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Sample records for advanced solid-state 13c

  1. Chemical structures of swine-manure chars produced under different carbonization conditions investigated by advanced solid-state 13C nuclear magnetic resonance (NMR) spectroscopy

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Two types of swine manure chars, hydrothermally-produced hydrochar and slow-pyrolysis pyrochar, and their raw swine manure solid were characterized using advanced 13C solid-state nuclear magnetic resonance (NMR) spectroscopy. Compared with the parent raw swine manure, both hydrochars and pyrochar di...

  2. Functional groups identified by solid state 13C NMR spectroscopy

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Animal manure is generally high in organic matter intensity so it is well suitable for 13C nuclear magnetic resonance (NMR) analysis. Solid-state 13C NMR techniques used in characterizing organic matter and its components include, but are not limited to, cross-polarization /magic angle spinning (CP...

  3. Chemical and nanometer-scale structure of kerogen and its change during thermal maturation investigated by advanced solid-state 13C NMR spectroscopy

    USGS Publications Warehouse

    Mao, J.; Fang, X.; Lan, Y.; Schimmelmann, A.; Mastalerz, Maria; Xu, L.; Schmidt-Rohr, K.

    2010-01-01

    We have used advanced and quantitative solid-state nuclear magnetic resonance (NMR) techniques to investigate structural changes in a series of type II kerogen samples from the New Albany Shale across a range of maturity (vitrinite reflectance R0 from 0.29% to 1.27%). Specific functional groups such as CH3, CH2, alkyl CH, aromatic CH, aromatic C-O, and other nonprotonated aromatics, as well as "oil prone" and "gas prone" carbons, have been quantified by 13C NMR; atomic H/C and O/C ratios calculated from the NMR data agree with elemental analysis. Relationships between NMR structural parameters and vitrinite reflectance, a proxy for thermal maturity, were evaluated. The aromatic cluster size is probed in terms of the fraction of aromatic carbons that are protonated (???30%) and the average distance of aromatic C from the nearest protons in long-range H-C dephasing, both of which do not increase much with maturation, in spite of a great increase in aromaticity. The aromatic clusters in the most mature sample consist of ???30 carbons, and of ???20 carbons in the least mature samples. Proof of many links between alkyl chains and aromatic rings is provided by short-range and long-range 1H-13C correlation NMR. The alkyl segments provide most H in the samples; even at a carbon aromaticity of 83%, the fraction of aromatic H is only 38%. While aromaticity increases with thermal maturity, most other NMR structural parameters, including the aromatic C-O fractions, decrease. Aromaticity is confirmed as an excellent NMR structural parameter for assessing thermal maturity. In this series of samples, thermal maturation mostly increases aromaticity by reducing the length of the alkyl chains attached to the aromatic cores, not by pronounced growth of the size of the fused aromatic ring clusters. ?? 2010 Elsevier Ltd. All rights reserved.

  4. Chemical structures of coal lithotypes before and after CO2 adsorption as investigated by advanced solid-state 13C nuclear magnetic resonance spectroscopy

    USGS Publications Warehouse

    Cao, X.; Mastalerz, Maria; Chappell, M.A.; Miller, L.F.; Li, Y.; Mao, J.

    2011-01-01

    Four lithotypes (vitrain, bright clarain, clarain, and fusain) of a high volatile bituminous Springfield Coal from the Illinois Basin were characterized using advanced solid-state 13C nuclear magnetic resonance (NMR) spectroscopy. The NMR techniques included quantitative direct polarization/magic angle spinning (DP/MAS), cross polarization/total sideband suppression (CP/TOSS), dipolar dephasing, CHn selection, and recoupled C-H long-range dipolar dephasing techniques. The lithotypes that experienced high-pressure CO2 adsorption isotherm analysis were also analyzed to determine possible changes in coal structure as a result of CO2 saturation at high pressure and subsequent evacuation. The main carbon functionalities present in original vitrain, bright clarain, clarain and fusain were aromatic carbons (65.9%-86.1%), nonpolar alkyl groups (9.0%-28.9%), and aromatic C-O carbons (4.1%-9.5%). Among these lithotypes, aromaticity increased in the order of clarain, bright clarain, vitrain, and fusain, whereas the fraction of alkyl carbons decreased in the same order. Fusain was distinct from other three lithotypes in respect to its highest aromatic composition (86.1%) and remarkably small fraction of alkyl carbons (11.0%). The aromatic cluster size in fusain was larger than that in bright clarain. The lithotypes studied responded differently to high pressure CO2 saturation. After exposure to high pressure CO2, vitrain and fusain showed a decrease in aromaticity but an increase in the fraction of alkyl carbons, whereas bright clarain and clarain displayed an increase in aromaticity but a decrease in the fraction of alkyl carbons. Aromatic fused-rings were larger for bright clarain but smaller for fusain in the post-CO2 adsorption samples compared to the original lithotypes. These observations suggested chemical CO2-coal interactions at high pressure and the selectivity of lithotypes in response to CO2 adsorption. ?? 2011 Elsevier B.V.

  5. Dipolar-coupling-mediated total correlation spectroscopy in solid-state 13C NMR: Selection of individual 13C- 13C dipolar interactions

    NASA Astrophysics Data System (ADS)

    Spano, Justin; Wi, Sungsool

    2010-06-01

    Herein is described a useful approach in solid-state NMR, for selecting homonuclear 13C- 13C spin pairs in a multiple- 13C homonuclear dipolar coupled spin system. This method builds upon the zero-quantum (ZQ) dipolar recoupling method introduced by Levitt and coworkers (Marin-Montesinos et al., 2006 [30]) by extending the originally introduced one-dimensional (1D) experiment into a two-dimensional (2D) method with selective irradiation scheme, while moving the 13C- 13C mixing scheme from the transverse to the longitudinal mode, together with a dramatic improvement in the proton decoupling efficiency. Selective spin-pair recoupling experiments incorporating Gaussian and cosine-modulated Gaussian pulses for inverting specific spins were performed, demonstrating the ability to detect informative, simplified/individualized, long-range 13C- 13C homonuclear dipolar coupling interactions more accurately by removing less informative, stronger, short-range 13C- 13C interactions from 2D correlation spectra. The capability of this new approach was demonstrated experimentally on uniformly 13C-labeled Glutamine and a tripeptide sample, GAL.

  6. 1H and 13C Solid-state NMR of Gossypium barbadense (Pima) Cotton

    Technology Transfer Automated Retrieval System (TEKTRAN)

    The interaction of water with cellulose and its influence on the nuclear spin dynamics in G. barbadense (Pima) cotton were investigated by 1H and 13C solid-state NMR techniques. 1H spin diffusion results from a Goldman-Shen experiment indicate that the water is multilayered. 1H MAS experiments pro...

  7. 1H and 13C Solid-state NMR of G. barbadense (Pima) Cotton

    Technology Transfer Automated Retrieval System (TEKTRAN)

    The interaction of water with cellulose and its influence on the nuclear spin dynamics in G. barbadense (Pima) cotton were investigated with 1H and 13C solid-state NMR techniques. 1H spin diffusion results from a Goldman-Shen experiment indicate that the water is multilayered. 1H MAS experiment...

  8. (13) C-TmDOTA as versatile thermometer compound for solid-state NMR of hydrated lipid bilayer membranes.

    PubMed

    Umegawa, Yuichi; Tanaka, Yuya; Nobuaki, Matsumori; Murata, Michio

    2016-03-01

    Recent advances in solid-state nuclear magnetic resonance (NMR) techniques, such as magic angle spinning and high-power decoupling, have dramatically increased the sensitivity and resolution of NMR. However, these NMR techniques generate extra heat, causing a temperature difference between the sample in the rotor and the variable temperature gas. This extra heating is a particularly crucial problem for hydrated lipid membrane samples. Thus, to develop an NMR thermometer that is suitable for hydrated lipid samples, thulium-1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetate (TmDOTA) was synthesized and labeled with (13) C (i.e., (13) C-TmDOTA) to increase the NMR sensitivity. The complex was mixed with a hydrated lipid membrane, and the system was subjected to solid-state NMR and differential scanning calorimetric analyses. The physical properties of the lipid bilayer and the quality of the NMR spectra of the membrane were negligibly affected by the presence of (13) C-TmDOTA, and the (13) C chemical shift of the complex exhibited a large-temperature dependence. The results demonstrated that (13) C-TmDOTA could be successfully used as a thermometer to accurately monitor temperature changes induced by (1) H decoupling pulses and/or by magic angle spinning and the temperature distribution of the sample inside the rotor. Thus, (13) C-TmDOTA was shown to be a versatile thermometer for hydrated lipid assemblies. Copyright © 2015 John Wiley & Sons, Ltd. PMID:26460094

  9. 2H-DNP-enhanced 2H–13C solid-state NMR correlation spectroscopy

    PubMed Central

    Maly, Thorsten; Andreas, Loren B.; Smith, Albert A.

    2015-01-01

    Perdeuteration of biological macromolecules for magic angle spinning solid-state NMR spectroscopy can yield high-resolution 2H–13C correlation spectra and the method is therefore of great interest for the structural biology community. Here we demonstrate that the combination of sample deuteration and dynamic nuclear polarization yields resolved 2H–13C correlation spectra with a signal enhancement of ε ≥ 700 compared to a spectrum recorded with microwaves off and otherwise identical conditions. To our knowledge, this is the first time that 2H-DNP has been employed to enhance MAS-NMR spectra of a biologically relevant system. The DNP process is studied using several polarizing agents and the technique is applied to obtain 2H–13C correlation spectra of U-[2H, 13C] proline. PMID:20458422

  10. Benchmarks for the 13C NMR chemical shielding tensors in peptides in the solid state

    NASA Astrophysics Data System (ADS)

    Czernek, Jiří; Pawlak, Tomasz; Potrzebowski, Marek J.

    2012-02-01

    The benchmark set is proposed, which comprises 126 principal elements of chemical shielding tensors, and the respective isotropic chemical shielding values, of all 42 13C nuclei in crystalline Tyr-D-Ala-Phe and Tyr-Ala-Phe tripeptides with known, but highly dissimilar structures. These data are obtained by both the NMR measurements and the density functional theory in the pseudopotential plane-wave scheme. Using the CASTEP program, several computational strategies are employed, for which the level of agreement between calculations and experiment is established. This set is mainly intended for the validation of methods capable of predicting the 13C NMR parameters in solid-state systems.

  11. Quantification of protein secondary structure by (13)C solid-state NMR.

    PubMed

    Andrade, Fabiana Diuk; Forato, Lucimara Aparecida; Bernardes Filho, Rubens; Colnago, Luiz Alberto

    2016-05-01

    High-resolution (13)C solid-state NMR stands out as one of the most promising techniques to solve the structure of insoluble proteins featuring biological and technological importance. The simplest nuclear magnetic resonance (NMR) spectroscopy method to quantify the secondary structure of proteins uses the areas of carbonyl and alpha carbon peaks. The quantification obtained by fitting procedures depends on the assignment of the peaks to the structure, type of line shape, number of peaks to be used, and other parameters that are set by the operator. In this paper, we demonstrate that the analysis of (13)C NMR spectra by a pattern recognition method-based on the singular value decomposition (SVD) regression, which does not depend on the operator-shows higher correlation coefficients for α-helix and β-sheet (0.96 and 0.91, respectively) than Fourier transform infrared spectroscopy (FTIR) method. Therefore, the use of (13)C solid-state NMR spectra and SVD is a simple and reliable method for quantifying the secondary structures of insoluble proteins in solid-state. PMID:27068694

  12. (13)C NMR assignments of regenerated cellulose from solid-state 2D NMR spectroscopy.

    PubMed

    Idström, Alexander; Schantz, Staffan; Sundberg, Johan; Chmelka, Bradley F; Gatenholm, Paul; Nordstierna, Lars

    2016-10-20

    From the assignment of the solid-state (13)C NMR signals in the C4 region, distinct types of crystalline cellulose, cellulose at crystalline surfaces, and disordered cellulose can be identified and quantified. For regenerated cellulose, complete (13)C assignments of the other carbon regions have not previously been attainable, due to signal overlap. In this study, two-dimensional (2D) NMR correlation methods were used to resolve and assign (13)C signals for all carbon atoms in regenerated cellulose. (13)C-enriched bacterial nanocellulose was biosynthesized, dissolved, and coagulated as highly crystalline cellulose II. Specifically, four distinct (13)C signals were observed corresponding to conformationally different anhydroglucose units: two signals assigned to crystalline moieties and two signals assigned to non-crystalline species. The C1, C4 and C6 regions for cellulose II were fully examined by global spectral deconvolution, which yielded qualitative trends of the relative populations of the different cellulose moieties, as a function of wetting and drying treatments. PMID:27474592

  13. 1H to 13C Energy Transfer in Solid State NMR Spectroscopy of Natural Organic Systems

    NASA Astrophysics Data System (ADS)

    Berns, Anne E.; Conte, Pellegrino

    2010-05-01

    Cross polarization (CP) magic angle spinning (MAS) 13C-NMR spectroscopy is a solid state NMR technique widely used to study chemical composition of organic materials with low or no solubility in the common deuterated solvents used to run liquid state NMR experiments. Based on the magnetization transfer from abundant nuclei (with spin of 1 -2) having a high gyromagnetic ratio (γ), such as protons, to the less abundant 13C nuclei with low γ values, 13C-CPMAS NMR spectroscopy is often applied in environmental chemistry to obtain quantitative information on the chemical composition of natural organic matter (NOM) (Conte et al., 2004), although its quantitative assessment is still matter of heavy debates. Many authors (Baldock et al., 1997; Conte et al., 1997, 2002; Dria et al., 2002; Kiem et al., 2000; Kögel-Knabner, 2000; Preston, 2001), reported that the application of appropriate instrument setup as well as the use of special pulse sequences and correct spectra elaboration may provide signal intensities that are directly proportional to the amount of nuclei creating a NMR signal. However, many other papers dealt with the quantitative unsuitability of 13C-CPMAS NMR spectroscopy. Among those, Mao et al. (2000), Smernik and Oades (2000 a,b), and Preston (2001) reported that cross-polarized NMR techniques may fail in a complete excitation of the 13C nuclei. In fact, the amount of observable carbons via 13C-CPMAS NMR spectroscopy appeared, in many cases, lower than that measured by a direct observation of the 13C nuclei. As a consequence, cross-polarized NMR techniques may provide spectra where signal distribution may not be representative of the quantitative distribution of the different natural organic matter components. Cross-polarization is obtained after application of an initial 90° x pulse on protons and a further spin lock pulse (along the y axis) having a fixed length (contact time) for both nuclei (1H and 13C) once the Hartmann-Hahn condition is matched

  14. (13)C and (15)N solid-state NMR studies on albendazole and cyclodextrin albendazole complexes.

    PubMed

    Ferreira, M João G; García, A; Leonardi, D; Salomon, Claudio J; Lamas, M Celina; Nunes, Teresa G

    2015-06-01

    (13)C and (15)N solid-state nuclear magnetic resonance (NMR) spectra were recorded from albendazole (ABZ) and from ABZ:β-cyclodextrin, ABZ:methyl-β-cyclodextrin, ABZ:hydroxypropyl-β-cyclodextrin and ABZ:citrate-β-cyclodextrin, which were prepared by the spray-drying technique. ABZ signals were typical of a crystalline solid for the pure drug and of an amorphous compound obtained from ABZ:cyclodextrin samples. Relevant spectral differences were correlated with chemical interaction between ABZ and cyclodextrins. The number and type of complexes revealed a strong dependence on the cyclodextrin group substituent. Solid-state NMR data were consistent with the presence of stable inclusion complexes. PMID:25843843

  15. Solid state 13C NMR characterisation study on fourth generation Ziegler-Natta catalysts.

    PubMed

    Heikkinen, Harri; Liitiä, Tiina; Virkkunen, Ville; Leinonen, Timo; Helaja, Tuulamari; Denifl, Peter

    2012-01-01

    In this study, solid state (13)C NMR spectroscopy was utilised to characterize and identify the metal-ester coordination in active fourth generation (phthalate) Ziegler-Natta catalysts. It is known that different donors affect the active species in ZN catalysts. However, there is still limited data available of detailed molecular information how the donors and the active species are interplaying. One of the main goals of this work was to get better insight into the interactions of donor and active species. Based on the anisotropy tensor values (δ(11), δ(22), δ(33)) from low magic-angle spinning (MAS) (13)C NMR spectra in combination with chemical shift anisotropy (CSA) calculations (δ(aniso) and η), both the coordinative metal (Mg/Ti) and the symmetry of this interaction between metal and the internal donor in the active catalyst (MgCl(2)/TiCl(4)/electron donor) system could be identified. PMID:22425229

  16. Quantifying the chemical composition of soil organic carbon with solid-state 13C NMR

    NASA Astrophysics Data System (ADS)

    Baldock, J. A.; Sanderman, J.

    2011-12-01

    The vulnerability of soil organic carbon (SOC) to biological decomposition and mineralisation to CO2 is defined at least partially by its chemical composition. Highly aromatic charcoal-like SOC components are more stable to biological decomposition than other forms of carbon including cellulose. Solid-state 13C NMR has gained wide acceptance as a method capable of defining SOC chemical composition and mathematical fitting processes have been developed to estimate biochemical composition. Obtaining accurate estimates depends on an ability to quantitatively detect all carbon present in a sample. Often little attention has been paid to defining the proportion of organic carbon present in a soil that is observable in solid-state 13C NMR analyses of soil samples. However, if such data is to be used to inform carbon cycling studies, it is critical that quantitative assessments of SOC observability be undertaken. For example, it is now well established that a significant discrimination exists against the detection of the low proton content polyaromatic structures typical of charcoal using cross polarisation 13C NMR analyses. Such discrimination does not exist where direct polarisation analyses are completed. In this study, the chemical composition of SOC as defined by cross polarisation and direct polarisation13C NMR analyses will be compared for Australian soils collected from under a diverse range of agricultural managements and climatic conditions. Results indicate that where significant charcoal C contents exist, it is highly under-represented in the acquired CP spectra. For some soils, a discrimination against alkyl carbon was also evident. The ability to derive correction factors to compensate for such discriminations will be assessed and presented.

  17. Characterisation of coke from FCC catalysts by solid state {sup 13}C NMR and mass spectrometry

    SciTech Connect

    Andresen, J.M.; McGhee, B.; Snape, C.E.

    1995-12-31

    Coke has been concentrated by demineralisation from deactivated FCC catalysts from both refinery operations with actual feeds and MAT tests using n-hexadecane to facilitate detailed characterisation by solid state {sup 13}C NMR and mass spectrometry. All the catalysts investigated contained about 1% w/w carbon. As for solid fuels, the use of a low-field spectrometer for solid state {sup 13}C NMR in conjunction with the single pulse excitation (SPE or Bloch decay) technique has enabled quantitative carbon skeletal parameters to be obtained for the cokes. Internal standard measurements demonstrated that most of the carbon was observed by SPE and, therefore, NMR-invisible graphitic layers are not thought to be major structural features of the cokes. Differences in feedstock composition were reflected in the structure of the refinery cokes with the aromatic nuclei from a residue feed (5% Conradson carbon) corresponding to 15-20 peri-condensed aromatic rings and being more highly condensed than those from a hydrotreated vacuum gas oil. Mass spectrometry (EI, CI and FIMS) has confirmed that the refinery cokes are highly condensed, but those obtained from n-hexadecane in the MAT tests displayed significant aliphatic character.

  18. Molecular structure of crude beeswax studied by solid-state 13C NMR

    PubMed Central

    Kameda, Tsunenori

    2004-01-01

    13C Solid-state NMR experiments were performed to investigate the structure of beeswax in the native state (crude beeswax) for the first time. From quantitative direct polarization 13C MAS NMR spectrum, it was found that the fraction of internal-chain methylene (int-(CH2)) component compared to other components of crude beeswax was over 95%. The line shape of the int-(CH2) carbon resonance region was comprehensively analyzed in terms of NMR chemical shift. The 13C broad peak component covering from 31 to 35ppm corresponds to int-(CH2) carbons with trans conformation in crystalline domains, whereas the sharp signal at 30.3 ppm corresponds to gauche conformation in the non-crystalline domain. From peak deconvolution of the aliphatic region, it was found that over 85% of the int-(CH2) has a crystal structure and several kinds of molecular packing for int-(CH2), at least three, exist in the crystalline domain. Abbreviation: NMR nuclear magnetic resonance int-(CH2) internal-chain methylene CP cross-polarization MAS magic angle spinning PMID:15861244

  19. 13C solid-state NMR analysis of heterogeneous structure of beeswax in native state

    NASA Astrophysics Data System (ADS)

    Kameda, Tsunenori

    2005-12-01

    I investigated the molecular structure of natural wax from Japanese bees (Apis cerana japonica) in its native state (neither purified nor recrystallized) by 13C and 1H solid-state NMR. Two strong 13C peaks at 32.9 and 34.0 ppm were attributed to signals from internal-chain methylene carbons [int-(CH2)] in two types of crystal form. The peak at 32.9 ppm was assigned to an orthorhombic crystal form, and that at 34.0 ppm was assigned to a triclinic or monoclinic form. In both crystalline regions, bi-exponential decay of 13C spin-lattice relaxation [T1(C)] for the crystalline peaks due to chain diffusion was observed. 1H spin-lattice relaxation [T1(H)] values for protons of the CH3 group and for int-(CH2) in the crystalline and amorphous regions were identical; this was interpreted as being due to averaging of the T1(H) relaxation rates via spin diffusion. In contrast, although the T_{{1}_{\\rho}}(H) decay curves for protons of the CH3 group and for int-(CH2) in the amorphous and orthorhombic forms were almost identical, those of the triclinic or monoclinic forms were different. This unhomogeneous character of T_{{1}_{\\rho}}(H) was interpreted as resulting from differences in the molecular composition of each crystal form. Moreover, two components with long and short 1H spin-spin relaxation [T2(H)] values, arising from the mobile and rigid phases, respectively, were observed at above about -30 °C.

  20. Quantitative solid-state 13C NMR with signal enhancement by multiple cross polarization

    NASA Astrophysics Data System (ADS)

    Johnson, Robert L.; Schmidt-Rohr, Klaus

    2014-02-01

    A simple new method is presented that yields quantitative solid-state magic-angle spinning (MAS) 13C NMR spectra of organic materials with good signal-to-noise ratios. It achieves long (>10 ms) cross polarization (CP) from 1H without significant magnetization losses due to relaxation and with a moderate duty cycle of the radio-frequency irradiation, by multiple 1-ms CP periods alternating with 1H spin-lattice relaxation periods that repolarize the protons. The new method incorporates previous techniques that yield less distorted CP/MAS spectra, such as a linear variation (“ramp”) of the radio-frequency field strength, and it overcomes their main limitation, which is T1ρ relaxation of the spin-locked 1H magnetization. The ramp of the radio-frequency field strength and the asymptotic limit of cross polarization makes the spectral intensity quite insensitive to the exact field strengths used. The new multiCP pulse sequence is a “drop-in” replacement for previous CP methods and produces no additional data-processing burden. Compared to the only reliable quantitative 13C NMR method for unlabeled solids previously available, namely direct-polarization NMR, the measuring time is reduced by more than a factor of 50, enabling higher-throughput quantitative NMR studies. The new multiCP technique is validated with 14-kHz MAS on amino-acid derivatives, plant matter, a highly aromatic humic acid, and carbon materials made by low-temperature pyrolysis.

  1. Characterization of Stratum Corneum Molecular Dynamics by Natural-Abundance 13C Solid-State NMR

    PubMed Central

    Bouwstra, Joke A.; Sparr, Emma; Topgaard, Daniel

    2013-01-01

    Despite the enormous potential for pharmaceutical applications, there is still a lack of understanding of the molecular details that can contribute to increased permeability of the stratum corneum (SC). To investigate the influence of hydration and heating on the SC, we record the natural-abundance 13C signal of SC using polarization transfer solid-state NMR methods. Resonance lines from all major SC components are assigned. Comparison of the signal intensities obtained with the INEPT and CP pulse sequences gives information on the molecular dynamics of SC components. The majority of the lipids are rigid at 32°C, and those lipids co-exist with a small pool of mobile lipids. The ratio between mobile and rigid lipids increases with hydration. An abrupt change of keratin filament dynamics occurs at RH = 80–85%, from completely rigid to a structure with rigid backbone and mobile protruding terminals. Heating has a strong effect on the lipid mobility, but only a weak influence on the keratin filaments. The results provide novel molecular insight into how the SC constituents are affected by hydration and heating, and improve the understanding of enhanced SC permeability, which is associated with elevated temperatures and SC hydration. PMID:23626744

  2. Solid-state 13C NMR study of cholesteric liquid crystals.

    PubMed

    Yamada, Kazuhiko; Marumo, Kazuhiro; Kang, Sungmin; Deguchi, Kenzo; Nakai, Toshihito; Shimizu, Tadashi; Watanabe, Junji

    2013-12-19

    We investigated the structural behavior of cholesteric liquid crystals of 4-(hexyloxy)-4'-cyanobiphenyl (6OCB) in an 11.7 T magnetic field by solid-state (13)C nuclear magnetic resonance. Five 6OCB cholesteric liquid crystal systems were prepared with 4-methoxyphenyl 3,4-O-isopropylidene-2,6-bis-O-(4-methylbenzoyl)-β-d-galactopyranoside (CR), in which 6OCB was doped with 0.51, 1.00, 2.34, 5.60, and 6.47 mol % CR, giving products with helical twisting powers (HTPs) of 0.28, 0.54, 1.27, 3.05, and 3.52 μm(-1), respectively. Analyses of the alignment-induced shifts showed that the liquid crystals directors in pure 6OCB and 6OCB doped with 0.51 and 1.00 mol % CR become aligned with the 11.7 T magnetic field direction. However, 6OCB doped with 2.34, 5.60, and 6.47 mol % CR retained their cholesteric structures when the magnetic field was applied. The critical HTP value for resisting realignment by magnetic field was estimated to be approximately 1.27 μm(-1). A biaxiality of the phase was partially considered during spectral simulations, although the molecular shape of 6OCB can be defined as cylinderical when it is rotating rapidly. Our current understanding is that the order parameters in the cholesteric structures are not uniform; i.e., the molecular directors already aligned almost perpendicular to the magnetic field are significantly perturbed by the external field. PMID:24188010

  3. Solid-State 13C Nuclear Magnetic Resonance Characterization of Cellulose in the Cell Walls of Arabidopsis thaliana Leaves.

    PubMed Central

    Newman, R. H.; Davies, L. M.; Harris, P. J.

    1996-01-01

    Solid-state 13C nuclear magnetic resonance was used to characterize the molecular ordering of cellulose in a cell-wall preparation containing mostly primary walls obtained from the leaves of Arabidopsis thaliana. Proton and 13C spin relaxation time constants showed that the cellulose was in a crystalline rather than a paracrystalline state or amorphous state. Cellulose chains were distributed between the interiors (40%) and surfaces (60%) of crystallites, which is consistent with crystallite cross-sectional dimensions of about 3 nm. Digital resolution enhancement revealed signals indicative of triclinic and monoclinic crystalline forms of cellulose mixed in similar proportions. Of the five nuclear spin relaxation processes used, proton rotating-frame relaxation provided the clearest distinction between cellulose and other cell-wall components for purposes of editing solid-state 13C nuclear magnetic resonance spectra. PMID:12226303

  4. Comprehensive signal assignment of 13C-labeled lignocellulose using multidimensional solution NMR and 13C chemical shift comparison with solid-state NMR.

    PubMed

    Komatsu, Takanori; Kikuchi, Jun

    2013-09-17

    A multidimensional solution NMR method has been developed using various pulse programs including HCCH-COSY and (13)C-HSQC-NOESY for the structural characterization of commercially available (13)C labeled lignocellulose from potatoes (Solanum tuberosum L.), chicory (Cichorium intybus), and corn (Zea mays). This new method allowed for 119 of the signals in the (13)C-HSQC spectrum of lignocelluloses to be assigned and was successfully used to characterize the structures of lignocellulose samples from three plants in terms of their xylan and xyloglucan structures, which are the major hemicelluloses in angiosperm. Furthermore, this new method provided greater insight into fine structures of lignin by providing a high resolution to the aromatic signals of the β-aryl ether and resinol moieties, as well as the diastereomeric signals of the β-aryl ether. Finally, the (13)C chemical shifts assigned in this study were compared with those from solid-state NMR and indicated the presence of heterogeneous dynamics in the polysaccharides where rigid cellulose and mobile hemicelluloses moieties existed together. PMID:24010724

  5. Chemical structural studies of natural lignin by dipolar dephasing solid-state 13C nuclear magnetic resonance

    USGS Publications Warehouse

    Hatcher, P.G.

    1987-01-01

    Two natural lignins, one from a gymnosperm wood the other from angiosperm wood, were examined by conventional solid-state and dipolar dephasing 13C nuclear magnetic resonance (NMR) techniques. The results obtained from both techniques show that the structure of natural lignins is consistent with models of softwood and hardwood lignin. The dipolar dephasing NMR data provide a measure of the degree of substitution on aromatic rings which is consistent with the models. ?? 1987.

  6. Solid-state 13C NMR analysis of Lower Cretaceous Baganuur (Mongolia) lignite

    NASA Astrophysics Data System (ADS)

    Erdenetsogt, B.; Lee, I.; Lee, S.; Ko, Y.

    2009-12-01

    The transformation of plant matter into peat and coal has two steps, called the biochemical and geochemical stages of coalification. Biochemical coalification begins with the accumulation of dead vegetable matter and ends at the rank of subbituminous coal. The rank of Baganuur lignite ranges from lignite to subbituminous coal. It is transition between biochemical and physico-chemical coalification stages. The changes of chemical structure of coal during the transition between above mentioned two stages were studied by solid state CP/MAS 13C NMR. The most predominant alteration is the disappearance of the resonances from oxygenated aliphatic carbons (63 ppm), protonated aromatic carbons (114 ppm), oxygen-substituted aromatic carbons (144 ppm) and carbonyl carbons (195 ppm). In addition, the intensity of resonances from methoxyl carbons (56 ppm) and oxygenated aliphatic carbons (72 ppm) decreased. While the intensities of resonance from aliphatic (30 ppm), protonated aromatic (125 ppm) and carboxyl carbon (174 ppm) increased or remained almost constant. The relative percent of O-substituted aromatic carbons decreased by ~25% mainly due to the intensity loss of the peak at 144 ppm, indicating removal of O-containing functional groups substituted to aromatic carbons. It is consistent with the decreased relative percent (~75%) of the peak at 114 ppm from protonated aromatic carbons nearby oxygen-substituted aromatic carbons. In addition, the resonance from 125 ppm was shifted to 128 ppm and its relative area increased by ~20%, indicating replacement of O-substituent of aromatic rings by hydrogen or carbon. Protonated aromatic carbons at least two bond away from an oxygen-substituted aromatic carbons give a resonance at 125 ppm and carbon-substituted aromatic carbons give a resonance at 130-132 ppm. With the increase relative percent of C-substituted aromatic carbons, their resonance were overlapped with protonated aromatic carbons and shifted to higher ppm. A decreasing

  7. Accurate measurements of {sup 13}C-{sup 13}C distances in uniformly {sup 13}C-labeled proteins using multi-dimensional four-oscillating field solid-state NMR spectroscopy

    SciTech Connect

    Straasø, Lasse Arnt; Nielsen, Jakob Toudahl; Bjerring, Morten; Nielsen, Niels Chr.; Khaneja, Navin

    2014-09-21

    Application of sets of {sup 13}C-{sup 13}C internuclear distance restraints constitutes a typical key element in determining the structure of peptides and proteins by magic-angle-spinning solid-state NMR spectroscopy. Accurate measurements of the structurally highly important {sup 13}C-{sup 13}C distances in uniformly {sup 13}C-labeled peptides and proteins, however, pose a big challenge due to the problem of dipolar truncation. Here, we present novel two-dimensional (2D) solid-state NMR experiments capable of extracting distances between carbonyl ({sup 13}C′) and aliphatic ({sup 13}C{sub aliphatic}) spins with high accuracy. The method is based on an improved version of the four-oscillating field (FOLD) technique [L. A. Straasø, M. Bjerring, N. Khaneja, and N. C. Nielsen, J. Chem. Phys. 130, 225103 (2009)] which circumvents the problem of dipolar truncation, thereby offering a base for accurate extraction of internuclear distances in many-spin systems. The ability to extract reliable accurate distances is demonstrated using one- and two-dimensional variants of the FOLD experiment on uniformly {sup 13}C,{sup 15}N-labeled-L-isoleucine. In a more challenging biological application, FOLD 2D experiments are used to determine a large number of {sup 13}C′-{sup 13}C{sub aliphatic} distances in amyloid fibrils formed by the SNNFGAILSS fibrillating core of the human islet amyloid polypeptide with uniform {sup 13}C,{sup 15}N-labeling on the FGAIL fragment.

  8. Characterization of pyrogenic organic matter by 2-dimenstional HETeronucleus CORelation solid-state 13C NMR (HETCOR) spectroscopy

    NASA Astrophysics Data System (ADS)

    Knicker, Heike

    2016-04-01

    During the last years, increasing evidences are provided that the common view of charcoal as a polyaromatic network is too much simplified. Experiments with model compounds indicated that it represents a heterogeneous mixture of thermally altered biomacromolecules with N, O and likely also S substitutions as common features. If produced from a N-rich feedstock, the so called black nitrogen (BN) has to be considered as an integral part of the aromatic charcoal network. In order to study this network one-dimensional (1D) solid-state nuclear magnetic resonance (NMR) spectroscopy is often applied. However, this technique suffers from broad resonance lines and low resolution. Applying 2D techniques can help but until recently, this was unfeasible for natural organic matter (NOM) due to sensitivity problems and the high complexity of the material. On the other hand, during the last decade, the development of stronger magnetic field instruments and advanced pulse sequences has put them into reach for NOM research. Although 2D NMR spectroscopy has many different applications, all pulse sequences are based on the introduction of a preparation time during which the magnetization of a spin system is adjusted into a state appropriate to whatever properties are to be detected in the indirect dimension. Then, the spins are allowed to evolve with the given conditions and after their additional manipulation during a mixing period the modulated magnetization is detected. Assembling several 1D spectra with incrementing evolution time creates a data set which is two-dimensional in time (t1, t2). Fourier transformation of both dimensions leads to a 2D contour plot correlating the interactions detected in the indirect dimension t1 with the signals detected in the direct dimension t2. The so called solid-state heteronuclear correlation (HETCOR) NMR spectroscopy represents a 2D technique allows the determination which protons are interacting with which carbons. In the present work this

  9. Differentiation of histidine tautomeric states using (15)N selectively filtered (13)C solid-state NMR spectroscopy.

    PubMed

    Miao, Yimin; Cross, Timothy A; Fu, Riqiang

    2014-08-01

    The histidine imidazole ring in proteins usually contains a mixture of three possible tautomeric states (two neutral - τ and π states and a charged state) at physiological pHs. Differentiating the tautomeric states is critical for understanding how the histidine residue participates in many structurally and functionally important proteins. In this work, one dimensional (15)N selectively filtered (13)C solid-state NMR spectroscopy is proposed to differentiate histidine tautomeric states and to identify all (13)C resonances of the individual imidazole rings in a mixture of tautomeric states. When (15)N selective 180° pulses are applied to the protonated or non-protonated nitrogen region, the (13)C sites that are bonded to the non-protonated or protonated nitrogen sites can be identified, respectively. A sample of (13)C, (15)N labeled histidine powder lyophilized from a solution at pH 6.3 has been used to illustrate the usefulness of this scheme by uniquely assigning resonances of the neutral τ and charged states from the mixture. PMID:25026459

  10. Differentiation of Histidine Tautomeric States using 15N Selectively Filtered 13C Solid-State NMR Spectroscopy

    PubMed Central

    Miao, Yimin; Cross, Timothy A.; Fu, Riqiang

    2014-01-01

    The histidine imidazole ring in proteins usually contains a mixture of three possible tautomeric states (two neutral - τ and π states and a charged state) at physiological pHs. Differentiating the tautomeric states is critical for understanding how the histidine residue participates in many structurally and functionally important proteins. In this work, one dimensional 15N selectively filtered 13C solid-state NMR spectroscopy is proposed to differentiate histidine tautomeric states and to identify all 13C resonances of the individual imidazole rings in a mixture of tautomeric states. When 15N selective 180° pulses are applied to the protonated or non-protonated nitrogen region, the 13C sites that are bonded to the non-protonated or protonated nitrogen sites can be identified, respectively. A sample of 13C,15N labeled histidine powder lyophilized from a solution at pH 6.3 has been used to illustrate the usefulness of this scheme by uniquely assigning resonances of the neutral τ and charged states from the mixture. PMID:25026459

  11. Solid-State Selective 13C Excitation and Spin Diffusion NMR to Resolve Spatial Dimensions in Plant Cell Walls

    SciTech Connect

    Foston, M.; Katahira, R.; Gjersing, E.; Davis, M. F.; Ragauskas, A. J.

    2012-02-15

    The average spatial dimensions between major biopolymers within the plant cell wall can be resolved using a solid-state NMR technique referred to as a {sup 13}C cross-polarization (CP) SELDOM (selectively by destruction of magnetization) with a mixing time delay for spin diffusion. Selective excitation of specific aromatic lignin carbons indicates that lignin is in close proximity to hemicellulose followed by amorphous and finally crystalline cellulose. {sup 13}C spin diffusion time constants (T{sub SD}) were extracted using a two-site spin diffusion theory developed for {sup 13}C nuclei under magic angle spinning (MAS) conditions. These time constants were then used to calculate an average lower-limit spin diffusion length between chemical groups within the plant cell wall. The results on untreated {sup 13}C enriched corn stover stem reveal that the lignin carbons are, on average, located at distances {approx}0.7-2.0 nm from the carbons in hemicellulose and cellulose, whereas the pretreated material had larger separations.

  12. Differentiation of histidine tautomeric states using 15N selectively filtered 13C solid-state NMR spectroscopy

    NASA Astrophysics Data System (ADS)

    Miao, Yimin; Cross, Timothy A.; Fu, Riqiang

    2014-08-01

    The histidine imidazole ring in proteins usually contains a mixture of three possible tautomeric states (two neutral - τ and π states and a charged state) at physiological pHs. Differentiating the tautomeric states is critical for understanding how the histidine residue participates in many structurally and functionally important proteins. In this work, one dimensional 15N selectively filtered 13C solid-state NMR spectroscopy is proposed to differentiate histidine tautomeric states and to identify all 13C resonances of the individual imidazole rings in a mixture of tautomeric states. When 15N selective 180° pulses are applied to the protonated or non-protonated nitrogen region, the 13C sites that are bonded to the non-protonated or protonated nitrogen sites can be identified, respectively. A sample of 13C, 15N labeled histidine powder lyophilized from a solution at pH 6.3 has been used to illustrate the usefulness of this scheme by uniquely assigning resonances of the neutral τ and charged states from the mixture.

  13. Characterisation of black carbon-rich samples by 13C solid-state nuclear magnetic resonance

    NASA Astrophysics Data System (ADS)

    Novotny, Etelvino H.; Hayes, Michael H. B.; Deazevedo, Eduardo R.; Bonagamba, Tito J.

    2006-09-01

    There are difficulties in quantifying and characterising the organic matter (OM) in soils that contain significant amounts of partially oxidised char or charcoal materials. The anthropogenic black carbon (BC), such as that found in the Terra Preta de Índio soils of the Amazon region, is a good example of the OM that is difficult to analyse in such soils. 13C direct polarisation/magic angle spinning (DP/MAS) at high MAS frequency, 1H-13C cross polarisation (CP)/MAS with total suppression of spinning sidebands (TOSS), and chemical shift anisotropy (CSA) filter nuclear magnetic resonance techniques have been applied successfully for quantifying the different components of OM. However, because pyrogenic materials present strong local magnetic susceptibility heterogeneities, the use of CSA-filter and TOSS make the pulse sequences very sensitive to imperfections in the π pulses. In this study, the DP/MAS pulse sequence was replaced by a CP with a radio frequency ramp—variable amplitude CP (VACP)—VACP/MAS pulse sequence, and composite π pulses were used in the CSA-filter and TOSS pulse sequences. In that way, the component functionalities in a humic acid from a BC soil were successfully determined. The spectrometer time needed was greatly decreased by employing this VACP/MAS technique. This development provides an accurate method for characterising BC-rich samples from different origins.

  14. Characterisation of black carbon-rich samples by (13)C solid-state nuclear magnetic resonance.

    PubMed

    Novotny, Etelvino H; Hayes, Michael H B; Deazevedo, Eduardo R; Bonagamba, Tito J

    2006-09-01

    There are difficulties in quantifying and characterising the organic matter (OM) in soils that contain significant amounts of partially oxidised char or charcoal materials. The anthropogenic black carbon (BC), such as that found in the Terra Preta de Indio soils of the Amazon region, is a good example of the OM that is difficult to analyse in such soils. (13)C direct polarisation/magic angle spinning (DP/MAS) at high MAS frequency, (1)H-(13)C cross polarisation (CP)/MAS with total suppression of spinning sidebands (TOSS), and chemical shift anisotropy (CSA) filter nuclear magnetic resonance techniques have been applied successfully for quantifying the different components of OM. However, because pyrogenic materials present strong local magnetic susceptibility heterogeneities, the use of CSA-filter and TOSS make the pulse sequences very sensitive to imperfections in the pi pulses. In this study, the DP/MAS pulse sequence was replaced by a CP with a radio frequency ramp--variable amplitude CP (VACP)--VACP/MAS pulse sequence, and composite pi pulses were used in the CSA-filter and TOSS pulse sequences. In that way, the component functionalities in a humic acid from a BC soil were successfully determined. The spectrometer time needed was greatly decreased by employing this VACP/MAS technique. This development provides an accurate method for characterising BC-rich samples from different origins. PMID:16688435

  15. Solid-state 13C nuclear magnetic resonance studies of coalified gymnosperm xylem tissue from Australian brown coals

    USGS Publications Warehouse

    Hatcher, P.G.; Lerch, H. E., III; Bates, A.L.; Verheyen, T.V.

    1989-01-01

    We report here on the use of solid-state 13C nuclear magnetic resonance (NMR) spectroscopy to contrast the average chemical composition of modern degraded gymnosperm woods with fossil gymnosperm woods from Australian brown coals (Miocene). We first established the quantitative nature of the NMR techniques for these samples so that the conventional solid-state 13C NMR spectra and the dipolar dephasing NMR spectra could be used with a high degree of reliability to depict average chemical compositions. The NMR results provide some valuable insights about the early coalification of xylem tissue from gymnosperms. Though the cellulosic components of wood are degraded to varying degrees during peatification and ensuing coalification, it is unlikely that they play a major role in the formation of aromatic structures in coalified woods. The NMR data show that gynmosperm lignin, the primary aromatic contribution to the coal, is altered in part by demethylation of guaiacyl-units to catechol-like structures. The dipolar dephasing NMR data indicate that the lignin also becomes more cross-linked or condensed. ?? 1989.

  16. 13C Solid State Nuclear Magnetic Resonance and µ-Raman Spectroscopic Characterization of Sicilian Amber.

    PubMed

    Barone, Germana; Capitani, Donatella; Mazzoleni, Paolo; Proietti, Noemi; Raneri, Simona; Longobardo, Ugo; Di Tullio, Valeria

    2016-08-01

    (13)C cross-polarization magic angle spinning (CPMAS) nuclear magnetic resonance (NMR) and µ-Raman spectroscopy were applied to characterize Sicilian amber samples. The main goal of this work was to supply a complete study of simetite, highlighting discriminating criteria useful to distinguish Sicilian amber from fossil resins from other regions and laying the foundations for building a spectroscopic database of Sicilian amber. With this aim, a private collection of unrefined simetite samples and fossil resins from the Baltic region and Dominican Republic was analyzed. Overall, the obtained spectra permitted simetite to be distinguished from the other resins. In addition, principal component analysis (PCA) was applied to the spectroscopic data, allowing the clustering of simetite samples with respect to the Baltic and Dominican samples and to group the simetite samples in two sets, depending on their maturity. Finally, the analysis of loadings allowed for a better understanding of the spectral features that mainly influenced the discriminating characteristics of the investigated ambers. PMID:27340217

  17. Solid-state 13C NMR studies of a large fossil gymnosperm from the Yallourn Open Cut, Latrobe Valley, Australia

    USGS Publications Warehouse

    Bates, A.L.; Hatcher, P.G.

    1989-01-01

    A series of samples taken from the cross section of a 3-m-diameter fossilized gymnospermous log (Araucariaceae) in the Yallourn Seam of the Australian brown coals was examined by solid state 13C nuclear magnetic resonance to delineate chemical changes related to the combined processes of peatification and coalification. The results show that cellulosic materials were degraded and lost on the periphery of the log, however, the degree of such degradation in the central core is substantially less. The lignin is uniformly altered by coalification reactions to a macromolecular substance displaying decreased aryl ether linkages but significantly greater amounts of carbon linkages compared to modern lignin. Changes in the methoxyl carbon contents of lignin in cross section reveal demethylation reactions, but these do not appear to be related to degree of carbon linking. Both the degredation of cellulosic materials and demethylation of lignin appear to be early diagenetic processes occurring during peatification independently of the coalification reactions. ?? 1989.

  18. Hydrothermal carbon from biomass: structural differences between hydrothermal and pyrolyzed carbons via 13C solid state NMR.

