprague-Dawley rat were acquired to qualitatively compare rat and fish metabolite profiles and to provide an estimate of the total urinary metabolite pool concentration difference. As a small proof-of-concept study, lyophilized urine samples from male fathead minnows exposed to three different concentrations of the antiandrogen vinclozolin were analyzed by 1D 1 H NMR to assess exposure-induced changes. Through a combination of principal components analysis (PCA) and measurements of 1 H NMR peak intensities, several metabolites were identified as changing with statistical significance in response to exposure. Among those changes occurring in response to exposure to the highest concentration (450 μg/L) of vinclozolin were large increases in taurine, lactate, acetate, and formate. These increases coincided with a marked decrease in hippurate, a combination potentially indicative of hepatotoxicity. The results of these investigations clearly demonstrate the potential utility of an NMR-based approach for assessing chemical exposures in male fathead minnow, using urine collected from individual fish

  14. Robust and transferable quantification of NMR spectral quality using IROC analysis

    Science.gov (United States)

    Zambrello, Matthew A.; Maciejewski, Mark W.; Schuyler, Adam D.; Weatherby, Gerard; Hoch, Jeffrey C.

    2017-12-01

    Non-Fourier methods are increasingly utilized in NMR spectroscopy because of their ability to handle nonuniformly-sampled data. However, non-Fourier methods present unique challenges due to their nonlinearity, which can produce nonrandom noise and render conventional metrics for spectral quality such as signal-to-noise ratio unreliable. The lack of robust and transferable metrics (i.e. applicable to methods exhibiting different nonlinearities) has hampered comparison of non-Fourier methods and nonuniform sampling schemes, preventing the identification of best practices. We describe a novel method, in situ receiver operating characteristic analysis (IROC), for characterizing spectral quality based on the Receiver Operating Characteristic curve. IROC utilizes synthetic signals added to empirical data as "ground truth", and provides several robust scalar-valued metrics for spectral quality. This approach avoids problems posed by nonlinear spectral estimates, and provides a versatile quantitative means of characterizing many aspects of spectral quality. We demonstrate applications to parameter optimization in Fourier and non-Fourier spectral estimation, critical comparison of different methods for spectrum analysis, and optimization of nonuniform sampling schemes. The approach will accelerate the discovery of optimal approaches to nonuniform sampling experiment design and non-Fourier spectrum analysis for multidimensional NMR.

  15. NMR analysis of seven selections of vermentino grape berry: metabolites composition and development.

    Science.gov (United States)

    Mulas, Gilberto; Galaffu, Maria Grazia; Pretti, Luca; Nieddu, Gianni; Mercenaro, Luca; Tonelli, Roberto; Anedda, Roberto

    2011-02-09

    The goal of this work was to study via NMR the unaltered metabolic profile of Sardinian Vermentino grape berry. Seven selections of Vermentino were harvested from the same vineyard. Berries were stored and extracted following an unbiased extraction protocol. Extracts were analyzed to investigate variability in metabolites concentration as a function of the clone, the position of berries in the bunch or growing area within the vineyard. Quantitative NMR and statistical analysis (PCA, correlation analysis, Anova) of the experimental data point out that, among the investigated sources of variation, the position of the berries within the bunch mainly influences the metabolic profile of berries, while the metabolic profile does not seem to be significantly influenced by growing area and clone. Significant variability of the amino acids such as arginine, proline, and organic acids (malic and citric) characterizes the rapid rearrangements of the metabolic profile in response to environmental stimuli. Finally, an application is described on the analysis of metabolite variation throughout the physiological development of berries.

  16. Detailed analysis of the ANO-2 turbine trip test

    International Nuclear Information System (INIS)

    McDonald, T.A.; Tessier, J.H.; Senda, Y.; Waterman, M.D.

    1983-01-01

    A RELAP5/MOD1 (Cycle 18) computer code simulation of the ANO-2 turbine trip test from 98% power level was performed for use in vendor code qualification studies. Results focused on potential improvements to simulation capabilities and plant data acquisition systems to provide meaningful comparisons between the calculations and the test data. The turbine trip test was selected because it resulted in an unplanned sequence of events that broadly affected the plant process systems and their controls. The pressurizer spray valve stuck open at an undetermined flow area, and an atmospheric dump valve remained stuck fully open while several atmospheric dump and secondary side safety valves were unavailable throughout. Thus, although the plant remained always in a safe condition, this transient potentially provided an unusual set of data against which the fidelity of a NSSS simulation by RELAP5/MOD1 along with certain vendor analysis codes might be judged

  17. Effect of rootstock on the scion of Hevea brasiliensis through metabolic analysis of latex samples by 1H NMR

    Directory of Open Access Journals (Sweden)

    Eduardo Sanches Pereira do Nascimento

    2011-01-01

    Full Text Available In this study, the effect of rootstock on grafting through metabolomic analysis of latex (Hevea brasiliensis samples was verified by 1H nuclear magnetic resonance (NMR and multivariate data analysis. Sixteen metabolites present in the latex cytosol were characterized by NMR. PCA analysis showed that the latex samples of the RR and GR groups can be differentiated. The GR group samples present a metabolic profile similar to the RR group samples, while the RG group is in an intermediate position between RR and GG groups. Sucrose and formate contributed greatly to the separation obtained by PCA, presenting a good correlation between the results. 1H NMR was an efficient technique to differentiate latex samples from different types of rootstocks and grafting and in the future could be used to predict rubber production by latex analysis.

  18. Parent heparin and daughter LMW heparin correlation analysis using LC-MS and NMR

    International Nuclear Information System (INIS)

    Liu, Xinyue; St Ange, Kalib; Wang, Xiaohua; Lin, Lei; Zhang, Fuming

    2017-01-01

    on LC-MS and NMR analysis. • Monosaccharide compositional analysis relied on top-down NMR analysis. • Intact chain, oligosaccharide, and disaccharide analyses relied on LC-MS. • Differences due to parent heparin were observed using principal component analysis.

  19. Parent heparin and daughter LMW heparin correlation analysis using LC-MS and NMR

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Xinyue, E-mail: liux22@rpi.edu [National Glycoengineering Research Center, Shandong Provincial Key Laboratory of Carbohydrate Chemistry and Glycobiology, State Key Laboratory of Microbial Technology, Shandong University, Jinan, Shandong, 250100 (China); Department of Chemistry and Chemical Biology, Department of Chemical and Biological Engineering, Department of Biology, Department of Biomedical Engineering, Center for Biotechnology and Interdisciplinary Studies, Rensselaer Polytechnic Institute, Troy, NY, 12180 (United States); St Ange, Kalib, E-mail: stangk2@rpi.edu [Department of Chemistry and Chemical Biology, Department of Chemical and Biological Engineering, Department of Biology, Department of Biomedical Engineering, Center for Biotechnology and Interdisciplinary Studies, Rensselaer Polytechnic Institute, Troy, NY, 12180 (United States); Wang, Xiaohua, E-mail: wangx35@rpi.edu [Department of Chemistry and Chemical Biology, Department of Chemical and Biological Engineering, Department of Biology, Department of Biomedical Engineering, Center for Biotechnology and Interdisciplinary Studies, Rensselaer Polytechnic Institute, Troy, NY, 12180 (United States); School of Computer and Information, Hefei University of Technology, Hefei (China); Lin, Lei, E-mail: Linl5@rpi.edu [Department of Chemistry and Chemical Biology, Department of Chemical and Biological Engineering, Department of Biology, Department of Biomedical Engineering, Center for Biotechnology and Interdisciplinary Studies, Rensselaer Polytechnic Institute, Troy, NY, 12180 (United States); Zhang, Fuming, E-mail: zhangf2@rpi.edu [Department of Chemistry and Chemical Biology, Department of Chemical and Biological Engineering, Department of Biology, Department of Biomedical Engineering, Center for Biotechnology and Interdisciplinary Studies, Rensselaer Polytechnic Institute, Troy, NY, 12180 (United States); and others

    2017-04-08

    approach relied on LC-MS and NMR analysis. • Monosaccharide compositional analysis relied on top-down NMR analysis. • Intact chain, oligosaccharide, and disaccharide analyses relied on LC-MS. • Differences due to parent heparin were observed using principal component analysis.

  20. Use of optimized 1D TOCSY NMR for improved quantitation and metabolomic analysis of biofluids

    International Nuclear Information System (INIS)

    Sandusky, Peter; Appiah-Amponsah, Emmanuel; Raftery, Daniel

    2011-01-01

    One dimensional selective TOCSY experiments have been shown to be advantageous in providing improved data inputs for principle component analysis (PCA) (Sandusky and Raftery 2005a, b). Better subpopulation cluster resolution in the observed scores plots results from the ability to isolate metabolite signals of interest via the TOCSY based filtering approach. This report reexamines the quantitative aspects of this approach, first by optimizing the 1D TOCSY experiment as it relates to the measurement of biofluid constituent concentrations, and second by comparing the integration of 1D TOCSY read peaks to the bucket integration of 1D proton NMR spectra in terms of precision and accuracy. This comparison indicates that, because of the extensive peak overlap that occurs in the 1D proton NMR spectra of biofluid samples, bucket integrals are often far less accurate as measures of individual constituent concentrations than 1D TOCSY read peaks. Even spectral fitting approaches have proven difficult in the analysis of significantly overlapped spectral regions. Measurements of endogenous taurine made over a sample population of human urine demonstrates that, due to background signals from other constituents, bucket integrals of 1D proton spectra routinely overestimate the taurine concentrations and distort its variation over the sample population. As a result, PCA calculations performed using data matrices incorporating 1D TOCSY determined taurine concentrations produce better scores plot subpopulation cluster resolution.

  1. Use of optimized 1D TOCSY NMR for improved quantitation and metabolomic analysis of biofluids

    Energy Technology Data Exchange (ETDEWEB)

    Sandusky, Peter [Eckerd College, Department of Chemistry (United States); Appiah-Amponsah, Emmanuel; Raftery, Daniel, E-mail: raftery@purdue.edu [Purdue University, Department of Chemistry (United States)

    2011-04-15

    One dimensional selective TOCSY experiments have been shown to be advantageous in providing improved data inputs for principle component analysis (PCA) (Sandusky and Raftery 2005a, b). Better subpopulation cluster resolution in the observed scores plots results from the ability to isolate metabolite signals of interest via the TOCSY based filtering approach. This report reexamines the quantitative aspects of this approach, first by optimizing the 1D TOCSY experiment as it relates to the measurement of biofluid constituent concentrations, and second by comparing the integration of 1D TOCSY read peaks to the bucket integration of 1D proton NMR spectra in terms of precision and accuracy. This comparison indicates that, because of the extensive peak overlap that occurs in the 1D proton NMR spectra of biofluid samples, bucket integrals are often far less accurate as measures of individual constituent concentrations than 1D TOCSY read peaks. Even spectral fitting approaches have proven difficult in the analysis of significantly overlapped spectral regions. Measurements of endogenous taurine made over a sample population of human urine demonstrates that, due to background signals from other constituents, bucket integrals of 1D proton spectra routinely overestimate the taurine concentrations and distort its variation over the sample population. As a result, PCA calculations performed using data matrices incorporating 1D TOCSY determined taurine concentrations produce better scores plot subpopulation cluster resolution.

  2. Phosphorus-31 NMR (nuclear magnetic resonance) analysis of gold plating baths

    Energy Technology Data Exchange (ETDEWEB)

    Smith, R.E.

    1990-01-01

    This report describes the nuclear magnetic resonance (NMR) analysis of the gold plating baths in the Micro-Miniature Electronic Assembly department of Allied-Signal Inc., Kansas City Division (KCD). The baths were analyzed for phosphorylated components. In freshly prepared gold plating baths, a 50-percent aqueous solution of aminotrimethylphosphonate (ATMP) is the principal compound observed. As the bath is used in production, the ATMP breaks down and new materials (phosphate, ADMP, and AMMP) are identified. The NMR method was used to monitor the concentrations of the ATMP and breakdown products for a nine-month period. The 225-liter bath had plated approximately 100 square feet of gold during the nine-month period. These results can be used to predict the performance of baths as they are used in production. The accuracy of the analysis is 96 percent for ATMP and 92 percent for phosphate. The precision (relative standard deviation) is 5.2 percent for ATMP and 4.5 percent for phosphate. 1 ref., 5 figs., 2 tabs.

  3. The Kepler Light Curves of AGN: A Detailed Analysis

    Science.gov (United States)

    Smith, Krista Lynne; Mushotzky, Richard F.; Boyd, Patricia T.; Malkan, Matt; Howell, Steve B.; Gelino, Dawn M.

    2018-04-01

    We present a comprehensive analysis of 21 light curves of Type 1 active galactic nuclei (AGN) from the Kepler spacecraft. First, we describe the necessity and development of a customized pipeline for treating Kepler data of stochastically variable sources like AGN. We then present the light curves, power spectral density functions (PSDs), and flux histograms. The light curves display an astonishing variety of behaviors, many of which would not be detected in ground-based studies, including switching between distinct flux levels. Six objects exhibit PSD flattening at characteristic timescales that roughly correlate with black hole mass. These timescales are consistent with orbital timescales or free-fall accretion timescales. We check for correlations of variability and high-frequency PSD slope with accretion rate, black hole mass, redshift, and luminosity. We find that bolometric luminosity is anticorrelated with both variability and steepness of the PSD slope. We do not find evidence of the linear rms–flux relationships or lognormal flux distributions found in X-ray AGN light curves, indicating that reprocessing is not a significant contributor to optical variability at the 0.1%–10% level.

  4. Principal components analysis of protein structure ensembles calculated using NMR data

    International Nuclear Information System (INIS)

    Howe, Peter W.A.

    2001-01-01

    One important problem when calculating structures of biomolecules from NMR data is distinguishing converged structures from outlier structures. This paper describes how Principal Components Analysis (PCA) has the potential to classify calculated structures automatically, according to correlated structural variation across the population. PCA analysis has the additional advantage that it highlights regions of proteins which are varying across the population. To apply PCA, protein structures have to be reduced in complexity and this paper describes two different representations of protein structures which achieve this. The calculated structures of a 28 amino acid peptide are used to demonstrate the methods. The two different representations of protein structure are shown to give equivalent results, and correct results are obtained even though the ensemble of structures used as an example contains two different protein conformations. The PCA analysis also correctly identifies the structural differences between the two conformations

  5. NMR-based Structural Analysis of Threonylcarbamoyl-AMP Synthase and Its Substrate Interactions.

    Science.gov (United States)

    Harris, Kimberly A; Bobay, Benjamin G; Sarachan, Kathryn L; Sims, Alexis F; Bilbille, Yann; Deutsch, Christopher; Iwata-Reuyl, Dirk; Agris, Paul F

    2015-08-14

    The hypermodified nucleoside N(6)-threonylcarbamoyladenosine (t(6)A37) is present in many distinct tRNA species and has been found in organisms in all domains of life. This post-transcriptional modification enhances translation fidelity by stabilizing the anticodon/codon interaction in the ribosomal decoding site. The biosynthetic pathway of t(6)A37 is complex and not well understood. In bacteria, the following four proteins have been discovered to be both required and sufficient for t(6)A37 modification: TsaC, TsaD, TsaB, and TsaE. Of these, TsaC and TsaD are members of universally conserved protein families. Although TsaC has been shown to catalyze the formation of L-threonylcarbamoyl-AMP, a key intermediate in the biosynthesis of t(6)A37, the details of the enzymatic mechanism remain unsolved. Therefore, the solution structure of Escherichia coli TsaC was characterized by NMR to further study the interactions with ATP and L-threonine, both substrates of TsaC in the biosynthesis of L-threonylcarbamoyl-AMP. Several conserved amino acids were identified that create a hydrophobic binding pocket for the adenine of ATP. Additionally, two residues were found to interact with L-threonine. Both binding sites are located in a deep cavity at the center of the protein. Models derived from the NMR data and molecular modeling reveal several sites with considerable conformational flexibility in TsaC that may be important for L-threonine recognition, ATP activation, and/or protein/protein interactions. These observations further the understanding of the enzymatic reaction catalyzed by TsaC, a threonylcarbamoyl-AMP synthase, and provide structure-based insight into the mechanism of t(6)A37 biosynthesis. © 2015 by The American Society for Biochemistry and Molecular Biology, Inc.

  6. Structural Analysis of N- and O-glycans Using ZIC-HILIC/Dialysis Coupled to NMR Detection

    Energy Technology Data Exchange (ETDEWEB)

    Qu, Yi; Feng, Ju; Deng, Shuang; Cao, Li; Zhang, Qibin; Zhao, Rui; Zhang, Zhaorui; Jiang, Yuxuan; Zink, Erika M.; Baker, Scott E.; Lipton, Mary S.; Pasa-Tolic, Ljiljana; Hu, Jian Z.; Wu, Si

    2014-11-19

    Protein glycosylation, an important and complex post-translational modification (PTM), is involved in various biological processes including the receptor-ligand and cell-cell interaction, and plays a crucial role in many biological functions. However, little is known about the glycan structures of important biological complex samples, and the conventional glycan enrichment strategy (i.e., size-exclusion column [SEC] separation,) prior to nuclear magnetic resonance (NMR) detection is time-consuming and tedious. In this study, we employed SEC, Zwitterionic hydrophilic interaction liquid chromatography (ZIC-HILIC), and ZIC-HILIC coupled with dialysis strategies to enrich the glycopeptides from the pronase E digests of RNase B, followed by NMR analysis of the glycoconjugate. Our results suggest that the ZIC-HILIC enrichment coupled with dialysis is the most efficient, which was thus applied to the analysis of biological complex sample, the pronase E digest of the secreted proteins from the fungi Aspergillus niger. The NMR spectra revealed that the secreted proteins from A. niger contain both N-linked glycans with a high-mannose core and O-linked glycans bearing mannose and glucose with 1->3 and 1->6 linkages. In all, our study provides compelling evidence that ZIC-HILIC separation coupled to dialysis is superior to the commonly used SEC separation to prepare glycopeptides for the downstream NMR analysis, which could greatly facilitate the future NMR-based glycoproteomics research.

  7. Simultaneous Gaussian and exponential inversion for improved analysis of shales by NMR relaxometry

    Science.gov (United States)

    Washburn, Kathryn E.; Anderssen, Endre; Vogt, Sarah J.; Seymour, Joseph D.; Birdwell, Justin E.; Kirkland, Catherine M.; Codd, Sarah L.

    2015-01-01

    Nuclear magnetic resonance (NMR) relaxometry is commonly used to provide lithology-independent porosity and pore-size estimates for petroleum resource evaluation based on fluid-phase signals. However in shales, substantial hydrogen content is associated with solid and fluid signals and both may be detected. Depending on the motional regime, the signal from the solids may be best described using either exponential or Gaussian decay functions. When the inverse Laplace transform, the standard method for analysis of NMR relaxometry results, is applied to data containing Gaussian decays, this can lead to physically unrealistic responses such as signal or porosity overcall and relaxation times that are too short to be determined using the applied instrument settings. We apply a new simultaneous Gaussian-Exponential (SGE) inversion method to simulated data and measured results obtained on a variety of oil shale samples. The SGE inversion produces more physically realistic results than the inverse Laplace transform and displays more consistent relaxation behavior at high magnetic field strengths. Residuals for the SGE inversion are consistently lower than for the inverse Laplace method and signal overcall at short T2 times is mitigated. Beyond geological samples, the method can also be applied in other fields where the sample relaxation consists of both Gaussian and exponential decays, for example in material, medical and food sciences.

  8. NMR spectroscopic and analytical ultracentrifuge analysis of membrane protein detergent complexes

    Directory of Open Access Journals (Sweden)

    Choe Senyon

    2007-11-01

    Full Text Available Abstract Background Structural studies of integral membrane proteins (IMPs are hampered by inherent difficulties in their heterologous expression and in the purification of solubilized protein-detergent complexes (PDCs. The choice and concentrations of detergents used in an IMP preparation play a critical role in protein homogeneity and are thus important for successful crystallization. Results Seeking an effective and standardized means applicable to genomic approaches for the characterization of PDCs, we chose 1D-NMR spectroscopic analysis to monitor the detergent content throughout their purification: protein extraction, detergent exchange, and sample concentration. We demonstrate that a single NMR measurement combined with a SDS-PAGE of a detergent extracted sample provides a useful gauge of the detergent's extraction potential for a given protein. Furthermore, careful monitoring of the detergent content during the process of IMP production allows for a high level of reproducibility. We also show that in many cases a simple sedimentation velocity measurement provides sufficient data to estimate both the oligomeric state and the detergent-to-protein ratio in PDCs, as well as to evaluate the homogeneity of the samples prior to crystallization screening. Conclusion The techniques presented here facilitate the screening and selection of the extraction detergent, as well as help to maintain reproducibility in the detergent exchange and PDC concentration procedures. Such reproducibility is particularly important for the optimization of initial crystallization conditions, for which multiple purifications are routinely required.

  9. Simultaneous Gaussian and exponential inversion for improved analysis of shales by NMR relaxometry

    Science.gov (United States)

    Washburn, Kathryn E.; Anderssen, Endre; Vogt, Sarah J.; Seymour, Joseph D.; Birdwell, Justin E.; Kirkland, Catherine M.; Codd, Sarah L.

    2014-01-01

    Nuclear magnetic resonance (NMR) relaxometry is commonly used to provide lithology-independent porosity and pore-size estimates for petroleum resource evaluation based on fluid-phase signals. However in shales, substantial hydrogen content is associated with solid and fluid signals and both may be detected. Depending on the motional regime, the signal from the solids may be best described using either exponential or Gaussian decay functions. When the inverse Laplace transform, the standard method for analysis of NMR relaxometry results, is applied to data containing Gaussian decays, this can lead to physically unrealistic responses such as signal or porosity overcall and relaxation times that are too short to be determined using the applied instrument settings. We apply a new simultaneous Gaussian-Exponential (SGE) inversion method to simulated data and measured results obtained on a variety of oil shale samples. The SGE inversion produces more physically realistic results than the inverse Laplace transform and displays more consistent relaxation behavior at high magnetic field strengths. Residuals for the SGE inversion are consistently lower than for the inverse Laplace method and signal overcall at short T2 times is mitigated. Beyond geological samples, the method can also be applied in other fields where the sample relaxation consists of both Gaussian and exponential decays, for example in material, medical and food sciences.

  10. Structural analysis of the exopolysaccharide produced by Streptococcus thermophilus ST1 solely by NMR spectroscopy

    International Nuclear Information System (INIS)

    Saewen, Elin; Huttunen, Eine; Zhang Xue; Yang Zhennai; Widmalm, Goeran

    2010-01-01

    The use of lactic acid bacteria in fermentation of milk results in favorable physical and rheological properties due to in situ exopolysaccharide (EPS) production. The EPS from S. thermophilus ST1 produces highly viscous aqueous solutions and its structure has been investigated by NMR spectroscopy. Notably, all aspects of the elucidation of its primary structure including component analysis and absolute configuration of the constituent monosaccharides were carried out by NMR spectroscopy. An array of techniques was utilized including, inter alia, PANSY and NOESY-HSQC TILT experiments. The EPS is composed of hexasaccharide repeating units with the following structure: → 3)[α-d-Glcp-(1 → 4)]-β-d-Galp-(1 → 4)-β-d-Glcp-(1 → 4)[β-d-Galf-(1 → 6)]-β-d-Glcp-(1 → 6)-β-d-Glcp-(1 → , in which the residues in square brackets are terminal groups substituting backbone sugar residues that consequently are branch-points in the repeating unit of the polymer. Thus, the EPS consists of a backbone of four sugar residues with two terminal sugar residues making up two side-chains of the repeating unit. The molecular mass of the polymer was determined using translational diffusion experiments which resulted in M w = 62 kDa, corresponding to 64 repeating units in the EPS.

  11. Structural analysis of the exopolysaccharide produced by Streptococcus thermophilus ST1 solely by NMR spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Saewen, Elin [Arrhenius Laboratory, Stockholm University, Department of Organic Chemistry (Sweden); Huttunen, Eine; Zhang Xue [University of Helsinki, Department of Food Technology (Finland); Yang Zhennai [Northeast Agricultural Research Center of China, Center of Agro-food Technology (China); Widmalm, Goeran, E-mail: gw@organ.su.s [Arrhenius Laboratory, Stockholm University, Department of Organic Chemistry (Sweden)

    2010-06-15

    The use of lactic acid bacteria in fermentation of milk results in favorable physical and rheological properties due to in situ exopolysaccharide (EPS) production. The EPS from S. thermophilus ST1 produces highly viscous aqueous solutions and its structure has been investigated by NMR spectroscopy. Notably, all aspects of the elucidation of its primary structure including component analysis and absolute configuration of the constituent monosaccharides were carried out by NMR spectroscopy. An array of techniques was utilized including, inter alia, PANSY and NOESY-HSQC TILT experiments. The EPS is composed of hexasaccharide repeating units with the following structure: {yields} 3)[{alpha}-d-Glcp-(1 {yields} 4)]-{beta}-d-Galp-(1 {yields} 4)-{beta}-d-Glcp-(1 {yields} 4)[{beta}-d-Galf-(1 {yields} 6)]-{beta}-d-Glcp-(1 {yields} 6)-{beta}-d-Glcp-(1 {sup {yields}}, in which the residues in square brackets are terminal groups substituting backbone sugar residues that consequently are branch-points in the repeating unit of the polymer. Thus, the EPS consists of a backbone of four sugar residues with two terminal sugar residues making up two side-chains of the repeating unit. The molecular mass of the polymer was determined using translational diffusion experiments which resulted in M{sub w} = 62 kDa, corresponding to 64 repeating units in the EPS.

  12. Extraction and [superscript 1]H NMR Analysis of Fats from Convenience Foods: A Laboratory Experiment for Organic Chemistry

    Science.gov (United States)

    Hartel, Aaron M.; Moore, Amy C.

    2014-01-01

    The extraction and analysis of fats from convenience foods (crackers, cookies, chips, candies) has been developed as an experiment for a second-year undergraduate organic chemistry laboratory course. Students gravimetrically determine the fat content per serving and then perform a [superscript 1]H NMR analysis of the recovered fat to determine the…

  13. 1 H NMR study and multivariate data analysis of reindeer skin tanning methods.

    Science.gov (United States)

    Zhu, Lizheng; Ilott, Andrew J; Del Federico, Eleonora; Kehlet, Cindie; Klokkernes, Torunn; Jerschow, Alexej

    2017-04-01

    Reindeer skin clothing has been an essential component in the lives of indigenous people of the arctic and sub-arctic regions, keeping them warm during harsh winters. However, the skin processing technology, which often conveys the history and tradition of the indigenous group, has not been well documented. In this study, NMR spectra and relaxation behaviors of reindeer skin samples treated with a variety of vegetable tannin extracts, oils and fatty substances are studied and compared. With the assistance of principal component analysis (PCA), one can recognize patterns and identify groupings of differently treated samples. These methods could be important aids in efforts to conserve museum leather artifacts with unknown treatment methods and in the analysis of reindeer skin tanning processes. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  14. 1H NMR quantification in very dilute toxin solutions: application to anatoxin-a analysis.

    Science.gov (United States)

    Dagnino, Denise; Schripsema, Jan

    2005-08-01

    A complete procedure is described for the extraction, detection and quantification of anatoxin-a in biological samples. Anatoxin-a is extracted from biomass by a routine acid base extraction. The extract is analysed by GC-MS, without the need of derivatization, with a detection limit of 0.5 ng. A method was developed for the accurate quantification of anatoxin-a in the standard solution to be used for the calibration of the GC analysis. 1H NMR allowed the accurate quantification of microgram quantities of anatoxin-a. The accurate quantification of compounds in standard solutions is rarely discussed, but for compounds like anatoxin-a (toxins with prices in the range of a million dollar a gram), of which generally only milligram quantities or less are available, this factor in the quantitative analysis is certainly not trivial. The method that was developed can easily be adapted for the accurate quantification of other toxins in very dilute solutions.

  15. Cool-Climate Red Wines—Chemical Composition and Comparison of Two Protocols for 1H–NMR Analysis

    Directory of Open Access Journals (Sweden)

    Violetta Aru

    2018-01-01

    Full Text Available This study investigates the metabolome of 26 experimental cool-climate wines made from 22 grape varieties using two different protocols for wine analysis by proton nuclear magnetic resonance (1H–NMR spectroscopy. The wine samples were analyzed as-is (wet and as dried samples. The NMR datasets were preprocessed by alignment and mean centering. No normalization or scaling was performed. The “wet” method preserved the inherent properties of the samples and provided a fast and effective overview of the molecular composition of the wines. The “dried” method yielded a slightly better sensitivity towards a broader range of the compounds present in wines. A total of 27 metabolites including amino acids, organic acids, sugars, and alkaloids were identified in the 1H–NMR spectra of the wine samples. Principal component analysis was performed on both NMR datasets evidencing well-defined molecular fingerprints for ‘Baco Noir’, ‘Bolero’, ‘Cabernet Cantor’, ‘Cabernet Cortis’, ‘Don Muscat’, ‘Eszter’, ‘Golubok’, ‘New York Muscat’, ‘Regent’, ‘Rondo’, ‘Triomphe d’Alsace’, ‘Précose Noir’, and ‘Vinoslivy’ wines. Amongst the identified metabolites, lactic acid, succinic acid, acetic acid, gallic acid, glycerol, and methanol were found to drive sample groupings. The 1H–NMR data was compared to the absolute concentration values obtained from a reference Fourier transform infrared method, evidencing a high correlation.

  16. Demetalation of Fe, Mn, and Cu chelates and complexes: application to the NMR analysis of micronutrient fertilizers.

    Science.gov (United States)

    López-Rayo, Sandra; Lucena, Juan J; Laghi, Luca; Cremonini, Mauro A

    2011-12-28

    The application of nuclear magnetic resonance (NMR) for the quality control of fertilizers based on Fe(3+), Mn(2+), and Cu(2+) chelates and complexes is precluded by the strong paramagnetism of metals. Recently, a method based on the use of ferrocyanide has been described to remove iron from commercial iron chelates based on the o,o-EDDHA [ethylenediamine-N,N'bis(2-hydroxyphenylacetic)acid] chelating agent for their analysis and quantification by NMR. The present work extended that procedure to other paramagnetic ions, manganese and copper, and other chelating, EDTA (ethylenediaminetetraacetic acid), IDHA [N-(1,2-dicarboxyethyl)-d,l-aspartic acid], and complexing agents, gluconate and heptagluconate. Results showed that the removal of the paramagnetic ions was complete, allowing us to obtain (1)H NMR spectra characterized by narrow peaks. The quantification of the ligands by NMR and high-performance liquid chromatography showed that their complete recovery was granted. The NMR analysis enabled detection and quantification of unknown impurities without the need of pure compounds as internal standards.

  17. relaxGUI: a new software for fast and simple NMR relaxation data analysis and calculation of ps-ns and μs motion of proteins

    International Nuclear Information System (INIS)

    Bieri, Michael; D’Auvergne, Edward J.; Gooley, Paul R.

    2011-01-01

    Investigation of protein dynamics on the ps-ns and μs-ms timeframes provides detailed insight into the mechanisms of enzymes and the binding properties of proteins. Nuclear magnetic resonance (NMR) is an excellent tool for studying protein dynamics at atomic resolution. Analysis of relaxation data using model-free analysis can be a tedious and time consuming process, which requires good knowledge of scripting procedures. The software relaxGUI was developed for fast and simple model-free analysis and is fully integrated into the software package relax. It is written in Python and uses wxPython to build the graphical user interface (GUI) for maximum performance and multi-platform use. This software allows the analysis of NMR relaxation data with ease and the generation of publication quality graphs as well as color coded images of molecular structures. The interface is designed for simple data analysis and management. The software was tested and validated against the command line version of relax.

  18. relaxGUI: a new software for fast and simple NMR relaxation data analysis and calculation of ps-ns and μs motion of proteins.

    Science.gov (United States)

    Bieri, Michael; d'Auvergne, Edward J; Gooley, Paul R

    2011-06-01

    Investigation of protein dynamics on the ps-ns and μs-ms timeframes provides detailed insight into the mechanisms of enzymes and the binding properties of proteins. Nuclear magnetic resonance (NMR) is an excellent tool for studying protein dynamics at atomic resolution. Analysis of relaxation data using model-free analysis can be a tedious and time consuming process, which requires good knowledge of scripting procedures. The software relaxGUI was developed for fast and simple model-free analysis and is fully integrated into the software package relax. It is written in Python and uses wxPython to build the graphical user interface (GUI) for maximum performance and multi-platform use. This software allows the analysis of NMR relaxation data with ease and the generation of publication quality graphs as well as color coded images of molecular structures. The interface is designed for simple data analysis and management. The software was tested and validated against the command line version of relax.

  19. Straightforward and complete deposition of NMR data to the PDBe

    International Nuclear Information System (INIS)

    Penkett, Christopher J.; Ginkel, Glen van; Velankar, Sameer; Swaminathan, Jawahar; Ulrich, Eldon L.; Mading, Steve; Stevens, Tim J.; Fogh, Rasmus H.; Gutmanas, Aleksandras; Kleywegt, Gerard J.; Henrick, Kim; Vranken, Wim F.

    2010-01-01

    We present a suite of software for the complete and easy deposition of NMR data to the PDB and BMRB. This suite uses the CCPN framework and introduces a freely downloadable, graphical desktop application called CcpNmr Entry Completion Interface (ECI) for the secure editing of experimental information and associated datasets through the lifetime of an NMR project. CCPN projects can be created within the CcpNmr Analysis software or by importing existing NMR data files using the CcpNmr FormatConverter. After further data entry and checking with the ECI, the project can then be rapidly deposited to the PDBe using AutoDep, or exported as a complete deposition NMR-STAR file. In full CCPN projects created with ECI, it is straightforward to select chemical shift lists, restraint data sets, structural ensembles and all relevant associated experimental collection details, which all are or will become mandatory when depositing to the PDB. Instructions and download information for the ECI are available from the PDBe web site at http://www.ebi.ac.uk/pdbe/nmr/deposition/eci.htmlhttp://www.ebi.ac.uk/pdbe/nmr/deposition/eci.html.

  20. NMR investigations of molecular dynamics

    Science.gov (United States)

    Palmer, Arthur

    2011-03-01

    NMR spectroscopy is a powerful experimental approach for characterizing protein conformational dynamics on multiple time scales. The insights obtained from NMR studies are complemented and by molecular dynamics (MD) simulations, which provide full atomistic details of protein dynamics. Homologous mesophilic (E. coli) and thermophilic (T. thermophilus) ribonuclease H (RNase H) enzymes serve to illustrate how changes in protein sequence and structure that affect conformational dynamic processes can be monitored and characterized by joint analysis of NMR spectroscopy and MD simulations. A Gly residue inserted within a putative hinge between helices B and C is conserved among thermophilic RNases H, but absent in mesophilic RNases H. Experimental spin relaxation measurements show that the dynamic properties of T. thermophilus RNase H are recapitulated in E. coli RNase H by insertion of a Gly residue between helices B and C. Additional specific intramolecular interactions that modulate backbone and sidechain dynamical properties of the Gly-rich loop and of the conserved Trp residue flanking the Gly insertion site have been identified using MD simulations and subsequently confirmed by NMR spin relaxation measurements. These results emphasize the importance of hydrogen bonds and local steric interactions in restricting conformational fluctuations, and the absence of such interactions in allowing conformational adaptation to substrate binding.

  1. [Non-invasive analysis of proteins in living cells using NMR spectroscopy].

    Science.gov (United States)

    Tochio, Hidehito; Murayama, Shuhei; Inomata, Kohsuke; Morimoto, Daichi; Ohno, Ayako; Shirakawa, Masahiro

    2015-01-01

    NMR spectroscopy enables structural analyses of proteins and has been widely used in the structural biology field in recent decades. NMR spectroscopy can be applied to proteins inside living cells, allowing characterization of their structures and dynamics in intracellular environments. The simplest "in-cell NMR" approach employs bacterial cells; in this approach, live Escherichia coli cells overexpressing a specific protein are subjected to NMR. The cells are grown in an NMR active isotope-enriched medium to ensure that the overexpressed proteins are labeled with the stable isotopes. Thus the obtained NMR spectra, which are derived from labeled proteins, contain atomic-level information about the structure and dynamics of the proteins. Recent progress enables us to work with higher eukaryotic cells such as HeLa and HEK293 cells, for which a number of techniques have been developed to achieve isotope labeling of the specific target protein. In this review, we describe successful use of electroporation for in-cell NMR. In addition, (19)F-NMR to characterize protein-ligand interactions in cells is presented. Because (19)F nuclei rarely exist in natural cells, when (19)F-labeled proteins are delivered into cells and (19)F-NMR signals are observed, one can safely ascertain that these signals originate from the delivered proteins and not other molecules.

  2. Untargeted NMR Spectroscopic Analysis of the Metabolic Variety of New Apple Cultivars

    Directory of Open Access Journals (Sweden)

    Philipp Eisenmann

    2016-09-01

    Full Text Available Metabolome analyses by NMR spectroscopy can be used in quality control by generating unique fingerprints of different species. Hundreds of components and their variation between different samples can be analyzed in a few minutes/hours with high accuracy and low cost of sample preparation. Here, apple peel and pulp extracts of a variety of apple cultivars were studied to assess their suitability to discriminate between the different varieties. The cultivars comprised mainly newly bred varieties or ones that were brought onto the market in recent years. Multivariate analyses of peel and pulp extracts were able to unambiguously identify all cultivars, with peel extracts showing a higher discriminative power. The latter was increased if the highly concentrated sugar metabolites were omitted from the analysis. Whereas sugar concentrations lay within a narrow range, polyphenols, discussed as potential health promoting substances, and acids varied remarkably between the cultivars.

  3. Analysis of ZDDP Content and Thermal Decomposition in Motor Oils Using NAA and NMR

    Science.gov (United States)

    Ferguson, S.; Johnson, J.; Gonzales, D.; Hobbs, C.; Allen, C.; Williams, S.

    Zinc dialkyldithiophosphates (ZDDPs) are one of the most common anti-wear additives present in commercially-available motor oils. The ZDDP concentrations of motor oils are most commonly determined using inductively coupled plasma atomic emission spectroscopy (ICP-AES). As part of an undergraduate research project, we have determined the Zn concentrations of eight commercially-available motor oils and one oil additive using neutron activation analysis (NAA), which has potential for greater accuracy and less sensitivity to matrix effects as compared to ICP-AES. The 31P nuclear magnetic resonance (31P-NMR) spectra were also obtained for several oil additive samples which have been heated to various temperatures in order to study the thermal decomposition of ZDDPs.

  4. Tannin structural elucidation and quantitative ³¹P NMR analysis. 1. Model compounds.

    Science.gov (United States)

    Melone, Federica; Saladino, Raffaele; Lange, Heiko; Crestini, Claudia

    2013-10-02

    Tannins and flavonoids are secondary metabolites of plants that display a wide array of biological activities. This peculiarity is related to the inhibition of extracellular enzymes that occurs through the complexation of peptides by tannins. Not only the nature of these interactions, but more fundamentally also the structure of these heterogeneous polyphenolic molecules are not completely clear. This first paper describes the development of a new analytical method for the structural characterization of tannins on the basis of tannin model compounds employing an in situ labeling of all labile H groups (aliphatic OH, phenolic OH, and carboxylic acids) with a phosphorus reagent. The ³¹P NMR analysis of ³¹P-labeled samples allowed the unprecedented quantitative and qualitative structural characterization of hydrolyzable tannins, proanthocyanidins, and catechin tannin model compounds, forming the foundations for the quantitative structural elucidation of a variety of actual tannin samples described in part 2 of this series.

  5. BnmrOffice: A Free Software for β-nmr Data Analysis

    Science.gov (United States)

    Saadaoui, Hassan

    A data-analysis framework with a graphical user interface (GUI) is developed to analyze β-nmr spectra in an automated and intuitive way. This program, named BnmrOffice is written in C++ and employs the QT libraries and tools for designing the GUI, and the CERN's Minuit optimization routines for minimization. The program runs under multiple platforms, and is available for free under the terms of the GNU GPL standards. The GUI is structured in tabs to search, plot and analyze data, along other functionalities. The user can tweak the minimization options; and fit multiple data files (or runs) using single or global fitting routines with pre-defined or new models. Currently, BnmrOffice reads TRIUMF's MUD data and ASCII files, and can be extended to other formats.

  6. Analysis of Hydroperoxides in Solid Polyethylene by MAS (13)C NMR and EPR

    International Nuclear Information System (INIS)

    ASSINK, ROGER A.; CELINA, MATHIAS C.; DUNBAR, TIMOTHY D.; ALAM, TODD M.; CLOUGH, ROGER LEE; GILLEN, KENNETH T.

    1999-01-01

    13 C-enriched polyethylene was subjected to γ-irradiation in the presence of air at 25 and 80 C for total doses ranging from 71 to 355 kGy. Significant quantities of hydroperoxides were detected in the 25 C irradiated sample by 13 C magic angle spinning NMR spectroscopy. This method of detection was performed on the solid polymer and required no chemical derivatization or addition of solvent. The chemical stability and subsequent products of the hydroperoxide species were studied by annealing the irradiated samples in air at temperatures ranging from 22 to 110 C. A time-temperature superposition analysis provided an activation energy of 108 kJ/mol for the hydroperoxide decomposition process. The primary products of hydroperoxide decomposition were ketones and secondary alcohols with lesser amounts of acids and esters. EPR measurements suggest that the reactive hydroperoxide species reside in the amorphous phase of polyethylene, consistent with degradation occurring in the amorphous phase

  7. Detection of counterfeit brand spirits using 1H NMR fingerprints in comparison to sensory analysis.

    Science.gov (United States)

    Kuballa, Thomas; Hausler, Thomas; Okaru, Alex O; Neufeld, Maria; Abuga, Kennedy O; Kibwage, Isaac O; Rehm, Jürgen; Luy, Burkhard; Walch, Stephan G; Lachenmeier, Dirk W

    2018-04-15

    Beverage fraud involving counterfeiting of brand spirits is an increasing problem not only due to deception of the consumer but also because it poses health risks e.g. from possible methanol admixture. Suspicious spirit samples from Russia and Kenya were analysed using 1 H nuclear magnetic resonance (NMR) spectroscopy in comparison to authentic products. Using linear regression analysis of spectral integral values, 4 counterfeited samples from Russia and 2 from Kenya were easily identifiable with R 2  counterfeited and authentic samples but the assessors were unable to correctly identify the counterfeited product in the majority of cases. An important conclusion is that consumers cannot assumed to be self-responsible when consuming counterfeit alcohol because there is no general ability to organoleptically detect counterfeit alcohol. Copyright © 2017 Elsevier Ltd. All rights reserved.

  8. Whole Blood Reveals More Metabolic Detail of the Human Metabolome than Serum as Measured by 1H-NMR Spectroscopy: Implications for Sepsis Metabolomics

    Science.gov (United States)

    Stringer, Kathleen A.; Younger, John G.; McHugh, Cora; Yeomans, Larisa; Finkel, Michael A.; Puskarich, Michael A.; Jones, Alan E.; Trexel, Julie; Karnovsky, Alla

    2015-01-01

    Serum is a common sample of convenience for metabolomics studies. Its processing time can be lengthy and may result in the loss of metabolites including those of red blood cells (RBC). Unlike serum, whole blood (WB) is quickly processed, minimizing the influence of variable hemolysis while including RBC metabolites. To determine differences between serum and WB metabolomes, both sample types, collected from healthy volunteers, were assayed by 1H-NMR spectroscopy. A total of 34 and 50 aqueous metabolites were quantified from serum and WB, respectively. Free hemoglobin (Hgb) levels in serum were measured and the correlation between Hgb and metabolite concentrations was determined. All metabolites detected in serum were at higher concentrations in WB with the exception of acetoacetate and propylene glycol. The 18 unique metabolites of WB included adenosine, AMP, ADP and ATP, which are associated with RBC metabolism. The use of serum results in the underrepresentation of a number of metabolic pathways including branched chain amino acid degradation and glycolysis and gluconeogenesis. The range of free Hgb in serum was 0.03-0.01 g/dL and 8 metabolites were associated (p ≤ 0.05) with free Hgb. The range of free Hgb in serum samples from 18 sepsis patients was 0.02-0.46 g/dL. WB and serum have unique aqueous metabolite profiles but the use of serum may introduce potential pathway bias. Use of WB for metabolomics may be particularly important for studies in diseases like sepsis in which RBC metabolism is altered and mechanical and sepsis-induced hemolysis contributes to variance in the metabolome. PMID:26009817

  9. Reproducibility of NMR analysis of urine samples: impact of sample preparation, storage conditions, and animal health status.

    Science.gov (United States)

    Schreier, Christina; Kremer, Werner; Huber, Fritz; Neumann, Sindy; Pagel, Philipp; Lienemann, Kai; Pestel, Sabine

    2013-01-01

    Spectroscopic analysis of urine samples from laboratory animals can be used to predict the efficacy and side effects of drugs. This employs methods combining (1)H NMR spectroscopy with quantification of biomarkers or with multivariate data analysis. The most critical steps in data evaluation are analytical reproducibility of NMR data (collection, storage, and processing) and the health status of the animals, which may influence urine pH and osmolarity. We treated rats with a solvent, a diuretic, or a nephrotoxicant and collected urine samples. Samples were titrated to pH 3 to 9, or salt concentrations increased up to 20-fold. The effects of storage conditions and freeze-thaw cycles were monitored. Selected metabolites and multivariate data analysis were evaluated after (1)H NMR spectroscopy. We showed that variation of pH from 3 to 9 and increases in osmolarity up to 6-fold had no effect on the quantification of the metabolites or on multivariate data analysis. Storage led to changes after 14 days at 4°C or after 12 months at -20°C, independent of sample composition. Multiple freeze-thaw cycles did not affect data analysis. Reproducibility of NMR measurements is not dependent on sample composition under physiological or pathological conditions.

  10. Reproducibility of NMR Analysis of Urine Samples: Impact of Sample Preparation, Storage Conditions, and Animal Health Status

    Directory of Open Access Journals (Sweden)

    Christina Schreier

    2013-01-01

    Full Text Available Introduction. Spectroscopic analysis of urine samples from laboratory animals can be used to predict the efficacy and side effects of drugs. This employs methods combining 1H NMR spectroscopy with quantification of biomarkers or with multivariate data analysis. The most critical steps in data evaluation are analytical reproducibility of NMR data (collection, storage, and processing and the health status of the animals, which may influence urine pH and osmolarity. Methods. We treated rats with a solvent, a diuretic, or a nephrotoxicant and collected urine samples. Samples were titrated to pH 3 to 9, or salt concentrations increased up to 20-fold. The effects of storage conditions and freeze-thaw cycles were monitored. Selected metabolites and multivariate data analysis were evaluated after 1H NMR spectroscopy. Results. We showed that variation of pH from 3 to 9 and increases in osmolarity up to 6-fold had no effect on the quantification of the metabolites or on multivariate data analysis. Storage led to changes after 14 days at 4°C or after 12 months at −20°C, independent of sample composition. Multiple freeze-thaw cycles did not affect data analysis. Conclusion. Reproducibility of NMR measurements is not dependent on sample composition under physiological or pathological conditions.

  11. Crystallinity and compositional changes in carbonated apatites: Evidence from 31P solid-state NMR, Raman, and AFM analysis

    Science.gov (United States)

    McElderry, John-David P.; Zhu, Peizhi; Mroue, Kamal H.; Xu, Jiadi; Pavan, Barbara; Fang, Ming; Zhao, Guisheng; McNerny, Erin; Kohn, David H.; Franceschi, Renny T.; Holl, Mark M. Banaszak; Tecklenburg, Mary M. J.; Ramamoorthy, Ayyalusamy; Morris, Michael D.

    2013-10-01

    Solid-state (magic-angle spinning) NMR spectroscopy is a useful tool for obtaining structural information on bone organic and mineral components and synthetic model minerals at the atomic-level. Raman and 31P NMR spectral parameters were investigated in a series of synthetic B-type carbonated apatites (CAps). Inverse 31P NMR linewidth and inverse Raman PO43-ν1 bandwidth were both correlated with powder XRD c-axis crystallinity over the 0.3-10.3 wt% CO32- range investigated. Comparison with bone powder crystallinities showed agreement with values predicted by NMR and Raman calibration curves. Carbonate content was divided into two domains by the 31P NMR chemical shift frequency and the Raman phosphate ν1 band position. These parameters remain stable except for an abrupt transition at 6.5 wt% carbonate, a composition which corresponds to an average of one carbonate per unit cell. This near-binary distribution of spectroscopic properties was also found in AFM-measured particle sizes and Ca/P molar ratios by elemental analysis. We propose that this transition differentiates between two charge-balancing ion-loss mechanisms as measured by Ca/P ratios. These results define a criterion for spectroscopic characterization of B-type carbonate substitution in apatitic minerals.

  12. Simultaneous analysis of amino acid and organic acid by NMR spectrometry, 2. Diagnostic aids for inborn error of metabolism

    Energy Technology Data Exchange (ETDEWEB)

    Koda, Naoya; Yamaguchi, Shuichi; Mori, Takeshi.

    1987-09-01

    Analysis of urine from patients with inborn error of metabolism were studied by /sup 1/H-nuclear magnetic resonance (NMR) spectrometry. Diseases studied were as follows; phenylketonuria, biotin responsive multiple carboxylase deficiency, non-ketotic hyperglycinemia, 3-ketothiolase deficiency, alkaptonuria, methylmalonic acidemia, isovaleric acidemia, glutaric aciduria, argininosuccinic aciduria and hyperornithinemia. In each disease, specific metabolites in urine were recognized by NMR spectrometry. This method is accomplished within 10 minutes with non-treated small volume of urine and will be successfully available for the screening andor diagnosis of inherited metabolic diseases of amino acid and organic acid.