    PubMed

    Falco, Camillo; Perez Caballero, Fernando; Babonneau, Florence; Gervais, Christel; Laurent, Guillaume; Titirici, Maria-Magdalena; Baccile, Niki

    2011-12-01

    The objective of this paper is to better describe the structure of the hydrothermal carbon (HTC) process and put it in relationship with the more classical pyrolytic carbons. Indeed, despite the low energetic impact and the number of applications described so far for HTC, very little is known about the structure, reaction mechanism, and the way these materials relate to coals. Are HTC and calcination processes equivalent? Are the structures of the processed materials related to each other in any way? Which is the extent of polyaromatic hydrocarbons (PAH) inside HTC? In this work, the effect of hydrothermal treatment and pyrolysis are compared on glucose, a good model carbohydrate; a detailed single-quantum double-quantum (SQ-DQ) solid state (13)C NMR study of the HTC and calcined HTC is used to interpret the spectral region corresponding to the signal of furanic and arene groups. These data are compared to the spectroscopic signatures of calcined glucose, starch, and xylose. A semiquantitative analysis of the (13)C NMR spectra provides an estimation of the furanic-to-arene ratio which varies from 1:1 to 4:1 according to the processing conditions and carbohydrate employed. In addition, we formulate some hypothesis, validated by DFT (density functional theory) modeling associated with (13)C NMR chemical shifts calculations, about the possible furan-rich structural intermediates that occur in the coalification process leading to condensed polyaromatic structures. In combination with a broad parallel study on the HTC processing conditions effect on glucose, cellulose, and raw biomass (Falco, C.; Baccile, N.; Titirici, M.-M. Green Chem., 2011, DOI: 10.1039/C1GC15742F), we propose a broad reaction scheme and in which we show that, through HTC, it is possible to tune the furan-to-arene ratio composing the aromatic core of the produced HTC carbons, which is not possible if calcination is used alone, in the temperature range below 350 °C. PMID:22050004

  19. Structural characterization of ion-vapor deposited hydrogenated amorphous carbon coatings by solid state {sup 13}C nuclear magnetic resonance

    SciTech Connect

    Xu, Jiao; Kato, Takahisa; Watanabe, Sadayuki; Hayashi, Hideo; Kawaguchi, Masahiro

    2014-01-07

    In the present study, unique structural heterogeneity was observed in ion-vapor deposited a-C:H coatings by performing {sup 13}C MAS and {sup 1}H-{sup 13}C CPMAS experiments on solid state nuclear magnetic resonance devices. Two distinct types of sp{sup 2} C clusters were discovered: one of them denoted as sp{sup 2} C′ in content of 3–12 at. % was non-protonated specifically localized in hydrogen-absent regions, while the other dominant one denoted as sp{sup 2} C″ was hydrogenated or at least proximate to proton spins. On basis of the notably analogous variation of sp{sup 2} C′ content and Raman parameters as function of substrate bias voltage in the whole range of 0.5 kV–3.5 kV, a model of nano-clustering configuration was proposed that the sp{sup 2} C′ clusters were embedded between sp{sup 2} C″ clusters and amorphous sp{sup 3} C matrix as trapped interfaces or boundaries where the sp{sup 2} carbon bonds were highly distorted. Continuous increase of bias voltage would promote the nano-clustering and re-ordering of dominant sp{sup 2} C″ clusters, thus results in a marked decrease of interspace and a change of the content of sp{sup 2} C′ clusters. Further investigation on the {sup 13}C magnetization recovery showed typical stretched-exponential approximation due to the prominent presence of paramagnetic centers, and the stretched power α varied within 0.6–0.9 from distinct types of sp{sup 2} C clusters. Differently, the magnetization recovery of {sup 1}H showed better bi-exponential approximation with long and short T{sub 1}(H) fluctuated within 40–60 ms and 0.1–0.3 ms approximately in content of 80% ± 5% and 20% ± 5%, respectively, varying with various bias voltages. Meanwhile, the interrupted {sup 13}C saturation recovery with an interval of short T{sub 1}(H) showed that most of quick-relaxing protons were localized in sp{sup 2} C″ clusters. Such a short T{sub 1}(H) was only possibly resulted from a relaxation mechanism

  20. Molecular organization in the native state of woody tissue: Studies of tertiary structure using the Raman microprobe Solid State [sup 13]C NMR and biomimetic tertiary aggregates

    SciTech Connect

    Atalla, R.H.

    1992-01-01

    A number of new approaches to the study of native wood tissue complementary to our earlier Raman spectroscopy including solid state [sup 13]C NMR and X-ray diffractometry. A wide variety of native cellulosic tissues were examined which led to the generation of biomimetic tertiary aggregates which simulate states of aggregation characteristic of cell walls. We have also explored charge transport characteristics of lignified tissue. Our Raman spectroscopic studies have advanced our understanding of key spectral features and confirmed the variability of the patterns of orientation of lignin reported earlier. A major effort was dedicated to assessing the contributions of electronic factors such as conjugation and the resonance Raman effect to enhancement of the spectra features associated with lignin. We have now established a solid foundation for spectral mapping of different regions in cell walls.

  1. Soil organic matter dynamics as characterized with 1H and 13C solid-state NMR techniques

    NASA Astrophysics Data System (ADS)

    Jäger, Alex; Schwarz, Jette; Bertmer, Marko; Schaumann, Gabriele E.

    2010-05-01

    Soil organic matter (SOM) is a complex and heterogeneous matter. Characterization by solid-state NMR methods on 1H and 13C nuclei is therefore demanding. Our goal is to obtain information on the dynamic behaviour of soil samples and to study the influence of external parameters on both structure and dynamics. We regard water molecules to be the pivotal agent of soil dynamics by generating a network between organic matter via intermolecular hydrogen bonding, which leads to cross linking of organic matter and increases its rigidity. Although 1H solid-state NMR on non-rotating samples are not so commonly used for soil characterization, they enable the differentiation of proton mobilities via their linewidths which are resulting from differences in the dipole-dipole coupling strengths. Therefore, even weak molecular interactions such as hydrogen bonding can be differentiated and changes due to heat treatments and the short and long term behaviour followed. Though in principle a simple technique, static 1H measurements are complicated by several means, one of them is the high abundance in almost all matter including probe head material that has to be excluded for analysis. Finally, we selected 1H DEPTH [1] and Hahn-echo sequences to distinguish different mobilities in soil, mainly free moving water and water fixed in the soil matrix. After decomposition using Gaussian and Lorentzian lineshapes, the relative amounts of mobile and rigid water molecules can be obtained. By heating the samples above 100°C in sealed glass tubes, the proposed water network is destroyed and able to rebuild after cooling. This long term behaviour is studied on the course of months. Furthermore, the instant changes before and after heating are shown for a series of soil samples to characterize soils based on this water network model. To combine the information obtained on the 1H mobility with focus on water dynamics, 13C 2D WISE (wideline separation) measurements were done. This method yields 1

  2. Identification of Li-Ion Battery SEI Compounds through (7)Li and (13)C Solid-State MAS NMR Spectroscopy and MALDI-TOF Mass Spectrometry.

    PubMed

    Huff, Laura A; Tavassol, Hadi; Esbenshade, Jennifer L; Xing, Wenting; Chiang, Yet-Ming; Gewirth, Andrew A

    2016-01-13

    Solid-state (7)Li and (13)C MAS NMR spectra of cycled graphitic Li-ion anodes demonstrate SEI compound formation upon lithiation that is followed by changes in the SEI upon delithiation. Solid-state (13)C DPMAS NMR shows changes in peaks associated with organic solvent compounds (ethylene carbonate and dimethyl carbonate, EC/DMC) upon electrochemical cycling due to the formation of and subsequent changes in the SEI compounds. Solid-state (13)C NMR spin-lattice (T1) relaxation time measurements of lithiated Li-ion anodes and reference poly(ethylene oxide) (PEO) powders, along with MALDI-TOF mass spectrometry results, indicate that large-molecular-weight polymers are formed in the SEI layers of the discharged anodes. MALDI-TOF MS and NMR spectroscopy results additionally indicate that delithiated anodes exhibit a larger number of SEI products than is found in lithiated anodes. PMID:26653886

  3. Structure and dynamics of homoleptic beryllocenes: a solid-state 9Be and 13C NMR study.

    PubMed

    Hung, Ivan; Macdonald, Charles L B; Schurko, Robert W

    2004-11-19

    The correlation between anisotropic 9Be NMR (quadrupolar and chemical shielding) interactions and the structure and dynamics in [Cp2Be], [Cp2*Be], and [(C5Me4H)2Be] is examined by solid-state 9Be NMR spectroscopy, as well as by ab initio and hybrid density functional theory calculations. The 9Be quadrupole coupling constants in the three compounds correspond well to the relative degrees of spherical ground-state electronic symmetry of the environment about beryllium. Theoretical computations of NMR interaction tensors are in excellent agreement with experimental values and aid in understanding the origins of NMR interaction tensors and their correlation to molecular symmetry. Variable-temperature (VT) 9Be and 13C NMR experiments reveal a highly fluxional structure in the condensed phase of [Cp2Be]. In particular, the pathway by which the Cp rings of [Cp2Be] 'invert' coordination modes is examined in detail using hybrid density functional theory in order to inspect variations of the 9Be NMR interaction tensors. The activation energy for the 'inversion' process is found to be 36.9 kJ mol(-1) from chemical exchange analysis of 13C VT CP/MAS NMR spectra. The low-temperature (ca. -100 degrees C) X-ray crystal structures of all three compounds have been collected and refined, and are in agreement with previously reported structures. In addition, the structure of the same Cp2Be crystal was determined at 20 degrees C and displays features consistent with increased intramolecular motion, supporting observations by 9Be VT NMR spectroscopy. PMID:15484199

  4. Hydration properties of regioselectively etherified celluloses monitored by 2H and 13C solid-state MAS NMR spectroscopy.

    PubMed

    Larsen, Flemming H; Schöbitz, Michael; Schaller, Jens

    2012-06-20

    The hydration properties of 2,3-O-hydroxypropylcellulose (HPC) and 2,3-O-hydroxyethylcellulose (HEC) were analyzed by multi-nuclear solid-state MAS NMR spectroscopy. By 13C single-pulse (SP) MAS and cross-polarization (CP) MAS NMR, differences between the immobile regions and all parts of the polysaccharides were detected as a function of hydration. Complementary information about the water environments was observed by 2H MAS NMR. By this approach it was demonstrated that side chains in 2,3-O-HPC and 2,3-O-HEC were easier to hydrate than the cellulose backbone. Furthermore the motion of water was more restricted (slower) in 2,3-O-HPC than in 2,3-O-HEC. For both polysaccharides the hydration could be explained by a two-step process: in step one increased ordering of the immobile regions occurs after which the entire polymer is hydrated in step two. PMID:24750769

  5. Solid-state 13C NMR studies of dissolved organic matter in pore waters from different depositional environments

    USGS Publications Warehouse

    Orem, W.H.; Hatcher, P.G.

    1987-01-01

    Dissolved organic matter (DOM) in pore waters from sediments of a number of different depositional environments was isolated by ultrafiltration using membranes with a nominal molecular weight cutoff of 500. This > 500 molecular weight DOM represents 70-98% of the total DOM in these pore waters. We determined the gross chemical structure of this material using both solid-state 13C nuclear magnetic resonance spectroscopy and elemental analysis. Our results show that the DOM in these pore waters appears to exist as two major types: one type dominated by carbohydrates and paraffinic structures and the second dominated by paraffinic and aromatic structures. We suggest that the dominance of one or the other structural type of DOM in the pore water depends on the relative oxidizing/reducing nature of the sediments as well as the source of the detrital organic matter. Under dominantly anaerobic conditions carbohydrates in the sediments are degraded by bacteria and accumulate in the pore water as DOM. However, little or no degradation of lignin occurs under these conditions. In contrast, sediments thought to be predominantly aerobic in character have DOM with diminished carbohydrate and enhanced aromatic character. The aromatic structures in the DOM from these sediments are thought to arise from the degradation of lignin. The large amounts of paraffinic structures in both types of DOM may be due to the degradation of unidentified paraffinic materials in algal or bacterial remains. ?? 1987.

  6. Molecular composition of recycled organic wastes, as determined by solid-state {sup 13}C NMR and elemental analyses

    SciTech Connect

    Eldridge, S.M.; Chen, C.R.; Xu, Z.H.; Nelson, P.N.; Boyd, S.E.; Meszaros, I.; Chan, K.Y.

    2013-11-15

    Highlights: • Model estimated the molecular C components well for most RO wastes. • Molecular nature of organic matter in RO wastes varied widely. • Molecular composition by NMR modelling preferable to extraction techniques. • Some model shortcomings in estimating molecular composition of biochars. • Waste molecular composition important for carbon/nutrient outcomes in soil. - Abstract: Using solid state {sup 13}C NMR data and elemental composition in a molecular mixing model, we estimated the molecular components of the organic matter in 16 recycled organic (RO) wastes representative of the major materials generated in the Sydney basin area. Close correspondence was found between the measured NMR signal intensities and those predicted by the model for all RO wastes except for poultry manure char. Molecular nature of the organic matter differed widely between the RO wastes. As a proportion of organic C, carbohydrate C ranged from 0.07 to 0.63, protein C from <0.01 to 0.66, lignin C from <0.01 to 0.31, aliphatic C from 0.09 to 0.73, carbonyl C from 0.02 to 0.23, and char C from 0 to 0.45. This method is considered preferable to techniques involving imprecise extraction methods for RO wastes. Molecular composition data has great potential as a predictor of RO waste soil carbon and nutrient outcomes.

  7. Quantitative solid-state 13C nuclear magnetic resonance spectrometric analyses of wood xylen: effect of increasing carbohydrate content

    USGS Publications Warehouse

    Bates, A.L.; Hatcher, P.G.

    1992-01-01

    Isolated lignin with a low carbohydrate content was spiked with increasing amounts of alpha-cellulose, and then analysed by solid-state 13C nuclear magnetic resonance (NMR) using cross-polarization with magic angle spinning (CPMAS) and dipolar dephasing methods in order to assess the quantitative reliability of CPMAS measurement of carbohydrate content and to determine how increasingly intense resonances for carbohydrate carbons affect calculations of the degree of lignin's aromatic ring substitution and methoxyl carbon content. Comparisons were made of the carbohydrate content calculated by NMR with carbohydrate concentrations obtained by phenol-sulfuric acid assay and by the calculation from the known amounts of cellulose added. The NMR methods used in this study yield overestimates for carbohydrate carbons due to resonance area overlap from the aliphatic side chain carbons of lignin. When corrections are made for these overlapping resonance areas, the NMR results agree very well with results obtained by other methods. Neither the calculated methoxyl carbon content nor the degree of aromatic ring substitution in lignin, both calculated from dipolar dephasing spectra, change with cellulose content. Likewise, lignin methoxyl content does not correlate with cellulose abundance when measured by integration of CPMAS spectra. ?? 1992.

  8. Conformational transitions and fibrillation mechanism of human calcitonin as studied by high-resolution solid-state 13C NMR.

    PubMed Central

    Kamihira, M.; Naito, A.; Tuzi, S.; Nosaka, A. Y.; Saitô, H.

    2000-01-01

    Conformational transitions of human calcitonin (hCT) during fibril formation in the acidic and neutral conditions were investigated by high-resolution solid-state 13C NMR spectroscopy. In aqueous acetic acid solution (pH 3.3), a local alpha-helical form is present around Gly10 whereas a random coil form is dominant as viewed from Phe22, Ala26, and Ala31 in the monomer form on the basis of the 13C chemical shifts. On the other hand, a local beta-sheet form as viewed from Gly10 and Phe22, and both beta-sheet and random coil as viewed from Ala26 and Ala31 were detected in the fibril at pH 3.3. The results indicate that conformational transitions from alpha-helix to beta-sheet, and from random coil to beta-sheet forms occurred in the central and C-terminus regions, respectively, during the fibril formation. The increased 13C resonance intensities of fibrils after a certain delay time suggests that the fibrillation can be explained by a two-step reaction mechanism in which the first step is a homogeneous association to form a nucleus, and the second step is an autocatalytic heterogeneous fibrillation. In contrast to the fibril at pH 3.3, the fibril at pH 7.5 formed a local beta-sheet conformation at the central region and exhibited a random coil at the C-terminus region. Not only a hydrophobic interaction among the amphiphilic alpha-helices, but also an electrostatic interaction between charged side chains can play an important role for the fibril formation at pH 7.5 and 3.3 acting as electrostatically favorable and unfavorable interactions, respectively. These results suggest that hCT fibrils are formed by stacking antiparallel beta-sheets at pH 7.5 and a mixture of antiparallel and parallel beta-sheets at pH 3.3. PMID:10850796

  9. Advanced mid-IR Solid-State Laser Developments

    NASA Technical Reports Server (NTRS)

    Yu, Jirong

    2005-01-01

    This paper reviews the state-of-the-art 2-micron solid-state laser developments. A world record one-Joule-per-pulse energy laser system and an advanced thermal management with fully conductive cooled laser technique are discussed

  10. High-resolution solid-state 13C CP MAS NMR spectra of some β-cyclodextrin inclusion complexes with nitriles

    NASA Astrophysics Data System (ADS)

    Okazaki, M.; McDowell, C. A.

    1983-11-01

    β-cyclodextrin inclusion complexes of 3-aminobenzonitrile, 4-aminobenzonitrile, and adamantane-1-carbonitrile were studied by means of high-resolution solid-state CP MAS 13C NMR spectroscopy. The interactions between the host and guest molecules are discussed.

  11. Differences between Lignin in Unprocessed Wood, Milled Wood, Mutant Wood, and Extracted Lignin Detected by 13C Solid-State NMR

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Solid-state 13C nuclear magnetic resonance (NMR) has been applied to an array of intact and isolated wood samples in order to identify potential structural changes induced by tree age, milling, lignin extraction, or naturally occurring mutations. Included in this study were mature loblolly pine mil...

  12. Polydisperse methyl β-cyclodextrin–epichlorohydrin polymers: variable contact time 13C CP-MAS solid-state NMR characterization

    PubMed Central

    Mallard, Isabelle; Baudelet, Davy; Castiglione, Franca; Ferro, Monica; Panzeri, Walter; Ragg, Enzio

    2015-01-01

    Summary The polymerization of partially methylated β-cyclodextrin (CRYSMEB) with epichlorohydrin was carried out in the presence of a known amount of toluene as imprinting agent. Three different preparations (D1, D2 and D3) of imprinted polymers were obtained and characterized by solid-state 13C NMR spectroscopy under cross-polarization magic angle spinning (CP-MAS) conditions. The polymers were prepared by using the same synthetic conditions but with different molar ratios of imprinting agent/monomer, leading to morphologically equivalent materials but with different absorption properties. The main purpose of the work was to find a suitable spectroscopic descriptor accounting for the different imprinting process in three homogeneous polymeric networks. The polymers were characterized by studying the kinetics of the cross-polarization process. This approach is based on variable contact time CP-MAS spectra, referred to as VCP-MAS. The analysis of the VCP-MAS spectra provided two relaxation parameters: T CH (the CP time constant) and T 1ρ (the proton spin-lattice relaxation time in the rotating frame). The results and the analysis presented in the paper pointed out that T CH is sensitive to the imprinting process, showing variations related to the toluene/cyclodextrin molar ratio used for the preparation of the materials. Conversely, the observed values of T 1ρ did not show dramatic variations with the imprinting protocol, but rather confirmed that the three polymers are morphologically similar. Thus the combined use of T CH and T 1ρ can be helpful for the characterization and fine tuning of imprinted polymeric matrices. PMID:26877800

  13. Polydisperse methyl β-cyclodextrin-epichlorohydrin polymers: variable contact time (13)C CP-MAS solid-state NMR characterization.

    PubMed

    Mallard, Isabelle; Baudelet, Davy; Castiglione, Franca; Ferro, Monica; Panzeri, Walter; Ragg, Enzio; Mele, Andrea

    2015-01-01

    The polymerization of partially methylated β-cyclodextrin (CRYSMEB) with epichlorohydrin was carried out in the presence of a known amount of toluene as imprinting agent. Three different preparations (D1, D2 and D3) of imprinted polymers were obtained and characterized by solid-state (13)C NMR spectroscopy under cross-polarization magic angle spinning (CP-MAS) conditions. The polymers were prepared by using the same synthetic conditions but with different molar ratios of imprinting agent/monomer, leading to morphologically equivalent materials but with different absorption properties. The main purpose of the work was to find a suitable spectroscopic descriptor accounting for the different imprinting process in three homogeneous polymeric networks. The polymers were characterized by studying the kinetics of the cross-polarization process. This approach is based on variable contact time CP-MAS spectra, referred to as VCP-MAS. The analysis of the VCP-MAS spectra provided two relaxation parameters: T CH (the CP time constant) and T 1ρ (the proton spin-lattice relaxation time in the rotating frame). The results and the analysis presented in the paper pointed out that T CH is sensitive to the imprinting process, showing variations related to the toluene/cyclodextrin molar ratio used for the preparation of the materials. Conversely, the observed values of T 1ρ did not show dramatic variations with the imprinting protocol, but rather confirmed that the three polymers are morphologically similar. Thus the combined use of T CH and T 1ρ can be helpful for the characterization and fine tuning of imprinted polymeric matrices. PMID:26877800

  14. Solid-state (13)C NMR and synchrotron SAXS/WAXS studies of uniaxially-oriented polyethylene.

    PubMed

    Afeworki, Mobae; Brant, Pat; Lustiger, Arnold; Norman, Alexander

    2015-11-01

    We report solid-state (13)C NMR and synchrotron wide-and small-angle X-ray scattering experiments (WAXS, SAXS) on metallocene linear low density polyethylene films (e.g., Exceed™ 1018 mLLDPE; nominally 1MI, 0.918 density ethylene-hexene metallocene copolymer) as a function of uniaxial draw ratio, λ. Combined, these experiments provide an unambiguous, quantitative molecular view of the orientation of both the crystalline and amorphous phases in the samples as a function of draw. Together with previously reported differential scanning calorimetry (DSC), gas transport measurements, transmission electron microscopy (TEM), optical birefringence, small angle X-ray scattering (SAXS) as well as other characterization techniques, this study of the state of orientation in both phases provides insight concerning the development of unusually high barrier properties of the most oriented samples (λ=10). In this work, static (non-spinning) solid-state NMR measurements indicate that in the drawn Exceed(TM) films both the crystalline and amorphous regions are highly oriented. In particular, chemical shift data show the amorphous phase is comprised increasingly of so-called "taut tie chains" (or tie chains under any state of tautness) in the mLLDPE with increasing draw ratio - the resonance lines associated with the amorphous phase shift to where the crystalline peaks are observed. In the sample with highest total draw (λ=10), virtually all of the chains in the non-crystalline region have responded and aligned in the machine (draw) direction. Both monoclinic and orthorhombic crystalline peaks are observed in high-resolution, solid-state magic-angle spinning (MAS) NMR measurements of the oriented PE films. The orientation is comparable to that obtained for ultra-high molecular weight HDPE fibers described as "ultra-oriented" in the literature. Furthermore, the presence of a monoclinic peak in cold-drawn samples suggests that there is an appreciable internal stress associated

  15. Chemical structure and heterogeneity differences of two lignins from loblolly pine as investigated by advanced solid-state NMR spectroscopy

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Advanced solid-state NMR was employed to investigate differences in chemical structure and heterogeneity between milled wood lignin (MWL) and residual enzyme lignin (REL). Wiley and conventional milled woods were also studied. The advanced NMR techniques included 13C quantitative direct polarization...

  16. The structural properties of the transmembrane segment of the integral membrane protein phospholamban utilizing (13)C CPMAS, (2)H, and REDOR solid-state NMR spectroscopy.

    PubMed

    Karp, Ethan S; Tiburu, Elvis K; Abu-Baker, Shadi; Lorigan, Gary A

    2006-06-01

    Solid-state NMR spectroscopic techniques were used to investigate the secondary structure of the transmembrane peptide phospholamban (TM-PLB), a sarcoplasmic Ca(2+) regulator. (13)C cross-polarization magic angle spinning spectra of (13)C carbonyl-labeled Leu39 of TM-PLB exhibited two peaks in a pure 1-palmitoyl-2-oleoyl-phosphocholine (POPC) bilayer, each due to a different structural conformation of phospholamban as characterized by the corresponding (13)C chemical shift. The addition of a negatively charged phospholipid (1-palmitoyl-2-oleoylphosphatidylglycerol (POPG)) to the POPC bilayer stabilized TM-PLB to an alpha-helical conformation as monitored by an enhancement of the alpha-helical carbonyl (13)C resonance in the corresponding NMR spectrum. (13)C-(15)N REDOR solid-state NMR spectroscopic experiments revealed the distance between the (13)C carbonyl carbon of Leu39 and the (15)N amide nitrogen of Leu42 to be 4.2+/-0.2A indicating an alpha-helical conformation of TM-PLB with a slight deviation from an ideal 3.6 amino acid per turn helix. Finally, the quadrupolar splittings of three (2)H labeled leucines (Leu28, Leu39, and Leu51) incorporated in mechanically aligned DOPE/DOPC bilayers yielded an 11 degrees +/-5 degrees tilt of TM-PLB with respect to the bilayer normal. In addition to elucidating valuable TM-PLB secondary structure information, the solid-state NMR spectroscopic data indicates that the type of phospholipids and the water content play a crucial role in the secondary structure and folding of TM-PLB in a phospholipid bilayer. PMID:16839519

  17. Mechanism of formation of humus coatings on mineral surfaces 3. Composition of adsorbed organic acids from compost leachate on alumina by solid-state 13C NMR

    USGS Publications Warehouse

    Wershaw, R. L.; Llaguno, E.C.; Leenheer, J.A.

    1996-01-01

    The adsorption of compost leachate DOC on alumina is used as a model for elucidation of the mechanism of formation of natural organic coatings on hydrous metal oxide surfaces in soils and sediments. Compost leachate DOC is composed mainly of organic acid molecules. The solid-state 13C NMR spectra of these organic acids indicate that they are very similar in composition to aquatic humic substances. Changes in the solid-state 13C NMR spectra of compost leachate DOC fractions adsorbed on alumina indicate that the DOC molecules are most likely adsorbed on metal oxide surfaces through a combination of polar and hydrophobic interaction mechanisms. This combination of polar and hydrophobic mechanism leads to the formation of bilayer coatings of the leachate molecules on the oxide surfaces.

  18. Detection of tannins in modern and fossil barks and in plant residues by high-resolution solid-state 13C nuclear magnetic resonance

    USGS Publications Warehouse

    Wilson, M.A.; Hatcher, P.G.

    1988-01-01

    Bark samples isolated from brown coal deposits in Victoria, Australia, and buried wood from Rhizophora mangle have been studies by high-resolution solid-state nuclear magnetic resonance (NMR) techniques. Dipolar dephasing 13C NMR appears to be a useful method of detecting the presence of tannins in geochemical samples including barks, buried woods, peats and leaf litter. It is shown that tannins are selectively preserved in bark during coalification to the brown coal stage. ?? 1988.

  19. Solid-state 13C-NMR spectroscopy of adduction products of 2,5-hexanedione with ribonuclease, albumin, and rat neurofilament protein.

    PubMed

    Yan, B; DeCaprio, A P; Zhu, M; Bank, S

    1996-10-21

    The Paal-Knorr condensation reaction between the gamma-diketone 2,5-hexanedione (2,5-HD) and epsilon-amine moieties of proteins of various molecular weight, including ribonuclease (RNase), bovine serum albumin (BSA) and rat neurofilament (NF), has been investigated by solid-state 13C-NMR spectroscopy. These proteins all reacted with 2,5-HD with the formation of 2,5-dimethylpyrrole (2,5-DMP) derivatives. The size and complexity of the protein affected the rate of formation of 2,5-DMP derivatives. Using the selective reducing reagent NaCNBH3, the Paal-Knorr reaction intermediates were trapped by conversion into amines, which were identified by solid-state NMR spectroscopy. The secondary autoxidation reaction following the formation of 2,5-DMP derivatives was also studied by solid-state NMR spectroscopy. PMID:8950225

  20. Low-temperature solid-state /sup 13/C NMR studies of the retinal chromophore in rhodopsin

    SciTech Connect

    Smith, S.O.; Palings, I.; Copie, V.; Raleigh, D.P.; Courtin, J.; Pardoen, J.A.; Lugtenburg, J.; Mathies, R.A.; Griffin, R.G.

    1987-03-24

    Magic angle sample spinning (MASS) /sup 13/C NMR spectra have been obtained of bovine rhodopsin regenerated with retinal prosthetic groups isotopically enriched with /sup 13/C at C-5 and C-14. In order to observe the /sup 13/C retinal chromophore resonances, it was necessary to employ low temperatures (-15 ..-->.. -35/sup 0/C) to restrict rotational diffusion of the protein. The isotropic chemical shift and principal values of the chemical shift tensor of the /sup 13/C-5 label indicate that the retinal chromophore is in the twisted 6-s-cis conformation in rhodopsin, in contrast to the planar 6-s-trans confirmation found in bacteriorhodopsin. The /sup 13/C-14 isotropic shift and shift tensor principal values show that the Schiff base C=N bond is anti. Furthermore, the /sup 13/C-14 chemical shift (121.2 ppm) is within the range of values (120-123 ppm) exhibited by protonated (C=N anti) Schiff base model compounds, indicating that the C=N linkage is protonated. The results are discussed with regard to the mechanism of wavelength regulation in rhodopsin.

  1. Characterization of a Mixture of CO2 Adsorption Products in Hyperbranched Aminosilica Adsorbents by (13)C Solid-State NMR.

    PubMed

    Moore, Jeremy K; Sakwa-Novak, Miles A; Chaikittisilp, Watcharop; Mehta, Anil K; Conradi, Mark S; Jones, Christopher W; Hayes, Sophia E

    2015-11-17

    Hyperbranched amine polymers (HAS) grown from the mesoporous silica SBA-15 (hereafter "SBA-15-HAS") exhibit large capacities for CO2 adsorption. We have used static in situ and magic-angle spinning (MAS) ex situ (13)C nuclear magnetic resonance (NMR) to examine the adsorption of CO2 by SBA-15-HAS. (13)C NMR distinguishes the signal of gas-phase (13)CO2 from that of the chemisorbed species. HAS polymers possess primary, secondary, and tertiary amines, leading to multiple chemisorption reaction outcomes, including carbamate (RnNCOO(-)), carbamic acid (RnNCOOH), and bicarbonate (HCO3(-)) moieties. Carbamates and bicarbonate fall within a small (13)C chemical shift range (162-166 ppm), and a mixture was observed including carbamic acid and carbamate, the former disappearing upon evacuation of the sample. By examining the (13)C-(14)N dipolar coupling through low-field (B0 = 3 T) (13)C{(1)H} cross-polarization MAS NMR, carbamate is confirmed through splitting of the (13)C resonance. A third species that is either bicarbonate or a second carbamate is evident from bimodal T2 decay times of the ∼163 ppm peak, indicating the presence of two species comprising that single resonance. The mixture of products suggests that (1) the presence of amines and water leads to bicarbonate being present and/or (2) the multiple types of amine sites in HAS permit formation of chemically distinct carbamates. PMID:26477882

  2. Global Fold of Human Cannabinoid Type 2 Receptor Probed by Solid-State 13C-, 15N-MAS NMR and Molecular Dynamics Simulations

    PubMed Central

    Kimura, Tomohiro; Vukoti, Krishna; Lynch, Diane L.; Hurst, Dow P.; Grossfield, Alan; Pitman, Michael C.; Reggio, Patricia H.; Yeliseev, Alexei A.; Gawrisch, Klaus

    2014-01-01

    The global fold of human cannabinoid type 2 (CB2) receptor in the agonist-bound active state in lipid bilayers was investigated by solid-state 13C- and 15N magic-angle spinning (MAS) NMR, in combination with chemical-shift prediction from a structural model of the receptor obtained by microsecond-long molecular dynamics (MD) simulations. Uniformly 13C-, and 15N-labeled CB2 receptor was expressed in milligram quantities by bacterial fermentation, purified, and functionally reconstituted into liposomes. 13C MAS NMR spectra were recorded without sensitivity enhancement for direct comparison of Cα, Cβ, and C=O bands of superimposed resonances with predictions from protein structures generated by MD. The experimental NMR spectra matched the calculated spectra reasonably well indicating agreement of the global fold of the protein between experiment and simulations. In particular, the 13C chemical shift distribution of Cα resonances was shown to be very sensitive to both the primary amino acid sequence and the secondary structure of CB2. Thus the shape of the Cα band can be used as an indicator of CB2 global fold. The prediction from MD simulations indicated that upon receptor activation a rather limited number of amino acid residues, mainly located in the extracellular loop 2 and the second half of intracellular loop 3, change their chemical shifts significantly (≥1.5 ppm for carbons and ≥5.0 ppm for nitrogens). Simulated two-dimensional 13Cα(i)-13C=O(i) and 13C=O(i)-15NH(i+1) dipolar-interaction correlation spectra provide guidance for selective amino-acid labeling and signal assignment schemes to study the molecular mechanism of activation of CB2 by solid-state MAS NMR. PMID:23999926

  3. Advances in actinide solid-state and coordination chemistry

    SciTech Connect

    Burns, Peter C; Ikeda, Y.; Czerwinski, K.

    2011-01-31

    Actinide solid-state and coordination chemistry has advanced through unexpected results that have further revealed the complex nature of the 5f elements. Nanoscale control of actinide materials is emerging, as shown by the creation of a considerable range of cluster and tubular topologies. Departures from established structural trends for actinyl ions are provided by cation-cation interactions in which an O atom of one actinyl ion is an equatorial ligand of a bipyramid of another actinyl ion. The solid-state structural complexity of actinide materials has been further demonstrated by open framework materials with interesting properties. The U(VI) tetraoxide core has been added to this cation's repertoire of coordination possibilities. The emergence of pentavalent uranium solid-state and coordination chemistry has resulted from the prudent selection of ligands. Finally, analogues of the uranyl ion have challenged our understanding of this normally unreactive functional group.

  4. Advanced Solid State Lighting for AES Deep Space Hab Project

    NASA Technical Reports Server (NTRS)

    Holbert, Eirik

    2015-01-01

    The advanced Solid State Lighting (SSL) assemblies augmented 2nd generation modules under development for the Advanced Exploration Systems Deep Space Habitat in using color therapy to synchronize crew circadian rhythms. Current RGB LED technology does not produce sufficient brightness to adequately address general lighting in addition to color therapy. The intent is to address both through a mix of white and RGB LEDs designing for fully addressable alertness/relaxation levels as well as more dramatic circadian shifts.

  5. A New Tool for NMR Crystallography: Complete (13)C/(15)N Assignment of Organic Molecules at Natural Isotopic Abundance Using DNP-Enhanced Solid-State NMR.

    PubMed

    Märker, Katharina; Pingret, Morgane; Mouesca, Jean-Marie; Gasparutto, Didier; Hediger, Sabine; De Paëpe, Gaël

    2015-11-01

    NMR crystallography of organic molecules at natural isotopic abundance (NA) strongly relies on the comparison of assigned experimental and computed NMR chemical shifts. However, a broad applicability of this approach is often hampered by the still limited (1)H resolution and/or difficulties in assigning (13)C and (15)N resonances without the use of structure-based chemical shift calculations. As shown here, such difficulties can be overcome by (13)C-(13)C and for the first time (15)N-(13)C correlation experiments, recorded with the help of dynamic nuclear polarization. We present the complete de novo (13)C and (15)N resonance assignment at NA of a self-assembled 2'-deoxyguanosine derivative presenting two different molecules in the asymmetric crystallographic unit cell. This de novo assignment method is exclusively based on aforementioned correlation spectra and is an important addition to the NMR crystallography approach, rendering firstly (1)H assignment straightforward, and being secondly a prerequisite for distance measurements with solid-state NMR. PMID:26485326

  6. Solid-state /sup 13/C nuclear magnetic resonance spectroscopy of simultaneously metabolized acetate and phenol in a soil Pseudomonas sp

    SciTech Connect

    Heiman, A.S.; Copper, W.T.

    1987-01-01

    An investigation was made of the concentration-dependent primary and secondary substrate relationships in the simultaneous metabolism of the ubiquitous pollutant phenol and the naturally occurring substrate acetate by a Pseudomonas sp. soil isolate capable of utilizing either substance as a sole source of carbon and energy. In addition to conventional analytical techniques, solid-state /sup 13/C nuclear magnetic resonance spectroscopy was used to follow the cellular distribution of (1-/sup 13/C)acetate in the presence of unlabeled phenol. These results suggest that, when phenol is present as the primary substrate, acetate is preferentially shuttled into fatty acyl chain synthesis, whereas phenol carbon is funnelled into the tricarboxylic acid cycle. Thus, simultaneous use of a xenobiotic compound and a natural substrate apparently does occur, and the relative concentrations of the two substrates do influence the rate and manner in which the compounds are utilized. These results also demonstrate the unique advantage of using solid-state nuclear magnetic resonance techniques combined with /sup 13/C labeling of specific sites in substrates when doing microbial degradation studies. In this work, the entire cellular biomass was examined directly without extensive extraction, fractionation, or isolation of subcellular units; thus, there is no uncertainty about chemical alteration of substrate metabolites as a result of these often harsh treatments.

  7. Solid-state and solution /sup 13/C NMR in the conformational analysis of methadone-hydrochloride and related narcotic analgesics

    SciTech Connect

    Sumner, S.C.J.

    1986-01-01

    Solid state and solution /sup 13/C NMR have been used to study the conformations of the racemic mixtures and single enantiomers of methadone hydrochloride, alpha and beta methadol hydrochloride, and alpha and beta acetylmethadol hydrochloride. The NMR spectra acquired for the compounds as solids, and in polar and nonpolar solvents are compared, in order to determine the conformation of the molecules in solution. To determine the reliability of assigning solution conformations by comparing solution and solid state chemical shift data, three bond coupling constants measured in solution are compared with those calculated from X-ray data. The conformations of the racemic mixture and plus enantiomer of methadone hydrochloride have been shown to be very similar in the solid state, where minor differences in conformation can be seen by comparing NMR spectra obtained for the solids. Also shown is that the molecules of methadone hydrochloride have conformations in polar and in nonpolar solvents which are very similar to the conformation of the molecules in the solid state.

  8. The study of a monocotyledon abscission zone using microscopic, chemical, enzymatic and solid state 13C CP/MAS NMR analyses.

    PubMed

    Henderson, J; Davies, H A; Heyes, S J; Osborne, D J

    2001-01-01

    We have investigated distinguishing features in cells of the abscission zone of a monocotyledon fruit, the oil palm Elaeis guineensis. The cell walls of the abscission zone and the subtending mesocarp and pedicel have been analysed by light and transmission electron microscopy, by chemical methods and by solid state 13C CP/MAS NMR spectroscopy. Results show that these abscission zone cells have specific characteristics which include high levels of unmethylated pectin in the walls and an inducible (x35) polygalacturonase enzyme expression. Together these findings help to explain the localised precision of cell separation events. PMID:11219806

  9. Effects of post-reactor functionalization on the phase behaviour of an ethylene-1-octene copolymer studied using solid-state high resolution 13C NMR spectroscopy.

    PubMed

    Calucci, Lucia; Cicogna, Francesca; Forte, Claudia

    2013-10-01

    The effects of post-reactor functionalization with naphthoate-TEMPO on the structure and morphology of an ethylene-1-octene copolymer were investigated by means of solid-state NMR techniques and DSC measurements. Selective (13)C MAS experiments allowed the orthorhombic and the monoclinic crystalline phases and two amorphous phases with different degree of mobility to be detected and quantified. (13)C and (1)H relaxation time measurements and spin diffusion experiments gave insight into the polymer dynamics within the different phases, the crystalline domain dimensions, and the rate of chain diffusion between amorphous and crystalline phases. Comparison of the results obtained for the pristine copolymer and the functionalized samples clearly indicated that the functionalization procedure causes redistribution within the crystalline and the amorphous phases with no relevant change in the degree of crystallinity or in the crystalline domain average size, and slows down chain diffusion. PMID:23942957

  10. Simultaneous cross polarization to 13C and 15N with 1H detection at 60 kHz MAS solid-state NMR

    NASA Astrophysics Data System (ADS)

    Das, Bibhuti B.; Opella, Stanley J.

    2016-01-01

    We describe high resolution MAS solid-state NMR experiments that utilize 1H detection with 60 kHz magic angle spinning; simultaneous cross-polarization from 1H to 15N and 13C nuclei; bidirectional cross-polarization between 13C and 15N nuclei; detection of both amide nitrogen and aliphatic carbon 1H; and measurement of both 13C and 15N chemical shifts through multi-dimensional correlation experiments. Three-dimensional experiments correlate amide 1H and alpha 1H selectively with 13C or 15N nuclei in a polypeptide chain. Two separate three-dimensional spectra correlating 1Hα/13Cα/1HN and 1HN/15N/1Hα are recorded simultaneously in a single experiment, demonstrating that a twofold savings in experimental time is potentially achievable. Spectral editing using bidirectional coherence transfer pathways enables simultaneous magnetization transfers between 15N, 13Cα(i) and 13C‧(i-1), facilitating intra- and inter-residue correlations for sequential resonance assignment. Non-uniform sampling is integrated into the experiments, further reducing the length of experimental time.

  11. Use of solid-state 13C NMR in structural studies of humic acids and humin from Holocene sediments

    USGS Publications Warehouse

    Hatcher, P.G.; VanderHart, D.L.; Earl, W.L.

    1980-01-01

    13C NMR spectra of solid humic substances in Holocene sediments have been obtained using cross polarization with magic-angle sample spinning techniques. The results demonstrate that this technique holds great promise for structural characterizations of complex macromolecular substances such as humin and humic acids. Quantifiable distinctions can be made between structural features of aquatic and terrestrial humic substances. The aliphatic carbons of the humic substances are dominant components suggestive of input from lipid-like materials. An interesting resemblance is also noted between terrestrial humic acid and humin spectra. ?? 1980.

  12. The T1 ρ13C spin-lattice relaxation time of interpenetrating networks by solid state NMR

    NASA Astrophysics Data System (ADS)

    Lim, Ae Ran; Schueneman, G. T.; Novak, B. M.

    1999-02-01

    Poly (2-hydroxyethyl methacrylate) (PHEMA) and poly(2-hydroxyethyl methacrylate) interpenetrated with 5% SiO 2 (PHEMA-IPN) were studied by 13C CP/MAS NMR. From these results, the structure of two polymers were verified by 13C NMR. Spin-lattice relaxation times for the polymer carbons in the rotating frame, T1 ρ, have been measured as a function of temperature. The T1 ρ spin-lattice relaxation times of the α-quarternary and carbonyl in the PHEMA and PHEMA-IPN undergo slow motions, i.e., motions on the slow side of the T1 ρ minimum, while those of the 1-,2-, β-methylene, and 3-methyl undergo fast motions, i.e., motions on the fast side of the T1 ρ minimum. From these T1 ρ spin-lattice relaxation times, we discuss the mobility, the correlation time, and activation energy for the PHEMA and PHEMA-IPN, respectively. The activation energies for the PHEMA-IPN were found to be generally higher than those of PHEMA. The higher activation energy for the side-chain 2-methylene in the PHEMA-IPN is attributed to bonding between the SiO 2 and the hydroxyl group of the PHEMA.

  13. Direct Detection of Supramolecular Reaction Centers in the Methanol-to-Olefins Conversion over Zeolite H-ZSM-5 by (13)C-(27)Al Solid-State NMR Spectroscopy.

    PubMed

    Wang, Chao; Wang, Qiang; Xu, Jun; Qi, Guodong; Gao, Pan; Wang, Weiyu; Zou, Yunyun; Feng, Ningdong; Liu, Xiaolong; Deng, Feng

    2016-02-12

    Hydrocarbon-pool chemistry is important in methanol to olefins (MTO) conversion on acidic zeolite catalysts. The hydrocarbon-pool (HP) species, such as methylbenzenes and cyclic carbocations, confined in zeolite channels during the reaction are essential in determining the reaction pathway. Herein, we experimentally demonstrate the formation of supramolecular reaction centers composed of organic hydrocarbon species and the inorganic zeolite framework in H-ZSM-5 zeolite by advanced (13)C-(27)Al double-resonance solid-state NMR spectroscopy. Methylbenzenes and cyclic carbocations located near Brønsted acid/base sites form the supramolecular reaction centers in the zeolite channel. The internuclear spatial interaction/proximity between the (13)C nuclei (associated with HP species) and the (27) Al nuclei (associated with Brønsted acid/base sites) determines the reactivity of the HP species. The closer the HP species are to the zeolite framework Al, the higher their reactivity in the MTO reaction. PMID:26732748

  14. Photochemically Induced Dynamic Nuclear Polarization Observed by Solid-State NMR in a Uniformly (13)C-Isotope-Labeled Photosynthetic Reaction Center.

    PubMed

    Paul, Shubhajit; Bode, Bela E; Matysik, Jörg; Alia, A

    2015-10-29

    A sample of solubilized and quinone-depleted reaction centers from the purple bacterium Rhodobacter (R.) sphaeroides wild type has been prepared entirely (13)C and (15)N isotope labeled at all positions of the protein as well as of the cofactors. In this sample, the occurrence of the solid-state photo-CIDNP (photochemically induced dynamic nuclear polarization) effect has been probed by (13)C solid-state magic-angle spinning NMR under illumination. Under continuous illumination, signal intensities are modified by the three-spin mixing (TSM) mechanism. Time-resolved illumination experiments reveal the occurrence of light-induced nuclear polarization on the time scale of hundreds of microseconds, initially dominated by the transient polarization of the singlet branch of the radical-pair mechanism. A first kinetic analysis shows that the lifetime of the polarization from the singlet branch, indicated by the enhanced absorptive intensities of the signals from aliphatic carbons, is significantly extended. Upon arrival of the polarization from the triplet decay branch, emissive polarization caused by the TSM mechanism is observed. Also, this arrival is significantly delayed. The decay of TSM polarization occurs in two steps, assigned to intra- and intermolecular spin diffusion. PMID:26110356

  15. Advanced Solid State Lighting for Human Evaluation Project

    NASA Technical Reports Server (NTRS)

    Zeitlin, Nancy; Holbert, Eirik

    2015-01-01

    Lighting intensity and color have a significant impact on human circadian rhythms. Advanced solid state lighting was developed for the Advanced Exploration System (AES) Deep Space Habitat(DSH) concept demonstrator. The latest generation of assemblies using the latest commercially available LED lights were designed for use in the Bigelow Aerospace Environmental Control and Life Support System (ECLSS) simulator and the University of Hawaii's Hawaii Space Exploration Analog and Simulation (Hi-SEAS) habitat. Agreements with both these organizations will allow the government to receive feedback on the lights and lighting algorithms from long term human interaction.

  16. Comparison of celery (Apium graveolens L.) collenchyma and parenchyma cell wall polysaccharides enabled by solid-state (13)C NMR.

    PubMed

    Zujovic, Zoran; Chen, Da; Melton, Laurence D

    2016-02-01

    Collenchyma cells with their thickened walls are one of specific mechanical support tissues for plants, while parenchyma cells are thin walled and serve multiple functions. The parenchyma tissue is what you enjoy eating, while collenchyma, because of its fibrous nature, is not so attractive. Celery is a useful model for comparing the cell walls (CWs) of the two cell types such as collenchyma and parenchyma. However, to date, the structural characteristics of collenchyma and parenchyma cell walls from the same plant have not been compared. Monosaccharide composition suggested the collenchyma cell walls contained less pectin but more hemicellulose in comparison to parenchyma. High-resolution solid-state NMR spectra of highly mobile pectins revealed that the arabinan signals were more evident in the collenchyma spectrum, while galactan showed a much stronger resonance in the parenchyma spectrum. In addition, methyl esterified and non-esterified galacturonic acid signals were observed in parenchyma CWs, but only the latter one appeared in the collenchyma. The ratio of cellulose surface/interior obtained from CP/MAS spectra for collenchyma suggested the cellulose microfibrils were ~2.4 nm, while in the parenchyma, these were somewhat larger. X-ray diffraction indicated the size of the cellulose microfibrils were the same for both types of CWs. PMID:26717549

  17. Solid-State (13)C NMR Delineates the Architectural Design of Biopolymers in Native and Genetically Altered Tomato Fruit Cuticles.