  13. Structure determination of the single glycan of rabbit serotransferrin by methylation analysis and 360 MHz /sup 1/H NMR spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Leger, D; Tordera, V; Spik, G [Lille-1 Univ., 59 - Villeneuve-d' Ascq (France); Dorland, L; Haverkamp, J; Vliegenthart, J F.G. [Rijksuniversiteit Utrecht (Netherlands)

    1978-09-15

    The glycopeptide fraction of rabbit serotransferrin (STF) has been investigated applying an original method for the determination of glycan primary structure combining monosaccharide determination, permethylation and 360 MHz /sup 1/H NMR. It is concluded that the highly purified rabbit transferrin contains only 1 glycan chain/molecule. A heterogeneity of the glycan moiety in the sialic acid residues was observed on isolation by paper electrophoresis of a disialylglycopeptide G-1 and a monosialylglycopeptide 2. The primary structure of glycopeptide G-1 deduced on the basis of the data of carbohydrate composition, permethylation analysis and 360 MHz /sup 1/H NMR spectroscopy is identical to the primary structure of human serotransferrin glycan and the glycopeptide G-2 was shown by /sup 1/H NMR spectroscopy, to be a mixture of two isomeric monosialylglycopeptides.

  14. Structure determination of the single glycan of rabbit serotransferrin by methylation analysis and 360 MHz 1H NMR spectroscopy

    International Nuclear Information System (INIS)

    Leger, D.; Tordera, V.; Spik, G.; Dorland, L.; Haverkamp, J.; Vliegenthart, J.F.G.

    1978-01-01

    The glycopeptide fraction of rabbit serotransferrin (STF) has been investigated applying an original method for the determination of glycan primary structure combining monosaccharide determination, permethylation and 360 MHz 1 H NMR. It is concluded that the highly purified rabbit transferrin contains only 1 glycan chain/molecule. A heterogeneity of the glycan moiety in the sialic acid residues was observed on isolation by paper electrophoresis of a disialylglycopeptide G-1 and a monosialylglycopeptide 2. The primary structure of glycopeptide G-1 deduced on the basis of the data of carbohydrate composition, permethylation analysis and 360 MHz 1 H NMR spectroscopy is identical to the primary structure of human serotransferrin glycan and the glycopeptide G-2 was shown by 1 H NMR spectroscopy, to be a mixture of two isomeric monosialylglycopeptides. (Auth.)

  15. NMR and IR Spectroscopy for the Structural Characterization of Edible Fats and Oils: An Instrumental Analysis Laboratory

    Science.gov (United States)

    Crowther, Molly W.

    2008-01-01

    This article describes an upper-level instrumental laboratory for undergraduates that explores the complementary nature of IR and NMR spectroscopy for analysis of several edible fats and oils that are structurally similar but differ in physical properties and health implications. Five different fats and oils are analyzed for average chain length,…

  16. A Solid-State NMR Experiment: Analysis of Local Structural Environments in Phosphate Glasses

    Science.gov (United States)

    Anderson, Stanley E.; Saiki, David; Eckert, Hellmut; Meise-Gresch, Karin

    2004-01-01

    An experiment that can be used to directly study the local chemical environments of phosphorus in solid amorphous materials is demonstrated. The experiment aims at familiarizing the students of chemistry with the principles of solid-state NMR, by having them synthesize a simple phosphate glass, and making them observe the (super 31)P NMR spectrum,…

  17. NMR-based lipidomic analysis of blood lipoproteins differentiates the progression of coronary heart disease.

    Science.gov (United States)

    Kostara, Christina E; Papathanasiou, Athanasios; Psychogios, Nikolaos; Cung, Manh Thong; Elisaf, Moses S; Goudevenos, John; Bairaktari, Eleni T

    2014-05-02

    Abnormal lipid composition and metabolism of plasma lipoproteins play a crucial role in the pathogenesis of coronary heart disease (CHD). A (1)H NMR-based lipidomic approach was used to investigate the correlation of coronary artery stenosis with the atherogenic (non-HDL) and atheroprotective (HDL) lipid profiles in 99 patients with CHD of various stages of disease and compared with 60 patients with normal coronary arteries (NCA), all documented in coronary angiography. The pattern recognition models created from lipid profiles predicted the presence of CHD with a sensitivity of 87% and a specificity of 88% in the HDL model and with 90% and 89% in the non-HDL model, respectively. Patients with mild, moderate, and severe coronary artery stenosis were progressively differentiated from those with NCA in the non-HDL model with a statistically significant separation of severe stage from both mild and moderate. In the HDL model, the progressive differentiation of the disease stages was statistically significant only between patients with mild and severe coronary artery stenosis. The lipid constituents of lipoproteins that mainly characterized the initial stages and then the progression of the disease were the high levels of saturated fatty acids in lipids in both HDL and non-HDL particles, the low levels of HDL-phosphatidylcholine, HDL-sphingomyelin, and omega-3 fatty acids and linoleic acid in lipids in non-HDL particles. The conventional lipid marker, total cholesterol, found in low levels in HDL and in high levels in non-HDL, also contributed to the onset of the disease but with a much lower coefficient of significance. (1)H NMR-based lipidomic analysis of atherogenic and atheroprotective lipoproteins could contribute to the early evaluation of the onset of coronary artery disease and possibly to the establishment of an appropriate therapeutic option.

  18. Analysis of Polycyclic Aromatic Hydrocarbon (PAH Mixtures Using Diffusion-Ordered NMR Spectroscopy and Adsorption by Powdered Activated Carbon and Biochar

    Directory of Open Access Journals (Sweden)

    Dong An

    2018-03-01

    Full Text Available Analysis of polycyclic aromatic hydrocarbons (PAHs in air and water sources is a key part of environmental chemistry research, since most PAHs are well known to be associated with negative health impacts on humans. This study explores an approach for analyzing PAH mixtures with advanced nuclear magnetic resonance (NMR spectroscopic techniques including high-resolution one-dimensional (1D NMR spectroscopy and diffusion-ordered NMR spectroscopy (DOSY NMR. With this method, different kinds of PAHs can be detected and differentiated from a mixture with high resolution. The adsorption process of PAH mixtures by PAC and biochar was studied to understand the mechanism and assess the method.

  19. Compositional differences among Chinese soy sauce types studied by (13)C NMR spectroscopy coupled with multivariate statistical analysis.

    Science.gov (United States)

    Kamal, Ghulam Mustafa; Wang, Xiaohua; Bin Yuan; Wang, Jie; Sun, Peng; Zhang, Xu; Liu, Maili

    2016-09-01

    Soy sauce a well known seasoning all over the world, especially in Asia, is available in global market in a wide range of types based on its purpose and the processing methods. Its composition varies with respect to the fermentation processes and addition of additives, preservatives and flavor enhancers. A comprehensive (1)H NMR based study regarding the metabonomic variations of soy sauce to differentiate among different types of soy sauce available on the global market has been limited due to the complexity of the mixture. In present study, (13)C NMR spectroscopy coupled with multivariate statistical data analysis like principle component analysis (PCA), and orthogonal partial least square-discriminant analysis (OPLS-DA) was applied to investigate metabonomic variations among different types of soy sauce, namely super light, super dark, red cooking and mushroom soy sauce. The main additives in soy sauce like glutamate, sucrose and glucose were easily distinguished and quantified using (13)C NMR spectroscopy which were otherwise difficult to be assigned and quantified due to serious signal overlaps in (1)H NMR spectra. The significantly higher concentration of sucrose in dark, red cooking and mushroom flavored soy sauce can directly be linked to the addition of caramel in soy sauce. Similarly, significantly higher level of glutamate in super light as compared to super dark and mushroom flavored soy sauce may come from the addition of monosodium glutamate. The study highlights the potentiality of (13)C NMR based metabonomics coupled with multivariate statistical data analysis in differentiating between the types of soy sauce on the basis of level of additives, raw materials and fermentation procedures. Copyright © 2016 Elsevier B.V. All rights reserved.

  20. NMR-based metabonomics and correlation analysis reveal potential biomarkers associated with chronic atrophic gastritis.

    Science.gov (United States)

    Cui, Jiajia; Liu, Yuetao; Hu, Yinghuan; Tong, Jiayu; Li, Aiping; Qu, Tingli; Qin, Xuemei; Du, Guanhua

    2017-01-05

    Chronic atrophic gastritis (CAG) is one of the most important pre-cancerous states with a high prevalence. Exploring of the underlying mechanism and potential biomarkers is of significant importance for CAG. In the present work, 1 H NMR-based metabonomics with correlative analysis was performed to analyze the metabolic features of CAG. 19 plasma metabolites and 18 urine metabolites were enrolled to construct the circulatory and excretory metabolome of CAG, which was in response to alterations of energy metabolism, inflammation, immune dysfunction, as well as oxidative stress. 7 plasma biomarkers and 7 urine biomarkers were screened to elucidate the pathogenesis of CAG based on the further correlation analysis with biochemical indexes. Finally, 3 plasma biomarkers (arginine, succinate and 3-hydroxybutyrate) and 2 urine biomarkers (α-ketoglutarate and valine) highlighted the potential to indicate risks of CAG in virtue of correlation with pepsin activity and ROC analysis. Here, our results paved a way for elucidating the underlying mechanisms in the development of CAG, and provided new avenues for the diagnosis of CAG and presented potential drug targets for treatment of CAG. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. 1H NMR Spectroscopy and MVA Analysis of Diplodus sargus Eating the Exotic Pest Caulerpa cylindracea.

    Science.gov (United States)

    De Pascali, Sandra A; Del Coco, Laura; Felline, Serena; Mollo, Ernesto; Terlizzi, Antonio; Fanizzi, Francesco P

    2015-06-05

    The green alga Caulerpa cylindracea is a non-autochthonous and invasive species that is severely affecting the native communities in the Mediterranean Sea. Recent researches show that the native edible fish Diplodus sargus actively feeds on this alga and cellular and physiological alterations have been related to the novel alimentary habits. The complex effects of such a trophic exposure to the invasive pest are still poorly understood. Here we report on the metabolic profiles of plasma from D. sargus individuals exposed to C. cylindracea along the southern Italian coast, using 1H NMR spectroscopy and multivariate analysis (Principal Component Analysis, PCA, Orthogonal Partial Least Square, PLS, and Orthogonal Partial Least Square Discriminant Analysis, OPLS-DA). Fish were sampled in two seasonal periods from three different locations, each characterized by a different degree of algal abundance. The levels of the algal bisindole alkaloid caulerpin, which is accumulated in the fish tissues, was used as an indicator of the trophic exposure to the seaweed and related to the plasma metabolic profiles. The profiles appeared clearly influenced by the sampling period beside the content of caulerpin, while the analyses also supported a moderate alteration of lipid and choline metabolism related to the Caulerpa-based diet.

  2. Functional studies using NMR

    International Nuclear Information System (INIS)

    McCready, V.R.; Leach, M.O.; Sutton; Ell, P.

    1986-01-01

    The object of this book is to discuss and evaluate an area of Nuclear Magnetic Resonance which to date has been less emphasized than it might be, namely the use of NMR for functional studies. The book commences with a discussion of the areas in which the NMR techniques might be needed due to deficiencies in other techniques. The physics of NMR especially relating to functional measurement are then explained. Technical factors in producing functional images are discussed and the use of paramagnetic substances for carrying out flow studies are detailed. Particular attention is paid to specific studies in the various organs. The book ends with a survey of imaging in each organ and the relation of NMR images to other techniques such as ultrasound, nuclear medicine and X-rays

  3. Two-Phase Extraction for Comprehensive Analysis of the Plant Metabolome by NMR.

    Science.gov (United States)

    Schripsema, Jan; Dagnino, Denise

    2018-01-01

    Metabolomics is the area of research, which strives to obtain complete metabolic fingerprints, to detect differences between them, and to provide hypothesis to explain those differences [1]. But obtaining complete metabolic fingerprints is not an easy task. Metabolite extraction is a key step during this process, and much research has been devoted to finding the best solvent mixture to extract as much metabolites as possible.Here a procedure is described for analysis of both polar and apolar metabolites using a two-phase extraction system. D 2 O and CDCl 3 are the solvents of choice, and their major advantage is that, for the identification of the compounds, standard databases can be used because D 2 O and CDCl 3 are the solvents most commonly used for pure compound NMR spectra. The procedure enables the absolute quantification of components via the addition of suitable internal standards. The extracts are also suitable for further analysis with other systems like LC-MS or GC-MS.

  4. NMR of unfolded proteins

    Indian Academy of Sciences (India)

    Unknown

    2005-01-03

    Jan 3, 2005 ... covering all the systems, so far discovered.5,7,8,12. With the increasing ... Structural investigations on proteins by NMR are, currently ... rapid analysis of unfolded proteins. ...... and hence help in design of drugs against them.

  5. Recommendations and Standardization of Biomarker Quantification Using NMR-based Metabolomics with Particular Focus on Urinary Analysis

    KAUST Repository

    Emwas, Abdul-Hamid M.

    2016-01-08

    NMR-based metabolomics has shown considerable promise in disease diagnosis and biomarker discovery because it allows one to non-destructively identify and quantify large numbers of novel metabolite biomarkers in both biofluids and tissues. Indeed, precise metabolite quantification is a necessary prerequisite to move any chemical biomarker or biomarker panel from the lab into the clinic. Among the many biofluids (urine, serum, plasma, cerebrospinal fluid and saliva) commonly used for disease diagnosis and prognosis, urine has several advantages. It is abundant, sterile, easily obtained, needs little sample preparation and does not require any invasive medical procedures for collection. Furthermore, urine captures and concentrates many “unwanted” or “undesirable” compounds throughout the body, thereby providing a rich source of potentially useful disease biomarkers. However, the incredible variation in urine chemical concentrations due to effects such as gender, age, diet, life style, health conditions, and physical activity make the analysis of urine and the identification of useful urinary biomarkers by NMR quite challenging. In this review, we discuss a number of the most significant issues regarding NMR-based urinary metabolomics with a specific emphasis on metabolite quantification for disease biomarker applications. We also propose a number of data collection and instrumental recommendations regarding NMR pulse sequences, acceptable acquisition parameter ranges, relaxation effects on quantitation, proper handling of instrumental differences, as well as recommendations regarding sample preparation and biomarker assessment.

  6. Recommendations and Standardization of Biomarker Quantification Using NMR-based Metabolomics with Particular Focus on Urinary Analysis

    KAUST Repository

    Emwas, Abdul-Hamid M.; Roy, Raja; McKay, Ryan T.; Ryan, Danielle; Brennan, Lorraine; Tenori, Leonardo; Luchinat, Claudio; Gao, Xin; Zeri, Ana Carolina; Gowda, G. A. Nagana; Raftery, Daniel; Steinbeck, Christoph; Salek, Reza M; Wishart, David S.

    2016-01-01

    NMR-based metabolomics has shown considerable promise in disease diagnosis and biomarker discovery because it allows one to non-destructively identify and quantify large numbers of novel metabolite biomarkers in both biofluids and tissues. Indeed, precise metabolite quantification is a necessary prerequisite to move any chemical biomarker or biomarker panel from the lab into the clinic. Among the many biofluids (urine, serum, plasma, cerebrospinal fluid and saliva) commonly used for disease diagnosis and prognosis, urine has several advantages. It is abundant, sterile, easily obtained, needs little sample preparation and does not require any invasive medical procedures for collection. Furthermore, urine captures and concentrates many “unwanted” or “undesirable” compounds throughout the body, thereby providing a rich source of potentially useful disease biomarkers. However, the incredible variation in urine chemical concentrations due to effects such as gender, age, diet, life style, health conditions, and physical activity make the analysis of urine and the identification of useful urinary biomarkers by NMR quite challenging. In this review, we discuss a number of the most significant issues regarding NMR-based urinary metabolomics with a specific emphasis on metabolite quantification for disease biomarker applications. We also propose a number of data collection and instrumental recommendations regarding NMR pulse sequences, acceptable acquisition parameter ranges, relaxation effects on quantitation, proper handling of instrumental differences, as well as recommendations regarding sample preparation and biomarker assessment.

  7. NMR signal analysis in the large COMPASS $^{14}$NH$_{3}$ target

    CERN Document Server

    Koivuniemi, J; Hess, C; Kisselev, Y U; Meyer, W; Radtke, E; Reicherz, G; Doshita, N; Iwata, T; Kondo, K; Michigami, T

    2009-01-01

    In the large COMPASS polarized proton target the 1508 cm$^{3}$ of irradiated granular ammonia is polarized with dynamic nuclear polarization method using 4 mm microwaves in 2.5 T eld. The nuclear polarization up to 90 - 93 % is determined with cw NMR. The properties of the observed ammonia proton signals are described and spin thermodynamics in high elds is presented. Also the second moment of the NMR line is estimated.

  8. Analysis of porous media and objects of cultural heritage by mobile NMR

    International Nuclear Information System (INIS)

    Haber, Agnes

    2012-01-01

    Low-field NMR techniques are used to study porous system, from simple to complex structures, and objects of cultural heritage. It is shown that NMR relaxometry can be used to study the fluid dynamics inside a porous system. A simple theoretical model for multi-site relaxation exchange NMR is used to extract exchange kinetic parameters when applied on a model porous systems. It provides a first step towards the study of more complex systems, where continuous relaxation distributions are present, such as soil systems or building materials. Moisture migration is observed in the soil systems with the help of 1D and 2D NMR relaxometry methods. In case of the concrete samples, the difference in composition makes a significant difference in the ability of water uptake. The single-sided NMR sensor proves to be a useful tool for on-site measurements. This is very important also in the case of the cultural heritage objects, as most of the objects can not be moved out of their environment. Mobile NMR turns out to be a simple but reliable and powerful tool to investigate moisture distributions and pore structures in porous media as well as the conservation state and history of objects of cultural heritage.

  9. NMR analysis of aldehydes in Sicilian extra-virgin olive oils by DPFGSE techniques

    Directory of Open Access Journals (Sweden)

    Enrico Rotondo

    2011-03-01

    Full Text Available The DPFGSE NMR sequences open new perspectives in the volatile compounds analysis of food matrices. Many fresh extra-virgin Sicilian olive oils, analyzed by this technique, show two main resonances in the aldehydic spectral region (9–10 ppm, at 9.18 and 9.58 ppm. The former was never reported so far, the latter was sometime highlighted as a minor aldehydic component signal of spectra showing stronger resonances at 9.45 and 9.70 ppm. Thermal treatment at 220°C of extra virgin olive oil samples lead to the complete transformation of the resonances at 9.18 and 9.58 ppm into those at 9.45 and 9.70 ppm in 50 minutes. Analogous transformation takes place place in CDCl3 at rt in several weeks. These results suggest the transformation of relatively unstable compounds into thermodynamically more stable products whose resonances are commonly reported in the literature. Even though these chemical changes involve minimal amount of product, they are of crucial importance to define: i organoleptic extra virgin olive oil properties; ii fraudulent chemical or thermal treatment detection; iii extra virgin oil ageing.

  10. Metabolic Effects of Hypoxia in Colorectal Cancer by 13C NMR Isotopomer Analysis

    Directory of Open Access Journals (Sweden)

    Ana M. Abrantes

    2014-01-01

    Full Text Available 13C NMR isotopomer analysis was used to characterize intermediary metabolism in three colorectal cancer cell lines (WiDr, LS1034, and C2BBe1 and determine the “metabolic remodeling” that occurs under hypoxia. Under normoxia, the three colorectal cancer cell lines present high rates of lactate production and can be seen as “Warburg” like cancer cells independently of substrate availability, since such profile was dominant at both high and low glucose media contents. The LS1034 was the less glycolytic of the three cell lines and was the most affected by the event of hypoxia, raising abruptly glucose consumption and lactate production. The other two colorectal cell lines, WiDr and C2BBe1, adapted better to hypoxia and were able to maintain their oxidative fluxes even at the very low levels of oxygen. These differential metabolic behaviors of the three colorectal cell lines show how important an adequate knowledge of the “metabolic remodeling” that follows a given cancer treatment is towards the correct (redesign of therapeutic strategies against cancer.

  11. Stochastic models (cooperative and non-cooperative) for NMR analysis of the hetero-association of aromatic molecules in aqueous solution

    Energy Technology Data Exchange (ETDEWEB)

    Evstigneev, Maxim P. [Department of Physics, Sevastopol National Technical University, Sevastopol 99053, Crimea (Ukraine)], E-mail: max_evstigneev@mail.ru; Davies, David B. [School of Biological and Chemical Sciences, Birkbeck College, University of London, Malet Street, London WC1E 7HX (United Kingdom); Veselkov, Alexei N. [Department of Physics, Sevastopol National Technical University, Sevastopol 99053, Crimea (Ukraine)

    2006-01-25

    Stochastic cooperative (STOCH-C) and non-cooperative (STOCH-NC) models have been developed for NMR analysis of the hetero-association of aromatic compounds in solution, in order to take into account all physically meaningful association reactions of molecules in which there are no limitations on the lengths of the aggregates and complexes. These algorithmical approaches are compared with previously published basic (BASE) and generalized (GEN) analytical statistical thermodynamical models of hetero-association of biologically active aromatic molecules using the same sets of published NMR data measured under the same solution conditions (0.1 M phosphate buffer, pD = 7.1, T = 298 K). It is shown that, within experimental errors, the BASE analytical model may be used to describe molecular systems characterized by relatively small contributions of hetero-association reactions, whereas the GEN model may be applied to hetero-association reactions of any aromatic compound with different self-association properties. The STOCH-C computational algorithm enabled the effect on hetero-association of the interactions of molecules with different cooperativity parameters of self-association to be estimated for the first time and it is proposed that the algorithm for the stochastic models has great potential for detailed investigation and understanding of the interactions of aromatic molecules in solution.

  12. Stochastic models (cooperative and non-cooperative) for NMR analysis of the hetero-association of aromatic molecules in aqueous solution

    International Nuclear Information System (INIS)

    Evstigneev, Maxim P.; Davies, David B.; Veselkov, Alexei N.

    2006-01-01

    Stochastic cooperative (STOCH-C) and non-cooperative (STOCH-NC) models have been developed for NMR analysis of the hetero-association of aromatic compounds in solution, in order to take into account all physically meaningful association reactions of molecules in which there are no limitations on the lengths of the aggregates and complexes. These algorithmical approaches are compared with previously published basic (BASE) and generalized (GEN) analytical statistical thermodynamical models of hetero-association of biologically active aromatic molecules using the same sets of published NMR data measured under the same solution conditions (0.1 M phosphate buffer, pD = 7.1, T = 298 K). It is shown that, within experimental errors, the BASE analytical model may be used to describe molecular systems characterized by relatively small contributions of hetero-association reactions, whereas the GEN model may be applied to hetero-association reactions of any aromatic compound with different self-association properties. The STOCH-C computational algorithm enabled the effect on hetero-association of the interactions of molecules with different cooperativity parameters of self-association to be estimated for the first time and it is proposed that the algorithm for the stochastic models has great potential for detailed investigation and understanding of the interactions of aromatic molecules in solution

  13. Complete determination of the Pin1 catalytic domain thermodynamic cycle by NMR lineshape analysis

    International Nuclear Information System (INIS)

    Greenwood, Alexander I.; Rogals, Monique J.; De, Soumya; Lu, Kun Ping; Kovrigin, Evgenii L.; Nicholson, Linda K.

    2011-01-01

    The phosphorylation-specific peptidyl-prolyl isomerase Pin1 catalyzes the isomerization of the peptide bond preceding a proline residue between cis and trans isomers. To best understand the mechanisms of Pin1 regulation, rigorous enzymatic assays of isomerization are required. However, most measures of isomerase activity require significant constraints on substrate sequence and only yield rate constants for the cis isomer, k cat cis and apparent Michaelis constants, K M App . By contrast, NMR lineshape analysis is a powerful tool for determining microscopic rates and populations of each state in a complex binding scheme. The isolated catalytic domain of Pin1 was employed as a first step towards elucidating the reaction scheme of the full-length enzyme. A 24-residue phosphopeptide derived from the amyloid precurser protein intracellular domain (AICD) phosphorylated at Thr668 served as a biologically-relevant Pin1 substrate. Specific 13 C labeling at the Pin1-targeted proline residue provided multiple reporters sensitive to individual isomer binding and on-enzyme catalysis. We have performed titration experiments and employed lineshape analysis of phosphopeptide 13 C– 1 H constant time HSQC spectra to determine k cat cis , k cat trans , K D cis , and K D trans for the catalytic domain of Pin1 acting on this AICD substrate. The on-enzyme equilibrium value of [E·trans]/[E·cis] = 3.9 suggests that the catalytic domain of Pin1 is optimized to operate on this substrate near equilibrium in the cellular context. This highlights the power of lineshape analysis for determining the microscopic parameters of enzyme catalysis, and demonstrates the feasibility of future studies of Pin1-PPIase mutants to gain insights on the catalytic mechanism of this important enzyme.

  14. Analysis of the mechanical properties and characterization by solid state 13 C NMR of recycled EVA copolymer/silica composites

    International Nuclear Information System (INIS)

    Stael, Giovanni Chaves; Rocha, Marisa Cristina Guimaraes

    2005-01-01

    The incorporation of micrometer sized silica particles on poly (ethylene-co-vinyl acetate) - EVA - residues from the footwear industry was evaluated. The effects of the processing parameters - temperature and mixing ratio - on the mechanical behavior of molded plates of neat recycled EVA and EVA/silica composites were also investigated. The mechanical properties measured by the tensile test, the fractographic analysis by scanning electron microscopy (SEM), and the 13 C Nuclear Magnetic Resonance (NMR) showed a reduced EVA to silica compatibility. Therefore, incorporation of untreated silica to recycled EVA copolymer produced a slight decrease on the mechanical performance of EVA/silica composites in respect to neat EVA copolymer. The NMR analysis also shows that the crosslinking process on recycled EVA may be occurring at the carbonyl group. (author)

  15. Fraction of boroxol rings in vitreous boron oxide from a first-principles analysis of Raman and NMR spectra.

    Science.gov (United States)

    Umari, P; Pasquarello, Alfredo

    2005-09-23

    We determine the fraction f of B atoms belonging to boroxol rings in vitreous boron oxide through a first-principles analysis. After generating a model structure of vitreous B2O3 by first-principles molecular dynamics, we address a large set of properties, including the neutron structure factor, the neutron density of vibrational states, the infrared spectra, the Raman spectra, and the 11B NMR spectra, and find overall good agreement with corresponding experimental data. From the analysis of Raman and 11B NMR spectra, we yield consistently for both probes a fraction f of approximately 0.75. This result indicates that the structure of vitreous boron oxide is largely dominated by boroxol rings.

  16. Analysis of the mechanical properties and characterization by solid state 13C NMR of recycled EVA copolymer/silica composites

    Directory of Open Access Journals (Sweden)

    Giovanni Chaves Stael

    2005-09-01

    Full Text Available The incorporation of micrometer sized silica particles on poly (ethylene-co-vinyl acetate - EVA - residues from the footwear industry was evaluated. The effects of the processing parameters - temperature and mixing ratio - on the mechanical behavior of molded plates of neat recycled EVA and EVA/silica composites were also investigated. The mechanical properties measured by the tensile test, the fractographic analysis by scanning electron microscopy (SEM, and the 13C Nuclear Magnetic Resonance (NMR showed a reduced EVA to silica compatibility. Therefore, incorporation of untreated silica to recycled EVA copolymer produced a slight decrease on the mechanical performance of EVA/silica composites in respect to neat EVA copolymer. The NMR analysis also shows that the crosslinking process on recycled EVA may be occurring at the carbonyl group.

  17. [Comparison of film-screen combination in a contrast detail diagram and with interactive image analysis. 1: Contrast detail diagram].

    Science.gov (United States)

    Hagemann, G; Eichbaum, G

    1997-07-01

    The following three film-screen combinations were compared: a) a combination of anticrossover film and UV-light emitting screens, b) a combination of blue-light emitting screens and film, and c) a conventional green fluorescing screen film combination. Radiographs of a specially designed plexiglass phantom (0.2 x 0.2 x 0.12 m3) were obtained that contained bar patterns of lead and plaster (calcium sulfate) to test high and intermediate contrast resolution and bar patterns of air to test low contrast resolution, respectively. An aluminum step wedge was integrated to evaluate dose-density curves of the radiographs. The dose values for the various step thicknesses were measured as percentage of the dose value in air for 60, 81, and 117 kV. Exposure conditions were the following: 12 pulse generator, 0.6 mm focus size, 4.7 mm aluminum prefilter, a grid with 40 lines/cm (12:1), and a focus-detector distance of 1.15 m. The thresholds of visible bars of the various pattern materials were assessed by seven radiologists, one technician, and the authors. The resulting contrast detail diagram could not prove any significant differences between the three tested screen film combinations. The pairwise comparison, however, found 8 of the 18 paired differences to be statistically significant between the conventional and the two new screen-film combinations. The authors concluded that subjective visual assessment of the threshold in a contrast detail study alone is of only limited value to grade image quality if no well-defined criteria are used (BIR report 20 [1989] 137-139). The statistical approach of paired differences of the estimated means appeared to be more appropriate.

  18. Nontargeted nuclear magnetic resonance (NMR) analysis to detect hazardous substances including methanol in unrecorded alcohol from Novosibirsk, Russia

    OpenAIRE

    Hausler, Thomas; Okaru,  Alex O.; Neufeld, Maria; Rehm, Jürgen; Kuballa, Thomas; Luy, Burkhard; Lachenmeier, Dirk W.

    2016-01-01

    Nuclear magnetic resonance (NMR) spectroscopy was applied to the analysis of alcoholic products in the context of health and safety control. A total of 86 samples of unrecorded alcohol were collected in Novosibirsk and nearby cities in Russia. Sampling was based on interviews with alcohol dependent patients, and unrecorded alcohol thus defined included illegally or informally produced alcoholic products (e.g., counterfeit or home-made alcoholic beverages) or surrogate alcohol in the form of c...

  19. Complex Mixture Analysis of Organic Compounds in Yogurt by NMR Spectroscopy

    Science.gov (United States)

    Lu, Yi; Hu, Fangyu; Miyakawa, Takuya; Tanokura, Masaru

    2016-01-01

    NMR measurements do not require separation and chemical modification of samples and therefore rapidly and directly provide non-targeted information on chemical components in complex mixtures. In this study, one-dimensional (1H, 13C, and 31P) and two-dimensional (1H-13C and 1H-31P) NMR spectroscopy were conducted to analyze yogurt without any pretreatment. 1H, 13C, and 31P NMR signals were assigned to 10 types of compounds. The signals of α/β-lactose and α/β-galactose were separately observed in the 1H NMR spectra. In addition, the signals from the acyl chains of milk fats were also successfully identified but overlapped with many other signals. Quantitative difference spectra were obtained by subtracting the diffusion ordered spectroscopy (DOSY) spectra from the quantitative 1H NMR spectra. This method allowed us to eliminate interference on the overlaps; therefore, the correct intensities of signals overlapped with those from the acyl chains of milk fat could be determined directly without separation. Moreover, the 1H-31P HMBC spectra revealed for the first time that N-acetyl-d-glucosamine-1-phosphate is contained in yogurt. PMID:27322339

  20. In vivo NMR analysis of incorporation of [2-13C] glycine into silk fibroin

    International Nuclear Information System (INIS)

    Asakura, Tetsuo; Nagashima, Mariko; Demura, Makoto; Osanai, Minoru.

    1990-01-01

    The biosynthetic mechanism of silk fibroin in silkworms, Bombyx mori, is unique because this fibrous protein composed mainly of glycine, alanine and serine is produced very rapidly in large quantity in the posterior silk glands. It is very meaningful to investigate into the biosynthesis of silk protein under nondestructive condition by in vivo NMR and C-13 labeling techniques. The sugar metabolism related to the production of silk fibroin was analyzed by monitoring the change in the C-13 labeled peaks in the NMR spectra for silkworms. In this paper, the monitoring of the 2-(C-13) glycine metabolism in Bombyx mori by the C-13 NMR in vivo is reported. In particular, the in vivo transport of glycine from the midgut to the posterior silk gland was measured, and the rate constants were determined with the course of the peak intensity in the C-13 NMR spectra. It is possible to discuss quantitatively the in vivo production of silk fibroin with these rate constants. The experiment and the results are reported. The in vivo C-13 NMR spectra of a 5 day old, 5th instar larva of Bombyx mori after the oral administration of 2-(C-13) glycine are shown. The significant increase of the peak intensity occurred. (K.I.)

  1. Micropore analysis of polymer networks by gas sorption and 129Xe NMR spectroscopy: toward a better understanding of intrinsic microporosity.

    Science.gov (United States)

    Weber, Jens; Schmidt, Johannes; Thomas, Arne; Böhlmann, Winfried

    2010-10-05

    The microporosity of two microporous polymer networks is investigated in detail. Both networks are based on a central spirobifluorene motif but have different linker groups, namely, imide and thiophene units. The microporosity of the networks is based on the "polymers of intrinsic microporosity (PIM)" design strategy. Nitrogen, argon, and carbon dioxide were used as sorbates in order to analyze the microporosity in greater detail. The gas sorption data was analyzed with respect to important parameters such as specific surface area, pore volume, and pore size (distribution). It is shown that the results can be strongly model dependent and swelling effects have to be regarded. (129)Xe NMR was used as an independent technique for the estimation of the average pore size of the polymer networks. The results indicate that both networks are mainly ultramicroporous (pore sizes microporous matter might have a different micropore size in the solvent swollen/filled state that in the dry state.

  2. Molecular characterization of dissolved organic matter from subtropical wetlands: a comparative study through the analysis of optical properties, NMR and FTICR/MS

    Science.gov (United States)

    Hertkorn, Norbert; Harir, Mourad; Cawley, Kaelin M.; Schmitt-Kopplin, Philippe; Jaffé, Rudolf

    2016-04-01

    Wetlands provide quintessential ecosystem services such as maintenance of water quality, water supply and biodiversity, among others; however, wetlands are also among the most threatened ecosystems worldwide. Natural dissolved organic matter (DOM) is an abundant and critical component in wetland biogeochemistry. This study describes the first detailed, comparative, molecular characterization of DOM in subtropical, pulsed, wetlands, namely the Everglades (USA), the Pantanal (Brazil) and the Okavango Delta (Botswana), using optical properties, high-field nuclear magnetic resonance (NMR) and ultrahigh-resolution mass spectrometry (FT-ICRMS), and compares compositional features to variations in organic matter sources and flooding characteristics (i.e., differences in hydroperiod). While optical properties showed a high degree of variability within and between the three wetlands, analogies in DOM fluorescence properties were such that an established excitation emission matrix fluorescence parallel factor analysis (EEM-PARAFAC) model for the Everglades was perfectly applicable to the other two wetlands. Area-normalized 1H NMR spectra of selected samples revealed clear distinctions of samples while a pronounced congruence within the three pairs of wetland DOM readily suggested the presence of an individual wetland-specific molecular signature. Within sample pairs (long- vs. short-hydroperiod sites), internal differences mainly referred to intensity variations (denoting variable abundance) rather than to alterations of NMR resonances positioning (denoting diversity of molecules). The relative disparity was largest between the Everglades long- and short-hydroperiod samples, whereas Pantanal and Okavango samples were more alike among themselves. Otherwise, molecular divergence was most obvious in the case of unsaturated protons (δH > 5 ppm). 2-D NMR spectroscopy for a particular sample revealed a large richness of aliphatic and unsaturated substructures, likely derived from

  3. Validation of quantitative 1H NMR method for the analysis of pharmaceutical formulations

    International Nuclear Information System (INIS)

    Santos, Maiara da S.

    2013-01-01

    The need for effective and reliable quality control in products from pharmaceutical industries renders the analyses of their active ingredients and constituents of great importance. This study presents the theoretical basis of ¹H NMR for quantitative analyses and an example of the method validation according to Resolution RE N. 899 by the Brazilian National Health Surveillance Agency (ANVISA), in which the compound paracetamol was the active ingredient. All evaluated parameters (selectivity, linearity, accuracy, repeatability and robustness) showed satisfactory results. It was concluded that a single NMR measurement provides structural and quantitative information of active components and excipients in the sample. (author)

  4. Conformational analysis of 9,10-dihydroanthracenes. Molecular mechanics calculations and /sup 13/C NMR

    Energy Technology Data Exchange (ETDEWEB)

    Rabideau, P.W.; Mooney, J.L.; Lipkowitz, K.B.

    1986-12-24

    The conformational analyses of 9, 10-dihydroanthracene and several of its methylated and ethylated derivatives are studied by empirical force field calculations (MM2 and MMPI). The computational results are considered in light of previous and current carbon NMR data. Model compounds are examined which involve fixed, planar, and boat-shaped conformations about the central ring, and these /sup 13/C NMR data are then compared with flexible systems. It is concluded that carbon chemical shifts and carbon-hydrogen coupling constants are consistent with the results of molecular mechanics calculations which indicate a greater tendency for planarity around the central ring than previously considered.

  5. 1H NMR and PCA-based analysis revealed variety dependent changes in phenolic contents of apple fruit after drying.

    Science.gov (United States)

    Francini, Alessandra; Romeo, Stefania; Cifelli, Mario; Gori, Daniele; Domenici, Valentina; Sebastiani, Luca

    2017-04-15

    Dry and fresh apples have been studied monitoring their polyphenolic profiles through 1 H NMR, antioxidant capacity and total polyphenol content. Six ancient and underutilized apple varieties (Mantovana, Mora, Nesta, Cipolla, Ruggina, Sassola) and a commercial one (Golden Delicious) were dried with an air-drying system at 45°C for 19h. Although some of their polyphenol constituents were lost during drying, the antioxidant capacity of some apple varieties remained higher compared to Golden Delicious. This result is very important for ancient and underutilized varieties that are not consumed on large scale as fresh product since they have low attractiveness, due to their ugly appearance. Combining quantitative NMR spectroscopy with principal component analysis we have identified and quantified several polyphenols (such as catechin, epicathechin, and chlorogenic acid) that are important to establish the nutraceutical value of the different investigated apple varieties. Copyright © 2016 Elsevier Ltd. All rights reserved.

  6. Si-O-Si bond-angle distribution in vitreous silica from first-principles 29Si NMR analysis

    International Nuclear Information System (INIS)

    Mauri, Francesco; Pasquarello, Alfredo; Pfrommer, Bernd G.; Yoon, Young-Gui; Louie, Steven G.

    2000-01-01

    The correlation between 29 Si chemical shifts and Si-O-Si bond angles in SiO 2 is determined within density-functional theory for the full range of angles present in vitreous silica. This relation closely reproduces measured shifts of crystalline polymorphs. The knowledge of the correlation allows us to reliably extract from the experimental NMR spectrum the mean (151 degree sign ) and the standard deviation (11 degree sign ) of the Si-O-Si angular distribution of vitreous silica. In particular, we show that the Mozzi-Warren Si-O-Si angular distribution is not consistent with the NMR data. This analysis illustrates the potential of our approach for structural determinations of silicate glasses. (c) 2000 The American Physical Society

  7. The use of IRMS, (1)H NMR and chemical analysis to characterise Italian and imported Tunisian olive oils.

    Science.gov (United States)

    Camin, Federica; Pavone, Anita; Bontempo, Luana; Wehrens, Ron; Paolini, Mauro; Faberi, Angelo; Marianella, Rosa Maria; Capitani, Donatella; Vista, Silvia; Mannina, Luisa

    2016-04-01

    Isotope Ratio Mass Spectrometry (IRMS), (1)H Nuclear Magnetic Resonance ((1)H NMR), conventional chemical analysis and chemometric elaboration were used to assess quality and to define and confirm the geographical origin of 177 Italian PDO (Protected Denomination of Origin) olive oils and 86 samples imported from Tunisia. Italian olive oils were richer in squalene and unsaturated fatty acids, whereas Tunisian olive oils showed higher δ(18)O, δ(2)H, linoleic acid, saturated fatty acids β-sitosterol, sn-1 and 3 diglyceride values. Furthermore, all the Tunisian samples imported were of poor quality, with a K232 and/or acidity values above the limits established for extra virgin olive oils. By combining isotopic composition with (1)H NMR data using a multivariate statistical approach, a statistical model able to discriminate olive oil from Italy and those imported from Tunisia was obtained, with an optimal differentiation ability arriving at around 98%. Copyright © 2015 Elsevier Ltd. All rights reserved.

  8. 78 FR 69669 - Intent To Conduct a Detailed Economic Impact Analysis

    Science.gov (United States)

    2013-11-20

    ... EXPORT-IMPORT BANK Intent To Conduct a Detailed Economic Impact Analysis This notice is to inform... guarantee, the value of the transaction, and the amount of new foreign production capacity are not included... date this notice appears in the Federal Register. James C. Cruse, Senior Vice President, Policy and...

  9. 78 FR 47317 - Intent To Conduct a Detailed Economic Impact Analysis

    Science.gov (United States)

    2013-08-05

    ... EXPORT-IMPORT BANK OF THE UNITED STATES Intent To Conduct a Detailed Economic Impact Analysis This... route service within China and from China to various regional and international destinations... to economic[email protected] or by mail to 811 Vermont Avenue NW., Room 442, Washington, DC 20571...

  10. Protein secondary structure assignment revisited: a detailed analysis of different assignment methods

    Directory of Open Access Journals (Sweden)

    de Brevern Alexandre G

    2005-09-01

    Full Text Available Abstract Background A number of methods are now available to perform automatic assignment of periodic secondary structures from atomic coordinates, based on different characteristics of the secondary structures. In general these methods exhibit a broad consensus as to the location of most helix and strand core segments in protein structures. However the termini of the segments are often ill-defined and it is difficult to decide unambiguously which residues at the edge of the segments have to be included. In addition, there is a "twilight zone" where secondary structure segments depart significantly from the idealized models of Pauling and Corey. For these segments, one has to decide whether the observed structural variations are merely distorsions or whether they constitute a break in the secondary structure. Methods To address these problems, we have developed a method for secondary structure assignment, called KAKSI. Assignments made by KAKSI are compared with assignments given by DSSP, STRIDE, XTLSSTR, PSEA and SECSTR, as well as secondary structures found in PDB files, on 4 datasets (X-ray structures with different resolution range, NMR structures. Results A detailed comparison of KAKSI assignments with those of STRIDE and PSEA reveals that KAKSI assigns slightly longer helices and strands than STRIDE in case of one-to-one correspondence between the segments. However, KAKSI tends also to favor the assignment of several short helices when STRIDE and PSEA assign longer, kinked, helices. Helices assigned by KAKSI have geometrical characteristics close to those described in the PDB. They are more linear than helices assigned by other methods. The same tendency to split long segments is observed for strands, although less systematically. We present a number of cases of secondary structure assignments that illustrate this behavior. Conclusion Our method provides valuable assignments which favor the regularity of secondary structure segments.

  11. NMR determination of chemically related metals in solution as a new method of inorganic analysis

    International Nuclear Information System (INIS)

    Fedorov, L.A.

    1989-01-01

    An NMR spectroscopic method for the determination of chemically related metals in solution is suggested. The metals are determined in complexes with specially selected polydentate ligands. Structural requirements to ligands, analytical properties and general limits of the application of the method are discussed. (orig.)

  12. Quantitative Analysis of Chemically Modified Starches by 1H-NMR Spectroscopy

    NARCIS (Netherlands)

    Graaf, R.A. de; Lammers, G.; Janssen, L.P.B.M.; Beenackers, A.A.C.M.

    1995-01-01

    A quantitative 1H-NMR method for the determination of the Molar Substitution (MS) of acetylated and hydroxypropylated starches was developed and tested for MS ranging from 0.09 to 0.5. Results were checked using the Johnson method and a titration method for hydroxypropylated and acetylated starch,

  13. Quantitative analysis of chemically modified starches by H-1-NMR spectroscopy

    NARCIS (Netherlands)

    de Graaf, R.A.; Lammers, G; Janssen, L.P.B.M.; Beenackers, A.A C M

    1995-01-01

    A quantitative H-1-NMR method for the determination of the Molar Substitution (MS) of acetylated and hydroxypropylated starches was developed and tested for MS ranging from 0.09 to 0.5. Results were checked using the Johnson method and a titration method for hydroxypropylated and acetylated starch,

  14. An Improved Spectral Analysis Method for Fatigue Damage Assessment of Details in Liquid Cargo Tanks

    Science.gov (United States)

    Zhao, Peng-yuan; Huang, Xiao-ping

    2018-03-01

    Errors will be caused in calculating the fatigue damages of details in liquid cargo tanks by using the traditional spectral analysis method which is based on linear system, for the nonlinear relationship between the dynamic stress and the ship acceleration. An improved spectral analysis method for the assessment of the fatigue damage in detail of a liquid cargo tank is proposed in this paper. Based on assumptions that the wave process can be simulated by summing the sinusoidal waves in different frequencies and the stress process can be simulated by summing the stress processes induced by these sinusoidal waves, the stress power spectral density (PSD) is calculated by expanding the stress processes induced by the sinusoidal waves into Fourier series and adding the amplitudes of each harmonic component with the same frequency. This analysis method can take the nonlinear relationship into consideration and the fatigue damage is then calculated based on the PSD of stress. Take an independent tank in an LNG carrier for example, the accuracy of the improved spectral analysis method is proved much better than that of the traditional spectral analysis method by comparing the calculated damage results with the results calculated by the time domain method. The proposed spectral analysis method is more accurate in calculating the fatigue damages in detail of ship liquid cargo tanks.

  15. NMR imaging

    International Nuclear Information System (INIS)

    Andrew, E.R.

    1983-01-01

    Since hydrogen is the most abundant element in all living organisms, proton NMR lends itself well as a method of investigation in biology and medicine. NMR imaging has some special advantages as a diagnostic tool: no ionizing radiation is used, it is noninvasive; it provides a safer means of imaging than the use of x-rays, gamma rays, positrons, or heavy ions. In contrast with ultrasound, the radiation penetrates the bony structures without attenuation. In additional to morphological information, NMR imaging provides additional diagnostic insights through relaxation parameters, which are not available from other imaging methods. In the decade since the first primitive NMR images were obtained, the quality of images now obtained approaches those from CT x-ray scanners. Prototype instruments are being constructed for clinical evaluation and the first whole-body scanners are beginning to appear on the market at costs comparable to CT scanners. Primary differences in equipment for conventional NMR and NMR imaging are the much larger aperture magnets that are required for the examination of human subjects and the addition of coils to generate field gradients and facilities for manipulating the gradients. Early results from clinical trials in many parts of the world are encouraging, and in a few years, the usefuleness of this modality of medical imaging to the medical profession in diagnosis and treatment of disease will be defined. 10 figures

  16. Detailed Analysis of Torque Ripple in High Frequency Signal Injection based Sensor less PMSM Drives

    Directory of Open Access Journals (Sweden)

    Ravikumar Setty A.

    2017-01-01

    Full Text Available High Frequency Signal Injection based techniques are robust and well proven to estimate the rotor position from stand still to low speed. However, Injected high frequency signal introduces, high frequency harmonics in the motor phase currents and results in significant Output Torque ripple. There is no detailed analysis exist in the literature, to study the effect of injected signal frequency on Torque ripple. Objective of this work is to study the Torque Ripple resulting from High Frequency signal injection in PMSM motor drives. Detailed MATLAB/Simulink simulations are carried to quantify the Torque ripple at different Signal frequencies.

  17. Technical basis for the ITER detailed design report, cost review and safety analysis (DDR)

    International Nuclear Information System (INIS)

    1997-01-01

    The ITER Detailed Design Report (DDR), Cost Review and Safety Analysis is the 3rd major milestone representing the progress made in the ITER Engineering Design Activities. With the approval of the Interim Design Report (IDR), it has been possible to freeze the main concepts and system approaches for ITER and to develop the design in more detail for the individual components and sub-systems. This report, although designed to be fully understandable as a separate document, focusses particularly on the main changes since the IDR

  18. Technical basis for the ITER detailed design report, cost review and safety analysis (DDR)

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1997-12-01

    The ITER Detailed Design Report (DDR), Cost Review and Safety Analysis is the 3rd major milestone representing the progress made in the ITER Engineering Design Activities. With the approval of the Interim Design Report (IDR), it has been possible to freeze the main concepts and system approaches for ITER and to develop the design in more detail for the individual components and sub-systems. This report, although designed to be fully understandable as a separate document, focusses particularly on the main changes since the IDR. Refs, figs, tabs

  19. Analysis of monoglycerides, diglycerides, sterols, and free fatty acids in coconut (Cocos nucifera L.) oil by 31P NMR spectroscopy.

    Science.gov (United States)

    Dayrit, Fabian M; Buenafe, Olivia Erin M; Chainani, Edward T; de Vera, Ian Mitchelle S

    2008-07-23

    Phosphorus-31 nuclear magnetic resonance spectroscopy ( (31)P NMR) was used to differentiate virgin coconut oil (VCO) from refined, bleached, deodorized coconut oil (RCO). Monoglycerides (MGs), diglycerides (DGs), sterols, and free fatty acids (FFAs) in VCO and RCO were converted into dioxaphospholane derivatives and analyzed by (31)P NMR. On the average, 1-MG was found to be higher in VCO (0.027%) than RCO (0.019%). 2-MG was not detected in any of the samples down to a detection limit of 0.014%. On the average, total DGs were lower in VCO (1.55%) than RCO (4.10%). When plotted in terms of the ratio [1,2-DG/total DGs] versus total DGs, VCO and RCO samples grouped separately. Total sterols were higher in VCO (0.096%) compared with RCO (0.032%), and the FFA content was 8 times higher in VCO than RCO (0.127% vs 0.015%). FFA determination by (31)P NMR and titration gave comparable results. Principal components analysis shows that the 1,2-DG, 1,3-DG, and FFAs are the most important parameters for differentiating VCO from RCO.