    PubMed

    Chatterjee, Subhasish; Matas, Antonio J; Isaacson, Tal; Kehlet, Cindie; Rose, Jocelyn K C; Stark, Ruth E

    2016-01-11

    Plant cuticles on outer fruit and leaf surfaces are natural macromolecular composites of waxes and polyesters that ensure mechanical integrity and mitigate environmental challenges. They also provide renewable raw materials for cosmetics, packaging, and coatings. To delineate the structural framework and flexibility underlying the versatile functions of cutin biopolymers associated with polysaccharide-rich cell-wall matrices, solid-state NMR spectra and spin relaxation times were measured in a tomato fruit model system, including different developmental stages and surface phenotypes. The hydrophilic-hydrophobic balance of the cutin ensures compatibility with the underlying polysaccharide cell walls; the hydroxy fatty acid structures of outer epidermal cutin also support deposition of hydrophobic waxes and aromatic moieties while promoting the formation of cell-wall cross-links that rigidify and strengthen the cuticle composite during fruit development. Fruit cutin-deficient tomato mutants with compromised microbial resistance exhibit less efficient local and collective biopolymer motions, stiffening their cuticular surfaces and increasing their susceptibility to fracture. PMID:26652188

  18. Roles of Arginine and Lysine Residues in the Translocation of a Cell-Penetrating Peptide from 13C, 31P and 19F Solid-State NMR

    PubMed Central

    Su, Yongchao; Doherty, Tim; Waring, Alan J.; Ruchala, Piotr; Hong, Mei

    2009-01-01

    Cell-penetrating peptides (CPPs) are small cationic peptides that cross the cell membrane while carrying macromolecular cargoes. We use solid-state NMR to investigate the structure and lipid interaction of two cationic residues, Arg10 and Lys13, in the CPP penetratin. 13C chemical shifts indicate that Arg10 adopts a rigid β-strand conformation in the liquid-crystalline state of anionic lipid membranes. This behavior contrasts with all other residues observed so far in this peptide, which adopt a dynamic β-turn conformation with coil-like chemical shifts at physiological temperature. Low-temperature 13C-31P distances between the peptide and the lipid phosphates indicate that both the Arg10 guanidinium Cζ and the Lys13 Cε lie in close proximity to the lipid 31P (4.0 - 4.2 Å), proving the existence of charge-charge interaction for both Arg10 and Lys13 in the gel-phase membrane. However, since lysine substitution in CPPs are known to reduce their translocation ability, we propose that low temperature stabilizes both lysine and arginine interactions with the phosphates, whereas at high temperature the lysine-phosphate interaction is much weaker than the arginine-phosphate interaction. This is supported by the unusually high rigidity of the Arg10 sidechain and its β-strand conformation at high temperature. The latter is proposed to be important for ion pair formation by allowing close approach of the lipid headgroups to guanidinium sidechains. 19F and 13C spin diffusion experiments indicate that penetratin is oligomerized into β-sheets in gel-phase membranes. These solid-state NMR data indicate that guanidinium-phosphate interactions exist in penetratin, and guanidinium groups play a stronger structural role than ammonium groups in the lipid-assisted translocation of CPPs across liquid-crystalline cell membranes. PMID:19364134

  19. Recoupling of chemical shift anisotropies in solid-state NMR under high-speed magic-angle spinning and in uniformly 13C-labeled systems

    NASA Astrophysics Data System (ADS)

    Chan, Jerry C. C.; Tycko, Robert

    2003-05-01

    We demonstrate the possibility of recoupling chemical shift anisotropy (CSA) interactions in solid-state nuclear magnetic resonance (NMR) under high-speed magic-angle spinning (MAS) while retaining a static CSA powder pattern line shape and simultaneously attenuating homonuclear dipole-dipole interactions. CSA recoupling is accomplished by a rotation-synchronized radio-frequency pulse sequence with symmetry properties that permit static CSA line shapes to be obtained. We suggest a specific recoupling sequence, which we call ROCSA, for which the scaling factors for CSA and homonuclear dipole-dipole interactions are 0.272 and approximately 0.05, respectively. This sequence is suitable for high-speed 13C MAS NMR experiments on uniformly 13C-labeled organic compounds, including biopolymers. We demonstrate the ROCSA sequence experimentally by measuring the 13C CSA patterns of the uniformly labeled, polycrystalline compounds L-alanine and N-acetyl-D,L-valine at MAS frequencies of 11 and 20 kHz. We also present experimental data for amyloid fibrils formed by a 15-residue fragment of the β-amyloid peptide associated with Alzheimer's disease, in which four amino acid residues are uniformly labeled, demonstrating the applicability to biochemical systems of high molecular weight and significant complexity. Analysis of the CSA patterns in the amyloid fibril sample demonstrates the utility of ROCSA measurements as probes of peptide and protein conformation in noncrystalline solids.

  20. Multidimensional solid-state NMR studies of the structure and dynamics of pectic polysaccharides in uniformly 13C-labeled Arabidopsis primary cell walls

    SciTech Connect

    Dick-Perez, Marilu; Wang, Tuo; Salazar, Andre; Zabotina, Olga A.; Hong, Mei

    2012-07-08

    Plant cell wall (CW) polysaccharides are responsible for the mechanical strength and growth of plant cells; however, the high-resolution structure and dynamics of the CW polysaccharides are still poorly understood because of the insoluble nature of these molecules. Here, we use 2D and 3D magic-angle-spinning (MAS) solid-state NMR (SSNMR) to investigate the structural role of pectins in the plant CW. Intact and partially depectinated primary CWs of Arabidopsis thaliana were uniformly labeled with 13C and their NMR spectra were compared. Recent 13C resonance assignment of the major polysaccharides in Arabidopsis thaliana CWs allowed us to determine the effects of depectination on the intermolecular packing and dynamics of the remaining wall polysaccharides. 2D and 3D correlation spectra show the suppression of pectin signals, confirming partial pectin removal by chelating agents and sodium carbonate. Importantly, higher cross peaks are observed in 2D and 3D 13C spectra of the depectinated CW, suggesting higher rigidity and denser packing of the remaining wall polysaccharides compared with the intact CW. 13C spin–lattice relaxation times and 1H rotating-frame spin–lattice relaxation times indicate that the polysaccharides are more rigid on both the nanosecond and microsecond timescales in the depectinated CW. Taken together, these results indicate that pectic polysaccharides are highly dynamic and endow the polysaccharide network of the primary CW with mobility and flexibility, which may be important for pectin functions. This study demonstrates the capability of multidimensional SSNMR to determine the intermolecular interactions and dynamic structures of complex plant materials under near-native conditions. Copyright © 2012 John Wiley & Sons, Ltd.

  1. Specific 13C labeling of leucine, valine and isoleucine methyl groups for unambiguous detection of long-range restraints in protein solid-state NMR studies

    NASA Astrophysics Data System (ADS)

    Fasshuber, Hannes Klaus; Demers, Jean-Philippe; Chevelkov, Veniamin; Giller, Karin; Becker, Stefan; Lange, Adam

    2015-03-01

    Here we present an isotopic labeling strategy to easily obtain unambiguous long-range distance restraints in protein solid-state NMR studies. The method is based on the inclusion of two biosynthetic precursors in the bacterial growth medium, α-ketoisovalerate and α-ketobutyrate, leading to the production of leucine, valine and isoleucine residues that are exclusively 13C labeled on methyl groups. The resulting spectral simplification facilitates the collection of distance restraints, the verification of carbon chemical shift assignments and the measurement of methyl group dynamics. This approach is demonstrated on the type-three secretion system needle of Shigella flexneri, where 49 methyl-methyl and methyl-nitrogen distance restraints including 10 unambiguous long-range distance restraints could be collected. By combining this labeling scheme with ultra-fast MAS and proton detection, the assignment of methyl proton chemical shifts was achieved.

  2. Specific 13C labeling of leucine, valine and isoleucine methyl groups for unambiguous detection of long-range restraints in protein solid-state NMR studies.

    PubMed

    Fasshuber, Hannes Klaus; Demers, Jean-Philippe; Chevelkov, Veniamin; Giller, Karin; Becker, Stefan; Lange, Adam

    2015-03-01

    Here we present an isotopic labeling strategy to easily obtain unambiguous long-range distance restraints in protein solid-state NMR studies. The method is based on the inclusion of two biosynthetic precursors in the bacterial growth medium, α-ketoisovalerate and α-ketobutyrate, leading to the production of leucine, valine and isoleucine residues that are exclusively (13)C labeled on methyl groups. The resulting spectral simplification facilitates the collection of distance restraints, the verification of carbon chemical shift assignments and the measurement of methyl group dynamics. This approach is demonstrated on the type-three secretion system needle of Shigella flexneri, where 49 methyl-methyl and methyl-nitrogen distance restraints including 10 unambiguous long-range distance restraints could be collected. By combining this labeling scheme with ultra-fast MAS and proton detection, the assignment of methyl proton chemical shifts was achieved. PMID:25625825

  3. Solid state structure of new 5-[2-(N,N-diethylamino)ethoxy]-4,7-dimethylcoumarins by X-ray and 13C CP/MAS NMR

    NASA Astrophysics Data System (ADS)

    Ostrowska, Kinga; Hejchman, Elżbieta; Dobrzycki, Łukasz; Maciejewska, Dorota

    2015-05-01

    5-[2-(N,N-diethylamino)ethoxy]-4,7-dimethylcoumarin (1) and 6-acetyl-5-[2-(N,N-diethylamino)ethoxy]-4,7-dimethylcoumarin (2) were synthesized in a traditional way and microwave-assisted synthesis. Crystals of 2 in form of hydrochloride salt (3) were investigated using single crystal X-ray diffraction technique. In the crystal lattice of 3 there is only one type of strong hydrogen bond present involving protonated amino group and chloride anion. The whole structure is dominated by weak C-H…Cl-, C-H…O contacts. There is also visible aggregation of cations in stacks due to π-π interactions. The solid state structures of 1 and 2 derived from 13C CP/MAS NMR spectra were also proposed.

  4. The interplay between the solid effect and the cross effect mechanisms in solid state 13C DNP at 95 GHz using trityl radicals

    NASA Astrophysics Data System (ADS)

    Banerjee, Debamalya; Shimon, Daphna; Feintuch, Akiva; Vega, Shimon; Goldfarb, Daniella

    2013-05-01

    The 13C solid state Dynamic Nuclear Polarization (DNP) mechanism using trityl radicals (OX63) as polarizers was investigated in the temperature range of 10-60 K. The solutions used were 6 M 13C urea in DMSO/H2O (50% v/v) with 15 mM and 30 mM OX63. The measurements were carried out at ˜3.5 T, which corresponds to Larmor frequencies of 95 GHz and 36 MHz for the OX63 and the 13C nuclei, respectively. Measurements of the 13C signal intensity as a function of the microwave (MW) irradiation frequency yielded 13C DNP spectra with temperature dependent lineshapes for both samples. The maximum enhancement for the 30 mM sample was reached at 40 K, while that of the 15 mM sample at 20-30 K. Furthermore, the lineshapes observed showed that both the cross effect (CE) and the solid effect (SE) DNP mechanisms are active in this temperature range and that their relative contribution is temperature dependent. Simulations of the spectra with the relative contributions of the CE and SE mechanisms as a fit parameter revealed that for both samples the CE contribution decreases with decreasing temperature while the SE contribution increases. In addition, for the 15 mM sample the contributions of the two mechanisms are comparable from 20 K to 60 K while for the 30 mM the CE dominates in this range, as expected from the higher concentration. The steep decrease of the CE contribution towards low temperatures is however unexpected. The temperature dependence of the OX63 longitudinal relaxation, DNP buildup times and 13C spin lattice relaxation times did not reveal any obvious correlation with the DNP temperature dependence. A similar behavior of the CE and SE mechanism was observed for 1H DNP with the nitroxide radical TEMPOL as a polarizer. This suggests that this effect is a general phenomenon involving a temperature dependent competition between the CE and SE mechanisms, the source of which is, however, still unknown.

  5. Solid-state 13C NMR study of the mobility of polysaccharides in the cell walls of two apple cultivars of different firmness.

    PubMed

    Ng, Jovyn K T; Zujovic, Zoran D; Smith, Bronwen G; Johnston, Jason W; Schröder, Roswitha; Melton, Laurence D

    2014-03-11

    Solid-state (13)C nuclear magnetic resonance (NMR) was used to compare differences in mobility of the cell wall polysaccharides of 'Scifresh' and 'Royal Gala' apples after 20 weeks of storage. The texture of 'Scifresh' apples was markedly firmer than that of 'Royal Gala' at the end of storage. In a novel approach Two Pulse Phase Modulation (TPPM) decoupling was combined with cross polarisation (CP) and single pulse excitation (SPE) experiments. The resulting high resolution solid-state SPE spectra, unprecedented for apple cell walls, allowed a detailed insight into the physical and chemical properties of very mobile polysaccharides such as the arabinan and galactan side chains of the pectic polysaccharide rhamnogalacturonan I (RG-I). NMR showed that the cellulose rigidity was the same in the two cultivars, while arabinans were more mobile than galactans in both. Unexpectedly, arabinans in 'Scifresh' cell walls were more mobile than those in 'Royal Gala' which was unforeseen considering the greater firmness of the 'Scifresh' cultivar. PMID:24423413

  6. Short hydrogen bonds in salts of dicarboxylic acids; structural correlations from solid-state 13C and 2H NMR spectroscopy

    NASA Astrophysics Data System (ADS)

    Kalsbeek, Nicoline; Schaumburg, Kjeld; Larsen, Sine

    1993-10-01

    Solid-state 13C and 2H NMR spectra are found to very suitable for characterizing the short Osbnd H...O hydrogen bonds observed in acid salts of dicarboxylic acids. The majority of the investigated compounds are acid salts of malonic, succinic and tartaric acid with monovalent cations derived from alkali metals and small aliphatic amines. They include systems with symmetric and asymmetric hydrogen bonds. Accurate structural information about their geometry is available from low-temperature X-ray diffraction data. The 13C chemical shifts of the C atoms in the different carboxy groups display a linear variation with the absolute difference between the two Csbnd O bond lengths. Theoretical ab initio calculations for model systems showed that the nuclear quadrupole coupling constant NQCC for 2H increases with increasing asymmetry of the hydrogen-bonded system. NQCC values for 2H in the short symmetric hydrogen-bonded systems are in the range 53-59 kHz compared with the larger values of up to 166kHz found in systems with longer asymmetric hydrogen bonds. The 2H NQCC values display a perfect linear dependence on the asymmetry of the hydrogen bond. 2H NQCC decreases with decreasing temperature in the symmetric hydrogen bonds showing that the corresponding potential has a single well.

  7. Solid state structure by X-ray and 13C CP/MAS NMR of new 5-[2-(N,N-dimethylamino)ethoxy]-4,7-dimethylcoumarins

    NASA Astrophysics Data System (ADS)

    Ostrowska, Kinga; Maciejewska, Dorota; Dobrzycki, Łukasz; Socha, Pawel

    2016-05-01

    5-[2-(N,N-dimethylamino)ethoxy]-4,7-dimethylcoumarin (1) and 6-acetyl-5-[2-(N,N-dimethylamino)ethoxy]-4,7-dimethylcoumarin (2), structurally related, were synthesized using both conventional and microwave-assisted approach. An impact of acetyl groups on the molecular structure of coumarin derivatives has been examined. Crystals of 2 were investigated using single crystal and powder X-ray diffraction techniques. Compound 2 crystallizes forming two polymorphs (denoted as 2_1 and 2_2), both belonging to P21/c space group. Both polymorphs are comparably stable and can be formed simultaneously during crystallization process. The solid state structure was also analysed using the fully resolved 13C CP/MAS NMR. The double signals with the intensity ratio of about 1:1 which were observed in the 13C CP/MAS NMR spectrum of compound 1 must arise due to the presence of two conformers of 1. In contrast, NMR spectrum recorded for powder mixture of two polymorphs of compound 2 displays no signal splitting. This is related to structural similarities of molecules in both polymorphs.

  8. Tracing bacterial metabolism using multi-nuclear (1H, 2H, and 13C) Solid State NMR: Realizing an Idea Initiated by James Scott

    NASA Astrophysics Data System (ADS)

    Cody, G.; Fogel, M. L.; Jin, K.; Griffen, P.; Steele, A.; Wang, Y.

    2011-12-01

    Approximately 6 years ago, while at the Geophysical Laboratory, James Scott became interested in the application of Solid State Nuclear Magnetic Resonance Spectroscopy to study bacterial metabolism. As often happens, other experiments intervened and the NMR experiments were not pursued. We have revisited Jame's question and find that using a multi-nuclear approach (1H, 2H, and 13C Solid State NMR) on laboratory cell culture has some distinct advantages. Our experiments involved batch cultures of E. coli (MG1655) harvested at stationary phase. In all experiments the growth medium consisted of MOPS medium for enterobacteria, where the substrate is glucose. In one set of experiments, 10 % of the water was D2O; in another 10 % of the glucose was per-deuterated. The control experiment used both water and glucose at natural isotopic abundance. A kill control of dead E. coli immersed in pure D2O for an extended period exhibited no deuterium incorporation. In both deuterium enriched experiments, considerable incorporation of deuterium into E. coli's biomolecular constituents was detected via 2H Solid State NMR. In the case of the D2O enriched experiment, 58 % of the incorporated deuterium is observed in a sharp peak at a frequency of 0.31 ppm, consistent with D incorporation in the cell membrane lipids, the remainder is observed in a broad peak at a higher frequency (centered at 5.4 ppm, but spanning out to beyond 10 ppm) that is consistent with D incorporation into predominantly DNA and RNA. In the case of the D-glucose experiments, 61 % of the deuterium is observed in a sharp resonance peak at 0.34 ppm, also consistent with D incorporation into membrane lipids, the remainder of the D is observed at a broad resonance peak centered at 4.3 ppm, consistent with D enrichment in glycogen. Deuterium abundance in the E. coli cells grown in 10 % D2O is nearly 2X greater than that grown with 10 % D-glucose. Very subtle differences are observed in both the 1H and 13C solid-state

  9. Early diagenesis of mangrove leaves in a tropical estuary: Bulk chemical characterization using solid-state 13C NMR and elemental analyses

    NASA Astrophysics Data System (ADS)

    Benner, Ronald; Hatcher, Patrick G.; Hedges, John I.

    1990-07-01

    Changes in the chemical composition of mangrove ( Rhizophora mangle) leaves during decomposition in tropical estuarine waters were characterized using solid-state 13C nuclear magnetic resonance (NMR) and elemental (CHNO) analysis. Carbohydrates were the most abundant components of the leaves accounting for about 50 wt% of senescent tissues. Tannins were estimated to account for about 20 wt% of leaf tissues, and lipid components, cutin, and possibly other aliphatic biopolymers in leaf cuticles accounted for about 15 wt%. Carbohydrates were generally less resistant to decomposition than the other constituents and decreased in relative concentration during decomposition. Tannins were of intermediate resistance to decomposition and remained in fairly constant proportion during decomposition. Paraffinic components were very resistant to decomposition and increased in relative concentration as decomposition progressed. Lignin was a minor component of all leaf tissues. Standard methods for the colorimetric determination of tannins (Folin-Dennis reagent) and the gravimetric determination of lignin (Klason lignin) were highly inaccurate when applied to mangrove leaves. The N content of the leaves was particularly dynamic with values ranging from 1.27 wt% in green leaves to 0.65 wt% in senescent yellow leaves attached to trees. During decomposition in the water the N content initially decreased to 0.51 wt% due to leaching, but values steadily increased thereafter to 1.07 wt% in the most degraded leaf samples. The absolute mass of N in the leaves increased during decomposition indicating that N immobilization was occurring as decomposition progressed.

  10. Early diagenesis of mangrove leaves in a tropical estuary: Bulk chemical characterization using solid-state 13C NMR and elemental analyses

    USGS Publications Warehouse

    Benner, R.; Hatcher, P.G.; Hedges, J.I.

    1990-01-01

    Changes in the chemical composition of mangrove (Rhizophora mangle) leaves during decomposition in tropical estuarine waters were characterized using solid-state 13C nuclear magnetic resonance (NMR) and elemental (CHNO) analysis. Carbohydrates were the most abundant components of the leaves accounting for about 50 wt% of senescent tissues. Tannins were estimated to account for about 20 wt% of leaf tissues, and lipid components, cutin, and possibly other aliphatic biopolymers in leaf cuticles accounted for about 15 wt%. Carbohydrates were generally less resistant to decomposition than the other constituents and decreased in relative concentration during decomposition. Tannins were of intermediate resistance to decomposition and remained in fairly constant proportion during decomposition. Paraffinic components were very resistant to decomposition and increased in relative concentration as decomposition progressed. Lignin was a minor component of all leaf tissues. Standard methods for the colorimetric determination of tannins (Folin-Dennis reagent) and the gravimetric determination of lignin (Klason lignin) were highly inaccurate when applied to mangrove leaves. The N content of the leaves was particularly dynamic with values ranging from 1.27 wt% in green leaves to 0.65 wt% in senescent yellow leaves attached to trees. During decomposition in the water the N content initially decreased to 0.51 wt% due to leaching, but values steadily increased thereafter to 1.07 wt% in the most degraded leaf samples. The absolute mass of N in the leaves increased during decomposition indicating that N immobilization was occurring as decomposition progressed. ?? 1990.

  11. Chemical structure of soil organic matter in slickspots as investigated by advanced solid-state NMR

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Slickspot soils are saline, and knowledge of their humic chemistry would contribute to our limited understanding how salinity affects soil C and N stocks. We characterized humic acids (HAs) from slickspot soils with solid-state 13C nuclear magnetic resonance (NMR). Expanding on previous use of cross...

  12. Solid state 13C NMR analysis of shales and coals from Laramide Basins. Final report, March 1, 1995--March 31, 1996

    SciTech Connect

    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.

  13. Characteristics and degradation of carbon and phosphorus from aquatic macrophytes in lakes: Insights from solid-state (13)C NMR and solution (31)P NMR spectroscopy.

    PubMed

    Liu, Shasha; Zhu, Yuanrong; Meng, Wei; He, Zhongqi; Feng, Weiying; Zhang, Chen; Giesy, John P

    2016-02-01

    Water extractable organic matter (WEOM) derived from macrophytes plays an important role in biogeochemical cycling of nutrients, including carbon (C), nitrogen (N) and phosphorus (P) in lakes. However, reports of their composition and degradation in natural waters are scarce. Therefore, compositions and degradation of WEOM derived from six aquatic macrophytes species of Tai Lake, China, were investigated by use of solid-state (13)C NMR and solution (31)P NMR spectroscopy. Carbohydrates were the predominant constituents of WEOM fractions, followed by carboxylic acid. Orthophosphate (ortho-P) was the dominant form of P (78.7% of total dissolved P) in the water extracts, followed by monoester P (mono-P) (20.6%) and little diester P (0.65%). The proportion of mono-P in total P species increased with the percentage of O-alkyl and O-C-O increasing in the WEOM, which is likely due to degradation and dissolution of biological membranes and RNA from aquatic plants. Whereas the proportion of mono-P decreased with alkyl-C, NCH/OCH3 and COO/N-C=O increasing, which may be owing to the insoluble compounds including C functional groups of alkyl-C, NCH/OCH3 and COO/N-C=O, such as aliphatic biopolymers, lignin and peptides. Based on the results of this study and information in the literature about water column and sediment, we propose that WEOM, dominated by polysaccharides, are the most labile and bioavailable component in debris of macrophytes. Additionally, these WEOMs would also be a potential source for bioavailable organic P (e.g., RNA, DNA and phytate) for lakes. PMID:26624522

  14. Advances in Solid State Joining of High Temperature Alloys

    NASA Technical Reports Server (NTRS)

    Ding, Jeff; Schneider, Judy

    2011-01-01

    Many of the metals used in the oil and gas industry are difficult to fusion weld including Titanium and its alloys. Solid state joining processes are being pursued as an alternative process to produce robust structures more amenable to high pressure applications. Various solid state joining processes include friction stir welding (FSW) and a patented modification termed thermal stir welding (TSW). The configuration of TSWing utilizes an induction coil to preheat the material minimizing the burden on the weld tool extending its life. This provides the ability to precisely select and control the temperature to avoid detrimental changes to the microstructure. The work presented in this presentation investigates the feasibility of joining various titanium alloys using the solid state welding processes of FSW and TSW. Process descriptions and attributes of each weld process will be presented. Weld process set ]up and welding techniques will be discussed leading to the challenges experienced. Mechanical property data will also be presented.

  15. Metal Carbonation of Forsterite in Supercritical CO2 and H2O Using Solid State 29Si, 13C NMR Spectroscop

    SciTech Connect

    Kwak, Ja Hun; Hu, Jian Z.; Hoyt, David W.; Sears, Jesse A.; Wang, Chong M.; Rosso, Kevin M.; Felmy, Andrew R.

    2010-03-11

    Ex situ solid state NMR was used for the first time to study fundamental mineral carbonation processes and reaction extent relevant to geologic carbon sequestration (GCS) using a model silicate mineral forsterite (Mg2SiO4)+supercriticalCO2 with and without H2O. Run conditions were 80 C and 96 atm. 29Si NMR clearly shows that in the absence of CO2, the role of H2O is to hydrolyze surface Mg-O-Si bonds to produce dissolved Mg2+, and mono- and oligomeric hydroxylated silica species. Surface hydrolysis products contain only Q0 (Si(OH)4) and Q1(Si(OH)3OSi) species. An equilibrium between Q0, Q1 and Mg2+ with a saturated concentration equivalent to less than 3.2% of the Mg2SiO4 conversion is obtained at a reaction time of up to 7 days. Using scCO2 without H2O, no reaction is observed within 7 days. Using both scCO2 and H2O, the surface reaction products for silica are mainly Q3 (SiOH(OSi)3) species accompanied by a lesser amount of Q2 (Si(OH)2(OSi)2) and Q4 (Si(OSi)4). However, no Q0 and Q1 were detected, indicating the carbonic acid formation/deprotonation and magnesite (MgCO3) precipitation reactions are faster than the forsterite hydrolysis process. Thus it can be concluded that the Mg2SiO4 hydrolysis process is the rate limiting step of the overall mineral carbonation process. 29Si NMR combined with XRD, TEM, SAED and EDX further reveal that the reaction is a surface reaction with the Mg2SiO4 crystallite in the core and with condensed Q2-Q4 species forming amorphous surface layers. 13C MAS NMR identified a possible reaction intermediate as (MgCO3)4-Mg(OH)2-5H2O. However, at long reaction times only crystallite magnesite MgCO3 products are observed.

  16. The guest ordering and dynamics in urea inclusion compounds studied by solid-state 1H and 13C MAS NMR spectroscopy

    NASA Astrophysics Data System (ADS)

    Yang, Xiaorong; Müller, Klaus

    2011-12-01

    Urea inclusion compounds with different guest species were studied by 13C CP MAS and 1H MAS NMR spectroscopy. It is possible to arrange the asymmetric guest species in three different ways: head-head, head-tail and tail-tail. 13C CP MAS NMR studies indicate that the preference arrangement is determined by the interaction strength of the end functional groups. 13C relaxation experiments are used to study the dynamic properties of urea inclusion compounds. 13C relaxation studies on urea inclusion compounds with n-alkane or decanoic acid show that the 13C T1 and 13C T1ρ values exhibit the position dependence towards the center of the chain, indicating internal chain mobility. The analysis of variable-temperature 13C T1ρ experiments on urea inclusion compounds with hexadecane and pentadecane, for the first time, suggests that chain fluctuations and lateral motion of n-alkane guests may contribute to the 13C T1ρ relaxation.

  17. Determination of the tautomeric equilibria of pyridoyl benzoyl β-diketones in the liquid and solid state through the use of deuterium isotope effects on (1)H and (13)C NMR chemical shifts and spin coupling constants.

    PubMed

    Hansen, Poul Erik; Borisov, Eugeny V; Lindon, John C

    2015-02-01

    The tautomeric equilibria for 2-pyridoyl-, 3-pyridoyl-, and 4-pyridoyl-benzoyl methane have been investigated using deuterium isotope effects on (1)H and (13)C chemical shifts both in the liquid and the solid state. Equilibria are established both in the liquid and the solid state. In addition, in the solution state the 2-bond and 3-bond J((1)H-(13)C) coupling constants have been used to confirm the equilibrium positions. The isotope effects due to deuteriation at the OH position are shown to be superior to chemical shift in determination of equilibrium positions of these almost symmetrical -pyridoyl-benzoyl methanes. The assignments of the NMR spectra are supported by calculations of the chemical shifts at the DFT level. The equilibrium positions are shown to be different in the liquid and the solid state. In the liquid state the 4-pyridoyl derivative is at the B-form (C-1 is OH), whereas the 2-and 3-pyridoyl derivatives are in the A-form. In the solid state all three compounds are on the B-form. The 4-pyridoyl derivative shows unusual deuterium isotope effects in the solid, which are ascribed to a change of the crystal structure of the deuteriated compound. PMID:24070650

  18. Advances in Solid State Joining of High Temperature Alloys

    NASA Technical Reports Server (NTRS)

    Ding, R. Jeff; Schneider, Judy; Walker, Bryant

    2011-01-01

    Many of the metals used in the oil and gas industry are difficult to fusion weld including titanium and its alloys. Thus solid state joining processes, such as friction stir welding (FSWing) and a patented modification termed thermal stir welding (TSWing), are being pursued as alternatives to produce robust structures more amenable to high pressure applications. Unlike the FSWing process where the tool is used to heat the workpiece, TSWing utilizes an induction coil to preheat the material prior to stirring thus minimizing the burden on the weld tool and thereby extending its life. This study reports on the initial results of using a hybrid (H)-TSW process to join commercially pure, 1.3cm thick panels of titanium (CP Ti) Grade 2.

  19. Quantitative (13)C Solid-State NMR Spectra by Multiple-Contact Cross-polarization for Drug Delivery: From Active Principles to Excipients and Drug Carriers.

    PubMed

    Saïdi, Fadila; Taulelle, Francis; Martineau, Charlotte

    2016-08-01

    In this contribution, we present an analysis of the main parameters influencing the efficiency of the (1)H → (13)C multiple-contact cross-polarization nuclear magnetic resonance (NMR) experiment in the context of solid pharmaceutical materials. Using the optimum experimental conditions, quantitative (13)C NMR spectra are then obtained for porous metal-organic frameworks (potential drug carriers) and for components present in drug formulations (active principle ingredient and excipients, amorphous or crystalline). Finally, we show that mixtures of components can also be quantified with this method and, hence, that it represents an ideal tool for quantification of pharmaceutical formulations by (13)C cross-polarization under magic-angle spinning NMR in the industry as it is robust and easy to set up, much faster than direct (13)C polarization and is efficient for samples at natural abundance. PMID:27372550

  20. Restraints on backbone conformations in solid state NMR studies of uniformly labeled proteins from quantitative amide 15N–15N and carbonyl 13C–13C dipolar recoupling data

    PubMed Central

    Hu, Kan-Nian; Qiang, Wei; Bermejo, Guillermo A.; Schwieters, Charles D.; Tycko, Robert

    2013-01-01

    Recent structural studies of uniformly 15N, 13C-labeled proteins by solid state nuclear magnetic resonance (NMR) rely principally on two sources of structural restraints: (i) restraints on backbone conformation from isotropic 15N and 13C chemical shifts, based on empirical correlations between chemical shifts and backbone torsion angles; (ii) restraints on inter-residue proximities from qualitative measurements of internuclear dipole–dipole couplings, detected as the presence or absence of inter-residue crosspeaks in multidimensional spectra. We show that site-specific dipole–dipole couplings among 15N-labeled backbone amide sites and among 13C-labeled backbone carbonyl sites can be measured quantitatively in uniformly-labeled proteins, using dipolar recoupling techniques that we call 15N-BARE and 13C-BARE (BAckbone REcoupling), and that the resulting data represent a new source of restraints on backbone conformation. 15N-BARE and 13C-BARE data can be incorporated into structural modeling calculations as potential energy surfaces, which are derived from comparisons between experimental 15N and 13C signal decay curves, extracted from crosspeak intensities in series of two-dimensional spectra, with numerical simulations of the 15N-BARE and 13C-BARE measurements. We demonstrate this approach through experiments on microcrystalline, uniformly 15N, 13C-labeled protein GB1. Results for GB1 show that 15N-BARE and 13C-BARE restraints are complementary to restraints from chemical shifts and inter-residue crosspeaks, improving both the precision and the accuracy of calculated structures. PMID:22449573

  1. Solid state nuclear magnetic resonance investigations of advanced energy materials

    NASA Astrophysics Data System (ADS)

    Bennett, George D.

    In order to better understand the physical electrochemical changes that take place in lithium ion batteries and asymmetric hybrid supercapacitors solid state nuclear magnetic resonance (NMR) spectroscopy has been useful to probe and identify changes on the atomic and molecular level. NMR is used to characterize the local environment and investigate the dynamical properties of materials used in electrochemical storage devices (ESD). NMR investigations was used to better understand the chemical composition of the solid electrolyte interphase which form on the negative and positive electrodes of lithium batteries as well as identify the breakdown products that occur in the operation of the asymmetric hybrid supercapacitors. The use of nano-structured particles in the development of new materials causes changes in the electrical, structural and other material properties. NMR was used to investigate the affects of fluorinated and non fluorinated single wall nanotubes (SWNT). In this thesis three experiments were performed using solid state NMR samples to better characterize them. The electrochemical reactions of a lithium ion battery determine its operational profile. Numerous means have been employed to enhance battery cycle life and operating temperature range. One primary means is the choice and makeup of the electrolyte. This study focuses on the characteristics of the solid electrolyte interphase (SEI) that is formed on the electrodes surface during the charge discharge cycle. The electrolyte in this study was altered with several additives in order to determine the influence of the additives on SEI formation as well as the intercalation and de-intercalation of lithium ions in the electrodes. 7Li NMR studies where used to characterize the SEI and its composition. Solid state NMR studies of the carbon enriched acetonitrile electrolyte in a nonaqueous asymmetric hybrid supercapacitor were performed. Magic angle spinning (MAS) coupled with cross polarization NMR

  2. Solid State Ionics Advanced Materials for Emerging Technologies

    NASA Astrophysics Data System (ADS)

    Chowdari, B. V. R.; Careem, M. A.; Dissanayake, M. A. K. L.; Rajapakse, R. M. G.; Seneviratne, V. A.

    2006-06-01

    Keynote lecture. Challenges and opportunities of solid state ionic devices / W. Weppner -- pt. I. Ionically conducting inorganic solids. Invited papers. Multinuclear NMR studies of mass transport of phosphoric acid in water / J. R. P. Jayakody ... [et al.]. Crystalline glassy and polymeric electrolytes: similarities and differences in ionic transport mechanisms / J.-L. Souquet. 30 years of NMR/NQR experiments in solid electrolytes / D. Brinkmann. Analysis of conductivity and NMR measurements in Li[symbol]La[symbol]TiO[symbol] fast Li[symbol] ionic conductor: evidence for correlated Li[symbol] motion / O. Bohnké ... [et al.]. Transport pathways for ions in disordered solids from bond valence mismatch landscapes / S. Adams. Proton conductivity in condensed phases of water: implications on linear and ball lightning / K. Tennakone -- Contributed papers. Proton transport in nanocrystalline bioceramic materials: an investigative study of synthetic bone with that of natural bone / H. Jena, B. Rambabu. Synthesis and properties of the nanostructured fast ionic conductor Li[symbol]La[symbol]TiO[symbol] / Q. N. Pham ... [et al.]. Hydrogen production: ceramic materials for high temperature water electrolysis / A. Hammou. Influence of the sintering temperature on pH sensor ability of Li[symbol]La[symbol]TiO[symbol]. Relationship between potentiometric and impedance spectroscopy measurements / Q. N. Pham ... [et al.]. Microstructure chracterization and ionic conductivity of nano-sized CeO[symbol]-Sm[symbol]O[symbol] system (x=0.05 - 0.2) prepared by combustion route / K. Singh, S. A. Acharya, S. S. Bhoga. Red soil in Northern Sri Lanka is a natural magnetic ceramic / K. Ahilan ... [et al.]. Neutron scattering of LiNiO[symbol] / K. Basar ... [et al.]. Preparation and properties of LiFePO[symbol] nanorods / L. Q. Mai ... [et al.]. Structural and electrochemical properties of monoclinic and othorhombic MoO[symbol] phases / O. M. Hussain ... [et al.]. Preparation of Zircon (Zr

  3. Solid State Ionics Advanced Materials for Emerging Technologies

    NASA Astrophysics Data System (ADS)

    Chowdari, B. V. R.; Careem, M. A.; Dissanayake, M. A. K. L.; Rajapakse, R. M. G.; Seneviratne, V. A.

    2006-06-01

    Keynote lecture. Challenges and opportunities of solid state ionic devices / W. Weppner -- pt. I. Ionically conducting inorganic solids. Invited papers. Multinuclear NMR studies of mass transport of phosphoric acid in water / J. R. P. Jayakody ... [et al.]. Crystalline glassy and polymeric electrolytes: similarities and differences in ionic transport mechanisms / J.-L. Souquet. 30 years of NMR/NQR experiments in solid electrolytes / D. Brinkmann. Analysis of conductivity and NMR measurements in Li[symbol]La[symbol]TiO[symbol] fast Li[symbol] ionic conductor: evidence for correlated Li[symbol] motion / O. Bohnké ... [et al.]. Transport pathways for ions in disordered solids from bond valence mismatch landscapes / S. Adams. Proton conductivity in condensed phases of water: implications on linear and ball lightning / K. Tennakone -- Contributed papers. Proton transport in nanocrystalline bioceramic materials: an investigative study of synthetic bone with that of natural bone / H. Jena, B. Rambabu. Synthesis and properties of the nanostructured fast ionic conductor Li[symbol]La[symbol]TiO[symbol] / Q. N. Pham ... [et al.]. Hydrogen production: ceramic materials for high temperature water electrolysis / A. Hammou. Influence of the sintering temperature on pH sensor ability of Li[symbol]La[symbol]TiO[symbol]. Relationship between potentiometric and impedance spectroscopy measurements / Q. N. Pham ... [et al.]. Microstructure chracterization and ionic conductivity of nano-sized CeO[symbol]-Sm[symbol]O[symbol] system (x=0.05 - 0.2) prepared by combustion route / K. Singh, S. A. Acharya, S. S. Bhoga. Red soil in Northern Sri Lanka is a natural magnetic ceramic / K. Ahilan ... [et al.]. Neutron scattering of LiNiO[symbol] / K. Basar ... [et al.]. Preparation and properties of LiFePO[symbol] nanorods / L. Q. Mai ... [et al.]. Structural and electrochemical properties of monoclinic and othorhombic MoO[symbol] phases / O. M. Hussain ... [et al.]. Preparation of Zircon (Zr

  4. Advanced solid-state NMR characterization of marine dissolved organic matter isolated using the coupled reverse osmosis/electrodialysis method.

    PubMed

    Mao, Jingdong; Kong, Xueqian; Schmidt-Rohr, Klaus; Pignatello, Joseph J; Perdue, E Michael

    2012-06-01

    Advanced (13)C solid-state techniques were employed to investigate the major structural characteristics of two surface-seawater dissolved organic matter (DOM) samples isolated using the novel coupled reverse osmosis/electrodialysis method. The NMR techniques included quantitative (13)C direct polarization/magic angle spinning (DP/MAS) and DP/MAS with recoupled dipolar dephasing, (13)C cross-polarization/total sideband suppression (CP/TOSS), (13)C chemical shift anisotropy filter, CH, CH(2), and CH(n) selection, two-dimensional (1)H-(13)C heteronuclear correlation NMR (2D HETCOR), 2D HETCOR combined with dipolar dephasing, and (15)N cross-polarization/magic angle spinning (CP/MAS). The two samples (Coastal and Marine DOM) were collected at the mouth of the Ogeechee River and in the Gulf Stream, respectively. The NMR results indicated that they were structurally distinct. Coastal DOM contained significantly more aromatic and carbonyl carbons whereas Marine DOM was markedly enriched in alkoxy carbon (e.g., carbohydrate-like moieties). Both samples contained significant amide N, but Coastal DOM had nitrogen bonded to aromatic carbons. Our dipolar-dephased spectra indicated that a large fraction of alkoxy carbons were not protonated. For Coastal DOM, our NMR results were consistent with the presence of the major structural units of (1) carbohydrate-like moieties, (2) lignin residues, (3) peptides or amino sugars, and (4) COO-bonded alkyls. For Marine DOM, they were (1) carbohydrate-like moieties, (2) peptides or amino sugars, and (3) COO-bonded alkyls. In addition, both samples contained significant amounts of nonpolar alkyl groups. The potential sources of the major structural units of DOM were discussed in detail. Nonprotonated O-alkyl carbon content was proposed as a possible index of humification. PMID:22553962

  5. Solid-state {sup 19}F and {sup 13}C NMR of room temperature fluorinated graphite and samples thermally treated under fluorine: Low-field and high-resolution studies

    SciTech Connect

    Giraudet, J.; Dubois, M.; Guerin, K.; Pinheiro, J.P.; Hamwi, A.; Stone, W.E.E.; Pirotte, P.; Masin, F. . E-mail: fmasin@ulb.ac.be

    2005-04-15

    Room temperature graphite fluorides consisting of raw material and samples post-treated in pure fluorine atmosphere in the temperature range 100-500 deg. C have been studied by solid-state NMR. Several NMR approaches have been used, both high and low-field {sup 19}F, {sup 19}F MAS and {sup 13}C MAS with {sup 19}F to {sup 13}C cross polarization. The modifications, in the graphitic lattice, of the catalytic iodine fluorides products have been examined. A transformation of the C-F bond character from semi-ionic to covalent has been found to occur at a post-treatment temperature close to 400 deg. C. It is shown that covalency increases with temperature.

  6. Distinguishing tautomerism in the crystal structure of (Z)-N-(5-ethyl-2,3-di-hydro-1,3,4-thiadiazol-2-ylidene) -4-methylbenzenesulfonamide using DFT-D calculations and {sup 13}C solid-state NMR

    SciTech Connect

    Li, Xiaozhou; Bond, Andrew D.; Johansson, Kristoffer E.; Van de Streek, Jacco

    2014-08-01

    The crystal structure of (Z)-N-(5-ethyl-2,3-di-hydro-1,3,4-thiadiazol-2-ylidene) -4-methylbenzenesulfonamide contains an imine tautomer, rather than the previously reported amine tautomer. The tautomers can be distinguished using dispersion-corrected density functional theory calculations and by comparison of calculated and measured {sup 13}C solid-state NMR spectra. The crystal structure of the title compound, C{sub 11}H{sub 13}N{sub 3}O{sub 2}S{sub 2}, has been determined previously on the basis of refinement against laboratory powder X-ray diffraction (PXRD) data, supported by comparison of measured and calculated {sup 13}C solid-state NMR spectra [Hangan et al. (2010 ▶). Acta Cryst. B66, 615–621]. The mol@@ecule is tautomeric, and was reported as an amine tautomer [systematic name: N-(5-ethyl-1,3,4-thia@@diazol-2-yl)-p-toluene@@sulfonamide], rather than the correct imine tautomer. The protonation site on the mol@@ecule’s 1,3,4-thia@@diazole ring is indicated by the inter@@molecular contacts in the crystal structure: N—H⋯O hydrogen bonds are established at the correct site, while the alternative protonation site does not establish any notable inter molecular inter@@actions. The two tautomers provide essentially identical Rietveld fits to laboratory PXRD data, and therefore they cannot be directly distinguished in this way. However, the correct tautomer can be distinguished from the incorrect one by previously reported qu@@anti@@tative criteria based on the extent of structural distortion on optimization of the crystal structure using dispersion-corrected density functional theory (DFT-D) calculations. Calculation of the {sup 13}C SS-NMR spectrum based on the correct imine tautomer also provides considerably better agreement with the measured {sup 13}C SS-NMR spectrum.

  7. (1)H-(13)C-(29)Si triple resonance and REDOR solid-state NMR-A tool to study interactions between biosilica and organic molecules in diatom cell walls.

    PubMed

    Wisser, Dorothea; Brückner, Stephan I; Wisser, Florian M; Althoff-Ospelt, Gerhard; Getzschmann, Jürgen; Kaskel, Stefan; Brunner, Eike

    2015-01-01

    Triple resonance solid-state NMR experiments using the spin combination (1)H-(13)C-(29)Si are still rarely found in the literature. This is due to the low natural abundance of the two heteronuclei. Such experiments are, however, increasingly important to study hybrid materials such as biosilica and others. A suitable model substance, ideally labeled with both (13)C and (29)Si, is thus very useful to optimize the experiments before applying them to studies of more complex samples such as biosilica. Tetraphenoxysilane could be synthesized in an easy, two-step synthesis including double isotope labelling. Using tetraphenoxysilane, we established a (1)H-(13)C-(29)Si double CP-based HETCOR experiment and applied it to diatom biosilica from the diatom species Thalassiosira pseudonana. Furthermore, we carried out (1)H-(13)C{(29)Si} CP-REDOR experiments in order to estimate the distance between the organic matrix and the biosilica. Our experiments on diatom biosilica strongly indicate a close contact between polyamine-containing parts of the organic matrix and the silica. This corroborates the assumption that the organic matrix is essential for the control of the cell wall formation. PMID:25638422

  8. Residue specific hydration of primary cell wall potato pectin identified by solid-state 13C single-pulse MAS and CP/MAS NMR spectroscopy.

    PubMed

    Larsen, Flemming H; Byg, Inge; Damager, Iben; Diaz, Jerome; Engelsen, Søren B; Ulvskov, Peter

    2011-05-01

    Hydration of rhamnogalacturonan-I (RG-I) derived from potato cell wall was analyzed by (13)C single-pulse (SP) magic-angle-spinning (MAS) and (13)C cross-polarization (CP) MAS nuclear magnetic resonance (NMR) and supported by (2)H SP/MAS NMR experiments. The study shows that the arabinan side chains hydrate more readily than the galactan side chains and suggests that the overall hydration properties can be controlled by modifying the ratio of these side chains. Enzymatic modification of native (NA) RG-I provided samples with reduced content of arabinan (sample DA), galactan (sample DG), or both side chains (sample DB). Results of these samples suggested that hydration properties were determined by the length and character of the side chains. NA and DA exhibited similar hydration characteristics, whereas DG and DB were difficult to hydrate because of the less hydrophilic properties of the rhamnose-galacturonic acid (Rha-GalA) backbone in RG-I. Potential food ingredient uses of RG-I by tailoring of its structure are discussed. PMID:21462966

  9. Quantitative comparison of structure and dynamics of elastin following three isolation schemes by 13C solid state NMR and MALDI mass spectrometry

    PubMed Central

    Papaioannou, A.; Louis, M.; Dhital, B.; Ho, H. P.; Chang, E. J.

    2015-01-01

    Methods for isolating elastin from fat, collagen, and muscle, commonly used in the design of artificial elastin based biomaterials, rely on exposing tissue to harsh pH levels and temperatures that usually denature many proteins. At present, a quantitative measurement of the modifications to elastin following isolation from other extracellular matrix constituents has not been reported. Using magic angle spinning 13C NMR spectroscopy and relaxation methodologies, we have measured the modification in structure and dynamics following three known purification protocols. Our experimental data reveal that the 13C spectra of the hydrated samples appear remarkably similar across the various purification methods. Subtle differences in the half maximum widths were observed in the backbone carbonyl suggesting possible structural heterogeneity across the different methods of purification. Additionally, small differences in the relative signal intensities were observed between purified samples. Lyophilizing the samples results in a reduction of backbone motion and reveals additional differences across the purification methods studied. These differences were most notable in the alanine motifs indicating possible changes in cross-linking or structural rigidity. The measured correlation times of glycine and proline moieties are observed to also vary considerably across the different purification methods, which may be related to peptide bond cleavage. Lastly, the relative concentration of desmosine cross-links in the samples quantified by MALDI mass spectrometry is reported. PMID:25592991

  10. Development of qualitative and quantitative analysis methods in pharmaceutical application with new selective signal excitation methods for 13 C solid-state nuclear magnetic resonance using 1 H T1rho relaxation time.