  20. FANTEN: a new web-based interface for the analysis of magnetic anisotropy-induced NMR data

    Energy Technology Data Exchange (ETDEWEB)

    Rinaldelli, Mauro; Carlon, Azzurra; Ravera, Enrico; Parigi, Giacomo, E-mail: parigi@cerm.unifi.it; Luchinat, Claudio, E-mail: luchinat@cerm.unifi.it [University of Florence, CERM and Department of Chemistry “Ugo Schiff” (Italy)

    2015-01-15

    Pseudocontact shifts (PCSs) and residual dipolar couplings (RDCs) arising from the presence of paramagnetic metal ions in proteins as well as RDCs due to partial orientation induced by external orienting media are nowadays routinely measured as a part of the NMR characterization of biologically relevant systems. PCSs and RDCs are becoming more and more popular as restraints (1) to determine and/or refine protein structures in solution, (2) to monitor the extent of conformational heterogeneity in systems composed of rigid domains which can reorient with respect to one another, and (3) to obtain structural information in protein–protein complexes. The use of both PCSs and RDCs proceeds through the determination of the anisotropy tensors which are at the origin of these NMR observables. A new user-friendly web tool, called FANTEN (Finding ANisotropy TENsors), has been developed for the determination of the anisotropy tensors related to PCSs and RDCs and has been made freely available through the WeNMR ( http://fanten-enmr.cerm.unifi.it:8080 http://fanten-enmr.cerm.unifi.it:8080 ) gateway. The program has many new features not available in other existing programs, among which the possibility of a joint analysis of several sets of PCS and RDC data and the possibility to perform rigid body minimizations.

  1. NMR-based metabonomic analysis of the hepatotoxicity induced by combined exposure to PCBs and TCDD in rats

    International Nuclear Information System (INIS)

    Lu Chunfeng; Wang Yimei; Sheng Zhiguo; Liu Gang; Fu Ze; Zhao Jing; Zhao Jun; Yan Xianzhong; Zhu Benzhan; Peng Shuangqing

    2010-01-01

    A metabonomic approach using 1 H NMR spectroscopy was adopted to investigate the metabonomic pattern of rat urine after oral administration of environmental endocrine disruptors (EDs) polychlorinated biphenyls (PCBs) and 2,3,7,8-tetrachlorodibenzo- p-dioxin (TCDD) alone or in combination and to explore the possible hepatotoxic mechanisms of combined exposure to PCBs and TCDD. 1 H NMR spectra of urines collected 24 h before and after exposure were analyzed via pattern recognition by using principal component analysis (PCA). Serum biochemistry and liver histopathology indicated significant hepatotoxicity in the rats of the combined group. The PCA scores plots of urinary 1 H NMR data showed that all the treatment groups could be easily distinguished from the control group, so could the PCBs or TCDD group and the combined group. The loadings plots of the PCA revealed remarkable increases in the levels of lactate, glucose, taurine, creatine, and 2-hydroxy-isovaleric acid and reductions in the levels of 2-oxoglutarate, citrate, succinate, hippurate, and trimethylamine-N-oxide in rat urine after exposure. These changes were more striking in the combined group. The changed metabolites may be considered possible biomarker for the hepatotoxicity. The present study demonstrates that combined exposure to PCBs and TCDD induced significant hepatotoxicity in rats, and mitochondrial dysfunction and fatty acid metabolism perturbations might contribute to the hepatotoxicity. There was good conformity between changes in the urine metabonomic pattern and those in serum biochemistry and liver histopathology. These results showed that the NMR-based metabonomic approach may provide a promising technique for the evaluation of the combined toxicity of EDs.

  2. Functional group analysis by H NMR/chemical derivatization for the characterization of organic aerosol from the SMOCC field campaign

    Directory of Open Access Journals (Sweden)

    E. Tagliavini

    2006-01-01

    Full Text Available Water soluble organic compounds (WSOC in aerosol samples collected in the Amazon Basin in a period encompassing the middle/late dry season and the beginning of the wet season, were investigated by H NMR spectroscopy. HiVol filter samples (PM2.5 and PM>2.5 and size-segregated samples from multistage impactor were subjected to H NMR characterization. The H NMR methodology, recently developed for the analysis of organic aerosol samples, has been improved by exploiting chemical methylation of carboxylic groups with diazomethane, which allows the direct determination of the carboxylic acid content of WSOC. The content of carboxylic carbons for the different periods and sizes ranged from 12% to 20% of total measured carbon depending on the season and aerosol size, with higher contents for the fine particles in the transition and wet periods with respect to the dry period. A comprehensive picture is presented of WSOC functional groups in aerosol samples representative of the biomass burning period, as well as of transition and semi-clean atmospheric conditions. A difference in composition between fine (PM2.5 and coarse (PM>2.5 size fractions emerged from the NMR data, the former showing higher alkylic content, the latter being largely dominated by R-O-H (or R-O-R' functional groups. Very small particles (<0.14 μm, however, present higher alkyl-chain content and less oxygenated carbons than larger fine particles (0.42–1.2 μm. More limited variations were found between the average compositions in the different periods of the campaign.

  3. Light water reactor fuel analysis code FEMAXI-IV(Ver.2). Detailed structure and user's manual

    International Nuclear Information System (INIS)

    Suzuki, Motoe; Saitou, Hiroaki.

    1997-11-01

    A light water reactor fuel behavior analysis code FEMAXI-IV(Ver.2) was developed as an improved version of FEMAXI-IV. Development of FEMAXI-IV has been already finished in 1992, though a detailed structure and input manual of the code have not been open to users yet. Here, the basic theories and structure, the models and numerical solutions applied to FEMAXI-IV(Ver.2), and the material properties adopted in the code are described in detail. In FEMAXI-IV(Ver.2), programming bugs in previous FEMAXI-IV were eliminated, renewal of the pellet thermal conductivity was performed, and a model of thermal-stress restraint on FP gas release was incorporated. For facilitation of effective and wide-ranging application of the code, methods of input/output of the code are also described in detail, and sample output is included. (author)

  4. Uniform procedure of 1H NMR analysis of rat urine and toxicometabonomics Part II : Comparison of NMR profiles classification of hepatotoxicity

    NARCIS (Netherlands)

    Schoonen, W.G.E.J.; Kloks, C.P.A.M.; Ploemen, J.-P.H.T.M.; Smit, M.J.; Zandberg, P.; Horbach, G.J.; Mellema, J.-R.; Zuylen, C.T. van; Tas, A.C.; Nesselrooij, J.H.J. van; Vogels, J.T.W.E.

    2007-01-01

    A procedure of nuclear magnetic resonance (NMR) urinalysis using pattern recognition is proposed for early detection of toxicity of investigational compounds in rats. The method is applied to detect toxicity upon administration of 13 toxic reference compounds and one nontoxic control compound

  5. Structural Biology: Practical NMR Applications

    CERN Document Server

    Teng, Quincy

    2005-01-01

    This textbook begins with an overview of NMR development and applications in biological systems. It describes recent developments in instrument hardware and methodology. Chapters highlight the scope and limitation of NMR methods. While detailed math and quantum mechanics dealing with NMR theory have been addressed in several well-known NMR volumes, chapter two of this volume illustrates the fundamental principles and concepts of NMR spectroscopy in a more descriptive manner. Topics such as instrument setup, data acquisition, and data processing using a variety of offline software are discussed. Chapters further discuss several routine stategies for preparing samples, especially for macromolecules and complexes. The target market for such a volume includes researchers in the field of biochemistry, chemistry, structural biology and biophysics.

  6. Spectroscopic data of Labdane Diterpenes: a theoretical analysis via NMR and DFT

    International Nuclear Information System (INIS)

    Souza, Fabrine S. de; Silva, Silvana de O.; Alves, Cláudio N.; Guilhon, Giselle M.S.P.

    2015-01-01

    Labdane diterpenes exhibit important bioactivities such as cardiovascular effects in rats as well as effects in the treatment of autoimmune diseases and Alzheimer syndrome. Recently, the labdane diterpenes ent-13-epi-manoil oxide, ribenone and ribenol were isolated from Croton palanostigma. The computational method DFT/B3LYP/cc-pVDZ was used to optimize the structures of these diterpenes and to calculate infrared data. Chemical shifts (δ H and δ C ) of the minimum energy structures (local minimum) were calculated and compared with the experimental data. Comparison of the NMR data by simple linear regression (SLR) showed satisfactory statistical results with a correlation coefficient (R 2 ) and predictive ability (Q 2 ) of over 98%. The predicted NMR data were used to confirm the δ H values that have not been published. (author)

  7. An instrument control and data analysis program for NMR imaging and spectroscopy

    International Nuclear Information System (INIS)

    Roos, M.S.; Mushlin, R.A.; Veklerov, E.; Port, J.D.; Ladd, C.; Harrison, C.G.

    1988-01-01

    We describe a software environment created to support real-time instrument control and signal acquisition as well as array-processor based signal and image processing in up to five dimensions. The environment is configured for NMR imaging and in vivo spectroscopy. It is designed to provide flexible tools for implementing novel NMR experiments in the research laboratory. Data acquisition and processing operations are programmed in macros which are loaded in assembled from to minimize instruction overhead. Data arrays are dynamically allocated for efficient use of memory and can be mapped directly into disk files. The command set includes primitives for real-time control of data acquisition, scalar arithmetic, string manipulation, branching, a file system and vector operations carried out by an array processor. 6 figs

  8. A structural homologue of colipase in black mamba venom revealed by NMR floating disulphide bridge analysis.

    Science.gov (United States)

    Boisbouvier, J; Albrand, J P; Blackledge, M; Jaquinod, M; Schweitz, H; Lazdunski, M; Marion, D

    1998-01-01

    The solution structure of mamba intestinal toxin 1 (MIT1), isolated from Dendroaspis polylepis polylepis venom, has been determined. This molecule is a cysteine-rich polypeptide exhibiting no recognised family membership. Resistance to MIT1 to classical specific endoproteases produced contradictory NMR and biochemical information concerning disulphide-bridge topology. We have used distance restraints allowing ambiguous partners between S atoms in combination with NMR-derived structural information, to correctly determine the disulphide-bridge topology. The resultant solution structure of MIT1, determined to a resolution of 0.5 A, reveals an unexpectedly similar global fold with respect to colipase, a protein involved in fatty acid digestion. Colipase exhibits an analogous resistance to endoprotease activity, indicating for the first time the possible topological origins of this biochemical property. The biochemical and structural homology permitted us to propose a mechanically related digestive function for MIT1 and provides novel information concerning snake venom protein evolution. Copyright 1998 Academic Press.

  9. Computer-aided structure analysis. Structure identification by infrared and /sup 13/C NMR measurements

    Energy Technology Data Exchange (ETDEWEB)

    Szalontai, G; Simon, Z; Csapo, Z; Farkas, M; Pfeifer, Gy [Nehezvegyipari Kutato Intezet, Veszprem (Hungary)

    1980-01-01

    The results obtained from the computer-aided interpretation of /sup 13/C NMR and IR spectra using the artificial intelligence approach are presented. In its present state the output of the system is a list of functional groups which are resonable candidates for the final structural isomers. The input requires empirical formula, /sup 13/C NMR data (off resonance data also) and IR spectral data. The confirmation of the presence of a functional group is based on comparison of the experimental data with the spectral properties of functional groups stored in a property matrix. If the molecular weight of the compounds studied is less or equal 500, the output contains usually 1.5-2.5 times more groups than really present, in most cases without the loss of the real ones.

  10. Detailed description and user`s manual of high burnup fuel analysis code EXBURN-I

    Energy Technology Data Exchange (ETDEWEB)

    Suzuki, Motoe [Japan Atomic Energy Research Inst., Tokai, Ibaraki (Japan). Tokai Research Establishment; Saitou, Hiroaki

    1997-11-01

    EXBURN-I has been developed for the analysis of LWR high burnup fuel behavior in normal operation and power transient conditions. In the high burnup region, phenomena occur which are different in quality from those expected for the extension of behaviors in the mid-burnup region. To analyze these phenomena, EXBURN-I has been formed by the incorporation of such new models as pellet thermal conductivity change, burnup-dependent FP gas release rate, and cladding oxide layer growth to the basic structure of low- and mid-burnup fuel analysis code FEMAXI-IV. The present report describes in detail the whole structure of the code, models, and materials properties. Also, it includes a detailed input manual and sample output, etc. (author). 55 refs.

  11. Fluid typing and tortuosity analysis with NMR-DE techniques in volcaniclastic reservoirs, Patagonia/Argentina

    Energy Technology Data Exchange (ETDEWEB)

    Bustos, Ulises Daniel [Schlumberger Argentina S.A., Buenos Aires (Argentina); Breda, Eduardo Walter [Repsol YPF Comodoro Rivadavia, Chubut (Argentina)

    2004-07-01

    Alternative hydrocarbon-detection techniques are used to differentiate water from hydrocarbon where resistivity-based methods are difficult to apply, such as freshwater reservoirs and complex lithologies. One of these areas is represented by the complex volcaniclastic freshwater reservoirs in the Golfo San Jorge basin, Patagonia Argentina, where water and oil have often identical response on conventional logs. Some advances in hydrocarbon identification based on nuclear magnetic resonance (NMR) techniques were achieved in long T1 environments (very light oils, gas) in the Golfo San Jorge basin by previous NMR fluid typing methods. However, since medium to heavy oils are commonly present in these intervals, hydrocarbon detection by such techniques cannot be properly achieved. In addition, restricted diffusion phenomena recognized in these intervals, constitute further complications in fluid typing since its presence have similar response than native oil. To address this problem, a fluid characterization method using NMR Diffusion-Editing techniques and processing/interpretation with D-T2 maps in a suite of NMR measurements was applied. The technique allowed the detection and evaluation of restricted diffusion in these reservoirs, enabling better hydrocarbon characterization in a broad viscosity range (from light to heavy). The method also improved the petrophysical evaluation because restricted diffusion is related to tortuosity in the reservoir. Since the application of this innovative reservoir evaluation method, fluid prognosis vs well completion results was increased from around 68% to around 88% in Golfo San Jorge basin. Moreover, in some of these areas rates above 95% were recently achieved in 2004. (author)

  12. LC-NMR Technique in the Analysis of Phytosterols in Natural Extracts

    Czech Academy of Sciences Publication Activity Database

    Horník, Štěpán; Sajfrtová, Marie; Karban, Jindřich; Sýkora, Jan; Březinová, Anna; Wimmer, Zdeněk

    2013-01-01

    Roč. 2013, č. 2013 (2013), ID 526818 ISSN 2090-8865 R&D Projects: GA TA ČR TA01010578 Grant - others:GA ČR(CZ) GAP503/11/0616 Program:GA Institutional support: RVO:67985858 ; RVO:61388963 ; RVO:61389030 Keywords : LC-NMR technique * phytosterols * analyses Subject RIV: CC - Organic Chemistry; EE - Microbiology, Virology (UEB-Q) Impact factor: 0.948, year: 2013

  13. Single corn kernel wide-line NMR oil analysis for breeding purpose

    Energy Technology Data Exchange (ETDEWEB)

    Wilmers, M C.C.; Rettori, C; Vargas, H; Barberis, G E [Universidade Estadual de Campinas (Brazil). Inst. de Fisica; da Silva, W J [Universidade Estadual de Campinas (Brazil). Inst. de Biologia

    1978-12-01

    The Wide-Line NMR technique was used to determine the oil content in single corn seeds. Using distinct radio frequency (RF) power, a systematic work was done in kernels with about 10% of moisture, and also in artificially dried seeds with approximated 5% of moisture. For nondried seeds NMR spectra showed clearly the presence of three resonances with different RF saturation factor. For dried seeds, the oil concentration determined by NMR was highly correlated (r = 0,997) with that determined by a gravimetric method. The highest discrepancy between the two methods was found to be about 1,3%. When relative measurements are required as in the case of single kernel for recurrent selection program, precision in the individual selected kernel will be about 2,5%. Applying this technique, a first cycle of recurrent selection using S/sub 1/ lines for low and high oil content was performed in an open pollinated variety. Gain from selection was 12.0 and 14.1% in the populations for high and low oil contents, respectively.

  14. Development of new probes for NMR based analysis of biomolecules' cellular functions

    International Nuclear Information System (INIS)

    Fernandes, Laetitia

    2015-01-01

    Most NMR studies are carried out in vitro, but the structure and dynamics of some biomolecules inside cells differ from those in vitro. It thus becomes interesting to analyze biomolecules such as proteins in their natural environment: the cell. Recent progress of in cell NMR allowed to better understand the behaviour of proteins: their dynamics and their interactions with other biomolecules in the cell. But the low concentration of proteins leads to low signal intensity. Moreover, the viscosity of the environment induces faster transverse relaxation, resulting in line broadening for proteins signals. The use of the Long-Lived States and Coherencies (LLS and LLC, respectively) as well as dissolution Dynamic Nuclear Polarization (dissolution-DNP) can improve NMR observations in cells. LLS were used to understand and characterize the structure of the N-terminal domain of c-Src, which is intrinsically disordered. To follow the phosphorylation of proteins, a first preliminary study of a 21-aa peptides derived from IKBa electroporated into HepG2 cell lines was carried out. (author)

  15. Engineered safeguards and passive safety features (safety analysis detailed report no. 6)

    Energy Technology Data Exchange (ETDEWEB)

    1988-01-15

    The Safety-Analysis Summary lists the reactor's safety aspects for passive and active prevention of severe accidents and mitigation of accident consequences, i.e., intrinsic and passive protections of the plant; intrinsic and passive protections of the core; inherent decay-heat removal systems; rapid-shutdown systems; four physical containment barriers. This report goes into further details regarding some of this aspects.

  16. Functional Group and Structural Characterization of Unmodified and Functionalized Lignin by Titration, Elemental Analysis, 1H NMR and FTIR Techniques

    Directory of Open Access Journals (Sweden)

    Ramin Bairami Habashi

    2017-11-01

    Full Text Available Lignin is the second most abundant polymer in the world after cellulose. Therefore, characterization of the structure and functional groups of lignin in order to assess its potential applications in various technical fields has become a necessity. One of the major problems related to the characterization of lignin is the lack of well-defined protocols and standards. In this paper, systematic studies have been done to characterize the structure and functional groups of lignin quantitatively using different techniques such as elemental analysis, titration and 1H NMR and FTIR techniques. Lignin as a black liquor was obtained from Choka Paper Factory and it was purified before any test. The lignin was reacted with α-bromoisobutyryl bromide to calculate the number of hydroxyl and methoxyl moles. Using 1H NMR spectroscopic method on α-bromoisobutyrylated lignin (BiBL in the presence of a given amount of N,N-dimethylformamide (DMF as an internal standard, the number of moles of hydroxyl and methoxyl groups per gram of lignin was found to be 6.44 mmol/g and 6.64 mmol/g, respectively. Using aqueous titration, the number of moles of phenolic hydroxyl groups and carboxyl groups of the lignin were calculated as 3.13 mmol/g and 2.84 mmol/g, respectively. The findings obtained by 1H NMR and elemental analysis indicated to phenyl propane unit of the lignin with C9 structural formula as C9 HAl 3.84HAr2.19S0.2O0.8(OH1.38(OCH31.42. Due to poor solubility of the lignin in tetrahydrofuran (THF, acetylated lignin was used in the GPC analysis, by which number-average molecular weight  of the lignin was calculated as 992 g/mol.

  17. Compact NMR

    Energy Technology Data Exchange (ETDEWEB)

    Bluemich, Bernhard; Haber-Pohlmeier, Sabina; Zia, Wasif [RWTH Aachen Univ. (Germany). Inst. fuer Technische und Makromolekulare Chemie (ITMC)

    2014-06-01

    Nuclear Magnetic Resonance (NMR) spectroscopy is the most popular method for chemists to analyze molecular structures, while Magnetic Resonance Imaging (MRI) is a non-invasive diagnostic tool for medical doctors that provides high-contrast images of biological tissue. In both applications, the sample (or patient) is positioned inside a large, superconducting magnet to magnetize the atomic nuclei. Interrogating radio-frequency pulses result in frequency spectra that provide the chemist with molecular information, the medical doctor with anatomic images, and materials scientist with NMR relaxation parameters. Recent advances in magnet technology have led to a variety of small permanent magnets to allow compact and low-cost instruments. The goal of this book is to provide an introduction to the practical use of compact NMR at a level nearly as basic as the operation of a smart phone.

  18. Characterization of mu s-ms dynamics of proteins using a combined analysis of N-15 NMR relaxation and chemical shift: Conformational exchange in plastocyanin induced by histidine protonations

    DEFF Research Database (Denmark)

    Hass, M. A. S.; Thuesen, Marianne Hallberg; Christensen, Hans Erik Mølager

    2004-01-01

    of the exchanging species can be determined independently of the relaxation rates. The applicability of the approach is demonstrated by a detailed analysis of the conformational exchange processes previously observed in the reduced form of the blue copper protein, plastocyanin from the cyanobacteria Anabaena......An approach is presented that allows a detailed, quantitative characterization of conformational exchange processes in proteins on the mus-ms time scale. The approach relies on a combined analysis of NMR relaxation rates and chemical shift changes and requires that the chemical shift...... quantitatively by the correlation between the R-ex terms and the corresponding chemical shift differences of the exchanging species. By this approach, the R-ex terms of N-15 nuclei belonging to contiguous regions in the protein could be assigned to the same exchange process. Furthermore, the analysis...

  19. Analysis of a nanocrystalline polymer dispersion of ebselen using solid-state NMR, Raman microscopy, and powder X-ray diffraction.

    Science.gov (United States)

    Vogt, Frederick G; Williams, Glenn R

    2012-07-01

    Nanocrystalline drug-polymer dispersions are of significant interest in pharmaceutical delivery. The purpose of this work is to demonstrate the applicability of methods based on two-dimensional (2D) and multinuclear solid-state NMR (SSNMR) to a novel nanocrystalline pharmaceutical dispersion of ebselen with polyvinylpyrrolidone-vinyl acetate (PVP-VA), after initial characterization with other techniques. A nanocrystalline dispersion of ebselen with PVP-VA was prepared and characterized by powder X-ray diffraction (PXRD), confocal Raman microscopy and mapping, and differential scanning calorimetry (DSC), and then subjected to detailed 1D and 2D SSNMR analysis involving ¹H, ¹³C, and ⁷⁷Se isotopes and ¹H spin diffusion. PXRD was used to show that dispersion contains nanocrystalline ebselen in the 35-60 nm size range. Confocal Raman microscopy and spectral mapping were able to detect regions where short-range interactions may occur between ebselen and PVP-VA. Spin diffusion effects were analyzed using 2D SSNMR experiments and are able to directly detect interactions between ebselen and the surrounding PVP-VA. The methods used here, particularly the 2D SSNMR methods based on spin diffusion, provided detailed structural information about a nanocrystalline polymer dispersion of ebselen, and should be useful in other studies of these types of materials.

  20. Light water reactor fuel analysis code. FEMAXI-6 (Ver.1). Detailed structure and user's manual

    International Nuclear Information System (INIS)

    Suzuki, Motoe; Saitou, Hiroaki

    2006-02-01

    A light water reactor fuel analysis code FEMAXI-6 is an advanced version which has been produced by integrating the former version FEMAXI-V with numerous functional improvements and extensions. In particular, the FEMAXI-6 code has attained a complete coupled solution of thermal analysis and mechanical analysis, enabling an accurate prediction of pellet-clad gap size and PCMI in high burnup fuel rods. Also, such new models have been implemented as pellet-clad bonding and fission gas bubble swelling, and linkage function with detailed burning analysis code has been enhanced. Furthermore, a number of new materials properties and parameters have been introduced. With these advancements, the FEMAXI-6 code has been upgraded to a versatile analytical tool for high burnup fuel behavior not only in the normal operation but also in anticipated transient conditions. This report describes in detail the design, basic theory and structure, models and numerical method, improvements and extensions, and method of model modification. In order to facilitate effective and wide-ranging application of the code, formats and methods of input/output of the code are also described, and a sample output in an actual form is included. (author)

  1. Solid-state NMR analysis of membrane proteins and protein aggregates by proton detected spectroscopy

    International Nuclear Information System (INIS)

    Zhou, Donghua H.; Nieuwkoop, Andrew J.; Berthold, Deborah A.; Comellas, Gemma; Sperling, Lindsay J.; Tang, Ming; Shah, Gautam J.; Brea, Elliott J.; Lemkau, Luisel R.; Rienstra, Chad M.

    2012-01-01

    Solid-state NMR has emerged as an important tool for structural biology and chemistry, capable of solving atomic-resolution structures for proteins in membrane-bound and aggregated states. Proton detection methods have been recently realized under fast magic-angle spinning conditions, providing large sensitivity enhancements for efficient examination of uniformly labeled proteins. The first and often most challenging step of protein structure determination by NMR is the site-specific resonance assignment. Here we demonstrate resonance assignments based on high-sensitivity proton-detected three-dimensional experiments for samples of different physical states, including a fully-protonated small protein (GB1, 6 kDa), a deuterated microcrystalline protein (DsbA, 21 kDa), a membrane protein (DsbB, 20 kDa) prepared in a lipid environment, and the extended core of a fibrillar protein (α-synuclein, 14 kDa). In our implementation of these experiments, including CONH, CO(CA)NH, CANH, CA(CO)NH, CBCANH, and CBCA(CO)NH, dipolar-based polarization transfer methods have been chosen for optimal efficiency for relatively high protonation levels (full protonation or 100 % amide proton), fast magic-angle spinning conditions (40 kHz) and moderate proton decoupling power levels. Each H–N pair correlates exclusively to either intra- or inter-residue carbons, but not both, to maximize spectral resolution. Experiment time can be reduced by at least a factor of 10 by using proton detection in comparison to carbon detection. These high-sensitivity experiments are especially important for membrane proteins, which often have rather low expression yield. Proton-detection based experiments are expected to play an important role in accelerating protein structure elucidation by solid-state NMR with the improved sensitivity and resolution.

  2. A many-body analysis of NMR in spin-1/2 system

    International Nuclear Information System (INIS)

    Roy, G.K.; Sinha, S.K.

    1977-01-01

    The NMR absorption in a spin-1/2 system at finite temperature has been analysed by using the linear response theory and calculating the finite-temperature retarted spin Green's function. In this calculations, the Drone-Fermion representation for the spin operators has been used. A model spin-lattice interaction which is linear in phonon and Fermion operators has been considered, and its effect on a mutually non-interacting spin system has been calculated using the diagrammatic expansions technique. It is found that the complete summing up of a particular class of diagrams yields the Lorentzian shape of the resonance line. (author)

  3. Analysis of Hydroperoxides in solid Polyethylene by NMR and EPR Spectroscopy

    International Nuclear Information System (INIS)

    Assink, Roger A.; Celina, Mathias C.; Dunbar, Timothy D.; Alam, Todd M.; Clough, Roger Lee; Gillen, Kenneth T.

    2000-01-01

    The authors have shown that the hydroperoxide species in γ-irradiated 13 C-polyethylene can be directly observed by 13 C MAS NMR spectroscopy. The experiment was performed without the need for special sample preparation such as chemical derivatization or dissolution. Annealing experiments were employed to study the thermal decomposition of the hydroperoxide species and to measure an activation energy of 98 kJ/mol. EPR spectroscopy suggests that residual polyenyl and alkylperoxy radicals are predominantly trapped in interracial or crystalline regions, while the peroxy radicals observed after UV-photolysis of hydroperoxides are in amorphous regions

  4. Bioinformatics tools for the analysis of NMR metabolomics studies focused on the identification of clinically relevant biomarkers.

    Science.gov (United States)

    Puchades-Carrasco, Leonor; Palomino-Schätzlein, Martina; Pérez-Rambla, Clara; Pineda-Lucena, Antonio

    2016-05-01

    Metabolomics, a systems biology approach focused on the global study of the metabolome, offers a tremendous potential in the analysis of clinical samples. Among other applications, metabolomics enables mapping of biochemical alterations involved in the pathogenesis of diseases, and offers the opportunity to noninvasively identify diagnostic, prognostic and predictive biomarkers that could translate into early therapeutic interventions. Particularly, metabolomics by Nuclear Magnetic Resonance (NMR) has the ability to simultaneously detect and structurally characterize an abundance of metabolic components, even when their identities are unknown. Analysis of the data generated using this experimental approach requires the application of statistical and bioinformatics tools for the correct interpretation of the results. This review focuses on the different steps involved in the metabolomics characterization of biofluids for clinical applications, ranging from the design of the study to the biological interpretation of the results. Particular emphasis is devoted to the specific procedures required for the processing and interpretation of NMR data with a focus on the identification of clinically relevant biomarkers. © The Author 2015. Published by Oxford University Press. For Permissions, please email: journals.permissions@oup.com.

  5. 1H NMR Spectroscopy and Multivariate Analysis of Monovarietal EVOOs as a Tool for Modulating Coratina-Based Blends

    Directory of Open Access Journals (Sweden)

    Laura Del Coco

    2014-04-01

    Full Text Available Coratina cultivar-based olives are very common among 100% Italian extra virgin olive oils (EVOOs. Often, the very spicy character of this cultivar, mostly due to the high polyphenols concentration, requires blending with other “sweetener” oils. In this work, monovarietal EVOO samples from the Coratina cultivar (Apulia, Italy were investigated and compared with monovarietal EVOO from native or recently introduced Apulian (Italy cultivars (Ogliarola Garganica, Ogliarola Barese, Cima di Mola, Peranzana, Picholine, from Calabria (Italy (Carolea and Rossanese and from other Mediterranean countries, such as Spain (Picual and Greece (Kalamata and Koroneiki by 1H NMR spectroscopy and multivariate analysis (principal component analysis (PCA. In this regard, NMR signals could allow a first qualitative evaluation of the chemical composition of EVOO and, in particular, of its minor component content (phenols and aldehydes, an intrinsic behavior of EVOO taste, related to the cultivar and geographical origins. Moreover, this study offers an opportunity to address blended EVOOs tastes by using oils from a specific region or country of origin.

  6. Author Details

    African Journals Online (AJOL)

    Journal Home > Advanced Search > Author Details. Log in or Register to get access to full text downloads. ... Okeke, EO. Vol 10 (2006) - Articles Analysis of Stokes waves theory as a diffusion problem. Abstract · Vol 11 (2007) - Articles On the impact of wave-current on Stokes waves. Abstract. ISSN: 1116-4336. AJOL African ...

  7. A suite of Mathematica notebooks for the analysis of protein main chain 15N NMR relaxation data

    International Nuclear Information System (INIS)

    Spyracopoulos, Leo

    2006-01-01

    A suite of Mathematica notebooks has been designed to ease the analysis of protein main chain 15 N NMR relaxation data collected at a single magnetic field strength. Individual notebooks were developed to perform the following tasks: nonlinear fitting of 15 N-T 1 and -T 2 relaxation decays to a two parameter exponential decay, calculation of the principal components of the inertia tensor from protein structural coordinates, nonlinear optimization of the principal components and orientation of the axially symmetric rotational diffusion tensor, model-free analysis of 15 N-T 1 , -T 2 , and { 1 H}- 15 N NOE data, and reduced spectral density analysis of the relaxation data. The principle features of the notebooks include use of a minimal number of input files, integrated notebook data management, ease of use, cross-platform compatibility, automatic visualization of results and generation of high-quality graphics, and output of analyses in text format

  8. Development of a detailed core flow analysis code for prismatic fuel reactors

    International Nuclear Information System (INIS)

    Bennett, R.G.

    1990-01-01

    The detailed analysis of the core flow distribution in prismatic fuel reactors is of interest for modular high-temperature gas-cooled reactor (MHTGR) design and safety analyses. Such analyses involve the steady-state flow of helium through highly cross-connected flow paths in and around the prismatic fuel elements. Several computer codes have been developed for this purpose. However, since they are proprietary codes, they are not generally available for independent MHTGR design confirmation. The previously developed codes do not consider the exchange or diversion of flow between individual bypass gaps with much detail. Such a capability could be important in the analysis of potential fuel block motion, such as occurred in the Fort St. Vrain reactor, or for the analysis of the conditions around a flow blockage or misloaded fuel block. This work develops a computer code with fairly general-purpose capabilities for modeling the flow in regions of prismatic fuel cores. The code, called BYPASS solves a finite difference control volume formulation of the compressible, steady-state fluid flow in highly cross-connected flow paths typical of the MHTGR

  9. Resolution requirements for monitor viewing of digital flat-panel detector radiographs: a contrast detail analysis

    International Nuclear Information System (INIS)

    Peer, Siegfried; Giacomuzzi, Salvatore M.; Peer, Regina; Gassner, Eva; Steingruber, Iris; Jaschke, Werner

    2003-01-01

    With the introduction of digital flat-panel detector systems into clinical practice, the still unresolved question of resolution requirements for picture archiving communication system (PACS) workstation monitors has gained new momentum. This contrast detail analysis was thus performed to define the differences in observer performance in the detection of small low-contrast objects on clinical 1K and 2K monitor workstations. Images of the CDRAD 2.0 phantom were acquired at varying exposures on an indirect-type digital flat-panel detector. Three observers evaluated a total of 15 images each with respect to the threshold contrast for each detail size. The numbers of correctly identified objects were determined for all image subsets. No significant difference in the correct detection ratio was detected among the observers; however, the difference between the two types of workstations (1K vs 2K monitors) despite less than 3% was significant at a 95% confidence level. Slight but statistically significant differences exist in the detection of low-contrast nodular details visualized on 1K- and 2K-monitor workstations. Further work is needed to see if this result holds true also for comparison of clinical flat-panel detector images and may, for example, exert an influence on the diagnostic accuracy of chest X-ray readings. (orig.)

  10. Structural properties of carbon nanotubes derived from 13C NMR

    KAUST Repository

    Abou-Hamad, E.; Babaa, M.-R.; Bouhrara, M.; Kim, Y.; Saih, Y.; Dennler, S.; Mauri, F.; Basset, Jean-Marie; Goze-Bac, C.; Wå gberg, T.

    2011-01-01

    We present a detailed experimental and theoretical study on how structural properties of carbon nanotubes can be derived from 13C NMR investigations. Magic angle spinning solid state NMR experiments have been performed on single- and multiwalled

  11. Three-dimensional absorbed dose determinations by N.M.R. analysis of phantom-dosemeters

    International Nuclear Information System (INIS)

    Gambarini, G.; Birattari, C.; Fumagalli, M.L.; Vai, A.; Monti, D.; Salvadori, P.; Facchielli, L.; Sichirollo, A.E.

    1996-01-01

    Magnetic resonance imaging of a tissue-equivalent phantom is a promising technique for three-dimensional determination of absorbed dose from ionizing radiation. A reliable method of determining the spatial distribution of absorbed dose is indispensable for the planning of treatment in the presently developed radiotherapy techniques aimed at obtaining high energy selectively delivered to cancerous tissues, with low dose delivered to the surrounding healthy tissue. Aqueous gels infused with the Fricke dosemeter (i.e. with a ferrous sulphate solution), as proposed in 1984 by Gore et al., have shown interesting characteristics and, in spite of some drawbacks that cause a few limitations to their utilisation, they have shown the feasibility of three-dimensional dose determinations by nuclear magnetic resonance (NMR) imaging. Fricke-infused agarose gels with various compositions have been analysed, considering the requirements of the new radiotherapy techniques, in particular Boron Neutron Capture Therapy (B.N.C.T.) and proton therapy. Special attention was paid to obtain good tissue equivalence for every radiation type of interest. In particular, the tissue equivalence for thermal neutrons, which is a not simple problem, has also been satisfactorily attained. The responses of gel-dosemeters having the various chosen compositions have been analysed, by mean of NMR instrumentation. Spectrophotometric measurements have also been performed, to verify the consistence of the results. (author)

  12. Piperamides from Piper ottonoides by NMR and GC-MS based mixture analysis

    International Nuclear Information System (INIS)

    Wolff, Thiago; Valente, Ligia M.M.; Magalhães, Alvicler; Guimarães, Elsie F.

    2015-01-01

    The species Piper ottonoides Yuncker (Piperaceae), known as 'joão-brandim', is a shrub that occurs in the Brazilian Amazon rainforest. Its roots and leaves are used in traditional medicine as local anesthetic to treat toothache and sore throat. In this study, the structural characterization in mixture of isobutyl amides present in semi-purified fractions from fruits, leaves, stems and roots of P. ottonoides was achieved by employing gas chromatography-mass spectrometry (GC-MS) and a combination of nuclear magnetic resonance (NMR) techniques ( 1 H, 1 H- 1 H COSY, 1 H- 13 CHSQC, 1 H- 13 CHMBC, TOCSY and 1 H- 1 H J-RES). The MS fragmentation patterns and the NMR chemical shifts, multiplicities, coupling constants and the signal correlations in the two-dimensional spectra were carefully analyzed also taking into account some key elements of differentiation among the compounds. The data set allowed identifying unequivocally the new amide N-isobutyl-7-(4'- methoxyphenyl)-2E,4E-heptadienamide, which we named ottonoidenamide as well as piperovatine and chingchengenamide A in all parts of the plant, the additional presence of pipercallosine and pipercallosidine in roots and of dihydropiperlonguminine in fruits and leaves. The presence of piperovatine and pipercallosine in P. ottonoides should be associated to its traditional use. (author)

  13. Automation of peak-tracking analysis of stepwise perturbed NMR spectra

    Energy Technology Data Exchange (ETDEWEB)

    Banelli, Tommaso; Vuano, Marco [Università di Udine, Dipartimento di Area Medica (Italy); Fogolari, Federico [INBB (Italy); Fusiello, Andrea [Università di Udine, Dipartimento Politecnico di Ingegneria e Architettura (Italy); Esposito, Gennaro [INBB (Italy); Corazza, Alessandra, E-mail: alessandra.corazza@uniud.it [Università di Udine, Dipartimento di Area Medica (Italy)

    2017-02-15

    We describe a new algorithmic approach able to automatically pick and track the NMR resonances of a large number of 2D NMR spectra acquired during a stepwise variation of a physical parameter. The method has been named Trace in Track (TinT), referring to the idea that a gaussian decomposition traces peaks within the tracks recognised through 3D mathematical morphology. It is capable of determining the evolution of the chemical shifts, intensity and linewidths of each tracked peak.The performances obtained in term of track reconstruction and correct assignment on realistic synthetic spectra were high above 90% when a noise level similar to that of experimental data were considered. TinT was applied successfully to several protein systems during a temperature ramp in isotope exchange experiments. A comparison with a state-of-the-art algorithm showed promising results for great numbers of spectra and low signal to noise ratios, when the graduality of the perturbation is appropriate. TinT can be applied to different kinds of high throughput chemical shift mapping experiments, with quasi-continuous variations, in which a quantitative automated recognition is crucial.

  14. Piperamides from Piper ottonoides by NMR and GC-MS based mixture analysis

    Energy Technology Data Exchange (ETDEWEB)

    Wolff, Thiago; Valente, Ligia M.M., E-mail: valente@iq.ufrj.br [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil). Inst. de Química; Santos, Priscila F.P. [Centro Federal de Educação Tecnológica Celso Suckow da Fonseca (UnED/CEFET), Angra dos Reis, RJ (Brazil); Magalhães, Alvicler [Universidade Estadual de Campinas (UNICAMP), SP (Brazil). Departamento de Química Inorgânica; Tinoco, Luzineide W. [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil). Instituto de Pesquisa em Produtos Naturais; Pereira, Rita C.A. [Embrapa Agroindústria Tropical, Fortaleza, CE (Brazil); Guimarães, Elsie F. [Instituto de Pesquisas Jardim Botânico do Rio de Janeiro, RJ (Brazil)

    2015-07-01

    The species Piper ottonoides Yuncker (Piperaceae), known as 'joão-brandim', is a shrub that occurs in the Brazilian Amazon rainforest. Its roots and leaves are used in traditional medicine as local anesthetic to treat toothache and sore throat. In this study, the structural characterization in mixture of isobutyl amides present in semi-purified fractions from fruits, leaves, stems and roots of P. ottonoides was achieved by employing gas chromatography-mass spectrometry (GC-MS) and a combination of nuclear magnetic resonance (NMR) techniques ({sup 1}H, {sup 1}H-{sup 1}H COSY, {sup 1}H-{sup 13}CHSQC, {sup 1}H-{sup 13}CHMBC, TOCSY and {sup 1}H-{sup 1}H J-RES). The MS fragmentation patterns and the NMR chemical shifts, multiplicities, coupling constants and the signal correlations in the two-dimensional spectra were carefully analyzed also taking into account some key elements of differentiation among the compounds. The data set allowed identifying unequivocally the new amide N-isobutyl-7-(4'- methoxyphenyl)-2E,4E-heptadienamide, which we named ottonoidenamide as well as piperovatine and chingchengenamide A in all parts of the plant, the additional presence of pipercallosine and pipercallosidine in roots and of dihydropiperlonguminine in fruits and leaves. The presence of piperovatine and pipercallosine in P. ottonoides should be associated to its traditional use. (author)

  15. Detailed Analysis of the Transient Voltage in a JT-60SA PF Coil Circuit

    International Nuclear Information System (INIS)

    Yamauchi, K.; Shimada, K.; Terakado, T.; Matsukawa, M.; Coletti, R.; Lampasi, A.; Gaio, E.; Coletti, A.; Novello, L.

    2013-01-01

    A superconducting coil system is actually complicated by the distributed parameters, e.g. the distributed mutual inductance among turns and the distributed capacitance between adjacent conductors. In this paper, such a complicated system was modeled with a reasonably simplified circuit network with lumped parameters. Then, a detailed circuit analysis was conducted to evaluate the possible voltage transient in the coil circuit. As a result, an appropriate (minimum) snubber capacitance for the Switching Network Unit, which is a fast high voltage generation circuit in JT-60SA, was obtained. (fusion engineering)

  16. Development of a detailed core flow analysis code for prismatic fuel reactors

    International Nuclear Information System (INIS)

    Bennett, R.G.

    1990-01-01

    The development of a computer code for the analysis of the detailed flow of helium in prismatic fuel reactors is reported. The code, called BYPASS, solves, a finite difference control volume formulation of the compressible, steady state fluid flow in highly cross-connected flow paths typical of the Modular High-Temperature Gas Cooled Reactor (MHTGR). The discretization of the flow in a core region typically considers the main coolant flow paths, the bypass gap flow paths, and the crossflow connections between them. 16 refs., 5 figs

  17. Fundamentals of Protein NMR Spectroscopy

    CERN Document Server

    Rule, Gordon S

    2006-01-01

    NMR spectroscopy has proven to be a powerful technique to study the structure and dynamics of biological macromolecules. Fundamentals of Protein NMR Spectroscopy is a comprehensive textbook that guides the reader from a basic understanding of the phenomenological properties of magnetic resonance to the application and interpretation of modern multi-dimensional NMR experiments on 15N/13C-labeled proteins. Beginning with elementary quantum mechanics, a set of practical rules is presented and used to describe many commonly employed multi-dimensional, multi-nuclear NMR pulse sequences. A modular analysis of NMR pulse sequence building blocks also provides a basis for understanding and developing novel pulse programs. This text not only covers topics from chemical shift assignment to protein structure refinement, as well as the analysis of protein dynamics and chemical kinetics, but also provides a practical guide to many aspects of modern spectrometer hardware, sample preparation, experimental set-up, and data pr...

  18. 1H NMR and Multivariate Analysis for Geographic Characterization of Commercial Extra Virgin Olive Oil: A Possible Correlation with Climate Data

    Directory of Open Access Journals (Sweden)

    Domenico Rongai

    2017-11-01

    Full Text Available 1H Nuclear Magnetic Resonance (NMR spectroscopy coupled with multivariate analysis has been applied in order to investigate metabolomic profiles of more than 200 extravirgin olive oils (EVOOs collected in a period of over four years (2009–2012 from different geographic areas. In particular, commercially blended EVOO samples originating from different Italian regions (Tuscany, Sicily and Apulia, as well as European (Spain and Portugal and non-European (Tunisia, Turkey, Chile and Australia countries. Multivariate statistical analysis (Principal Component Analisys (PCA and Orthogonal Partial Least Squares Discriminant Analysis (OPLS-DA applied on the NMR data revealed the existence of marked differences between Italian (in particular from Tuscany, Sicily and Apulia regions and foreign (in particular Tunisian EVOO samples. A possible correlation with available climate data has been also investigated. These results aim to develop a powerful NMR-based tool able to protect Italian olive oil productions.

  19. DNA oligonucleotide conformations: high resolution NMR studies

    International Nuclear Information System (INIS)

    Mellema, J.-R.

    1984-01-01

    The present work describes a DNA double-helix model, which is well comparable with the models derived from fibre-diffraction studies. The model has a mononucleotide repeat with torsion angles in accordance with average geometries as derived from 1 H NMR studies. Special attention was paid to reduce the number of short H-H nonbonding contacts, which are abundantly present in the 'classical' fibre-diffraction models. Chapter 3 describes the first complete assignment of a 1 H NMR spectrum of a DNA tetramer, d(TAAT). Preliminary conformational data derived from the spectral parameters recorded at 27 0 C are given. A more detailed analysis employing temperature-dependence studies is given in Chapter 4. (Auth.)

  20. Stable and rigid DTPA-like paramagnetic tags suitable for in vitro and in situ protein NMR analysis.

    Science.gov (United States)

    Chen, Jia-Liang; Zhao, Yu; Gong, Yan-Jun; Pan, Bin-Bin; Wang, Xiao; Su, Xun-Cheng

    2018-02-01

    Organic synthesis of a ligand with high binding affinities for paramagnetic lanthanide ions is an effective way of generating paramagnetic effects on proteins. These paramagnetic effects manifested in high-resolution NMR spectroscopy are valuable dynamic and structural restraints of proteins and protein-ligand complexes. A paramagnetic tag generally contains a metal chelating moiety and a reactive group for protein modification. Herein we report two new DTPA-like tags, 4PS-PyDTTA and 4PS-6M-PyDTTA that can be site-specifically attached to a protein with a stable thioether bond. Both protein-tag adducts form stable lanthanide complexes, of which the binding affinities and paramagnetic tensors are tunable with respect to the 6-methyl group in pyridine. Paramagnetic relaxation enhancement (PRE) effects of Gd(III) complex on protein-tag adducts were evaluated in comparison with pseudocontact shift (PCS), and the results indicated that both 4PS-PyDTTA and 4PS-6M-PyDTTA tags are rigid and present high-quality PREs that are crucially important in elucidation of the dynamics and interactions of proteins and protein-ligand complexes. We also show that these two tags are suitable for in-situ protein NMR analysis.

  1. Protein energetic conformational analysis from NMR chemical shifts (PECAN) and its use in determining secondary structural elements

    Energy Technology Data Exchange (ETDEWEB)

    Eghbalnia, Hamid R.; Wang Liya; Bahrami, Arash [National Magnetic Resonance Facility at Madison, Biochemistry Department (United States); Assadi, Amir [University of Wisconsin-Madison, Mathematics Department (United States); Markley, John L. [National Magnetic Resonance Facility at Madison, Biochemistry Department (United States)], E-mail: eghbalni@nmrfam.wisc.edu

    2005-05-15

    We present an energy model that combines information from the amino acid sequence of a protein and available NMR chemical shifts for the purposes of identifying low energy conformations and determining elements of secondary structure. The model ('PECAN', Protein Energetic Conformational Analysis from NMR chemical shifts) optimizes a combination of sequence information and residue-specific statistical energy function to yield energetic descriptions most favorable to predicting secondary structure. Compared to prior methods for secondary structure determination, PECAN provides increased accuracy and range, particularly in regions of extended structure. Moreover, PECAN uses the energetics to identify residues located at the boundaries between regions of predicted secondary structure that may not fit the stringent secondary structure class definitions. The energy model offers insights into the local energetic patterns that underlie conformational preferences. For example, it shows that the information content for defining secondary structure is localized about a residue and reaches a maximum when two residues on either side are considered. The current release of the PECAN software determines the well-defined regions of secondary structure in novel proteins with assigned chemical shifts with an overall accuracy of 90%, which is close to the practical limit of achievable accuracy in classifying the states.

  2. Protein energetic conformational analysis from NMR chemical shifts (PECAN) and its use in determining secondary structural elements

    International Nuclear Information System (INIS)

    Eghbalnia, Hamid R.; Wang Liya; Bahrami, Arash; Assadi, Amir; Markley, John L.

    2005-01-01

    We present an energy model that combines information from the amino acid sequence of a protein and available NMR chemical shifts for the purposes of identifying low energy conformations and determining elements of secondary structure. The model ('PECAN', Protein Energetic Conformational Analysis from NMR chemical shifts) optimizes a combination of sequence information and residue-specific statistical energy function to yield energetic descriptions most favorable to predicting secondary structure. Compared to prior methods for secondary structure determination, PECAN provides increased accuracy and range, particularly in regions of extended structure. Moreover, PECAN uses the energetics to identify residues located at the boundaries between regions of predicted secondary structure that may not fit the stringent secondary structure class definitions. The energy model offers insights into the local energetic patterns that underlie conformational preferences. For example, it shows that the information content for defining secondary structure is localized about a residue and reaches a maximum when two residues on either side are considered. The current release of the PECAN software determines the well-defined regions of secondary structure in novel proteins with assigned chemical shifts with an overall accuracy of 90%, which is close to the practical limit of achievable accuracy in classifying the states

  3. Statistical Analysis of Detailed 3-D CFD LES Simulations with Regard to CCV Modeling

    Directory of Open Access Journals (Sweden)

    Vítek Oldřich

    2016-06-01

    Full Text Available The paper deals with statistical analysis of large amount of detailed 3-D CFD data in terms of cycle-to-cycle variations (CCVs. These data were obtained by means of LES calculations of many consecutive cycles. Due to non-linear nature of Navier-Stokes equation set, there is a relatively significant CCV. Hence, every cycle is slightly different – this leads to requirement to perform statistical analysis based on ensemble averaging procedure which enables better understanding of CCV in ICE including its quantification. The data obtained from the averaging procedure provides results on different space resolution levels. The procedure is applied locally, i.e., in every cell of the mesh. Hence there is detailed CCV information on local level – such information can be compared with RANS simulations. Next, volume/mass averaging provides information at specific locations – e.g., gap between electrodes of a spark plug. Finally, volume/mass averaging of the whole combustion chamber leads to global information which can be compared with experimental data or results of system simulation tools (which are based on 0-D/1-D approach.

  4. Application of a logistic function to the analysis of contrast-detail curves

    International Nuclear Information System (INIS)

    Mumma, C.G.; Prince, J.R.

    1987-01-01

    A general logistic function has been applied to the regression analysis of radioscintigraphic contrast-detail (CD) curves obtained in the authors' laboratory and to previously published results in assorted imaging modalities. Regression analysis is based on the logistic function: d/sub min/ = d/sub min//sup sat/(1 - EXP - (K + CX)), where d/sub min/ is the minimum perceptible detail diameter at a primary contrast X, and d/sub min//sup sat/ is the saturation value of d/sub min/. K and C are regression parameters. Logistic regression in assorted imaging modalities yielded r 2 values ranging from 0.95 to 0.99. A figure of merit (FOM), the area under the CD curve (AUC), is obtained by integrating the logistic function over mathematically and clinically acceptable limits. For count densities of 200 countscm 2 and 1,000 countscm 2 , the AUC differed approximately by a factor of 2. Thus, the AUC may be a sensitive FOM

  5. Detailed Structural Analysis of Critical Wendelstein 7-X Magnet System Components

    International Nuclear Information System (INIS)

    Egorov, K.

    2006-01-01

    The Wendelstein 7-X (W7-X) stellarator experiment is presently under construction and assembly in Greifswald, Germany. The goal of the experiment is to verify that the stellarator magnetic confinement concept is a viable option for a fusion reactor. The complex W7-X magnet system requires a multi-level approach to structural analysis for which two types of finite element models are used: Firstly, global models having reasonably coarse meshes with a number of simplifications and assumptions, and secondly, local models with detailed meshes of critical regions and elements. Widely known sub-modelling technique with boundary conditions extracted from the global models is one of the approaches for local analysis with high assessment efficiency. In particular, the winding pack (WP) of the magnet coils is simulated in the global model as a homogeneous orthotropic material with effective mechanical characteristic representing its real composite structure. This assumption allows assessing the whole magnet system in terms of general structural factors like forces and moments on the support elements, displacements of the main components, deformation and stress in the coil casings, etc. In a second step local models with a detailed description of more critical WP zones are considered in order to analyze their internal components like conductor jackets, turn insulation, etc. This paper provides an overview of local analyses of several critical W7-X magnet system components with particular attention on the coil winding packs. (author)

  6. NMR imaging

    International Nuclear Information System (INIS)

    Ouchi, Toshihiro; Steiner, R.E.

    1984-01-01

    Three epidermoid and two dermoid tumours, pathologically proven, were examined by NMR and CT scans. Although most brain tumours have a low signal with a long T 1 , a dermoid cyst and one of the two components of the other dermoid tumour had a high signal and therefore a short T 1 . All three epidermoid tumours had a low signal and a long T 1 . Because of the high level contrast between some of the tumours and cerebrospinal fluid, NMR is helpful to detect the lesion. Neither of the liquid fluid levels in the tumour cysts or floating fat in the subarachnoid space was recognized in one patients, but the fine leakage of the content from the epidermoid cyst into the lateral ventricle was detected on a saturation recovery 1000 image in one case. (author)

  7. A detailed analysis of codon usage patterns and influencing factors in Zika virus.

    Science.gov (United States)

    Singh, Niraj K; Tyagi, Anuj

    2017-07-01

    Recent outbreaks of Zika virus (ZIKV) in Africa, Latin America, Europe, and Southeast Asia have resulted in serious health concerns. To understand more about evolution and transmission of ZIKV, detailed codon usage analysis was performed for all available strains. A high effective number of codons (ENC) value indicated the presence of low codon usage bias in ZIKV. The effect of mutational pressure on codon usage bias was confirmed by significant correlations between nucleotide compositions at third codon positions and ENCs. Correlation analysis between Gravy values, Aroma values and nucleotide compositions at third codon positions also indicated some influence of natural selection. However, the low codon adaptation index (CAI) value of ZIKV with reference to human and mosquito indicated poor adaptation of ZIKV codon usage towards its hosts, signifying that natural selection has a weaker influence than mutational pressure. Additionally, relative dinucleotide frequencies, geographical distribution, and evolutionary processes also influenced the codon usage pattern to some extent.

  8. KNOW YOUR NEIGHBORHOOD: A DETAILED MODEL ATMOSPHERE ANALYSIS OF NEARBY WHITE DWARFS

    Energy Technology Data Exchange (ETDEWEB)

    Giammichele, N.; Bergeron, P. [Kitt Peak National Observatory, National Optical Astronomy Observatory, which is operated by the Association of Universities for Research in Astronomy (AURA) under cooperative agreement with the National Science Foundation (United States); Dufour, P., E-mail: noemi.giammichele@astro.umontreal.ca, E-mail: pierre.bergeron@astro.umontreal.ca, E-mail: patrick.dufour@astro.umontreal.ca [Departement de Physique, Universite de Montreal, C.P. 6128, Succ. Centre-Ville, Montreal, Quebec H3C 3J7 (Canada)

    2012-04-01

    We present improved atmospheric parameters of nearby white dwarfs lying within 20 pc of the Sun. The aim of the current study is to obtain the best statistical model of the least-biased sample of the white dwarf population. A homogeneous analysis of the local population is performed combining detailed spectroscopic and photometric analyses based on improved model atmosphere calculations for various spectral types including DA, DB, DC, DQ, and DZ stars. The spectroscopic technique is applied to all stars in our sample for which optical spectra are available. Photometric energy distributions, when available, are also combined to trigonometric parallax measurements to derive effective temperatures, stellar radii, as well as atmospheric compositions. A revised catalog of white dwarfs in the solar neighborhood is presented. We provide, for the first time, a comprehensive analysis of the mass distribution and the chemical distribution of white dwarf stars in a volume-limited sample.

  9. Determination of muscle protein synthesis rates in fish using (2)H2O and (2)H NMR analysis of alanine.

    Science.gov (United States)

    Marques, Cátia; Viegas, Filipa; Rito, João; Jones, John; Viegas, Ivan

    2016-09-15

    Following administration of deuterated water ((2)H2O), the fractional synthetic rate (FSR) of a given endogenous protein can be estimated by (2)H-enrichment quantification of its alanine residues. Currently, this is measured by mass spectrometry following a derivatization procedure. Muscle FSR was measured by (1)H/(2)H NMR analysis of alanine from seabass kept for 6 days in 5% (2)H-enriched saltwater, following acid hydrolysis and amino acid isolation by cation-exchange chromatography of muscle tissue. The analysis is simple and robust, and provides precise measurements of excess alanine (2)H-enrichment in the 0.1-0.4% range from 50 mmol of alanine recovered from muscle protein. Copyright © 2016 Elsevier Inc. All rights reserved.

  10. Detailed Modeling and Irreversible Transfer Process Analysis of a Multi-Element Thermoelectric Generator System

    Science.gov (United States)

    Xiao, Heng; Gou, Xiaolong; Yang, Suwen

    2011-05-01

    Thermoelectric (TE) power generation technology, due to its several advantages, is becoming a noteworthy research direction. Many researchers conduct their performance analysis and optimization of TE devices and related applications based on the generalized thermoelectric energy balance equations. These generalized TE equations involve the internal irreversibility of Joule heating inside the thermoelectric device and heat leakage through the thermoelectric couple leg. However, it is assumed that the thermoelectric generator (TEG) is thermally isolated from the surroundings except for the heat flows at the cold and hot junctions. Since the thermoelectric generator is a multi-element device in practice, being composed of many fundamental TE couple legs, the effect of heat transfer between the TE couple leg and the ambient environment is not negligible. In this paper, based on basic theories of thermoelectric power generation and thermal science, detailed modeling of a thermoelectric generator taking account of the phenomenon of energy loss from the TE couple leg is reported. The revised generalized thermoelectric energy balance equations considering the effect of heat transfer between the TE couple leg and the ambient environment have been derived. Furthermore, characteristics of a multi-element thermoelectric generator with irreversibility have been investigated on the basis of the new derived TE equations. In the present investigation, second-law-based thermodynamic analysis (exergy analysis) has been applied to the irreversible heat transfer process in particular. It is found that the existence of the irreversible heat convection process causes a large loss of heat exergy in the TEG system, and using thermoelectric generators for low-grade waste heat recovery has promising potential. The results of irreversibility analysis, especially irreversible effects on generator system performance, based on the system model established in detail have guiding significance for

  11. Principal component analysis for verifying 1H NMR spectral assignments. The case of 3-aryl (1,2,4)-oxadiazole-5-carbohydrazide benzylidene

    International Nuclear Information System (INIS)

    Silva, Joao Bosco P. da; Malvestiti, Ivani; Hallwass, Fernando; Ramos, Mozart N.; Leite, Lucia F.C. da Costa; Barreiro, Eliezer J.

    2005-01-01

    The 1 H NMR data set of a series of 3-aryl (1,2,4)-oxadiazole-5-carbohydrazide benzylidene derivatives synthesized in our group was analyzed using the chemometric technique of principal component analysis (PCA). Using the original 1H NMR data PCA allowed identifying some misassignments of the proton aromatic chemical shifts. As a consequence of this multivariate analysis, nuclear Overhauser difference experiments were performed to investigate the ambiguity of other assignments of the ortho and meta aromatic hydrogens for the compound with the bromine substituent. The effect of the 1,2,4-oxadiazole group as an electron acceptor, mainly for the hydrogens 12,13, has been highlighted. (author)

  12. Facile deferration of commercial fertilizers containing iron chelates for their NMR analysis.

    Science.gov (United States)

    Laghi, Luca; Alcañiz, Sara; Cerdán, Mar; Gomez-Gallego, Mar; Sierra, Miguel Angel; Placucci, Giuseppe; Cremonini, Mauro Andrea

    2009-06-24

    Ethylenediamine-N,N'-bis(o-hydroxyphenylacetic) acid (o,o-EDDHA) is widely used in commercial formulations as a Fe(3+) chelating agent to remedy iron shortage in calcareous and alkaline soils. Commercially available o,o-EDDHA-Fe(3+) formulations contain a mixture of EDDHA regioisomers (o,p-EDDHA and p,p-EDDHA), together with other, still uncharacterized, products. NMR spectroscopy can be applied to their study as long as iron is accurately removed prior to the observation. This paper shows that it is possible to obtain a deferrated solution of the organic ligands present in commercial fertilizers containing the EDDHA-Fe(3+) chelate by treating the chelate with ferrocyanide, thus forming Prussian Blue that can be easily removed by centrifugation. This iron removal process does not cause significant losses of the o,o-EDDHA ligand or its minor structural isomers.

  13. Detailed analysis of surface asperity deformation mechanism in diffusion bonding of steel hollow structural components

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, C. [School of Materials Science and Engineering, Northwestern Polytechnical University, Xi’an 710072 (China); Laboratoire de Mecanique des Contacts et des Structures (LaMCoS), INSA Lyon, 20 Avenue des Sciences, F-69621 Villeurbanne Cedex (France); Li, H. [School of Materials Science and Engineering, Northwestern Polytechnical University, Xi’an 710072 (China); Li, M.Q., E-mail: zc9997242256@126.com [School of Materials Science and Engineering, Northwestern Polytechnical University, Xi’an 710072 (China)

    2016-05-15

    Graphical abstract: This study focused on the detailed analysis of surface asperity deformation mechanism in diffusion bonding of steel hollow structural component. A special surface with regular patterns was processed to be joined so as to observe the extent of surface asperity deformation under different applied bonding pressures. Fracture surface characteristic combined with surface roughness profiles distinctly revealed the enhanced surface asperity deformation as the applied pressure increases. The influence of surface asperity deformation mechanism on joint formation was analyzed: (a) surface asperity deformation not only directly expanded the interfacial contact areas, but also released deformation heat and caused defects, indirectly accelerating atomic diffusion, then benefits to void shrinkage; (b) surface asperity deformation readily introduced stored energy difference between two opposite sides of interface grain boundary, resulting in strain induced interface grain boundary migration. In addition, the influence of void on interface grain boundary migration was analyzed in detail. - Highlights: • A high quality hollow structural component has been fabricated by diffusion bonding. • Surface asperity deformation not only expands the interfacial contact areas, but also causes deformation heat and defects to improve the atomic diffusion. • Surface asperity deformation introduces the stored energy difference between the two opposite sides of interface grain boundary, leading to strain induced interface grain boundary migration. • The void exerts a dragging force on the interface grain boundary to retard or stop interface grain boundary migration. - Abstract: This study focused on the detailed analysis of surface asperity deformation mechanism in similar diffusion bonding as well as on the fabrication of high quality martensitic stainless steel hollow structural components. A special surface with regular patterns was processed to be joined so as to

  14. Integrative NMR for biomolecular research

    International Nuclear Information System (INIS)

    Lee, Woonghee; Cornilescu, Gabriel; Dashti, Hesam; Eghbalnia, Hamid R.; Tonelli, Marco; Westler, William M.; Butcher, Samuel E.; Henzler-Wildman, Katherine A.; Markley, John L.

    2016-01-01

    NMR spectroscopy is a powerful technique for determining structural and functional features of biomolecules in physiological solution as well as for observing their intermolecular interactions in real-time. However, complex steps associated with its practice have made the approach daunting for non-specialists. We introduce an NMR platform that makes biomolecular NMR spectroscopy much more accessible by integrating tools, databases, web services, and video tutorials that can be launched by simple installation of NMRFAM software packages or using a cross-platform virtual machine that can be run on any standard laptop or desktop computer. The software package can be downloaded freely from the NMRFAM software download page ( http://pine.nmrfam.wisc.edu/download-packages.html http://pine.nmrfam.wisc.edu/download_packages.html ), and detailed instructions are available from the Integrative NMR Video Tutorial page ( http://pine.nmrfam.wisc.edu/integrative.html http://pine.nmrfam.wisc.edu/integrative.html ).

  15. Integrative NMR for biomolecular research

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Woonghee, E-mail: whlee@nmrfam.wisc.edu; Cornilescu, Gabriel; Dashti, Hesam; Eghbalnia, Hamid R.; Tonelli, Marco; Westler, William M.; Butcher, Samuel E.; Henzler-Wildman, Katherine A.; Markley, John L., E-mail: markley@nmrfam.wisc.edu [University of Wisconsin-Madison, National Magnetic Resonance Facility at Madison and Biochemistry Department (United States)

    2016-04-15

    NMR spectroscopy is a powerful technique for determining structural and functional features of biomolecules in physiological solution as well as for observing their intermolecular interactions in real-time. However, complex steps associated with its practice have made the approach daunting for non-specialists. We introduce an NMR platform that makes biomolecular NMR spectroscopy much more accessible by integrating tools, databases, web services, and video tutorials that can be launched by simple installation of NMRFAM software packages or using a cross-platform virtual machine that can be run on any standard laptop or desktop computer. The software package can be downloaded freely from the NMRFAM software download page ( http://pine.nmrfam.wisc.edu/download-packages.html http://pine.nmrfam.wisc.edu/download{sub p}ackages.html ), and detailed instructions are available from the Integrative NMR Video Tutorial page ( http://pine.nmrfam.wisc.edu/integrative.html http://pine.nmrfam.wisc.edu/integrative.html ).

  16. Developments in remote sensing technology enable more detailed urban flood risk analysis.

    Science.gov (United States)

    Denniss, A.; Tewkesbury, A.

    2009-04-01

    digital airborne sensors, both optical and lidar, to produce the input layer for surface water flood modelling. A national flood map product has been created. The new product utilises sophisticated modelling techniques, perfected over many years, which harness graphical processing power. This product will prove particularly valuable for risk assessment decision support within insurance/reinsurance, property/environmental, utilities, risk management and government agencies. However, it is not just the ground elevation that determines the behaviour of surface water. By combining height information (surface and terrain) with high resolution aerial photography and colour infrared imagery, a high definition land cover mapping dataset (LandBase) is being produced, which provides a precise measure of sealed versus non sealed surface. This will allows even more sophisticated modelling of flood scenarios. Thus, the value of airborne survey data can be demonstrated by flood risk analysis down to individual addresses in urban areas. However for some risks, an even more detailed survey may be justified. In order to achieve this, Infoterra is testing new 360˚ mobile lidar technology. Collecting lidar data from a moving vehicle allows each street to be mapped in very high detail, allowing precise information about the location, size and shape of features such as kerbstones, gullies, road camber and building threshold level to be captured quickly and accurately. These data can then be used to model the problem of overland flood risk at the scale of individual properties. Whilst at present it might be impractical to undertake such detailed modelling for all properties, these techniques can certainly be used to improve the flood risk analysis of key locations. This paper will demonstrate how these new high resolution remote sensing techniques can be combined to provide a new resolution of detail to aid urban flood modelling.

  17. Business Management Simulations – a detailed industry analysis as well as recommendations for the future

    Directory of Open Access Journals (Sweden)

    Michael Batko

    2016-06-01

    Full Text Available Being exposed to serious games showed that some simulations widely vary in quality and learning outcome. In order to get to the bottom of best practices a detailed review of business management simulation literature was conducted. Additionally, an industry analysis was performed, by interviewing 17 simulation companies, testing a range of full and demo games, and conducting secondary research. The findings from both research efforts were then collated and cross-referenced against each other in order to determine three things: firstly, the practices and features used by simulation companies that have not yet been the subject of academic research; secondly, the most effective features, elements and inclusions within simulations that best assist in the achievement of learning outcomes and enhancement the user experience; and finally, ‘best practices’ in teaching a business management course in a university or company with the assistance of a simulation. Identified gaps in the current research were found to include the effectiveness of avatars, transparent pricing and the benefits of competing the simulation against other teams as opposed to the computer. In relation to the second and third objectives of the research, the findings were used to compile a business plan, with detailed recommendations for companies looking to develop a new simulation, and for instructors implementing and coordinating the use of a simulation in a business management context.

  18. Contrast-detail analysis of three flat panel detectors for digital radiography

    International Nuclear Information System (INIS)

    Borasi, Giovanni; Samei, Ehsan; Bertolini, Marco; Nitrosi, Andrea; Tassoni, Davide

    2006-01-01

    In this paper we performed a contrast detail analysis of three commercially available flat panel detectors, two based on the indirect detection mechanism (GE Revolution XQ/i, system A, and Trixell/Philips Pixium 4600, system B) and one based on the direct detection mechanism (Hologic DirectRay DR 1000, system C). The experiment was conducted using standard x-ray radiation quality and a widely used contrast-detail phantom. Images were evaluated using a four alternative forced choice paradigm on a diagnostic-quality softcopy monitor. At the low and intermediate exposures, systems A and B gave equivalent performances. At the high dose levels, system A performed better than system B in the entire range of target sizes, even though the pixel size of system A was about 40% larger than that of system B. At all the dose levels, the performances of the system C (direct system) were lower than those of system A and B (indirect systems). Theoretical analyses based on the Perception Statistical Model gave similar predicted SNR T values corresponding to an observer efficiency of about 0.08 for systems A and B and 0.05 for system C

  19. Detailed precision and accuracy analysis of swarm parameters from a pulsed Townsend experiment

    Science.gov (United States)

    Haefliger, P.; Franck, C. M.

    2018-02-01

    A newly built pulsed Townsend experimental setup which allows one to measure both electron and ion currents is presented. The principle of pulsed Townsend measurements itself is well established to obtain swarm parameters such as the effective ionization rate coefficient, the density-reduced mobility, and the density-normalized longitudinal diffusion coefficient. The main novelty of the present contribution is a detailed and comprehensive analysis of the entire measurement and evaluation chain with respect to accuracy, precision, and reproducibility. The influence of the input parameters (gap distance, applied voltage, measured pressure, and temperature) is analyzed in detail. An overall accuracy of ±0.5% in the density reduced electric field (E/N) is achieved, which is close to the theoretically possible limit using the chosen components. The precision of the experimental results is higher than the accuracy. Through an extensive measurement campaign, the repeatability of our measurements proved to be high and similar to the precision. The reproducibility of results at identical (E/N) is similar to the precision for different distances but decreases for varying pressures. For benchmark purposes, measurements for Ar, CO2, and N2 are presented and compared with our previous experimental setup, simulations, and other experimental references.

  20. A self optimizing synthetic organic reactor system using real-time in-line NMR spectroscopy† †Electronic supplementary information (ESI) available: Details about the methodology, LabView scripts, experimental set-ups, additional spectra and self-optimization can be found in the SI. See DOI: 10.1039/c4sc03075c Click here for additional data file.

    Science.gov (United States)

    Sans, Victor; Porwol, Luzian; Dragone, Vincenza

    2015-01-01

    A configurable platform for synthetic chemistry incorporating an in-line benchtop NMR that is capable of monitoring and controlling organic reactions in real-time is presented. The platform is controlled via a modular LabView software control system for the hardware, NMR, data analysis and feedback optimization. Using this platform we report the real-time advanced structural characterization of reaction mixtures, including 19F, 13C, DEPT, 2D NMR spectroscopy (COSY, HSQC and 19F-COSY) for the first time. Finally, the potential of this technique is demonstrated through the optimization of a catalytic organic reaction in real-time, showing its applicability to self-optimizing systems using criteria such as stereoselectivity, multi-nuclear measurements or 2D correlations. PMID:29560211

  1. Autonomous driving in NMR.

    Science.gov (United States)

    Perez, Manuel

    2017-01-01

    The automatic analysis of NMR data has been a much-desired endeavour for the last six decades, as it is the case with any other analytical technique. This need for automation has only grown as advances in hardware; pulse sequences and automation have opened new research areas to NMR and increased the throughput of data. Full automatic analysis is a worthy, albeit hard, challenge, but in a world of artificial intelligence, instant communication and big data, it seems that this particular fight is happening with only one technique at a time (let this be NMR, MS, IR, UV or any other), when the reality of most laboratories is that there are several types of analytical instrumentation present. Data aggregation, verification and elucidation by using complementary techniques (e.g. MS and NMR) is a desirable outcome to pursue, although a time-consuming one if performed manually; hence, the use of automation to perform the heavy lifting for users is required to make the approach attractive for scientists. Many of the decisions and workflows that could be implemented under automation will depend on the two-way communication with databases that understand analytical data, because it is desirable not only to query these databases but also to grow them in as much of an automatic manner as possible. How these databases are designed, set up and the data inside classified will determine what workflows can be implemented. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  2. Quantum mechanical, spectroscopic studies (FT-IR, FT-Raman, NMR, UV) and normal coordinates analysis on 3-([2-(diaminomethyleneamino) thiazol-4-yl] methylthio)-N'-sulfamoylpropanimidamide

    Science.gov (United States)

    Muthu, S.; Uma Maheswari, J.; Sundius, Tom

    2013-05-01

    Famotidine (3-([2-(diaminomethyleneamino) thiazol-4-yl] methylthio)-N'-sulfamoylpropanimidamide) is a histamine H2-receptor antagonist that inhibits stomach acid production, and it is commonly used in the treatment of peptic ulcer disease (PUD) and gastroesophageal reflux disease (GERD/GORD). Quantum chemical calculations of the equilibrium geometry of famotidine in the ground state were carried out using density functional theory (DFT/B3LYP) with the 6-311G(d,p) basis set. In addition, harmonic vibrational frequencies, infrared intensities and Raman activities were calculated at the same level of theory. A detailed interpretation of the infrared and Raman spectrum of the drug is also reported. Theoretical simulations of the FT-IR, and FT-Raman spectra of the title compound have been calculated. Good correlations between the experimental 1H and 13C NMR chemical shifts and calculated GIAO shielding tensors were found. The results of the energy and oscillator strength calculations by time-dependent density functional theory (TD-DFT) supplement the experimental findings. Total and partial density of state (TDOS and PDOS) and also overlap population density of state (COOP or OPDOS) diagrams analysis were presented. The dipole moment, linear polarizability and first order hyperpolarizability values were also computed. The linear polarizability and first order hyperpolarizabilities of the studied molecule indicate that the compound is a good candidate for nonlinear optical materials.

  3. A software framework for analysing solid-state MAS NMR data

    International Nuclear Information System (INIS)

    Stevens, Tim J.; Fogh, Rasmus H.; Boucher, Wayne; Higman, Victoria A.; Eisenmenger, Frank; Bardiaux, Benjamin; Rossum, Barth-Jan van; Oschkinat, Hartmut; Laue, Ernest D.

    2011-01-01

    Solid-state magic-angle-spinning (MAS) NMR of proteins has undergone many rapid methodological developments in recent years, enabling detailed studies of protein structure, function and dynamics. Software development, however, has not kept pace with these advances and data analysis is mostly performed using tools developed for solution NMR which do not directly address solid-state specific issues. Here we present additions to the CcpNmr Analysis software package which enable easier identification of spinning side bands, straightforward analysis of double quantum spectra, automatic consideration of non-uniform labelling schemes, as well as extension of other existing features to the needs of solid-state MAS data. To underpin this, we have updated and extended the CCPN data model and experiment descriptions to include transfer types and nomenclature appropriate for solid-state NMR experiments, as well as a set of experiment prototypes covering the experiments commonly employed by solid-sate MAS protein NMR spectroscopists. This work not only improves solid-state MAS NMR data analysis but provides a platform for anyone who uses the CCPN data model for programming, data transfer, or data archival involving solid-state MAS NMR data.

  4. Contrast to Noise Ratio and Contrast Detail Analysis in Mammography:A Monte Carlo Study

    International Nuclear Information System (INIS)

    Metaxas, V; Delis, H; Panayiotakis, G; Kalogeropoulou, C; Zampakis, P

    2015-01-01

    The mammographic spectrum is one of the major factors affecting image quality in mammography. In this study, a Monte Carlo (MC) simulation model was used to evaluate image quality characteristics of various mammographic spectra. The anode/filter combinations evaluated, were those traditionally used in mammography, for tube voltages between 26 and 30 kVp. The imaging performance was investigated in terms of Contrast to Noise Ratio (CNR) and Contrast Detail (CD) analysis, by involving human observers, utilizing a mathematical CD phantom. Soft spectra provided the best characteristics in terms of both CNR and CD scores, while tube voltage had a limited effect. W-anode spectra filtered with k-edge filters demonstrated an improved performance, that sometimes was better compared to softer x-ray spectra, produced by Mo or Rh anode. Regarding the filter material, k-edge filters showed superior performance compared to Al filters. (paper)

  5. Emission Properties, Solubility, Thermodynamic Analysis and NMR Studies of Rare-Earth Complexes with Two Different Phosphine Oxides

    Directory of Open Access Journals (Sweden)

    Hiroki Iwanaga

    2010-07-01

    Full Text Available The paper proposes novel molecular designs for rare-earth complexes involving the introduction of two different phosphine oxide structures into one rare-earth ion. These designs are effective for improving solubility and emission intensity. Additionally, the complexes are indispensable for realizing high performances in LEDs and security media. The thermodynamic properties of Eu(III complexes are correlated with the solubility. Correlations between coordination structures and emission intensity were explained by NMR analysis. The luminous flux of red LED devices with Eu(III complexes is very high (20 mA, 870 m lumen. A new white LED has its largest spectra intensity in the red region and a human look much more vividly under this light.

  6. Selective {sup 2}H and {sup 13}C labeling in NMR analysis of solution protein structure and dynamics

    Energy Technology Data Exchange (ETDEWEB)

    LeMaster, D.M. [Northwestern Univ., Evanston, IL (United States)

    1994-12-01

    Preparation of samples bearing combined isotope enrichment patterns has played a central role in the recent advances in NMR analysis of proteins in solution. In particular, uniform {sup 13}C, {sup 15}N enrichment has made it possible to apply heteronuclear multidimensional correlation experiments for the mainchain assignments of proteins larger than 30 KDa. In contrast, selective labeling approaches can offer advantages in terms of the directedness of the information provided, such as chirality and residue type assignments, as well as through enhancements in resolution and sensitivity that result from editing the spectral complexity, the relaxation pathways and the scalar coupling networks. In addition, the combination of selective {sup 13}C and {sup 2}H enrichment can greatly facilitate the determination of heteronuclear relaxation behavior.

  7. Patterns of Failure After MammoSite Brachytherapy Partial Breast Irradiation: A Detailed Analysis

    International Nuclear Information System (INIS)

    Chen, Sea; Dickler, Adam; Kirk, Michael; Shah, Anand; Jokich, Peter; Solmos, Gene; Strauss, Jonathan; Dowlatshahi, Kambiz; Nguyen, Cam; Griem, Katherine

    2007-01-01

    Purpose: To report the results of a detailed analysis of treatment failures after MammoSite breast brachytherapy for partial breast irradiation from our single-institution experience. Methods and Materials: Between October 14, 2002 and October 23, 2006, 78 patients with early-stage breast cancer were treated with breast-conserving surgery and accelerated partial breast irradiation using the MammoSite brachytherapy applicator. We identified five treatment failures in the 70 patients with >6 months' follow-up. Pathologic data, breast imaging, and radiation treatment plans were reviewed. For in-breast failures more than 2 cm away from the original surgical bed, the doses delivered to the areas of recurrence by partial breast irradiation were calculated. Results: At a median follow-up time of 26.1 months, five treatment failures were identified. There were three in-breast failures more than 2 cm away from the original surgical bed, one failure directly adjacent to the original surgical bed, and one failure in the axilla with synchronous distant metastases. The crude failure rate was 7.1% (5 of 70), and the crude local failure rate was 5.7% (4 of 70). Estimated progression-free survival at 48 months was 89.8% (standard error 4.5%). Conclusions: Our case series of 70 patients with >6 months' follow-up and a median follow-up of 26 months is the largest single-institution report to date with detailed failure analysis associated with MammoSite brachytherapy. Our failure data emphasize the importance of patient selection when offering partial breast irradiation

  8. Structure determination of helical filaments by solid-state NMR spectroscopy

    Science.gov (United States)

    Ahmed, Mumdooh; Spehr, Johannes; König, Renate; Lünsdorf, Heinrich; Rand, Ulfert; Lührs, Thorsten; Ritter, Christiane

    2016-01-01

    The controlled formation of filamentous protein complexes plays a crucial role in many biological systems and represents an emerging paradigm in signal transduction. The mitochondrial antiviral signaling protein (MAVS) is a central signal transduction hub in innate immunity that is activated by a receptor-induced conversion into helical superstructures (filaments) assembled from its globular caspase activation and recruitment domain. Solid-state NMR (ssNMR) spectroscopy has become one of the most powerful techniques for atomic resolution structures of protein fibrils. However, for helical filaments, the determination of the correct symmetry parameters has remained a significant hurdle for any structural technique and could thus far not be precisely derived from ssNMR data. Here, we solved the atomic resolution structure of helical MAVSCARD filaments exclusively from ssNMR data. We present a generally applicable approach that systematically explores the helical symmetry space by efficient modeling of the helical structure restrained by interprotomer ssNMR distance restraints. Together with classical automated NMR structure calculation, this allowed us to faithfully determine the symmetry that defines the entire assembly. To validate our structure, we probed the protomer arrangement by solvent paramagnetic resonance enhancement, analysis of chemical shift differences relative to the solution NMR structure of the monomer, and mutagenesis. We provide detailed information on the atomic contacts that determine filament stability and describe mechanistic details on the formation of signaling-competent MAVS filaments from inactive monomers. PMID:26733681

  9. Uruguay Energy Supply Options Study: a Detailed Multi-Sector Integrated Energy Supply and Demand Analysis

    International Nuclear Information System (INIS)

    Conzelmann, G.; Veselka, T.

    1997-01-01

    Uruguay is in the middle of making critical decisions affecting the design of its future energy supply system.Momentum for change is expected to come from several directions including recent and foreseeable upgrades and modifications to energy conversion facilities, the importation of natural gas from Argentina, the possibility for a stronger interconnection of regional electricity systems, the country s membership in MERCOSUR, and the potential for energy sector reforms by the Government of Uruguay.The objective of this study is to analyze the effects of several fuel diversification strategies on Uruguay s energy supply system.The analysis pays special attention to fuel substitution trends due to potential imports of natural gas via a gas pipeline from Argentina and increasing electricity ties with neighboring countries.The Government of Uruguay contracted Argonne National Laboratory (ANL) to study several energy development scenario ns with the support of several Uruguayan Institutions.Specifically, ANL was asked to conduct a detailed energy supply and demand analysis, develop energy demand projections based on an analysis of past energy demand patterns with support from local institutions, evaluate the effects of potential natural gas imports and electricity exchanges, and determine the market penetration of natural gas under various scenarios

  10. Crystallization and preliminary X-ray crystallographic analysis of the NmrA-like DDB-G0286605 protein from the social amoeba Dictyostelium discoideum

    International Nuclear Information System (INIS)

    Kim, Min-Kyu; Yim, Hyung-Soon; Kang, Sa-Ouk

    2010-01-01

    In order to investigate its structure and function, the NmrA-like domain-containing DDB-G0286605 protein from D. discoideum was expressed, purified and crystallized. X-ray diffraction analysis is reported to a resolution of 1.64 Å. The DDB-G0286605 gene product from Dictyostelium discoideum, an NmrA-like protein that belongs to the short-chain dehydrogenase/reductase family, has been crystallized by the hanging-drop vapour-diffusion method at 295 K. A 1.64 Å resolution data set was collected using synchrotron radiation. The DDB-G0286605 protein crystals belonged to space group P2 1 , with unit-cell parameters a = 67.598, b = 54.935, c = 84.219 Å, β = 109.620°. Assuming the presence of two molecules in the asymmetric unit, the solvent content was estimated to be about 43.25% with 99% probability. Molecular-replacement trials were attempted with three NmrA-like proteins, NmrA, HSCARG and QOR2, as search models, but failed. This may be a consequence of the low sequence identity between the DDB-G0286605 protein and the search models (DDB-G0286605 has a primary-sequence identity of 28, 32 and 19% to NmrA, HCARG and QOR2, respectively)

  11. Analysis of the hydrolysis of inulin using real time 1H NMR spectroscopy

    Science.gov (United States)

    Barclay, Thomas; Ginic-Markovic, Milena; Johnston, Martin R.; Cooper, Peter D.; Petrovsky, Nikolai

    2012-01-01

    The hydrolysis of various carbohydrates was investigated under acidic conditions in real time by 1H NMR spectroscopy, with a focus on the polysaccharide inulin. Sucrose was used as a model compound to illustrate the applicability of this technique. The hydrolysis of sucrose was shown to follow pseudo first order kinetics and have an activation energy of 107.0 kJ.mol−1 (s.d. 1.7 kJ.mol−1). Inulin, pullulan and glycogen also all followed pseudo first order kinetics, but had an initiation phase at least partially generated by the protonation of the glycosidic bonds. It was also demonstrated that polysaccharide chain length has an effect on the hydrolysis of inulin. For short chain inulin (DPn 18, s.d. 0.70) the activation energy calculated for the hydrolytic cleavage of glucose was similar to sucrose at 108.5 kJ.mol−1 (std. dev. 0.60). For long chain inulin (DPn 30, s.d. 1.3) the activation energy for the hydrolytic cleavage of glucose was reduced to 80.5 kJ.mol−1 (s.d. 2.3 kJ.mol−1). This anomaly has been attributed to varied conformations for the two different lengths of inulin chain in solution. PMID:22464225

  12. Age-dependent changes in metabolic profile of turkey spermatozoa as assessed by NMR analysis

    Science.gov (United States)

    Di Iorio, Michele; Mannina, Luisa; Paventi, Gianluca; Rosato, Maria Pina; Cerolini, Silvia; Sobolev, Anatoly P.

    2018-01-01

    Metabolic profile of fresh turkey spermatozoa at three different reproductive period ages, namely 32, 44 and 56 weeks, was monitored by Nuclear Magnetic Resonance (NMR) spectroscopy and correlated to sperm quality parameters. The age-related decrease in sperm quality as indicated by reduction of sperm concentration, sperm mobility and osmotic tolerance was associated to variation in the level of specific water-soluble and liposoluble metabolites. In particular, the highest levels of isoleucine, phenylalanine, leucine, tyrosine and valine were found at 32 weeks of age, whereas aspartate, lactate, creatine, carnitine, acetylcarnitine levels increased during the ageing. Lipid composition also changed during the ageing: diunsaturated fatty acids level increased from 32 to 56 weeks of age, whereas a reduction of polyunsaturated fatty acids content was observed at 56 weeks. The untargeted approach attempts to give a wider picture of metabolic changes occurring in ageing suggesting that the reduction of sperm quality could be due to a progressive deficiency in mitochondrial energy producing systems, as also prompted by the negative correlation found between sperm mobility and the increase in certain mitochondrial metabolites. PMID:29534088

  13. Stereochemical analysis of (+)-limonene using theoretical and experimental NMR and chiroptical data

    Science.gov (United States)

    Reinscheid, F.; Reinscheid, U. M.

    2016-02-01

    Using limonene as test molecule, the success and the limitations of three chiroptical methods (optical rotatory dispersion (ORD), electronic and vibrational circular dichroism, ECD and VCD) could be demonstrated. At quite low levels of theory (mpw1pw91/cc-pvdz, IEFPCM (integral equation formalism polarizable continuum model)) the experimental ORD values differ by less than 10 units from the calculated values. The modelling in the condensed phase still represents a challenge so that experimental NMR data were used to test for aggregation and solvent-solute interactions. After establishing a reasonable structural model, only the ECD spectra prediction showed a decisive dependence on the basis set: only augmented (in the case of Dunning's basis sets) or diffuse (in the case of Pople's basis sets) basis sets predicted the position and shape of the ECD bands correctly. Based on these result we propose a procedure to assign the absolute configuration (AC) of an unknown compound using the comparison between experimental and calculated chiroptical data.

  14. Animal manure phosphorus characterization by sequential chemical fractionation, release kinetics and 31P-NMR analysis

    Directory of Open Access Journals (Sweden)

    Tales Tiecher

    2014-10-01

    Full Text Available Phosphate release kinetics from manures are of global interest because sustainable plant nutrition with phosphate will be a major concern in the future. Although information on the bioavailability and chemical composition of P present in manure used as fertilizer are important to understand its dynamics in the soil, such studies are still scarce. Therefore, P extraction was evaluated in this study by sequential chemical fractionation, desorption with anion-cation exchange resin and 31P nuclear magnetic resonance (31P-NMR spectroscopy to assess the P forms in three different dry manure types (i.e. poultry, cattle and swine manure. All three methods showed that the P forms in poultry, cattle and swine dry manures are mostly inorganic and highly bioavailable. The estimated P pools showed that organic and recalcitrant P forms were negligible and highly dependent on the Ca:P ratio in manures. The results obtained here showed that the extraction of P with these three different methods allows a better understanding and complete characterization of the P pools present in the manures.

  15. Interactions of ionic liquids and acetone: thermodynamic properties, quantum-chemical calculations, and NMR analysis.

    Science.gov (United States)

    Ruiz, Elia; Ferro, Victor R; Palomar, Jose; Ortega, Juan; Rodriguez, Juan Jose

    2013-06-20

    The interactions between ionic liquids (ILs) and acetone have been studied to obtain a further understanding of the behavior of their mixtures, which generally give place to an exothermic process, mutual miscibility, and negative deviation of Raoult's law. COSMO-RS was used as a suitable computational method to systematically analyze the excess enthalpy of IL-acetone systems (>300), in terms of the intermolecular interactions contributing to the mixture behavior. Spectroscopic and COSMO-RS results indicated that acetone, as a polar compound with strong hydrogen bond acceptor character, in most cases, establishes favorable hydrogen bonding with ILs. This interaction is strengthened by the presence of an acidic cation and an anion with dispersed charge and non-HB acceptor character in the IL. COSMO-RS predictions indicated that gas-liquid and vapor-liquid equilibrium data for IL-acetone systems can be finely tuned by the IL selection, that is, acting on the intermolecular interactions between the molecular and ionic species in the liquid phase. NMR measurements for IL-acetone mixtures at different concentrations were also carried out. Quantum-chemical calculations by using molecular clusters of acetone and IL species were finally performed. These results provided additional evidence of the main role played by hydrogen bonding in the behavior of systems containing ILs and HB acceptor compounds, such as acetone.

  16. On low-dimensional models at NMR line shape analysis in nanomaterial systems

    Science.gov (United States)

    Kucherov, M. M.; Falaleev, O. V.

    2018-03-01

    We present a model of localized spin dynamics at room temperature for the low-dimensional solid-state spin system, which contains small ensembles of magnetic nuclei (N ~ 40). The standard spin Hamiltonian (XXZ model) is the sum of the Zeeman term in a strong external magnetic field and the magnetic dipole interaction secular term. The 19F spins in a single crystal of fluorapatite [Ca5(PO4)3F] have often been used to approximate a one-dimensional spin system. If the constant external field is parallel to the c axis, the 3D 19F system may be treated as a collection of many identical spin chains. When considering the longitudinal part of the secular term, we suggest that transverse component of a spin in a certain site rotates in a constant local magnetic field. This field changes if the spin jumps to another site. On return, this spin continues to rotate in the former field. Then we expand the density matrix in a set of eigenoperators of the Zeeman Hamiltonian. A system of coupled differential equations for the expansion coefficients then solved by straightforward numerical methods, and the fluorine NMR line shapes of fluorapatite for different chain lengths are calculated.

  17. Identification of heparin samples that contain impurities or contaminants by chemometric pattern recognition analysis of proton NMR spectral data

    Energy Technology Data Exchange (ETDEWEB)

    Zang, Qingda [University of Medicine and Dentistry of New Jersey, Department of Pharmacology, Robert Wood Johnson Medical School, Piscataway, NJ (United States); Snowdon, Inc., Monmouth Junction, NJ (United States); University of Medicine and Dentistry of New Jersey, Department of Health Informatics, School of Health Related Professions, Newark, NJ (United States); Keire, David A.; Buhse, Lucinda F.; Trehy, Michael L. [Food and Drug Administration, CDER, Division of Pharmaceutical Analysis, St. Louis, MO (United States); Wood, Richard D. [Snowdon, Inc., Monmouth Junction, NJ (United States); Mital, Dinesh P.; Haque, Syed; Srinivasan, Shankar [University of Medicine and Dentistry of New Jersey, Department of Health Informatics, School of Health Related Professions, Newark, NJ (United States); Moore, Christine M.V.; Nasr, Moheb; Al-Hakim, Ali [Food and Drug Administration, CDER, Office of New Drug Quality Assessment, Silver Spring, MD (United States); Welsh, William J. [University of Medicine and Dentistry of New Jersey, Department of Pharmacology, Robert Wood Johnson Medical School, Piscataway, NJ (United States)

    2011-08-15

    Chemometric analysis of a set of one-dimensional (1D) {sup 1}H nuclear magnetic resonance (NMR) spectral data for heparin sodium active pharmaceutical ingredient (API) samples was employed to distinguish USP-grade heparin samples from those containing oversulfated chondroitin sulfate (OSCS) contaminant and/or unacceptable levels of dermatan sulfate (DS) impurity. Three chemometric pattern recognition approaches were implemented: classification and regression tree (CART), artificial neural network (ANN), and support vector machine (SVM). Heparin sodium samples from various manufacturers were analyzed in 2008 and 2009 by 1D {sup 1}H NMR, strong anion-exchange high-performance liquid chromatography, and percent galactosamine in total hexosamine tests. Based on these data, the samples were divided into three groups: Heparin, DS {<=} 1.0% and OSCS = 0%; DS, DS > 1.0% and OSCS = 0%; and OSCS, OSCS > 0% with any content of DS. Three data sets corresponding to different chemical shift regions (1.95-2.20, 3.10-5.70, and 1.95-5.70 ppm) were evaluated. While all three chemometric approaches were able to effectively model the data in the 1.95-2.20 ppm region, SVM was found to substantially outperform CART and ANN for data in the 3.10-5.70 ppm region in terms of classification success rate. A 100% prediction rate was frequently achieved for discrimination between heparin and OSCS samples. The majority of classification errors between heparin and DS involved cases where the DS content was close to the 1.0% DS borderline between the two classes. When these borderline samples were removed, nearly perfect classification results were attained. Satisfactory results were achieved when the resulting models were challenged by test samples containing blends of heparin APIs spiked with non-, partially, or fully oversulfated chondroitin sulfate A, heparan sulfate, or DS at the 1.0%, 5.0%, and 10.0% (w/w) levels. This study demonstrated that the combination of 1D {sup 1}H NMR spectroscopy

  18. Sensitivity of 1H NMR analysis of rat urine in relation to toxicometabonomics. Part I: Dose-dependent toxic fffects of Bromobenzene and paracetamol

    NARCIS (Netherlands)

    Schoonen, W.G.E.J.; Kloks, C.P.A.M.; Ploemen, J.P.H.T.M.; Horbach, G.J.; Smit, M.J.; Zandberg, P.; Mellema, J.R.; Zuylen, C.T. van; Tas, A.C.; Nesselrooij, J.H.J. van; Vogels, J.T.W.E.

    2007-01-01

    1H nuclear magnetic resonance (NMR) spectroscopy of rat urine in combination with pattern recognition analysis was evaluated for early noninvasive detection of toxicity of investigational chemical entities. Bromobenzene (B) and paracetamol (P) were administered at five single oral dosages between 2

  19. 1H NMR-Based Metabolomic Analysis of Sub-Lethal Perfluorooctane Sulfonate Exposure to the Earthworm, Eisenia fetida, in Soil

    Directory of Open Access Journals (Sweden)

    Myrna J. Simpson

    2013-08-01

    Full Text Available 1H NMR-based metabolomics was used to measure the response of Eisenia fetida earthworms after exposure to sub-lethal concentrations of perfluorooctane sulfonate (PFOS in soil. Earthworms were exposed to a range of PFOS concentrations (five, 10, 25, 50, 100 or 150 mg/kg for two, seven and fourteen days. Earthworm tissues were extracted and analyzed by 1H NMR. Multivariate statistical analysis of the metabolic response of E. fetida to PFOS exposure identified time-dependent responses that were comprised of two separate modes of action: a non-polar narcosis type mechanism after two days of exposure and increased fatty acid oxidation after seven and fourteen days of exposure. Univariate statistical analysis revealed that 2-hexyl-5-ethyl-3-furansulfonate (HEFS, betaine, leucine, arginine, glutamate, maltose and ATP are potential indicators of PFOS exposure, as the concentrations of these metabolites fluctuated significantly. Overall, NMR-based metabolomic analysis suggests elevated fatty acid oxidation, disruption in energy metabolism and biological membrane structure and a possible interruption of ATP synthesis. These conclusions obtained from analysis of the metabolic profile in response to sub-lethal PFOS exposure indicates that NMR-based metabolomics is an excellent discovery tool when the mode of action (MOA of contaminants is not clearly defined.

  20. NMR spectroscopy

    International Nuclear Information System (INIS)

    Gruenert, J.

    1989-01-01

    The book reviews the applications of NMR-spectroscopy in medicine and biology. The first chapter of about 40 pages summarizes the history of development and explains the chemical and physical fundamentals of this new and non-invasive method in an easily comprehensible manner. The other chapters summarize diagnostic results obtained with this method in organs and tissues, so that the reader will find a systematic overview of the available findings obtained in the various organ systems. It must be noted, however, that ongoing research work and new insight quite naturally will necessitate corrections to be done, as is the case here with some biochemical interpretations which would need adjustment to latest research results. NMR-spectroscopy is able to measure very fine energy differences on the molecular level, and thus offers insight into metabolic processes, with the advantage that there is no need of applying ionizing radiation in order to qualitatively or quantitatively analyse the metabolic processes in the various organ systems. (orig./DG) With 40 figs., 4 tabs [de

  1. Analysis of exergy loss of gasoline surrogate combustion process based on detailed chemical kinetics

    International Nuclear Information System (INIS)

    Sun, Hongjie; Yan, Feng; Yu, Hao; Su, W.H.