    PubMed

    Nasu, Mamiko; Nemoto, Takayuki; Mimura, Hisashi; Sako, Kazuhiro

    2013-01-01

    Most pharmaceutical drug substances and excipients in formulations exist in a crystalline or amorphous form, and an understanding of their state during manufacture and storage is critically important, particularly in formulated products. Carbon 13 solid-state nuclear magnetic resonance (NMR) spectroscopy is useful for studying the chemical and physical state of pharmaceutical solids in a formulated product. We developed two new selective signal excitation methods in (13) C solid-state NMR to extract the spectrum of a target component from such a mixture. These methods were based on equalization of the proton relaxation time in a single domain via rapid intraproton spin diffusion and the difference in proton spin-lattice relaxation time in the rotating frame ((1) H T1rho) of individual components in the mixture. Introduction of simple pulse sequences to one-dimensional experiments reduced data acquisition time and increased flexibility. We then demonstrated these methods in a commercially available drug and in a mixture of two saccharides, in which the (13) C signals of the target components were selectively excited, and showed them to be applicable to the quantitative analysis of individual components in solid mixtures, such as formulated products, polymorphic mixtures, or mixtures of crystalline and amorphous phases. PMID:23147444

  11. Use of solid waste for chemical stabilization: Adsorption isotherms and {sup 13}C solid-state NMR study of hazardous organic compounds sorbed on coal fly ash

    SciTech Connect

    Netzel, D.A.; Lane, D.C.; Rovani, J.F.; Cox, J.D.; Clark, J.A.; Miknis, F.P.

    1993-09-01

    Adsorption of hazardous organic compounds on the Dave Johnston plant fly ash is described. Fly ash from Dave Johnston and Laramie River power plants were characterized using elemental, x-ray, and {sup 29}Si NMR; the Dave Johnston (DJ) fly ash had higher quartz contents, while the Laramie River fly ash had more monomeric silicate anions. Adsorption data for hydroaromatics and chlorobenzenes indicate that the adsorption capacity of DJ coal fly ash is much less than that of activated carbon by a factor of >3000; but it is needed to confirm that solid-gas and solid-liquid equilibrium isotherms can indeed be compared. However, for pyridine, pentachlorophenol, naphthalene, and 1,1,2,2-tetrachloroethane, the DJ fly ash appears to adsorb these compounds nearly as well as activated carbon. {sup 13}C NMR was used to study the adsorption of hazardous org. cpds on coal fly ash; the nuclear spin relaxation times often were very long, resulting in long experimental times to obtain a spectrum. Using a jumbo probe, low concentrations of some hazardous org. cpds could be detected; for pentachlorophenol adsorbed onto fly ash, the chemical shift of the phenolic carbon was changed. Use of NMR to study the adsorption needs further study.

  12. Solid-state 13C NMR study of banana liquid crystals - 3: Alkyl-tail-group packing environments of an acute-angle bent-core molecule in the hexagonal columnar and cubic phases

    NASA Astrophysics Data System (ADS)

    Kurosu, Hiromichi; Endo, Yumi; Kimura, Saori; Hashimoto, Tomoko; Harada, Motoi; Lee, Eun-Woo; Sone, Masato; Watanabe, Junji; Kang, Sungmin

    2016-02-01

    Solid-state 13C nuclear magnetic resonance (NMR) measurements were performed on the hexagonal columnar and cubic phases of an acute-angle banana-shaped molecule, N(1,7)-S30. In the hexagonal columnar phase, three peaks appear at the NMR chemical shifts assigned to the internal methylene carbons of alkyl tails, indicating that the two alkyl tails have different packing structures, and one of the tails has two different conformations within a single molecule. Combined cross-polarization/magic-angle spinning and pulse saturation transfer/magic-angle spinning measurements show that one of the alkyl chains is located inside and the other is located outside the columnar structure. In the cubic phase, pulse saturation transfer/magic-angle spinning measurement shows that only one peak appears at the NMR chemical shifts assigned to the internal methylene carbons of alkyl tails, indicating that both of the alkyl chains are located outside the cubic structure.

  13. A study of conformational stability of poly(L-alanine), poly(L-valine), and poly(L-alanine)/poly(L-valine) blends in the solid state by (13)C cross-polarization/magic angle spinning NMR.

    PubMed

    Murata, Katsuyoshi; Kuroki, Shigeki; Kimura, Hideaki; Ando, Isao

    2002-06-01

    13C cross-polarization/magic angle spinning (CP/MAS) NMR and (1)H T(1rho) experiments of poly(L-alanine) (PLA), poly(L-valine) (PLV), and PLA/PLV blends have been carried out in order to elucidate the conformational stability of the polypeptides in the solid state. These were prepared by adding a trifluoroacetic acid (TFA) solution of the polymer with a 2.0 wt/wt % of sulfuric acid (H(2)SO(4)) to alkaline water. From these experimental results, it is clarified that the conformations of PLA and PLV in their blends are strongly influenced by intermolecular hydrogen-bonding interactions that cause their miscibility at the molecular level. PMID:11948439

  14. Accurate measurement of methyl 13C chemical shifts by solid-state NMR for the determination of protein side chain conformation: the influenza a M2 transmembrane peptide as an example.

    PubMed

    Hong, Mei; Mishanina, Tatiana V; Cady, Sarah D

    2009-06-10

    The use of side chain methyl (13)C chemical shifts for the determination of the rotameric conformation of Val and Leu residues in proteins by solid-state NMR spectroscopy is described. Examination of the solution NMR stereospecifically assigned methyl groups shows significant correlation between the difference in the two methyl carbons' chemical shifts and the side chain conformation. It is found that alpha-helical and beta-sheet backbones cause different side chain methyl chemical shift trends. In alpha-helical Leu's, a relatively large absolute methyl (13)C shift difference of 2.89 ppm is found for the most populated mt rotamer (chi(1) = -60 degrees, chi(2) = 180 degrees), while a much smaller value of 0.73 ppm is found for the next populated tp rotamer (chi(1) = 180 degrees, chi(2) = 60 degrees). For alpha-helical Val residues, the dominant t rotamer (chi(1) = 180 degrees) has more downfield Cgamma2 chemical shifts than Cgamma1 by 1.71 ppm, while the next populated m rotamer (chi(1) = -60 degrees) shows the opposite trend of more downfield Cgamma1 chemical shift by 1.23 ppm. These significantly different methyl (13)C chemical shifts exist despite the likelihood of partial rotameric averaging at ambient temperature. We show that these conformation-dependent methyl (13)C chemical shifts can be utilized for side chain structure determination once the methyl (13)C resonances are accurately measured by double-quantum (DQ) filtered 2D correlation experiments, most notably the dipolar DQ to single-quantum (SQ) correlation technique. The advantage of the DQ-SQ correlation experiment over simple 2D SQ-SQ correlation experiments is demonstrated on the transmembrane peptide of the influenza A M2 proton channel. The methyl chemical shifts led to predictions of the side chain rotameric states for several Val and Leu residues in this tetrameric helical bundle. The predicted Val rotamers were further verified by dipolar correlation experiments that directly measure the chi(1

  15. Secondary Structure, Backbone Dynamics, and Structural Topology of Phospholamban and Its Phosphorylated and Arg9Cys-Mutated Forms in Phospholipid Bilayers Utilizing 13C and 15N Solid-State NMR Spectroscopy

    PubMed Central

    2015-01-01

    Phospholamban (PLB) is a membrane protein that regulates heart muscle relaxation rates via interactions with the sarcoplasmic reticulum Ca2+ ATPase (SERCA). When PLB is phosphorylated or Arg9Cys (R9C) is mutated, inhibition of SERCA is relieved. 13C and 15N solid-state NMR spectroscopy is utilized to investigate conformational changes of PLB upon phosphorylation and R9C mutation. 13C=O NMR spectra of the cytoplasmic domain reveal two α-helical structural components with population changes upon phosphorylation and R9C mutation. The appearance of an unstructured component is observed on domain Ib. 15N NMR spectra indicate an increase in backbone dynamics of the cytoplasmic domain. Wild-type PLB (WT-PLB), Ser16-phosphorylated PLB (P-PLB), and R9C-mutated PLB (R9C-PLB) all have a very dynamic domain Ib, and the transmembrane domain has an immobile component. 15N NMR spectra indicate that the cytoplasmic domain of R9C-PLB adopts an orientation similar to P-PLB and shifts away from the membrane surface. Domain Ib (Leu28) of P-PLB and R9C-PLB loses the alignment. The R9C-PLB adopts a conformation similar to P-PLB with a population shift to a more extended and disordered state. The NMR data suggest the more extended and disordered forms of PLB may relate to inhibition relief. PMID:24511878

  16. Environmental performance evaluation of an advanced-design solid-state television camera

    NASA Technical Reports Server (NTRS)

    1979-01-01

    The development of an advanced-design black-and-white solid-state television camera which can survive exposure to space environmental conditions was undertaken. A 380 x 488 element buried-channel CCD is utilized as the image sensor to ensure compatibility with 525-line transmission and display equipment. Specific camera design approaches selected for study and analysis included: (1) component and circuit sensitivity to temperature; (2) circuit board thermal and mechanical design; and (3) CCD temperature control. Preferred approaches were determined and integrated into the final design for two deliverable solid-state TV cameras. One of these cameras was subjected to environmental tests to determine stress limits for exposure to vibration, shock, acceleration, and temperature-vacuum conditions. These tests indicate performance at the design goal limits can be achieved for most of the specified conditions.

  17. Advanced Solid State Pixel Detectors for Future High Energy X-ray Missions

    NASA Astrophysics Data System (ADS)

    Harrison, Fiona

    We propose to advance the state of the art in solid state high energy X-ray pixel detectors for astrophysics. This program builds on advanced readout technology developed for suborbital and the NuSTAR space mission, and combines newly-developed CdTe PIN sensors and materials characterization techniques to achieve detectors broad band (1 - 200 keV), sub-keV energy resolution, and 300 micron spatial resolution. The low-noise readout technology will also be taken to the next generation with reduced pixel size, lower noise and significantly reduced dead time.

  18. Experimental (X-ray, (13)C CP/MAS NMR, IR, RS, INS, THz) and Solid-State DFT Study on (1:1) Co-Crystal of Bromanilic Acid and 2,6-Dimethylpyrazine.

    PubMed

    Łuczyńska, Katarzyna; Drużbicki, Kacper; Lyczko, Krzysztof; Dobrowolski, Jan Cz

    2015-06-01

    A combined structural, vibrational spectroscopy, and solid-state DFT study of the hydrogen-bonded complex of bromanilic acid with 2,6-dimethylpyrazine is reported. The crystallographic structure was determined by means of low-temperature single-crystal X-ray diffraction, which reveals the molecular units in their native protonation states, forming one-dimensional infinite nets of moderate-strength O···H-N hydrogen bonds. The nature of the crystallographic forces, stabilizing the studied structure, has been drawn by employing the noncovalent interactions analysis. It was found that, in addition to the hydrogen bonding, the intermolecular forces are dominated by stacking interactions and C-H···O contacts. The thermal and calorimetric analysis was employed to probe stability of the crystal phase. The structural analysis was further supported by a computationally assisted (13)C CP/MAS NMR study, providing a complete assignment of the recorded resonances. The vibrational dynamics was explored by combining the optical (IR, Raman, TDs-THz) and inelastic neutron scattering (INS) spectroscopy techniques with the state-of-the-art solid-state density functional theory (DFT) computations. Despite the quasi-harmonic approximation assumed throughout the study, an excellent agreement between the theoretical and experimental data was achieved over the entire spectral range, allowing for a deep and possibly thorough understanding of the vibrational characteristics of the system. Particularly, the significant influence of the long-range dipole coupling on the IR spectrum has been revealed. On the basis of a wealth of information gathered, the recent implementation of a dispersion-corrected linear-response scheme has been extensively examined. PMID:25961154

  19. Advanced Solid-State 13C NMR Analysis of Organic Matter in a Nebraska Corn Soil Amended with Cattle Manure

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Annual application of cattle manure in a farmer's field in eastern Nebraska for four years caused improved soil nitrogen (N) and phosphorus (P) supply and increased corn yield in less productive portions of the field. As a first step toward identifying the soil processes that led to these changes, t...

  20. Examination of the structure in solid state of amino analogs of 4,4‧-[1,5-pentanediylbis(oxy)]bisbenzonitrile by means of X-ray diffraction, 13C CP/MAS NMR, and theoretical calculations

    NASA Astrophysics Data System (ADS)

    Maciejewska, Dorota; Wolska, Irena; Żabiński, Jerzy

    2008-05-01

    A single crystal of X-ray diffraction structures is presented for 4,4'-[1,5-(3-oxapentanediylbis(amino))]bisbenzonitrile 2 and 4,4'-[1,5-( N-methyl-3-azapentane-diylbis(oxy))]bisbenzonitrile 3. The molecular structures of these derivatives differ especially in conformations of the central linker: in 2 this linker adopts a trans/ gauche conformation, whereas in 3 - a fully extended conformation. The N atoms in various positions of the aliphatic linker change dramatically the molecular packing mode of both bisnitriles. But in both cases the nitrile groups take part in intermolecular hydrogen bonds: a type of N sbnd H···N in 2 and of C sbnd H···N in 3. Various conformations of both molecules were reflected in 13C CP/MAS NMR spectra in solid state as single and double resonance patterns for 2 and 3, respectively. A preliminary anticancer assay against 60 cell lines of 3 reveals strong growth inhibition of leukemia, melanoma, and renal cancer cells.

  1. Model-free estimation of the effective correlation time for C-H bond reorientation in amphiphilic bilayers: 1H-13C solid-state NMR and MD simulations

    NASA Astrophysics Data System (ADS)

    Ferreira, Tiago Mendes; Ollila, O. H. Samuli; Pigliapochi, Roberta; Dabkowska, Aleksandra P.; Topgaard, Daniel

    2015-01-01

    Molecular dynamics (MD) simulations give atomically detailed information on structure and dynamics in amphiphilic bilayer systems on timescales up to about 1 μs. The reorientational dynamics of the C-H bonds is conventionally verified by measurements of 13C or 2H nuclear magnetic resonance (NMR) longitudinal relaxation rates R1, which are more sensitive to motional processes with correlation times close to the inverse Larmor frequency, typically around 1-10 ns on standard NMR instrumentation, and are thus less sensitive to the 10-1000 ns timescale motion that can be observed in the MD simulations. We propose an experimental procedure for atomically resolved model-free estimation of the C-H bond effective reorientational correlation time τe, which includes contributions from the entire range of all-atom MD timescales and that can be calculated directly from the MD trajectories. The approach is based on measurements of 13C R1 and R1ρ relaxation rates, as well as 1H-13C dipolar couplings, and is applicable to anisotropic liquid crystalline lipid or surfactant systems using a conventional solid-state NMR spectrometer and samples with natural isotopic composition. The procedure is demonstrated on a fully hydrated lamellar phase of 1-palmitoyl-2-oleoyl-phosphatidylcholine, yielding values of τe from 0.1 ns for the methyl groups in the choline moiety and at the end of the acyl chains to 3 ns for the g1 methylene group of the glycerol backbone. MD simulations performed with a widely used united-atom force-field reproduce the τe-profile of the major part of the acyl chains but underestimate the dynamics of the glycerol backbone and adjacent molecular segments. The measurement of experimental τe-profiles can be used to study subtle effects on C-H bond reorientational motions in anisotropic liquid crystals, as well as to validate the C-H bond reorientation dynamics predicted in MD simulations of amphiphilic bilayers such as lipid membranes.

  2. Optimized strategy of 1H and 13C solid-state NMR methods to investigate water dynamics in soil organic matter as well as the influence of crystallinity of poly(methylene) segments

    NASA Astrophysics Data System (ADS)

    Bertmer, Marko; Jaeger, Alexander; Schwarz, Jette; Schaumann, Gabriele

    2010-05-01

    Water plays a crucial role in soil organic matter (SOM) having various different functions such as transport of material, elution of ,e. g., pollutants in soil, and also the sequestration of humic substances. Furthermore, the generation and quantification of hydrophilic and hydrophobic regions in soil has several effects on SOM which can also include the storage amount and time of certain material, especially chemical pollutants. The importance of water in soil is also documented by the multitude of scientific approaches to characterize soils including diffusion NMR to study the water channel structure in soil. Our focus is on the study of water dynamics and soil structure to elucidate mechanisms of physicochemical aging. The approach uses the application of various solid-state NMR techniques - including 1H and 13C NMR - to get a multitude of information on SOM. In non-rotating samples, 1H lines are usually very broad and unstructured. Nevertheless, this rather simple technique allows for a differentiation of 1H containing chemicals based on their dynamics in soil. This includes rather solid soil components and solid as well as mobile water molecules. Based on an optimized 1H solid-state NMR strategy to study soil material together with a straightforward lineshape analysis, a series of soils and peats are characterized. Although even 1H NMR with sample spinning (MAS) often gives only limited information on different structures, we present results on the application of 2D 1H-1H phase-modulated Lee-Goldburg sequences (PMLG), that show already at medium spinning speeds the separation of functional groups. Their quantification can be correlated with sample composition, type of sample conditioning, and other parameters such as cation type or concentration and heat treatment. We are especially interested to correlate NMR data with DSC measurements based on a certain heat treatment of the soils. Our proposed model describes the presence of water in soil as a matrix

  3. Structural features of a bituminous coal and their changes during low-temperature oxidation and loss of volatiles investigated by advanced solid-state NMR spectroscopy

    USGS Publications Warehouse

    Mao, J.-D.; Schimmelmann, A.; Mastalerz, Maria; Hatcher, P.G.; Li, Y.

    2010-01-01

    Quantitative and advanced 13C solid-state NMR techniques were employed to investigate (i) the chemical structure of a high volatile bituminous coal, as well as (ii) chemical structural changes of this coal after evacuation of adsorbed gases, (iii) during oxidative air exposure at room temperature, and (iv) after oxidative heating in air at 75 ??C. The solid-state NMR techniques employed in this study included quantitative direct polarization/magic angle spinning (DP/MAS) at a high spinning speed of 14 kHz, cross polarization/total sideband suppression (CP/TOSS), dipolar dephasing, CH, CH2, and CHn selection, 13C chemical shift anisotropy (CSA) filtering, two-dimensional (2D) 1H-13C heteronuclear correlation NMR (HETCOR), and 2D HETCOR with 1H spin diffusion. With spectral editing techniques, we identified methyl CCH 3, rigid and mobile methylene CCH2C, methine CCH, quaternary Cq, aromatic CH, aromatic carbons bonded to alkyls, small-sized condensed aromatic moieties, and aromatic C-O groups. With direct polarization combined with spectral-editing techniques, we quantified 11 different types of functional groups. 1H-13C 2D HETCOR NMR experiments indicated spatial proximity of aromatic and alkyl moieties in cross-linked structures. The proton spin diffusion experiments indicated that the magnetization was not equilibrated at a 1H spin diffusion time of 5 ms. Therefore, the heterogeneity in spatial distribution of different functional groups should be above 2 nm. Recoupled C-H long-range dipolar dephasing showed that the fraction of large charcoal-like clusters of polycondensed aromatic rings was relatively small. The exposure of this coal to atmospheric oxygen at room temperature for 6 months did not result in obvious chemical structural changes of the coal, whereas heating at 75 ??C in air for 10 days led to oxidation of coal and generated some COO groups. Evacuation removed most volatiles and caused a significant reduction in aliphatic signals in its DP

  4. Advanced 2-micron Solid-state Laser for Wind and CO2 Lidar Applications

    NASA Technical Reports Server (NTRS)

    Yu, Jirong; Trieu, Bo C.; Petros, Mulugeta; Bai, Yingxin; Petzar, Paul J.; Koch, Grady J.; Singh, Upendra N.; Kavaya, Michael J.

    2006-01-01

    Significant advancements in the 2-micron laser development have been made recently. Solid-state 2-micron laser is a key subsystem for a coherent Doppler lidar that measures the horizontal and vertical wind velocities with high precision and resolution. The same laser, after a few modifications, can also be used in a Differential Absorption Lidar (DIAL) system for measuring atmospheric CO2 concentration profiles. The world record 2-micron laser energy is demonstrated with an oscillator and two amplifiers system. It generates more than one joule per pulse energy with excellent beam quality. Based on the successful demonstration of a fully conductive cooled oscillator by using heat pipe technology, an improved fully conductively cooled 2-micron amplifier was designed, manufactured and integrated. It virtually eliminates the running coolant to increase the overall system efficiency and reliability. In addition to technology development and demonstration, a compact and engineering hardened 2-micron laser is under development. It is capable of producing 250 mJ at 10 Hz by an oscillator and one amplifier. This compact laser is expected to be integrated to a lidar system and take field measurements. The recent achievements push forward the readiness of such a laser system for space lidar applications. This paper will review the developments of the state-of-the-art solid-state 2-micron laser.

  5. Advances in solid state switchgear technology for large space power systems

    NASA Technical Reports Server (NTRS)

    Sundberg, G. R.

    1984-01-01

    High voltage solid state remote power controllers (RPC's) and the required semiconductor power switches to provide baseline technology for large, high power distribution systems in the space station, all electric airplane and other advanced aerospace applications were developed. The RPC's were developed for dc voltages from 28 to 1200 V and ac voltages of 115, 230, and 440 V at frequencies of 400 Hz to 20 kHz. The benefits and operation of solid state RPC's and highlights of several developments to bring the RPC to technology readiness for future aerospace needs are examined. The 28 V dc Space Shuttle units, three RPC types at 120 V dc, two at 270/300 V dc, two at 230 V ac and several high power RPC models at voltages up to 1200 V dc with current ratings up to 100 A are reviewed. New technology programs to develop a new family of (DI)2 semiconductor switches and 20 kHz, 440 V ac RPC's are described.

  6. Solid state fermentation for production of microbial cellulases: Recent advances and improvement strategies.

    PubMed

    Behera, Sudhanshu S; Ray, Ramesh C

    2016-05-01

    Lignocellulose is the most plentiful non-food biomass and one of the most inexhaustible renewable resources on the planet, which is an alternative sustainable energy source for the production of second generation biofuels. Lignocelluloses are composed of cellulose, hemicellulose and lignin, in which the sugar polymers account for a large portion of the biomass. Cellulases belong to the glycoside hydrolase family and catalyze the hydrolysis of glyosidic linkages depolymerizing cellulose to fermentable sugars. They are multi-enzymatic complex proteins and require the synergistic action of three key enzymes: endoglucanase (E.C. 3.2.1.4), exoglucanase (E.C. 3.2.1.176) (E.C. 3.2.1.91) and β-glucosidase (E.C. 3.2.1.21) for the depolymerization of cellulose to glucose. Solid state fermentation, which holds growth of microorganisms on moist solid substrates in the absence of free flowing water, has gained considerable attention of late due its several advantages over submerged fermentation. The review summarizes the critical analysis of recent literature covering production of cellulase in solid state fermentation using advance technologies such as consolidated bioprocessing, metabolic engineering and strain improvement, and circumscribes the strategies to improve the enzyme yield. PMID:26601764

  7. Determination of methyl 13C-15N dipolar couplings in peptides and proteins by three-dimensional and four-dimensional magic-angle spinning solid-state NMR spectroscopy

    NASA Astrophysics Data System (ADS)

    Helmus, Jonathan J.; Nadaud, Philippe S.; Höfer, Nicole; Jaroniec, Christopher P.

    2008-02-01

    We describe three- and four-dimensional semiconstant-time transferred echo double resonance (SCT-TEDOR) magic-angle spinning solid-state nuclear magnetic resonance (NMR) experiments for the simultaneous measurement of multiple long-range N15-Cmethyl13 dipolar couplings in uniformly C13, N15-enriched peptides and proteins with high resolution and sensitivity. The methods take advantage of C13 spin topologies characteristic of the side-chain methyl groups in amino acids alanine, isoleucine, leucine, methionine, threonine, and valine to encode up to three distinct frequencies (N15-Cmethyl13 dipolar coupling, N15 chemical shift, and Cmethyl13 chemical shift) within a single SCT evolution period of initial duration ˜1/JCC1 (where JCC1≈35Hz, is the one-bond Cmethyl13-C13 J-coupling) while concurrently suppressing the modulation of NMR coherences due to C13-C13 and N15-C13 J-couplings and transverse relaxation. The SCT-TEDOR schemes offer several important advantages over previous methods of this type. First, significant (approximately twofold to threefold) gains in experimental sensitivity can be realized for weak N15-Cmethyl13 dipolar couplings (corresponding to structurally interesting, ˜3.5Å or longer, distances) and typical Cmethyl13 transverse relaxation rates. Second, the entire SCT evolution period can be used for Cmethyl13 and/or N15 frequency encoding, leading to increased spectral resolution with minimal additional coherence decay. Third, the experiments are inherently "methyl selective," which results in simplified NMR spectra and obviates the use of frequency-selective pulses or other spectral filtering techniques. Finally, the N15-C13 cross-peak buildup trajectories are purely dipolar in nature (i.e., not influenced by J-couplings or relaxation), which enables the straightforward extraction of N15-Cmethyl13 distances using an analytical model. The SCT-TEDOR experiments are demonstrated on a uniformly C13, N15-labeled peptide, N-acetyl-valine, and a 56

  8. Model-free estimation of the effective correlation time for C–H bond reorientation in amphiphilic bilayers: {sup 1}H–{sup 13}C solid-state NMR and MD simulations

    SciTech Connect

    Ferreira, Tiago Mendes; Ollila, O. H. Samuli; Pigliapochi, Roberta; Dabkowska, Aleksandra P.; Topgaard, Daniel

    2015-01-28

    Molecular dynamics (MD) simulations give atomically detailed information on structure and dynamics in amphiphilic bilayer systems on timescales up to about 1 μs. The reorientational dynamics of the C–H bonds is conventionally verified by measurements of {sup 13}C or {sup 2}H nuclear magnetic resonance (NMR) longitudinal relaxation rates R{sub 1}, which are more sensitive to motional processes with correlation times close to the inverse Larmor frequency, typically around 1-10 ns on standard NMR instrumentation, and are thus less sensitive to the 10-1000 ns timescale motion that can be observed in the MD simulations. We propose an experimental procedure for atomically resolved model-free estimation of the C–H bond effective reorientational correlation time τ{sub e}, which includes contributions from the entire range of all-atom MD timescales and that can be calculated directly from the MD trajectories. The approach is based on measurements of {sup 13}C R{sub 1} and R{sub 1ρ} relaxation rates, as well as {sup 1}H−{sup 13}C dipolar couplings, and is applicable to anisotropic liquid crystalline lipid or surfactant systems using a conventional solid-state NMR spectrometer and samples with natural isotopic composition. The procedure is demonstrated on a fully hydrated lamellar phase of 1-palmitoyl-2-oleoyl-phosphatidylcholine, yielding values of τ{sub e} from 0.1 ns for the methyl groups in the choline moiety and at the end of the acyl chains to 3 ns for the g{sub 1} methylene group of the glycerol backbone. MD simulations performed with a widely used united-atom force-field reproduce the τ{sub e}-profile of the major part of the acyl chains but underestimate the dynamics of the glycerol backbone and adjacent molecular segments. The measurement of experimental τ{sub e}-profiles can be used to study subtle effects on C–H bond reorientational motions in anisotropic liquid crystals, as well as to validate the C–H bond reorientation dynamics predicted in MD

  9. Formation of carboxylic acids from alcohols and olefins in zeolite H-ZSM-5 under mild conditions via trapping of alkyl carbenium ions with carbon monoxide: An in situ {sup 13}C solid state NMR study

    SciTech Connect

    Stepanov, A.G.; Luzgin, M.V.; Romannikov, V.N.; Sidelnikov, V.N.; Zamaraev K.I.

    1996-12-01

    Using in situ {sup 13}C solid state MAS NMR (for some reagents in combination with ex situ GC-MS), it is shown that butyl alcohols and olefins (ethene, isobutene, octene-1) undergo carbonylation to form carboxylic acids (the Koch reaction) with high conversion on zeolite H-ZSM-5 at 296-373 K. The reactions proceed without application of pressurized conditions, just upon coadsorption of CO and alcohols or CO, H{sub 2}O, and olefins on zeolite. The observed Koch reaction under mild conditions provides strong evidence for the formation of alkyl carbenium ions from alcohols and olefins on the zeolites as crucial reaction intermediates. Of the family of carbenium ions, CO reacts selectively with tertiary cations to produce tertiary carboxylic acids, unless the carbonylated molecule is too large for more bulky tertiary moieties to be accommodated and carbonylated in the narrow pores of H-ZSM05. Thus, t-BuOH, i-BuOH, and isobutene produce trimethylacetic acid with high selectivity and conversion, while ethene transforms selectively into 2-methyl-2-ethyl butyric acid. Reaction of octene-1 molecules with CO and H{sub 2}O results in acids of the C{sub 8}H{sub 17}COOH and C{sub 16}H{sub 33}COOH families with predominantly linear hydrocarbon chains. The data obtained may open up new possibilities in using solid acids in organic synthesis as carbonylation catalysts under mild conditions i.e., low temperature and normal atmospheric pressure. 55 refs., 8 figs.

  10. Advanced solid-state array spectroradiometer data collection during HAPEX-2 Sahel

    NASA Technical Reports Server (NTRS)

    Walthall, Charles L.; Halthore, Rangshai N.; Russell, Carol; Dabney, Phillip W.; Irons, James R.; Kovalick, Bill; Graham, David; Bur, Mike

    1993-01-01

    Data collection using the Advanced Solid-state Array Spectroradiometer (ASAS) during the Hydrologic Atmospheric Pilot Experiment in the Sahel (HAPEX-II Sahel) field campaign in the Republic of Niger, West Central Africa from 22 Aug. to 19 Sep. 1992 is documented. Details on the ASAS system such as the hardware, data collection methods, information on system calibration, and data processing procedures are included. The ASAS configuration deployed for HAPEX-II Sahel contains several new components, including a new sensor array and pointing system. Because of this, new calibration procedures are being developed at the same time that the first ASAS images from HAPEX-II Sahel are being processed. These new calibration procedures will be documented in a future publication.

  11. Solid state 13C-NMR, infrared, X-ray powder diffraction and differential thermal studies of the homologous series of some mono-valent metal (Li, Na, K, Ag) n-alkanoates: A comparative study

    NASA Astrophysics Data System (ADS)

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

    2015-06-01

    A comparative study of the molecular packing, lattice structures and phase behaviors of the homologous series of some mono-valent metal carboxylates (Li, Na, K and Ag) is carried out via solid state FT-infrared and 13C-NMR spectroscopes, X-rays powder diffraction, density measurements, differential scanning calorimetry, polarizing light microscopy and variable temperature infrared spectroscopy. It is proposed that, for lithium, sodium and potassium carboxylates, metal-carboxyl coordination is via asymmetric chelating bidentate bonding with extensive intermolecular interactions to form tetrahedral metal centers, irrespective of chain length. However, for silver n-alkanoates, carboxyl moieties are bound to silver ions via syn-syn type bridging bidentate coordination to form dimeric units held together by extensive head group inter-molecular interactions. Furthermore, the fully extended hydrocarbon chains which are crystallized in the all-trans conformation are tilted at ca. 30°, 27°, 15° and 31° with respect to a normal to the metal plane, for lithium, sodium, silver and potassium carboxylates, respectively. All compounds are packed as lamellar bilayer structures, however, lithium compounds are crystallized in a triclinic crystal system whilst silver, sodium and potassium n-alkanoates are all monoclinic with possible P1 bravais lattice. Odd-even alternation observed in various physical features is associated with different inter-planar spacing between closely packed layers in the bilayer which are not in the same plane; a phenomenon controlled by lattice packing symmetry requirements. All compounds, except silver carboxylates, show partially reversibly first order pre-melting transitions; the number of which increases with increasing chain length. These transitions are associated, for the most part, with lamellar collapse followed by increased gauche-trans isomerism in the methylene group assembly, irrespective of chain length. It is proposed that the absence of

  12. Forest and grassland ecosystem studies using the advanced solid-state array spectroradiometer

    NASA Technical Reports Server (NTRS)

    Irons, James R.; Ranson, K. Jon; Williams, Darrel L.; Irish, Richard R.

    1989-01-01

    The advanced solid-state array spectroradiometer (ASAS) is an airborne, off-nadir pointing imaging spectroradiometer used to acquire bidirectional radiance data for terrestrial targets. As its platform aircraft flies over a target the sensor can image the target through a sequence of at least seven fore-to-aft view directions ranging up to 45 deg on either side of nadir. ASAS acquires data for 29 spectral bands in the visible and near-infrared portions of the spectrum with a resolution of 15 nm. ASAS data were recently acquired for a prairie ecosystem and a northern forest ecosystem. The data demonstrate the combined effects of reflectance anisotropy and increased atmospheric path length on off-nadir observations. One result of these effects is a variation in vegetation indices as a function of view direction. Normalized-difference-vegetation-indices for prairie grass, coniferous, and deciduous canopies varied up to 14 percent, 23 percent, and 6 percent, respectively, relative to nadir as a function of view zenith angle along the solar principal plane.

  13. Recent advances and challenges for diode-pumped solid-state lasers as an inertial fusion energy driver candidate

    SciTech Connect

    Payne, S.A.; Beach, R.J.; Bibeau, C.

    1997-12-23

    We discuss how solid-state laser technology can serve in the interests of fusion energy beyond the goals of the National Ignition Facility (NIF), which is now being constructed to ignite a deuterium-tritium target to fusion conditions in the laboratory for the first time. We think that advanced solid-state laser technology can offer the repetition-rate and efficiency needed to drive a fusion power plant, in contrast to the single-shot character of NIF. As discuss below, we propose that a gas-cooled, diode-pumped Yb:S-FAP laser can provide a new paradigm for fusion laser technology leading into the next century.

  14. Advanced fusion welding processes, solid state joining and a successful marriage. [production of aerospace structures

    NASA Technical Reports Server (NTRS)

    Miller, F. R.

    1972-01-01

    Joining processes for aerospace systems combine fusion welding and solid state joining during production of metal structures. Detailed characteristics of electron beam welding, plasma arc welding, diffusion welding, inertia welding and weldbond processes are discussed.

  15. Ground-fire effects on the composition of dissolved and total organic matter in forest floor and soil solutions from Scots pine forests in Germany: new insights from solid state 13C NMR analysis

    NASA Astrophysics Data System (ADS)

    Näthe, Kerstin; Michalzik, Beate; Levia, Delphis; Steffens, Markus

    2016-04-01

    Fires represent an ecosystem disturbance and are recognized to seriously pertubate the nutrient budgets of forested ecosystems. While the effects of fires on chemical, biological, and physical soil properties have been intensively studied, especially in Mediterranean areas and North America, few investigations examined the effects of fire-induced alterations in the water-bound fluxes and the chemical composition of dissolved and particulate organic carbon and nitrogen (DOC, POC, DN, PN). The exclusion of the particulate organic matter fraction (0.45 μm < POM < 500 μm) potentially results in misleading inferences and budgeting gaps when studying the effects of fires on nutrient and energy fluxes. To our best knowledge, this is the first known study to present fire-induced changes on the composition of dissolved and total organic matter (DOM, TOM) in forest floor (FF) and soil solutions (A, B horizon) from Scots pine forests in Germany. In relation to control sites, we test the effects of low-severity fires on: (1) the composition of DOM and TOM in forest floor and soil solutions; and (2) the translocated amount of particulate in relation to DOC and DN into the subsoil. The project aims to uncover the mechanisms of water-bound organic matter transport along an ecosystem profile and its compositional changes following a fire disturbance. Forest floor and soil solutions were fortnightly sampled from March to December 2014 on fire-manipulated and control plots in a Scots pine forest in Central Germany. Shortly after the experimental duff fire in April 2014 pooled solutions samples were taken for solid-state 13C NMR spectroscopy to characterize DOM (filtered solution < 0.8μm pore size) and TOM in unfiltered solutions. Independent from fire manipulation, the composition of TOM was generally less aromatic (aromaticity index [%] according to Hatcher et al., 1981) with values between 18 (FF) - 25% (B horizon) than the DOM fraction with 23 (FF) - 27% (B horizon). For DOM

  16. Solid-state distortions of nominally square-planar palladium and platinum (R sub 3 P) sub 2 MX sub 2 complexes as determined by a combination of sup 13 C( sup 1 H) and sup 31 P( sup 31 H) NMR spectroscopy

    SciTech Connect

    Rahn, J.A.; Nelson, J.H. ); O'Donnell, D.J.; Pamer, A.R. )

    1989-06-28

    Phosphorus-31 and carbon-13 NMR spectra have been obtained for a series of 20 (R{sub 3}P){sub 2}MX{sub 2} complexes (R{sub 3}P = MePh{sub 2}P and Me{sub 2}PhP; M = Pd, Pt; X = Cl, Br, I, CN, N{sub 3}) in the solid state by cross-polarization and magic-angle-spinning (CP/MAS) techniques. Comparison of these data with spectral data obtained at 300 K in CDCl{sub 3} solutions was made in order to investigate the influence of local symmetry on {sup 31}P and {sup 13}C chemical shifts in the solid state. It was found that most of these compounds, which have regular square-planar geometries in solution, are distorted in the solid state. The solid-state distortions are evidenced by additional {sup 31}P and {sup 13}C resonances in the CP/MAS spectra as compared to the solution spectra. The nature and degree of these distortions are discussed. 25 refs., 2 figs., 6 tabs.

  17. Recent advances in mapping environmental microbial metabolisms through 13C isotopic fingerprints.

    PubMed

    Tang, Joseph Kuo-Hsiang; You, Le; Blankenship, Robert E; Tang, Yinjie J

    2012-11-01

    After feeding microbes with a defined (13)C substrate, unique isotopic patterns (isotopic fingerprints) can be formed in their metabolic products. Such labelling information not only can provide novel insights into functional pathways but also can determine absolute carbon fluxes through the metabolic network via metabolic modelling approaches. This technique has been used for finding pathways that may have been mis-annotated in the past, elucidating new enzyme functions, and investigating cell metabolisms in microbial communities. In this review paper, we summarize the applications of (13)C approaches to analyse novel cell metabolisms for the past 3 years. The isotopic fingerprints (defined as unique isotopomers useful for pathway identifications) have revealed the operations of the Entner-Doudoroff pathway, the reverse tricarboxylic acid cycle, new enzymes for biosynthesis of central metabolites, diverse respiration routes in phototrophic metabolism, co-metabolism of carbon nutrients and novel CO(2) fixation pathways. This review also discusses new isotopic methods to map carbon fluxes in global metabolisms, as well as potential factors influencing the metabolic flux quantification (e.g. metabolite channelling, the isotopic purity of (13)C substrates and the isotopic effect). Although (13)C labelling is not applicable to all biological systems (e.g. microbial communities), recent studies have shown that this method has a significant value in functional characterization of poorly understood micro-organisms, including species relevant for biotechnology and human health. PMID:22896564

  18. Recent advances in mapping environmental microbial metabolisms through 13C isotopic fingerprints

    PubMed Central

    Tang, Joseph Kuo-Hsiang; You, Le; Blankenship, Robert E.; Tang, Yinjie J.

    2012-01-01

    After feeding microbes with a defined 13C substrate, unique isotopic patterns (isotopic fingerprints) can be formed in their metabolic products. Such labelling information not only can provide novel insights into functional pathways but also can determine absolute carbon fluxes through the metabolic network via metabolic modelling approaches. This technique has been used for finding pathways that may have been mis-annotated in the past, elucidating new enzyme functions, and investigating cell metabolisms in microbial communities. In this review paper, we summarize the applications of 13C approaches to analyse novel cell metabolisms for the past 3 years. The isotopic fingerprints (defined as unique isotopomers useful for pathway identifications) have revealed the operations of the Entner–Doudoroff pathway, the reverse tricarboxylic acid cycle, new enzymes for biosynthesis of central metabolites, diverse respiration routes in phototrophic metabolism, co-metabolism of carbon nutrients and novel CO2 fixation pathways. This review also discusses new isotopic methods to map carbon fluxes in global metabolisms, as well as potential factors influencing the metabolic flux quantification (e.g. metabolite channelling, the isotopic purity of 13C substrates and the isotopic effect). Although 13C labelling is not applicable to all biological systems (e.g. microbial communities), recent studies have shown that this method has a significant value in functional characterization of poorly understood micro-organisms, including species relevant for biotechnology and human health. PMID:22896564

  19. Characterization of oil shale, isolated kerogen, and post-pyrolysis residues using advanced 13 solid-state nuclear magnetic resonance spectroscopy

    USGS Publications Warehouse

    Cao, Xiaoyan; Birdwell, Justin E.; Chappell, Mark A.; Li, Yuan; Pignatello, Joseph J.; Mao, Jingdong

    2013-01-01

    Characterization of oil shale kerogen and organic residues remaining in postpyrolysis spent shale is critical to the understanding of the oil generation process and approaches to dealing with issues related to spent shale. The chemical structure of organic matter in raw oil shale and spent shale samples was examined in this study using advanced solid-state 13C nuclear magnetic resonance (NMR) spectroscopy. Oil shale was collected from Mahogany zone outcrops in the Piceance Basin. Five samples were analyzed: (1) raw oil shale, (2) isolated kerogen, (3) oil shale extracted with chloroform, (4) oil shale retorted in an open system at 500°C to mimic surface retorting, and (5) oil shale retorted in a closed system at 360°C to simulate in-situ retorting. The NMR methods applied included quantitative direct polarization with magic-angle spinning at 13 kHz, cross polarization with total sideband suppression, dipolar dephasing, CHn selection, 13C chemical shift anisotropy filtering, and 1H-13C long-range recoupled dipolar dephasing. The NMR results showed that, relative to the raw oil shale, (1) bitumen extraction and kerogen isolation by demineralization removed some oxygen-containing and alkyl moieties; (2) unpyrolyzed samples had low aromatic condensation; (3) oil shale pyrolysis removed aliphatic moieties, leaving behind residues enriched in aromatic carbon; and (4) oil shale retorted in an open system at 500°C contained larger aromatic clusters and more protonated aromatic moieties than oil shale retorted in a closed system at 360°C, which contained more total aromatic carbon with a wide range of cluster sizes.

  20. Characterization of animal manure using advanced solid-state C-13 NMR spectroscopy

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Knowledge of chemical structure of animal manure is necessary for its effective utilization. However, characterization of animal manure is challenging since it is a complex mixture and partially soluble. Solid-state C-13 NMR (nuclear magnetic resonance) spectroscopy is regarded as the best tool to i...

  1. Advances in solid state laser technology for space and medical applications

    NASA Technical Reports Server (NTRS)

    Byvik, C. E.; Buoncristiani, A. M.

    1988-01-01

    Recent developments in laser technology and their potential for medical applications are discussed. Gas discharge lasers, dye lasers, excimer lasers, Nd:YAG lasers, HF and DF lasers, and other commonly used lasers are briefly addressed. Emerging laser technology is examined, including diode-pumped lasers and other solid state lasers.

  2. Comparison of structure in solid state of new 1,5- bis(4-cyano-2,6-dimethoxyphenoxy)alkanes by means of 13C CP/MAS NMR and X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Żabiński, Jerzy; Wolska, Irena; Maciejewska, Dorota

    2007-05-01

    The synthesis and structural studies in solid state of new 1,5- bis(4-cyano-2,6-dimethoxyphenoxy)-3-oxapentane 1 and 1,5- bis(4-cyano-2,6-methoxyphenoxy)pentane 2 are presented. The observed complicated network of intermolecular interaction with participation of nitrile groups could play a role in their interaction with the biological target. In vitro screen against 60 human tumor cell lines revealed that compound 1 has promising growth inhibitory power GI 50 against SR (leukemia) and HOP-92 (non-small lung cancer) equal to 4.33 ×10 -6 and 1.03 ×10 -5 M, respectively.

  3. Advances in Solid State Joining of Haynes 230 High Temperature Alloy

    NASA Technical Reports Server (NTRS)

    Ding, Jeff; Schneider, Judy; Walker, Bryant

    2010-01-01

    The J-2X engine is being designed for NASA s new class of crew and launch vehicles, the Ares I and Ares V. The J-2X is a LOX/Hydrogen upper stage engine with 294,000 lbs of thrust and a minimum Isp of 448 seconds. As part of the design criteria to meet the performance requirements a large film-cooled nozzle extension is being designed to further expand the hot gases and increases the specific impulse. The nozzle extension is designed using Haynes 230, a nickel-chromium-tungsten-molybdenum superalloy. The alloy was selected for its high strength at elevated temperatures and resistance to hydrogen embrittlement. The nozzle extension is manufactured from Haynes 230 plate spun-forged to form the contour and chemically-milled pockets for weight reduction. Currently fusion welding is being evaluated for joining the panels which are then mechanically etched and thinned to required dimensions for the nozzle extension blank. This blank is then spun formed into the parabolic geometry required for the nozzle. After forming the nozzle extension, weight reduction pockets are chemically milled into the nozzle. Fusion welding of Haynes results in columnar grains which are prone to hot cracking during forming processes. This restricts the ability to use spin forging to produce the nozzle contour. Solid state joining processes are being pursued as an alternative process to produce a structure more amenable to spin forming. Solid state processes have been shown to produce a refined grain structure within the joint regions as illustrated in Figure 1. Solid state joining processes include friction stir welding (FSW) and a patented modification termed thermal stir welding (TSW). The configuration of TSWing utilizes an induction coil to preheat the material minimizing the burden on the weld tool extending its life. This provides the ability to precisely select and control the temperature. The work presented in this presentation investigates the feasibility of joining the Haynes 230

  4. Investigation of a solid-state detector for advanced computed tomography.

    PubMed

    Hsieh, J; Gurmen, O E; King, K F

    2000-09-01

    Utilization of solid-state detectors for computed tomography (CT) has been the focus of many studies. Previous phantom and clinical experiments have shown that one of the important performance parameters for the solid-state detector is the primary speed and afterglow. In this paper, we present a detailed investigation on the signal decay characteristics of the HiLight (GE Medical Systems, Milwaukee, WI) scintillating detector. The detector primary speed and afterglow are modeled by a multiexponential function and fully characterized by a set of time constants and relative strengths. The sensitivity of these parameters to X-ray photon energy, detector aging, and radiation exposure is then established and analyzed. No statistically significant variation is observed in these parameters due to changes in the above external variables. The impact of various decay time constants on CT image quality, such as spatial resolution, noise, and artifacts, is subsequently illustrated with computer simulations and phantom experiments. Finally, an algorithmic correction scheme is derived to compensate for detector afterglow. The correction scheme employs a recursive filter to remove adverse effects of the detector decay on image quality. Experimental results have shown that the correction scheme successfully restores system spatial resolution, produces a more homogeneous noise pattern, and eliminates ring-band image artifacts due to detector afterglow. The effectiveness and robustness of the correction scheme are demonstrated by extensive phantom and clinical experiments. PMID:11127606

  5. Probing Quadrupolar Nuclei by Solid-State NMR Spectroscopy: Recent Advances

    SciTech Connect

    Fernandez, Christian; Pruski, Marek

    2011-06-08

    Solid-state nuclear magnetic resonance (NMR) of quadrupolar nuclei has recently undergone remarkable development of capabilities for obtaining structural and dynamic information at the molecular level. This review summarizes the key achievements attained during the last couple of decades in solid-state NMR of both integer spin and half-integer spin quadrupolar nuclei. We provide a concise description of the first- and second-order quadrupolar interactions, and their effect on the static and magic angle spinning (MAS) spectra. Methods are explained for efficient excitation of single- and multiple-quantum coherences, and acquisition of spectra under low- and high-resolution conditions. Most of all, we present a coherent, comparative description of the high-resolution methods for half-integer quadrupolar nuclei, including double rotation (DOR), dynamic angle spinning (DAS), multiple-quantum magic angle spinning (MQMAS), and satellite transition magic angle spinning (STMAS). Also highlighted are methods for processing and analysis of the spectra. Finally, we review methods for probing the heteronuclear and homonuclear correlations between the quadrupolar nuclei and their quadrupolar or spin-1/2 neighbors.

  6. Advanced concepts for high power RF generation using solid state materials

    SciTech Connect

    Fazio, M.V.; Erickson, G.A.