    2015-01-01

    Highlights: • We explored the exergy loss sources of gasoline engine like combustion process. • The model combined non-equilibrium thermodynamics with detailed chemical kinetics. • We explored effects of initial conditions on exergy loss of combustion process. • Exergy loss decreases 15% of fuel chemical exergy by design of initial conditions. • Correspondingly, the second law efficiency increases from 38.9% to 68.9%. - Abstract: Chemical reaction is the most important source of combustion irreversibility in premixed conditions, but details of the exergy loss mechanisms have not been explored yet. In this study numerical analysis based on non-equilibrium thermodynamics combined with detailed chemical kinetics is conducted to explore the exergy loss mechanism of gasoline engine like combustion process which is simplified as constant volume combustion. The fuel is represented by the common accepted gasoline surrogates which consist of four components: iso-octane (57%), n-heptane (16%), toluene (23%), and 2-pentene (4%). We find that overall exergy loss is mainly composed of three peaks along combustion generated from chemical reactions in three stages, the conversion from large fuel molecules into small molecules (as Stage 1), the H 2 O 2 loop-related reactions (as Stage 2), and the violent oxidation reactions of CO, H, and O (as Stage 3). The effects of individual combustion boundaries, including temperature, pressure, equivalence ratio, oxygen concentration, on combustion exergy loss have been widely investigated. The combined effects of combustion boundaries on the total loss of gasoline surrogates are also investigated. We find that in a gasoline engine with a compression ratio of 10, the total loss can be reduced from 31.3% to 24.3% using lean combustion. The total loss can be further reduced to 22.4% by introducing exhaust gas recirculation and boosting the inlet charge. If the compression ratio is increased to 17, the total loss can be decreased to

  2. Detailed analysis of evolution of the state of polarization in all-fiber polarization transformers.

    Science.gov (United States)

    Zhu, Xiushan; Jain, Ravinder K

    2006-10-30

    We present a detailed analysis of key attributes and performance characteristics of controllably-spun birefringent-fiber-based all-fiber waveplates or "all fiber polarization transformers" (AFPTs), first proposed and demonstrated by Huang [11]; these AFPTs consist essentially of a long carefully-designed "spin-twisted" high-birefringence fiber, fabricated by slowly varying the spin rate of a birefringent fiber preform (either from very fast to very slow or vice versa) while the fiber is being drawn. The evolution of the eigenstate from a linear polarization state to a circular polarization state, induced by slow variation of the intrinsic structure from linear anisotropy at the unspun end to circular anisotropy at the fast-spun end, enables the AFPT to behave like an all-fiber quarter-wave plate independent of the wavelength of operation. Power coupling between local eigenstates causes unique evolution of the polarization state along the fiber, and has been studied to gain insight into - as well as to understand detailed characteristics of -- the polarization transformation behavior. This has been graphically illustrated via plots of the relative power in these local eigenstates as a function of distance along the length of the fiber and plots of the extinction ratio of the output state of polarization (SOP) as a function of distance and the normalized spin rate. Deeper understanding of such polarization transformers has been further elucidated by quantitative calculations related to two crucial requirements for fabricating practical AFPT devices. Our calculations have also indicated that the polarization mode dispersion behaviour of the AFPT is much smaller than that of the original birefringent fiber. Finally, a specific AFPT was experimentally investigated at two widely-separated wavelengths (1310 nm and 1550 nm) of interest in telecommunications systems applications, further demonstrating and elucidating the broadband character of such AFPTs.

  3. Quantitative Quantum Mechanical Spectral Analysis (qQMSA) of (1)H NMR spectra of complex mixtures and biofluids.

    Science.gov (United States)

    Tiainen, Mika; Soininen, Pasi; Laatikainen, Reino

    2014-05-01

    The quantitative interpretation of (1)H NMR spectra of mixtures like the biofluids is a demanding task due to spectral complexity and overlap. Complications may arise also from water suppression, T2-editing, protein interactions, relaxation differences of the species, experimental artifacts and, furthermore, the spectra may contain unknown components and macromolecular background which cannot be easily separated from baseline. In this work, tools and strategies for quantitative Quantum Mechanical Spectral Analysis (qQMSA) of (1)H NMR spectra from complex mixtures were developed and systematically assessed. In the present approach, the signals of well-defined, stoichiometric components are described by a QM model, while the background is described by a multiterm baseline function and the unknown signals using optimizable and adjustable lines, regular multiplets or any spectral structures which can be composed from spectral lines. Any prior knowledge available from the spectrum can also be added to the model. Fitting strategies for weak and strongly overlapping spectral systems were developed and assessed using two basic model systems, the metabolite mixtures without and with macromolecular (serum) background. The analyses show that if the spectra are measured in high-throughput manner, the consistent absolute quantification demands some calibration to compensate the different response factors of the protons and compounds. On the other hand, the results show that also the T2-edited spectra can be measured so that they obey well the QM rules. In general, qQMSA exploits and interprets the spectral information in maximal way taking full advantage from the QM properties of the spectra and, at the same time, offers chemical confidence which means that individual components can be identified with high confidence on the basis of their accurate spectral parameters. Copyright © 2014 Elsevier Inc. All rights reserved.

  4. Protein samples for NMR: expression and analysis without purification, and stabilization by covalent cyclization

    International Nuclear Information System (INIS)

    Otting, G.; Ozawa, K.; Prosselkov, P.; Williams, N.K.; Dixon, N.E.; Liepinsh, E.

    2002-01-01

    Full text: A modified cell-free in vitro expression system was established for the expression of milligram quantities of protein per mL reaction medium. Expression levels of the E coli cytoplasmic peptidyl-prolyl cis-trans isomerase, PpiB, in 0 6 mL reaction medium were sufficient for the direct recording of clean 15N-HSQC spectra without chromatographic purification or sample concentration steps, using a 600 MHz NMR spectrometer with cryoprobe. Besides providing a route to high-throughput sample preparation, in vitro expression systems are known to be highly economic in their utilization of selectively labelled ammo acids. Using dual-selective labelling with 15N- and 13C-labelled amino acids, the 15N-HSQC cross peaks of strategically selected ammo acids can readily be identified and monitored for their response to the presence of ligand molecules, again without sample purification. 2) The N-terminal domain of E coli DnaB is a protein of ca 110 residues with a structured core composed of 6 helices. Additional segments of 10 residues each at the N- and C-termini are highly mobile. Both ends are close in space and can be linked together in a covalent peptide bond using intern technology. The core structures of linear (lin-DnaB-N) and cyclized (cz-DnaB-N) protein are conserved, as evidenced by superimposable NOESY spectra and chemical shifts. The linker segment in cz-DnaB-N is mobile as shown by 1H-15N NOEs. Yet, the cyclic protein melts about 10 degrees higher than the linear version. A stabilization free energy of ca 2 kcal/mol is in agreement with predictions based on the reduced entropy in the unfolded state. Amide proton exchange rates are much slower in the cyclic protein and reveal cooperative exchange through total, global unfolding at a rate of once every 100 minutes in the linear protein

  5. FT-IR, FT-Raman, NMR studies and ab initio-HF, DFT-B3LYP vibrational analysis of 4-chloro-2-fluoroaniline.

    Science.gov (United States)

    Arivazhagan, M; Anitha Rexalin, D

    2012-10-01

    The Fourier transform infrared (FT-IR) and Fourier transform Raman (FT-Raman) spectra of 4-chloro-2-fluoroaniline (CFA) have been recorded and analyzed. The equilibrium geometry, bonding features and harmonic vibrational frequencies have been investigated with the help of ab initio and density functional theory (DFT) methods. The assignments of the vibrational spectra have been carried out with the help of normal coordinate analysis (NCA) following the scaled quantum mechanical force field methodology. The (1)H and (13)C nuclear magnetic resonance (NMR) chemical shifts of the molecule are calculated by the Gauge including atomic orbital (GIAO) method. The first order hyperpolarizability (β(0)) of this novel molecular system and related properties (β, α(0) and Δα) of CFA are calculated using B3LYP/6-311++G(d,p) and HF/6-311++G(d,p) methods on the finite-field approach. The calculated results also show that the CFA molecule might have microscopic nonlinear optical (NLO) behavior with non-zero values. Stability of the molecule arising from hyper conjugative interactions, charge delocalization has been analyzed using natural bond orbital (NBO) analysis. The result confirms the occurrence of intramolecular charge transfer (ICT) within the molecule. The HOMO-LUMO energies UV-vis spectral analysis and MEP are performed by B3LYP/6-311++G(d,p) approach. A detailed interpretation of the infrared and Raman spectra of CFA is also reported based on total energy distribution (TED). The difference between the observed and scaled wave number values of the most of the fundamentals is very small. Copyright © 2012 Elsevier B.V. All rights reserved.

  6. Author Details

    African Journals Online (AJOL)

    Methyl Iodide Oxidative Addition to Rhodium(I) Complexes: a DFT and NMR Study of [Rh(FcCOCHCOCF3)(CO)(PPh3)] and the Rhodium(III) Reaction Products Abstract PDF PDF · Vol 63 (2010) - Articles Characterization and Oxidative Addition Reactions of Different Rhodium and Iridium Triazolato Complexes Abstract PDF ...

  7. Fast and Efficient Fragment-Based Lead Generation by Fully Automated Processing and Analysis of Ligand-Observed NMR Binding Data.

    Science.gov (United States)

    Peng, Chen; Frommlet, Alexandra; Perez, Manuel; Cobas, Carlos; Blechschmidt, Anke; Dominguez, Santiago; Lingel, Andreas

    2016-04-14

    NMR binding assays are routinely applied in hit finding and validation during early stages of drug discovery, particularly for fragment-based lead generation. To this end, compound libraries are screened by ligand-observed NMR experiments such as STD, T1ρ, and CPMG to identify molecules interacting with a target. The analysis of a high number of complex spectra is performed largely manually and therefore represents a limiting step in hit generation campaigns. Here we report a novel integrated computational procedure that processes and analyzes ligand-observed proton and fluorine NMR binding data in a fully automated fashion. A performance evaluation comparing automated and manual analysis results on (19)F- and (1)H-detected data sets shows that the program delivers robust, high-confidence hit lists in a fraction of the time needed for manual analysis and greatly facilitates visual inspection of the associated NMR spectra. These features enable considerably higher throughput, the assessment of larger libraries, and shorter turn-around times.

  8. Polymeric proanthocyanidins 13C NMR studies of procyanidins

    Science.gov (United States)

    Lawrence J. Porter; Roger H. Newman; Lai Yeap Foo; Herbert Wong; Richard W. Hemingway

    1982-01-01

    Proanthocyanidin polymers have been shown to consist entirely of flavan-3-ol units by a combination of techniques including 13C n.m.r. spectroscopy. The 13C n.m.r. spectra of the polymers and related molecules are now considered in more detail. Prior to this study UC n.m.r. data has been published of procyanidins and...

  9. Solid-state NMR of inorganic semiconductors.

    Science.gov (United States)

    Yesinowski, James P

    2012-01-01

    Studies of inorganic semiconductors by solid-state NMR vary widely in terms of the nature of the samples investigated, the techniques employed to observe the NMR signal, and the types of information obtained. Compared with the NMR of diamagnetic non-semiconducting substances, important differences often result from the presence of electron or hole carriers that are the hallmark of semiconductors, and whose theoretical interpretation can be involved. This review aims to provide a broad perspective on the topic for the non-expert by providing: (1) a basic introduction to semiconductor physical concepts relevant to NMR, including common crystal structures and the various methods of making samples; (2) discussions of the NMR spin Hamiltonian, details of some of the NMR techniques and strategies used to make measurements and theoretically predict NMR parameters, and examples of how each of the terms in the Hamiltonian has provided useful information in bulk semiconductors; (3) a discussion of the additional considerations needed to interpret the NMR of nanoscale semiconductors, with selected examples. The area of semiconductor NMR is being revitalized by this interest in nanoscale semiconductors, the great improvements in NMR detection sensitivity and resolution that have occurred, and the current interest in optical pumping and spintronics-related studies. Promising directions for future research will be noted throughout.

  10. Detailed performance analysis of realistic solar photovoltaic systems at extensive climatic conditions

    International Nuclear Information System (INIS)

    Gupta, Ankit; Chauhan, Yogesh K.

    2016-01-01

    In recent years, solar energy has been considered as one of the principle renewable energy source for electric power generation. In this paper, single diode photovoltaic (PV) system and double/bypass diode based PV system are designed in MATLAB/Simulink environment based on their mathematical modeling and are validated with a commercially available solar panel. The novelty of the paper is to include the effect of climatic conditions i.e. variable irradiation level, wind speed, temperature, humidity level and dust accumulation in the modeling of both the PV systems to represent a realistic PV system. The comprehensive investigations are made on both the modeled PV systems. The obtained results show the satisfactory performance for realistic models of the PV system. Furthermore, an in depth comparative analysis is carried out for both PV systems. - Highlights: • Modeling of Single diode and Double diode PV systems in MATLAB/Simulink software. • Validation of designed PV systems with a commercially available PV panel. • Acquisition and employment of key climatic factors in modeling of the PV systems. • Evaluation of main model parameters of both the PV systems. • Detailed comparative assessment of both the modeled PV system parameters.

  11. The neutral kaon decays to $\\pi^+ \\pi^- \\pi^0$ a detailed analysis of the CPLEAR data

    CERN Document Server

    Angelopoulos, Angelos; Aslanides, Elie; Backenstoss, Gerhard; Bargassa, P; Behnke, O; Benelli, A; Bertin, V; Blanc, F; Bloch, P; Carlson, P J; Carroll, M; Cawley, E; Chertok, M B; Danielsson, M; Dejardin, M; Derré, J; Ealet, A; Eleftheriadis, C; Faravel, L; Fassnacht, P; Fetscher, W; Fidecaro, Maria; Filipcic, A; Francis, D; Fry, J; Gabathuler, Erwin; Gamet, R; Gerber, H J; Go, A; Haselden, A; Hayman, P J; Henry-Coüannier, F; Hollander, R W; Jon-And, K; Kettle, P R; Kokkas, P; Kreuger, R; Le Gac, R; Leimgruber, F; Mandic, I; Manthos, N; Marel, Gérard; Mikuz, M; Miller, J; Montanet, François; Nakada, Tatsuya; Pagels, B; Papadopoulos, I M; Pavlopoulos, P; Polivka, G; Rickenbach, R; Roberts, B L; Ruf, T; Schäfer, M; Schaller, L A; Schietinger, T; Schopper, A; Tauscher, Ludwig; Thibault, C; Touchard, F; Touramanis, C; van Eijk, C W E; Vlachos, S; Weber, P; Wigger, O; Wolter, M; Zavrtanik, D; Zimmerman, D

    1998-01-01

    A detailed analysis of neutral kaons decaying to \\Pgpp \\Pgpm \\Pgpz\\ is presented based on the complete data set containing half a million events. Time-dependent decay rate asymmetries are measured between initially tagged \\PKz\\ and \\PaKz\\ and for different regions of the phase space. These asymmetries, resulting from the interference between the CP-conserving decay amplitude of \\PKzL\\ and the decay amplitude of \\PKzS\\ -- either CP-violating or CP-conserving -- allow the determinationof the \\PKzS\\ parameters \\etapmz\\ (CP-violating) and \\lampmz\\ (CP-conserving), and also of the main i sospin components of the \\PKzS\\ decay amplitude. The branching ratio of \\PKzS\\ $\\rightarrow$ \\Pgpp \\Pgpm \\Pgpz\\ (CP-conserving) is deduced directly from \\lampmz . In addition, we extract the slope parameters describing the energy dependence of the $\\PKzL \\rightarrow \\Pgpp \\Pgpm \\Pgpz $ Dalitz plot. The whole set of our results fits well within the current phenomenological picture of the neut ral-kaon system including CP violation ...

  12. Analysis of Detailed Energy Audits and Energy Use Measures of University Buildings

    Directory of Open Access Journals (Sweden)

    Kęstutis Valančius

    2011-12-01

    Full Text Available The paper explains the results of a detailed energy audit of the buildings of Vilnius Gediminas Technical University. Energy audits were performed with reference to the international scientific project. The article presents the methodology and results of detailed measurements of energy balance characteristics.Article in Lithuanian

  13. Systematic NMR Analysis of Stable Isotope Labeled Metabolite Mixtures in Plant and Animal Systems: Coarse Grained Views of Metabolic Pathways

    Science.gov (United States)

    Chikayama, Eisuke; Suto, Michitaka; Nishihara, Takashi; Shinozaki, Kazuo; Hirayama, Takashi; Kikuchi, Jun

    2008-01-01

    Background Metabolic phenotyping has become an important ‘bird's-eye-view’ technology which can be applied to higher organisms, such as model plant and animal systems in the post-genomics and proteomics era. Although genotyping technology has expanded greatly over the past decade, metabolic phenotyping has languished due to the difficulty of ‘top-down’ chemical analyses. Here, we describe a systematic NMR methodology for stable isotope-labeling and analysis of metabolite mixtures in plant and animal systems. Methodology/Principal Findings The analysis method includes a stable isotope labeling technique for use in living organisms; a systematic method for simultaneously identifying a large number of metabolites by using a newly developed HSQC-based metabolite chemical shift database combined with heteronuclear multidimensional NMR spectroscopy; Principal Components Analysis; and a visualization method using a coarse-grained overview of the metabolic system. The database contains more than 1000 1H and 13C chemical shifts corresponding to 142 metabolites measured under identical physicochemical conditions. Using the stable isotope labeling technique in Arabidopsis T87 cultured cells and Bombyx mori, we systematically detected >450 HSQC peaks in each 13C-HSQC spectrum derived from model plant, Arabidopsis T87 cultured cells and the invertebrate animal model Bombyx mori. Furthermore, for the first time, efficient 13C labeling has allowed reliable signal assignment using analytical separation techniques such as 3D HCCH-COSY spectra in higher organism extracts. Conclusions/Significance Overall physiological changes could be detected and categorized in relation to a critical developmental phase change in B. mori by coarse-grained representations in which the organization of metabolic pathways related to a specific developmental phase was visualized on the basis of constituent changes of 56 identified metabolites. Based on the observed intensities of 13C atoms of

  14. Detailed analysis of latencies in image-based dynamic MLC tracking

    International Nuclear Information System (INIS)

    Poulsen, Per Rugaard; Cho, Byungchul; Sawant, Amit; Ruan, Dan; Keall, Paul J.

    2010-01-01

    Purpose: Previous measurements of the accuracy of image-based real-time dynamic multileaf collimator (DMLC) tracking show that the major contributor to errors is latency, i.e., the delay between target motion and MLC response. Therefore the purpose of this work was to develop a method for detailed analysis of latency contributions during image-based DMLC tracking. Methods: A prototype DMLC tracking system integrated with a linear accelerator was used for tracking a phantom with an embedded fiducial marker during treatment delivery. The phantom performed a sinusoidal motion. Real-time target localization was based on x-ray images acquired either with a portal imager or a kV imager mounted orthogonal to the treatment beam. Each image was stored in a file on the imaging workstation. A marker segmentation program opened the image file, determined the marker position in the image, and transferred it to the DMLC tracking program. This program estimated the three-dimensional target position by a single-imager method and adjusted the MLC aperture to the target position. Imaging intervals ΔT image from 150 to 1000 ms were investigated for both kV and MV imaging. After the experiments, the recorded images were synchronized with MLC log files generated by the MLC controller and tracking log files generated by the tracking program. This synchronization allowed temporal analysis of the information flow for each individual image from acquisition to completed MLC adjustment. The synchronization also allowed investigation of the MLC adjustment dynamics on a considerably finer time scale than the 50 ms time resolution of the MLC log files. Results: For ΔT image =150 ms, the total time from image acquisition to completed MLC adjustment was 380±9 ms for MV and 420±12 ms for kV images. The main part of this time was from image acquisition to completed image file writing (272 ms for MV and 309 ms for kV). Image file opening (38 ms), marker segmentation (4 ms), MLC position

  15. Detailed analysis of latencies in image-based dynamic MLC tracking

    Energy Technology Data Exchange (ETDEWEB)

    Poulsen, Per Rugaard; Cho, Byungchul; Sawant, Amit; Ruan, Dan; Keall, Paul J. [Department of Radiation Oncology, Stanford University, Stanford, California 94305 and Department of Oncology and Department of Medical Physics, Aarhus University Hospital, 8000 Aarhus (Denmark); Department of Radiation Oncology, Stanford University, Stanford, California 94305 and Department of Radiation Oncology, Asan Medical Center, Seoul 138-736 (Korea, Republic of); Department of Radiation Oncology, Stanford University, Stanford, California 94305 (United States)

    2010-09-15

    Purpose: Previous measurements of the accuracy of image-based real-time dynamic multileaf collimator (DMLC) tracking show that the major contributor to errors is latency, i.e., the delay between target motion and MLC response. Therefore the purpose of this work was to develop a method for detailed analysis of latency contributions during image-based DMLC tracking. Methods: A prototype DMLC tracking system integrated with a linear accelerator was used for tracking a phantom with an embedded fiducial marker during treatment delivery. The phantom performed a sinusoidal motion. Real-time target localization was based on x-ray images acquired either with a portal imager or a kV imager mounted orthogonal to the treatment beam. Each image was stored in a file on the imaging workstation. A marker segmentation program opened the image file, determined the marker position in the image, and transferred it to the DMLC tracking program. This program estimated the three-dimensional target position by a single-imager method and adjusted the MLC aperture to the target position. Imaging intervals {Delta}T{sub image} from 150 to 1000 ms were investigated for both kV and MV imaging. After the experiments, the recorded images were synchronized with MLC log files generated by the MLC controller and tracking log files generated by the tracking program. This synchronization allowed temporal analysis of the information flow for each individual image from acquisition to completed MLC adjustment. The synchronization also allowed investigation of the MLC adjustment dynamics on a considerably finer time scale than the 50 ms time resolution of the MLC log files. Results: For {Delta}T{sub image}=150 ms, the total time from image acquisition to completed MLC adjustment was 380{+-}9 ms for MV and 420{+-}12 ms for kV images. The main part of this time was from image acquisition to completed image file writing (272 ms for MV and 309 ms for kV). Image file opening (38 ms), marker segmentation (4 ms

  16. Comparison between the efficacy of two cleanup methods for the 1H NMR analysis of food samples contaminated with Cypermethrin

    International Nuclear Information System (INIS)

    Silva, M.M.; Figueroa-Villar, J.D.; Aguiar, A.P.; Riehl, C.A.S.

    2004-01-01

    This work aimed to study the use of 1 H NMR for the identification of cypermethrin in cooked foods. 1 H NMR is not commonly used in these cases, because food samples ready for consumption have complex substances, mainly lipids, which usually interfere with the identification of cypermethrin. Thus, we drew a comparison between the most applied method for the treatment of those samples and an alternative route that made possible the use of 1 H NMR in the identification of cypermethrin in a matrix consisting of rice, bean, and chicken, which allows the Forensic work for such cases.(author)

  17. Permeability in Rotliegend gas sandstones to gas and brine as predicted from NMR, mercury injection and image analysis

    DEFF Research Database (Denmark)

    Rosenbrand, Esther; Fabricius, Ida Lykke; Fisher, Quentin

    2015-01-01

    Permeability characterisation of low permeability, clay-rich gas sandstones is part of production forecasting and reservoir management. The physically based Kozeny (1927) equation linking permeability with porosity and pore size is derived for a porous medium with a homogeneous pore size, whereas...... the pore sizes in tight sandstones can range from nm to μm. Nuclear magnetic resonance (NMR) transverse relaxation was used to estimate a pore size distribution for 63 samples of Rotliegend sandstone. The surface relaxation parameter required to relate NMR to pore size is estimated by combination of NMR...

  18. Basics of spectroscopic instruments. Hardware of NMR spectrometer

    International Nuclear Information System (INIS)

    Sato, Hajime

    2009-01-01

    NMR is a powerful tool for structure analysis of small molecules, natural products, biological macromolecules, synthesized polymers, samples from material science and so on. Magnetic Resonance Imaging (MRI) is applicable to plants and animals Because most of NMR experiments can be done by an automation mode, one can forget hardware of NMR spectrometers. It would be good to understand features and performance of NMR spectrometers. Here I present hardware of a modern NMR spectrometer which is fully equipped with digital technology. (author)

  19. Petrophysical properties of greensand as predicted from NMR measurements

    DEFF Research Database (Denmark)

    Hossain, Zakir; Grattoni, Carlos A.; Solymar, Mikael

    2011-01-01

    ABSTRACT: Nuclear magnetic resonance (NMR) is a useful tool in reservoir evaluation. The objective of this study is to predict petrophysical properties from NMR T2 distributions. A series of laboratory experiments including core analysis, capillary pressure measurements, NMR T2 measurements...... with macro-pores. Permeability may be predicted from NMR by using Kozeny's equation when surface relaxivity is known. Capillary pressure drainage curves may be predicted from NMR T2 distribution when pore size distribution within a sample is homogeneous....

  20. CRAFT (complete reduction to amplitude frequency table)--robust and time-efficient Bayesian approach for quantitative mixture analysis by NMR.

    Science.gov (United States)

    Krishnamurthy, Krish

    2013-12-01

    The intrinsic quantitative nature of NMR is increasingly exploited in areas ranging from complex mixture analysis (as in metabolomics and reaction monitoring) to quality assurance/control. Complex NMR spectra are more common than not, and therefore, extraction of quantitative information generally involves significant prior knowledge and/or operator interaction to characterize resonances of interest. Moreover, in most NMR-based metabolomic experiments, the signals from metabolites are normally present as a mixture of overlapping resonances, making quantification difficult. Time-domain Bayesian approaches have been reported to be better than conventional frequency-domain analysis at identifying subtle changes in signal amplitude. We discuss an approach that exploits Bayesian analysis to achieve a complete reduction to amplitude frequency table (CRAFT) in an automated and time-efficient fashion - thus converting the time-domain FID to a frequency-amplitude table. CRAFT uses a two-step approach to FID analysis. First, the FID is digitally filtered and downsampled to several sub FIDs, and secondly, these sub FIDs are then modeled as sums of decaying sinusoids using the Bayesian approach. CRAFT tables can be used for further data mining of quantitative information using fingerprint chemical shifts of compounds of interest and/or statistical analysis of modulation of chemical quantity in a biological study (metabolomics) or process study (reaction monitoring) or quality assurance/control. The basic principles behind this approach as well as results to evaluate the effectiveness of this approach in mixture analysis are presented. Copyright © 2013 John Wiley & Sons, Ltd.

  1. A Model for the Detailed Analysis of Radio Links Involving Tree Canopies

    Directory of Open Access Journals (Sweden)

    F. Perez-Fontan

    2016-12-01

    Full Text Available Detailed analysis of tree canopy interaction with incident radiowaves has mainly been limited to remote sensing for the purpose of forest classification among many other applications. This represents a monostatic configuration, unlike the case of communication links, which are bistatic. In general, link analyses have been limited to the application of simple, empirical formulas based on the use of specific attenuation values in dB/m and the traversed vegetated mass as, e.g., the model in Recommendation ITU-R P.833-8 [1]. In remote sensing, two main techniques are used: Multiple Scattering Theory (MST [2][5] and Radiative Transfer Theory (RT, [5] and [6]. We have paid attention in the past to MST [7][10]. It was shown that a full application of MST leads to very long computation times which are unacceptable in the case where we have to analyze a scenario with several trees. Extensive work using MST has been also presented by others in [11][16] showing the interest in this technique. We have proposed a simplified model for scattering from tree canopies based on a hybridization of MST and a modified physical optics (PO approach [16]. We assume that propagation through a canopy is accounted for by using the complex valued propagation constant obtained by MST. Unlike the case when the full MST is applied, the proposed approach offers significant benefits including a direct software implementation and acceptable computation times even for high frequencies and electrically large canopies. The proposed model thus replaces the coherent component in MST, significant in the forward direction, but keeps the incoherent or diffuse scattering component present in all directions. The incoherent component can be calculated within reasonable times. Here, we present tests of the proposed model against MST using an artificial single-tree scenario at 2 GHz and 10 GHz.

  2. Propagating Disturbances in Coronal Loops: A Detailed Analysis of Propagation Speeds

    Science.gov (United States)

    Kiddie, G.; De Moortel, I.; Del Zanna, G.; McIntosh, S. W.; Whittaker, I.

    2012-08-01

    Quasi-periodic disturbances have been observed in the outer solar atmosphere for many years. Although first interpreted as upflows (Schrijver et al., Solar Phys. 187, 261, 1999), they have been widely regarded as slow magneto-acoustic waves, due to their observed velocities and periods. However, recent observations have questioned this interpretation, as periodic disturbances in Doppler velocity, line width, and profile asymmetry were found to be in phase with the intensity oscillations (De Pontieu and McIntosh, Astrophys. J. 722, 1013, 2010; Tian, McIntosh, and De Pontieu, Astrophys. J. Lett. 727, L37, 2011), suggesting that the disturbances could be quasi-periodic upflows. Here we conduct a detailed analysis of the velocities of these disturbances across several wavelengths using the Atmospheric Imaging Assembly (AIA) onboard the Solar Dynamics Observatory (SDO). We analysed 41 examples, including both sunspot and non-sunspot regions of the Sun. We found that the velocities of propagating disturbances (PDs) located at sunspots are more likely to be temperature dependent, whereas the velocities of PDs at non-sunspot locations do not show a clear temperature dependence. This suggests an interpretation in terms of slow magneto-acoustic waves in sunspots but the nature of PDs in non-sunspot (plage) regions remains unclear. We also considered on what scale the underlying driver is affecting the properties of the PDs. Finally, we found that removing the contribution due to the cooler ions in the 193 Å wavelength suggests that a substantial part of the 193 Å emission of sunspot PDs can be attributed to the cool component of 193 Å.

  3. Cardiometabolic risk in Canada: a detailed analysis and position paper by the cardiometabolic risk working group.

    Science.gov (United States)

    Leiter, Lawrence A; Fitchett, David H; Gilbert, Richard E; Gupta, Milan; Mancini, G B John; McFarlane, Philip A; Ross, Robert; Teoh, Hwee; Verma, Subodh; Anand, Sonia; Camelon, Kathryn; Chow, Chi-Ming; Cox, Jafna L; Després, Jean-Pierre; Genest, Jacques; Harris, Stewart B; Lau, David C W; Lewanczuk, Richard; Liu, Peter P; Lonn, Eva M; McPherson, Ruth; Poirier, Paul; Qaadri, Shafiq; Rabasa-Lhoret, Rémi; Rabkin, Simon W; Sharma, Arya M; Steele, Andrew W; Stone, James A; Tardif, Jean-Claude; Tobe, Sheldon; Ur, Ehud

    2011-01-01

    The concepts of "cardiometabolic risk," "metabolic syndrome," and "risk stratification" overlap and relate to the atherogenic process and development of type 2 diabetes. There is confusion about what these terms mean and how they can best be used to improve our understanding of cardiovascular disease treatment and prevention. With the objectives of clarifying these concepts and presenting practical strategies to identify and reduce cardiovascular risk in multiethnic patient populations, the Cardiometabolic Working Group reviewed the evidence related to emerging cardiovascular risk factors and Canadian guideline recommendations in order to present a detailed analysis and consolidated approach to the identification and management of cardiometabolic risk. The concepts related to cardiometabolic risk, pathophysiology, and strategies for identification and management (including health behaviours, pharmacotherapy, and surgery) in the multiethnic Canadian population are presented. "Global cardiometabolic risk" is proposed as an umbrella term for a comprehensive list of existing and emerging factors that predict cardiovascular disease and/or type 2 diabetes. Health behaviour interventions (weight loss, physical activity, diet, smoking cessation) in people identified at high cardiometabolic risk are of critical importance given the emerging crisis of obesity and the consequent epidemic of type 2 diabetes. Vascular protective measures (health behaviours for all patients and pharmacotherapy in appropriate patients) are essential to reduce cardiometabolic risk, and there is growing consensus that a multidisciplinary approach is needed to adequately address cardiometabolic risk factors. Health care professionals must also consider risk factors related to ethnicity in order to appropriately evaluate everyone in their diverse patient populations. Copyright © 2011 Elsevier Inc. All rights reserved.

  4. Morphological features and associated anomalies of schizencephaly in the clinical population: detailed analysis of MR images

    International Nuclear Information System (INIS)

    Hayashi, N.; Tsutsumi, Y.; Barkovich, A.J.

    2002-01-01

    Although they are well documented in autopsy series, the macroscopic features and associated anomalies of schizencephalies have not been described in detail in a large clinical population. To assess the macroscopic findings of schizencephaly and the prevalence of associated findings, we conducted a retrospective MR analysis of a group of patients with schizencephaly. The MR studies of 35 patients with schizencephaly were retrospectively reviewed. The images were examined for the location and size of the schizencephalic cleft, the presence and location of associated polymicrogyria, and the presence, location, and severity of other brain anomalies. A total of 54 schizencephalic clefts were seen in the 35 patients. These clefts were unilateral in 18 (51%) patients and bilateral in 17 (49%) patients; three clefts were identified in two patients. Nine clefts (17%) had fused lips and 45 had separated-lip clefts (83%). Polymicrogyria was present inside 23 clefts (43%), while subependymal heterotopias were present at the cleft orifice in 27 clefts (50%). Polymicrogyria was identified outside the cleft, both adjacent to and remote from the cleft, in 23 patients (66%). Abnormal cerebral white-matter signal intensity was present in seven patients (20%), while white-matter volume diminution was noted in all patients. Ventricular diverticula with mass effect, roofing membranes, remnant floors, and cord-like remnants were present in 12, 1, 11, and 3 patients, respectively. Our results show that the spectrum of macroscopic findings in schizencephaly includes fused-lip and separated-lip clefts, polymicrogyric and non-polymicrogyric cleft linings, cyst-like diverticula and membranous structures, and subependymal heterotopia at the cleft. Concomitant anomalies are polymicrogyria outside the cleft, white-matter diminution, septal and optic pathway anomalies, callosal anomalies and hippocampal anomalies. Unilateral and bilateral clefts occur in a nearly equal frequency in the clinical

  5. Analysis of magnetic-dipole transitions in tungsten plasmas using detailed and configuration-average descriptions

    Science.gov (United States)

    Na, Xieyu; Poirier, Michel

    2017-06-01

    This paper is devoted to the analysis of transition arrays of magnetic-dipole (M1) type in highly charged ions. Such transitions play a significant role in highly ionized plasmas, for instance in the tungsten plasma present in tokamak devices. Using formulas recently published and their implementation in the Flexible Atomic Code for M1-transition array shifts and widths, absorption and emission spectra arising from transitions inside the 3*n complex of highly-charged tungsten ions are analyzed. A comparison of magnetic-dipole transitions with electric-dipole (E1) transitions shows that, while the latter are better described by transition array formulas, M1 absorption and emission structures reveal some insufficiency of these formulas. It is demonstrated that the detailed spectra account for significantly richer structures than those predicted by the transition array formalism. This is due to the fact that M1 transitions may occur between levels inside the same relativistic configuration, while such inner configuration transitions are not accounted for by the currently available averaging expression. In addition, because of configuration interaction, transition processes involving more than one electron jump, such as 3p1/23d5/2 → 3p3/23d3/2, are possible but not accounted for in the transition array formulas. These missing transitions are collected in pseudo-arrays using a post-processing method described in this paper. The relative influence of inner- and inter-configuration transitions is carefully analyzed in cases of tungsten ions with net charge around 50. The need for an additional theoretical development is emphasized.

  6. Detailed puncture analyses tank cars : analysis of different impactor threats and impact conditions.

    Science.gov (United States)

    2013-03-01

    There has been significant research in recent years to analyze and improve the impact behavior and puncture resistance of railroad tank cars. Much of this research has been performed using detailed nonlinear finite element analyses supported by full ...

  7. Combining NMR and small angle X-ray and neutron scattering in the structural analysis of a ternary protein-RNA complex

    International Nuclear Information System (INIS)

    Hennig, Janosch; Wang, Iren; Sonntag, Miriam; Gabel, Frank; Sattler, Michael

    2013-01-01

    Many processes in the regulation of gene expression and signaling involve the formation of protein complexes involving multi-domain proteins. Individual domains that mediate protein-protein and protein-nucleic acid interactions are typically connected by flexible linkers, which contribute to conformational dynamics and enable the formation of complexes with distinct binding partners. Solution techniques are therefore required for structural analysis and to characterize potential conformational dynamics. Nuclear magnetic resonance spectroscopy (NMR) provides such information but often only sparse data are obtained with increasing molecular weight of the complexes. It is therefore beneficial to combine NMR data with additional structural restraints from complementary solution techniques. Small angle X-ray/neutron scattering (SAXS/SANS) data can be efficiently combined with NMR-derived information, either for validation or by providing additional restraints for structural analysis. Here, we show that the combination of SAXS and SANS data can help to refine structural models obtained from data-driven docking using HADDOCK based on sparse NMR data. The approach is demonstrated with the ternary protein-protein-RNA complex involving two RNA recognition motif (RRM) domains of Sex-lethal, the N-terminal cold shock domain of Upstream-to-N-Ras, and msl-2 mRNA. Based on chemical shift perturbations we have mapped protein-protein and protein-RNA interfaces and complemented this NMR-derived information with SAXS data, as well as SANS measurements on subunit-selectively deuterated samples of the ternary complex. Our results show that, while the use of SAXS data is beneficial, the additional combination with contrast variation in SANS data resolves remaining ambiguities and improves the docking based on chemical shift perturbations of the ternary protein-RNA complex.

  8. Combining NMR and small angle X-ray and neutron scattering in the structural analysis of a ternary protein-RNA complex

    Energy Technology Data Exchange (ETDEWEB)

    Hennig, Janosch; Wang, Iren; Sonntag, Miriam [Institute of Structural Biology, Helmholtz Zentrum Muenchen (Germany); Gabel, Frank [Extremophiles and Large Molecular Assemblies Group (ELMA), Institut de Biologie Structurale (IBS) CEA-CNRS-UJF (France); Sattler, Michael, E-mail: sattler@helmholtz-muenchen.de [Institute of Structural Biology, Helmholtz Zentrum Muenchen (Germany)

    2013-05-15

    Many processes in the regulation of gene expression and signaling involve the formation of protein complexes involving multi-domain proteins. Individual domains that mediate protein-protein and protein-nucleic acid interactions are typically connected by flexible linkers, which contribute to conformational dynamics and enable the formation of complexes with distinct binding partners. Solution techniques are therefore required for structural analysis and to characterize potential conformational dynamics. Nuclear magnetic resonance spectroscopy (NMR) provides such information but often only sparse data are obtained with increasing molecular weight of the complexes. It is therefore beneficial to combine NMR data with additional structural restraints from complementary solution techniques. Small angle X-ray/neutron scattering (SAXS/SANS) data can be efficiently combined with NMR-derived information, either for validation or by providing additional restraints for structural analysis. Here, we show that the combination of SAXS and SANS data can help to refine structural models obtained from data-driven docking using HADDOCK based on sparse NMR data. The approach is demonstrated with the ternary protein-protein-RNA complex involving two RNA recognition motif (RRM) domains of Sex-lethal, the N-terminal cold shock domain of Upstream-to-N-Ras, and msl-2 mRNA. Based on chemical shift perturbations we have mapped protein-protein and protein-RNA interfaces and complemented this NMR-derived information with SAXS data, as well as SANS measurements on subunit-selectively deuterated samples of the ternary complex. Our results show that, while the use of SAXS data is beneficial, the additional combination with contrast variation in SANS data resolves remaining ambiguities and improves the docking based on chemical shift perturbations of the ternary protein-RNA complex.

  9. Solid state NMR sequential resonance assignments and conformational analysis of the 2x10.4 kDa dimeric form of the Bacillus subtilis protein Crh

    Energy Technology Data Exchange (ETDEWEB)

    Boeckmann, Anja [Institut de Biologie et Chimie des Proteines, C.N.R.S UMR 5086 (France)], E-mail: a.bockmann@ibcp.fr; Lange, Adam [Max-Planck-Institute for Biophysical Chemistry, Solid-state NMR (Germany); Galinier, Anne [Institut de Biologie Structurale et Microbiologie, C.N.R.S UPR 9043 (France); Luca, Sorin [Max-Planck-Institute for Biophysical Chemistry, Solid-state NMR (Germany); Giraud, Nicolas; Juy, Michel [Institut de Biologie et Chimie des Proteines, C.N.R.S UMR 5086 (France); Heise, Henrike [Max-Planck-Institute for Biophysical Chemistry, Solid-state NMR (Germany); Montserret, Roland; Penin, Francois [Institut de Biologie et Chimie des Proteines, C.N.R.S UMR 5086 (France); Baldus, Marc [Max-Planck-Institute for Biophysical Chemistry, Solid-state NMR (Germany)], E-mail: maba@mpibpc.mpg.de

    2003-12-15

    Solid state NMR sample preparation and resonance assignments of the U-[{sup 13}C,{sup 15}N] 2x10.4 kDa dimeric form of the regulatory protein Crh in microcrystalline, PEG precipitated form are presented. Intra- and interresidue correlations using dipolar polarization transfer methods led to nearly complete sequential assignments of the protein, and to 88% of all {sup 15}N, {sup 13}C chemical shifts. For several residues, the resonance assignments differ significantly from those reported for the monomeric form analyzed by solution state NMR. Dihedral angles obtained from a TALOS-based statistical analysis suggest that the microcrystalline arrangement of Crh must be similar to the domain-swapped dimeric structure of a single crystal form recently solved using X-ray crystallography. For a limited number of protein residues, a remarkable doubling of the observed NMR resonances is observed indicative of local static or dynamic conformational disorder. Our study reports resonance assignments for the largest protein investigated by solid state NMR so far and describes the conformational dimeric variant of Crh with previously unknown chemical shifts.

  10. Feasibility study for biomass power plants in Thailand. Volume 2. appendix: Detailed financial analysis results. Export trade information

    International Nuclear Information System (INIS)

    1997-01-01

    This study, conducted by Black and Veatch, was funded by the U.S. Trade and Development Agency. The report presents a technical and commercial analysis for the development of three nearly identical electricity generating facilities (biomass steam power plants) in the towns of Chachgoengsao, Suphan Buri, and Pichit in Thailand. Volume 2 of the study contains the following appendix: Detailed Financial Analysis Results

  11. Microstructural Analysis of Carbonyl Signal in the 13C NMR Spectra of Methyl Methacrylate - n-Butyl Acrylate Copolymer

    International Nuclear Information System (INIS)

    Bujak, P.; Matlengiewicz, M.

    2005-01-01

    Microstructural information on acrylic copolymers, i.e. distribution of the comonomers along the macromolecular chain and their stereochemical arrangement (tacticity) can be derived from 13 C NMR, analyzing the splitting of their carbonyl signal. In the 100 MHz 13 C NMR spectrum of poly(methyl methacrylate-co-n-butyl acrylate), PMMA-nBA, the carbonyl signal at 174-178,5 ppm is clearly split into the lines of configurational-compositional pentads. This splitting is slightly different in different solvents, hence, recording of the same sample in different solvents may reveal differences important to correct assignment of individual sequences, since their probabilities (intensities) remain the same, while the chemical shift can vary in different solvents. If we would like to perform a complete analysis at this level we have to determine the distribution of 272 individual pentads. The outermost lines in the carbonyl signal of the copolymer can be assigned to the sequences of pure composition by simple comparison with the spectra of respective homopolymers. The rest of the inner lines cannot be easily attributed, therefore, a series of copolymer samples of different composition were synthesized in order to observe the different heterosequences, since depending on copolymer composition, different signals representing individual sequences, assume different relative intensities. To confirm the correctness of proposed attribution a simulation of the carbonyl signal can be performed. It is therefore necessary to know the intensities and positions of individual signals, representing individual compositional-configurational pentads. Calculation of the intensity of the lines can be performed assuming Bernoullian and/or Markov statistics, separately for compositional and configurational sequences and verifying the overall distribution of the individual probabilities. The position of the individual lines cannot be straightforwardly determined, therefore, we have adopted an

  12. Magic angle spinning NMR below 6 K with a computational fluid dynamics analysis of fluid flow and temperature gradients

    Science.gov (United States)

    Sesti, Erika L.; Alaniva, Nicholas; Rand, Peter W.; Choi, Eric J.; Albert, Brice J.; Saliba, Edward P.; Scott, Faith J.; Barnes, Alexander B.

    2018-01-01

    We report magic angle spinning (MAS) up to 8.5 kHz with a sample temperature below 6 K using liquid helium as a variable temperature fluid. Cross polarization 13C NMR spectra exhibit exquisite sensitivity with a single transient. Remarkably, 1H saturation recovery experiments show a 1H T1 of 21 s with MAS below 6 K in the presence of trityl radicals in a glassy matrix. Leveraging the thermal spin polarization available at 4.2 K versus 298 K should result in 71 times higher signal intensity. Taking the 1H longitudinal relaxation into account, signal averaging times are therefore predicted to be expedited by a factor of >500. Computer assisted design (CAD) and finite element analysis were employed in both the design and diagnostic stages of this cryogenic MAS technology development. Computational fluid dynamics (CFD) models describing temperature gradients and fluid flow are presented. The CFD models bearing and drive gas maintained at 100 K, while a colder helium variable temperature fluid stream cools the center of a zirconia rotor. Results from the CFD were used to optimize the helium exhaust path and determine the sample temperature. This novel cryogenic experimental platform will be integrated with pulsed dynamic nuclear polarization and electron decoupling to interrogate biomolecular structure within intact human cells.

  13. NMR of geophysical drill cores with a mobile Halbach scanner

    International Nuclear Information System (INIS)

    Talnishnikh, E.

    2007-01-01

    This thesis is devoted to a mobile NMR with an improved Halbach scanner. This is a lightweight tube-shaped magnet with sensitive volume larger and a homogeneity of the magnetic field higher than the previous prototype version. The improved Halbach scanner is used for analysis of water-saturated drill cores and plugs with diameters up to 60 mm. To provide the analysis, the standard 1D technique with the CPMG sequence as well as 2D correlation experiments were successfully applied and adapted to study properties of fluid-saturated sediments. Afterwards the Halbach scanner was calibrated to fast non-destructive measurements of porosity, relaxation time distributions, and estimation of permeability. These properties can be calculated directly from the NMR data using the developed methodology. Any independent measurements of these properties with other methods are not needed. One of the main results of this work is the development of a new NMR on-line core scanner for measurements of porosity in long cylindrical and semi cylindrical drill cores. Also dedicated software was written to operate the NMR on-line core scanner. The physical background of this work is the study of the diffusion influence on transverse relaxation. The diffusion effect in the presence of internal gradients in porous media was probed by 1D and 2D experiments. The transverse relaxation time distributions obtained from 1D and from 2D experiments are comparable but different in fine details. Two new methodologies were developed based on the results of this study. First is the methodology quantifying the influence of diffusion in the internal gradients of water-saturated sediments on transverse relaxation from 2D correlation experiments. The second one is the correction of the permeability estimation from the NMR data taking in account the influence of the diffusion. Furthermore, PFG NMR technique was used to study restricted diffusion in the same kind of samples. Preliminary results are reported

  14. NMR of geophysical drill cores with a mobile Halbach scanner

    Energy Technology Data Exchange (ETDEWEB)

    Talnishnikh, E.

    2007-08-21

    This thesis is devoted to a mobile NMR with an improved Halbach scanner. This is a lightweight tube-shaped magnet with sensitive volume larger and a homogeneity of the magnetic field higher than the previous prototype version. The improved Halbach scanner is used for analysis of water-saturated drill cores and plugs with diameters up to 60 mm. To provide the analysis, the standard 1D technique with the CPMG sequence as well as 2D correlation experiments were successfully applied and adapted to study properties of fluid-saturated sediments. Afterwards the Halbach scanner was calibrated to fast non-destructive measurements of porosity, relaxation time distributions, and estimation of permeability. These properties can be calculated directly from the NMR data using the developed methodology. Any independent measurements of these properties with other methods are not needed. One of the main results of this work is the development of a new NMR on-line core scanner for measurements of porosity in long cylindrical and semi cylindrical drill cores. Also dedicated software was written to operate the NMR on-line core scanner. The physical background of this work is the study of the diffusion influence on transverse relaxation. The diffusion effect in the presence of internal gradients in porous media was probed by 1D and 2D experiments. The transverse relaxation time distributions obtained from 1D and from 2D experiments are comparable but different in fine details. Two new methodologies were developed based on the results of this study. First is the methodology quantifying the influence of diffusion in the internal gradients of water-saturated sediments on transverse relaxation from 2D correlation experiments. The second one is the correction of the permeability estimation from the NMR data taking in account the influence of the diffusion. Furthermore, PFG NMR technique was used to study restricted diffusion in the same kind of samples. Preliminary results are reported

  15. Author Details

    African Journals Online (AJOL)

    PROMOTING ACCESS TO AFRICAN RESEARCH. AFRICAN JOURNALS ONLINE (AJOL) · Journals · Advanced Search · USING AJOL · RESOURCES. Author Details. Journal Home > Advanced Search > Author Details. Log in or Register to get access to full text downloads.

  16. Author Details

    African Journals Online (AJOL)

    Author Details. Journal Home > Advanced Search > Author Details. Log in or Register to get access to full text downloads. ... An algorithm to retrieve Land Surface Temperature using Landsat-8 Dataset Abstract PDF. ISSN: 2225-8531.