    1999-05-01

    Traditionally, high power radio frequency and microwave energy have been generated using electron beam driven hard-vacuum tubes such as klystrons and magnetrons. High-power solid-state sources of RF have not been available. It is well known that a non-linear, dispersive system can convert a pulse into an array of solitons. Although this effect has been exploited in the optical field, using non-linear optical materials, little work has been done in the field of high voltage electronics. It is the goal of this work, which is just beginning, to develop sources of RF in the few hundreds of megahertz to gigahertz range with power levels in the hundreds of megawatts to the gigawatt level. To generate solitons a high voltage pulse is fed onto a transmission line that is periodically loaded with a non-linear ceramic dielectric in the paraelectric phase. The combination of the non-linearity and dispersion causes the pulse to break up into an array of solitons. A soliton-based system has several components: the solid state, high voltage, high current switch to provide the initial high voltage pulse; a shock line to decrease the rise time of the initial pulse to less than a few nanoseconds; and the soliton generating transmission line where the high power RF is generated when driven by the fast rising pulse from the shock line. The approach and progress to date will be described. {copyright} {ital 1999 American Institute of Physics.}

  7. Solid-state resistance upset welding: A process with unique advantages for advanced materials

    SciTech Connect

    Kanne, W.R. Jr.

    1993-12-31

    Solid-state resistance upset welding is suitable for joining many alloys that are difficult to weld using fusion processes. Since no melting takes place, the weld metal retains many of the characteristics of the base metal. Resulting welds have a hot worked structure, and thereby have higher strength than fusion welds in the same mate. Since the material being joined is not melted, compositional gradients are not introduced, second phase materials are minimally disrupted, and minor alloying elements, do not affect weldability. Solid-state upset welding has been adapted for fabrication of structures considered very large compared to typical resistance welding applications. The process has been used for closure of capsules, small vessels, and large containers. Welding emphasis has been on 304L stainless steel, the material for current applications. Other materials have, however, received enough attention to have demonstrated capability for joining alloys that are not readily weldable using fusion welding methods. A variety of other stainless steels (including A-286), superalloys (including TD nickel), refractory metals (including tungsten), and aluminum alloys (including 2024) have been successfully upset welded.

  8. Study of wheat high molecular weight 1Dx5 subunit by (13)C and (1)H solid-state NMR. II. Roles of nonrepetitive terminal domains and length of repetitive domain.

    PubMed

    Alberti, Enrica; Gilbert, Simon M; Tatham, Arthur S; Shewry, Peter R; Naito, Akira; Okuda, Kanna; Saitô, Hazime; Gil, Ana M

    2002-10-15

    This work follows a previous article that addressed the role of disulfide bonds in the behavior of the 1Dx5 subunit upon hydration. Here the roles of nonrepetitive terminal domains present and the length of the central repetitive domain in the hydration of 1Dx5 are investigated. This was achieved by comparing the hydration behavior of suitable model samples determined by (13)C- and (1)H-NMR: an alkylated 1Dx5 subunit (alk1Dx5), a recombinant 58-kDa peptide corresponding to the central repetitive domain of 1Dx5 (i.e., lacking the terminal domains), and two synthetic peptides (with 6 and 21 amino acid residues) based on the consensus repeat motifs of the central domain. The (13)C cross-polarization and magic angle spinning (MAS) experiments recorded as a function of hydration gave information about the protein or peptide fractions resisting plasticization. Conversely, (13)C single pulse excitation and (1)H-MAS gave information on the more plasticized segments. The results are consistent with the previous proposal of a hydrated network held by hydrogen-bonded glutamines and possibly hydrophobic interactions. The nonrepetitive terminal domains were found to induce water insolubility and a generally higher network hindrance. Shorter chain lengths were shown to increase plasticization and water solubility. However, at low water contents, the 21-mer peptide was characterized by higher hindrance in the megahertz and kilohertz frequency ranges compared to the longer peptide; and a tendency for a few hydrogen-bonded glutamines and hydrophobic residues to remain relatively hindered was still observed, as for the protein and large peptide. It is suggested that this ability is strongly dependent on the peptide primary structure. PMID:12209466

  9. Advances in room-temperature solid-state gamma-ray spectrometry

    SciTech Connect

    Iwanczyk, J.S.

    1983-01-01

    This article presents a review and analysis of different concepts of gamma-ray spectrometry using room-temperature solid-state detectors. The classical approach involving the use of a charge-sensitive preamplifier and attempting to collect all the ionization charge produced by the gamma ray is analyzed and discussed in terms of the charge transport parameters of the most promising compound semiconductor materials. It is concluded that compound semiconductor detector materials having a large disparity between the ..mu.. tau products for electrons and holes (such as HgI/sub 2/ and CdTe) will have rather poor energy resolution if the classical method of spectrometry requiring full charge collection is employed. 30 references.

  10. Chemical structures of manure from conventional and phytase transgenic pigs investigated by advanced solid-state NMR spectroscopy.

    PubMed

    Mao, Jingdong; Ajakaiye, Ayodele; Lan, Yeqing; Olk, Dan C; Ceballos, Michael; Zhang, Tiequan; Fan, Ming Z; Forsberg, Cecil W

    2008-03-26

    Nonpoint phosphorus (P) pollution from animal manure is becoming a serious global problem. The current solution for the swine industry includes the enzyme phytase as a component in oil meal and cereal grain-based swine diets. A long-term approach is the production of transgenic phytase pigs that express phytase in the salivary glands and secrete it in the saliva. This study provides a detailed comparison of chemical structures of manure from conventional pigs and transgenic pigs that express phytase under growing and finishing phases using new solid-state NMR techniques. Spectral editing techniques and quantitative NMR techniques were used to identify and quantify specific functional groups. Two-dimensional (1)H- (13)C heteronuclear correlation NMR was used to detect their connectivity. Manure from conventional and transgenic pigs had similar peptide, carbohydrate, and fatty acid components, while those from transgenic pigs contained more carbohydrates and fewer nonpolar alkyls. There was no consistent effect from diets with or without supplemental phosphate or growth stages. PMID:17973446

  11. Optimization of amino acid type-specific 13C and 15N labeling for the backbone assignment of membrane proteins by solution- and solid-state NMR with the UPLABEL algorithm.

    PubMed

    Hefke, Frederik; Bagaria, Anurag; Reckel, Sina; Ullrich, Sandra Johanna; Dötsch, Volker; Glaubitz, Clemens; Güntert, Peter

    2011-02-01

    We present a computational method for finding optimal labeling patterns for the backbone assignment of membrane proteins and other large proteins that cannot be assigned by conventional strategies. Following the approach of Kainosho and Tsuji (Biochemistry 21:6273-6279 (1982)), types of amino acids are labeled with (13)C or/and (15)N such that cross peaks between (13)CO(i - 1) and (15)NH(i) result only for pairs of sequentially adjacent amino acids of which the first is labeled with (13)C and the second with (15)N. In this way, unambiguous sequence-specific assignments can be obtained for unique pairs of amino acids that occur exactly once in the sequence of the protein. To be practical, it is crucial to limit the number of differently labeled protein samples that have to be prepared while obtaining an optimal extent of labeled unique amino acid pairs. Our computer algorithm UPLABEL for optimal unique pair labeling, implemented in the program CYANA and in a standalone program, and also available through a web portal, uses combinatorial optimization to find for a given amino acid sequence labeling patterns that maximize the number of unique pair assignments with a minimal number of differently labeled protein samples. Various auxiliary conditions, including labeled amino acid availability and price, previously known partial assignments, and sequence regions of particular interest can be taken into account when determining optimal amino acid type-specific labeling patterns. The method is illustrated for the assignment of the human G-protein coupled receptor bradykinin B2 (B(2)R) and applied as a starting point for the backbone assignment of the membrane protein proteorhodopsin. PMID:21170670

  12. Advanced technologies for high-efficiency GaInN LEDs for solid state lighting

    NASA Astrophysics Data System (ADS)

    Harle, Volker; Hahn, Berthold; Baur, Johannes; Fehrer, Michael; Weimar, Andreas; Kaiser, Stephan; Eisert, Dominik; Eberhard, Franz; Plossl, Andreas; Bader, Stefan

    2004-01-01

    Solid state lighting has seen a rapid development over the last decade. They compete and even outperform light sources like incandescent bulbs and halogen lamps. LEDs are used in applications where brightness, power consumption, reliability and costs are key parameters as automotive, mobile and display applications. In the future LEDs will also enter the market of general lighting. For all of these new applications highly efficient, scalable and cost efficient technologies are required. These targets can be matched by SiC based flip chip LEDs which enable the design of high current chips with efficiencies of up to 28 lm/W in white solderable packages. An alternative approach is the implementation of thinfilm technology for GaInN. The LED is fabricated by transferring the epilayers with laser lift off from sapphire to a GaAs host substrate. In combination with efficient surface roughening and highly reflective p-mirror metalization an extraction efficiency of 70% and wall plug efficiency of 24% at 460 nm have been shown. The chips showed 16 mW @ 20 mA with a Voltage of 3.2 V. The technology is scalable from small size LEDs to high current Chips and is being transferred to mass production.

  13. Advances in CMOS Solid-state Photomultipliers for Scintillation Detector Applications

    PubMed Central

    Christian, James F.; Stapels, Christopher J.; Johnson, Erik B.; McClish, Mickel; Dokhale, Purushotthom; Shah, Kanai S.; Mukhopadhyay, Sharmistha; Chapman, Eric; Augustine, Frank L.

    2014-01-01

    Solid-state photomultipliers (SSPMs) are a compact, lightweight, potentially low-cost alternative to a photomultiplier tube for a variety of scintillation detector applications, including digital-dosimeter and medical-imaging applications. Manufacturing SSPMs with a commercial CMOS process provides the ability for rapid prototyping, and facilitates production to reduce the cost. RMD designs CMOS SSPM devices that are fabricated by commercial foundries. This work describes the characterization and performance of these devices for scintillation detector applications. This work also describes the terms contributing to device noise in terms of the excess noise of the SSPM, the binomial statistics governing the number of pixels triggered by a scintillation event, and the background, or thermal, count rate. The fluctuations associated with these terms limit the resolution of the signal pulse amplitude. We explore the use of pixel-level signal conditioning, and characterize the performance of a prototype SSPM device that preserves the digital nature of the signal. In addition, we explore designs of position-sensitive SSPM detectors for medical imaging applications, and characterize their performance. PMID:25540471

  14. Advanced Solid State Nanopores Architectures: From Early Cancer Detection to Nano-electrochemistry

    NASA Astrophysics Data System (ADS)

    Bashir, Rashid

    2013-03-01

    Solid-state nanopores (ssNPs) are potentially low-cost and highly scalable technologies for rapid and reliable se-quencing of the human diploid genome for under 1,000. The ssNPs detect ionic current changes while molecules translocate through the pore. Several key challenges must be overcome in order for ssNPs to become ubiquitous in the fields of medical diagnostics and personalized healthcare. One major challenge is to reduce the speed at which DNA translocates through the nanopore from microseconds to milliseconds per nucleotide, enabling reliable identification of single nucleotides. The other major challenge is to improve the sensitivity of the approach requiring new sensing modalities and novel device architectures. In this paper, we review our recent efforts to (i) develop ssNPs for early cancer detection, (ii) to embed graphene electrodes in dielectric nanolaminates to form 3 and 4 terminal nanopore devices, and (iii) we demonstrate a nanopore based structure consisting of stacked graphene and Al2O3 dielectric layers to study electrochemical activity at graphene edges. The electrochemical signal corresponding to the atomically thin graphene layer could also provide a pathway to DNA sequencing. Supported by National Institute of Health.

  15. Advances in the Dynallax solid-state dynamic parallax barrier autostereoscopic visualization display system.

    SciTech Connect

    Peterka, T.; Kooima, R. L.; Sandin, D. J.; Johnson, A.; Leigh, J.; DeFanti, T. A.; Mathematics and Computer Science; Univ. of Illinois at Chicago; Univ. of Calif. at San Diego

    2008-05-01

    A solid-state dynamic parallax barrier autostereoscopic display mitigates some of the restrictions present in static barrier systems such as fixed view-distance range, slow response to head movements, and fixed stereo operating mode. By dynamically varying barrier parameters in real time, viewers may move closer to the display and move faster laterally than with a static barrier system, and the display can switch between 3D and 2D modes by disabling the barrier on a per-pixel basis. Moreover, Dynallax can output four independent eye channels when two viewers are present, and both head-tracked viewers receive an independent pair of left-eye and right-eye perspective views based on their position in 3D space. The display device is constructed by using a dual-stacked LCD monitor where a dynamic barrier is rendered on the front display and a modulated virtual environment composed of two or four channels is rendered on the rear display. Dynallax was recently demonstrated in a small-scale head-tracked prototype system. This paper summarizes the concepts presented earlier, extends the discussion of various topics, and presents recent improvements to the system.

  16. Analysis of commercial proanthocyanidins. Part 4: solid state (13)C NMR as a tool for in situ analysis of proanthocyanidin tannins, in heartwood and bark of quebracho and acacia, and related species.

    PubMed

    Reid, David G; Bonnet, Susan L; Kemp, Gabre; van der Westhuizen, Jan H

    2013-10-01

    (13)C NMR is an effective method of characterizing proanthocyanidin (PAC) tannins in quebracho (Schinopsis lorentzii) heartwood and black wattle (Acacia mearnsii) bark, before and after commercial extraction. The B-rings of the constituent flavan-3-ols, catechols (quebracho) or pyrogallols (wattle), are recognized in unprocessed source materials by "marker" signals at ca. 118 or 105ppm, respectively. NMR allows the minimum extraction efficiency to be calculated; ca. 30%, and ca. 80%, for quebracho heartwood and black wattle bark, respectively. NMR can also identify PAC tannin (predominantly robinetinidin), and compare tannin content, in bark from other acacia species; tannin content decreases in the order A. mearnsii, Acacia pycnantha (87% of A. mearnsii), Acacia dealbata and Acacia decurrens (each 74%) and Acacia karroo (30%). Heartwood from an underexploited PAC tannin source, Searsia lancea, taxonomically close to quebracho, shows abundant profisetinidin and catechin PACs. NMR offers the advantage of being applicable to source materials in their native state, and has potential applications in optimizing extraction processes, identification of tannin sources, and characterization of tannin content in cultivar yield improvement programmes. PMID:23838626

  17. Development of Advanced LED Phosphors by Spray-based Processes for Solid State Lighting

    SciTech Connect

    Cabot Corporation

    2007-09-30

    The overarching goal of the project was to develop luminescent materials using aerosol processes for making improved LED devices for solid state lighting. In essence this means improving white light emitting phosphor based LEDs by improvement of the phosphor and phosphor layer. The structure of these types of light sources, displayed in Figure 1, comprises of a blue or UV LED under a phosphor layer that converts the blue or UV light to a broad visible (white) light. Traditionally, this is done with a blue emitting diode combined with a blue absorbing, broadly yellow emitting phosphor such as Y{sub 3}Al{sub 5}O{sub 12}:Ce (YAG). A similar result may be achieved by combining a UV emitting diode and at least three different UV absorbing phosphors: red, green, and blue emitting. These emitted colors mix to make white light. The efficiency of these LEDs is based on the combined efficiency of the LED, phosphor, and the interaction between the two. The Cabot SSL project attempted to improve the over all efficiency of the LED light source be improving the efficiency of the phosphor and the interaction between the LED light and the phosphor. Cabot's spray based process for producing phosphor powders is able to improve the brightness of the powder itself by increasing the activator (the species that emits the light) concentration without adverse quenching effects compared to conventional synthesis. This will allow less phosphor powder to be used, and will decrease the cost of the light source; thus lowering the barrier of entry to the lighting market. Cabot's process also allows for chemical flexibility of the phosphor particles, which may result in tunable emission spectra and so light sources with improved color rendering. Another benefit of Cabot's process is the resulting spherical morphology of the particles. Less light scattering results when spherical particles are used in the phosphor layer (Figure 1) compared to when conventional, irregular shaped phosphor particles

  18. Solid State Lighting

    SciTech Connect

    Hastbacka, Mildred; Dieckmann, John; Bouza, Antonio

    2013-03-30

    The article discusses solid state lighting technologies. This topic was covered in two previous ASHRAE Journal columns (2010). This article covers advancements in technologies and the associated efficacies. The life-cycle, energy savings and market potential of these technologies are addressed as well.

  19. Litter decomposition over broad spatial and long time scales investigated by advanced solid-state NMR: insight into effects of climate, litter quality, and time

    NASA Astrophysics Data System (ADS)

    Mao, J.; Chen, N.; Harmon, M. E.; Li, Y.; Cao, X.; Chappell, M.

    2012-12-01

    Advanced 13C solid-state NMR techniques were employed to study the chemical structural changes of litter decomposition across broad spatial and long time scales. The fresh and decomposed litter samples of four species (Acer saccharum (ACSA), Drypetes glauca (DRGL), Pinus resinosa (PIRE), and Thuja plicata (THPL)) incubated for up to 10 years at four sites under different climatic conditions (from Arctic to tropical forest) were examined. Decomposition generally led to an enrichment of cutin and surface wax materials, and a depletion of carbohydrates causing overall composition to become more similar compared with original litters. However, the changes of main constituents in the four litters were inconsistent with the four litters following different pathways of decomposition at the same site. As decomposition proceeded, waxy materials decreased at the early stage and then gradually increased in PIRE; DRGL showed a significant depletion of lignin and tannin while the changes of lignin and tannin were relative small and inconsistent for ACSA and THPL. In addition, the NCH groups, which could be associated with either fungal cell wall chitin or bacterial wall petidoglycan, were enriched in all litters except THPL. Contrary to the classic lignin-enrichment hypothesis, DRGL with low-quality C substrate had the highest degree of composition changes. Furthermore, some samples had more "advanced" compositional changes in the intermediate stage of decomposition than in the highly-decomposed stage. This pattern might be attributed to the formation of new cross-linking structures, that rendered substrates more complex and difficult for enzymes to attack. Finally, litter quality overrode climate and time factors as a control of long-term changes of chemical composition.

  20. Multiple Locations of Peptides in the Hydrocarbon Core of Gel-Phase Membranes Revealed by Peptide 13C to Lipid 2H Rotational-Echo Double-Resonance Solid-State Nuclear Magnetic Resonance

    PubMed Central

    2015-01-01

    Membrane locations of peptides and proteins are often critical to their functions. Solid-state rotational-echo double-resonance (REDOR) nuclear magnetic resonance is applied to probe the locations of two peptides via peptide 13CO to lipid 2H distance measurements. The peptides are KALP, an α-helical membrane-spanning peptide, and HFP, the β-sheet N-terminal fusion peptide of the HIV gp41 fusion protein that plays an important role in HIV–host cell membrane fusion. Both peptides are shown to have at least two distinct locations within the hydrocarbon core of gel-phase membranes. The multiple locations are attributed to snorkeling of lysine side chains for KALP and to the distribution of antiparallel β-sheet registries for HFP. The relative population of each location is also quantitated. To the best of our knowledge, this is the first clear experimental support of multiple peptide locations within the membrane hydrocarbon core. These data are for gel-phase membranes, but the approach should work for liquid-ordered membranes containing cholesterol and may be applicable to liquid-disordered membranes with appropriate additional analysis to take into account protein and lipid motion. This paper also describes the methodological development of 13CO–2H REDOR using the lyophilized I4 peptide that is α-helical and 13CO-labeled at A9 and 2Hα-labeled at A8. The I4 spins are well-approximated as an ensemble of isolated 13CO–2H spin pairs each separated by 5.0 Å with a 37 Hz dipolar coupling. A pulse sequence with rectangular 100 kHz 2H π pulses results in rapid and extensive buildup of REDOR (ΔS/S0) with a dephasing time (τ). The buildup is well-fit by a simple exponential function with a rate of 24 Hz and an extent close to 1. These parameter values reflect nonradiative transitions between the 2H spin states during the dephasing period. Each spin pair spends approximately two-thirds of its time in the 13CO–2H (m = ±1) states and approximately one-third of

  1. Solid-state laser source of narrowband ultraviolet B light for skin disease care with advanced performance

    NASA Astrophysics Data System (ADS)

    Tarasov, Aleksandr A.; Chu, Hong; Buchwald, Kristian

    2015-02-01

    Two years ago we reported about the development of solid state laser source for medical skin treatment with wavelength 310.6 nm and average power 200 mW. Here we describe the results of investigation of the advanced version of the laser, which is a more compact device with increased output power and flat top beam profile. Ti: Sapphire laser, the main module of our source, was modified and optimized such, that UV average power of the device was increased 1.7 times. Fiber optic homogenizer was replaced by articulated arm with diffraction diffuser, providing round spot with flat profile at the skin. We investigated and compare characteristics of Ti: Sapphire lasers with volume Bragg grating and with fused silica transmission grating, which was used first time for Ti: Sapphire laser spectral selection and tuning. Promising performance of last gratings is demonstrated.

  2. Recent advances in efficient long-life, eye-safe solid state and CO2 lasers for laser radar applications

    NASA Technical Reports Server (NTRS)

    Hess, R. V.; Buoncristiani, A. M.; Brockman, P.; Bair, C. H.; Schryer, D. R.; Upchurch, B. T.; Wood, G. M.

    1989-01-01

    The key problems in the development of eye-safe solid-state lasers are discussed, taking into account the energy transfer mechanisms between the complicated energy level manifolds of the Tm, Ho, Er ion dopants in hosts with decreasing crystal fields such as YAG or YLF. Optimization of energy transfer for efficient lasing through choice of dopant concentration, power density, crystal field and temperature is addressed. The tailoring of energy transfer times to provide efficient energy extraction for short pulses used in DIAL and Doppler lidar is considered. Recent advances in Pt/SnO2 oxide catalysts and other noble metal/metal oxide combinations for CO2 lasers are discussed. Emphasis is given to the dramatic effects of small quantities of H2O vapor for increasing the activity and lifetime of Pt/SnO2 catalysts and to increased lifetime operation with rare isotope (C-12)(O-18)2 lasing mixtures.

  3. Conducting Reflective, Hands-On Research with Advanced Characterization Instruments: A High-Level Undergraduate Practical Exploring Solid-State Polymorphism

    ERIC Educational Resources Information Center

    Coles, S. J.; Mapp, L. K.

    2016-01-01

    An undergraduate practical exercise has been designed to provide hands-on, instrument-based experience of advanced characterization techniques. A research experience approach is taken, centered around the concept of solid-state polymorphism, which requires a detailed knowledge of molecular and crystal structure to be gained by advanced analytical…

  4. Degradation of mangrove tissues by arboreal termites (Nasutitermes acajutlae) and their role in the mangrove C cycle (Puerto Rico): Chemical characterization and organic matter provenance using bulk δ13C, C/N, alkaline CuO oxidation-GC/MS, and solid-state 13C NMR

    NASA Astrophysics Data System (ADS)

    Vane, Christopher H.; Kim, Alexander W.; Moss-Hayes, Vicky; Snape, Colin E.; Diaz, Miguel Castro; Khan, Nicole S.; Engelhart, Simon E.; Horton, Benjamin P.

    2013-08-01

    Arboreal termites are wood decaying organisms that play an important role in the first stages of C cycling in mangrove systems. The chemical composition of Rhizophora mangle, Avicennia germinans, and Laguncularia racemosa leaf, stem, and pneumatophore tissues as well as associated sediments was compared to that of nests of the termite Nasutitermes acajutlae. Nests gave δ13C values of -26.1 to -27.2‰ (±0.1) and C/N of 43.3 (±2.0) to 98.6 (±16.2) which were similar to all stem and pneumatophores but distinct from mangrove leaves or sediments. Organic matter processed by termites yielded lignin phenol concentrations (Λ, lambda) that were 2-4 times higher than stem or pneumatophores and 10-20 times higher than that of leaves or sediments, suggesting that the nests were more resistant to biodegradation than the mangrove vegetation source. 13C NMR revealed that polysaccharide content of mangrove tissues (50-69% C) was higher than that of the nests (46-51% C). Conversely, lignin accounted for 16.2-19.6% C of nest material, a threefold increase relative to living mangrove tissues; a similar increase in aromatic methoxyl content was also observed in the nests. Lipids (aliphatic and paraffinic moieties) were also important but rather variable chemical components of all three mangrove species, representing between 13.5 and 28.3% of the C content. Termite nests contained 3.14 Mg C ha-1 which represents approximately 2% of above ground C storage in mangroves, a value that is likely to increase upon burial due to their refractory chemical composition.

  5. An advanced solid state pressure transducer for high reliability SSME application

    NASA Technical Reports Server (NTRS)

    Johnson, R. L.; Wamstad, D. B.

    1985-01-01

    New methods to advance the state-of-the-art of pressure sensors for the Space Shuttle Main Engine were demonstrated. The results of the feasibility and breadboard demonstration phase and the current status of the research development prototype follow-on phase are presented. A technology breakthrough utilizing silicon piezoresistive technology was achieved in the first phase. A transducer design concept for the SSME application utilizes packaging materials with similar thermal coefficients of expansion and maintains the transducer seals primarily in compression. The silicon chip design will provide dual sensing outputs with laser trimmable integrated compensating electronics. The silicon resistor ion implant dose was customized for the SSME temperature requirement. A basic acoustic modeling software program was developed to evaluate the frequency response characteristics for the package design.

  6. Advanced solid-state NMR techniques for characterization of membrane protein structure and dynamics: Application to Anabaena Sensory Rhodopsin

    NASA Astrophysics Data System (ADS)

    Ward, Meaghan E.; Brown, Leonid S.; Ladizhansky, Vladimir

    2015-04-01

    Studies of the structure, dynamics, and function of membrane proteins (MPs) have long been considered one of the main applications of solid-state NMR (SSNMR). Advances in instrumentation, and the plethora of new SSNMR methodologies developed over the past decade have resulted in a number of high-resolution structures and structural models of both bitopic and polytopic α-helical MPs. The necessity to retain lipids in the sample, the high proportion of one type of secondary structure, differential dynamics, and the possibility of local disorder in the loop regions all create challenges for structure determination. In this Perspective article we describe our recent efforts directed at determining the structure and functional dynamics of Anabaena Sensory Rhodopsin, a heptahelical transmembrane (7TM) protein. We review some of the established and emerging methods which can be utilized for SSNMR-based structure determination, with a particular focus on those used for ASR, a bacterial protein which shares its 7TM architecture with G-protein coupled receptors.

  7. Advanced Solid-State Array Spectrometer (ASAS) data sets from the 1990 field season: A unique look at two forested ecosystems

    NASA Technical Reports Server (NTRS)

    Walthall, Charles L.; Irons, James; Dabney, Phillip; Peterson, David L.; Williams, Darrel L.; Johnson, Lee F.; Ranson, K. Jon

    1991-01-01

    The Advanced Solid-state Array Spectrometer (ASAS) is a pointable imaging spectrometer which uses a solid-state array to acquire imagery of terrestrial targets in 29 spectral bands from .4 to .8 microns. Performance and calibration of the instrument are described. The ASAS data sets obtained in 1990 provide a unique look at forest canopies from two different forest regions of the North America continent under varying temporal, spectral, and bidirectional conditions. These data sets will be used to study such parameters as the albedo of forest canopies, the dynamics of scene radiation due to factors such as canopy architecture, moisture stress, leaf chemistry, topography, and understory composition.

  8. Recent developments in solid-state magic-angle spinning, nuclear magnetic resonance of fully and significantly isotopically labelled peptides and proteins.

    PubMed Central

    Straus, Suzana K

    2004-01-01

    In recent years, a large number of solid-state nuclear magnetic resonance (NMR) techniques have been developed and applied to the study of fully or significantly isotopically labelled ((13)C, (15)N or (13)C/(15)N) biomolecules. In the past few years, the first structures of (13)C/(15)N-labelled peptides, Gly-Ile and Met-Leu-Phe, and a protein, Src-homology 3 domain, were solved using magic-angle spinning NMR, without recourse to any structural information obtained from other methods. This progress has been made possible by the development of NMR experiments to assign solid-state spectra and experiments to extract distance and orientational information. Another key aspect to the success of solid-state NMR is the advances made in sample preparation. These improvements will be reviewed in this contribution. Future prospects for the application of solid-state NMR to interesting biological questions will also briefly be discussed. PMID:15306412

  9. Advanced CPMAS-13C NMR techniques for molecular characterization of size-separated fractions from a soil humic acid.

    PubMed

    Conte, Pellegrino; Spaccini, Riccardo; Piccolo, Alessandro

    2006-09-01

    A humic acid extracted from a volcanic soil was subjected to preparative high-performance size-exclusion chromatography (HPSEC) to reduce its molecular complexity and eleven different size fractions were obtained. Cross-polarization magic-angle spinning 13C NMR (CPMAS 13C NMR) analysis performed with variable contact-time (VCT) pulse sequences showed that the largest molecular-size fractions contained aromatic, alkyl, and carbohydrate-like components. The carbohydrate-like content and the alkyl chain length seemed to decrease with decreasing molecular size. Progressive reduction of aromatic carbon atoms was also observed with decreasing molecular size of the separated fractions. Mathematical treatment of the results from VCT experiments enabled cross polarization (T (CH)) and proton spin-lattice relaxation (T(1rho)(H)) times to be related to structural differences among the size fractions. The conformational distribution indicated that the eleven size fractions could be allocated to two main groups. The first group, with larger nominal molecular sizes, was characterized by molecular domains with slower local molecular motion. The second group of size fractions, with smaller nominal molecular sizes, was characterized by a larger number of molecular domains with faster local molecular motion. The T (CH) and (T(1rho)(H)) values suggested that either condensed or strongly associated aromatic systems were predominant in the size fractions with the largest apparent molecular dimensions. PMID:16896626

  10. Quantitative Determination of Methylcyclohexanone Mixtures Using 13C NMR Spectroscopy: A Project for an Advanced Chemistry Laboratory

    NASA Astrophysics Data System (ADS)

    Lefevre, Joseph W.; Silveira, Augustine, Jr.

    2000-01-01

    The percentage composition of mixtures of four methylcyclohexanones was determined using 13C NMR spectroscopy as a quantitative analytical method. The data were acquired using standard broadband proton decoupling and inverse-gated decoupling, the latter done both with and without the paramagnetic relaxation reagent chromium(III) acetylacetonate [Cr(acac)3]. The standard broadband decoupled spectrum resulted in percentages far from the actual values owing to the varying nuclear Overhauser enhancements (NOEs) and spin-lattice relaxation times (T1's) of the various carbon atoms. These effects were eliminated in the inverse-gated experiments, and the results were very close to the actual percentages. Before examining the mixtures, the students studied a pure sample of 2-methylcyclohexanone. They assigned the 13C spectrum and determined the T1 of the carbonyl group both with and without Cr(acac)3 using the inversion-recovery method. Then a five-times-T1 delay was inserted between pulses in all subsequent inverse-gated decoupling experiments. This project provides students with valuable experience with modern NMR techniques. These include COrrelated SpectroscopY (COSY), Distortionless Enhancement by Polarization Transfer (DEPT) spectroscopy, HETeronuclear CORrelated (HETCOR) spectroscopy, T1 determination, standard broadband versus inverse-gated decoupling, and the addition of a paramagnetic relaxation reagent to dramatically shorten both the T

  11. Development of an image converter of radical design. [employing solid state electronics towards the production of an advanced engineering model camera system

    NASA Technical Reports Server (NTRS)

    Irwin, E. L.; Farnsworth, D. L.

    1972-01-01

    A long term investigation of thin film sensors, monolithic photo-field effect transistors, and epitaxially diffused phototransistors and photodiodes to meet requirements to produce acceptable all solid state, electronically scanned imaging system, led to the production of an advanced engineering model camera which employs a 200,000 element phototransistor array (organized in a matrix of 400 rows by 500 columns) to secure resolution comparable to commercial television. The full investigation is described for the period July 1962 through July 1972, and covers the following broad topics in detail: (1) sensor monoliths; (2) fabrication technology; (3) functional theory; (4) system methodology; and (5) deployment profile. A summary of the work and conclusions are given, along with extensive schematic diagrams of the final solid state imaging system product.

  12. Advances in High Energy Solid-State 2-micron Laser Transmitter Development for Ground and Airborne Wind and CO2 Measurements

    NASA Technical Reports Server (NTRS)

    Singh, Upendra N.; Yu, Jirong; Petros, Mulugeta; Chen, Songsheng; Kavaya, Michael J.; Trieu, Bo; Bai, Yingxin; Petzar, Paul; Modlin, Edward A.; Koch, Grady; Beyon, Jeffrey

    2010-01-01

    Sustained research efforts at NASA Langley Research Center (LaRC) during last fifteen years have resulted in a significant advancement in 2-micron diode-pumped, solid-state laser transmitter for wind and carbon dioxide measurement from ground, air and space-borne platform. Solid-state 2-micron laser is a key subsystem for a coherent Doppler lidar that measures the horizontal and vertical wind velocities with high precision and resolution. The same laser, after a few modifications, can also be used in a Differential Absorption Lidar (DIAL) system for measuring atmospheric CO2 concentration profiles. Researchers at NASA Langley Research Center have developed a compact, flight capable, high energy, injection seeded, 2-micron laser transmitter for ground and airborne wind and carbon dioxide measurements. It is capable of producing 250 mJ at 10 Hz by an oscillator and one amplifier. This compact laser transmitter was integrated into a mobile trailer based coherent Doppler wind and CO2 DIAL system and was deployed during field measurement campaigns. This paper will give an overview of 2-micron solid-state laser technology development and discuss results from recent ground-based field measurements.

  13. Solid-State Nuclear Power

    NASA Technical Reports Server (NTRS)

    George, Jeffrey A.

    2012-01-01

    A strategy for "Solid-State" Nuclear Power is proposed to guide development of technologies and systems into the second 50 years of nuclear spaceflight. The strategy emphasizes a simple and highly integrated system architecture with few moving parts or fluid loops; the leverage of modern advances in materials, manufacturing, semiconductors, microelectromechanical and nanotechnology devices; and the targeted advancement of high temperature nuclear fuels, materials and static power conversion to enable high performance from simple system topologies.

  14. OSA Proceedings on Advanced Solid-State Lasers. Vol. 10 - Proceedings of the Topical Meeting, Hilton Head, SC, Mar. 18-20, 1991

    SciTech Connect

    Dube, G.; Chase, L. Lawrence Livermore National Laboratory, Livermore, CA )

    1991-01-01

    The present volume on advanced solid-state lasers discusses Cr(3+), Cr(4+), short-pulse, titanium, F-center, mid-IR, and diode-pumped lasers, and nonlinear optics. Attention is given to the stabilization and a spectral characterization of an alexandrite laser for water vapor lidar measurements, crystal growth and spectroscopy of Cr:LiBaAlF6, a Q-switched tunable forsterite laser, and electron paramagnetic resonance spectroscopy of chromium-doped forsterite. Topics addressed include efficient frequency doubling of a self-starting additive-pulse mode-locked diode-pumped Nd:YAG laser, recent advances in Ti:Al2O3 unstable-resonator lasers, all-solid-state operation of a CW Ti:Al2O3 laser, and upconversion studies of flashlamp-pumped Cr,T,Ho:YAG. Also discussed are the top output parameters of an Ho-laser, spectroscopy and the 3-micron laser potential of Er crystals, the pulsed operation of microchip lasers, and blue optical parametric generation in LiB3O5.

  15. Solid State Division

    SciTech Connect

    Green, P.H.; Watson, D.M.

    1989-08-01

    This report contains brief discussions on work done in the Solid State Division of Oak Ridge National Laboratory. The topics covered are: Theoretical Solid State Physics; Neutron scattering; Physical properties of materials; The synthesis and characterization of materials; Ion beam and laser processing; and Structure of solids and surfaces. (LSP)

  16. Solid-state configurations

    NASA Technical Reports Server (NTRS)

    Schroeder, K. G.

    1980-01-01

    Two prototype solid-state phased array systems concepts developed for the solar power satellite (SPS) are described. In both concepts, the beam was centered on the rectenna by means of phase conjugation of a pilot signal emanating from the ground. Also discussed are results of solid state studies.

  17. Advances In Vertical Solid-State Current Limiters For Individual Field Emitter Regulation In High-Density Arrays

    NASA Astrophysics Data System (ADS)

    Hill, Frances A.; Velásquez-García, Luis F.

    2015-12-01

    We report the design, fabrication, and characterization of improved solid-state elements intended for individual regulation of field emitters part of high-density arrays. We demonstrate a high-yield, CMOS compatible fabrication process of single-crystal, vertical, ungated, n-type silicon field-effect transistors (FETs); each device behaves as a current source when is biased at a voltage larger than its drain-source saturation voltage. An ungated FET in saturation connected in series to a field emitter can compensate for the wide variation in current-voltage characteristics of the field emitters due to the tip radii spread present in any field emitter array, which should result in emitter burn-out protection, larger array utilization, and smaller array emission non-uniformity. Using 1-2 Ωcm single-crystal n-Si wafers, we fabricated arrays of 25 μm tall vertical ungated FETs with 0.5 μm diameter that span two orders of magnitude of array size. Experimental characterization of the arrays demonstrates that the current is limited with > 3.5 V bias voltage to the same ∼6 μA (6 A.cm-2) per-FET value. Finite element simulations of the device predict a saturation voltage close to the experimental value and a saturation current within a factor of two of the experimental value.

  18. 15N chemical shift referencing in solid state NMR.

    PubMed

    Bertani, Philippe; Raya, Jésus; Bechinger, Burkhard

    2014-01-01

    Solid-state NMR spectroscopy has much advanced during the last decade and provides a multitude of data that can be used for high-resolution structure determination of biomolecules, polymers, inorganic compounds or macromolecules. In some cases the chemical shift referencing has become a limiting factor to the precision of the structure calculations and we have therefore evaluated a number of methods used in proton-decoupled (15)N solid-state NMR spectroscopy. For (13)C solid-state NMR spectroscopy adamantane is generally accepted as an external standard, but to calibrate the (15)N chemical shift scale several standards are in use. As a consequence the published chemical shift values exhibit considerable differences (up to 22 ppm). In this paper we report the (15)N chemical shift of several commonly used references compounds in order to allow for comparison and recalibration of published data and future work. We show that (15)NH4Cl in its powdered form (at 39.3 ppm with respect to liquid NH3) is a suitable external reference as it produces narrow lines when compared to other reference compounds and at the same time allows for the set-up of cross-polarization NMR experiments. The compound is suitable to calibrate magic angle spinning and static NMR experiments. Finally the temperature variation of (15)NH4Cl chemical shift is reported. PMID:24746715

  19. The Organic Solid State.

    ERIC Educational Resources Information Center

    Cowan, Dwaine O.; Wlygul, Frank M.

    1986-01-01

    Reviews interesting and useful electrical, magnetic, and optical properties of the organic solid state. Offers speculation as to areas of fruitful research. Discusses organic superconductors, conducting organic polymers, organic metals, and traces recent history of creation of organic metals. (JM)

  20. Solid-State 2-Micron Laser Transmitter Advancement for Wind and Carbon Dioxide Measurements From Ground, Airborne, and Space-Based Lidar Systems

    NASA Technical Reports Server (NTRS)

    Singh, Upendra N.; Kavaya, Michael J.; Koch, Grady; Yu, Jirong; Ismail, Syed

    2008-01-01

    NASA Langley Research Center has been developing 2-micron lidar technologies over a decade for wind measurements, utilizing coherent Doppler wind lidar technique and carbon dioxide measurements, utilizing Differential Absorption Lidar (DIAL) technique. Significant advancements have been made towards developing state-of-the-art technologies towards laser transmitters, detectors, and receiver systems. These efforts have led to the development of solid-state lasers with high pulse energy, tunablility, wavelength-stability, and double-pulsed operation. This paper will present a review of these technological developments along with examples of high resolution wind and high precision CO2 DIAL measurements in the atmosphere. Plans for the development of compact high power lasers for applications in airborne and future space platforms for wind and regional to global scale measurement of atmospheric CO2 will also be discussed.

  1. Solid state switch

    DOEpatents

    Merritt, Bernard T.; Dreifuerst, Gary R.

    1994-01-01

    A solid state switch, with reverse conducting thyristors, is designed to operate at 20 kV hold-off voltage, 1500 A peak, 1.0 .mu.s pulsewidth, and 4500 pps, to replace thyratrons. The solid state switch is more reliable, more economical, and more easily repaired. The switch includes a stack of circuit card assemblies, a magnetic assist and a trigger chassis. Each circuit card assembly contains a reverse conducting thyristor, a resistor capacitor network, and triggering circuitry.

  2. Final LDRD report : design and fabrication of advanced device structures for ultra high efficiency solid state lighting.

    SciTech Connect

    Koleske, Daniel David; Bogart, Katherine Huderle Andersen; Shul, Randy John; Wendt, Joel Robert; Crawford, Mary Hagerott; Allerman, Andrew Alan; Fischer, Arthur Joseph

    2005-04-01

    The goal of this one year LDRD was to improve the overall efficiency of InGaN LEDs by improving the extraction of light from the semiconductor chip. InGaN LEDs are currently the most promising technology for producing high efficiency blue and green semiconductor light emitters. Improving the efficiency of InGaN LEDs will enable a more rapid adoption of semiconductor based lighting. In this LDRD, we proposed to develop photonic structures to improve light extraction from nitride-based light emitting diodes (LEDs). While many advanced device geometries were considered for this work, we focused on the use of a photonic crystal for improved light extraction. Although resonant cavity LEDs and other advanced structures certainly have the potential to improve light extraction, the photonic crystal approach showed the most promise in the early stages of this short program. The photonic crystal (PX)-LED developed here incorporates a two dimensional photonic crystal, or photonic lattice, into a nitride-based LED. The dimensions of the photonic crystal are selected such that there are very few or no optical modes in the plane of the LED ('lateral' modes). This will reduce or eliminate any radiation in the lateral direction so that the majority of the LED radiation will be in vertical modes that escape the semiconductor, which will improve the light-extraction efficiency. PX-LEDs were fabricated using a range of hole diameters and lattice constants and compared to control LEDs without a photonic crystal. The far field patterns from the PX-LEDs were dramatically modified by the presence of the photonic crystal. An increase in LED brightness of 1.75X was observed for light measured into a 40 degree emission cone with a total increase in power of 1.5X for an unencapsulated LED.

  3. Solid state switch

    DOEpatents

    Merritt, B.T.; Dreifuerst, G.R.

    1994-07-19

    A solid state switch, with reverse conducting thyristors, is designed to operate at 20 kV hold-off voltage, 1,500 A peak, 1.0 [mu]s pulsewidth, and 4,500 pps, to replace thyratrons. The solid state switch is more reliable, more economical, and more easily repaired. The switch includes a stack of circuit card assemblies, a magnetic assist and a trigger chassis. Each circuit card assembly contains a reverse conducting thyristor, a resistor capacitor network, and triggering circuitry. 6 figs.

  4. MRI with hyperpolarised [1-13C]pyruvate detects advanced pancreatic preneoplasia prior to invasive disease in a mouse model

    PubMed Central

    Serrao, Eva M; Kettunen, Mikko I; Rodrigues, Tiago B; Dzien, Piotr; Wright, Alan J; Gopinathan, Aarthi; Gallagher, Ferdia A; Lewis, David Y; Frese, Kristopher K; Almeida, Jaime; Howat, William J; Tuveson, David A; Brindle, Kevin M

    2016-01-01

    Objectives Pancreatic cancer (PCa) is treatable by surgery when detected at an early stage. Non-invasive imaging methods able to detect both established tumours and their precursor lesions are needed to select patients for surgery. We investigated here whether pancreatic preneoplasia could be detected prior to the development of invasive cancers in genetically engineered mouse models of PCa using metabolic imaging. Design The concentrations of alanine and lactate and the activities of lactate dehydrogenase (LDH) and alanine aminotransferase (ALT) were measured in extracts prepared from the pancreas of animals at different stages of disease progression; from pancreatitis, through tissue with predominantly low-grade and then high-grade pancreatic intraepithelial neoplasia and then tumour. 13C magnetic resonance spectroscopic imaging (13C-MRSI) was used to measure non-invasively changes in 13C labelling of alanine and lactate with disease progression, following injection of hyperpolarised [1-13C]pyruvate. Results Progressive decreases in the alanine/lactate concentration ratio and ALT/LDH activity ratio with disease progression were accompanied by a corresponding decrease in the [1-13C]alanine/[1-13C]lactate signal ratio observed in 13C-MRSI images of the pancreas. Conclusions Metabolic imaging with hyperpolarised [1-13C]pyruvate enables detection and monitoring of the progression of PCa precursor lesions. Translation of this MRI technique to the clinic has the potential to improve the management of patients at high risk of developing PCa. PMID:26347531

  5. Solid-state NMR and Membrane Proteins

    PubMed Central

    Opella, Stanley J.

    2015-01-01

    The native environment for a membrane protein is a phospholipid bilayer. Because the protein is immobilized on NMR timescales by the interactions within a bilayer membrane, solid-state NMR methods are essential to obtain high-resolution spectra. Approaches have been developed for both unoriented and oriented samples, however, they all rest on the foundation of the most fundamental aspects solid-state NMR, and the chemical shift and homo- and hetero-nuclear dipole-dipole interactions. Solid-state NMR has advanced sufficiently to enable the structures of membrane proteins to be determined under near-native conditions in phospholipid bilayers. PMID:25681966

  6. Solid-State Devices.

    ERIC Educational Resources Information Center

    Sutliff, Ronald D.; And Others

    This self-study course is designed to familiarize Marine Corps enlisted personnel with the principles of solid-state devices and their functions. The course contains four study units. Each study unit begins with a general objective, which is a statement of what the student should learn from the unit. The study units are divided into numbered work…

  7. Nanoscale mapping of lithium-ion diffusion in a cathode within an all-solid-state lithium-ion battery by advanced scanning probe microscopy techniques.

    PubMed

    Zhu, Jing; Lu, Li; Zeng, Kaiyang

    2013-02-26

    High-resolution real-space mapping of Li-ion diffusion in the LiNi(1/3)Co(1/3)Mn(1/3)O₂ cathode within an all-solid-state thin film Li-ion battery has been conducted using advanced scanning probe microscopy techniques, namely, band excitation electrochemical strain microscopy (BE-ESM) and conductive atomic force microscopy. In addition, local variations of the electrochemical response in the LiNi(1/3)Co(1/3)Mn(1/3)O₂ thin film cathode at different cycling stages have been investigated. This work demonstrates the unique feature and applications of the BE-ESM technique on battery research. The results allow us to establish a direct relationship of the changes in ionic mobility as well as the electrochemical activity at the nanoscale with the numbers of charge/discharge cycles. Furthermore, various factors influencing the BE-ESM measurements, including sample mechanical properties (e.g., elastic and dissipative properties) as well as surface electrical properties, have also been studied to investigate the coupling effects on the electrochemical strain. The study on the relationships between the Li-ion redistribution and microstructure of the electrode materials within thin film Li-ion battery will provide further understanding of the electrochemical degradation mechanisms of Li-ion rechargeable batteries at the nanoscale. PMID:23336441

  8. Solid State Laser

    NASA Technical Reports Server (NTRS)

    1990-01-01

    The Titan-CW Ti:sapphire (titanium-doped sapphire) tunable laser is an innovation in solid-state laser technology jointly developed by the Research and Solid State Laser Divisions of Schwartz Electro-optics, Inc. (SEO). SEO is producing the laser for the commercial market, an outgrowth of a program sponsored by Langley Research Center to develop Ti:sapphire technology for space use. SEO's Titan-CW series of Ti:sapphire tunable lasers have applicability in analytical equipment designed for qualitative analysis of carbohydrates and proteins, structural analysis of water, starch/sugar analyses, and measurements of salt in meat. Further applications are expected in semiconductor manufacture, in medicine for diagnosis and therapy, and in biochemistry.