  17. Detailed analysis of contrast-enhanced MRI of hands and wrists in patients with psoriatic arthritis

    International Nuclear Information System (INIS)

    Tehranzadeh, Jamshid; Ashikyan, Oganes; Anavim, Arash; Shin, John

    2008-01-01

    The objective was to perform detailed analysis of the involved soft tissues, tendons, joints, and bones in the hands and wrists of patients with psoriatic arthritis (PsA). We reviewed 23 contrast-enhanced MR imaging studies (13 hands and 10 wrists) in 10 patients with the clinical diagnosis of PsA. We obtained clinical information from medical records and evaluated images for the presence of erosions, bone marrow edema, joint synovitis, tenosynovitis, carpal tunnel, and soft tissue involvement. Two board-certified musculoskeletal radiologists reviewed all images independently. Differences were resolved during a subsequent joint session. The average duration of disease was 71.3 months, ranging from 1 month to 25 years. Eight of the 10 wrists (80%) and 6 of the 13 hands demonstrated bone erosions. Bone marrow abnormalities were shown in 5 of the 10 wrists (50%) and 4 of the 14 hands (31%). Triangular fibrocartilage tears were seen in 6 of the 10 wrists (60%). Wrist and hand joint synovitis were present in all studies (67 wrist joints and 101 hand joints). Wrist soft tissue involvement was detected in 9 of the 10 wrists (90%) and hand soft tissue involvement was present in 12 of the 13 wrists (92%). Findings adjacent to the region of soft tissue involvement included synovitis (4 wrists) and tenosynovitis (3 wrists). Bone marrow edema adjacent to the region of soft tissue involvement was seen in one wrist. Bulge of the flexor retinaculum was seen in 4 of the 10 wrists (40%) and median nerve enhancement was seen in 8 of the 10 wrists (80%). Tenosynovitis was seen in all studies (all 10 of the hands and all 13 of the wrists). The ''rheumatoid'' type of distribution of bony lesions was common in our study. Interobserver agreement for various findings ranged from 83% to 100%. Contrast-enhanced MRI unequivocally demonstrated bone marrow edema, erosions, tendon and soft-tissue disease, and median nerve involvement, with good interobserver reliability in patients with PsA of

  18. Detailed analysis of contrast-enhanced MRI of hands and wrists in patients with psoriatic arthritis

    Energy Technology Data Exchange (ETDEWEB)

    Tehranzadeh, Jamshid [University of California, Department of Radiological Sciences, Irvine (United States); University of California Medical Center, Department of Radiological Sciences R-140, Orange, CA (United States); Ashikyan, Oganes; Anavim, Arash; Shin, John [University of California, Department of Radiological Sciences, Irvine (United States)

    2008-05-15

    The objective was to perform detailed analysis of the involved soft tissues, tendons, joints, and bones in the hands and wrists of patients with psoriatic arthritis (PsA). We reviewed 23 contrast-enhanced MR imaging studies (13 hands and 10 wrists) in 10 patients with the clinical diagnosis of PsA. We obtained clinical information from medical records and evaluated images for the presence of erosions, bone marrow edema, joint synovitis, tenosynovitis, carpal tunnel, and soft tissue involvement. Two board-certified musculoskeletal radiologists reviewed all images independently. Differences were resolved during a subsequent joint session. The average duration of disease was 71.3 months, ranging from 1 month to 25 years. Eight of the 10 wrists (80%) and 6 of the 13 hands demonstrated bone erosions. Bone marrow abnormalities were shown in 5 of the 10 wrists (50%) and 4 of the 14 hands (31%). Triangular fibrocartilage tears were seen in 6 of the 10 wrists (60%). Wrist and hand joint synovitis were present in all studies (67 wrist joints and 101 hand joints). Wrist soft tissue involvement was detected in 9 of the 10 wrists (90%) and hand soft tissue involvement was present in 12 of the 13 wrists (92%). Findings adjacent to the region of soft tissue involvement included synovitis (4 wrists) and tenosynovitis (3 wrists). Bone marrow edema adjacent to the region of soft tissue involvement was seen in one wrist. Bulge of the flexor retinaculum was seen in 4 of the 10 wrists (40%) and median nerve enhancement was seen in 8 of the 10 wrists (80%). Tenosynovitis was seen in all studies (all 10 of the hands and all 13 of the wrists). The 'rheumatoid' type of distribution of bony lesions was common in our study. Interobserver agreement for various findings ranged from 83% to 100%. Contrast-enhanced MRI unequivocally demonstrated bone marrow edema, erosions, tendon and soft-tissue disease, and median nerve involvement, with good interobserver reliability in patients with

  19. NMR-based Metabolomics Analysis of Liver from C57BL/6 Mouse Exposed to Ionizing Radiation

    Energy Technology Data Exchange (ETDEWEB)

    Xiao, Xiongjie [Pacific Northwest National Laboratory, Richland, Washington 99352; State Key Laboratory of Magnetic Resonance and Atomic and Molecular Physics, National Center for Magnetic Resonance in Wuhan, Wuhan Institute of Physics and Mathematics, the Chinese Academy of Sciences, Wuhan, 430071, PR China; University of Chinese Academy of Sciences, Beijing 100049, China; Hu, Mary [Pacific Northwest National Laboratory, Richland, Washington 99352; Zhang, Xu [State Key Laboratory of Magnetic Resonance and Atomic and Molecular Physics, National Center for Magnetic Resonance in Wuhan, Wuhan Institute of Physics and Mathematics, the Chinese Academy of Sciences, Wuhan, 430071, PR China; Hu, Jian Zhi [Pacific Northwest National Laboratory, Richland, Washington 99352

    2017-07-01

    The health effects of exposing to ionizing radiation are attracting great interest in the space exploration community and patients considering radiotherapy. However, the impact to metabolism after exposure to high dose radiation has not yet been clearly defined in livers. In the present study, 1H nuclear magnetic resonance (NMR) based metabolomics combined with multivariate data analysis are applied to study the changes of metabolism in the liver of C57BL/6 mouse after whole body exposure to either gamma (3.0 and 7.8 Gy) or proton (3.0 Gy) radiation. Principal component analysis (PCA) and orthogonal projection to latent structures analysis (OPLS) are employed for classification and identification of potential biomarkers associated with gamma and proton irradiation. The results show that the radiation exposed groups can be well separated from the control group. At the same radiation dosage, the group exposed to proton radiation is well separated from the group exposed to gamma radiation, indicating different radiation sources induce different alterations based on metabolic profiling. Common to both gamma and proton radiation at the high radiation doses studied in this work, compared with the control groups the concentrations of choline, O-phosphocholine and trimethylamine N-oxide are decreased statistically, while those of glutamine, glutathione, malate, creatinine, phosphate, betaine and 4-hydroxyphenylacetate are statistically and significantly elevated after exposure to radiation. Since these altered metabolites are associated with multiple biological pathways, the changes suggest that the exposure to radiation induce abnormality in multiple biological pathways. In particular, metabolites such as 4-hydroxyphenylacetate, betaine, glutamine, choline and trimethylamine N-oxide may be good candidates of pre-diagnose biomarkers for ionizing radiation in liver.

  20. NMR spectroscopy using liquid crystal solvents

    CERN Document Server

    Emsley, JW

    2013-01-01

    NMR Spectroscopy using Liquid Crystal Solvents covers the importance of using a liquid crystal solvent in NMR to derive nuclear dipolar spin-spin coupling constants. This book is composed of ten chapters, and begins with a brief description of the features and benefits of liquid crystal in NMR spectroscopic analysis. The succeeding chapters deal with the mode of operation of nuclear spin Hamiltonian for partially oriented molecules and the analysis of NMR spectra of partially oriented molecules, as well as the determination of rigid molecule structure. These topics are followed by discussions

  1. Solid state 13C NMR analysis of shales and coals from Laramide Basins. Final report, March 1, 1995--March 31, 1996

    Energy Technology Data Exchange (ETDEWEB)

    Miknis, F.P.; Jiao, Z.S.; Zhao, Hanqing; Surdam, R.C.

    1998-12-31

    This Western Research Institute (WRI) jointly sponsored research (JSR) project augmented and complemented research conducted by the University of Wyoming Institute For Energy Research for the Gas Research Institute. The project, {open_quotes}A New Innovative Exploitation Strategy for Gas Accumulations Within Pressure Compartments,{close_quotes} was a continuation of a project funded by the GRI Pressure Compartmentalization Program that began in 1990. That project, {open_quotes}Analysis of Pressure Chambers and Seals in the Powder River Basin, Wyoming and Montana,{close_quotes} characterized a new class of hydrocarbon traps, the discovery of which can provide an impetus to revitalize the domestic petroleum industry. In support of the UW Institute For Energy Research`s program on pressure compartmentalization, solid-state {sup 13}C NMR measurements were made on sets of shales and coals from different Laramide basins in North America. NMR measurements were made on samples taken from different formations and depths of burial in the Alberta, Bighorn, Denver, San Juan, Washakie, and Wind River basins. The carbon aromaticity determined by NMR was shown to increase with depth of burial and increased maturation. In general, the NMR data were in agreement with other maturational indicators, such as vitrinite reflectance, illite/smectite ratio, and production indices. NMR measurements were also obtained on residues from hydrous pyrolysis experiments on Almond and Lance Formation coals from the Washakie Basin. These data were used in conjunction with mass and elemental balance data to obtain information about the extent of carbon aromatization that occurs during artificial maturation. The data indicated that 41 and 50% of the original aliphatic carbon in the Almond and Lance coals, respectively, aromatized during hydrous pyrolysis.

  2. Author Details

    African Journals Online (AJOL)

    Details PDF · Vol 22, No 2 (1999) - Articles Vegetation under different tree species in Acacia woodland in the Rift Valley of Ethiopia Details PDF · Vol 22, No 2 (1999) - Articles Preliminary evaluation of Phytomyza orobanchia (Diptera: Agromyzidae) as a controller of Orobanche spp in Ethiopia Details PDF. ISSN: 2520–7997.

  3. Analysis of the mechanical properties and characterization by solid state {sup 13} C NMR of recycled EVA copolymer/silica composites

    Energy Technology Data Exchange (ETDEWEB)

    Stael, Giovanni Chaves [Observatorio Nacional, Rio de Janeiro, RJ (Brazil)]. E-mail: stael@on.br; Rocha, Marisa Cristina Guimaraes [Universidade do Estado do Rio de Janeiro, Nova Friburgo, RJ (Brazil). Instituto Politecnico; Menezes, Sonia Maria Cabral de [PETROBRAS, Rio de Janeiro, RJ (Brazil). Centro de Pesquisas. Quimica; D' Almeida, Jose Roberto Morais; Ruiz, Naira Machado da Silva [Pontificia Universidade Catolica do Rio de Janeiro, RJ (Brazil)

    2005-07-15

    The incorporation of micrometer sized silica particles on poly (ethylene-co-vinyl acetate) - EVA - residues from the footwear industry was evaluated. The effects of the processing parameters - temperature and mixing ratio - on the mechanical behavior of molded plates of neat recycled EVA and EVA/silica composites were also investigated. The mechanical properties measured by the tensile test, the fractographic analysis by scanning electron microscopy (SEM), and the {sup 13} C Nuclear Magnetic Resonance (NMR) showed a reduced EVA to silica compatibility. Therefore, incorporation of untreated silica to recycled EVA copolymer produced a slight decrease on the mechanical performance of EVA/silica composites in respect to neat EVA copolymer. The NMR analysis also shows that the crosslinking process on recycled EVA may be occurring at the carbonyl group. (author)

  4. Introducing Undergraduate Students to Metabolomics Using a NMR-Based Analysis of Coffee Beans

    Science.gov (United States)

    Sandusky, Peter Olaf

    2017-01-01

    Metabolomics applies multivariate statistical analysis to sets of high-resolution spectra taken over a population of biologically derived samples. The objective is to distinguish subpopulations within the overall sample population, and possibly also to identify biomarkers. While metabolomics has become part of the standard analytical toolbox in…

  5. GIS-assisted spatial analysis for urban regulatory detailed planning: designer's dimension in the Chinese code system

    Science.gov (United States)

    Yu, Yang; Zeng, Zheng

    2009-10-01

    By discussing the causes behind the high amendments ratio in the implementation of urban regulatory detailed plans in China despite its law-ensured status, the study aims to reconcile conflict between the legal authority of regulatory detailed planning and the insufficient scientific support in its decision-making and compilation by introducing into the process spatial analysis based on GIS technology and 3D modeling thus present a more scientific and flexible approach to regulatory detailed planning in China. The study first points out that the current compilation process of urban regulatory detailed plan in China employs mainly an empirical approach which renders it constantly subjected to amendments; the study then discusses the need and current utilization of GIS in the Chinese system and proposes the framework of a GIS-assisted 3D spatial analysis process from the designer's perspective which can be regarded as an alternating processes between the descriptive codes and physical design in the compilation of regulatory detailed planning. With a case study of the processes and results from the application of the framework, the paper concludes that the proposed framework can be an effective instrument which provides more rationality, flexibility and thus more efficiency to the compilation and decision-making process of urban regulatory detailed plan in China.

  6. Human projected area factors for detailed direct and diffuse solar radiation analysis

    DEFF Research Database (Denmark)

    Kubaha, K.; Fiala, D.; Toftum, Jørn

    2004-01-01

    Projected area factors for individual segments of the standing and sedentary human body were modelled for both direct and diffuse solar radiation using detailed 3D geometry and radiation models. The local projected area factors with respect to direct short-wave radiation are a function of the solar...

  7. A detailed cost analysis of in vitro fertilization and intracytoplasmic sperm injection treatment.

    NARCIS (Netherlands)

    Bouwmans, C.A.; Lintsen, A.M.E.; Eijkemans, M.J.; Habbema, J.D.F.; Braat, D.D.M.; Hakkaart, L.

    2008-01-01

    OBJECTIVE: To provide detailed information about costs of in vitro fertilization (IVF) and intracytoplasmic sperm injection (ICSI) treatment stages and to estimate the cost per IVF and ICSI treatment cycle and ongoing pregnancy. DESIGN: Descriptive micro-costing study. SETTING: Four Dutch IVF

  8. NMR, ESI/MS, and MALDI-TOF/MS analysis of pear juice polymeric proanthocyanidins with potent free radical scavenging activity.

    Science.gov (United States)

    Es-Safi, Nour-Eddine; Guyot, Sylvain; Ducrot, Paul-Henri

    2006-09-20

    The structure of a polymeric proanthocyanidin fraction isolated from pear juice was characterized by NMR, ESI/MS, and MALDI-TOF/MS analyses, and its antioxidant activity was investigated using the DPPH free radical scavenging method. The results obtained from 13C NMR analysis showed the predominance of signals representative of procyanidins. Typical signals in the chemical shift region between 70 and 90 ppm demonstrated the exclusive presence of epicatechin units. The results obtained through negative ESI/MS analysis showed singly and doubly charged ions corresponding to the molecular mass of procyanidins with a degree of polymerization up to 22. The spectra obtained through MALDI-TOF/MS analysis revealed the presence of two series of tannin oligomers. Supporting the observations from NMR spectroscopy, the first series consists of well-resolved tannin identified as procyanidin polymers units with chain lengths of up to 25. A second series of monogalloyl flavan-3-ols polymers with polymerization degree up to 25 were also detected. This is the first mass spectrometric evidence confirming the existence of galloylated procyanidin oligomers in pear fruits. Within each of these oligomers, various signals exist suggesting the presence of several oligomeric tannins. The antioxidant properties of the polymeric fraction were investigated through reduction of the DPPH free radical, and the results obtained showed that the polymeric fraction exhibited a higher antioxidant power compared to those of (+)-catechin and B3 procyanidin dimer.

  9. Metabolomic profiling of the phytomedicinal constituents of Carica papaya L. leaves and seeds by 1H NMR spectroscopy and multivariate statistical analysis.

    Science.gov (United States)

    Gogna, Navdeep; Hamid, Neda; Dorai, Kavita

    2015-11-10

    Extracts from the Carica papaya L. plant are widely reported to contain metabolites with antibacterial, antioxidant and anticancer activity. This study aims to analyze the metabolic profiles of papaya leaves and seeds in order to gain insights into their phytomedicinal constituents. We performed metabolite fingerprinting using 1D and 2D 1H NMR experiments and used multivariate statistical analysis to identify those plant parts that contain the most concentrations of metabolites of phytomedicinal value. Secondary metabolites such as phenyl propanoids, including flavonoids, were found in greater concentrations in the leaves as compared to the seeds. UPLC-ESI-MS verified the presence of significant metabolites in the papaya extracts suggested by the NMR analysis. Interestingly, the concentration of eleven secondary metabolites namely caffeic, cinnamic, chlorogenic, quinic, coumaric, vanillic, and protocatechuic acids, naringenin, hesperidin, rutin, and kaempferol, were higher in young as compared to old papaya leaves. The results of the NMR analysis were corroborated by estimating the total phenolic and flavonoid content of the extracts. Estimation of antioxidant activity in leaves and seed extracts by DPPH and ABTS in-vitro assays and antioxidant capacity in C2C12 cell line also showed that papaya extracts exhibit high antioxidant activity. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Characterization of organic matter in sediment cores of the Todos os Santos Bay, Bahia, Brazil, by elemental analysis and 13C NMR

    International Nuclear Information System (INIS)

    Costa, A.B.; Novotny, E.H.; Bloise, A.C.; Azevedo, E.R. de; Bonagamba, T.J.; Zucchi, M.R.; Santos, V.L.C.S.; Azevedo, A.E.G.

    2011-01-01

    Highlights: → The impact of human activity on the sediments of Todos os Santos Bay in Brazil was evaluated by EA and 13 C NMR. → This article reports a study of six sediment cores collected at different depths and regions. → The elemental profiles of cores suggest an abrupt change in the sedimentation regime, corresponds to about 50 years ago, coinciding with the implantation of major onshore industrial projects. → The results presented illustrate several important aspects of environmental impact of human activity on this bay. - Abstract: The impact of human activity on the sediments of Todos os Santos Bay in Brazil was evaluated by elemental analysis and 13 C Nuclear Magnetic Resonance ( 13 C NMR). This article reports a study of six sediment cores collected at different depths and regions of Todos os Santos Bay. The elemental profiles of cores collected on the eastern side of Frades Island suggest an abrupt change in the sedimentation regime. Autoregressive Integrated Moving Average (ARIMA) analysis corroborates this result. The range of depths of the cores corresponds to about 50 years ago, coinciding with the implantation of major onshore industrial projects in the region. Principal Component Analysis of the 13 C NMR spectra clearly differentiates sediment samples closer to the Subae estuary, which have high contents of terrestrial organic matter, from those closer to a local oil refinery. The results presented in this article illustrate several important aspects of environmental impact of human activity on this bay.

  11. Multicomponent analysis of fat- and water-soluble vitamins and auxiliary substances in multivitamin preparations by qNMR.

    Science.gov (United States)

    Eiff, Julia; Monakhova, Yulia B; Diehl, Bernd W K

    2015-04-01

    A nuclear magnetic resonance (NMR) spectroscopic method was tested to control 12 vitamins and accompanying substances in multivitamin preparations. The limits of detection (LODs) and limits of quantification (LOQs) varied in the 9.0-77.0 mg/kg and in the 34.5-93.5 mg/kg range, respectively. The coefficients of variation (CVs) ranged between 0.9% and 12%. The (1)H NMR spectra showed linearity for the 140-260 mg sample weight (R(2) > 0.918). The NMR spectra of multivitamin preparations showed the presence of different degradation products of ascorbic acid. The NMR method was applied to 13 different multivitamin preparations including tablets, capsules, and effervescent tablets with average recovery rates between 85% and 132%. A number of accompanying substances (citric acid, mannitol, saccharin, cyclamate, sum of steviol glycosides, and butylhydroxytoluene) were additionally identified and quantified. NMR was found to be suitable for the simultaneous qualitative measurement of water- and fat-soluble vitamins and accompanying substances and shows some promise for quantitative determination of at least 5 vitamins (B1, B3, B5, B6, and E) in multivitamin preparations.

  12. Analysis of the backbone dynamics of capsicein using 15N NMR relaxation rate measurements

    International Nuclear Information System (INIS)

    Van Heijenoort, C.; Bouaziz, S.; Guittet, E.

    1994-01-01

    15 N relaxation times T 1 and T 1ρ , and heteronuclear steady state nOes, were measured on capsicein, a 98 residue protein. The classical analysis of these data using directly the Lipari and Szabo formalism was shown to give incoherent results, probably due to the presence of a slow exchange along the whole protein. This global exchange broadening made the usual preliminary evaluation of the overall correlation time of capsicein using the Lipari and Szabo expression for the spectral densities impossible. (authors). 2 figs., 23 refs

  13. Detailed budget analysis of HONO in central London reveals a missing daytime source

    Directory of Open Access Journals (Sweden)

    J. D. Lee

    2016-03-01

    Full Text Available Measurements of HONO were carried out at an urban background site near central London as part of the Clean air for London (ClearfLo project in summer 2012. Data were collected from 22 July to 18 August 2014, with peak values of up to 1.8 ppbV at night and non-zero values of between 0.2 and 0.6 ppbV seen during the day. A wide range of other gas phase, aerosol, radiation, and meteorological measurements were made concurrently at the same site, allowing a detailed analysis of the chemistry to be carried out. The peak HONO/NOx ratio of 0.04 is seen at  ∼  02:00 UTC, with the presence of a second, daytime, peak in HONO/NOx of similar magnitude to the night-time peak, suggesting a significant secondary daytime HONO source. A photostationary state calculation of HONO involving formation from the reaction of OH and NO and loss from photolysis, reaction with OH, and dry deposition shows a significant underestimation during the day, with calculated values being close to 0, compared to the measurement average of 0.4 ppbV at midday. The addition of further HONO sources from the literature, including dark conversion of NO2 on surfaces, direct emission, photolysis of ortho-substituted nitrophenols, the postulated formation from the reaction of HO2 ×  H2O with NO2, photolysis of adsorbed HNO3 on ground and aerosols, and HONO produced by photosensitized conversion of NO2 on the surface increases the daytime modelled HONO to 0.1 ppbV, still leaving a significant missing daytime source. The missing HONO is plotted against a series of parameters including NO2 and OH reactivity (used as a proxy for organic material, with little correlation seen. Much better correlation is observed with the product of these species with j(NO2, in particular NO2 and the product of NO2 with OH reactivity. This suggests the missing HONO source is in some way related to NO2 and also requires sunlight. Increasing the photosensitized surface conversion rate of NO2 by a

  14. Assessment of preparation methods for organic phosphorus analysis in phosphorus-polluted Fe/Al-rich Haihe river sediments using solution 31P-NMR.

    Directory of Open Access Journals (Sweden)

    Wenqiang Zhang

    Full Text Available Fe/Al-rich river sediments that were highly polluted with phosphorus (P were used in tests to determine the optimum preparation techniques for measuring organic P (Po using solution (31P nuclear magnetic resonance spectroscopy ((31P-NMR. The optimum pre-treatment, extraction time, sediment to solution ratio and sodium hydroxide-ethylenediaminetetraacetic acid (NaOH-EDTA extractant solution composition were determined. The total P and Po recovery rates were higher from freeze- and air-dried samples than from fresh samples. An extraction time of 16 h was adequate for extracting Po, and a shorter or longer extraction time led to lower recoveries of total P and Po, or led to the degradation of Po. An ideal P recovery rate and good-quality NMR spectra were obtained at a sediment:solution ratio of 1:10, showing that this ratio is ideal for extracting Po. An extractant solution of 0.25 M NaOH and 50 mM EDTA was found to be more appropriate than either NaOH on its own, or a more concentrated NaOH-EDTA mixture for (31P-NMR analysis, as this combination minimized interference from paramagnetic ions and was appropriate for the detected range of Po concentrations. The most appropriate preparation method for Po analysis, therefore, was to extract the freeze-dried and ground sediment sample with a 0.25 M NaOH and 50 mM EDTA solution at a sediment:solution ratio of 1:10, for 16 h, by shaking. As lyophilization of the NaOH-EDTA extracts proved to be an optimal pre-concentration method for Po analysis in the river sediment, the extract was lyophilized as soon as possible, and analyzed by (31P-NMR.

  15. Detailed Aerodynamic Analysis of a Shrouded Tail Rotor Using an Unstructured Mesh Flow Solver

    Science.gov (United States)

    Lee, Hee Dong; Kwon, Oh Joon

    The detailed aerodynamics of a shrouded tail rotor in hover has been numerically studied using a parallel inviscid flow solver on unstructured meshes. The numerical method is based on a cell-centered finite-volume discretization and an implicit Gauss-Seidel time integration. The calculation was made for a single blade by imposing a periodic boundary condition between adjacent rotor blades. The grid periodicity was also imposed at the periodic boundary planes to avoid numerical inaccuracy resulting from solution interpolation. The results were compared with available experimental data and those from a disk vortex theory for validation. It was found that realistic three-dimensional modeling is important for the prediction of detailed aerodynamics of shrouded rotors including the tip clearance gap flow.

  16. Determination of average molecular parameters of vacuum residues and asphalt by elementary analysis and 1 H NMR and comparison with 13 C NMR results

    International Nuclear Information System (INIS)

    Teixeira, Marco Antonio; Marques, Rosana Garrido

    1995-01-01

    This work proposes a new approach for determining average molecular parameters in petroleum fractions, from some approximation based on consideration about average composition of petroleum heavy fractions. A comparative evaluation between the proposed method and the traditional one has been carried out, showing 60 hours saving in time spent at analysis. The results were present and discussed

  17. Determination of connected components inthe analysis of homogeneous and detail zonesin color images

    Directory of Open Access Journals (Sweden)

    Cristina Pérez-Benito

    2018-02-01

    Full Text Available A model based on local graphs to classify pixels coming from at or detail regions of an image is presented. For each pixel a local graph is dened. Its structure will depend on the similarity between neighbouring pixels. Its features allow us to classify each image pixel as belonging to one type of region or the other. This classication is an essential pre-processing technique for many Computer Vision tools, such as smoothingor sharpening of digital color images.

  18. An Implementation and Detailed Analysis of the K-SVD Image Denoising Algorithm

    Directory of Open Access Journals (Sweden)

    Marc Lebrun

    2012-05-01

    Full Text Available K-SVD is a signal representation method which, from a set of signals, can derive a dictionary able to approximate each signal with a sparse combination of the atoms. This paper focuses on the K-SVD-based image denoising algorithm. The implementation is described in detail and its parameters are analyzed and varied to come up with a reliable implementation.

  19. General method of preparation of uniformly 13C, 15N-labeled DNA fragments for NMR analysis of DNA structures

    International Nuclear Information System (INIS)

    Rene, Brigitte; Masliah, Gregoire; Zargarian, Loussine; Mauffret, Olivier; Fermandjian, Serge

    2006-01-01

    Summary 13 C, 15 N labeling of biomolecules allows easier assignments of NMR resonances and provides a larger number of NMR parameters, which greatly improves the quality of DNA structures. However, there is no general DNA-labeling procedure, like those employed for proteins and RNAs. Here, we describe a general and widely applicable approach designed for preparation of isotopically labeled DNA fragments that can be used for NMR studies. The procedure is based on the PCR amplification of oligonucleotides in the presence of labeled deoxynucleotides triphosphates. It allows great flexibility thanks to insertion of a short DNA sequence (linker) between two repeats of DNA sequence to study. Size and sequence of the linker are designed as to create restriction sites at the junctions with DNA of interest. DNA duplex with desired sequence and size is released upon enzymatic digestion of the PCR product. The suitability of the procedure is validated through the preparation of two biological relevant DNA fragments

  20. Protein analysis by 31p NMR spectroscopy in ionic liquid: quantitative determination of enzymatically created cross-links.

    Science.gov (United States)

    Monogioudi, Evanthia; Permi, Perttu; Filpponen, Ilari; Lienemann, Michael; Li, Bin; Argyropoulos, Dimitris; Buchert, Johanna; Mattinen, Maija-Liisa

    2011-02-23

    Cross-linking of β-casein by Trichoderma reesei tyrosinase (TrTyr) and Streptoverticillium mobaraense transglutaminase (Tgase) was analyzed by (31)P nuclear magnetic resonance (NMR) spectroscopy in ionic liquid (IL). According to (31)P NMR, 91% of the tyrosine side chains were cross-linked by TrTyr at high dosages. When Tgase was used, no changes were observed because a different cross-linking mechanism was operational. However, this verified the success of the phosphitylation of phenolics within the protein matrix in the IL. Atomic force microscopy (AFM) in solid state showed that disk-shaped nanoparticles were formed in the reactions with average diameters of 80 and 20 nm for TrTyr and Tgase, respectively. These data further advance the current understanding of the action of tyrosinases on proteins on molecular and chemical bond levels. Quantitative (31)P NMR in IL was shown to be a simple and efficient method for the study of protein modification.

  1. A Meta-Analysis Detailing Overall Sexual Function and Orgasmic Function in Women Undergoing Midurethral Sling Surgery for Stress Incontinence

    Directory of Open Access Journals (Sweden)

    Nicole Szell, DO

    2017-06-01

    Szell N, Komisaruk B, Goldstein SW, et al. A Meta-Analysis Detailing Overall Sexual Function and Orgasmic Function in Women Undergoing Midurethral Sling Surgery for Stress Incontinence. Sex Med 2017;5:e84–e93.

  2. Remote sensing of selective logging in Amazonia Assessing limitations based on detailed field observations, Landsat ETM+, and textural analysis.

    Science.gov (United States)

    Gregory P. Asner; Michael Keller; Rodrigo Pereira; Johan C. Zweede

    2002-01-01

    We combined a detailed field study of forest canopy damage with calibrated Landsat 7 Enhanced Thematic Mapper Plus (ETM+) reflectance data and texture analysis to assess the sensitivity of basic broadband optical remote sensing to selective logging in Amazonia. Our field study encompassed measurements of ground damage and canopy gap fractions along a chronosequence of...

  3. AGB nucleosynthesis in the Large Magellanic Cloud. Detailed abundance analysis of the RV Tauri star MACHO 47.2496.8

    NARCIS (Netherlands)

    Reyniers, M.; Abia, C.; van Winckel, H.; Lloyd Evans, T.; Decin, L.K.E.; Eriksson, K.; Pollard, K.R.

    2007-01-01

    Context: .Abundance analysis of post-AGB objects as probes of AGB nucleosynthesis. Aims: .A detailed photospheric abundance study is performed on the carbon-rich post-AGB candidate MACHO 47.2496.8 in the LMC. Methods: .High-resolution, high signal-to-noise ESO VLT-UVES spectra of MACHO 47.2496.8 are

  4. HPLC, NMR and MALDI-TOF MS analysis of condensed tannins from Lithocarpus glaber leaves with potent free radical scavenging activity.

    Science.gov (United States)

    Zhang, Liang Liang; Lin, Yi Ming

    2008-12-04

    Using acid-catalyzed degradation in the presence of cysteamine, the condensed tannins from Lithocarpus glaber leaves were characterized, following thiolysis, by means of reversed-phase HPLC, 13C-NMR and matrix-assisted laser desorption/ionization time of flight mass spectrometry (MALDI-TOF MS) analyses. The thiolysis reaction products showed the presence of the procyanidin (PC) and prodelphinidin (PD) structures. The 13C-NMR spectrum revealed that the condensed tannins were comprised of PD (72.4%) and PC (27.6%), and with a greater content of cis configuration rather than the trans configuration of C2-C3. The MALDI-TOF MS analysis proved the presence of PD units, and the maximum degree of polymerization (DP) was an undecamer. The antioxidant activity of condensed tannins from L. glaber leaves was evaluated by using a free radical scavenging activity assay.

  5. Magic-Angle-Spinning NMR Magnet Development: Field Analysis and Prototypes

    Science.gov (United States)

    Voccio, John; Hahn, Seungyong; Park, Dong Keun; Ling, Jiayin; Kim, Youngjae; Bascuñán, Juan; Iwasa, Yukikazu

    2013-01-01

    We are currently working on a program to complete a 1.5 T/75 mm RT bore magic-angle-spinning nuclear magnetic resonance magnet. The magic-angle-spinning magnet comprises a z-axis 0.866-T solenoid and an x-axis 1.225-T dipole, each to be wound with NbTi wire and operated at 4.2 K in persistent mode. A combination of the fields creates a 1.5-T field pointed at 54.74 degrees (magic angle) from the rotation (z) axis. In the first year of this 3-year program, we have completed magnetic analysis and design of both coils. Also, using a winding machine of our own design and fabrication, we have wound several prototype dipole coils with NbTi wire. As part of this development, we have repeatedly made successful persistent NbTi-NbTi joints with this multifilamentary NbTi wire. PMID:24058275

  6. NMR in structure-based drug design.

    Science.gov (United States)

    Carneiro, Marta G; Ab, Eiso; Theisgen, Stephan; Siegal, Gregg

    2017-11-08

    NMR spectroscopy is a powerful technique that can provide valuable structural information for drug discovery endeavors. Here, we discuss the strengths (and limitations) of NMR applications to structure-based drug discovery, highlighting the different levels of resolution and throughput obtainable. Additionally, the emerging field of paramagnetic NMR in drug discovery and recent developments in approaches to speed up and automate protein-observed NMR data collection and analysis are discussed. © 2017 The Author(s). Published by Portland Press Limited on behalf of the Biochemical Society.

  7. NMR analysis of t-butyl-catalyzed deuterium exchange at unactivated arene localities.

    Science.gov (United States)

    Stack, Douglas E; Eastman, Rachel

    2016-10-01

    Regioselective labelling of arene rings via electrophilic exchange is often dictated by the electronic environment caused by substituents present on the aromatic system. Previously, we observed the presence of a t-butyl group, either covalently bond or added as an external reagent, could impart deuterium exchange to the unactivated, C1-position of estrone. Here, we provide nuclear magnetic resonance analysis of this exchange in a solvent system composed of 50:50 trifluoroacetic acid and D 2 O with either 2-t-butylestrone or estrone in the presence of t-butyl alcohol has shed insights into the mechanism of this t-butyl-catalyzed exchange. Fast exchange of the t-butyl group concurrent with the gradual reduction of the H1 proton signal in both systems suggest a mechanism involving ipso attack of the t-butyl position by deuterium. The reversible addition/elimination of the t-butyl group activates the H1 proton towards exchange by a mechanism of t-butyl incorporation, H1 activation and exchange, followed by eventual t-butyl elimination. Density functional calculations are consistent with the observation of fast t-butyl exchange concurrent with slower H1 exchange. The σ-complex resulting from ipso attack of deuterium at the t-butyl carbon was 6.6 kcal/mol lower in energy than that of the σ-complex resulting from deuterium attack at C1. A better understanding of the t-butyl-catalyzed exchange could help in the design of labelling recipes for other phenolic metabolites. Copyright © 2016 The Authors. Journal of Labelled Compounds and Radiopharmaceuticals published by John Wiley & Sons, Ltd.

  8. A solid-phase extraction procedure coupled to 1H NMR, with chemometric analysis, to seek reliable markers of the botanical origin of honey

    International Nuclear Information System (INIS)

    Beretta, Giangiacomo; Caneva, Enrico; Regazzoni, Luca; Bakhtyari, Nazanin Golbamaki; Maffei Facino, Roberto

    2008-01-01

    The aim of this work was to establish an analytical method for identifying the botanical origin of honey, as an alternative to conventional melissopalynological, organoleptic and instrumental methods (gas-chromatography coupled to mass spectrometry (GC-MS), high-performance liquid chromatography HPLC). The procedure is based on the 1 H nuclear magnetic resonance (NMR) profile coupled, when necessary, with electrospray ionisation-mass spectrometry (ESI-MS) and two-dimensional NMR analyses of solid-phase extraction (SPE)-purified honey samples, followed by chemometric analyses. Extracts of 44 commercial Italian honeys from 20 different botanical sources were analyzed. Honeydew, chestnut and linden honeys showed constant, specific, well-resolved resonances, suitable for use as markers of origin. Honeydew honey contained the typical resonances of an aliphatic component, very likely deriving from the plant phloem sap or excreted into it by sap-sucking aphids. Chestnut honey contained the typical signals of kynurenic acid and some structurally related metabolite. In linden honey the 1 H NMR profile gave strong signals attributable to the mono-terpene derivative cyclohexa-1,3-diene-1-carboxylic acid (CDCA) and to its 1-O-β-gentiobiosyl ester (CDCA-GBE). These markers were not detectable in the other honeys, except for the less common nectar honey from rosa mosqueta. We compared and analyzed the data by multivariate techniques. Principal component analysis found different clusters of honeys based on the presence of these specific markers. The results, although obviously only preliminary, suggest that the 1 H NMR profile (with HPLC-MS analysis when necessary) can be used as a reference framework for identifying the botanical origin of honey

  9. A solid-phase extraction procedure coupled to {sup 1}H NMR, with chemometric analysis, to seek reliable markers of the botanical origin of honey

    Energy Technology Data Exchange (ETDEWEB)

    Beretta, Giangiacomo [Istituto di Chimica Farmaceutica e Tossicologica ' Pietro Pratesi' , Faculty of Pharmacy, University of Milan, via Mangiagalli 25, 20133 Milan (Italy)], E-mail: giangiacomo.beretta@unimi.it; Caneva, Enrico [Ciga - Centro Interdipartimentale Grandi Apparecchiature, University of Milan, via Golgi 19, 20133 Milan (Italy); Regazzoni, Luca; Bakhtyari, Nazanin Golbamaki; Maffei Facino, Roberto [Istituto di Chimica Farmaceutica e Tossicologica ' Pietro Pratesi' , Faculty of Pharmacy, University of Milan, via Mangiagalli 25, 20133 Milan (Italy)

    2008-07-14

    The aim of this work was to establish an analytical method for identifying the botanical origin of honey, as an alternative to conventional melissopalynological, organoleptic and instrumental methods (gas-chromatography coupled to mass spectrometry (GC-MS), high-performance liquid chromatography HPLC). The procedure is based on the {sup 1}H nuclear magnetic resonance (NMR) profile coupled, when necessary, with electrospray ionisation-mass spectrometry (ESI-MS) and two-dimensional NMR analyses of solid-phase extraction (SPE)-purified honey samples, followed by chemometric analyses. Extracts of 44 commercial Italian honeys from 20 different botanical sources were analyzed. Honeydew, chestnut and linden honeys showed constant, specific, well-resolved resonances, suitable for use as markers of origin. Honeydew honey contained the typical resonances of an aliphatic component, very likely deriving from the plant phloem sap or excreted into it by sap-sucking aphids. Chestnut honey contained the typical signals of kynurenic acid and some structurally related metabolite. In linden honey the {sup 1}H NMR profile gave strong signals attributable to the mono-terpene derivative cyclohexa-1,3-diene-1-carboxylic acid (CDCA) and to its 1-O-{beta}-gentiobiosyl ester (CDCA-GBE). These markers were not detectable in the other honeys, except for the less common nectar honey from rosa mosqueta. We compared and analyzed the data by multivariate techniques. Principal component analysis found different clusters of honeys based on the presence of these specific markers. The results, although obviously only preliminary, suggest that the {sup 1}H NMR profile (with HPLC-MS analysis when necessary) can be used as a reference framework for identifying the botanical origin of honey.

  10. Detailed analysis for a control rod worth of the gas turbine high temperature reactor (GTHTR300)

    Energy Technology Data Exchange (ETDEWEB)

    Nakata, Tetsuo; Katanishi, Shoji; Takada, Shoji; Yan, Xing; Kunitomi, Kazuhiko [Japan Atomic Energy Research Inst., Oarai, Ibaraki (Japan). Oarai Research Establishment

    2002-11-01

    GTHTR300 is composed of a simplified and economical power plant based on an inherent safe 600 MWt reactor and a nearly 50% high efficiency gas turbine power conversion cycle. GTHTR300 core consist of annular fuel region, center and outer side reflectors because of cooling it effectively in depressurized accident conditions, and all control rods are located in both side reflectors of annular core. As a thermal neutron spectrum is strongly distorted in reflector regions, an accurate calculation is especially required for the control rod worth evaluation. In this study, we applied the detailed Monte Carlo calculations of a full core model, and confirmed that our design method has enough accuracy. (author)

  11. Dynamical twisted mass fermions with light quarks. Simulation and analysis details

    International Nuclear Information System (INIS)

    Boucaud, P.; Dimopoulos, P.; Farchioni, F.

    2008-03-01

    In a recent paper (2007) we presented precise lattice QCD results of our European Twisted Mass Collaboration (ETMC). They were obtained by employing two mass-degenerate flavours of twisted mass fermions at maximal twist. In the present paper we give details on our simulations and the computation of physical observables. In particular, we discuss the problem of tuning to maximal twist, the techniques we have used to compute correlators and error estimates. In addition, we provide more information on the algorithm used, the autocorrelation times and scale determination, the evaluation of disconnected contributions and the description of our data by means of chiral perturbation theory formulae. (orig.)

  12. Dynamical twisted mass fermions with light quarks. Simulation and analysis details

    Energy Technology Data Exchange (ETDEWEB)

    Boucaud, P. [Paris-11 Univ., 91 - Orsay (France). Lab. de Physique Theorique; Dimopoulos, P. [Rome-2 Univ. (Italy). Dipt. di Fisica; Farchioni, F. [Muenster Univ. (DE). Inst. fuer Theoretische Physik] (and others)

    2008-03-15

    In a recent paper (2007) we presented precise lattice QCD results of our European Twisted Mass Collaboration (ETMC). They were obtained by employing two mass-degenerate flavours of twisted mass fermions at maximal twist. In the present paper we give details on our simulations and the computation of physical observables. In particular, we discuss the problem of tuning to maximal twist, the techniques we have used to compute correlators and error estimates. In addition, we provide more information on the algorithm used, the autocorrelation times and scale determination, the evaluation of disconnected contributions and the description of our data by means of chiral perturbation theory formulae. (orig.)

  13. Author Details

    African Journals Online (AJOL)

    Petrology of the Cenomanian Upper Member of the Mamfe Embayment, southwestern Cameroon Details · Vol 38, No 1 (2002) - Articles Sequence stratigraphy of Iso field, western onshore Niger Delta, Nigeria Details · Vol 39, No 2 (2003) - Articles Preliminary studies on the lithostratigraphy and depositional environment of ...

  14. Author Details

    African Journals Online (AJOL)

    An Overview of Africa's Marine Resources: Their Utilization and Sustainable Management Details · Vol 12, No 3 (2000) - Articles EDITORIAL Ganoderma Lucidum - Paramount among Medicinal Mushrooms. Details · Vol 15, No 3 (2003) - Articles Editorial: Africa's Mushrooms: A neglected bioresource whose time has come

  15. Author Details

    African Journals Online (AJOL)

    Author Details. Journal Home > Advanced Search > Author Details. Log in or Register to get access to full text downloads. ... Abstract PDF · Vol 3, No 6 (2011) - Articles Mixed convection flow and heat transfer in a vertical wavy channel containing porous and fluid layer with traveling thermal waves. Abstract PDF · Vol 3, No 8 ...

  16. Author Details

    African Journals Online (AJOL)

    Author Details. Journal Home > Advanced Search > Author Details. Log in or Register to get access to full text downloads. ... Singh, J. Vol 3, No 2 (2011) - Articles Plane waves in a rotating generalized thermo-elastic solid with voids. Abstract PDF. ISSN: 2141-2839. AJOL African Journals Online. HOW TO USE AJOL.

  17. Author Details

    African Journals Online (AJOL)

    Author Details. Journal Home > Advanced Search > Author Details. Log in or Register to get access to full text downloads. ... Vol 12 (2008) - Articles On the wave equations of shallow water with rough bottom topography. Abstract · Vol 14 (2009) - Articles Energy generation in a plant due to variable sunlight intensity

  18. Author Details

    African Journals Online (AJOL)

    Author Details. Journal Home > Advanced Search > Author Details. Log in or Register to get access to full text downloads. ... Iliopsoas haematoma in a rugby player. Abstract PDF · Vol 29, No 1 (2017) - Articles The use of negative pressure wave treatment in athlete recovery. Abstract PDF. ISSN: 2078-516X. AJOL African ...

  19. Author Details

    African Journals Online (AJOL)

    Author Details. Journal Home > Advanced Search > Author Details. Log in or Register to get access to full text downloads. ... Ismail, A. Vol 9, No 3S (2017): Special Issue - Articles Investigate of wave absorption performance for oil palm frond and empty fruit bunch at 5.8 GHz. Abstract PDF · Vol 9, No 3S (2017): Special Issue ...

  20. Author Details

    African Journals Online (AJOL)

    Author Details. Journal Home > Advanced Search > Author Details. Log in or Register to get access to full text downloads. ... Isa, M.F.M.. Vol 9, No 3S (2017): Special Issue - Articles Experimental and numerical investigation on blast wave propagation in soil structure. Abstract PDF · Vol 9, No 3S (2017): Special Issue - ...

  1. Author Details

    African Journals Online (AJOL)

    Author Details. Journal Home > Advanced Search > Author Details. Log in or Register to get access to full text downloads. ... No 3S (2017): Special Issue - Articles Experimental and numerical investigation on blast wave propagation in soil structure. Abstract PDF · Vol 9, No 3S (2017): Special Issue - Articles Simulation on ...

  2. Author Details

    African Journals Online (AJOL)

    Author Details. Journal Home > Advanced Search > Author Details. Log in or Register to get access to full text downloads. ... Duwa, S S. Vol 8 (2004) - Articles Lower hybrid waves instability in a velocity–sheared inhomogenous charged dust beam. Abstract · Vol 9 (2005) - Articles The slide away theory of lower hybrid bursts

  3. Author Details

    African Journals Online (AJOL)

    Author Details. Journal Home > Advanced Search > Author Details. Log in or Register to get access to full text downloads. ... Vol 45 (2016) - Articles From vectors to waves and streams: An alternative approach to semantic maps1. Abstract PDF · Vol 48 (2017) - Articles Introduction: 'n Klein ietsie for Johan Oosthuizen

  4. Author Details

    African Journals Online (AJOL)

    Author Details. Journal Home > Advanced Search > Author Details. Log in or Register to get access to full text downloads. ... to blast loadings. Abstract PDF · Vol 9, No 3S (2017): Special Issue - Articles Experimental and numerical investigation on blast wave propagation in soil structure. Abstract PDF. ISSN: 1112-9867.

  5. Author Details

    African Journals Online (AJOL)

    Author Details. Journal Home > Advanced Search > Author Details. Log in or Register to get access to full text downloads. ... The use of negative pressure wave treatment in athlete recovery. Abstract PDF · Vol 29, No 1 (2017) - Articles The prevalence, risk factors predicting injury and the severity of injuries sustained during ...

  6. Author Details

    African Journals Online (AJOL)

    Author Details. Journal Home > Advanced Search > Author Details. Log in or Register to get access to full text downloads. ... Vol 29, No 1 (2017) - Articles The use of negative pressure wave treatment in athlete recovery. Abstract PDF · Vol 29, No 1 (2017) - Articles The prevalence, risk factors predicting injury and the ...

  7. NMR imaging of the brain: initial impressions

    International Nuclear Information System (INIS)

    Spencer, D.H.; Bydder, G.M.

    1983-01-01

    An NMR imaging system designed and built by Thorn-EMI Ltd was installed at Hammersmith Hospital in March 1981. In the first year of operation 180 patients and 40 volunteers have had cranial examinations and initial impressions bases on this experience are presented. Patients with a wide variety of neurological diseases have been studied to provide a basis for diagnostic interpretation, to define distinctive features, and to evaluate different types of scanning sequences. NMR imaging appears to be of considerable value in neurological diagnosis and has a number of advantages over CT. The detailed evaluation of NMR imaging will require much more work but the initial results are very promising

  8. Introduction to some basic aspects of NMR

    International Nuclear Information System (INIS)

    Goldman, M.

    1992-01-01

    The principal interactions are reviewed that are experienced by nuclear spins making magnetic resonance feasible and which disturb it in a way that gives access to the properties of bulk matter. The interactions leading to NMR include Zeeman interaction, dipole-dipole interactions, and exchange interactions. Spin-lattice relaxation relevant to NMR is revisited next. It is followed by an overview of spin temperature. Finally, the care of periodic Hamiltonian is discussed in detail as another contribution to NMR. (R.P.) 48 refs., 12 figs

  9. High resolution NMR spectroscopy of synthetic polymers in bulk

    International Nuclear Information System (INIS)

    Komorski, R.A.

    1986-01-01

    The contents of this book are: Overview of high-resolution NMR of solid polymers; High-resolution NMR of glassy amorphous polymers; Carbon-13 solid-state NMR of semicrystalline polymers; Conformational analysis of polymers of solid-state NMR; High-resolution NMR studies of oriented polymers; High-resolution solid-state NMR of protons in polymers; and Deuterium NMR of solid polymers. This work brings together the various approaches for high-resolution NMR studies of bulk polymers into one volume. Heavy emphasis is, of course, given to 13C NMR studies both above and below Tg. Standard high-power pulse and wide-line techniques are not covered

  10. Supra-molecular structure of TGBC* phases studied by means of Deuterium NMR line-shape analysis

    Czech Academy of Sciences Publication Activity Database

    Domenici, V.; Veracini, C.A.; Hamplová, Věra; Kašpar, Miroslav

    2008-01-01

    Roč. 495, č. 11 (2008), s. 133-144 ISSN 1542-1406 Institutional research plan: CEZ:AV0Z10100520 Keywords : banana -shaped * deuterium NMR * magnetic field * rod-like * smectic * twist grain boundary Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.537, year: 2008

  11. Synthesis of deuterium-labeled plant sterols and analysis of their side-chain mobility by solid state deuterium NMR

    International Nuclear Information System (INIS)

    Marsan, M.P.; Muller, I.; Milon, A.

    1996-01-01

    Sitosterol and stigmasterol, plant sterols, were deuterated at specific positions. Orientation and mobility of the deuterated sitosterol and stigmasterol (and two of their diasteromers) on oriented lipid bilayers were analyzed by deuterium NMR spectroscopy. Orientation and mobility of the side chains was revealed by these studies

  12. FTIR, FT-RAMAN, NMR, spectra, normal co-ordinate analysis, NBO, NLO and DFT calculation of N,N-diethyl-4-methylpiperazine-1-carboxamide molecule.