  9. Solid State Research

    NASA Technical Reports Server (NTRS)

    Shaver, David C.

    1996-01-01

    This report covers in detail the research work of the Solid State Division at Lincoln Laboratory for the period 1 May - 31 July 1996. The topics covered are Electrooptical Devices, Quantum Electronics, Materials Research, Submicrometer Technology, High Speed Electronics, Microelectronics, and Analog Device Technology. Funding is provided primarily by the Air Force, with additional Support provided by the Army, DARPA, Navy, BMDO, NASA, and NIST.

  10. Solid State Research

    NASA Technical Reports Server (NTRS)

    Shaver, David C.

    1995-01-01

    This report covers in detail the research work of the Solid State Division at Lincoln Laboratory for the period 1 May-31 July 1995. The topics covered are: Electrooptical Devices, Quantum Electronics, Materials Research, Submicrometer Technology, High Speed Electronics, Microelectronics, and analog device technology. Funding is provided primarily by the Air Force, with additional Support provided by the Army, ARPA, Navy, BMDO, NASA and NIST.

  11. Tunable solid state lasers

    SciTech Connect

    Hammerling, R.; Budgor, A.B.; Pinto, A.

    1985-01-01

    This book presents the papers given at a conference on solid state lasers. Topics considered at the conference included transition-metal-doped lasers, line-narrowed alexandrite lasers, NASA specification, meteorological lidars, laser materials spectroscopy, laser pumped single pass gain, vibronic laser materials growth, crystal growth methods, vibronic laser theory, cross-fertilization through interdisciplinary fields, and laser action of color centers in diamonds.

  12. Solid state research

    NASA Astrophysics Data System (ADS)

    McWhorter, Alan L.

    1995-02-01

    This report covers in detail the research work of the Solid State Division at Lincoln Laboratory for the period 1 May through 31 July 1994. The topics covered are Electrooptical Devices, Quantum Electronics, Materials Research, Submicrometer Technology, High Speed Electronics, Microelectronics, and Analog Device Technology. Funding is provided primarily by the Air Force, with additional support provided by the Army, ARPA, Navy, BMDO, NASA, and NIST.

  13. Solid state research

    NASA Astrophysics Data System (ADS)

    Shaver, David C.

    1994-11-01

    This report covers in detail the research work of the Solid State Division at Lincoln Laboratory for the period 1 August through 31 October 1994. The topics covered are Electrooptical Devices, Quantum Electronics, Materials Research, Submicrometer Technology, High Speed Electronics, Microelectronics, and Analog Device Technology. Funding is provided primarily by the Air Force, with additional support provided by the Army, ARPA, Navy, BMDO, NASA, and NIST.

  14. Structural changes of humic acids from sinking organic matter and surface sediments investigated by advanced solid-state NMR: Insights into sources, preservation and molecularly uncharacterized components

    NASA Astrophysics Data System (ADS)

    Mao, Jingdong; Tremblay, Luc; Gagné, Jean-Pierre

    2011-12-01

    Knowledge of the structural changes that particulate organic matter (POM) undergoes in natural systems is essential for determining its reactivity and fate. In the present study, we used advanced solid-state NMR techniques to investigate the chemical structures of sinking particulate matter collected at different depths as well as humic acids (HAs) extracted from these samples and underlying sediments from the Saguenay Fjord and the St. Lawrence Lower Estuary (Canada). Compared to bulk POM, HAs contain more non-polar alkyls, aromatics, and aromatic C-O, but less carbohydrates (or carbohydrate-like structures). In the two locations studied, the C and N contents of the samples (POM and HAs) decreased with depth and after deposition onto sediments, leaving N-poor but O-enriched HAs and suggesting the involvement of partial oxidation reactions during POM microbial degradation. Advanced NMR techniques revealed that, compared to the water-column HAs, sedimentary HAs contained more protonated aromatics, non-protonated aromatics, aromatic C-O, carbohydrates (excluding anomerics), anomerics, OC q, O-C q-O, OCH, and OCH 3 groups, but less non-polar alkyls, NCH, and mobile CH 2 groups. These results are consistent with the relatively high reactivity of lipids and proteins or peptides. In contrast, carbohydrate-like structures were selectively preserved and appeared to be involved in substitution and copolymerization reactions. Some of these trends support the selective degradation (or selective preservation) theory. The results provide insights into mechanisms that likely contribute to the preservation of POM and the formation of molecules that escape characterization by traditional methods. Despite the depletion of non-polar alkyls with depth in HAs, a significant portion of their general structure survived and can be assigned to a model phospholipid. In addition, little changes in the connectivities of different functional groups were observed. Substituted and copolymerized

  15. Solid-state magnetic resonance spectroscopy of fullerenes

    SciTech Connect

    Tycko, R.; Haddon, R.C.; Dabbagh, G.; Glarum, S.H.; Douglass, D.C.; Mujsce, A.M. )

    1991-01-24

    The authors report solid-state {sup 13}C NMR measurements on powder samples of C{sub 60} and of a mixture of C{sub 60} and C{sub 70}. The NMR results show that, at 296 K, C{sub 60} molecules rotate rapidly and isotropically in the solid state, while C{sub 70} molecules rotate somewhat more anisotropically. These results are consistent with the proposed spherical geometry of C{sub 60} and prolate spheroidal geometry of C{sub 70}. The rotational correlation time of C{sub 60} molecules in the solid state becomes greater than 50 {mu}s at about 100 K.

  16. Fractional deuteration applied to biomolecular solid-state NMR spectroscopy.

    PubMed

    Nand, Deepak; Cukkemane, Abhishek; Becker, Stefan; Baldus, Marc

    2012-02-01

    Solid-state Nuclear Magnetic Resonance can provide detailed insight into structural and dynamical aspects of complex biomolecules. With increasing molecular size, advanced approaches for spectral simplification and the detection of medium to long-range contacts become of critical relevance. We have analyzed the protonation pattern of a membrane-embedded ion channel that was obtained from bacterial expression using protonated precursors and D(2)O medium. We find an overall reduction of 50% in protein protonation. High levels of deuteration at H(α) and H(β) positions reduce spectral congestion in ((1)H,(13)C,(15)N) correlation experiments and generate a transfer profile in longitudinal mixing schemes that can be tuned to specific resonance frequencies. At the same time, residual protons are predominantly found at amino-acid side-chain positions enhancing the prospects for obtaining side-chain resonance assignments and for detecting medium to long-range contacts. Fractional deuteration thus provides a powerful means to aid the structural analysis of complex biomolecules by solid-state NMR. PMID:22105305

  17. CARBON-13 NMR OR SOLID STATE HYDROCARBONS AND RELATED SUBSTANCES-FINAL REPORT

    SciTech Connect

    Grant, David M.

    2007-08-16

    CARBON-13 NMR OR SOLID STATE HYDROCARBONS AND RELATED SUBSTANCES-FINAL REPORT Abstract: During recent years we have been engaged in SSNMR (Solid State NMR) structural studies of unusual tetracyanoethylene compounds with unusually long bonds between four carbons centered on two electrons. The chemical shift tensors reflect these unusual atomic arrangements. Quantum chemistry predicts the strange tensor shifts. The three dimensional molecular structure may be determined in this manner. Despite significant advances in structural determination from powder diffraction data, NMR shift tensors argument the structural accuracy and also suggest initial trial structures. Mixtures of polymorphs are difficult to analyze with diffraction methods whereas the SSNMR methods are able to characterize such mixtures in one another’s presence. Spectroscopic developments in our laboratory include SSNMR INADEQUATE and FIREMAT methods. We have used these methods to study the 13C and 15N NMR explosive CL-20.

  18. Solid state thermal engine

    SciTech Connect

    Wayman, C.M.

    1981-01-27

    An improved solid state thermal engine utilizes as a drive member a braided belt fabricated from a memory alloy such as nickel-titanium and nickel-titanium ternary alloys, copper-zinc and copper-zinc ternary alloys, and the like. The braided belt is mounted on a set of pulleys to provide passage through a hot zone where the belt contracts and develops tension, and through a cold zone where it relaxes and stretches. Since more energy is delivered by contraction than is required for relaxation, positive work output results with an efficiency of between onefifth and one-third of the carnot cycle.

  19. Solid state devices

    NASA Technical Reports Server (NTRS)

    1991-01-01

    The Solid State Device research program is directed toward developing innovative devices for space remote and in-situ sensing, and for data processing. Innovative devices can result from the standard structures in innovative materials such as low and high temperature superconductors, strained layer superlattices, or diamond films. Innovative devices can also result from innovative structures achieved using electron tunneling or nanolithography in standard materials. A final step is to use both innovative structures and innovative materials. A new area of emphasis is the miniaturization of sensors and instruments molded by using the techniques of electronic device fabrication to micromachine silicon into micromechanical and electromechanical sensors and actuators.

  20. Solid state optical microscope

    DOEpatents

    Young, Ian T.

    1983-01-01

    A solid state optical microscope wherein wide-field and high-resolution images of an object are produced at a rapid rate by utilizing conventional optics with a charge-coupled photodiode array. A galvanometer scanning mirror, for scanning in one of two orthogonal directions is provided, while the charge-coupled photodiode array scans in the other orthogonal direction. Illumination light from the object is incident upon the photodiodes, creating packets of electrons (signals) which are representative of the illuminated object. The signals are then processed, stored in a memory, and finally displayed as a video signal.

  1. Solid state optical microscope

    DOEpatents

    Young, I.T.

    1983-08-09

    A solid state optical microscope wherein wide-field and high-resolution images of an object are produced at a rapid rate by utilizing conventional optics with a charge-coupled photodiode array. A galvanometer scanning mirror, for scanning in one of two orthogonal directions is provided, while the charge-coupled photodiode array scans in the other orthogonal direction. Illumination light from the object is incident upon the photodiodes, creating packets of electrons (signals) which are representative of the illuminated object. The signals are then processed, stored in a memory, and finally displayed as a video signal. 2 figs.

  2. Solid state oxygen sensor

    DOEpatents

    Garzon, Fernando H.; Chung, Brandon W.; Raistrick, Ian D.; Brosha, Eric L.

    1996-01-01

    Solid state oxygen sensors are provided with a yttria-doped zirconia as an electrolyte and use the electrochemical oxygen pumping of the zirconia electrolyte. A linear relationship between oxygen concentration and the voltage arising at a current plateau occurs when oxygen accessing the electrolyte is limited by a diffusion barrier. A diffusion barrier is formed herein with a mixed electronic and oxygen ion-conducting membrane of lanthanum-containing perovskite or zirconia-containing fluorite. A heater may be used to maintain an adequate oxygen diffusion coefficient in the mixed conducting layer.

  3. Solid state oxygen sensor

    DOEpatents

    Garzon, F.H.; Chung, B.W.; Raistrick, I.D.; Brosha, E.L.

    1996-08-06

    Solid state oxygen sensors are provided with a yttria-doped zirconia as an electrolyte and use the electrochemical oxygen pumping of the zirconia electrolyte. A linear relationship between oxygen concentration and the voltage arising at a current plateau occurs when oxygen accessing the electrolyte is limited by a diffusion barrier. A diffusion barrier is formed herein with a mixed electronic and oxygen ion-conducting membrane of lanthanum-containing perovskite or zirconia-containing fluorite. A heater may be used to maintain an adequate oxygen diffusion coefficient in the mixed conducting layer. 4 figs.

  4. Polymorphs of Theophylline Characterized by DNP Enhanced Solid-State NMR.

    PubMed

    Pinon, Arthur C; Rossini, Aaron J; Widdifield, Cory M; Gajan, David; Emsley, Lyndon

    2015-11-01

    We show how dynamic nuclear polarization (DNP) enhanced solid-state NMR spectroscopy can be used to characterize polymorphs and solvates of organic solids. We applied DNP to three polymorphs and one hydrated form of the asthma drug molecule theophylline. For some forms of theophylline, sample grinding and impregnation with the radical-containing solution, which are necessary to prepare the samples for DNP, were found to induce polymorphic transitions or desolvation between some forms. We present protocols for sample preparation for solid-state magic-angle spinning (MAS) DNP experiments that avoid the polymorphic phase transitions in theophylline. These protocols include cryogrinding, grinding under inert atmosphere, and the appropriate choice of the impregnating liquid. By applying these procedures, we subsequently demonstrate that two-dimensional correlation experiments, such as (1)H-(13)C and (1)H-(15)N HETCOR or (13)C-(13)C INADEQUATE, can be obtained at natural isotopic abundance in reasonable times, thus enabling more advanced structural characterization of polymorphs. PMID:26393368

  5. Solid state heat engine

    SciTech Connect

    Cory, J.S.

    1981-12-15

    A compact solid state turbine heat engine can be devised by pairing the nitinol elements. Each element is characterized by being in thermal contact with at least one hot water and one cold water bath and mechanically coupled to at least one driven pulley and driver pulley. A second nitinol element is similarly configured with a driver pulley, driven pulley, hot and cold water bath. The driver pulley associated with the first nitinol element is mechanically coupled to the driven pulley of the second nitinol element. Similarly, the driver pulley of the second nitinol element is mechanically coupled to the driven pulley of the first nitinol element. The paired nitinol elements form a compound solid state turbine engine wherein each nitinol element lies in a single plane and wherein the engine may be combined with a plurality of such pairs for increased power output. The nitinol elements may also incorporate a snubber to limit the strain on the element and the engine may further incorporate a variable radius pulley to increase the efficiency of mechanical conversion.

  6. Packaging of solid state devices

    DOEpatents

    Glidden, Steven C.; Sanders, Howard D.

    2006-01-03

    A package for one or more solid state devices in a single module that allows for operation at high voltage, high current, or both high voltage and high current. Low thermal resistance between the solid state devices and an exterior of the package and matched coefficient of thermal expansion between the solid state devices and the materials used in packaging enables high power operation. The solid state devices are soldered between two layers of ceramic with metal traces that interconnect the devices and external contacts. This approach provides a simple method for assembling and encapsulating high power solid state devices.

  7. Solid state power controllers

    NASA Technical Reports Server (NTRS)

    Gibbs, R. S.

    1973-01-01

    The rationale, analysis, design, breadboarding and testing of the incremental functional requirements are reported that led to the development of prototype 1 and 5 Amp dc and 1 Amp ac solid state power controllers (SSPC's). The SSPC's are to be considered for use as a replacement of electro-mechanical relays and circuit breakers in future spacecraft and aircraft. They satisfy the combined function of both the relay and circuit breaker and can be remotely controlled by small signals, typically 10 mA, 5 to 28 Vdc. They have the advantage over conventional relay/circuit breaker systems in that they can be located near utilization equipment and the primary ac or dc bus. The low level control, trip indication and status signals can be circuited by small guage wire for control, computer interface, logic, electrical multiplexing, unboard testing, and power management and distribution purposes. This results in increased system versatility at appreciable weight saving and increased reliability.

  8. Solid state television camera

    NASA Technical Reports Server (NTRS)

    1976-01-01

    The design, fabrication, and tests of a solid state television camera using a new charge-coupled imaging device are reported. An RCA charge-coupled device arranged in a 512 by 320 format and directly compatible with EIA format standards was the sensor selected. This is a three-phase, sealed surface-channel array that has 163,840 sensor elements, which employs a vertical frame transfer system for image readout. Included are test results of the complete camera system, circuit description and changes to such circuits as a result of integration and test, maintenance and operation section, recommendations to improve the camera system, and a complete set of electrical and mechanical drawing sketches.

  9. Solid state rapid thermocycling

    SciTech Connect

    Beer, Neil Reginald; Spadaccini, Christopher

    2014-05-13

    The rapid thermal cycling of a material is targeted. A solid state heat exchanger with a first well and second well is coupled to a power module. A thermoelectric element is coupled to the first well, the second well, and the power module, is configured to transfer thermal energy from the first well to the second well when current from the power module flows through the thermoelectric element in a first direction, and is configured to transfer thermal energy from the second well to the first well when current from the power module flows through the thermoelectric element in a second direction. A controller may be coupled to the thermoelectric elements, and may switch the direction of current flowing through the thermoelectric element in response to a determination by sensors coupled to the wells that the amount of thermal energy in the wells falls below or exceeds a pre-determined threshold.

  10. The Pythagorean Theorem and the Solid State

    ERIC Educational Resources Information Center

    Kelly, Brenda S.; Splittgerber, Allan G.

    2005-01-01

    Packing efficiency and crystal density can be calculated from basic geometric principles employing the Pythagorean theorem, if the unit-cell structure is known. The procedures illustrated have applicability in courses such as general chemistry, intermediate and advanced inorganic, materials science, and solid-state physics.

  11. Modular nonvolatile solid state recorder (MONSSTR) update

    NASA Astrophysics Data System (ADS)

    Klang, Mark R.; Small, Martin B.; Beams, Tom

    2001-12-01

    Solid state recorders have begun replacing traditional tape recorders in fulfilling the requirement to record images on airborne platforms. With the advances in electro-optical, IR, SAR, Multi and Hyper-spectral sensors and video recording requirements, solid state recorders have become the recorder of choice. Solid state recorders provide the additional storage, higher sustained bandwidth, less power, less weight and smaller footprint to meet the current and future recording requirements. CALCULEX, Inc., manufactures a non-volatile flash memory solid state recorder called the MONSSTR (Modular Non-volatile Solid State Recorder). MONSSTR is being used to record images from many different digital sensors on high performance aircraft such as the RF- 4, F-16 and the Royal Air Force Tornado. MONSSTR, with its internal multiplexer, is also used to record instrumentation data. This includes multiple streams of PCM and multiple channels of 1553 data. Instrumentation data is being recorded by MONSSTR systems in a range of platforms including F-22, F-15, F-16, Comanche Helicopter and US Navy torpedos. MONSSTR can also be used as a cockpit video recorder. This paper will provide an update of the MONSSTR.

  12. Solid State Lighting Program (Falcon)

    SciTech Connect

    Meeks, Steven

    2012-06-30

    Over the past two years, KLA-Tencor and partners successfully developed and deployed software and hardware tools that increase product yield for High Brightness LED (HBLED) manufacturing and reduce product development and factory ramp times. This report summarizes our development effort and details of how the results of the Solid State Light Program (Falcon) have started to help HBLED manufacturers optimize process control by enabling them to flag and correct identified killer defect conditions at any point of origin in the process manufacturing flow. This constitutes a quantum leap in yield management over current practice. Current practice consists of die dispositioning which is just rejection of bad die at end of process based upon probe tests, loosely assisted by optical in-line monitoring for gross process deficiencies. For the first time, and as a result of our Solid State Lighting Program, our LED manufacturing partners have obtained the software and hardware tools that optimize individual process steps to control killer defects at the point in the processes where they originate. Products developed during our two year program enable optimized inspection strategies for many product lines to minimize cost and maximize yield. The Solid State Lighting Program was structured in three phases: i) the development of advanced imaging modes that achieve clear separation between LED defect types, improves signal to noise and scan rates, and minimizes nuisance defects for both front end and back end inspection tools, ii) the creation of defect source analysis (DSA) software that connect the defect maps from back-end and front-end HBLED manufacturing tools to permit the automatic overlay and traceability of defects between tools and process steps, suppress nuisance defects, and identify the origin of killer defects with process step and conditions, and iii) working with partners (Philips Lumileds) on product wafers, obtain a detailed statistical correlation of automated

  13. In-situ Li7La3Zr2O12/LiCoO2 interface modification for advanced all-solid-state battery

    NASA Astrophysics Data System (ADS)

    Kato, Takehisa; Hamanaka, Tadashi; Yamamoto, Kazuo; Hirayama, Tsukasa; Sagane, Fumihiro; Motoyama, Munekazu; Iriyama, Yasutoshi

    2014-08-01

    The inherent high resistance of electrolyte/electrode interface in all-solid-state-lithium-secondary batteries (SSLB) poses a significant hurdle for the SSLB development. The interfacial resistivity between Li7La3Zr2O12 (LLZ) and LiCoO2 is decreased by introducing a thin Nb layer (∼10 nm) at this interface. The interface modification approach using a Nb interlayer dramatically improves the discharge capacity and rate capability of a SSLB.

  14. Solid state lasers - The next 10 years

    NASA Astrophysics Data System (ADS)

    Byer, Robert L.

    1988-10-01

    Major advances in solid state laser technology historically have been preceded by advances in pumping technology. The helical lamp used to pump the early ruby lasers was superseded by the linear flashlamp now used to pump Nd:YAG lasers. The next advance in pumping technology is the diode laser array. The improvements in power and efficiency of the diode laser coupled with the fortuitous spectral overlap of the diode laser emission wavelength with the Nd ion absorption bands near 805 nm have led to a revolution in solid state laser capability. Progress has been rapid with new ions and wavelengths reported in the near infrared from 946 nm to 2010 nm. Frequency extension via nonlinear interactions has led to green and blue sources of coherent radiation. Linewidths of less than 10 kHz have been demonstrated. Overall electrical efficiencies of greater than 10% have been achieved. As diode laser sources decrease in cost, high average power diode laser pumped solid state laser sources will become available. Power levels exceeding 1 kW appear possible. Potential applications of these compact all solid state laser sources to spectroscopy, quantum noise limited sensors, astronomy, and materials processing will be discussed.

  15. A Solid State Pyranometer

    NASA Astrophysics Data System (ADS)

    Dumitrescu, Anca Laura; Paulescu, Marius; Ercuta, Aurel

    2015-12-01

    The construction of a solid state device-based pyranometer designated to broadband irradiance measurements is presented in this paper. The device is built on the physical basis that the temperature difference between two bodies of identical shape and external surface area, identically exposed to the incident radiation, but having different absorption and heat transfer coefficients (e.g. one body is painted white and the other is painted black), is proportional to the incident irradiance. This proportionality may be put in evidence if the two bodies consisting of identical arrays of correspondingly painted semiconductor diodes, due to the thermal behaviour of their p-n junction. It is theoretically predicted and experimentally confirmed that the voltage drop across a diode passed through a constant forward current linearly decreases with the temperature of the junction. In other words, a signal proportional to the irradiance of the light source may be obtained via conventional analog electronics. The calibration of the apparatus, as performed by means of a professional device (LP PYRA 03), indicates a good linearity.

  16. Solid state power controllers

    NASA Technical Reports Server (NTRS)

    Gibbs, R. S.

    1974-01-01

    Solid state power controllers (SSPC's) are to be considered for use as replacements of electromechanical relays and circuit breakers in future spacecraft and aircraft. They satisfy the combined function of both the relay and circuit breaker and can be remotely controlled by small signals, typically 10 mA, 5 to 28 v(dc). They have the advantage over conventional relay/circuit breaker systems in that they can be located near the utilization equipment and the primary ac or dc bus. The low level control, trip indication and status signals can be circuited by small gauge wire for control, computer interface, logic, electrical multiplexing, onboard testing, power management, and distribution purposes. This results in increased system versatility at appreciable weight saving and increased reliability. Conventional systems require the heavy gage load wiring and the control wiring to be routed from the bus to the load to other remote relay contacts, switches, sensors, etc. and to the circuit breaker located in the flight engineer's compartment for purposes of manual reset.

  17. Solid state laser

    NASA Technical Reports Server (NTRS)

    Rines, Glen A. (Inventor); Moulton, Peter F. (Inventor); Harrison, James (Inventor)

    1993-01-01

    A wavelength-tunable, injection-seeded, dispersion-compensated, dispersively-pumped solid state laser includes a lasing medium; a highly reflective mirror; an output coupler; at least one isosceles Brewster prism oriented to the minimum deviation angle between the medium and the mirror for directing light of different wavelengths along different paths; means for varying the angle of the highly reflective mirror relative to the light from at least one Brewster angle for selecting a predetermined laser operating wavelength; a dispersion compensation apparatus associated with the lasing medium; a laser injection seeding port disposed between the dispersion compensation apparatus and one of the mirror and coupler and including a reflective surface at an acute non-Brewster angle to the laser beam for introducing a seed input; a dispersion compensation apparatus associated with the laser medium including opposite chirality optical elements; the lasing medium including a pump surface disposed at an acute angle to the laser beam to define a discrete path for the pumping laser beam separate from the pumped laser beam.

  18. A Study of the Abundance and 13C/12C Ratio of Atmospheric Carbon Dioxide to Advance the Scientific Understanding of Terrestrial Processes Regulating the Global Carbon Cycle

    SciTech Connect

    Stephen C. Piper

    2005-10-15

    The primary goal of our research program, consistent with the goals of the U.S. Climate Change Science Program and funded by the terrestrial carbon processes (TCP) program of DOE, has been to improve understanding of changes in the distribution and cycling of carbon among the active land, ocean and atmosphere reservoirs, with particular emphasis on terrestrial ecosystems. Our approach is to systematically measure atmospheric CO2 to produce time series data essential to reveal temporal and spatial patterns. Additional measurements of the 13C/12C isotopic ratio of CO2 provide a basis for distinguishing organic and inorganic processes. To pursue the significance of these patterns further, our research also involved interpretations of the observations by models, measurements of inorganic carbon in sea water, and of CO2 in air near growing land plants.

  19. Polymorphs of Theophylline Characterized by DNP Enhanced Solid-State NMR

    PubMed Central

    2015-01-01

    We show how dynamic nuclear polarization (DNP) enhanced solid-state NMR spectroscopy can be used to characterize polymorphs and solvates of organic solids. We applied DNP to three polymorphs and one hydrated form of the asthma drug molecule theophylline. For some forms of theophylline, sample grinding and impregnation with the radical-containing solution, which are necessary to prepare the samples for DNP, were found to induce polymorphic transitions or desolvation between some forms. We present protocols for sample preparation for solid-state magic-angle spinning (MAS) DNP experiments that avoid the polymorphic phase transitions in theophylline. These protocols include cryogrinding, grinding under inert atmosphere, and the appropriate choice of the impregnating liquid. By applying these procedures, we subsequently demonstrate that two-dimensional correlation experiments, such as 1H–13C and 1H–15N HETCOR or 13C–13C INADEQUATE, can be obtained at natural isotopic abundance in reasonable times, thus enabling more advanced structural characterization of polymorphs. PMID:26393368

  20. Dynamic nuclear polarization-enhanced solid-state NMR spectroscopy of GNNQQNY nanocrystals and amyloid fibrils

    PubMed Central

    Debelouchina, Galia T.; Bayro, Marvin J.; van der Wel, Patrick C. A.; Caporini, Marc A.; Barnes, Alexander B.; Rosay, Melanie; Maas, Werner E.; Griffin, Robert G.

    2015-01-01

    Dynamic nuclear polarization (DNP) utilizes the inherently larger polarization of electrons to enhance the sensitivity of conventional solid-state NMR experiments at low temperature. Recent advances in instrumentation development and sample preparation have transformed this field and have opened up new opportunities for its application to biological systems. Here, we present DNP-enhanced 13C–13C and 15N–13C correlation experiments on GNNQQNY nanocrystals and amyloid fibrils acquired at 9.4 T and 100 K and demonstrate that DNP can be used to obtain assignments and site-specific structural information very efficiently. We investigate the influence of temperature on the resolution, molecular conformation, structural integrity and dynamics in these two systems. In addition, we assess the low-temperature performance of two commonly used solid-state NMR experiments, proton-driven spin diffusion (PDSD) and transferred echo double resonance (TEDOR), and discuss their potential as tools for measurement of structurally relevant distances at low temperature in combination with DNP. PMID:20454733

  1. Nanoscale solid-state cooling: a review

    NASA Astrophysics Data System (ADS)

    Ziabari, Amirkoushyar; Zebarjadi, Mona; Vashaee, Daryoosh; Shakouri, Ali

    2016-09-01

    The recent developments in nanoscale solid-state cooling are reviewed. This includes both theoretical and experimental studies of different physical concepts, as well as nanostructured material design and device configurations. We primarily focus on thermoelectric, thermionic and thermo-magnetic coolers. Particular emphasis is given to the concepts based on metal–semiconductor superlattices, graded materials, non-equilibrium thermoelectric devices, Thomson coolers, and photon assisted Peltier coolers as promising methods for efficient solid-state cooling. Thermomagnetic effects such as magneto–Peltier and Nernst–Ettingshausen cooling are briefly described and recent advances and future trends in these areas are reviewed. The ongoing progress in solid-state cooling concepts such as spin-calorimetrics, electrocalorics, non-equilibrium/nonlinear Peltier devices, superconducting junctions and two-dimensional materials are also elucidated and practical achievements are reviewed. We explain the thermoreflectance thermal imaging microscopy and the transient Harman method as two unique techniques developed for characterization of thermoelectric microrefrigerators. The future prospects for solid-state cooling are briefly summarized.

  2. Nanoscale solid-state cooling: a review.

    PubMed

    Ziabari, Amirkoushyar; Zebarjadi, Mona; Vashaee, Daryoosh; Shakouri, Ali

    2016-09-01

    The recent developments in nanoscale solid-state cooling are reviewed. This includes both theoretical and experimental studies of different physical concepts, as well as nanostructured material design and device configurations. We primarily focus on thermoelectric, thermionic and thermo-magnetic coolers. Particular emphasis is given to the concepts based on metal-semiconductor superlattices, graded materials, non-equilibrium thermoelectric devices, Thomson coolers, and photon assisted Peltier coolers as promising methods for efficient solid-state cooling. Thermomagnetic effects such as magneto-Peltier and Nernst-Ettingshausen cooling are briefly described and recent advances and future trends in these areas are reviewed. The ongoing progress in solid-state cooling concepts such as spin-calorimetrics, electrocalorics, non-equilibrium/nonlinear Peltier devices, superconducting junctions and two-dimensional materials are also elucidated and practical achievements are reviewed. We explain the thermoreflectance thermal imaging microscopy and the transient Harman method as two unique techniques developed for characterization of thermoelectric microrefrigerators. The future prospects for solid-state cooling are briefly summarized. PMID:27519021

  3. On the solid-state NMR spectra of naproxen

    NASA Astrophysics Data System (ADS)

    Czernek, Jiří

    2015-01-01

    Two previous measurements of the 13C and 1H NMR isotropic chemical shifts in crystalline naproxen, which is an important pharmaceutical compound, are confronted with the results obtained from several theoretical approaches capable of the proper treatment of solid-phase effects. In the underlying geometrical optimizations, two crystal structures are considered. The agreement between the data sets is quantified, including an evaluation of the similarity between the experimental solid-state NMR spectra. The 13C-1H heteronuclear correlations are analyzed, and their various assignments are discussed employing the statistical treatment of the differences between the measured and theoretical isotropic chemical shifts.

  4. High energy efficient solid state laser sources

    NASA Technical Reports Server (NTRS)

    Byer, Robert L.

    1987-01-01

    Investigations continue of diode-laser-pumped solid-state laser oscillators and nonlinear processes using them as sources. Diode laser array pumped Nd:YAG and Nd:glass lasers have been demonstrated. Theoretical studies of non-planar oscillators have been advanced, producing new designs which should be more resistant to feedback and offer better frequency stability. A monolithic, singly resonant Optical Parametric Oscillator in MgO:LiNbO3 has been operated.

  5. High power solid state lasers

    SciTech Connect

    Weber, H.

    1988-01-01

    These proceedings discuss the following subjects: trends in materials processing with laser radiation; slabs and high power systems; glasses and new crystals; solid state lasers at HOYA Corp.; lamps, resonators and transmission; glasses as active materials for high average power solid state lasers; flashlamp pumped GGG-crystals; alexandrite lasers; designing telescope resonators; mode operation of neodymium: YAG lasers; intracavity frequency doubling with KTP crystal and thermal effects in cylinder lasers.

  6. Solid State Photovoltaic Research Branch

    SciTech Connect

    Not Available

    1990-09-01

    This report summarizes the progress of the Solid State Photovoltaic Research Branch of the Solar Energy Research Institute (SERI) from October 1, 1988, through September 30,l 1989. Six technical sections of the report cover these main areas of SERIs in-house research: Semiconductor Crystal Growth, Amorphous Silicon Research, Polycrystalline Thin Films, III-V High-Efficiency Photovoltaic Cells, Solid-State Theory, and Laser Raman and Luminescence Spectroscopy. Sections have been indexed separately for inclusion on the data base.

  7. Rotary resonance recoupling of 13C- 1H dipolar interactions in magic angle spinning 13C NMR of dynamic solids

    NASA Astrophysics Data System (ADS)

    Kitchin, Simon J.; Harris, Kenneth D. M.; Aliev, Abil E.; Apperley, David C.

    2000-06-01

    Rotary resonance recoupling of heteronuclear 13C- 1H dipolar interactions in magic angle spinning solid state 13C NMR spectra (recorded under conditions of 1H decoupling at frequency ν1 and magic angle spinning at frequency νr) has been studied for three examples of molecular solids (adamantane, ferrocene and hexamethylbenzene) in which substantial molecular motion is known to occur. It is shown that when rotary resonance conditions are satisfied (i.e. ν1/νr= n, for n=1 or 2), the recoupling can lead to motionally averaged Pake-like powder patterns from which information on 13C- 1H internuclear distances and/or molecular motion can be derived.

  8. Two-dimensional (13)C-(13)C correlation spectroscopy with magic angle spinning and dynamic nuclear polarization.

    PubMed

    Rosay, Melanie; Weis, Volker; Kreischer, Kenneth E; Temkin, Richard J; Griffin, Robert G

    2002-04-01

    The sensitivity of solid-state NMR experiments can be enhanced with dynamic nuclear polarization (DNP), a technique that transfers the high Boltzmann polarization of unpaired electrons to nuclei. Signal enhancements of up to 23 have been obtained for magic angle spinning (MAS) experiments at 5 T and 85-90 K using a custom-designed high-power gyrotron. The extended stability of MAS/DNP experiments at low temperature is demonstrated with (1)H-driven (13)C spin-diffusion experiments on the amino acid proline. These (13)C-(13)C chemical shift correlation spectra are the first two-dimensional MAS/DNP experiments performed at high field (>1.4 T). PMID:11916398

  9. Modern solid state laser materials

    SciTech Connect

    Krupke, W.F.

    1984-06-20

    This document contains visual aids used in an invited talk entitled Modern Solid State Laser Materials, presented at the Conference on Lasers and Electro-Optics (CLEO) held in Anaheim, California, on June 20, 1984. Interest at LLNL in solid state lasers focuses on evaluating the potential of solid state laser media for high average power applications, including inertial fusion power production. This talk identifies the relevant bulk material parameters characterizing average power capacity and uses chromium and neodymium co-doped gadolinium scandium gallium garnet (Nd:Cr:GSGG) as an example of a laser material with improved laser properties relative to Nd:YAG (plausible large-scale growth, more efficient spectral coupling to xenon flashlamp radiation, reduced stimulated emission cross section, adequate thermal shock and optical damage threshold parameters, etc.). Recently measured spectroscopic, kinetic, and thermo-mechanical properties of Nd:Cr:GSGG are given.

  10. Solid-state lithium battery

    SciTech Connect

    Ihlefeld, Jon; Clem, Paul G; Edney, Cynthia; Ingersoll, David; Nagasubramanian, Ganesan; Fenton, Kyle Ross

    2014-11-04

    The present invention is directed to a higher power, thin film lithium-ion electrolyte on a metallic substrate, enabling mass-produced solid-state lithium batteries. High-temperature thermodynamic equilibrium processing enables co-firing of oxides and base metals, providing a means to integrate the crystalline, lithium-stable, fast lithium-ion conductor lanthanum lithium tantalate (La.sub.1/3-xLi.sub.3xTaO.sub.3) directly with a thin metal foil current collector appropriate for a lithium-free solid-state battery.

  11. Solid State Reactor Final Report

    SciTech Connect

    Mays, G.T.

    2004-03-10

    The Solid State Reactor (SSR) is an advanced reactor concept designed to take advantage of Oak Ridge National Laboratory's (ORNL's) recently developed graphite foam that has enhanced heat transfer characteristics and excellent high-temperature mechanical properties, to provide an inherently safe, self-regulated, source of heat for power and other potential applications. This work was funded by the U.S. Department of Energy's Nuclear Energy Research Initiative (NERI) program (Project No. 99-064) from August 1999 through September 30, 2002. The initial concept of utilizing the graphite foam as a basis for developing an advanced reactor concept envisioned that a suite of reactor configurations and power levels could be developed for several different applications. The initial focus was looking at the reactor as a heat source that was scalable, independent of any heat removal/power conversion process. These applications might include conventional power generation, isotope production and destruction (actinides), and hydrogen production. Having conducted the initial research on the graphite foam and having performed the scoping parametric analyses from neutronics and thermal-hydraulic perspectives, it was necessary to focus on a particular application that would (1) demonstrate the viability of the overall concept and (2) require a reasonably structured design analysis process that would synthesize those important parameters that influence the concept the most as part of a feasible, working reactor system. Thus, the application targeted for this concept was supplying power for remote/harsh environments and a design that was easily deployable, simplistic from an operational standpoint, and utilized the new graphite foam. Specifically, a 500-kW(t) reactor concept was pursued that is naturally load following, inherently safe, optimized via neutronic studies to achieve near-zero reactivity change with burnup, and proliferation resistant. These four major areas of research

  12. Chemical shift referencing in MAS solid state NMR

    NASA Astrophysics Data System (ADS)

    Morcombe, Corey R.; Zilm, Kurt W.

    2003-06-01

    Solid state 13C magic angle spinning (MAS) NMR spectra are typically referenced externally using a probe which does not incorporate a field frequency lock. Solution NMR shifts on the other hand are more often determined with respect to an internal reference and using a deuterium based field frequency lock. Further differences arise in solution NMR of proteins and nucleic acids where both 13C and 1H shifts are referenced by recording the frequency of the 1H resonance of DSS (sodium salt of 2,2-dimethyl-2-silapentane-5-sulphonic acid) instead of TMS (tetramethylsilane). In this note we investigate the difficulties in relating shifts measured relative to TMS and DSS by these various approaches in solution and solids NMR, and calibrate adamantane as an external 13C standard for solids NMR. We find that external chemical shift referencing of magic angle spinning spectra is typically quite reproducible and accurate, with better than ±0.03 ppm accuracy being straight forward to achieve. Solid state and liquid phase NMR shifts obtained by magic angle spinning with external referencing agree with those measured using typical solution NMR hardware with the sample tube aligned with the applied field as long as magnetic susceptibility corrections and solvent shifts are taken into account. The DSS and TMS reference scales for 13C and 1H are related accurately using MAS NMR. Large solvent shifts for the 13C resonance in TMS in either deuterochloroform or methanol are observed, being +0.71 ppm and -0.74 ppm from external TMS, respectively. The ratio of the 13C resonance frequencies for the two carbons in solid adamantane to the 1H resonance of TMS is reported.

  13. Chemical shift referencing in MAS solid state NMR.

    PubMed

    Morcombe, Corey R; Zilm, Kurt W

    2003-06-01

    Solid state 13C magic angle spinning (MAS) NMR spectra are typically referenced externally using a probe which does not incorporate a field frequency lock. Solution NMR shifts on the other hand are more often determined with respect to an internal reference and using a deuterium based field frequency lock. Further differences arise in solution NMR of proteins and nucleic acids where both 13C and 1H shifts are referenced by recording the frequency of the 1H resonance of DSS (sodium salt of 2,2-dimethyl-2-silapentane-5-sulphonic acid) instead of TMS (tetramethylsilane). In this note we investigate the difficulties in relating shifts measured relative to TMS and DSS by these various approaches in solution and solids NMR, and calibrate adamantane as an external 13C standard for solids NMR. We find that external chemical shift referencing of magic angle spinning spectra is typically quite reproducible and accurate, with better than +/-0.03 ppm accuracy being straight forward to achieve. Solid state and liquid phase NMR shifts obtained by magic angle spinning with external referencing agree with those measured using typical solution NMR hardware with the sample tube aligned with the applied field as long as magnetic susceptibility corrections and solvent shifts are taken into account. The DSS and TMS reference scales for 13C and 1H are related accurately using MAS NMR. Large solvent shifts for the 13C resonance in TMS in either deuterochloroform or methanol are observed, being +0.71 ppm and -0.74 ppm from external TMS, respectively. The ratio of the 13C resonance frequencies for the two carbons in solid adamantane to the 1H resonance of TMS is reported. PMID:12810033

  14. Influence of 13C isotopic labeling location of 13C DNP of acetate using TEMPO free radical

    NASA Astrophysics Data System (ADS)

    Parish, Christopher; Niedbalski, Peter; Lumata, Lloyd

    2015-03-01

    Dynamic nuclear polarization (DNP) via the dissolution method enhances the liquid-state magnetic resonance (NMR or MRI) signals of insensitive nuclear spins by at least 10,000-fold. The basis for all these signal enhancements at room temperature is the polarization transfer from the electrons to nuclear spins at cryogenic temperature and high magnetic field. In this work, we have studied the influence of the location of 13C isotopic labeling on the DNP of sodium acetate at 3.35 T and 1.4 K using a wide ESR linewidth free radical 4-oxo-TEMPO. The carbonyl [1-13C]acetate spins produced a polarization level that is almost twice that of the methyl [2-13C]acetate spins. On the other hand, the polarization of the methyl 13C spins doubled to reach the level of [1-13C]acetate when the methyl group was deuterated. Meanwhile, the solid-state nuclear relaxation of these samples are the same and do not correlate with the polarization levels. These behavior implies that the nuclear relaxation for these samples is dominated by the contribution from the free radicals and the polarization levels can be explained by a thermodynamic picture of DNP.

  15. Solid State Processing of Bulk Metallic Glasses

    NASA Astrophysics Data System (ADS)

    Eckert, Jurgen

    1998-03-01

    Glasses are generally produced from the undercooled liquid state by rapid quenching methods or quasi-statically at slow cooling by the effective control of heterogeneous nucleation. For metallic systems, the latter method has recently led to the development of multicomponent metallic glasses with large glass forming ability and a wide supercooled liquid region before crystallization. Large-scale bulk samples can now be produced by conventional casting techniques. These materials exhibit advanced engineering properties such as excellent wear behavior, almost theoretical strength and good corrosion resistance, and are highly processable at temperatures above the glass transition temperature. As an alternative to quenching or casting techniques, glass formation can also be achieved by solid state processing without passing through the liquid state. Therefore, mechanical alloying as a special form of solid state reaction technique and subsequent consolidation of the resulting powders above the glass transition temperature can be used to prepare bulk metallic glasses through the powder metallurgy route. This paper surveys results of studies regarding the factors governing glass formation by solid state processing. The thermal stability of mechanically alloyed powders is compared with data for melt quenched samples, showing that basically the same glassy state can be reached approaching it from the liquid or the solid state. Special emphasis is given to the glass forming ranges achievable by the different techniques, and to preparation of nanostructured composite materials based on glassy alloys. The results are discussed with respect to the influence of processing conditions, impurity effects and heterogeneous nucleation of crystalline phases. Examples for consolidated bulk samples from mechanically alloyed powders are presented and compared with data for cast bulk specimens.

  16. Solid-state radioluminescent compositions

    DOEpatents

    Clough, Roger L.; Gill, John T.; Hawkins, Daniel B.; Renschler, Clifford L.; Shepodd, Timothy J.; Smith, Henry M.

    1991-01-01

    A solid state radioluminescent composition for light source comprises an optically clear polymer organic matrix containing tritiated organic materials and dyes capable of "red" shifting primary scintillation emissions from the polymer matrix. The tritiated organic materials are made by reducing, with tritium, an unsaturated organic compound that prior to reduction contains olefinic or alkynylic bonds.

  17. High Speed Solid State Circuit Breaker

    NASA Technical Reports Server (NTRS)

    Podlesak, Thomas F.

    1993-01-01

    The U.S. Army Research Laboratory, Fort Monmouth, NJ, has developed and is installing two 3.3 MW high speed solid state circuit breakers at the Army's Pulse Power Center. These circuit breakers will interrupt 4160V three phase power mains in no more than 300 microseconds, two orders of magnitude faster than conventional mechanical contact type circuit breakers. These circuit breakers utilize Gate Turnoff Thyristors (GTO's) and are currently utility type devices using air cooling in an air conditioned enclosure. Future refinements include liquid cooling, either water or two phase organic coolant, and more advanced semiconductors. Each of these refinements promises a more compact, more reliable unit.

  18. Nanoengineering for solid-state lighting.

    SciTech Connect

    Schubert, E. Fred; Koleske, Daniel David; Wetzel, Christian; Lee, Stephen Roger; Missert, Nancy A.; Lin, Shawn-Yu; Crawford, Mary Hagerott; Fischer, Arthur Joseph

    2009-09-01

    This report summarizes results from a 3-year Laboratory Directed Research and Development project performed in collaboration with researchers at Rensselaer Polytechnic Institute. Our collaborative effort was supported by Sandia's National Institute for Nanoengineering and focused on the study and application of nanoscience and nanoengineering concepts to improve the efficiency of semiconductor light-emitting diodes for solid-state lighting applications. The project explored LED efficiency advances with two primary thrusts: (1) the study of nanoscale InGaN materials properties, particularly nanoscale crystalline defects, and their impact on internal quantum efficiency, and (2) nanoscale engineering of dielectric and metal materials and integration with LED heterostructures for enhanced light extraction efficiency.

  19. Solid-state membrane module

    DOEpatents

    Gordon, John Howard; Taylor, Dale M.

    2011-06-07

    Solid-state membrane modules comprising at least one membrane unit, where the membrane unit has a dense mixed conducting oxide layer, and at least one conduit or manifold wherein the conduit or manifold comprises a dense layer and at least one of a porous layer and a slotted layer contiguous with the dense layer. The solid-state membrane modules may be used to carry out a variety of processes including the separating of any ionizable component from a feedstream wherein such ionizable component is capable of being transported through a dense mixed conducting oxide layer of the membrane units making up the membrane modules. For ease of construction, the membrane units may be planar.

  20. Solid-state membrane module

    SciTech Connect

    Hinklin, Thomas Ray; Lewinsohn, Charles Arthur

    2015-06-30

    A module for separating oxygen from an oxygen-containing gaseous mixture comprising planar solid-state membrane units, each membrane unit comprising planar dense mixed conducting oxides layers, planar channel-free porous support layers, and one or more planar intermediate support layers comprising at least one channeled porous support layer. The porosity of the planar channeled porous support layers is less than the porosity of the planar channel-free porous support layers.

  1. Solid state electrochemical current source

    DOEpatents

    Potanin, Alexander Arkadyevich; Vedeneev, Nikolai Ivanovich

    2002-04-30

    A cathode and a solid state electrochemical cell comprising said cathode, a solid anode and solid fluoride ion conducting electrolyte. The cathode comprises a metal oxide and a compound fluoride containing at least two metals with different valences. Representative compound fluorides include solid solutions of bismuth fluoride and potassium fluoride; and lead fluoride and potassium fluoride. Representative metal oxides include copper oxide, lead oxide, manganese oxide, vanadium oxide and silver oxide.

  2. Radiation sensitive solid state switch

    NASA Technical Reports Server (NTRS)

    Hutto, R. J. (Inventor)

    1973-01-01

    A mechanically operable solid state switch suited for use in achieving a variable circuit-switching function is described. This switch is characterized by an annular array of photoresponsive switching devices, disposed in communication with an included source of radiation, and a plurality of interchangeable, mechanically operable interrupter disks. Each disk has a predetermined pattern of transparent and opaque portions. Operative displacement of each disk serves to make and break selected electrical circuits through the photo responsive devices of said array.

  3. Solid-state NMR study of fluorinated steroids.

    PubMed

    Yang, Kai-Jay; Lin, Su-Ching; Huang, Shing-Jong; Ching, Wei-Min; Hung, Chen-Hsiung; Tzou, Der-Lii M

    2014-02-01

    Solid-state {(1)H}(13)C cross-polarization/magic angle spinning (CP/MAS) NMR spectroscopy was performed to analyze two fluorinated steroids, i.e., betamethasone (BMS) and fludrocortisone acetate (FCA), that have fluorine attached to C9, as well as two non-fluorinated analogs, i.e., prednisolone (PRD) and hydrocortisone 21-acetate (HCA). The (13)C signals of BMS revealed multiplet patterns with splittings of 16-215Hz, indicating multiple ring conformations, whereas the (13)C signals of FCA, HCA, and PRD exhibited only singlet patterns, implying a unique conformation. In addition, BMS and FCA exhibited substantial deviation (>3.5ppm) in approximately half of the (13)C signals and significant deviation (>45ppm) in the (13)C9 signal compared to PRD and HCA, respectively. In this study, we demonstrate that fluorinated steroids, such as BMS and FCA, have steroidal ring conformation(s) that are distinct from non-fluorinated analogs, such as PRD and HCA. PMID:24316163

  4. Solid state amorphization kinetic of alpha lactose upon mechanical milling.

    PubMed

    Caron, Vincent; Willart, Jean-François; Lefort, Ronan; Derollez, Patrick; Danède, Florence; Descamps, Marc

    2011-11-29

    It has been previously reported that α-lactose could be totally amorphized by ball milling. In this paper we report a detailed investigation of the structural and microstructural changes by which this solid state amorphization takes place. The investigations have been performed by Powder X-ray Diffraction, Solid State Nuclear Magnetic Resonance ((13)C CP-MAS) and Differential Scanning Calorimetry. The results reveal the structural complexity of the material in the course of its amorphization so that it cannot be considered as a simple mixture made of a decreasing crystalline fraction and an increasing amorphous fraction. Heating this complexity can give rise to a fully nano-crystalline material. The results also show that chemical degradations upon heating are strongly connected to the melting process. PMID:21983262

  5. Fermentation and Cost-Effective 13C/15N Labeling of the Nonribosomal Peptide Gramicidin S for Nuclear Magnetic Resonance Structure Analysis.

    PubMed

    Berditsch, Marina; Afonin, Sergii; Steineker, Anna; Orel, Nataliia; Jakovkin, Igor; Weber, Christian; Ulrich, Anne S

    2015-06-01

    Gramicidin S (GS) is a nonribosomally synthesized decapeptide from Aneurinibacillus migulanus. Its pronounced antibiotic activity is attributed to amphiphilic structure and enables GS interaction with bacterial membranes. Despite its medical use for over 70 years, the peptide-lipid interactions of GS and its molecular mechanism of action are still not fully understood. Therefore, a comprehensive structural analysis of isotope-labeled GS needs to be performed in its biologically relevant membrane-bound state, using advanced solid-state nuclear magnetic resonance (NMR) spectroscopy. Here, we describe an efficient method for producing the uniformly (13)C/(15)N-labeled peptide in a minimal medium supplemented by selected amino acids. As GS is an intracellular product of A. migulanus, we characterized the producer strain DSM 5759 (rough-convex phenotype) and examined its biosynthetic activity in terms of absolute and biomass-dependent peptide accumulation. We found that the addition of either arginine or ornithine increases the yield only at very high supplementing concentrations (1% and 0.4%, respectively) of these expensive (13)C/(15)N-labeled amino acids. The most cost-effective production of (13)C/(15)N-GS, giving up to 90 mg per gram of dry cell weight, was achieved in a minimal medium containing 1% (13)C-glycerol and 0.5% (15)N-ammonium sulfate, supplemented with only 0.025% of (13)C/(15)N-phenylalanine. The 100% efficiency of labeling is corroborated by mass spectrometry and preliminary solid-state NMR structure analysis of the labeled peptide in the membrane-bound state. PMID:25795666

  6. Fermentation and Cost-Effective 13C/15N Labeling of the Nonribosomal Peptide Gramicidin S for Nuclear Magnetic Resonance Structure Analysis

    PubMed Central

    Berditsch, Marina; Afonin, Sergii; Steineker, Anna; Orel, Nataliia; Jakovkin, Igor; Weber, Christian

    2015-01-01

    Gramicidin S (GS) is a nonribosomally synthesized decapeptide from Aneurinibacillus migulanus. Its pronounced antibiotic activity is attributed to amphiphilic structure and enables GS interaction with bacterial membranes. Despite its medical use for over 70 years, the peptide-lipid interactions of GS and its molecular mechanism of action are still not fully understood. Therefore, a comprehensive structural analysis of isotope-labeled GS needs to be performed in its biologically relevant membrane-bound state, using advanced solid-state nuclear magnetic resonance (NMR) spectroscopy. Here, we describe an efficient method for producing the uniformly 13C/15N-labeled peptide in a minimal medium supplemented by selected amino acids. As GS is an intracellular product of A. migulanus, we characterized the producer strain DSM 5759 (rough-convex phenotype) and examined its biosynthetic activity in terms of absolute and biomass-dependent peptide accumulation. We found that the addition of either arginine or ornithine increases the yield only at very high supplementing concentrations (1% and 0.4%, respectively) of these expensive 13C/15N-labeled amino acids. The most cost-effective production of 13C/15N-GS, giving up to 90 mg per gram of dry cell weight, was achieved in a minimal medium containing 1% 13C-glycerol and 0.5% 15N-ammonium sulfate, supplemented with only 0.025% of 13C/15N-phenylalanine. The 100% efficiency of labeling is corroborated by mass spectrometry and preliminary solid-state NMR structure analysis of the labeled peptide in the membrane-bound state. PMID:25795666

  7. Solid-State Personal Dosimetry

    NASA Technical Reports Server (NTRS)

    Wrbanek, John D.; Fralick, Gustave C.; Wrbanek, Susan Y.

    2005-01-01

    This document is a web site page, and a data sheet about Personal protection (i.e., space suits) presented to the Radiation and Micrometeoroid Mitigation Technology Focus Group meeting. The website describes the work of the PI to improve solid state personal radiation dosimetry. The data sheet presents work on the active personal radiation detection system that is to provide real-time local radiation exposure information during EVA. Should undue exposure occur, knowledge of the dynamic intensity conditions during the exposure will allow more precise diagnostic assessment of the potential health risk to the exposed individual.

  8. Solid state electrochromic light modulator

    DOEpatents

    Cogan, S.F.; Rauh, R.D.

    1990-07-03

    An all solid-state variable transmission electrochromic device has a source of charge compensating ions. An inorganic oxide counter electrode film which on reduction with the accompanying insertion of the charge compensating ions increases its transmission of light of predetermined wavelength is separated from a primary electrochromic film which on reduction with the accompanying insertion of the charge compensating ions decreases its transmission of light of predetermined wavelength by an insulating electrolyte film that transports the charge compensating ions. First and second electrodes are contiguous with the inorganic oxide counter electrode film and the primary electrochromic film, respectively, and separated by the three films. 4 figs.

  9. Solid state nuclear track detection

    SciTech Connect

    Durrani, S.A.; Bull, R.K.

    1987-01-01

    This book is a basic work on the technique variously known as 'nuclear track analysis', 'track-etch technique', or 'solid state nuclear tract detection'. This has greatly expanded in range, scope and depth since the early 1960's, soon after its discovery, until there is hardly a field now in which it has not found an actual or potential use. Such applications range from archaeology, geology, space physics, medicine and biology to reactor physics and nuclear physics-to name but a few.

  10. Solid state electrochromic light modulator

    DOEpatents

    Cogan, Stuart F.; Rauh, R. David

    1993-12-07

    An all solid-state variable transmission electrochromic device has a source of charge compensating ions. An inorganic oxide counterelectrode film which on reduction with the accompanying insertion of the charge compensating ions increases its transmission of light of predetermined wavelength is separated from a primary electrochromic film which on reduction with the accompanying insertion of the charge compensating ions decreases its transmission of light of predetermined wavelength by an insulating electrolyte film that transports the charge compensating ions. First and second electrodes are contiguous with the inorganic oxide counter electrode film and the primary electrochromic film, respectively, and separated by the three films.

  11. Solid-state optical microscope

    DOEpatents

    Young, I.T.

    1981-01-07

    A solid state optical microscope is described wherein wide-field and high-resolution images of an object are produced at a rapid rate by utilizing conventional optics with a charge-coupled photodiode array. Means for scanning in one of two orthogonal directions are provided, while the charge-coupled photodiode array scans in the other orthogonal direction. Illumination light from the object is incident upon the photodiodes, creating packets of electrons (signals) which are representative of the illuminated object. The signals are then processed, stored in a memory, and finally displayed as a video signal.

  12. Solid state electrochromic light modulator

    DOEpatents

    Cogan, Stuart F.; Rauh, R. David

    1993-01-01

    An all solid-state variable transmission electrochromic device has a source of charge compensating ions. An inorganic oxide counterelectrode film which on reduction with the accompanying insertion of the charge compensating ions increases its transmission of light of predetermined wavelength is separated from a primary electrochromic film which on reduction with the accompanying insertion of the charge compensating ions decreases its transmission of light of predetermined wavelength by an insulating electrolyte film that transports the charge compensating ions. First and second electrodes are contiguous with the inorganic oxide counter electrode film and the primary electrochromic film, respectively, and separated by the three films.

  13. Solid state electrochromic light modulator

    DOEpatents

    Cogan, Stuart F.; Rauh, R. David

    1990-01-01

    An all solid-state variable transmission electrochromic device has a source of charge compensating ions. An inorganic oxide counterelectrode film which on reduction with the accompanying insertion of the charge compensating ions increases its transmission of light of predetermined wavelength is separated from a primary electrochromic film which on reduction with the accompanying insertion of the charge compensating ions decreases its transmission of light of predetermined wavelength by an insulating electrolyte film that transports the charge compensating ions. First and second electrodes are contiguous with the inorganic oxide counter electrode film and the primary electrochromic film, respectively, and separated by the three films.

  14. Solid State Memory Study Final Report

    NASA Technical Reports Server (NTRS)

    Katti, R.

    1994-01-01

    Existing and future solid state nonvolatile memory technologies are described and evaluated in this report. Solid state memory technologies can offer size, speed, power, weight, and ruggedness advantages over conventional moving media storage technologoies such as disk or tape. This technology list is a broad sampling of past, present, emerging, and future solid state memory technologies.

  15. Solid-state proton conductors

    SciTech Connect

    Jewulski, J.R.; Osif, T.L.; Remick, R.J.

    1990-12-01

    The purpose of this program was to survey the field of solid-state proton conductors (SSPC), identify conductors that could be used to develop solid-state fuel cells suitable for use with coal derived fuel gases, and begin the experimental research required for the development of these fuel cells. This document covers the following topics: the history of developments and current status of the SSPC, including a review of proton conducting electrolyte structures, the current status of the medium temperature SSPC development, electrodes for moderate temperature (SSPC) fuel cell, basic material and measurement techniques applicable for SSPC development, modeling and optimization studies. Correlation and optimization studies, to include correlation studies on proton conduction and oxide cathode optimization for the SSPC fuel cell. Experiments with the SSPC fuel cells including the fabrication of the electrolyte disks, apparatus for conducting measurements, the strontium-cerium based electrolyte, the barium-cerium based electrolyte with solid foil electrodes, the barium-cerium based electrolyte with porous electrodes, and conduction mechanisms. 164 refs., 27 figs., 13 tabs.

  16. Contamination and solid state welds.

    SciTech Connect

    Mills, Bernice E.

    2007-05-01

    Since sensitivity to contamination is one of the verities of solid state joining, there is a need for assessing contamination of the part(s) to be joined, preferably nondestructively while it can be remedied. As the surfaces that are joined in pinch welds are inaccessible and thus provide a greater challenge, most of the discussion is of the search for the origin and effect of contamination on pinch welding and ways to detect and mitigate it. An example of contamination and the investigation and remediation of such a system is presented. Suggestions are made for techniques for nondestructive evaluation of contamination of surfaces for other solid state welds as well as for pinch welds. Surfaces that have good visual access are amenable to inspection by diffuse reflection infrared Fourier transform (DRIFT) spectroscopy. Although other techniques are useful for specific classes of contaminants (such as hydrocarbons), DRIFT can be used most classes of contaminants. Surfaces such as the interior of open tubes or stems that are to be pinch welded can be inspected using infrared reflection spectroscopy. It must be demonstrated whether or not this tool can detect graphite based contamination, which has been seen in stems. For tubes with one closed end, the technique that should be investigated is emission infrared spectroscopy.

  17. Solid state Raman image amplification

    NASA Astrophysics Data System (ADS)

    Calmes, Lonnie K.; Murray, James T.; Austin, William L.; Powell, Richard C.

    1998-07-01

    Lite Cycles has developed a new type of eye-safe, range-gated, lidar sensing element based on Solid-state Raman Image Amplification (SSRIA) in a solid-state optical crystal. SSRIA can amplify low-level infrared images with gains greater than 106 with the addition of only quantum-limited noise. The high gains from SSRIA can compensate for low quantum efficiency detectors and can reduce the need for detector cooling. The range-gate of SSRIA is controlled by the pulsewidth of the pump laser and can be as short as 30 - 100 cm for nanosecond pulses and less than 5 mm if picosecond pulses are used. SSRIA results in higher SNR images throughout a broad range of incident light levels, in contrast to the increasing noise factor with reduced gain in image intensified CCDs. A theoretical framework for the optical resolution of SSRIA is presented and it is shown that SSRIA can produce higher resolution than ICCDs. SSRIA is also superior in rejecting unwanted sunlight background, further increasing image SNR, and can be used for real-time optical signal processing. Applications for military use include eye-safe imaging lidars that can be used for autonomous vehicle identification and targeting.

  18. Solid-state array cameras.

    PubMed

    Strull, G; List, W F; Irwin, E L; Farnsworth, D L

    1972-05-01

    Over the past few years there has been growing interest shown in the rapidly maturing technology of totally solid-state imaging. This paper presents a synopsis of developments made in this field at the Westinghouse ATL facilities with emphasis on row-column organized monolithic arrays of diffused junction phototransistors. The complete processing sequence applicable to the fabrication of modern highdensity arrays is described from wafer ingot preparation to final sensor testing. Special steps found necessary for high yield processing, such as surface etching prior to both sawing and lapping, are discussed along with the rationale behind their adoption. Camera systems built around matrix array photosensors are presented in a historical time-wise progression beginning with the first 50 x 50 element converter developed in 1965 and running through the most recent 400 x 500 element system delivered in 1972. The freedom of mechanical architecture made available to system designers by solid-state array cameras is noted from the description of a bare-chip packaged cubic inch camera. Hybrid scan systems employing one-dimensional line arrays are cited, and the basic tradeoffs to their use are listed. PMID:20119094

  19. Investigation of Moisture Interaction with Cellulose Using Solid-State NMR

    Technology Transfer Automated Retrieval System (TEKTRAN)

    The interaction of water with cellulose and its influence on the nuclear spin dynamics in Gossypium barbadense (Pima) cotton were investigated by 1H and 13C solid-state NMR techniques. 1H spin diffusion results indicate that water is present in multiple layers within the cotton fiber, each layer bei...

  20. Advanced dimming strategy for solid state luminaires

    NASA Astrophysics Data System (ADS)

    Beczkowski, Szymon

    2010-08-01

    Increased luminaire gamut as well as increase in luminous efficiency is found when the LED based luminaire is driven by a hybrid PWM/AM dimming technique. This technique is applicable to any n-chromaticity luminaire but it is especially suitable for trichromatic RGB luminaires that do not have inherent degrees of freedom. Diodes' properties under the hybrid dimming method were measured and used in nonlinear optimization routine to find the driving conditions that yield e.g. the highest possible efficacy for a given color point.

  1. Inexpensive solid state radiation detector

    NASA Astrophysics Data System (ADS)

    Aplin, Karen; Hastings, Peter; Harrison, R. Giles; Nicoll, Keri

    2015-04-01

    Monitoring of environmental radioactivity is of interest both within the geosciences community and to groups such as the emergency services who need to quickly assess the safety of an environment. Here we present a light weight and inexpensive detector based on solid state technology, that can be easily worn or carried, or used disposably. It responds to gamma radiation and other radioactive particles such as those from space weather and cosmic rays. Unlike traditional technology such as the Geiger counter, the detector can operate at low voltage without the need for step-up circuitry, and it can also distinguish different particle energies. It is suitable for monitoring background radioactivity from cosmic rays and radon as well as responding to higher radioactivity levels. We anticipate that the device will have a broad range of end users, from terrestrial to space applications.

  2. A compact solid state laser

    NASA Astrophysics Data System (ADS)

    Pati, Bhabana; Park, Eric D.; Stebbins, Kenneth

    2016-03-01

    A compact laser producing green wavelength with a volume of < 8 cm3 and a weight of < 80 g finds its application in many fields from military to space based. We built a small solid-state laser that produces 1 mJ of energy per-pulse at a 1 - 20 Hz repetition rate. The laser is passively Q-switched using a Cr4+:YAG saturable absorber to generate pulses <10 ns. A nonlinear crystal doubles the frequency to generate light at 523 nm. The laser is side-pumped by a single bar diode laser using a unique pump cavity to homogenize the pump intensity in the laser rod. The laser components can easily be modified to change the output wavelength from UV to mid IR.

  3. Study of solid state photomultiplier

    NASA Technical Reports Server (NTRS)

    Hays, K. M.; Laviolette, R. A.

    1987-01-01

    Available solid state photomultiplier (SSPM) detectors were tested under low-background, low temperature conditions to determine the conditions producing optimal sensitivity in a space-based astronomy system such as a liquid cooled helium telescope in orbit. Detector temperatures varied between 6 and 9 K, with background flux ranging from 10 to the 13th power to less than 10 to the 6th power photons/square cm-s. Measured parameters included quantum efficiency, noise, dark current, and spectral response. Experimental data were reduced, analyzed, and combined with existing data to build the SSPM data base included herein. The results were compared to analytical models of SSPM performance where appropriate models existed. Analytical models presented here were developed to be as consistent with the data base as practicable. Significant differences between the theory and data are described. Some models were developed or updated as a result of this study.

  4. Solid-State Spectral Light Source System

    NASA Technical Reports Server (NTRS)

    Maffione, Robert; Dana, David

    2011-01-01

    A solid-state light source combines an array of light-emitting diodes (LEDs) with advanced electronic control and stabilization over both the spectrum and overall level of the light output. The use of LEDs provides efficient operation over a wide range of wavelengths and power levels, while electronic control permits extremely stable output and dynamic control over the output. In this innovation, LEDs are used instead of incandescent bulbs. Optical feedback and digital control are used to monitor and regulate the output of each LED. Because individual LEDs generate light within narrower ranges of wavelengths than incandescent bulbs, multiple LEDs are combined to provide a broad, continuous spectrum, or to produce light within discrete wavebands that are suitable for specific radiometric sensors.

  5. Structure of a protein determined by solid-state magic-angle-spinning NMR spectroscopy

    NASA Astrophysics Data System (ADS)

    Castellani, Federica; van Rossum, Barth; Diehl, Annette; Schubert, Mario; Rehbein, Kristina; Oschkinat, Hartmut

    2002-11-01

    The determination of a representative set of protein structures is a chief aim in structural genomics. Solid-state NMR may have a crucial role in structural investigations of those proteins that do not easily form crystals or are not accessible to solution NMR, such as amyloid systems or membrane proteins. Here we present a protein structure determined by solid-state magic-angle-spinning (MAS) NMR. Almost complete 13C and 15N resonance assignments for a micro-crystalline preparation of the α-spectrin Src-homology 3 (SH3) domain formed the basis for the extraction of a set of distance restraints. These restraints were derived from proton-driven spin diffusion (PDSD) spectra of biosynthetically site-directed, labelled samples obtained from bacteria grown using [1,3-13C]glycerol or [2-13C]glycerol as carbon sources. This allowed the observation of long-range distance correlations up to ~7Å. The calculated global fold of the α-spectrin SH3 domain is based on 286 inter-residue 13C-13C and six 15N-15N restraints, all self-consistently obtained by solid-state MAS NMR. This MAS NMR procedure should be widely applicable to small membrane proteins that can be expressed in bacteria.

  6. Preparation of RNA samples with narrow line widths for solid state NMR investigations

    NASA Astrophysics Data System (ADS)

    Huang, Wei; Bardaro, Michael F.; Varani, Gabriele; Drobny, Gary P.

    2012-10-01

    Solid state NMR can provide detailed structural and dynamic information on biological systems that cannot be studied under solution conditions, and can investigate motions which occur with rates that cannot be fully studied by solution NMR. This approach has successfully been used to study proteins, but the application of multidimensional solid state NMR to RNA has been limited because reported line widths have been too broad to execute most multidimensional experiments successfully. A reliable method to generate spectra with narrow line widths is necessary to apply the full range of solid state NMR spectroscopic approaches to RNA. Using the HIV-1 transactivation response (TAR) RNA as a model, we present an approach based on precipitation with polyethylene glycol that improves the line width of 13C signals in TAR from >6 ppm to about 1 ppm, making solid state 2D NMR studies of selectively enriched RNAs feasible at ambient temperature.

  7. Topical meeting on tunable solid state lasers. Digest of technical papers

    SciTech Connect

    Not Available

    1985-01-01

    This book presents the papers given at a conference on solid state lasers. Topics considered at the conference included lidar remote sensing, advances in alexandrite technology, photoluminescence, tunable laser materials selection, flash-pumped titanium lasers, color center lasers, Q-switching, alexandrite lasers, transparent glass ceramics, diode-pumped solid-state lasers for NASA space station lidar experiments, sources for optically pumped solid-state lasers, laser tuning, and monochromator wavelength measurement devices.

  8. Path toward a high-energy solid-state laser

    NASA Astrophysics Data System (ADS)

    Wood, Gary L.; Merkle, Larry D.; Dubinskii, Mark; Zandi, Bahram

    2004-04-01

    Lasers have come a long way since the first demonstration by Maiman of a ruby crystal laser in 1960. Lasers are used as scientific tools as well as for a wide variety of applications for both commercial industry and the military. Today lasers come in all types, shapes and sizes depending on their application. The solid-state laser has some distinct advantages in that it can be rugged, compact, and self contained, making it reliable over long periods of time. With the advent of diode laser pumping a ten times increase in overall laser efficiency has been realized. This significant event, and others, is changing the way solid-state lasers are applied and allows new possibilities. One of those new areas of exploration is the high energy laser. Solid-state lasers for welding are already developed and yield energies in the 0.5 to 6 kilojoule range. These lasers are at the forefront of what is possible in terms of high energy solid-state lasers. It is possible to achieve energies of greater than 100 kJ. These sorts of energies would allow applications, in addition to welding, such as directed energy weapons, extremely remote sensing, power transfer, propulsion, biological and chemical agent neutralization and unexploded and mine neutralization. This article will review these new advances in solid-state lasers and the different paths toward achieving a high energy laser. The advantages and challenges of each approach will be highlighted.

  9. Solid-state rechargeable magnesium battery

    DOEpatents

    Shao, Yuyan; Liu, Jun; Liu, Tianbiao; Li, Guosheng

    2016-09-06

    Embodiments of a solid-state electrolyte comprising magnesium borohydride, polyethylene oxide, and optionally a Group IIA or transition metal oxide are disclosed. The solid-state electrolyte may be a thin film comprising a dispersion of magnesium borohydride and magnesium oxide nanoparticles in polyethylene oxide. Rechargeable magnesium batteries including the disclosed solid-state electrolyte may have a coulombic efficiency .gtoreq.95% and exhibit cycling stability for at least 50 cycles.

  10. Solid state radiative heat pump

    DOEpatents

    Berdahl, P.H.

    1984-09-28

    A solid state radiative heat pump operable at room temperature (300 K) utilizes a semiconductor having a gap energy in the range of 0.03-0.25 eV and operated reversibly to produce an excess or deficit of change carriers as compared equilibrium. In one form of the invention an infrared semiconductor photodiode is used, with forward or reverse bias, to emit an excess or deficit of infrared radiation. In another form of the invention, a homogenous semiconductor is subjected to orthogonal magnetic and electric fields to emit an excess or deficit of infrared radiation. Three methods of enhancing transmission of radiation the active surface of the semiconductor are disclosed. In one method, an anti-refection layer is coated into the active surface of the semiconductor, the anti-reflection layer having an index of refraction equal to the square root of that of the semiconductor. In the second method, a passive layer is speaced trom the active surface of the semiconductor by a submicron vacuum gap, the passive layer having an index of refractive equal to that of the semiconductor. In the third method, a coupler with a paraboloid reflecting surface surface is in contact with the active surface of the semiconductor, the coupler having an index of refraction about the same as that of the semiconductor.

  11. Solid state radiative heat pump

    DOEpatents

    Berdahl, Paul H.

    1986-01-01

    A solid state radiative heat pump (10, 50, 70) operable at room temperature (300.degree. K.) utilizes a semiconductor having a gap energy in the range of 0.03-0.25 eV and operated reversibly to produce an excess or deficit of charge carriers as compared to thermal equilibrium. In one form of the invention (10, 70) an infrared semiconductor photodiode (21, 71) is used, with forward or reverse bias, to emit an excess or deficit of infrared radiation. In another form of the invention (50), a homogeneous semiconductor (51) is subjected to orthogonal magnetic and electric fields to emit an excess or deficit of infrared radiation. Three methods of enhancing transmission of radiation through the active surface of the semiconductor are disclosed. In one method, an anti-reflection layer (19) is coated into the active surface (13) of the semiconductor (11), the anti-reflection layer (19) having an index of refraction equal to the square root of that of the semiconductor (11). In the second method, a passive layer (75) is spaced from the active surface (73) of the semiconductor (71) by a submicron vacuum gap, the passive layer having an index of refractive equal to that of the semiconductor. In the third method, a coupler (91) with a paraboloid reflecting surface (92) is in contact with the active surface (13, 53) of the semiconductor (11, 51), the coupler having an index of refraction about the same as that of the semiconductor.

  12. XANES: Solid state mineral analysis

    NASA Astrophysics Data System (ADS)

    Bell, Peter M.

    Researchers in the field of mineral physics have become aware of new analytical techniques for studying the electronic structure of solids; one such technique is the X ray absorption fine structure (XFAS) method. In this technique the fine structure of the X ray K-edge, for example, can b e employed as a critical probe of t h e intricacies of a crystal structure (P. A. Lee, P. H. Citrin, P. Eisenberger, and B. M. Kincaid, Rev. Mod. Phys., 53, 799, 1981).A similar, related technique, X ray absorption near-edge spectroscopy (XANES), is a relatively unknown method of studying the electronic structure of solids. XANES is new, and due to its complex nature, data on all but very simple solids have not yet been applied rigorously. Among the first XANES results on minerals is the recent study reported by G. Knapp, B. Veal, H. Pan, and T. Klipper (Solid State Comm. 44, 1343, 1982) on perovskites, magnesiowustites, and other 3d oxides in the zircon and spinel groups. The interpretation of these results is still semiquantitative, being based on ground state and basic selection rule considerations. The results show, however, a strong correlation between near-edge spectra and crystal structure.

  13. Solid state safety jumper cables

    DOEpatents

    Kronberg, J.W.

    1993-02-23

    Solid state jumper cables for connecting two batteries in parallel, having two bridge rectifiers for developing a reference voltage, a four-input decoder for determining which terminals are to be connected based on a comparison of the voltage at each of the four terminals to the reference voltage, and a pair of relays for effecting the correct connection depending on the determination of the decoder. No connection will be made unless only one terminal of each battery has a higher voltage than the reference voltage, indicating positive'' terminals, and one has a lower voltage than the reference voltage, indicating negative'' terminals, and that, therefore, the two high voltage terminals may be connected and the two lower voltage terminals may be connected. Current flows once the appropriate relay device is closed. The relay device is preferably a MOSFET (metal oxide semiconductor field effect transistor) combined with a series array of photodiodes that develop MOSFET gate-closing potential when the decoder output causes an LED to light.

  14. Solid state photochemistry of polycarbonates

    NASA Technical Reports Server (NTRS)

    Gupta, A.; Rembaum, A.; Moacanin, J.

    1978-01-01

    The quantum yield of photoFries rearrangement in a polycarbonate film has been analyzed as a function of temperature and humidity on the basis of previously reported (Koyler and Mann, 1977) experimental data. Results indicate that in the homogeneous amorphous phase, photoFries rearrangement is a concerted process proceeding either from the pi star reversed arrow n singlet, in which case it must be subject to considerable self quenching, or from a triplet, presumably the first triplet since the lifetime of higher triplets is expected to be very short in the solid phase. If the parent excited state is the first triplet, chain scission is possibly an independent process, probably occurring from the pi star reversed arrow n singlet. Evidence of chain scission on photodegradation in the solid state includes loss of C-O and C-C bond intensities revealed in the Fourier transform infrared spectra, gel permeation chromotography elution profiles of degraded film samples dissolved in CHCl3, and a decrease in tensile strength and T sub g as photodegradation proceeds. Chain scission is apparently inhibited as photoFries products accumulate.

  15. Solid state safety jumper cables

    DOEpatents

    Kronberg, James W.

    1993-01-01

    Solid state jumper cables for connecting two batteries in parallel, having two bridge rectifiers for developing a reference voltage, a four-input decoder for determining which terminals are to be connected based on a comparison of the voltage at each of the four terminals to the reference voltage, and a pair of relays for effecting the correct connection depending on the determination of the decoder. No connection will be made unless only one terminal of each battery has a higher voltage than the reference voltage, indicating "positive" terminals, and one has a lower voltage than the reference voltage, indicating "negative" terminals, and that, therefore, the two high voltage terminals may be connected and the two lower voltage terminals may be connected. Current flows once the appropriate relay device is closed. The relay device is preferably a MOSFET (metal oxide semiconductor field effect transistor) combined with a series array of photodiodes that develop MOSFET gate-closing potential when the decoder output causes an LED to light.

  16. Solid-state NMR studies of supercapacitors.

    PubMed

    Griffin, John M; Forse, Alexander C; Grey, Clare P

    2016-01-01

    Electrochemical double-layer capacitors, or 'supercapacitors' are attracting increasing attention as high-power energy storage devices for a wide range of technological applications. These devices store charge through electrostatic interactions between liquid electrolyte ions and the surfaces of porous carbon electrodes. However, many aspects of the fundamental mechanism of supercapacitance are still not well understood, and there is a lack of experimental techniques which are capable of studying working devices. Recently, solid-state NMR has emerged as a powerful tool for studying the local environments and behaviour of electrolyte ions in supercapacitor electrodes. In this Trends article, we review these recent developments and applications. We first discuss the basic principles underlying the mechanism of supercapacitance, as well as the key NMR observables that are relevant to the study of supercapacitor electrodes. We then review some practical aspects of the study of working devices using ex situ and in situ methodologies and explain the key advances that these techniques have allowed on the study of supercapacitor charging mechanisms. NMR experiments have revealed that the pores of the carbon electrodes contain a significant number of electrolyte ions in the absence of any charging potential. This has important implications for the molecular mechanisms of supercapacitance, as charge can be stored by different ion adsorption/desorption processes. Crucially, we show how in situ NMR experiments can be used to quantitatively study and characterise the charging mechanism, with the experiments providing the most detailed picture of charge storage to date, offering the opportunity to design enhanced devices. Finally, an outlook for future directions for solid-state NMR in supercapacitor research is offered. PMID:26974032

  17. 13C NMR Metabolomics: INADEQUATE Network Analysis

    PubMed Central

    Clendinen, Chaevien S.; Pasquel, Christian; Ajredini, Ramadan; Edison, Arthur S.

    2015-01-01

    The many advantages of 13C NMR are often overshadowed by its intrinsically low sensitivity. Given that carbon makes up the backbone of most biologically relevant molecules, 13C NMR offers a straightforward measurement of these compounds. Two-dimensional 13C-13C correlation experiments like INADEQUATE (incredible natural abundance double quantum transfer experiment) are ideal for the structural elucidation of natural products and have great but untapped potential for metabolomics analysis. We demonstrate a new and semi-automated approach called INETA (INADEQUATE network analysis) for the untargeted analysis of INADEQUATE datasets using an in silico INADEQUATE database. We demonstrate this approach using isotopically labeled Caenorhabditis elegans mixtures. PMID:25932900

  18. New guidelines for δ13C measurements

    USGS Publications Warehouse

    Coplen, Tyler B.; Brand, Willi A.; Gehre, Matthias; Groning, Manfred; Meijer, Harro A. J.; Toman, Blaza; Verkouteren, R. Michael

    2006-01-01

    Consistency of δ13C measurements can be improved 39−47% by anchoring the δ13C scale with two isotopic reference materials differing substantially in 13C/12C. It is recommended thatδ13C values of both organic and inorganic materials be measured and expressed relative to VPDB (Vienna Peedee belemnite) on a scale normalized by assigning consensus values of −46.6‰ to L-SVEC lithium carbonate and +1.95‰ to NBS 19 calcium carbonate. Uncertainties of other reference material values on this scale are improved by factors up to two or more, and the values of some have been notably shifted:  the δ13C of NBS 22 oil is −30.03%.

  19. Density functional investigation of intermolecular effects on {sup 13}C NMR chemical-shielding tensors modeled with molecular clusters

    SciTech Connect

    Holmes, Sean T.; Dybowski, Cecil; Iuliucci, Robbie J.; Mueller, Karl T.

    2014-10-28

    A quantum-chemical method for modeling solid-state nuclear magnetic resonance chemical-shift tensors by calculations on large symmetry-adapted clusters of molecules is demonstrated. Four hundred sixty five principal components of the {sup 13}C chemical-shielding tensors of 24 organic materials are analyzed. The comparison of calculations on isolated molecules with molecules in clusters demonstrates that intermolecular effects can be successfully modeled using a cluster that represents a local portion of the lattice structure, without the need to use periodic-boundary conditions (PBCs). The accuracy of calculations which model the solid state using a cluster rivals the accuracy of calculations which model the solid state using PBCs, provided the cluster preserves the symmetry properties of the crystalline space group. The size and symmetry conditions that the model cluster must satisfy to obtain significant agreement with experimental chemical-shift values are discussed. The symmetry constraints described in the paper provide a systematic approach for incorporating intermolecular effects into chemical-shielding calculations performed at a level of theory that is more advanced than the generalized gradient approximation. Specifically, NMR parameters are calculated using the hybrid exchange-correlation functional B3PW91, which is not available in periodic codes. Calculations on structures of four molecules refined with density plane waves yield chemical-shielding values that are essentially in agreement with calculations on clusters where only the hydrogen sites are optimized and are used to provide insight into the inherent sensitivity of chemical shielding to lattice structure, including the role of rovibrational effects.

  20. Dynamic nuclear polarization-enhanced 13C NMR spectroscopy of static biological solids

    PubMed Central

    Potapov, Alexey; Yau, Wai-Ming; Tycko, Robert

    2013-01-01

    We explore the possibility of using dynamic nuclear polarization (DNP) to enhance signals in structural studies of biological solids by solid state NMR without sample spinning. Specifically, we use 2D 13C-13C exchange spectroscopy to probe the peptide backbone torsion angles (ϕ,ψ) in a series of selectively 13C-labeled 40-residue β-amyloid (Aβ1–40) samples, in both fibrillar and non-fibrillar states. Experiments are carried out at 9.39 T and 8 K, using a static double-resonance NMR probe and low-power microwave irradiation at 264 GHz. In frozen solutions of Aβ1–40 fibrils doped with DOTOPA-TEMPO, we observe DNP signal enhancement factors of 16–21. We show that the orientation- and frequency-dependent spin polarization exchange between sequential backbone carbonyl 13C labels can be simulated accurately using a simple expression for the exchange rate, after experimentally determined homogeneous 13C lineshapes are incorporated in the simulations. The experimental 2D 13C-13C exchange spectra place constraints on the ϕ and ψ angles between the two carbonyl labels. Although the data are not sufficient to determine ϕ and ψ uniquely, the data do provide non-trivial constraints that could be included in structure calculations. With DNP at low temperatures, 2D 13C-13C exchange spectra can be obtained from a 3.5 mg sample of Aβ1–40 fibrils in 4 hr or less, despite the broad 13C chemical shift anisotropy line shapes that are observed in static samples. PMID:23562665

  1. Dynamic nuclear polarization-enhanced 13C NMR spectroscopy of static biological solids

    NASA Astrophysics Data System (ADS)

    Potapov, Alexey; Yau, Wai-Ming; Tycko, Robert

    2013-06-01

    We explore the possibility of using dynamic nuclear polarization (DNP) to enhance signals in structural studies of biological solids by solid state NMR without sample spinning. Specifically, we use 2D 13C-13C exchange spectroscopy to probe the peptide backbone torsion angles (ϕ, ψ) in a series of selectively 13C-labeled 40-residue β-amyloid (Aβ1-40) samples, in both fibrillar and non-fibrillar states. Experiments are carried out at 9.39 T and 8 K, using a static double-resonance NMR probe and low-power microwave irradiation at 264 GHz. In frozen solutions of Aβ1-40 fibrils doped with DOTOPA-TEMPO, we observe DNP signal enhancement factors of 16-21. We show that the orientation- and frequency-dependent spin polarization exchange between sequential backbone carbonyl 13C labels can be simulated accurately using a simple expression for the exchange rate, after experimentally determined homogeneous 13C lineshapes are incorporated in the simulations. The experimental 2D 13C-13C exchange spectra place constraints on the ϕ and ψ angles between the two carbonyl labels. Although the data are not sufficient to determine ϕ and ψ uniquely, the data do provide non-trivial constraints that could be included in structure calculations. With DNP at low temperatures, 2D 13C-13C exchange spectra can be obtained from a 3.5 mg sample of Aβ1-40 fibrils in 4 h or less, despite the broad 13C chemical shift anisotropy line shapes that are observed in static samples.

  2. /sup 13/C spin diffusion of adamantane

    SciTech Connect

    Bronniman, C.E.; Szeverenyi, N.M.; Maciel, G.E.

    1983-10-15

    Two-dimensional exchange spectroscopy of natural abundance /sup 13/C--/sup 13/C spin diffusion in solid adamantane illustrates the influence that /sup 13/C--/sup 1/H dipole--dipole coupling exerts on /sup 13/C spin diffusion by determining spectral overlap in the /sup 13/C system. 2D /sup 13/C spectra were obtained for several values of mixing time tau/sub m/ and compared with spectra calculated in the limit of nearest-neighbor coupling. Good agreement is obtained for short tau/sub m/, during which the equilibration of neighboring spins dominates. For longer tau/sub m/, slower spin diffusion that is not acounted for by the simple model is seen; after nearest-neighbor spins equilibrate, communication over larger distances produces further mixing. It is possible to modify spin diffusion rates by altering experimental conditions, e.g., magic-angle spinning, low-power /sup 1/H decoupling, or spin locking /sup 13/C in the rotating frame during tau/sub m/.

  3. Solid state recorders for airborne reconnaissance

    NASA Astrophysics Data System (ADS)

    Klang, Mark R.

    2003-08-01

    Solid state recorders have become the recorder of choice for meeting airborne ruggedized requirements for reconnaissance and flight test. The cost of solid state recorders have decreased over the past few years that they are now less expense than the traditional high speed tape recorders. CALCULEX, Inc manufactures solid state recorders called MONSSTR (Modular Non-volatile Solid State Recorder). MONSSTR is being used on many different platforms such as F/A-22, Global Hawk, F-14, F-15, F-16, U-2, RF-4, and Tornado. This paper will discuss the advantages of using solid state recorders to meet the airborne reconnaissance requirement and the ability to record instrumentation data. The CALCULEX recorder has the ability to record sensor data and flight test data in the same chassis. This is an important feature because it eliminates additional boxes on the aircraft. The major advantages to using a solid state recorder include; reliability, small size, light weight, and power. Solid state recorders also have a larger storage capacity and higher bandwidth capability than other recording devices.

  4. Monitoring Cocrystal Formation via In Situ Solid-State NMR.

    PubMed

    Mandala, Venkata S; Loewus, Sarel J; Mehta, Manish A

    2014-10-01

    A detailed understanding of the mechanism of organic cocrystal formation remains elusive. Techniques that interrogate a reacting system in situ are preferred, though experimentally challenging. We report here the results of a solid-state in situ NMR study of the spontaneous formation of a cocrystal between a pharmaceutical mimic (caffeine) and a coformer (malonic acid). Using (13)C magic angle spinning NMR, we show that the formation of the cocrystal may be tracked in real time. We find no direct evidence for a short-lived, chemical shift-resolved amorphous solid intermediate. However, changes in the line width and line center of the malonic acid methylene resonance, in the course of the reaction, provide subtle clues to the mode of mass transfer that underlies cocrystal formation. PMID:26278442

  5. NASA developments in solid state power amplifiers

    NASA Technical Reports Server (NTRS)

    Leonard, Regis F.

    1990-01-01

    Over the last ten years, NASA has undertaken an extensive program aimed at development of solid state power amplifiers for space applications. Historically, the program may be divided into three phases. The first efforts were carried out in support of the advanced communications technology satellite (ACTS) program, which is developing an experimental version of a Ka-band commercial communications system. These first amplifiers attempted to use hybrid technology. The second phase was still targeted at ACTS frequencies, but concentrated on monolithic implementations, while the current, third phase, is a monolithic effort that focusses on frequencies appropriate for other NASA programs and stresses amplifier efficiency. The topics covered include: (1) 20 GHz hybrid amplifiers; (2) 20 GHz monolithic MESFET power amplifiers; (3) Texas Instruments' (TI) 20 GHz variable power amplifier; (4) TI 20 GHz high power amplifier; (5) high efficiency monolithic power amplifiers; (6) GHz high efficiency variable power amplifier; (7) TI 32 GHz monolithic power amplifier performance; (8) design goals for Hughes' 32 GHz variable power amplifier; and (9) performance goals for Hughes' pseudomorphic 60 GHz power amplifier.

  6. Inorganic membranes and solid state sciences

    NASA Astrophysics Data System (ADS)

    Cot, Louis; Ayral, André; Durand, Jean; Guizard, Christian; Hovnanian, Nadine; Julbe, Anne; Larbot, André

    2000-05-01

    The latest developments in inorganic membranes are closely related to recent advances in solid state science. Sol-gel processing, plasma-enhanced chemical vapor deposition and hydrothermal synthesis are methods that can be used for inorganic membrane preparation. Innovative concepts from material science (templating effect, nanophase materials, growing of continuous zeolite layers, hybrid organic-inorganic materials) have been applied by our group to the preparation of inorganic membrane materials. Sol-gel-derived nanophase ceramic membranes are presented with current applications in nanofiltration and catalytic membrane reactors. Silica membranes with an ordered porosity, due to liquid crystal phase templating effect, are described with potential application in pervaporation. Defect-free and thermally stable zeolite membranes can be obtained through an original synthesis method, in which zeolite crystals are grown inside the pores of a support. Hybrid organic-inorganic materials with permselective properties for gas separation and facilitated transport of solutes in liquid media, have been successfully adapted to membrane applications. Potential membrane developments offered by CVD deposition techniques are also illustrated through several examples related to the preparation of purely inorganic and hybrid organic-inorganic membrane materials.

  7. In vivo13C spectroscopy in the rat brain using hyperpolarized [1- 13C]pyruvate and [2- 13C]pyruvate

    NASA Astrophysics Data System (ADS)

    Marjańska, Małgorzata; Iltis, Isabelle; Shestov, Alexander A.; Deelchand, Dinesh K.; Nelson, Christopher; Uğurbil, Kâmil; Henry, Pierre-Gilles

    2010-10-01

    The low sensitivity of 13C spectroscopy can be enhanced using dynamic nuclear polarization. Detection of hyperpolarized [1- 13C]pyruvate and its metabolic products has been reported in kidney, liver, and muscle. In this work, the feasibility of measuring 13C signals of hyperpolarized 13C metabolic products in the rat brain in vivo following the injection of hyperpolarized [1- 13C]pyruvate and [2- 13C]pyruvate is investigated. Injection of [2- 13C]pyruvate led to the detection of [2- 13C]lactate, but no other downstream metabolites such as TCA cycle intermediates were detected. Injection of [1- 13C]pyruvate enabled the detection of both [1- 13C]lactate and [ 13C]bicarbonate. A metabolic model was used to fit the hyperpolarized 13C time courses obtained during infusion of [1- 13C]pyruvate and to determine the values of VPDH and VLDH.

  8. A New All Solid State Approach to Gaseous Pollutant Detection

    NASA Technical Reports Server (NTRS)

    Brown, V.; Tamstorf, K.

    1971-01-01

    Recent efforts in our laboratories have concentrated on the development of an all solid state gas sensor, by combining solid electrolyte (ion exchange membrane) technology with advanced thin film deposition processes. With the proper bias magnitude and polarity these miniature electro-chemical,cells show remarkable current responses for many common pollution gases. Current activity is now focused on complementing a multiple array (matrix) of these solid state sensors, with a digital electronic scanner device possessing "scan-compare-identify-alarm: capability. This innovative approach to multi-component pollutant gas analysis may indeed be the advanced prototype for the "third generation" class of pollution analysis instrumentation so urgently needed in the decade ahead.

  9. Protonation of carbon single-walled nanotubes studied using 13C and 1H-13C cross polarization nuclear magnetic resonance and Raman spectroscopies.

    PubMed

    Engtrakul, Chaiwat; Davis, Mark F; Gennett, Thomas; Dillon, Anne C; Jones, Kim M; Heben, Michael J

    2005-12-14

    The reversible protonation of carbon single-walled nanotubes (SWNTs) in sulfuric acid and Nafion was investigated using solid-state nuclear magnetic resonance (NMR) and Raman spectroscopies. Magic-angle spinning (MAS) was used to obtain high-resolution 13C and 1H-13C cross polarization (CP) NMR spectra. The 13C NMR chemical shifts are reported for bulk SWNTs, H2SO4-treated SWNTs, SWNT-Nafion polymer composites, SWNT-AQ55 polymer composites, and SWNTs in contact with water. Protonation occurs without irreversible oxidation of the nanotube substrate via a charge-transfer process. This is the first report of a chemically induced change in a SWNT 13C resonance brought about by a reversible interaction with an acidic proton, providing additional evidence that carbon nanotubes behave as weak bases. Cross polarization was found to be a powerful technique for providing an additional contrast mechanism for studying nanotubes in contact with other chemical species. The CP studies confirmed polarization transfer from nearby protons to nanotube carbon atoms. The CP technique was also applied to investigate water adsorbed on carbon nanotube surfaces. Finally, the degree of bundling of the SWNTs in Nafion films was probed with the 1H-13C CP-MAS technique. PMID:16332107

  10. Solid-state NMR studies of theophylline co-crystals with dicarboxylic acids.

    PubMed

    Pindelska, Edyta; Sokal, Agnieszka; Szeleszczuk, Lukasz; Pisklak, Dariusz Maciej; Kolodziejski, Waclaw

    2014-11-01

    In this work, three polycrystalline materials containing co-crystals of theophylline with malonic, maleic, and glutaric acids were studied using (13)C, (15)N and (1)H solid-state NMR and FT-IR spectroscopy. The NMR assignments were supported by gauge including projector augmented waves (GIPAW) calculations of chemical shielding, performed using X-ray determined geometry. The experimental (13)C cross polarization/magic angle spinning (CP/MAS) NMR results and the calculated isotropic chemical shifts were in excellent agreement. A rapid and convenient method for theophylline co-crystals crystal structure analysis has been proposed for co-crystals, which are potentially new APIs. PMID:25194346

  11. Lithium Polymer Electrolytes and Solid State NMR

    NASA Technical Reports Server (NTRS)

    Berkeley, Emily R.