    Science.gov (United States)

    Muthu, S; Elamurugu Porchelvi, E

    2013-11-01

    The Fourier Transform Infrared (FT-IR) and FT-Raman of N,N-diethyl-4-methylpiperazine-1-carboxamide (NND4MC) have been recorded and analyzed. The structure of the compound was optimized and the structural characteristics were determined by density functional theory (DFT) using B3LYP method with 6-31G(d,p) and 6-311G(d,p) basis sets. The difference between the observed and scaled wavenumber values of most of the fundamentals is very small. The theoretically predicted FT-IR and FT-Raman spectra of the title molecule have been constructed. The detailed interpretation of the vibrational spectra has been carried out with aid of normal coordinate analysis (NCA) following the scaled quantum mechanical force field methodology. Stability of the molecule arising from hyperconjugative interactions and charge delocalization has been analyzed using natural bond orbital (NBO) analysis. The results show that electron density (ED) in the σ(*) and π(*) antibonding orbitals and second order delocalization energies (E2) confirm the occurrence of intramolecular charge transfer (ICT) within the molecule. The electronic dipole moment (μD) and the first hyperpolarizability (βtot) values of the investigated molecule were computed using Density Functional Theory (DFT/B3LYP) with 6-31G(d,p) and 6-311G(d,p) basis sets. The calculated results also show that the NND4MC molecule may have microscopy nonlinear optical (NLO) behavior with non zero values. Mulliken atomic charges of NND4MC were calculated. The (13)C nuclear magnetic resonance (NMR) chemical shifts of the molecule were calculated by the gauge independent atomic orbital (GIAO) method and compared with experimental results. The UV-Vis spectrum of the compound was recorded. The theoretical electronic absorption spectra have been calculated by using CIS, TD-DFT methods. A study on the electronic properties, such as HOMO and LUMO energies, molecular electrostatic potential (MEP) were also performed. Copyright © 2013 Elsevier B

  13. Light water reactor fuel analysis code FEMAXI-IV(Ver.2). Detailed structure and user`s manual

    Energy Technology Data Exchange (ETDEWEB)

    Suzuki, Motoe [Japan Atomic Energy Research Inst., Tokai, Ibaraki (Japan). Tokai Research Establishment; Saitou, Hiroaki

    1997-11-01

    A light water reactor fuel behavior analysis code FEMAXI-IV(Ver.2) was developed as an improved version of FEMAXI-IV. Development of FEMAXI-IV has been already finished in 1992, though a detailed structure and input manual of the code have not been open to users yet. Here, the basic theories and structure, the models and numerical solutions applied to FEMAXI-IV(Ver.2), and the material properties adopted in the code are described in detail. In FEMAXI-IV(Ver.2), programming bugs in previous FEMAXI-IV were eliminated, renewal of the pellet thermal conductivity was performed, and a model of thermal-stress restraint on FP gas release was incorporated. For facilitation of effective and wide-ranging application of the code, methods of input/output of the code are also described in detail, and sample output is included. (author)

  14. Characterization of natural bentonite by NMR

    International Nuclear Information System (INIS)

    Leite, Sidnei Q.M.; Dieguez, Lidia C.; Menezes, Sonia M.C.; San Gil, Rosane A.S.

    1993-01-01

    Solid state NMR as well as several other instrumental chemical analysis techniques were used in order to characterize two natural occurring bentonite. The methodology is described. The NMR spectra, together with the other used techniques suggest that the observed differences are due to iron inclusions in tetrahedral and octahedral sites

  15. Synthesis and NMR Elucidation of Novel Pentacycloundecane ...

    African Journals Online (AJOL)

    Herein we report the synthesis and NMR elucidation of five novel pentacycloundecane (PCU)-derived short peptides as potential HIV protease inhibitors. 1H and 13C spectral analysis show major overlapping of methine resonance of the PCU 'cage' thereby making it extremely difficult to assign the NMR signals. Attachment ...

  16. Development and applications of quantitative NMR spectroscopy

    International Nuclear Information System (INIS)

    Yamazaki, Taichi

    2016-01-01

    Recently, quantitative NMR spectroscopy has attracted attention as an analytical method which can easily secure traceability to SI unit system, and discussions about its accuracy and inaccuracy are also started. This paper focuses on the literatures on the advancement of quantitative NMR spectroscopy reported between 2009 and 2016, and introduces both NMR measurement conditions and actual analysis cases in quantitative NMR. The quantitative NMR spectroscopy using an internal reference method enables accurate quantitative analysis with a quick and versatile way in general, and it is possible to obtain the precision sufficiently applicable to the evaluation of pure substances and standard solutions. Since the external reference method can easily prevent contamination to samples and the collection of samples, there are many reported cases related to the quantitative analysis of biologically related samples and highly scarce natural products in which NMR spectra are complicated. In the precision of quantitative NMR spectroscopy, the internal reference method is superior. As the quantitative NMR spectroscopy widely spreads, discussions are also progressing on how to utilize this analytical method as the official methods in various countries around the world. In Japan, this method is listed in the Pharmacopoeia and Japanese Standard of Food Additives, and it is also used as the official method for purity evaluation. In the future, this method will be expected to spread as the general-purpose analysis method that can ensure traceability to SI unit system. (A.O.)

  17. An analysis of the NMR-CT image by the measurement of proton-relaxation times in tissue

    International Nuclear Information System (INIS)

    Naruse, Shoji; Horikawa, Yoshiharu; Tanaka, Chuzo; Hirakawa, Kimiyoshi; Nishikawa, Hiroyasu; Shimizu, Koji; Kiri, Motosada.

    1984-01-01

    NMR-CT images were analyzed by measuring the proton-relaxation times in tissues. The NMR-CT images were obtained in 10 normal volunteers and 16 patients with brain tumors with a prototype superconducting magnet (Shimadzu Corp., Japan) operating at 0.2 T and 0.375 T. A smooth T 1 relaxation curve was obtained in each part of the brain and the brain tumor by the use of the data of the NMR-CT image; consequently, the in vivo T 1 value was proved to be reliable. The in vivo T 1 value showed the specific value corresponding to each region of the normal brain in all cases. Cerebral gray matter normally had the longest T 1 value, followed by the medulla oblongata, the pons, and white matter. The T 1 value of each region of the brain varied to the same degree in proportion to the strength of the static magnetic field. The in vivo T 1 values of the brain tumor varied with the histological type. All were longer than any part of the brain parenchyma, being between 480 and 780 msec at 0.2 T. The prolongation of the T 1 value does not always correspond to the degree of the malignancy in a tumor. The in vitro T 1 and T 2 values were also prolonged in all tumors. Although the absolute value of T 1 did not coincide between the in vitro and in vivo data, the tendency of the prolongation was the same between them. This result indicated that the NMR-CT images could be analysed by the use of the data of the in vitro T 1 and T 2 values in the tumor tissues. It is important to analyse the NMR-CT image by both in vivo and in vitro examinations of the relaxation times. (J.P.N.)

  18. An in-depth analysis of the biological functional studies based on the NMR M2 channel structure of influenza A virus

    International Nuclear Information System (INIS)

    Huang Ribo; Du Qishi; Wang Chenghua; Chou, K.-C.

    2008-01-01

    The long-sought three-dimensional structure of the M2 proton channel of influenza A virus was successfully determined recently by the high-resolution NMR [J.R. Schnell, J.J. Chou, Structure and mechanism of the M2 proton channel of influenza A virus, Nature 451 (2008) 591-595]. Such a milestone work has provided a solid structural basis for studying drug-resistance problems. However, the action mechanism revealed from the NMR structure is completely different from the traditional view and hence prone to be misinterpreted as 'conflicting' with some previous biological functional studies. To clarify this kind of confusion, an in-depth analysis was performed for these functional studies, particularly for the mutations D44N, D44A and N44D on position 44, and the mutations on positions 27-38. The analyzed results have provided not only compelling evidences to further validate the NMR structure but also very useful clues for dealing with the drug-resistance problems and developing new effective drugs against H5N1 avian influenza virus, an impending threat to human beings.

  19. Confirmatory analysis and detail design of the magnet system for mirror fusion test facility (MFTF)

    International Nuclear Information System (INIS)

    Tatro, R.E.; Baldi, R.W.

    1978-10-01

    This summary covers the six individual reports delivered to the LLL MFTF program staff. They are: (1) literature survey (helium heat transfer), (2) thermodynamic analysis, (3) structural analysis, (4) manufacturing/producibility study, (5) instrumentation plan and (6) quality assurance report

  20. CoMA, an experiment for the detailed in-situ analysis of collected cometary particulates

    International Nuclear Information System (INIS)

    Kissel, J.; Fechtig, H.; Jessberger, E.K.; Krueger, F.R.; Niemczyk, N.; Schaefer, G.; Zscheeg, H.

    1989-01-01

    After NASA accepted for the implementation phase (up to October 1990) our proposal for the CoMA investigation to be flown onboard CRAF to rendezvous with a comet, funding by the BMFT for instrument pre-development has been obtained. Most contracts could be let, some, however, with substantial delay due to administrative problems. Progress can be reported as the group in Bremen could demonstrate a mass resolution of 60 000 for a low magnetic field ICR-experiment, resolving 12 CH + and 13 C + ions. Also a first successful attempt was made to theoretically describe the dust collection efficiencies of different materials. As yet such a model did not exist - a fact that made the interpretation and extrapolation of laboratory data obsolete. The experimental setup in which the Indium liquid ion source is tested could be completed by the successful addition of a bunching structure. In future it will serve those partners that develop in detail the primary beam system. (orig.)

  1. New SUSYQM coherent states for Pöschl-Teller potentials: a detailed mathematical analysis

    Science.gov (United States)

    Bergeron, H.; Siegl, P.; Youssef, A.

    2012-06-01

    In a recent short note (Bergeron et al 2010 Europhys. Lett. 92 60003), we have presented the good properties of a new family of semi-classical states for Pöschl-Teller potentials. These states are built from a supersymmetric quantum mechanics (SUSYQM) approach and the parameters of these ‘coherent’ states are points in the classical phase space. In this paper, we develop all the mathematical aspects that have been left out of the previous paper (proof of the resolution of unity, detailed calculations of the quantized version of classical observables and mathematical study of the resulting operators: problems of domains, self-adjointness or self-adjoint extensions). Some additional questions such as asymptotic behavior are also studied. Moreover, the framework is extended to a larger class of Pöschl-Teller potentials. This article is part of a special issue of Journal of Physics A: Mathematical and Theoretical devoted to ‘Coherent states: mathematical and physical aspects’.

  2. Detailed analysis of coolant mixing in WWER-440 fuel assembly heads

    International Nuclear Information System (INIS)

    Toth, S.; Aszodi, A.

    2008-01-01

    Based on experiences of former validation and sensitivity studies, a CFD model for head part of real working fuel assemblies with pitch of 12.3 mm has been developed with the code ANSYS CFX. Calculations were performed for typical fuel assemblies used in the Paks NPP. Differences between the outlet average temperatures and thermocouple signals were determined. Effect of the mixing grid position on thermocouple signal was investigated also. Mixing was analyzed in details with using so-called mixing scalars and weight factors of the central tube and rod bundle regions for in-core thermocouple signal were determined. Sensitivity of the weight factors for pin power distribution and mixing grid position were investigated. (Authors)

  3. NMR of lignins

    Science.gov (United States)

    John Ralph; Larry L. Landucci

    2010-01-01

    This chapter will consider the basic aspects and findings of several forms of NMR spectroscopy, including separate discussions of proton, carbon, heteronuclear, and multidimensional NMR. Enhanced focus will be on 13C NMR, because of its qualitative and quantitative importance, followed by NMR’s contributions to our understanding of lignin...

  4. An improved synthesis, spectroscopic (FT-IR, NMR) study and DFT computational analysis (IR, NMR, UV-Vis, MEP diagrams, NBO, NLO, FMO) of the 1,5-methanoazocino[4,3-b]indole core structure

    Science.gov (United States)

    Uludağ, Nesimi; Serdaroğlu, Goncagül

    2018-03-01

    This study examines the synthesis of azocino[4,3-b]indole structure, which constitutes the tetracyclic framework of uleine, dasycarpidoneand tubifolidineas well as ABDE substructure of the strychnosalkaloid family. It has been synthesized by Fischer indolization of 2 and through the cylization of 4 by 2,3-dichlor-5-6-dicyanobenzoquinone (DDQ). 1H and 1C NMR chemical shifts have been predicted with GIAO approach and the calculated chemical shifts show very good agreement with observed shifts. FT-IR spectroscopy is important for the analysis of functional groups of synthesized compounds and we also supported FT-IR vibrational analysis with computational IR analysis. The vibrational spectral analysis was performed at B3LYP level of the theory in both the gas and the water phases and it was compared with the observed IR values for the important functional groups. The DFT calculations have been conducted to determine the most stable structure of the 1,2,3,4,5,6,7-Hexahydro-1,5-methanoazocino [4,3-b] indole (5). The Frontier Molecular Orbital Analysis, quantum chemical parameters, physicochemical properties have been predicted by using the same theory of level in both gas phase and the water phase, at 631 + g** and 6311++g** basis sets. TD- DFT calculations have been performed to predict the UV- Vis spectral analysis for this synthesized molecule. The Natural Bond Orbital (NBO) analysis have been performed at B3LYP level of theory to elucidate the intra-molecular interactions such as electron delocalization and conjugative interactions. NLO calculations were conducted to obtain the electric dipole moment and polarizability of the title compound.

  5. Author Details

    African Journals Online (AJOL)

    Journal Home > Advanced Search > Author Details. Log in or Register ... (2013) - Articles Technical Note: Development of a Photobioreactor for Microalgae Culture ... Design, Construction and Evaluation of Motorized Okra Slicer Abstract PDF ...

  6. Author Details

    African Journals Online (AJOL)

    Journal Home > Advanced Search > Author Details. Log in or Register to ... No 1 (2014) - Articles Knowledge and Attitudes towards Basic Cardiopulmonary Resuscitation (CPR) among Community Nurses in Remo Area of Ogun State, Nigeria

  7. Author Details

    African Journals Online (AJOL)

    Journal Home > Advanced Search > Author Details. Log in or Register to get ... Optical bus of centralized relay protection and automation system of medium voltage switchgear for data collection and transmission. Abstract PDF. ISSN: 1112- ...

  8. Author Details

    African Journals Online (AJOL)

    Journal Home > Advanced Search > Author Details. Log in or ... The prevention of mother-to-child HIV transmission programme and infant feeding practices ... Evaluation of a diagnostic algorithm for smear-negative pulmonary tuberculosis in ...

  9. Author Details

    African Journals Online (AJOL)

    Journal Home > Advanced Search > Author Details ... Design and Implementation of an M/M/1 Queuing Model Algorithm and its Applicability in ... Vehicle Identification Technology to Intercept Small Arms and Ammunition on Nigeria Roads

  10. CFD analysis of municipal solid waste combustion using detailed chemical kinetic modelling.

    Science.gov (United States)

    Frank, Alex; Castaldi, Marco J

    2014-08-01

    Nitrogen oxides (NO x ) emissions from the combustion of municipal solid waste (MSW) in waste-to-energy (WtE) facilities are receiving renewed attention to reduce their output further. While NO x emissions are currently 60% below allowed limits, further reductions will decrease the air pollution control (APC) system burden and reduce consumption of NH3. This work combines the incorporation of the GRI 3.0 mechanism as a detailed chemical kinetic model (DCKM) into a custom three-dimensional (3D) computational fluid dynamics (CFD) model fully to understand the NO x chemistry in the above-bed burnout zones. Specifically, thermal, prompt and fuel NO formation mechanisms were evaluated for the system and a parametric study was utilized to determine the effect of varying fuel nitrogen conversion intermediates between HCN, NH3 and NO directly. Simulation results indicate that the fuel nitrogen mechanism accounts for 92% of the total NO produced in the system with thermal and prompt mechanisms accounting for the remaining 8%. Results also show a 5% variation in final NO concentration between HCN and NH3 inlet conditions, demonstrating that the fuel nitrogen intermediate assumed is not significant. Furthermore, the conversion ratio of fuel nitrogen to NO was 0.33, revealing that the majority of fuel nitrogen forms N2. © The Author(s) 2014.

  11. A detailed cost analysis of in vitro fertilization and intracytoplasmic sperm injection treatment.

    Science.gov (United States)

    Bouwmans, Clazien A M; Lintsen, Bea M E; Eijkemans, Marinus J C; Habbema, J Dik F; Braat, Didi D M; Hakkaart, Leona

    2008-02-01

    To provide detailed information about costs of in vitro fertilization (IVF) and intracytoplasmic sperm injection (ICSI) treatment stages and to estimate the cost per IVF and ICSI treatment cycle and ongoing pregnancy. Descriptive micro-costing study. Four Dutch IVF centers. Women undergoing their first treatment cycle with IVF or ICSI. IVF or ICSI. Costs per treatment stage, per cycle started, and for ongoing pregnancy. Average costs of IVF and ICSI hormonal stimulation were euro 1630 and euro 1585; the costs of oocyte retrieval were euro 500 and euro 725, respectively. The cost of embryo transfer was euro 185. Costs per IVF and ICSI cycle started were euro 2381 and euro 2578, respectively. Costs per ongoing pregnancy were euro 10,482 and euro 10,036, respectively. Hormonal stimulation covered the main part of the costs per cycle (on average 68% and 61% for IVF and ICSI, respectively) due to the relatively high cost of medication. The costs of medication increased with increasing age of the women, irrespective of the type of treatment (IVF or ICSI). Fertilization costs (IVF laboratory) constituted 12% and 20% of the total costs of IVF and ICSI. The total cost per ICSI cycle was 8.3% higher than IVF.

  12. Preliminary evaluation of crisis-relocation fallout-shelter options. Volume 2. Detailed analysis

    International Nuclear Information System (INIS)

    Santini, D.J.; Clinch, J.M.; Davis, F.H.; Hill, L.G.; Lynch, E.P.; Tanzman, E.A.; Wernette, D.R.

    1982-12-01

    This report presents a preliminary, detailed evaluation of various shelter options for use if the President orders crisis relocation of the US urban population because of strong expectation of a nuclear war. The availability of livable shelter space at 40 ft 2 per person (congregate-care space) by state is evaluated. Options are evaluated for construction of fallout shelters allowing 10 ft 2 per person - such shelters are designed to provide 100% survival at projected levels of radioactive fallout. The FEMA concept of upgrading existing buildings to act as fallout shelters can, in principle, provide adequate shelter throughout most of the US. Exceptions are noted and remedies proposed. In terms of upgrading existing buildings to fallout shelter status, great benefits are possible by turning away from a standard national approach and adopting a more site-specific approach. Existing FEMA research provides a solid foundation for successful crisis relocation planning, but the program can be refined by making suitable modifications in its locational, engineering, and institutionally specific elements

  13. Detailed seismotectonic analysis of Sumatra subduction zone revealed by high precision earthquake location

    Science.gov (United States)

    Sagala, Ricardo Alfencius; Harjadi, P. J. Prih; Heryandoko, Nova; Sianipar, Dimas

    2017-07-01

    Sumatra was one of the most high seismicity regions in Indonesia. The subduction of Indo-Australian plate beneath Eurasian plate in western Sumatra contributes for many significant earthquakes that occur in this area. These earthquake events can be used to analyze the seismotectonic of Sumatra subduction zone and its system. In this study we use teleseismic double-difference method to obtain more high precision earthquake distribution in Sumatra subduction zone. We use a 3D nested regional-global velocity model. We use a combination of data from both of ISC (International Seismological Center) and BMKG (Agency for Meteorology Climatology and Geophysics, Indonesia). We successfully relocate about 6886 earthquakes that occur on period of 1981-2015. We consider that this new location is more precise than the regular bulletin. The relocation results show greatly reduced of RMS residual of travel time. Using this data, we can construct a new seismotectonic map of Sumatra. A well-built geometry of subduction slab, faults and volcano arc can be obtained from the new bulletin. It is also showed that at a depth of 140-170 km, there is many events occur as moderate-to-deep earthquakes, and we consider about the relation of the slab's events with volcanic arc and inland fault system. A reliable slab model is also built from regression equation using new relocated data. We also analyze the spatial-temporal of seismotectonic using b-value mapping that inspected in detail horizontally and vertically cross-section.

  14. Preliminary evaluation of crisis-relocation fallout-shelter options. Volume 2. Detailed analysis

    Energy Technology Data Exchange (ETDEWEB)

    Santini, D.J.; Clinch, J.M.; Davis, F.H.; Hill, L.G.; Lynch, E.P.; Tanzman, E.A.; Wernette, D.R.

    1982-12-01

    This report presents a preliminary, detailed evaluation of various shelter options for use if the President orders crisis relocation of the US urban population because of strong expectation of a nuclear war. The availability of livable shelter space at 40 ft/sup 2/ per person (congregate-care space) by state is evaluated. Options are evaluated for construction of fallout shelters allowing 10 ft/sup 2/ per person - such shelters are designed to provide 100% survival at projected levels of radioactive fallout. The FEMA concept of upgrading existing buildings to act as fallout shelters can, in principle, provide adequate shelter throughout most of the US. Exceptions are noted and remedies proposed. In terms of upgrading existing buildings to fallout shelter status, great benefits are possible by turning away from a standard national approach and adopting a more site-specific approach. Existing FEMA research provides a solid foundation for successful crisis relocation planning, but the program can be refined by making suitable modifications in its locational, engineering, and institutionally specific elements.

  15. New SUSYQM coherent states for Pöschl–Teller potentials: a detailed mathematical analysis

    International Nuclear Information System (INIS)

    Bergeron, H; Siegl, P; Youssef, A

    2012-01-01

    In a recent short note (Bergeron et al 2010 Europhys. Lett. 92 60003), we have presented the good properties of a new family of semi-classical states for Pöschl–Teller potentials. These states are built from a supersymmetric quantum mechanics (SUSYQM) approach and the parameters of these ‘coherent’ states are points in the classical phase space. In this paper, we develop all the mathematical aspects that have been left out of the previous paper (proof of the resolution of unity, detailed calculations of the quantized version of classical observables and mathematical study of the resulting operators: problems of domains, self-adjointness or self-adjoint extensions). Some additional questions such as asymptotic behavior are also studied. Moreover, the framework is extended to a larger class of Pöschl–Teller potentials. This article is part of a special issue of Journal of Physics A: Mathematical and Theoretical devoted to ‘Coherent states: mathematical and physical aspects’. (paper)

  16. A detailed analysis of adhesion mechanics between a compliant elastic coating and a spherical probe

    International Nuclear Information System (INIS)

    Sridhar, I; Zheng, Z W; Johnson, K L

    2004-01-01

    As length scales decrease, adhesive forces become increasingly important. These adhesive forces contribute to the normal load in experiments conducted on thin layered systems using micro-probe instruments such as the surface force apparatus (SFA) and the atomic force microscope (AFM). Adhesion between these thin-layer systems was analysed by Sridhar et al (1997 J. Phys. D: Appl. Phys. 30 1710) for the SFA geometry and Johnson and Sridhar (2001 J. Phys. D: Appl. Phys. 34 683) for AFM using a numerical SJF (Sridhar-Johnson-Fleck) version of the JKR (Johnson-Kendal-Roberts) theory. In this paper, adhesion mechanics between a compliant elastic coating and a spherical probe is investigated using the SJF model in detail. When the substrate is rigid, the non-dimensional pull-off force may differ from the JKR value of -0.5 by as much as 90%. Computations of the contact size at zero load and pull-off force are presented for a range of values of adhesion energy. Finally, empirical relations for the contact load and contact compliance as a function of contact radius were obtained from the numerical data for practical layer-substrate material systems

  17. Detailed analysis of the resonant backscattering spectrum for deeply penetrating protons in carbon

    International Nuclear Information System (INIS)

    Tosaki, Mitsuo; Ito, Shin; Maeda, Nobuhiro

    2000-01-01

    In order to study the spectral response in Rutherford backscattering spectroscopy (RBS) for deeply penetrating ions in matter, the resonant backscattering spectra for 5.05-, 5.5- and 6.0-MeV proton incidence on solid carbon material have been measured at a scattering angle of 179.2 deg. (in lab.). Prominent peaks resulting from the sharp 4.8-MeV resonance in 12 C(p,p) 12 C nuclear elastic scattering are observed, even for a penetration depth of 79 μm. Detailed numerical calculations based on an algorithm of straightforward step-by-step evaluation have been made to simulate the observed spectra. The algorithm enables one to rigorously treat both the effect of sharp resonance structure and that of energy-dependent energy loss. Calculations with the SIMNRA code are also made. Through comparison of these calculations with the measured results, some conclusions on the two effects above are presented. In addition, it is demonstrated that the peak profile due to a sharp resonance is very sensitive to the degree of energy straggling

  18. Detailed analysis of polybrominated biphenyl congeners in bird eggs from Norway

    International Nuclear Information System (INIS)

    Vetter, Walter; Recke, Roland von der; Herzke, Dorte; Nygard, Torgeir

    2008-01-01

    Individual eggs of six species of birds from Norway representing different food chains were analysed for residues of polybrominated biphenyls (PBBs). In all species, the residue pattern was dominated by hexaBBs. The dominating congeners were PBB 153, PBB 154, and PBB 155. Whereas PBB 153 is present in technical hexabromobiphenyl, PBB 154 and PBB 155 are formed by the reductive debromination of decabromobiphenyl. This was evidenced by the detection of several heptaBBs and octaBBs all of which are typical degradation intermediates of PBB 209. Hepta- and octaBBs were more than one order of magnitude less abundant than the hexaBBs. The second most prevailing homologue group was pentaBBs. The most relevant pentabrominated isomers were PBB 99 and PBB 101. Concentrations of the three hexaBBs - PBB 153, PBB 154, and PBB 155 - amounted to 1.3-13 ng/g wet weight or 3-23% of the contamination with polybrominated diphenyl ethers. - We provide for the first time detailed information on the PBB congeners present in eggs of bird of prey, and quantified three hexabromo congeners

  19. Detailed analysis of the blade root flow of a horizontal axis wind turbine

    Directory of Open Access Journals (Sweden)

    I. Herráez

    2016-07-01

    Full Text Available The root flow of wind turbine blades is subjected to complex physical mechanisms that influence significantly the rotor aerodynamic performance. Spanwise flows, the Himmelskamp effect, and the formation of the root vortex are examples of interrelated aerodynamic phenomena that take place in the blade root region. In this study we address those phenomena by means of particle image velocimetry (PIV measurements and Reynolds-averaged Navier–Stokes (RANS simulations. The numerical results obtained in this study are in very good agreement with the experiments and unveil the details of the intricate root flow. The Himmelskamp effect is shown to delay the stall onset and to enhance the lift force coefficient Cl even at moderate angles of attack. This improvement in the aerodynamic performance occurs in spite of the negative influence of the mentioned effect on the suction peak of the involved blade sections. The results also show that the vortex emanating from the spanwise position of maximum chord length rotates in the opposite direction to the root vortex, which affects the wake evolution. Furthermore, the aerodynamic losses in the root region are demonstrated to take place much more gradually than at the tip.

  20. NMR studies of stock process water and reaction pathways in hydrothermal carbonization of furfural residue

    Directory of Open Access Journals (Sweden)

    Fen Yue

    2018-04-01

    Full Text Available Hydrothermal carbonization (HTC is a valuable approach to convert furfural residue (FR into carbon material. The prepared biochars are usually characterized comprehensively, while the stock process water still remains to be studied in detail. Herein, a NMR study of the main components in stock process water generated at different HTC reaction conditions was reported. Various qualitative and quantitative NMR techniques (1H and 13C NMR, 1H–1H COSY and 1H13C HSQC etc. especially 1D selective gradient total correlation spectroscopy (TOCSY NMR were strategically applied in the analysis of HTC stock process water. Without separation and purification, it was demonstrated that the main detectable compounds are 5-hydroxymethylfurfural, formic acid, methanol, acetic acid, levulinic acid, glycerol, hydroxyacetone and acetaldehyde in this complicate mixture. Furthermore, the relationship between the concentration of major products and the reaction conditions (180–240 °C at 8 h, and 1–24 h at 240 °C was established. Finally, reasonable reaction pathways for hydrothermal conversion of FR were proposed based on this result and our previously obtained characteristics of biochars. The routine and challenging NMR methods utilized here would be an alternative other than HPLC or GC for biomass conversion research and can be extended to more studies. Keywords: NMR, Hydrothermal carbonization, Furfural residue, Stock process water

  1. Automated Solid Phase Extraction (SPE) LC/NMR Applied to the Structural Analysis of Extractable Compounds from a Pharmaceutical Packaging Material of Construction.

    Science.gov (United States)

    Norwood, Daniel L; Mullis, James O; Davis, Mark; Pennino, Scott; Egert, Thomas; Gonnella, Nina C

    2013-01-01

    The structural analysis (i.e., identification) of organic chemical entities leached into drug product formulations has traditionally been accomplished with techniques involving the combination of chromatography with mass spectrometry. These include gas chromatography/mass spectrometry (GC/MS) for volatile and semi-volatile compounds, and various forms of liquid chromatography/mass spectrometry (LC/MS or HPLC/MS) for semi-volatile and relatively non-volatile compounds. GC/MS and LC/MS techniques are complementary for structural analysis of leachables and potentially leachable organic compounds produced via laboratory extraction of pharmaceutical container closure/delivery system components and corresponding materials of construction. Both hyphenated analytical techniques possess the separating capability, compound specific detection attributes, and sensitivity required to effectively analyze complex mixtures of trace level organic compounds. However, hyphenated techniques based on mass spectrometry are limited by the inability to determine complete bond connectivity, the inability to distinguish between many types of structural isomers, and the inability to unambiguously determine aromatic substitution patterns. Nuclear magnetic resonance spectroscopy (NMR) does not have these limitations; hence it can serve as a complement to mass spectrometry. However, NMR technology is inherently insensitive and its ability to interface with chromatography has been historically challenging. This article describes the application of NMR coupled with liquid chromatography and automated solid phase extraction (SPE-LC/NMR) to the structural analysis of extractable organic compounds from a pharmaceutical packaging material of construction. The SPE-LC/NMR technology combined with micro-cryoprobe technology afforded the sensitivity and sample mass required for full structure elucidation. Optimization of the SPE-LC/NMR analytical method was achieved using a series of model compounds

  2. Determination of partition coefficients using 1 H NMR spectroscopy and time domain complete reduction to amplitude-frequency table (CRAFT) analysis.

    Science.gov (United States)

    Soulsby, David; Chica, Jeryl A M

    2017-08-01

    We have developed a simple, direct and novel method for the determination of partition coefficients and partitioning behavior using 1 H NMR spectroscopy combined with time domain complete reduction to amplitude-frequency tables (CRAFT). After partitioning into water and 1-octanol using standard methods, aliquots from each layer are directly analyzed using either proton or selective excitation NMR experiments. Signal amplitudes for each compound from each layer are then extracted directly from the time domain data in an automated fashion and analyzed using the CRAFT software. From these amplitudes, log P and log D 7.4 values can be calculated directly. Phase, baseline and internal standard issues, which can be problematic when Fourier transformed data are used, are unimportant when using time domain data. Furthermore, analytes can contain impurities because only a single resonance is examined and need not be UV active. Using this approach, we examined a variety of pharmaceutically relevant compounds and determined partition coefficients that are in excellent agreement with literature values. To demonstrate the utility of this approach, we also examined salicylic acid in more detail demonstrating an aggregation effect as a function of sample loading and partition coefficient behavior as a function of pH value. This method provides a valuable addition to the medicinal chemist toolbox for determining these important constants. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  3. Application of Detailed Phase Comparison Protection Models for the Analysis of its Operation in Networks with Facts Devices

    Directory of Open Access Journals (Sweden)

    Ruban Nikolay Yu.

    2015-01-01

    Full Text Available The problem of relay protection misoperations in networks with FACTS devices is considered in the paper. It is offered a solution to this problem for a phase comparison protection of transmission power line through the use of its detailed model for the analysis of the functioning for a case of various normal, emergency and post-emergency modes of electric power systems. The research results of this approach are given in the paper.

  4. Data Analysis Details (DS): SE40_DS1 [Metabolonote[Archive

    Lifescience Database Archive (English)

    Full Text Available tware without cut off value and peaks are extracted from the text files by PowerFT ...SE40_DS1 PowerGet analysis for detection of all peaks Raw data files are converted to text file by MSGet sof

  5. Data Analysis Details (DS): SE41_DS1 [Metabolonote[Archive

    Lifescience Database Archive (English)

    Full Text Available tware without cut off value and peaks are extracted from the text files by PowerFT ...SE41_DS1 PowerGet analysis for detection of all peaks Raw data files are converted to text file by MSGet sof

  6. Non-destructive digital imaging in poplar allows detailed analysis of adventitious rooting dynamics

    Science.gov (United States)

    R.J. Kodrzycki; R.B. Michaels; A.L. Friend; R.S. Zalesny; Ch.P. Mawata; D.W. McDonald

    2008-01-01

    The dynamics of root formation are difficult to observe directly over time without disturbing the rooting environment. A novel system for a non-destructive, non-invasive root analysis (RootViz FS, Phenotype Screening Corp.) was evaluated for its ability to analyze root formation from cuttings over a 32 day period in three poplar genotypes (DN70, P. Deltoides x...

  7. Detailed Analysis of Solar Data Related to Historical Extreme Geomagnetic Storms: 1868 – 2010

    DEFF Research Database (Denmark)

    Lefèvre, Laure; Vennerstrøm, Susanne; Dumbović, Mateja

    2016-01-01

    An analysis of historical Sun–Earth connection events in the context of the most extreme space weather events of the last ∼ 150 years is presented. To identify the key factors leading to these extreme events, a sample of the most important geomagnetic storms was selected based mainly on the well-...

  8. Tuberculosis in Sulaimaniyah, Iraqi Kurdistan: A Detailed Analysis of Cases Registered in Treatment Centers.

    Science.gov (United States)

    Karadakhy, Kamaran; Othman, Nasih; Ibrahimm, Faredun; Saeed, Akam Ali; Amin, Ari Abdul-Adheem Hama

    2016-01-01

    Tuberculosis (TB) remains a major public health problem especially in low and middle-income countries. The current study was undertaken to estimate the incidence of the disease and describe its epidemiological characteristics in Iraqi Kurdistan. A retrospective study was carried out on cases registered in the directly observed treatment-short course (DOTS) centers in Sulaimaniyah province. Information was collected from the summary reports of all cases registered in 2010 and detailed information was obtained from 307 cases in the main center. During 2010, a total of 530 new and relapsed cases were registered in the DOTS centers amounting to an annual incidence of 31 per 100,000. Over 73% of cases were pulmonary TB and 45% of all cases had positive smear. Most common symptoms were cough (58%), sweating (49%) and fever (48). Almost 43% of patients were diagnosed by direct swab examination, 30% by biopsy and 23% through clinical and radiologic examination. In relation to outcome, 89% of patients were treated successfully, 7% died and 3% defaulted. Mortality rate was 8% in pulmonary infection and 4% in extrapulmonary infection. Old age (65 years and over) was significantly associated with higher odds of death compared to people aged 34 years and younger (OR 6.7, 95% CI 1.3-36.1, P=0.03). The incidence of TB is still high in the Iraqi Kurdistan. The DOTS has been successful in treating the majority of cases but there are areas needing improvement especially record-keeping and patient follow-up during and after treatment.

  9. 1H NMR analysis of complexation of hydrotropic agents nicotinamide and caffeine with aromatic biologically active molecules in aqueous solution

    Science.gov (United States)

    Lantushenko, Anastasia O.; Mukhina, Yulia V.; Veselkov, Kyrill A.; Davies, David B.; Veselkov, Alexei N.

    2004-07-01

    NMR spectroscopy has been used to elucidate the molecular mechanism of solubilization action of hydrotropic agents nicotinamide (NA) and caffeine (CAF). Hetero-association of NA with riboflavine-mononucleotide (FMN) and CAF with low soluble in aqueous solution synthetic analogue of antibiotic actinomycin D, actinocyl-bis-(3-dimethylaminopropyl) amine (Actill), has been investigated by 500 MHz 1H NMR spectroscopy. Concentration and temperature dependences of proton chemical shifts have been analysed in terms of a statistical-thermodynamic model of indefinite self- and heteroassociation of aromatic molecules. The obtained results enable to conclude that NA-FMN and CAF-Actill intermolecular complexes are mainly stabilized by the stacking interactions of the aromatic chromophores. Hetero-association of the investigated molecules plays an important role in solubilization of aromatic drugs by hydrotropic agents nicotinamide and caffeine.

  10. Structural analysis of flavonoids in solution through DFT 1H NMR chemical shift calculations: Epigallocatechin, Kaempferol and Quercetin

    Science.gov (United States)

    De Souza, Leonardo A.; Tavares, Wagner M. G.; Lopes, Ana Paula M.; Soeiro, Malucia M.; De Almeida, Wagner B.

    2017-05-01

    In this work, we showed that comparison between experimental and theoretical 1H NMR chemical shift patterns, calculated using Density Functional Theory (DFT), can be used for the prediction of molecular structure of flavonoids in solution, what is experimentally accessible for gas phase (electron diffraction methods) and solid samples (X-ray diffraction). The best match between B3LYP/6-31G(d,p)-PCM 1H NMR calculations for B ring rotated structures and experimental spectra can provide information on the conformation adopted by polyphenols in solution (usually DMSO-d6, acetone-d6 as solvents), which may differ from solid state and gas phase observed structures, and also DFT optimized geometry in the vacuum.

  11. (1)H-NMR-based metabolomic analysis of the effect of moderate wine consumption on subjects with cardiovascular risk factors

    OpenAIRE

    Vázquez Fresno, Rosa; Llorach, Rafael; Alcaro, Francesca; Rodríguez Martínez, Miguel Ángel; Vinaixa Crevillent, Maria; Chiva Blanch, Gemma; Estruch Riba, Ramon; Correig Blanchar, Xavier; Andrés Lacueva, Ma. Cristina

    2012-01-01

    Moderate wine consumption is associated with health-promoting activities. An H-NMR-based metabolomic approach was used to identify urinary metabolomic differences of moderate wine intake in the setting of a prospective, randomized, crossover, and controlled trial. Sixty-one male volunteers with high cardiovascular risk factors followed three dietary interventions (28 days): dealcoholized red wine (RWD) (272mL/day, polyphenol control), alcoholized red wine (RWA) (272mL/day) and gin (GIN) (100m...

  12. NMR and rotational angles in solution conformation of polypeptides

    Science.gov (United States)

    Bystrov, V. F.

    1985-01-01

    Professor San-Ichiro Mizushima and Professor Yonezo Morino's classical contributions provided unique means and firm basis for understanding of conformational states and internal rotation in polypeptide molecules. Now the NMR spectroscopy is the best choice to study molecular conformation, mechanism of action and structure-functional relationships of peptide and proteins in solution under conditions approaching those of their physiological environments. Crucial details of spatial structure and interactions of these molecules in solution are revealed by using proton-proton and carbon-proton vicinal coupling constants, proton nuclear Overhauser effect and spectral perturbation techniques. The results of NMR conformational analysis are presented for valinomycin "bracelet", gramicidin A double helices, honey-bee neurotoxin apamin, scorpion insectotoxins and snake neurotoxins of long and short types.

  13. Optimized co-solute paramagnetic relaxation enhancement for the rapid NMR analysis of a highly fibrillogenic peptide

    International Nuclear Information System (INIS)

    Oktaviani, Nur Alia; Risør, Michael W.; Lee, Young-Ho; Megens, Rik P.; Jong, Djurre H. de; Otten, Renee; Scheek, Ruud M.; Enghild, Jan J.; Nielsen, Niels Chr.; Ikegami, Takahisa; Mulder, Frans A. A.

    2015-01-01

    Co-solute paramagnetic relaxation enhancement (PRE) is an attractive way to speed up data acquisition in NMR spectroscopy by shortening the T 1 relaxation time of the nucleus of interest and thus the necessary recycle delay. Here, we present the rationale to utilize high-spin iron(III) as the optimal transition metal for this purpose and characterize the properties of its neutral chelate form Fe(DO3A) as a suitable PRE agent. Fe(DO3A) effectively reduces the T 1 values across the entire sequence of the intrinsically disordered protein α-synuclein with negligible impact on line width. The agent is better suited than currently used alternatives, shows no specific interaction with the polypeptide chain and, due to its high relaxivity, is effective at low concentrations and in ‘proton-less’ NMR experiments. By using Fe(DO3A) we were able to complete the backbone resonance assignment of a highly fibrillogenic peptide from α 1 -antitrypsin by acquiring the necessary suite of multidimensional NMR datasets in 3 h

  14. Optimized co-solute paramagnetic relaxation enhancement for the rapid NMR analysis of a highly fibrillogenic peptide

    Energy Technology Data Exchange (ETDEWEB)

    Oktaviani, Nur Alia [University of Groningen, Groningen Biomolecular Sciences and Biotechnology Institute (Netherlands); Risør, Michael W. [University of Aarhus, Interdisciplinary Nanoscience Center (iNANO) and Department of Chemistry (Denmark); Lee, Young-Ho [Osaka University, Institute for Protein Research (Japan); Megens, Rik P. [University of Groningen, Stratingh Institute for Chemistry (Netherlands); Jong, Djurre H. de; Otten, Renee; Scheek, Ruud M. [University of Groningen, Groningen Biomolecular Sciences and Biotechnology Institute (Netherlands); Enghild, Jan J. [University of Aarhus, Interdisciplinary Nanoscience Center (iNANO) and Department of Molecular Biology and Genetics (Denmark); Nielsen, Niels Chr. [University of Aarhus, Interdisciplinary Nanoscience Center (iNANO) and Department of Chemistry (Denmark); Ikegami, Takahisa [Yokohama City University, Graduate School of Medical Life Science (Japan); Mulder, Frans A. A., E-mail: fmulder@chem.au.dk [University of Groningen, Groningen Biomolecular Sciences and Biotechnology Institute (Netherlands)

    2015-06-15

    Co-solute paramagnetic relaxation enhancement (PRE) is an attractive way to speed up data acquisition in NMR spectroscopy by shortening the T{sub 1} relaxation time of the nucleus of interest and thus the necessary recycle delay. Here, we present the rationale to utilize high-spin iron(III) as the optimal transition metal for this purpose and characterize the properties of its neutral chelate form Fe(DO3A) as a suitable PRE agent. Fe(DO3A) effectively reduces the T{sub 1} values across the entire sequence of the intrinsically disordered protein α-synuclein with negligible impact on line width. The agent is better suited than currently used alternatives, shows no specific interaction with the polypeptide chain and, due to its high relaxivity, is effective at low concentrations and in ‘proton-less’ NMR experiments. By using Fe(DO3A) we were able to complete the backbone resonance assignment of a highly fibrillogenic peptide from α{sub 1}-antitrypsin by acquiring the necessary suite of multidimensional NMR datasets in 3 h.

  15. Variations of pH as an additional tool in the analysis of crowded NMR spectra of fucosylated chondroitin sulfates.

    Science.gov (United States)

    Ustyuzhanina, Nadezhda E; Dmitrenok, Andrey S; Bilan, Maria I; Shashkov, Alexander S; Gerbst, Alexey G; Usov, Anatolii I; Nifantiev, Nikolay E

    2016-03-24

    The influence of pH variation on chemical shift values in NMR spectra of fucosylated chondroitin sulfates was studied using polysaccharides isolated from three sea cucumber species Apostichopus japonicus, Actinopyga mauritiana and Cucumaria japonica. The signals of glucuronic acid residues were found to be the most sensitive to pH changes in comparison to the chemical shifts of the sulfated galactosamine and fucosyl units, most of which were altered insignificantly. It was shown that in the presence of imidazole-HCl buffer (pH 7.2) NMR spectra of the polysaccharides from A. japonicus and A. mauritiana were sufficiently resolved, whereas under acidic conditions their (1)H NMR spectra were complicated by overlapping of H-1 signals of GlcA and GalNAc. In the case of polysaccharide from C. japonica bearing 3-O-fucosylated and 3-O-sulfated glucuronic acid residues in the backbone, acidification of the medium led to separation of H-1 signals of GlcA3S and GalNAc. Therefore, the combination of data obtained at different pH values may be useful for interpretation of overcrowded spectra of fucosylated chondroitin sulfates. Copyright © 2016 Elsevier Ltd. All rights reserved.

  16. Detailed Analysis of Japanese Population Substructure with a Focus on the Southwest Islands of Japan

    Science.gov (United States)

    Nishiyama, Takeshi; Kishino, Hirohisa; Suzuki, Sadao; Ando, Ryosuke; Niimura, Hideshi; Uemura, Hirokazu; Horita, Mikako; Ohnaka, Keizo; Kuriyama, Nagato; Mikami, Haruo; Takashima, Naoyuki; Mastuo, Keitaro; Guang, Yin; Wakai, Kenji; Hamajima, Nobuyuki; Tanaka, Hideo

    2012-01-01

    Uncovering population structure is important for properly conducting association studies and for examining the demographic history of a population. Here, we examined the Japanese population substructure using data from the Japan Multi-Institutional Collaborative Cohort (J-MICC), which covers all but the northern region of Japan. Using 222 autosomal loci from 4502 subjects, we investigated population substructure by estimating FST among populations, testing population differentiation, and performing principal component analysis (PCA) and correspondence analysis (CA). All analyses revealed a low but significant differentiation between the Amami Islanders and the mainland Japanese population. Furthermore, we examined the genetic differentiation between the mainland population, Amami Islanders and Okinawa Islanders using six loci included in both the Pan-Asian SNP (PASNP) consortium data and the J-MICC data. This analysis revealed that the Amami and Okinawa Islanders were differentiated from the mainland population. In conclusion, we revealed a low but significant level of genetic differentiation between the mainland population and populations in or to the south of the Amami Islands, although genetic variation between both populations might be clinal. Therefore, the possibility of population stratification must be considered when enrolling the islander population of this area, such as in the J-MICC study. PMID:22509376

  17. Detailed analysis of allergic cutaneous reactions to spinal cord stimulator devices

    Directory of Open Access Journals (Sweden)

    Chaudhry ZA

    2013-08-01

    Full Text Available Zeshan Ahmed Chaudhry,1 Umer Najib,2 Zahid H Bajwa,3 W Carl Jacobs,4 Javed Sheikh,5 Thomas T Simopoulos61Department of Diagnostic and Interventional Neuroradiology, Massachusetts General Hospital/Harvard Medical School, Boston, MA, USA; 2Department of Neurology, Robert C Byrd Health Sciences Center of West Virginia University, Morgantown, WV, USA; 3Boston Headache Institute, Waltham, MA, USA; 4Department of Pathology, Beth Israel Deaconess Medical Center, Harvard Medical School, Boston, MA, USA; 5Department of Medicine, Allergy and Immunology, 6Department of Anesthesia, Beth Israel Deaconess Medical Center, Brookline, MA, USAAbstract: The use of spinal cord stimulation (SCS devices to treat chronic, refractory neuropathic pain continues to expand in application. While device-related complications have been well described, inflammatory reactions to the components of these devices remain underreported. In contrast, hypersensitivity reactions associated with other implanted therapies, such as endovascular and cardiac rhythm devices, have been detailed. The purpose of this case series is to describe the clinical presentation and course of inflammatory reactions as well as the histology of these reactions. All patients required removal of the entire device after developing inflammatory reactions over a time course of 1–3 months. Two patients developed a foreign body reaction in the lead insertion wound as well as at the implantable pulse generator site, with histology positive for giant cells. One patient developed an inflammatory dermatitis on the flank and abdomen that resolved with topical hydrocortisone. “In vivo” testing with a lead extension fragment placed in the buttock resulted in a negative reaction followed by successful reimplantation of an SCS device. Inflammatory reactions to SCS devices can manifest as contact dermatitis, granuloma formation, or foreign body reactions with giant cell formation. Tissue diagnosis is essential, and

  18. Detailed analysis of putative genes encoding small proteins in legume genomes

    Directory of Open Access Journals (Sweden)

    Gabriel eGuillén

    2013-06-01

    Full Text Available Diverse plant genome sequencing projects coupled with powerful bioinformatics tools have facilitated massive data analysis to construct specialized databases classified according to cellular function. However, there are still a considerable number of genes encoding proteins whose function has not yet been characterized. Included in this category are small proteins (SPs, 30-150 amino acids encoded by short open reading frames (sORFs. SPs play important roles in plant physiology, growth, and development. Unfortunately, protocols focused on the genome-wide identification and characterization of sORFs are scarce or remain poorly implemented. As a result, these genes are underrepresented in many genome annotations. In this work, we exploited publicly available genome sequences of Phaseolus vulgaris, Medicago truncatula, Glycine max and Lotus japonicus to analyze the abundance of annotated SPs in plant legumes. Our strategy to uncover bona fide sORFs at the genome level was centered in bioinformatics analysis of characteristics such as evidence of expression (transcription, presence of known protein regions or domains, and identification of orthologous genes in the genomes explored. We collected 6170, 10461, 30521, and 23599 putative sORFs from P. vulgaris, G. max, M. truncatula, and L. japonicus genomes, respectively. Expressed sequence tags (ESTs available in the DFCI Gene Index database provided evidence that ~one-third of the predicted legume sORFs are expressed. Most potential SPs have a counterpart in a different plant species and counterpart regions or domains in larger proteins. Potential functional sORFs were also classified according to a reduced set of GO categories, and the expression of 13 of them during P. vulgaris nodule ontogeny was confirmed by qPCR. This analysis provides a collection of sORFs that potentially encode for meaningful SPs, and offers the possibility of their further functional evaluation.

  19. Assessment of constituents in Allium by multivariate data analysis, high-resolution α-glucosidase inhibition assay and HPLC-SPE-NMR

    DEFF Research Database (Denmark)

    Schmidt, Jeppe Secher; Nyberg, Nils; Stærk, Dan

    2014-01-01

    Bulbs and leaves of 35 Allium species and cultivars bought or collected in 2010–2012 were investigated with multivariate data analysis, high-resolution α-glucosidase inhibition assays and HPLC-HRMS-SPE-NMR with the aim of exploring the potential of Allium as a future functional food for management...... of type 2 diabetes. It was found that 30 out of 106 crude extracts showed more than 80% inhibition of the α-glucosidase enzyme at a concentration of 40 mg/mL (dry sample) or 0.4 g/mL (fresh sample). High-resolution α-glucosidase biochromatograms of these extracts allowed fast identification of three...

  20. Author Details

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    Njubi, Francis. Vol 15, No 1 (2001): Media Freedom and Human Rights - Articles New Media, Old Struggles: Pan Africanism, Anti-racism and Information Technology Details. ISSN: 0256-004. AJOL African Journals Online. HOW TO USE AJOL... for Researchers · for Librarians · for Authors · FAQ's · More about AJOL · AJOL's ...

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    Radwan M.D, Mona Ahmed. Vol 12, No 1 (2000) - Articles RELAPSING REMITTING MULTIPLE SCLEROSIS: CT AND MRI IMAGING VS CLINICAL FINDINGIN THE DIAGNOSIS AND DETERMINATION OF DISEASE ACTIVITY. Details. ISSN: 1110-5607. AJOL African Journals Online. HOW TO USE AJOL... for Researchers ...

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    Comarof, Jean. Vol 1999, No 3-4 (1999) - Articles Alien-Nation: Zombies, Immigrants and Millennial Capitalism Details. ISSN: 0850-8712. AJOL African Journals Online. HOW TO USE AJOL... for Researchers · for Librarians · for Authors · FAQ's · More about AJOL · AJOL's Partners · Terms and Conditions of Use · Contact ...

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    NENTY, N. JOHNSON. Vol 7, No 3 (2001) - Articles Common errors and perfomance of students in junior secondary mathematics certificate examinations in Cross River State, Nigeria Details PDF. ISSN: 1118-0579. AJOL African Journals Online. HOW TO USE AJOL... for Researchers · for Librarians · for Authors · FAQ's ...

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    A Preliminary Investigation of Relative Frequency of Undiagnosed and Previously Diagnosed Hypertension Before First Stroke in a Lagos Hospital Abstract · Vol 9, No 4 (1999) - Articles Localised tetanus in Lagos, Nigeria Details · Vol 9, No 4 (1999) - Articles Stroke with localised infarction of Wernicke's Area misdiagnosed ...

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    SAMA, G. Vol 2 (2002): Supplement - Articles A Longitudinal Study of the Role of T Cell subset, Th1/Th2 cytokines and antiplasmodial antibodies in uncomplicated Malaria in a Village Population Chronically Exposed to Plasmodium falciparum Malaria. Details PDF · AJOL African Journals Online. HOW TO USE AJOL.

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    QUAKYI, A.I.. Vol 2 (2002): Supplement - Articles A Longitudinal Study of the Role of T Cell subset, Th1/Th2 cytokines and antiplasmodial antibodies in uncomplicated Malaria in a Village Population Chronically Exposed to Plasmodium falciparum Malaria. Details PDF · AJOL African Journals Online. HOW TO USE AJOL.

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    KOUONTCHOU, Samuel. Vol 2 (2002): Supplement - Articles Prevalence of Multiple Concomitant Intestinal Parasitic Infections in Simbok a Malaria Endemic Village in Cameroon. Details PDF · Vol 2 (2002): Supplement - Articles A Longitudinal Study of the Role of T Cell subset, Th1/Th2 cytokines and antiplasmodial ...

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    ALAKE, J. Vol 2 (2002): Supplement - Articles A Longitudinal Study of the Role of T Cell subset, Th1/Th2 cytokines and antiplasmodial antibodies in uncomplicated Malaria in a Village Population Chronically Exposed to Plasmodium falciparum Malaria. Details PDF · AJOL African Journals Online. HOW TO USE AJOL.

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    Rakotonirina, Alice. Vol 2, No 2 (2002) - Articles Effect of the decoction of rhizomes of Cyperus articulatus on bicuculline-, N-methyl-D-aspartate- and strychnine-induced behavioural excitation and convulsions in mice. Details PDF · AJOL African Journals Online. HOW TO USE AJOL... for Researchers · for Librarians ...

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    Love, Alison. Vol 29, No 2 (2002) - Articles Policy-makers, the Press and Politics: Reporting a Public Policy Document Details. ISSN: 0379-0622. AJOL African Journals Online. HOW TO USE AJOL... for Researchers · for Librarians · for Authors · FAQ's · More about AJOL · AJOL's Partners · Terms and Conditions of Use ...

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    Focho, DA. Vol 2, No 1 (2002) - Articles Observations on the Meiotic Process in the African Pest Grasshopper Taphronota thaelephora Stal. (Orthoptera : Pyrgomorphidae) Details PDF · AJOL African Journals Online. HOW TO USE AJOL... for Researchers · for Librarians · for Authors · FAQ's · More about AJOL · AJOL's ...

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    Idowu, OO. Vol 8, No 1 (2003) - Articles Evaluation of Different Substrates and Combinations on the Growth of Pleurotus pulmonarius (Fries) Quelet (Sajor-caju) Details. ISSN: 1118-2733. AJOL African Journals Online. HOW TO USE AJOL... for Researchers · for Librarians · for Authors · FAQ's · More about AJOL · AJOL's ...

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    Ligthelm, A.A.. Vol 5, No 2 (2001) - Articles Community attitudes towards Casinos and the estimated magnitude of problem gambling The Mpumalanga case. Details PDF. ISSN: 1027-4332. AJOL African Journals Online. HOW TO USE AJOL... for Researchers · for Librarians · for Authors · FAQ's · More about AJOL · AJOL's ...

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    Kioni, P N. Vol 9, No 1 (2007) - Articles Detailed structure of pipe flow with water hammer oscillations. Abstract. ISSN: 1561-7645. AJOL African Journals Online. HOW TO USE AJOL... for Researchers · for Librarians · for Authors · FAQ's · More about AJOL · AJOL's Partners · Terms and Conditions of Use · Contact AJOL ...

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    Development of a trap to contaminate variegated grasshoppers (Zonocerus variegatus L.) (Orthoptera: Pyrgomorphidae) with Metarrhyzium flavo-viride Gams & Rozsypal in the field. Details · Vol 40, No 1 (2007) - Articles Yam pests in the Ashanti and Brong Ahafo regions of Ghana: A study of farmers\\' indigenous technical ...

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    Brown, Duncan. Vol 16, No 2 (2002): Continental Africans & the Question of Identity - Articles Environment and Identity: Douglas Livingstone's A Littoral Zone Details. ISSN: 0256-004. AJOL African Journals Online. HOW TO USE AJOL... for Researchers · for Librarians · for Authors · FAQ's · More about AJOL · AJOL's ...

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    Aderinokun, GA. Vol 9, No 1 (1999) - Articles Relative Influence Of Sociodemographic Variables On Oral Health And Habits Of Some Nigerian School Children Abstract · Vol 9, No 4 (1999) - Articles Oral health services in Nigeria Details. ISSN: 0189-2657. AJOL African Journals Online. HOW TO USE AJOL.

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    EKPA, O. D.. Vol 7, No 2 (2001) - Articles Variental differences AND polymorphism in palm oil: a case study of palm oils blended with coconut oil. Details PDF. ISSN: 1118-0579. AJOL African Journals Online. HOW TO USE AJOL... for Researchers · for Librarians · for Authors · FAQ's · More about AJOL · AJOL's Partners ...

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    SONUGA, F A. Vol 6, No 1 (2000) - Articles Geophysical investigation of Karkarku earthdam embankment. Details. ISSN: 1118-0579. AJOL African Journals Online. HOW TO USE AJOL... for Researchers · for Librarians · for Authors · FAQ's · More about AJOL · AJOL's Partners · Terms and Conditions of Use · Contact AJOL ...

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    Geotechnical properties of lateritic soil developed over quartz schist in Ishara area, south western Nigeria Details · Vol 44, No 1 (2008) - Articles Comparative study of the influence of cement and lime stabilization on geotechnical properties of lateritic soil derived from pegmatite in Ago-Iwoye area, southwestern Nigeria

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    McCarthy, Greg. Vol 15, No 1 (2001): Media Freedom and Human Rights - Articles Caught between Empires: Ambivalence in Australian Films Details. ISSN: 0256-004. AJOL African Journals Online. HOW TO USE AJOL... for Researchers · for Librarians · for Authors · FAQ's · More about AJOL · AJOL's Partners · Terms and ...

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    Legwaila, GM. Vol 12 (2003) - Articles Review of sweet sorghum: a potential cash and forage crop in Botswana Details. ISSN: 1021-0873. AJOL African Journals Online. HOW TO USE AJOL... for Researchers · for Librarians · for Authors · FAQ's · More about AJOL · AJOL's Partners · Terms and Conditions of Use · Contact ...

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    Admasu, Assefa. Vol 22, No 2 (1999) - Articles Preliminary evaluation of Phytomyza orobanchia (Diptera: Agromyzidae) as a controller of Orobanche spp in Ethiopia Details PDF. ISSN: 2520–7997. AJOL African Journals Online. HOW TO USE AJOL... for Researchers · for Librarians · for Authors · FAQ's · More about AJOL ...

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    Journal Home > Advanced Search > Author Details. Log in or Register to get access to full text downloads. ... Obtaining the green's function for electromagnetic waves propagating in layered in-homogeneous thin film media of spherical particles on a substrate. Abstract · Vol 20, No 2 (2008) - Articles solution growth and ...

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    Journal Home > Advanced Search > Author Details. Log in or Register to get access to full text ... Abstract · Vol 17 (2010) - Articles Investigating The Travelling Wave Solution For an SIR Endemic Disease Model With No Disease Related Death (When The Spatial Spread Of The Susceptible Is Not Negligible). Abstract.

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    Journal Home > Advanced Search > Author Details. Log in or Register to get access to full text downloads. ... Vol 8 (2004) - Articles Further on stokes expansions for the finite amplitude water waves. Abstract · Vol 11 (2007) - Articles On the effects of wave steepness on higher order Stokes waves. Abstract. ISSN: 1116-4336.

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    Akum, ZE. Vol 1, No 3 (2001) - Articles Basic home range characteristics for the conservation of the African grey parrot in the Korup national park, Cameroon Details PDF · AJOL African Journals Online. HOW TO USE AJOL... for Researchers · for Librarians · for Authors · FAQ's · More about AJOL · AJOL's Partners · Terms ...

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    Bobcokono, Irene Yatabene. Vol 1, No 1 (2001) - Articles Utilisation du papier filtre dans la gestion de programme de lute contre le SIDA au Cameroun Details PDF · AJOL African Journals Online. HOW TO USE AJOL... for Researchers · for Librarians · for Authors · FAQ's · More about AJOL · AJOL's Partners · Terms and ...

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    Lema, VM. Vol 80, No 9 (2003): - Articles Fournier's gangrene complicating vasectomy. Details PDF · Vol 86, No 6 (2009) - Articles Therapeutic misconception and clinical trials in sub-saharan Africa: A review. Abstract PDF · Vol 86, No 11 (2009) - Articles HIV/AIDS and pregnancy-related deaths in Blantyre, Malawi

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    Green, J.M.. Vol 10, No 1 (2001) - Articles Information from Radio Telemetry on movements and exploitation of naturalized Rainbow trout, Oncorhynchus mykiss (Walbaum), in Kenya cold water streams. Details. ISSN: 0002-0036. AJOL African Journals Online. HOW TO USE AJOL... for Researchers · for Librarians ...

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    Erasmus, GJ. Vol 1, No 1 (2001) - Articles Genetic parameter estimates for growth traits in purebred Gudali and two-breed synthetic Wakwa beef cattle in a tropical environment. Details PDF · AJOL African Journals Online. HOW TO USE AJOL... for Researchers · for Librarians · for Authors · FAQ's · More about AJOL · AJOL's ...

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    Odigie, IP. Vol 10, No 4 (2000) - Articles High dose vitamin E administration attenuates hypertensin in 2-Kidney 1 Clip Goldblatt hypertensive rats. Details. ISSN: 0189-2657. AJOL African Journals Online. HOW TO USE AJOL... for Researchers · for Librarians · for Authors · FAQ's · More about AJOL · AJOL's Partners · Terms ...

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    Motabagani, MA. Vol 80, No 9 (2003): - Articles Anomalies of the renal, phrenic and suprarenal arteries: Case Report Details PDF · Vol 81, No 3 (2004): - Articles Morphological study of the uncommon rectus sterni muscle in German cadavers. Abstract PDF. ISSN: 0012-835X. AJOL African Journals Online. HOW TO USE ...

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    Ibeabuchi, NM. Vol 10, No 3 (2000) - Articles Comparison of the effects of Methylsalicylate Cream with cryotherapy on delayed onset muscle soreness. Details · Vol 22, No 2 (2012) - Articles X-ray Pelvimetry And Labour Outcome In Term Pregnancy In A Rural Nigerian Population Abstract. ISSN: 0189-2657. AJOL African ...

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    Warnorff, DK. Vol 13, No 4 (2001) - Articles Development of a scoring system for the diagnosis of tuberculous lymphadenitis. Details PDF. ISSN: 1995-7262. AJOL African Journals Online. HOW TO USE AJOL... for Researchers · for Librarians · for Authors · FAQ's · More about AJOL · AJOL's Partners · Terms and Conditions ...

  16. A path flux analysis method for the reduction of detailed chemical kinetic mechanisms

    Energy Technology Data Exchange (ETDEWEB)

    Sun, Wenting; Ju, Yiguang [Department of Mechanical and Aerospace Engineering, Princeton University, Princeton, NJ 08544 (United States); Chen, Zheng [State Key Laboratory for Turbulence and Complex Systems, College of Engineering, Peking University, Beijing 100871 (China); Gou, Xiaolong [School of Power Engineering, Chongqing University, Chongqing 400044 (China)

    2010-07-15

    A direct path flux analysis (PFA) method for kinetic mechanism reduction is proposed and validated by using high temperature ignition, perfect stirred reactors, and steady and unsteady flame propagations of n-heptane and n-decane/air mixtures. The formation and consumption fluxes of each species at multiple reaction path generations are analyzed and used to identify the important reaction pathways and the associated species. The formation and consumption path fluxes used in this method retain flux conservation information and are used to define the path indexes for the first and the second generation reaction paths related to a targeted species. Based on the indexes of each reaction path for the first and second generations, different sized reduced chemical mechanisms which contain different number of species are generated. The reduced mechanisms of n-heptane and n-decane obtained by using the present method are compared to those generated by the direct relation graph (DRG) method. The reaction path analysis for n-decane is conducted to demonstrate the validity of the present method. The comparisons of the ignition delay times, flame propagation speeds, flame structures, and unsteady spherical flame propagation processes showed that with either the same or significantly less number of species, the reduced mechanisms generated by the present PFA are more accurate than that of DRG in a broad range of initial pressures and temperatures. The method is also integrated with the dynamic multi-timescale method and a further increase of computation efficiency is achieved. (author)

  17. Cath lab costs in patients undergoing percutaneous coronary angioplasty - detailed analysis of consecutive procedures.

    Science.gov (United States)

    Dziki, Beata; Miechowicz, Izabela; Iwachów, Piotr; Kuzemczak, Michał; Kałmucki, Piotr; Szyszka, Andrzej; Baszko, Artur; Siminiak, Tomasz

    2017-01-01

    Costs of percutaneous coronary interventions (PCI) have an important impact on health care expenditures. Despite the present stress upon the cost-effectiveness issues in medicine, few comprehensive data exist on costs and resource use in different clinical settings. To assess catheterisation laboratory costs related to use of drugs and single-use devices in patients undergoing PCI due to coronary artery disease. Retrospective analysis of 1500 consecutive PCIs (radial approach, n = 1103; femoral approach, n = 397) performed due to ST segment elevation myocardial infarction (STEMI; n = 345) and non ST-segment elevation myocardial infarction (NSTEMI; n = 426) as well as unstable angina (UA; n = 489) and stable angina (SA; n = 241) was undertaken. Comparative cost analysis was performed and shown in local currency units (PLN). The cath lab costs were higher in STEMI (4295.01 ± 2384.54PLN, p costs were positively correlated with X-ray dose, fluoroscopy, and total procedure times. Patients' age negatively correlated with cath lab costs in STEMI/NSTEMI patients. Cath lab costs were higher in STEMI patients compared to other groups. In STEMI/NSTEMI they were lower in older patients. In all analysed groups costs were related to the level of procedural difficulty. In female patients, the costs of PCI performed via radial approach were higher compared to femoral approach. Despite younger age, male patients underwent more expensive procedures.

  18. Detailed analysis of the TMI-2 accident scenario by using MARS/SCDAP

    International Nuclear Information System (INIS)

    Park, Rae Joon; Lee, Young Jin; Chung, Bub Dong

    2009-01-01

    As part of a benchmark analysis, the Three Mile Island Unit 2 (TMI-2) accident has been analyzed by using the MARS/SCDAP computer code. This analysis has been performed to estimate the efficiency of the MARS/SCDAP computer code and the predictive qualities of its models from an initiating event to a severe accident. The MARS/SCDAP results have shown that a reduction feed water to the steam generator caused the coolant to expand and initially increased the reactor coolant system (RCS) pressure. The pilot-operated relief valve (PORV) opened when the pressure reached 15.7 MPa, with a reactor scram occurring when the pressure reached 16.3 MPa. The PORV failed to close as the RCS pressure decreased, initiating a small break loss of coolant accident. The emergency core cooling was reduced by operators who thought that the pressurizer liquid level indicated a nearly full RCS, while coolant continued to be lost from the PORV. After an initial decrease in the RCS pressure, the pressurizer pressure remained at approximately 7 MPa. After a pump termination at 6,000 seconds, the liquid level in the reactor vessel decreased, which resulted in a core uncovery. Continued core degradation with a coolant boiling caused the pressurizer pressure to increase. The MARS/SCDAP results are very similar to the TMI-2 data

  19. Detailed electromagnetic analysis for optimization of a tungsten divertor plate for JET

    International Nuclear Information System (INIS)

    Sadakov, S.; Bondarchuk, E.; Doinikov, N.; Kitaev, B.; Kozhukhovskaya, N.; Maximiva, I.; Hirai, T.; Mertens, P.; Neubauer, O.; Obidenko, T.

    2006-01-01

    The ITER-like wall project at JET involves the replacement of the divertor tiles by either tungsten-coated carbon fibre composite (CFC) or solid tungsten. The background is a full replacement of CFC in order to avoid tritium retention due to co-deposition of carbon. In a R-and-D phase (T.Hirai et al., R-and-D on full tungsten divertor and beryllium wall for JET ITER-like Wall Project.), both tungsten coating and solid tungsten are investigated. Tungsten has a high electrical conductivity, exceeding that of graphite or CFC by two orders of magnitude. This drawback has to be compensated by a proper design (Ph. Mertens et al., Conceptual Design for a Bulk Tungsten Divertor Tile in JET (both citations: this conference)). This report shows how detailed electromagnetic consideration has influenced the design of the solid tungsten divertor for JET. Patterns and sum values were calculated for: (1) eddy currents induced by variation of two orthogonal magnetic fields; (2) toroidal eddy current induced by variation of the poloidal magnetic flux, (3) eddy-current related loads in three orthogonal magnetic fields; (4) Halo current pattern for two cases; (5) Halo-current related loads in three orthogonal magnetic fields; (6) the worst loads combinations; (7) stresses in fixtures. Analytical and numerical methods were combined and cross-checked. The load-bearing septum replacement plate (LB-SRP) which is currently used in the JET divertor consists of two large CFC tiles attached to two superimposed Inconel frames, namely wedge and adapter. The present design is quite loaded by eddy-currents and does not allow for simple replacement of the CFC with solid tungsten. A tree-like shape, which excludes large contours of eddy currents, is proposed. In realization of the tree-like shape, the wedge has a narrow middle part, elongated in radial direction, and eight wings, elongated in toroidal direction. Eight feet form the Halo current path. Each wing carries one tungsten lamellae stack

  20. Quantitative analysis of detailed lignin monomer composition by pyrolysis-gas chromatography combined with preliminary acetylation of the samples.

    Science.gov (United States)

    Sonoda, T; Ona, T; Yokoi, H; Ishida, Y; Ohtani, H; Tsuge, S

    2001-11-15

    Detailed quantitative analysis of lignin monomer composition comprising p-coumaryl, coniferyl, and sinapyl alcohol and p-coumaraldehyde, coniferaldehyde, and sinapaldehyde in plant has not been studied from every point mainly because of artifact formation during the lignin isolation procedure, partial loss of the lignin components inherent in the chemical degradative methods, and difficulty in the explanation of the complex spectra generally observed for the lignin components. Here we propose a new method to quantify lignin monomer composition in detail by pyrolysis-gas chromatography (Py-GC) using acetylated lignin samples. The lignin acetylation procedure would contribute to prevent secondary formation of cinnamaldehydes from the corresponding alcohol forms during pyrolysis, which are otherwise unavoidable in conventional Py-GC process to some extent. On the basis of the characteristic peaks on the pyrograms of the acetylated sample, lignin monomer compositions in various dehydrogenative polymers (DHP) as lignin model compounds were determined, taking even minor components such as cinnamaldehydes into consideration. The observed compositions by Py-GC were in good agreement with the supplied lignin monomer contents on DHP synthesis. The new Py-GC method combined with sample preacetylation allowed us an accurate quantitative analysis of detailed lignin monomer composition using a microgram order of extractive-free plant samples.

  1. Detailed analysis of the Valdes slide: a landward facing slope failure off Chile

    Science.gov (United States)

    Anasetti, Andrea; Krastel, Sebastian; Weinrebe, Willy; Klaucke, Ingo; Bialas, Jorge

    2010-05-01

    The Chilean continental margin is a very active area interested by important tectonic movements and characterized by a fast morphological evolution. Geophysical data acquired during cruise JC 23, aboard RV JAMES COOK in March/April 2008 and previous cruises cover most of the active Chilean continental margin between 33° and 37° S. Integrated interpretation of multi-beam bathymetric, sub-bottom profiles, side-scan sonar and seismic data allowed the identification of a number of slope failures. The main topic of this project is the morphological and sedimentological analysis of the Valdes slide, a medium-sized submarine landslide offshore the city of Talcahuano (300 km south of Santiago). In contrast to most other slides along continental margins, the Valdes slide is located on the landward facing eastern slope of a submarine ridge. This setting has important implications for the associated tsunami wave field (first arrival of positive amplitude). We measured geometrical parameters of the failure and adjacent slope. The slide affected an area of 19 km2 between ~1060 m and >1700 m water depths. Its is ~ 6 km long, up to 3 km wide and involved a total sedimentary volume of about 0,8 km3. The failure process was characterized by a multiple-event and we assume its tsunami potential to be high. Using the high resolution bathymetric data and the seismic profiles along the slide deposit it was possible to reconstruct the original morphology of the area in order to understand the relation between the slide event and the structural evolution of the ridge. Through the analysis of the data and bibliographic information about the Chilean margin, we analyzed potential trigger mechanisms for the landslide. The Valdes slide is situated on a steep ridge flank. The ridge follows an elongated fault zone running app. parallel to the margin. This fault zone has a dextral component which in combination with the faults elongation results in a compressional regime that is superimposed on

  2. Vicinal 1H-1H NMR coupling constants from density functional theory as reliable tools for stereochemical analysis of highly flexible multichiral center molecules.

    Science.gov (United States)

    López-Vallejo, Fabian; Fragoso-Serrano, Mabel; Suárez-Ortiz, Gloria Alejandra; Hernández-Rojas, Adriana C; Cerda-García-Rojas, Carlos M; Pereda-Miranda, Rogelio

    2011-08-05

    A protocol for stereochemical analysis, based on the systematic comparison between theoretical and experimental vicinal (1)H-(1)H NMR coupling constants, was developed and applied to a series of flexible compounds (1-8) derived from the 6-heptenyl-5,6-dihydro-2H-pyran-2-one framework. The method included a broad conformational search, followed by geometry optimization at the DFT B3LYP/DGDZVP level, calculation of the vibrational frequencies, thermochemical parameters, magnetic shielding tensors, and the total NMR spin-spin coupling constants. Three scaling factors, depending on the carbon atom hybridizations, were found for the (1)H-C-C-(1)H vicinal coupling constants: f((sp3)-(sp3)) = 0.910, f((sp3)-(sp2)) = 0.929, and f((sp2)-(sp2))= 0.977. A remarkable correlation between the theoretical (J(pre)) and experimental (1)H-(1)H NMR (J(exp)) coupling constants for spicigerolide (1), a cytotoxic natural product, and some of its synthetic stereoisomers (2-4) demonstrated the predictive value of this approach for the stereochemical assignment of highly flexible compounds containing multiple chiral centers. The stereochemistry of two natural 6-heptenyl-5,6-dihydro-2H-pyran-2-ones (14 and 15) containing diverse functional groups in the heptenyl side chain was also analyzed by application of this combined theoretical and experimental approach, confirming its reliability. Additionally, a geometrical analysis for the conformations of 1-8 revealed that weak hydrogen bonds substantially guide the conformational behavior of the tetraacyloxy-6-heptenyl-2H-pyran-2-ones.

  3. The complexity of Rhipicephalus (Boophilus microplus genome characterised through detailed analysis of two BAC clones

    Directory of Open Access Journals (Sweden)

    Valle Manuel

    2011-07-01

    Full Text Available Abstract Background Rhipicephalus (Boophilus microplus (Rmi a major cattle ectoparasite and tick borne disease vector, impacts on animal welfare and industry productivity. In arthropod research there is an absence of a complete Chelicerate genome, which includes ticks, mites, spiders, scorpions and crustaceans. Model arthropod genomes such as Drosophila and Anopheles are too taxonomically distant for a reference in tick genomic sequence analysis. This study focuses on the de-novo assembly of two R. microplus BAC sequences from the understudied R microplus genome. Based on available R. microplus sequenced resources and comparative analysis, tick genomic structure and functional predictions identify complex gene structures and genomic targets expressed during tick-cattle interaction. Results In our BAC analyses we have assembled, using the correct positioning of BAC end sequences and transcript sequences, two challenging genomic regions. Cot DNA fractions compared to the BAC sequences confirmed a highly repetitive BAC sequence BM-012-E08 and a low repetitive BAC sequence BM-005-G14 which was gene rich and contained short interspersed elements (SINEs. Based directly on the BAC and Cot data comparisons, the genome wide frequency of the SINE Ruka element was estimated. Using a conservative approach to the assembly of the highly repetitive BM-012-E08, the sequence was de-convoluted into three repeat units, each unit containing an 18S, 5.8S and 28S ribosomal RNA (rRNA encoding gene sequence (rDNA, related internal transcribed spacer and complex intergenic region. In the low repetitive BM-005-G14, a novel gene complex was found between to 2 genes on the same strand. Nested in the second intron of a large 9 Kb papilin gene was a helicase gene. This helicase overlapped in two exonic regions with the papilin. Both these genes were shown expressed in different tick life stage important in ectoparasite interaction with the host. Tick specific sequence

  4. NONLINEAR FINITE ELEMENT ANALYSIS OF NONSEISMICALLY DETAILED INTERIOR RC BEAM-COLUMN CONNECTION UNDER REVERSED CYCLIC LOAD

    Directory of Open Access Journals (Sweden)

    Teeraphot Supaviriyakit

    2017-11-01

    Full Text Available This paper presents a nonlinear finite element analysis of non-seismically detailed RC beam column connections under reversed cyclic load. The test of half-scale nonductile reinforced concrete beam-column joints was conducted. The tested specimens represented those of the actual mid-rise reinforced concrete frame buildings designed according to the non-seismic provisions of the ACI building code.  The test results show that specimens representing small and medium column tributary area failed in brittle joint shear while specimen representing large column tributary area failed by ductile flexure though no ductile reinforcement details were provided. The nonlinear finite element analysis was applied to simulate the behavior of the specimens. The finite element analysis employs the smeared crack approach for modeling beam, column and joint, and employs the discrete crack approach for modeling the interface between beam and joint face. The nonlinear constitutive models of reinforced concrete elements consist of coupled tension-compression model to model normal force orthogonal and parallel to the crack and shear transfer model to capture the shear sliding mechanism. The FEM shows good comparison with test results in terms of load-displacement relations, hysteretic loops, cracking process and the failure mode of the tested specimens. The finite element analysis clarifies that the joint shear failure was caused by the collapse of principal diagonal concrete strut.

  5. Recommendations of the wwPDB NMR Validation Task Force

    Science.gov (United States)

    Montelione, Gaetano T.; Nilges, Michael; Bax, Ad; Güntert, Peter; Herrmann, Torsten; Richardson, Jane S.; Schwieters, Charles; Vranken, Wim F.; Vuister, Geerten W.; Wishart, David S.; Berman, Helen M.; Kleywegt, Gerard J.; Markley, John L.

    2013-01-01

    As methods for analysis of biomolecular structure and dynamics using nuclear magnetic resonance spectroscopy (NMR) continue to advance, the resulting 3D structures, chemical shifts, and other NMR data are broadly impacting biology, chemistry, and medicine. Structure model assessment is a critical area of NMR methods development, and is an essential component of the process of making these structures accessible and useful to the wider scientific community. For these reasons, the Worldwide Protein Data Bank (wwPDB) has convened an NMR Validation Task Force (NMR-VTF) to work with the wwPDB partners in developing metrics and policies for biomolecular NMR data harvesting, structure representation, and structure quality assessment. This paper summarizes the recommendations of the NMR-VTF, and lays the groundwork for future work in developing standards and metrics for biomolecular NMR structure quality assessment. PMID:24010715

  6. Enhanced Ethanol and Biogas Production from Pinewood by NMMO Pretreatment and Detailed Biomass Analysis

    Directory of Open Access Journals (Sweden)

    Marzieh Shafiei

    2014-01-01

    Full Text Available N-Methyl morpholine-N-oxide (NMMO is an environmentally friendly and commercially applied cellulose solvent that is suggested for pretreatment of lignocelluloses to improve biofuel productions. However, the underlying mechanisms of the improvements have been poorly understood yet. In an attempt to investigate the mechanisms, pinewood powder and chips were pretreated with 85% (w/w NMMO at 120°C for 1–15 h. The pretreatment improved ethanol production yield from 7.2% (g/g for the untreated wood powder to 68.1–86.1% (g/g and from 1.7% (g/g for the untreated wood chips to 12.6–51.2% (g/g of theoretical yield. Similarly, the biogas yields of untreated wood chips and powder were improved from 21 and 66 (mL/g volatile solids by 3.5–6.8- and 2.6–3.4-folds, respectively. SEM micrographs indicated major increase in the wood porosity by the pretreatment, which would confirm increase in the water swelling capacity as well as enzyme adsorption. The analysis of X-ray diffraction showed considerable reduction in the cellulose crystallinity by the pretreatment, while FTIR spectroscopy results indicated reduction of lignin on the wood surface by the pretreatment.

  7. Research priorities by professional background - A detailed analysis of the James Lind Alliance Priority Setting Partnership.

    Science.gov (United States)

    Arulkumaran, Nishkantha; Reay, Hannah; Brett, Stephen J

    2016-05-01

    The Intensive Care Foundation, in partnership with the James Lind Alliance, has supported a national project to identify and prioritise unanswered questions about adult intensive care that are important to people who have been critically ill, their families, and the health professionals who care for them. We conducted a secondary analysis to explore differences in priorities determined by different respondent groups in order to identify different groups' perceptions of gaps in knowledge. There were two surveys conducted as part of the original project. Survey 1 comprised a single open question to identify important research topics; survey 2 aimed to prioritise these topics using a 10-point Likert scale. In survey 1, despite clear differences in suggestions amongst the respondent groups, themes of comfort/communication and post-ICU rehabilitation were the within the top 2 suggestions across all groups. Patients and relatives suggested research topics to which they could easily relate, whereas there was a greater breadth of suggestions from clinicians. In survey 2, the number of research priorities that received a mode score of 10 varied from 1 to 36. Patients scored 36 out of the 37 topics with a mode score of 10. All other groups scored topics with more discrimination, with the number of topics with a mode score of 10 ranging from 1 to 20. Differences in the proportions of the representative groups are therefore unlikely to have translated to an impartial conclusion. Clinicians, patients, and family members have jointly identified the research priorities for UK ICM practice.

  8. Detailed tail proteomic analysis of axolotl (Ambystoma mexicanum) using an mRNA-seq reference database.

    Science.gov (United States)

    Demircan, Turan; Keskin, Ilknur; Dumlu, Seda Nilgün; Aytürk, Nilüfer; Avşaroğlu, Mahmut Erhan; Akgün, Emel; Öztürk, Gürkan; Baykal, Ahmet Tarık

    2017-01-01

    Salamander axolotl has been emerging as an important model for stem cell research due to its powerful regenerative capacity. Several advantages, such as the high capability of advanced tissue, organ, and appendages regeneration, promote axolotl as an ideal model system to extend our current understanding on the mechanisms of regeneration. Acknowledging the common molecular pathways between amphibians and mammals, there is a great potential to translate the messages from axolotl research to mammalian studies. However, the utilization of axolotl is hindered due to the lack of reference databases of genomic, transcriptomic, and proteomic data. Here, we introduce the proteome analysis of the axolotl tail section searched against an mRNA-seq database. We translated axolotl mRNA sequences to protein sequences and annotated these to process the LC-MS/MS data and identified 1001 nonredundant proteins. Functional classification of identified proteins was performed by gene ontology searches. The presence of some of the identified proteins was validated by in situ antibody labeling. Furthermore, we have analyzed the proteome expressional changes postamputation at three time points to evaluate the underlying mechanisms of the regeneration process. Taken together, this work expands the proteomics data of axolotl to contribute to its establishment as a fully utilized model. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Reference accident (Core disruption accident - safety analysis detailed report no. 11)

    Energy Technology Data Exchange (ETDEWEB)

    1988-01-15

    The PEC safety analysis led to the conclusion that all credible sequences (incident sequences characterized by a frequency of occurrence above 10/sup minus 7/ events per year) are limited to the design basis conditions of components of the plant protection systems, and that none of them leads to a release of mechanical energy or to an extensive damage of the core and primary containment structures event in the case of failure to scram. Nevertheless, as is done in other countries for similar reactors, some events beyond the limits of credibility were considered for the PEC reactor. These were defined on a absolutely hypothetical basis that involves severe core disruption and dynamic loading of primary containment boundary. A series of containments, each having a different role, was designed to mitigate the radiological effects of a postulated core disruptive accident. The final aim was to demonstrate that residual heat can be removed and that the release of radioactivity to the environment is within acceptable limits.

  10. The economics of recovery after pancreatic surgery: detailed cost minimization analysis of an enhanced recovery program.

    Science.gov (United States)

    Kagedan, Daniel J; Devitt, Katharine S; Tremblay St-Germain, Amélie; Ramjaun, Aliya; Cleary, Sean P; Wei, Alice C

    2017-11-01

    Clinical pathways (CPW) are considered safe and effective at decreasing postoperative length of stay (LoS), but the effect on economic costs is uncertain. This study sought to elucidate the effect of a CPW on direct hospitalization costs for patients undergoing pancreaticoduodenectomy (PD). A CPW for PD patients at a single Canadian institution was implemented. Outcomes included LoS, 30-day readmissions, and direct costs of hospital care. A retrospective cost minimization analysis compared patients undergoing PD prior to and following CPW implementation, using a bootstrapped t test and deviation-based cost modeling. 121 patients undergoing PD after CPW implementation were compared to 74 controls. Index LoS was decreased following CPW implementation (9 vs. 11 days, p = 0.005), as was total LoS (10 vs. 11 days, p = 0.003). The mean total cost of postoperative hospitalization per patient decreased in the CPW group ($15,678.45 CAD vs. $25,732.85 CAD, p = 0.024), as was the mean 30-day cost including readmissions ($16,627.15 CAD vs. $29,872.72 CAD, p = 0.016). Areas of significant cost savings included laboratory tests and imaging investigations. CPWs may generate cost savings by reducing unnecessary investigations, and improve quality of care through process standardization and decreasing practice variation. Copyright © 2017 International Hepato-Pancreato-Biliary Association Inc. Published by Elsevier Ltd. All rights reserved.

  11. Initiation of and distributed deformation at and around stylolite interfaces: Insights from detailed microstructural analysis

    Science.gov (United States)

    Ebner, M.; Piazolo, S.; Koehn, D.

    2009-04-01

    In the present contribution we investigate the microstructure of bedding parallel and bedding normal stylolites in carbonate rocks. We focused our study on micro-stylolites which represent an initial stage of this localised pressure solution process as stylolite roughness amplitude is a function of strain. We use electron backscatter diffraction analysis (EBSD) and orientation contrast imaging to address the following issues: (i) What causes the initiation of stylolite interfaces at a submicroscopic scale, (ii) is there distributed deformation around the stylolite interface and (iii) what is the role of the interface (residuum)? Our findings demonstrate that the characteristic stylolite teeth are initiated at a pre-existing heterogeneity in the host-rock. This quenched noise in carbonate rocks is typically composed of clay particles in the submicron scale. In addition, qtz-grains are present along especially pronounced stylolite peaks. The stylolite interface evolves with increasing strain from individual clay particles separated by grain-grain contacts of calcite along the interface to a continuous layer of clay and oxides. Thickness variation of the residuum along the interface is inferred to be strongly influenced by the pre-existing distribution of pinning particles that are more resistant to dissolution. Another important observation is that a shaped preferred orientation (SPO) exists in a halo around the stylolite. This SPO increases with proximity to the stylolite interface. Within this halo, crystal plastic deformation is expressed by subgrain formation with subgrain boundaries usually aligned parallel to shortening direction. Bedding normal (tectonic) stylolites which overprint already compacted beds i.e. with a pre-existing sedimentary SPO parallel to the bedding plane exhibit a SPO at a high angle to the sedimentary SPO. We conclude that stylolite roughness is primarily caused by pre-existing heterogeneities in the host-rock which are more resistant to

  12. Detailed microstructure analysis of as-deposited and etched porous ZnO films

    International Nuclear Information System (INIS)

    Shang, Congcong; Thimont, Yohann; Barnabé, Antoine; Presmanes, Lionel; Pasquet, Isabelle; Tailhades, Philippe

    2015-01-01

    Graphical abstract: - Highlights: • Porous ZnO thin films were deposited by rf magnetron sputtering. • Surface enhancement factors were deduced from geometrical considerations. • Enlargement of the inter-grain spaces have been achieved by HCl chemical etching. • Microstructural parameters were deduced from SEM, AFM and optical measurements. - Abstract: ZnO nanostructured materials in thin film forms are of particular interest for photovoltaic or photocatalysis processes but they suffer from a lack of simple methods for optimizing their microstructure. We have demonstrated that microporous ZnO thin films with optimized inter grain accessibility can be produce by radio frequency magnetron sputtering process and chemical etching with 2.75 mM HCl solution for different duration. The as-deposited ZnO thin films were first characterized in terms of structure, grain size, inter grain space, open cavity depth and total thickness of the film by XRD, AFM, SEM, profilometry and optical measurements. A specific attention was dedicated to the determination of the surface enhancement factor (SEF) by using basic geometrical considerations and images treatments. In addition, the porous fraction and its distribution in the thickness have been estimated thanks to the optical simulation of the experimental UV–Visible–IR spectrums using the Bruggeman dielectric model and cross section SEM images analysis respectively. This study showed that the microstructure of the as-deposited films consists of a dense layer covered by a porous upper layer developing a SEF of 12–13 m 2 m −2 . This two layers architecture is not modified by the etching process. The etching process only affects the upper porous layer in which the overall porosity and the inter-grain space increase with the etching duration. Column diameter and total film thickness decrease at the same time when the films are soaked in the HCl bath. The microporous structure obtained after the etching process could

  13. 2H Solid-State NMR Analysis of the Dynamics and Organization of Water in Hydrated Chitosan

    Directory of Open Access Journals (Sweden)

    Fenfen Wang

    2016-04-01

    Full Text Available Understanding water–biopolymer interactions, which strongly affect the function and properties of biopolymer-based tissue engineering and drug delivery materials, remains a challenge. Chitosan, which is an important biopolymer for the construction of artificial tissue grafts and for drug delivery, has attracted extensive attention in recent decades, where neutralization with an alkali solution can substantially enhance the final properties of chitosan films cast from an acidic solution. In this work, to elucidate the effect of water on the properties of chitosan films, we investigated the dynamics and different states of water in non-neutralized (CTS-A and neutralized (CTS-N hydrated chitosan by mobility selective variable-temperature (VT 2H solid-state NMR spectroscopy. Four distinct types of water exist in all of the samples with regards to dynamic behavior. First, non-freezable, rigid and strongly bound water was found in the crystalline domain at low temperatures. The second component consists of weakly bound water, which is highly mobile and exhibits isotropic motion, even below 260 K. Another type of water undergoes well-defined 180° flips around their bisector axis. Moreover, free water is also present in the films. For the CTS-A sample in particular, another special water species were bounded to acetic acid molecules via strong hydrogen bonding. In the case of CTS-N, the onset of motions of the weakly bound water molecules at 260 K was revealed by 2H-NMR spectroscopy. This water is not crystalline, even below 260 K, which is also the major contribution to the flexibility of chitosan chains and thus toughness of materials. By contrast, such motion was not observed in CTS-A. On the basis of the 2H solid-state NMR results, it is concluded that the unique toughness of CTS-N mainly originates from the weakly bound water as well as the interactions between water and the chitosan chains.

  14. Ratiometric analysis in hyperpolarized NMR (I): test of the two-site exchange model and the quantification of reaction rate constants.

    Science.gov (United States)

    Li, Lin Z; Kadlececk, Stephen; Xu, He N; Daye, Dania; Pullinger, Benjamin; Profka, Harrilla; Chodosh, Lewis; Rizi, Rahim

    2013-10-01

    Conventional methods for the analysis of in vivo hyperpolarized (13) C NMR data from the lactate dehydrogenase (LDH) reaction usually make assumptions on the stability of rate constants and/or the validity of the two-site exchange model. In this study, we developed a framework to test the validity of the assumption of stable reaction rate constants and the two-site exchange model in vivo via ratiometric fitting of the time courses of the signal ratio L(t)/P(t). Our analysis provided evidence that the LDH enzymatic kinetics observed by hyperpolarized NMR are in near-equilibrium and satisfy the two-site exchange model for only a specific time window. In addition, we quantified both the forward and reverse exchange rate constants of the LDH reaction for the transgenic and mouse xenograft models of breast cancer using the ratio fitting method developed, which includes only two modeling parameters and is less sensitive to the influence of instrument settings/protocols, such as flip angles, degree of polarization and tracer dosage. We further compared the ratio fitting method with a conventional two-site exchange modeling method, i.e. the differential equation fitting method, using both the experimental and simulated hyperpolarized NMR data. The ratio fitting method appeared to fit better than the differential equation fitting method for the reverse rate constant on the mouse tumor data, with less relative errors on average, whereas the differential equation fitting method also resulted in a negative reverse rate constant for one tumor. The simulation results indicated that the accuracy of both methods depends on the width of the transport function, noise level and rate constant ratio; one method may be more accurate than the other based on the experimental/biological conditions aforementioned. We were able to categorize our tumor models into specific conditions of the computer simulation and to estimate the errors of rate quantification. We also discussed possible

  15. Strategy for NMR metabolomic analysis of urine in mouse models of obesity- from sample collection to interpretation of acquired data

    Czech Academy of Sciences Publication Activity Database

    Pelantová, Helena; Bugáňová, Martina; Anýž, J.; Železná, Blanka; Maletínská, Lenka; Novák, D.; Haluzík, M.; Kuzma, Marek

    2015-01-01

    Roč. 115, NOV 10 (2015), s. 225-235 ISSN 0731-7085 R&D Projects: GA ČR GA13-14105S; GA MŠk LO1509 Grant - others:OPPC(XE) CZ.2.16/3.1.00/24023 Institutional support: RVO:61388971 ; RVO:61388963 Keywords : NMR metabolomics * Mouse * Obesity Subject RIV: CB - Analytical Chemistry, Separation; CB - Analytical Chemistry, Separation (UOCHB-X) OBOR OECD: Analytical chemistry; Analytical chemistry (UOCHB-X) Impact factor: 3.169, year: 2015

  16. 1H NMR analysis of the heteroassociation of antitumor antibiotics novotrone and actinomycin D in aqueous solution

    International Nuclear Information System (INIS)

    Evstigneev, M.P.; Rozvadovskaya, A.O.; Kisurkin, D.V.; Dehvis, D.B.; Veselkov, A.N.

    2004-01-01

    The heteroassociation of antitumor antibiotics novotrone (NOV) and actinomycin D (AMD) in aqueous solution has been studied by one- and two-dimensional 1 H-NMR spectroscopy (500 MHz) in order to elucidate the molecular mechanism of the action of antibiotics in combination. It has been shown that heterocomplexes become predominant in the mixed solution at r > 12. It is concluded that aromatic antibiotics (e. g. novotrone and actinomycin D) may form energetically stable heteroassociation complexes in aqueous solution and hence affect their medical-biological activity

  17. NSTX Disruption Simulations of Detailed Divertor and Passive Plate Models by Vector Potential Transfer from OPERA Global Analysis Results

    International Nuclear Information System (INIS)

    Titus, P.H.; Avasaralla, S.; Brooks, A.; Hatcher, R.

    2010-01-01

    The National Spherical Torus Experiment (NSTX) project is planning upgrades to the toroidal field, plasma current and pulse length. This involves the replacement of the center-stack, including the inner legs of the TF, OH, and inner PF coils. A second neutral beam will also be added. The increased performance of the upgrade requires qualification of the remaining components including the vessel, passive plates, and divertor for higher disruption loads. The hardware needing qualification is more complex than is typically accessible by large scale electromagnetic (EM) simulations of the plasma disruptions. The usual method is to include simplified representations of components in the large EM models and attempt to extract forces to apply to more detailed models. This paper describes a more efficient approach of combining comprehensive modeling of the plasma and tokamak conducting structures, using the 2D OPERA code, with much more detailed treatment of individual components using ANSYS electromagnetic (EM) and mechanical analysis. This capture local eddy currents and resulting loads in complex details, and allows efficient non-linear, and dynamic structural analyses.

  18. NSTX Disruption Simulations of Detailed Divertor and Passive Plate Models by Vector Potential Transfer from OPERA Global Analysis Results

    Energy Technology Data Exchange (ETDEWEB)

    P. H. Titus, S. Avasaralla, A.Brooks, R. Hatcher

    2010-09-22

    The National Spherical Torus Experiment (NSTX) project is planning upgrades to the toroidal field, plasma current and pulse length. This involves the replacement of the center-stack, including the inner legs of the TF, OH, and inner PF coils. A second neutral beam will also be added. The increased performance of the upgrade requires qualification of the remaining components including the vessel, passive plates, and divertor for higher disruption loads. The hardware needing qualification is more complex than is typically accessible by large scale electromagnetic (EM) simulations of the plasma disruptions. The usual method is to include simplified representations of components in the large EM models and attempt to extract forces to apply to more detailed models. This paper describes a more efficient approach of combining comprehensive modeling of the plasma and tokamak conducting structures, using the 2D OPERA code, with much more detailed treatment of individual components using ANSYS electromagnetic (EM) and mechanical analysis. This capture local eddy currents and resulting loads in complex details, and allows efficient non-linear, and dynamic structural analyses.

  19. A detailed description of the analysis of the decay of neutral kaons to $\\pi^+ \\pi^-$ in the CPLEAR experiment

    CERN Document Server

    Apostolakis, Alcibiades J; Backenstoss, Gerhard; Bargassa, P; Behnke, O; Benelli, A; Bertin, V; Blanc, F; Bloch, P; Carlson, P J; Carroll, M; Cawley, E; Chertok, M B; Danielsson, M; Dejardin, M; Derré, J; Ealet, A; Eleftheriadis, C; Fetscher, W; Fidecaro, Maria; Filipcic, A; Francis, D; Fry, J; Gabathuler, Erwin; Gamet, R; Gerber, H J; Go, A; Haselden, A; Hayman, P J; Henry-Coüannier, F; Hollander, R W; Jon-And, K; Kettle, P R; Kokkas, P; Kreuger, R; Le Gac, R; Leimgruber, F; Mandic, I; Manthos, N; Marel, Gérard; Mikuz, M; Miller, J; Montanet, François; Müller, A; Nakada, Tatsuya; Pagels, B; Papadopoulos, I M; Pavlopoulos, P; Polivka, G; Rickenbach, R; Roberts, B L; Ruf, T; Sakelliou, L; Schäfer, M; Schaller, L A; Schietinger, T; Schopper, A; Tauscher, Ludwig; Thibault, C; Touchard, F; Touramanis, C; van Eijk, C W E; Vlachos, S; Weber, P; Wigger, O; Wolter, M; Yéche, C; Zavrtanik, D; Zimmerman, D

    2000-01-01

    A detailed description is given of the analysis of neutral kaons decaying to \\pipi , based on the complete data sample collected with the CPLEAR experiment.Using a novel approach involving initially strangeness-tagged \\kn\\ and \\knb ,the time-dependent decay rate asymmetry has been measured. This asymmetry, resulting from the interference between the \\ks\\and \\kl\\ decay amplitudes, has enabled both the magnitudeand phase of the CP-violation parameter, \\ita , to be measured, with aprecision comparable to that of the current world average values.

  20. A Chemical Eight Group Separation Method for Routine Use in Gamma Spectrometric Analysis. II. Detailed analytical schema

    Energy Technology Data Exchange (ETDEWEB)

    Samsahl, K

    1961-06-15

    A detailed ion-exchange procedure for the separation of chemical elements in eight groups suitable for subsequent gamma spectrometric analysis is described. The method has been in use for gamma spectrometry of some inorganic - but mostly organic - samples for one year. The separation time for inorganic samples, is usually about 1.5 hours and for organic samples as least 2 hours. One man can separate and count three samples per day. In comparative measurements of short-lived isotopes in biological material 10-12 elements can be analysed thus making possible 30 - 35 determinations per day for one man.