    2004-01-01

    Research is being done at the Glenn Research Center (GRC) developing new kinds of batteries that do not depend on a solution. Currently, batteries use liquid electrolytes containing lithium. Problems with the liquid electrolyte are (1) solvents used can leak out of the battery, so larger, more restrictive, packages have to be made, inhibiting the diversity of application and decreasing the power density; (2) the liquid is incompatible with the lithium metal anode, so alternative, less efficient, anodes are required. The Materials Department at GRC has been working to synthesize polymer electrolytes that can replace the liquid electrolytes. The advantages are that polymer electrolytes do not have the potential to leak so they can be used for a variety of tasks, small or large, including in the space rover or in space suits. The polymers generated by Dr. Mary Ann Meador's group are in the form of rod -coil structures. The rod aspect gives the polymer structural integrity, while the coil makes it flexible. Lithium ions are used in these polymers because of their high mobility. The coils have repeating units of oxygen which stabilize the positive lithium by donating electron density. This aids in the movement of the lithium within the polymer, which contributes to higher conductivity. In addition to conductivity testing, these polymers are characterized using DSC, TGA, FTIR, and solid state NMR. Solid state NMR is used in classifying materials that are not soluble in solvents, such as polymers. The NMR spins the sample at a magic angle (54.7') allowing the significant peaks to emerge. Although solid state NMR is a helpful technique in determining bonding, the process of preparing the sample and tuning it properly are intricate jobs that require patience; especially since each run takes about six hours. The NMR allows for the advancement of polymer synthesis by showing if the expected results were achieved. Using the NMR, in addition to looking at polymers, allows for

  12. Solid-state diffusion in amorphous zirconolite

    SciTech Connect

    Yang, C.; Dove, M. T.; Trachenko, K.; Zarkadoula, E.; Todorov, I. T.; Geisler, T.; Brazhkin, V. V.

    2014-11-14

    We discuss how structural disorder and amorphization affect solid-state diffusion, and consider zirconolite as a currently important case study. By performing extensive molecular dynamics simulations, we disentangle the effects of amorphization and density, and show that a profound increase of solid-state diffusion takes place as a result of amorphization. Importantly, this can take place at the same density as in the crystal, representing an interesting general insight regarding solid-state diffusion. We find that decreasing the density in the amorphous system increases pre-factors of diffusion constants, but does not change the activation energy in the density range considered. We also find that atomic species in zirconolite are affected differently by amorphization and density change. Our microscopic insights are relevant for understanding how solid-state diffusion changes due to disorder and for building predictive models of operation of materials to be used to encapsulate nuclear waste.

  13. Standards Development for Solid-State Lighting

    SciTech Connect

    2011-12-16

    To accelerate the development and implementation of needed standards for solid-state lighting products, DOE works closely with a network of standards-setting organizations and offers technical assistance and support

  14. Solid-state light sources getting smart.

    PubMed

    Schubert, E Fred; Kim, Jong Kyu

    2005-05-27

    More than a century after the introduction of incandescent lighting and half a century after the introduction of fluorescent lighting, solid-state light sources are revolutionizing an increasing number of applications. Whereas the efficiency of conventional incandescent and fluorescent lights is limited by fundamental factors that cannot be overcome, the efficiency of solid-state sources is limited only by human creativity and imagination. The high efficiency of solid-state sources already provides energy savings and environmental benefits in a number of applications. However, solid-state sources also offer controllability of their spectral power distribution, spatial distribution, color temperature, temporal modulation, and polarization properties. Such "smart" light sources can adjust to specific environments and requirements, a property that could result in tremendous benefits in lighting, automobiles, transportation, communication, imaging, agriculture, and medicine. PMID:15919985

  15. Concepts for future solid state lighting solutions

    NASA Astrophysics Data System (ADS)

    von Malm, N.; Wirth, R.; Illek, S.; Steegmüller, U.

    2010-08-01

    In this contribution the relevant technological aspects of LED-based lamps for solid state lighting are discussed. In addition to general energy efficiency considerations improvements in LED chip technology and white light generation are presented.

  16. Solution and Solid State Nuclear Magnetic Resonance Spectroscopic Characterization of Efavirenz.

    PubMed

    Sousa, Eduardo Gomes Rodrigues de; Carvalho, Erika Martins de; San Gil, Rosane Aguiar da Silva; Santos, Tereza Cristina Dos; Borré, Leandro Bandeira; Santos-Filho, Osvaldo Andrade; Ellena, Javier

    2016-09-01

    Samples of efavirenz (EFZ) were evaluated to investigate the influence of the micronization process on EFZ stability. A combination of X-ray diffraction, thermal analysis, FTIR, observations of isotropic chemical shifts of (1)H in distinct solvents, their temperature dependence and spin-lattice relaxation time constants (T1), solution (1D and 2D) (13)C nuclear magnetic resonance (NMR), and solid-state (13)C NMR (CPMAS NMR) provides valuable structural information and structural elucidation of micronized EFZ and heptane-recrystallized polymorphs (EFZ/HEPT). This study revealed that the micronization process did not affect the EFZ crystalline structure. It was observed that the structure of EFZ/HEPT is in the same form as that obtained from ethyl acetate/hexane, as shown in the literature. A comparison of the solid-state NMR spectra revealed discrepancies regarding the assignments of some carbons published in the literature that have been resolved. PMID:26886313

  17. Grating enhanced solid-state laser amplifiers

    DOEpatents

    Erlandson, Alvin C.; Britten, Jerald A.

    2010-11-09

    A novel method and apparatus for suppressing ASE and parasitic oscillation modes in a high average power laser is introduced. Such an invention, as disclosed herein, uses diffraction gratings to increase gain, stored energy density, and pumping efficiency of solid-state laser gain media, such as, but not limited to rods, disks and slabs. By coupling predetermined gratings to solid-state gain media, such as crystal or ceramic laser gain media, ASE and parasitic oscillation modes can be effectively suppressed.

  18. Parallel β-Sheet Structure of Alanine Tetrapeptide in the Solid State As Studied by Solid-State NMR Spectroscopy.

    PubMed

    Asakura, Tetsuo; Horiguchi, Kumiko; Aoki, Akihiro; Tasei, Yugo; Naito, Akira

    2016-09-01

    The structural analysis of alanine oligopeptides is important for understanding the crystalline region in silks from spiders and wild silkworms and also the mechanism of cellular toxicity of human diseases arising from expansion in polyalanine sequences. The atomic-level structures of alanine tripeptide and tetrapeptide with antiparallel β-sheet structures (AP-Ala3 and AP-Ala4, respectively) together with alanine tripeptide with parallel β-sheet structures (P-Ala3) have been determined, but alanine tetrapeptide with a parallel β-sheet structure (P-Ala4) has not been reported yet. In this article, first, we established the preparation protocol of P-Ala4 from more stable AP-Ala4. Second, complete assignments of the (13)C, (15)N, and (1)H solid-state NMR spectra were performed with (13)C- and (15)N-labeled Ala4 samples using several solid-state NMR techniques. Then, the structural constraints were obtained, for example, the amide proton peaks of P-Ala4 in the (1)H double-quantum magic-angle spinning NMR spectrum were heavily overlapped and observed at about 7.4 ppm, which was a much higher field than that of 8.7-9.1 ppm observed for AP-Ala4, indicating that the intermolecular hydrogen-bond lengths across strands (N-H···O═C) were considerably longer for P-Ala4, that is, 2.21-2.34 Å, than those reported for AP-Ala4, that is, 1.8-1.9 Å. The structural model was proposed for P-Ala4 by NMR results and MD calculations. PMID:27482868

  19. Measurements of 13C multiple-quantum coherences in amyloid fibrils under magic-angle spinning.

    PubMed

    Chou, Fang-Chieh; Tsai, Tim W T; Cheng, Hsin-Mei; Chan, Jerry C C

    2012-06-21

    The excitation and detection of high-order multiple quantum coherences among (13)C nuclear spins are demonstrated in the samples of [1-(13)C]-L-alanine and (13)C labeled amyloid fibrils at a spinning frequency of 20 kHz. The technique is based on the double-quantum average Hamiltonian prepared by the DRAMA-XY4 pulse sequence. Empirically, we find that multiple supercycles are required to suppress the higher-order effects for real applications. Measurements for the fibril samples formed by the polypeptides of PrP(113-127) provide the first solid-state NMR evidence for the stacking of multiple β-sheet layers at the structural core of amyloid fibrils. PMID:22632418

  20. Magnetic susceptibility effects on 13C MAS NMR spectra of carbon materials and graphite.

    PubMed

    Freita, J C; Emmerich, F G; Cernicchiaro, G R; Sampaio, L C; Bonagamba, T J

    2001-01-01

    13C high-resolution solid-state nuclear magnetic resonance (NMR) was employed to study carbon materials prepared through the thermal decomposition of four different organic precursors (rice hulls, endocarp of babassu coconut, peat, and PVC). For heat treatment temperatures (HTTs) above about 600 C, all materials presented 13C NMR spectra composed of a unique resonance line associated with carbon atoms in aromatic planes. With increasing HTT a continuous broadening of this resonance and a diamagnetic shift in its central frequency were verified for all samples. The evolution of the magnitude and anisotropy of the magnetic susceptibility of the heat-treated carbon samples with HTT explains well these findings. It is shown that these results are better understood when a comparison is made with the features of the 13C NMR spectrum of polycrystalline graphite, for which the magnetic susceptibility effect is also present and is much more pronounced. PMID:11529420

  1. Analysis of hyperpolarized dynamic 13C lactate imaging in a transgenic mouse model of prostate cancer☆

    PubMed Central

    Lupo, Janine M.; Chen, Albert P.; Zierhut, Matthew L.; Bok, Robert A.; Cunningham, Charles H.; Kurhanewicz, John; Vigneron, Daniel B.; Nelson, Sarah J.

    2011-01-01

    This study investigated the application of an acquisition that selectively excites the [1-13C]lactate resonance and allows dynamic tracking of the conversion of 13C-lactate from hyperpolarized 13C-pyruvate at a high spatial resolution. In order to characterize metabolic processes occurring in a mouse model of prostate cancer, 20 sequential 3D images of 13C-lactate were acquired 5 s apart using a pulse sequence that incorporated a spectral–spatial excitation pulse and a flyback echo-planar readout to track the time course of newly converted 13C-lactate after injection of prepolarized 13C-pyruvate. The maximum lactate signal (MLS), full-width half-maximum (FWHM), time to the peak 13C-lactate signal (TTP) and area under the dynamic curve were calculated from the dynamic images of 10 TRAMP mice and two wild-type controls. The regional variation in 13C-lactate associated with the injected pyruvate was demonstrated by the peak of the 13C-lactate signal occurring earlier in the kidney than in the tumor region. The intensity of the dynamic 13C-lactate curves also varied spatially within the tumor, illustrating the heterogeneity in metabolism that was most prominent in more advanced stages of disease development. The MLS was significantly higher in TRAMP mice that had advanced disease. PMID:19695815

  2. Diamond deposition and defect chemistry studied via solid state NMR

    NASA Astrophysics Data System (ADS)

    Gleason, Karen K.

    1994-06-01

    Diamond defects were quantified by nuclear magnetic resonance (NMR). While maintaining the macroscopic integrity of the films, concentrations between 0.001 and 1.0 at.% H were measured, among the lowest ever reported by solid-state 1H NMR. These concentrations were correlated to infrared absorption in the 8 to 10 micron region and to thermal conductivity. Despite the low concentrations, Multiple Quantum NMR reveals a high degree of hydrogen clustering consistent with grain boundary passivation. Most hydrogen is rigidly held, but some, probably in -OCH3 and -NCH3 defects, undergoes rotation at room temperature. Similar results were obtained for hot-filament, microwave-plasma and DC arc-jet films, suggesting a common surface chemistry, but no hydrogen was detected in an as-deposited combustion film. 13C NMR provided the first quantitative determination of non-diamond bonded carbon defects, providing a benchmark for Raman spectroscopy, the primary characterization method for diamond. Selective 13C labeling demonstrated heterogeneous reactions involving carbon occur at the hot-filament. With high-speed magic-angle-spinning 19F NMR, CFx (x=1-3) functionalities were resolved on the surface of plasma-treated diamond powder. Understanding these defects impacts the understanding of film growth mechanisms and structure-property relationships for CVD diamond.

  3. Solid state ionics 3. Materials Research Society Symposium Proceedings, volume 293

    NASA Astrophysics Data System (ADS)

    Nazri, Gholam A.; Tarascon, Jean M.; Armand, Michel

    This proceedings volume includes most of the invited and contributed papers presented as Symposium U, Solid State Ionics, at the 1992 MRS Fall meeting in Boston, Massachusetts, U.S.A. The Symposium covered material aspects of solid state ionics, theory of ion transfer in solids, ionically and electronically conductive polymers and their application in solid state devices, and various in-situ and ex-situ techniques for materials characterization. The first part of this proceedings volume deals with physics and chemistry of insertion compounds and application of these in advanced solid state batteries. The optical and electrochemical properties of insertion compounds are also presented. The second part of the proceedings deals with ionic and electronic conductive polymers. A new class of rubbery phase polymer electrolytes and their structure-conductivity relationship are presented. Physical and chemical properties of polymer electrolytes and electrodes and their application in solid state devices are presented.

  4. Materials for solid state lighting

    SciTech Connect

    Johnson, S.G.; Simmons, J.A.

    2002-03-26

    Dramatic improvement in the efficiency of inorganic and organic light emitting diodes (LEDs and OLEDs) within the last decade has made these devices viable future energy efficient replacements for current light sources. However, both technologies must overcome major technical barriers, requiring significant advances in material science, before this goal can be achieved. Attention will be given to each technology associated with the following major areas of material research: (1) material synthesis, (2) process development, (3) device and defect physics, and (4) packaging. The discussion on material synthesis will emphasize the need for further development of component materials, including substrates and electrodes, necessary for improving device performance. The process technology associated with the LEDs and OLEDs is very different, but in both cases it is one factor limiting device performance. Improvements in process control and methodology are expected to lead to additional benefits of higher yield, greater reliability and lower costs. Since reliability and performance are critical to these devices, an understanding of the basic physics of the devices and device failure mechanisms is necessary to effectively improve the product. The discussion will highlight some of the more basic material science problems remaining to be solved. In addition, consideration will be given to packaging technology and the need for the development of novel materials and geometries to increase the efficiencies and reliability of the devices. The discussion will emphasize the performance criteria necessary to meet lighting applications, in order to illustrate the gap between current status and market expectations for future product.

  5. Structural analysis of geochemical samples by solid-state nuclear magnetic resonance spectrometry. Role of paramagnetic material

    USGS Publications Warehouse

    Vassallo, A.M.; Wilson, M.A.; Collin, P.J.; Oades, J.M.; Waters, A.G.; Malcolm, R.L.

    1987-01-01

    An examination of coals, coal tars, a fulvic acid, and soil fractions by solid-state 13C NMR spectrometry has demonstrated widely differing behavior regarding quantitative representation in the spectrum. Spin counting experiments on coal tars and the fulvic acid show that almost all the sample carbon is observed in both solution and solid-state NMR spectra. Similar experiments on two coals (a lignite and a bituminous coal) show that most (70-97%) of the carbon is observed; however, when the lignite is ion exchanged with 3% (w/w) Fe3+, the fraction of carbon observed drops to below 10%. In additional experiments signal intensity from soil samples is enhanced by a simple dithionite treatment. This is illustrated by 13C, 27Al, and 29Si solid-state NMR experiments on soil fractions. ?? 1987 American Chemical Society.

  6. Analysing Groundwater Using the 13C Isotope

    NASA Astrophysics Data System (ADS)

    Awad, Sadek

    The stable isotope of the carbon atom (13C) give information about the type of the mineralisation of the groundwater existing during the water seepage and about the recharge conditions of the groundwater. The concentration of the CO2(aq.) dissolved during the infiltration of the water through the soil's layers has an effect on the mineralisation of this water. The type of the photosynthesis's cycle (C-3 or C-4 carbon cycle) can have a very important role to determine the conditions (closed or open system) of the mineralisation of groundwater. The isotope 13C of the dissolved CO2 in water give us a certain information about the origin and the area of pollution of water. The proportion of the biogenic carbon and its percentage in the mineralisation of groundwater is determined by using the isotope 13C.

  7. States of 13C with abnormal radii

    NASA Astrophysics Data System (ADS)

    Demyanova, A. S.; Ogloblin, A. A.; Danilov, A. N.; Goncharov, S. A.; Belyaeva, T. L.; Sobolev, Yu. G.; Khlebnikov, S. V.; Burtebaev, N.; Trzaska, W.; Heikkinen, P.; Tyurin, G. P.; Janseitov, D.; Gurov, Yu. B.

    2016-05-01

    Differential cross-sections of the elastic and inelastic 13C + α scattering were measured at E(α) = 90 MeV. The root mean-square radii() of 13C nucleus in the states: 8.86 (1/2-), 3.09 (1/2+) and 9.90 (3/2-) MeV were determined by the Modified diffraction model (MDM). The radii of the first two levels are enhanced compared to that of the ground state of 13C, confirming the suggestion that the 8.86 MeV state is an analogue of the Hoyle state in 12C and the 3.09 MeV state has a neutron halo. Some indications to the abnormally small size of the 9.90 MeV state were obtained.

  8. Scaling of solid state lasers for satellite power beaming applications

    SciTech Connect

    Friedman, H.; Albrecht, G.; Beach, R.

    1994-12-31

    The power requirements for a satellite power beaming laser system depend upon the diameter of the beam director, the performance of the adaptive optics system, and the mission requirements. For an 8 meter beam director and overall Strehl ratio of 50%, a 30 kW laser at 850 nm can deliver an equivalent solar flux to a satellite at geostationary orbit. Advances in Diode Pumped Solid State Lasers (DPSSL) have brought these small, efficient and reliable devices to high average power and they should be considered for satellite power beaming applications. Two solid state systems are described: a diode pumped Alexandrite and diode pumped Thulium doped YAG. Both can deliver high average power at 850 nm in a single aperture.

  9. Scaling of solid state lasers for satellite power beaming applications

    SciTech Connect

    Friedman, H.W.; Albrecht, G.F.; Beach, R.J.

    1994-01-01

    The power requirements for a satellite power beaming laser system depend upon the diameter of the beam director, the performance of the adaptive optics system, and the mission requirements. For an 8 meter beam director and overall Strehl ratio of 50%, a 30 kW laser at 850 nm can deliver an equivalent solar flux to a satellite at geostationary orbit. Advances in Diode Pumped Solid State Lasers (DPSSL) have brought these small, efficient and reliable devices to high average power and they should be considered for satellite power beaming applications. Two solid state systems are described: a diode pumped Alexandrite and diode pumped Thulium doped YAG. Both can deliver high average power at 850 nm in a single aperture.

  10. Compact Solid State Cooling Systems: Compact MEMS Electrocaloric Module

    SciTech Connect

    2010-10-01

    BEETIT Project: UCLA is developing a novel solid-state cooling technology to translate a recent scientific discovery of the so-called giant electrocaloric effect into commercially viable compact cooling systems. Traditional air conditioners use noisy, vapor compression systems that include a polluting liquid refrigerant to circulate within the air conditioner, absorb heat, and pump the heat out into the environment. Electrocaloric materials achieve the same result by heating up when placed within an electric field and cooling down when removed—effectively pumping heat out from a cooler to warmer environment. This electrocaloric-based solid state cooling system is quiet and does not use liquid refrigerants. The innovation includes developing nano-structured materials and reliable interfaces for heat exchange. With these innovations and advances in micro/nano-scale manufacturing technologies pioneered by semiconductor companies, UCLA is aiming to extend the performance/reliability of the cooling module.

  11. A review of lithium and non-lithium based solid state batteries

    NASA Astrophysics Data System (ADS)

    Kim, Joo Gon; Son, Byungrak; Mukherjee, Santanu; Schuppert, Nicholas; Bates, Alex; Kwon, Osung; Choi, Moon Jong; Chung, Hyun Yeol; Park, Sam

    2015-05-01

    Conventional lithium-ion liquid-electrolyte batteries are widely used in portable electronic equipment such as laptop computers, cell phones, and electric vehicles; however, they have several drawbacks, including expensive sealing agents and inherent hazards of fire and leakages. All solid state batteries utilize solid state electrolytes to overcome the safety issues of liquid electrolytes. Drawbacks for all-solid state lithium-ion batteries include high resistance at ambient temperatures and design intricacies. This paper is a comprehensive review of all aspects of solid state batteries: their design, the materials used, and a detailed literature review of various important advances made in research. The paper exhaustively studies lithium based solid state batteries, as they are the most prevalent, but also considers non-lithium based systems. Non-lithium based solid state batteries are attaining widespread commercial applications, as are also lithium based polymeric solid state electrolytes. Tabular representations and schematic diagrams are provided to underscore the unique characteristics of solid state batteries and their capacity to occupy a niche in the alternative energy sector.

  12. Millimeter and submillimeter wave spectra of 13C-glycolaldehydes

    NASA Astrophysics Data System (ADS)

    Haykal, I.; Motiyenko, R. A.; Margulès, L.; Huet, T. R.

    2013-01-01

    Context. Glycolaldehyde (CH2OHCHO) is the simplest sugar and an important intermediate in the path toward forming more complex biologically relevant molecules. Astronomical surveys of interstellar molecules, such as those available with the very sensitive ALMA telescope, require preliminary laboratory investigations of the microwave and submillimeter-wave spectra of molecular species including new isotopologs - to identify these in the interstellar media. Aims: To achieve the detection of the 13C isotopologs of glycolaldehyde in the interstellar medium, their rotational spectra in the millimeter and submillimeter-wave regions were studied. Methods: The spectra of 13CH2OHCHO and CH2OH13CHO were recorded in the 150-945 GHz spectral range in the laboratory using a solid-state submillimeter-wave spectrometer in Lille. The observed line frequencies were measured with an accuracy of 30 kHz up to 700 GHz and of 50 kHz above 700 GHz. We analyzed the spectra with a standard Watson Hamiltonian. Results: About 10 000 new lines were identified for each isotopolog. The spectroscopic parameters were determined for the ground- and the three lowest vibrational states up to 945 and 630 GHz. Previous microwave assignments of 13CH2OHCHO were not confirmed. Conclusions: The provided line-lists and sets of molecular parameters meet the needs for a first astrophysical search of 13C-glycolaldehydes. Full Tables 3 and 4 are only available at the CDS via anonymous ftp to cdsarc.u-strasbg.fr (130.79.128.5) or via http://cdsarc.u-strasbg.fr/viz-bin/qcat?J/A+A/549/A96

  13. Driver circuit for solid state light sources

    DOEpatents

    Palmer, Fred; Denvir, Kerry; Allen, Steven

    2016-02-16

    A driver circuit for a light source including one or more solid state light sources, a luminaire including the same, and a method of so driving the solid state light sources are provided. The driver circuit includes a rectifier circuit that receives an alternating current (AC) input voltage and provides a rectified AC voltage. The driver circuit also includes a switching converter circuit coupled to the light source. The switching converter circuit provides a direct current (DC) output to the light source in response to the rectified AC voltage. The driver circuit also includes a mixing circuit, coupled to the light source, to switch current through at least one solid state light source of the light source in response to each of a plurality of consecutive half-waves of the rectified AC voltage.

  14. Is solid state the future of lighting?

    NASA Astrophysics Data System (ADS)

    Kirkpatrick, Douglas A.

    2004-01-01

    The rapid pace of solid state technological development over the past four decades has resulted in almost universal acceptance of the phrase "Moore's Law," whether it is used accurately to refer to the exponential increase in computer processor power or to refer to some more amorphous scope of rapid change. More recent breakthroughs in LED science and engineering have precipitated a vigorous discussion of the depth and pace with which solid state light sources will penetrate the $50-billion world-wide lighting market. This discussion has not two perspectives but many, and each perspective can provide valuable insight into key issues that will determine the role that solid state technology will play in the lighting market of 2020 and beyond.

  15. Solid state recording current meter conversion

    USGS Publications Warehouse

    Cheng, Ralph T.; Wang, Lichen

    1985-01-01

    The authors describe the conversion of an Endeco-174 current meter to a solid-state recording current meter. A removable solid-state module was designed to fit in the space originally occupied by an 8-track tape cartridge. The module contains a CPU and 128 kilobytes of nonvolatile CMOS memory. The solid-state module communicates with any terminal or computer using an RS-232C interface at 4800 baud rate. A primary consideration for conversion was to keep modifications of the current meter to a minimum. The communication protocol was designed to emulate the Endeco tape translation unit, thus the need for a translation unit was eliminated and the original data reduction programs can be used without any modification. After conversion, the data recording section of the current meter contains no moving parts; the storage capacity of the module is equivalent to that of the original tape cartridge.

  16. Protect motors with solid-state overloads

    SciTech Connect

    Forsell, K.A. )

    1993-03-01

    Magnetic motor starters that rely on bimetal or melting alloy overload protection do not provide the flexibility of solid-state overload technology. The point is best illustrated by the number of different overload relay trip curves that describe tripping time as a function of motor current. Solid-state overloads have a trip curve for a cold start with three-phase current, and a family of trip curves for three-phase conditions where the overload and motor are already warm. An overload relay can also be described by its single-phase trip-time curves for cold and warm initial states. All thermal overloads have single phase trip curves that are similar in shape to their three-phase curves. Slower response to phase loss for motor loads less than locked rotor is inherent in thermal overload relay design. The paper describes the power source problem; single-phase problems; thermal overloads versus solid state; and thermal NEMA overload.

  17. Monolithic solid-state lasers for spaceflight

    NASA Astrophysics Data System (ADS)

    Krainak, Michael A.; Yu, Anthony W.; Stephen, Mark A.; Merritt, Scott; Glebov, Leonid; Glebova, Larissa; Ryasnyanskiy, Aleksandr; Smirnov, Vadim; Mu, Xiaodong; Meissner, Stephanie; Meissner, Helmuth

    2015-02-01

    A new solution for building high power, solid state lasers for space flight is to fabricate the whole laser resonator in a single (monolithic) structure or alternatively to build a contiguous diffusion bonded or welded structure. Monolithic lasers provide numerous advantages for space flight solid-state lasers by minimizing misalignment concerns. The closed cavity is immune to contamination. The number of components is minimized thus increasing reliability. Bragg mirrors serve as the high reflector and output coupler thus minimizing optical coatings and coating damage. The Bragg mirrors also provide spectral and spatial mode selection for high fidelity. The monolithic structure allows short cavities resulting in short pulses. Passive saturable absorber Q-switches provide a soft aperture for spatial mode filtering and improved pointing stability. We will review our recent commercial and in-house developments toward fully monolithic solid-state lasers.

  18. Scalar operators in solid-state NMR

    SciTech Connect

    Sun, Boqin

    1991-11-01

    Selectivity and resolution of solid-state NMR spectra are determined by dispersion of local magnetic fields originating from relaxation effects and orientation-dependent resonant frequencies of spin nuclei. Theoretically, the orientation-dependent resonant frequencies can be represented by a set of irreducible tensors. Among these tensors, only zero rank tensors (scalar operators) are capable of providing high resolution NMR spectra. This thesis presents a series of new developments in high resolution solid-state NMR concerning the reconstruction of various scalar operators motion in solid C{sub 60} is analyzed.

  19. Solid State Lasers from an Efficiency Perspective

    NASA Technical Reports Server (NTRS)

    Barnes, Norman P.

    2007-01-01

    Solid state lasers have remained a vibrant area of research because several major innovations expanded their capability. Major innovations are presented with emphasis focused on the laser efficiency. A product of efficiencies approach is developed and applied to describe laser performance. Efficiency factors are presented in closed form where practical and energy transfer effects are included where needed. In turn, efficiency factors are used to estimate threshold and slope efficiency, allowing a facile estimate of performance. Spectroscopic, thermal, and mechanical data are provided for common solid state laser materials.

  20. Solid State Joining of Dissimilar Titanium Alloys

    NASA Astrophysics Data System (ADS)

    Morton, Todd W.

    Solid state joining of titanium via friction stir welding and diffusion bonding have emerged as enablers of efficient monolithic structural designs by the eliminations fasteners for the aerospace industry. As design complexity and service demands increase, the need for joints of dissimilar alloys has emerged. Complex thermomechanical conditions in friction stir weld joints and high temperature deformation behavior differences between alloys used in dissimilar joints gives rise to a highly variable flow pattern within a stir zone. Experiments performed welding Ti-6Al-4V to beta21S show that mechanical intermixing of the two alloys is the primary mechanism for the generation of the localized chemistry and microstructure, the magnitude of which can be directly related to pin rotation and travel speed weld parameters. Mechanical mixing of the two alloys is heavily influenced by strain rate softening phenomena, and can be used to manipulate weld nugget structure by switching which alloy is subjected to the advancing side of the pin. Turbulent mixing of a weld nugget and a significant reduction in defects and weld forces are observed when the beta21S is put on the advancing side of the weld where higher strain rates are present. Chemical diffusion driven by the heat of weld parameters is characterized using energy dispersive x-ray spectroscopy (EDS) and is shown to be a secondary process responsible for generating short-range chemical gradients that lead to a gradient of alpha particle structures. Diffusion calculations are inconsistent with an assumption of steady-state diffusion and show that material interfaces in the weld nugget evolve through the break-down of turbulent interface features generated by material flows. A high degree of recrystallization is seen throughout the welds, with unique, hybrid chemistry grains that are generated at material interfaces in the weld nugget that help to unify the crystal structure of dissimilar alloys. The degree of

  1. Synthesis Of [2h, 13c] And [2h3, 13c]Methyl Aryl Sulfides

    DOEpatents

    Martinez, Rodolfo A.; Alvarez, Marc A.; Silks, III, Louis A.; Unkefer, Clifford J.

    2004-03-30

    The present invention is directed to labeled compounds, [.sup.2 H.sub.1, .sup.13 C], [.sup.2 H.sub.2, .sup.13 C] and [.sup.2 H.sub.3, .sup.13 C]methyl aryl sulfides wherein the .sup.13 C methyl group attached to the sulfur of the sulfide includes exactly one, two or three deuterium atoms and the aryl group is selected from the group consisting of 1-naphthyl, substituted 1-naphthyl, 2-naphthyl, substituted 2-naphthyl, and phenyl groups with the structure ##STR1## wherein R.sub.1, R.sub.2, R.sub.3, R.sub.4, and R.sub.5 are each independently, hydrogen, a C.sub.1 -C.sub.4 lower alkyl, a halogen, an amino group from the group consisting of NH.sub.2, NHR and NRR' where R and R' are each a C.sub.1 -C.sub.4 lower alkyl, a phenyl, or an alkoxy group. The present invention is also directed to processes of preparing [.sup.2 H.sub.1, .sup.13 C], [.sup.2 H.sub.2,.sup.13 C] and [.sup.2 H.sub.3, .sup.13 C]methyl aryl sulfides wherein the .sup.13 C methyl group attached to the sulfur of the sulfide includes exactly one, two or three deuterium atoms. The present invention is also directed to the labeled compounds of [.sup.2 H.sub.1, .sup.13 C]methyl iodide and [.sup.2 H.sub.2, .sup.13 C]methyl iodide.

  2. Dynamic nuclear polarization of carbonyl and methyl 13C spins in acetate using trityl OX063

    NASA Astrophysics Data System (ADS)

    Niedbalski, Peter; Parish, Christopher; Lumata, Lloyd

    2015-03-01

    Hyperpolarization via dissolution dynamic nuclear polarization (DNP) is a physics technique that amplifies the magnetic resonance signals by several thousand-fold for biomedical NMR spectroscopy and imaging (MRI). Herein we have investigated the effect of carbon-13 isotopic location on the DNP of acetate (one of the biomolecules commonly used for hyperpolarization) at 3.35 T and 1.4 K using a narrow ESR linewidth free radical trityl OX063. We have found that the carbonyl 13C spins yielded about twice the polarization produced in methyl 13C spins. Deuteration of the methyl group, beneficial in the liquid-state, did not produce an improvement in the polarization level at cryogenic conditions. Concurrently, the solid-state nuclear relaxation of these samples correlate with the polarization levels achieved. These results suggest that the location of the 13C isotopic labeling in acetate has a direct impact on the solid-state polarization achieved and is mainly governed by the nuclear relaxation leakage factor.

  3. Solid-state NMR imaging system

    DOEpatents

    Gopalsami, Nachappa; Dieckman, Stephen L.; Ellingson, William A.

    1992-01-01

    An apparatus for use with a solid-state NMR spectrometer includes a special imaging probe with linear, high-field strength gradient fields and high-power broadband RF coils using a back projection method for data acquisition and image reconstruction, and a real-time pulse programmer adaptable for use by a conventional computer for complex high speed pulse sequences.

  4. Technique for improving solid state mosaic images

    NASA Technical Reports Server (NTRS)

    Saboe, J. M.

    1969-01-01

    Method identifies and corrects mosaic image faults in solid state visual displays and opto-electronic presentation systems. Composite video signals containing faults due to defective sensing elements are corrected by a memory unit that contains the stored fault pattern and supplies the appropriate fault word to the blanking circuit.

  5. Self-protecting solid state isolated switch

    NASA Technical Reports Server (NTRS)

    Hoffman, A. C.; Gooder, S. T.

    1974-01-01

    Solid state switch has following capabilities: (1) Hybrid or IC from compatible with direct mounting on solar array substrate; (2) Continuous signal is not required to hold it in either on or off state; (3) Separate signal lines for on and off control; (4) Electrically isolated from input signals; and (5) Current surges will not cause switch failure.

  6. Solar-pumped solid state Nd lasers

    NASA Technical Reports Server (NTRS)

    Williams, M. D.; Zapata, L.

    1985-01-01

    Solid state neodymium lasers are considered candidates for space-based polar-pumped laser for continuous power transmission. Laser performance for three different slab laser configurations has been computed to show the excellent power capability of such systems if heat problems can be solved. Ideas involving geometries and materials are offered as potential solutions to the heat problem.

  7. Solid-state NMR for bacterial biofilms

    NASA Astrophysics Data System (ADS)

    Reichhardt, Courtney; Cegelski, Lynette

    2014-04-01

    Bacteria associate with surfaces and one another by elaborating an extracellular matrix to encapsulate cells, creating communities termed biofilms. Biofilms are beneficial in some ecological niches, but also contribute to the pathogenesis of serious and chronic infectious diseases. New approaches and quantitative measurements are needed to define the composition and architecture of bacterial biofilms to help drive the development of strategies to interfere with biofilm assembly. Solid-state nuclear magnetic resonance (NMR) is uniquely suited to the examination of insoluble and complex macromolecular and whole-cell systems. This article highlights three examples that implement solid-state NMR to deliver insights into bacterial biofilm composition and changes in cell-wall composition as cells transition to the biofilm lifestyle. Most recently, solid-state NMR measurements provided a total accounting of the protein and polysaccharide components in the extracellular matrix of an Escherichia coli biofilm and transformed our qualitative descriptions of matrix composition into chemical parameters that permit quantitative comparisons among samples. We present additional data for whole biofilm samples (cells plus the extracellular matrix) that complement matrix-only analyses. The study of bacterial biofilms by solid-state NMR is an exciting avenue ripe with many opportunities and we close the article by articulating some outstanding questions and future directions in this area.

  8. Solid-state NMR imaging system

    SciTech Connect

    Gopalsami, N.; Dieckman, S.L.; Ellingson, W.A.

    1990-01-01

    An accessory for use with a solid-state NMR spectrometer includes a special imaging probe with linear, high-field strength gradient fields and high-power broadband RF coils using a back projection method for data acquisition and image reconstruction, and a real-time pulse programmer adaptable for use by a conventional computer for complex high speed pulse sequences.

  9. Density functional theory in the solid state

    PubMed Central

    Hasnip, Philip J.; Refson, Keith; Probert, Matt I. J.; Yates, Jonathan R.; Clark, Stewart J.; Pickard, Chris J.

    2014-01-01

    Density functional theory (DFT) has been used in many fields of the physical sciences, but none so successfully as in the solid state. From its origins in condensed matter physics, it has expanded into materials science, high-pressure physics and mineralogy, solid-state chemistry and more, powering entire computational subdisciplines. Modern DFT simulation codes can calculate a vast range of structural, chemical, optical, spectroscopic, elastic, vibrational and thermodynamic phenomena. The ability to predict structure–property relationships has revolutionized experimental fields, such as vibrational and solid-state NMR spectroscopy, where it is the primary method to analyse and interpret experimental spectra. In semiconductor physics, great progress has been made in the electronic structure of bulk and defect states despite the severe challenges presented by the description of excited states. Studies are no longer restricted to known crystallographic structures. DFT is increasingly used as an exploratory tool for materials discovery and computational experiments, culminating in ex nihilo crystal structure prediction, which addresses the long-standing difficult problem of how to predict crystal structure polymorphs from nothing but a specified chemical composition. We present an overview of the capabilities of solid-state DFT simulations in all of these topics, illustrated with recent examples using the CASTEP computer program. PMID:24516184

  10. SPS solid state antenna power combiner

    NASA Technical Reports Server (NTRS)

    Fitzsimmons, G. W.

    1980-01-01

    Solid state dc-rf converters offer potential improvements in reliability, mass and low voltage operation, provided that anticipated efficiencies in excess of 80 percent can be realized. Field effect transistors offer the greatest potential in the SPS frequency band at 2.45 GHz. To implement this approach it is essential that means be found to sum the power of many relatively low power solid state sources in a low-loss manner, and that means be provided to properly control the phase of the outputs of the large number of solid state sources required. To avoid the power combining losses associated with circuit hybrids it was proposed that the power from multiple solid state amplifiers be combined by direct coupling of each amplifier's output to the radiating antenna structure. The selected power-combining antenna consists of a unique printed (metalized) microstrip circuit on a ceramic type dielectric substrate which is backed by a shallow lightweight aluminum cavity which sums the power of four microwave sources. The antenna behaves like two one-half wavelength slot-line antennas coupled together via their common cavity structure.

  11. Solid state, S-band, power amplifier

    NASA Technical Reports Server (NTRS)

    Digrindakis, M.

    1973-01-01

    The final design and specifications for a solid state, S-band, power amplifier is reported. Modifications from a previously proposed design were incorporated to improve efficiency and meet input overdrive and noise floor requirements. Reports on the system design, driver amplifier, power amplifier, and voltage and current limiter are included along with a discussion of the testing program.

  12. Light activated solid-state opening switches

    SciTech Connect

    Petr, R.A.; Kachen, G.I.; Reilly, J.P.; Schaefer, R.B. ); Heyse, M.W. )

    1993-01-01

    Light-activated solid-state opening switches are shown to be a viable approach for switching inductive circuits. Measured photoswitch performance indicates that light-activated opening switches have the power density ratings needed to develop compact inductive power systems.

  13. Light activated solid-state opening switches

    NASA Astrophysics Data System (ADS)

    Petr, R. A.; Kachen, G. I.; Reilly, J. P.; Schaefer, R. B.; Heyse, M. W.

    1993-01-01

    The paper shows light-activated solid-state opening switches to be a viable approach for switching inductive circuits. Measured photoswitch performance indicates that light-activated opening switches have the power density ratings required to develop compact inductive power systems.

  14. Coordinated garbage collection for raid array of solid state disks

    DOEpatents

    Dillow, David A; Ki, Youngjae; Oral, Hakki S; Shipman, Galen M; Wang, Feiyi

    2014-04-29

    An optimized redundant array of solid state devices may include an array of one or more optimized solid-state devices and a controller coupled to the solid-state devices for managing the solid-state devices. The controller may be configured to globally coordinate the garbage collection activities of each of said optimized solid-state devices, for instance, to minimize the degraded performance time and increase the optimal performance time of the entire array of devices.

  15. On The Potential of Dynamic Nuclear Polarization Enhanced Diamonds in Solid-State and Dissolution (13) C NMR Spectroscopy.

    PubMed

    Bretschneider, Christian O; Akbey, Ümit; Aussenac, Fabien; Olsen, Greg L; Feintuch, Akiva; Oschkinat, Hartmut; Frydman, Lucio

    2016-09-01

    Dynamic nuclear polarization (DNP) is a versatile option to improve the sensitivity of NMR and MRI. This versatility has elicited interest for overcoming potential limitations of these techniques, including the achievement of solid-state polarization enhancement at ambient conditions, and the maximization of (13) C signal lifetimes for performing in vivo MRI scans. This study explores whether diamond's (13) C behavior in nano- and micro-particles could be used to achieve these ends. The characteristics of diamond's DNP enhancement were analyzed for different magnetic fields, grain sizes, and sample environments ranging from cryogenic to ambient temperatures, in both solution and solid-state experiments. It was found that (13) C NMR signals could be boosted by orders of magnitude in either low- or room-temperature solid-state DNP experiments by utilizing naturally occurring paramagnetic P1 substitutional nitrogen defects. We attribute this behavior to the unusually long electronic/nuclear spin-lattice relaxation times characteristic of diamond, coupled with a time-independent cross-effect-like polarization transfer mechanism facilitated by a matching of the nitrogen-related hyperfine coupling and the (13) C Zeeman splitting. The efficiency of this solid-state polarization process, however, is harder to exploit in dissolution DNP-enhanced MRI contexts. The prospects for utilizing polarized diamond approaching nanoscale dimensions for both solid and solution applications are briefly discussed. PMID:27416769

  16. Mid-infrared solid-state lasers and laser materials

    NASA Technical Reports Server (NTRS)

    Barnes, Norman P.; Byvik, Charles E.

    1988-01-01

    An account is given of NASA-Langley's objectives for the development of advanced lasers and laser materials systems applicable to remote sensing in the mid-IR range. Prominent among current concerns are fiber-optic spectroscopy, eye-safe solid-state lasers for both Doppler sensing and mid-IR wavelength-generation laser pumping, and nonlinear optics generating tunable mid-IR radiation. Ho:YAG lasers are noted to exhibit intrinsic advantages for the desired applications, and are pumpable by GaAlAs laser diodes with a quantum efficiency approaching 2.

  17. Accurate determinations of one-bond 13C-13C couplings in 13C-labeled carbohydrates

    NASA Astrophysics Data System (ADS)

    Azurmendi, Hugo F.; Freedberg, Darón I.

    2013-03-01

    Carbon plays a central role in the molecular architecture of carbohydrates, yet the availability of accurate methods for 1DCC determination has not been sufficiently explored, despite the importance that such data could play in structural studies of oligo- and polysaccharides. Existing methods require fitting intensity ratios of cross- to diagonal-peaks as a function of the constant-time (CT) in CT-COSY experiments, while other methods utilize measurement of peak separation. The former strategies suffer from complications due to peak overlap, primarily in regions close to the diagonal, while the latter strategies are negatively impacted by the common occurrence of strong coupling in sugars, which requires a reliable assessment of their influence in the context of RDC determination. We detail a 13C-13C CT-COSY method that combines a variation in the CT processed with diagonal filtering to yield 1JCC and RDCs. The strategy, which relies solely on cross-peak intensity modulation, is inspired in the cross-peak nulling method used for JHH determinations, but adapted and extended to applications where, like in sugars, large one-bond 13C-13C couplings coexist with relatively small long-range couplings. Because diagonal peaks are not utilized, overlap problems are greatly alleviated. Thus, one-bond couplings can be determined from different cross-peaks as either active or passive coupling. This results in increased accuracy when more than one determination is available, and in more opportunities to measure a specific coupling in the presence of severe overlap. In addition, we evaluate the influence of strong couplings on the determination of RDCs by computer simulations. We show that individual scalar couplings are notably affected by the presence of strong couplings but, at least for the simple cases studied, the obtained RDC values for use in structural calculations were not, because the errors introduced by strong couplings for the isotropic and oriented phases are very

  18. Structural heterogeneity in microcrystalline ubiquitin studied by solid-state NMR

    PubMed Central

    Fasshuber, Hannes Klaus; Lakomek, Nils-Alexander; Habenstein, Birgit; Loquet, Antoine; Shi, Chaowei; Giller, Karin; Wolff, Sebastian; Becker, Stefan; Lange, Adam

    2015-01-01

    By applying [1-13C]- and [2-13C]-glucose labeling schemes to the folded globular protein ubiquitin, a strong reduction of spectral crowding and increase in resolution in solid-state NMR (ssNMR) spectra could be achieved. This allowed spectral resonance assignment in a straightforward manner and the collection of a wealth of long-range distance information. A high precision solid-state NMR structure of microcrystalline ubiquitin was calculated with a backbone rmsd of 1.57 to the X-ray structure and 1.32 Å to the solution NMR structure. Interestingly, we can resolve structural heterogeneity as the presence of three slightly different conformations. Structural heterogeneity is most significant for the loop region β1-β2 but also for β-strands β1, β2, β3, and β5 as well as for the loop connecting α1 and β3. This structural polymorphism observed in the solid-state NMR spectra coincides with regions that showed dynamics in solution NMR experiments on different timescales. PMID:25644665

  19. Solid-state NMR characterization of Mowry Formation shales

    SciTech Connect

    Miknis, F.P.

    1992-04-01

    Solid-state {sup 13}C and {sup 29}Si NMR measurements were carried out on a series of petroleum source rocks from the Mowry Formation of the Powder River Basin in Wyoming. The objectives of this study wereto use CP/MAS {sup 13}C NMR measurements to monitor changes in the carbon structure of the kerogen that result from depth of burial, and to examine the feasibility of {sup 29}Si NMR for studying the thermal alteration of clay minerals during diagenesis. Carbon and silicon NMR measurements were made on a suite of samples covering a present-day depth interval of 3,000 to 11,500 ft.In general, the NMR results endorsed other geochemical analyses that were performed on the source rocks as part of another study to examine pressure compartmentalization in the Mowry Formation. The carbon aromaticity of the kerogen increased with depth of burial, and at depths greater that approximately 10,000 ft the kerogen showed little capacity to generate additional oil because of the small fraction of residual aliphatic carbon. By combining NMR and Rock-Eval measurements, an estimate of the hydrogen budget was obtained. The calculations indicated that approximately 20% of the kerogen was converted to hydrocarbons, and that sufficient hydrogen was liberated from aromatization and condensation reactions to stabilize the generated products. The {sup 29}Si NMR spectra were characterized by a relatively sharp quartz resonance and a broad resonance from the clay minerals. With increasing depth of burial, the clay resonance became broader and shifted slightly downfield. These changes qualitatively support X-ray analysis that shows progressive alteration of illite to smectite with depth of burial.

  20. Solid-state NMR characterization of Mowry Formation shales

    SciTech Connect

    Miknis, F.P.

    1992-04-01

    Solid-state [sup 13]C and [sup 29]Si NMR measurements were carried out on a series of petroleum source rocks from the Mowry Formation of the Powder River Basin in Wyoming. The objectives of this study wereto use CP/MAS [sup 13]C NMR measurements to monitor changes in the carbon structure of the kerogen that result from depth of burial, and to examine the feasibility of [sup 29]Si NMR for studying the thermal alteration of clay minerals during diagenesis. Carbon and silicon NMR measurements were made on a suite of samples covering a present-day depth interval of 3,000 to 11,500 ft.In general, the NMR results endorsed other geochemical analyses that were performed on the source rocks as part of another study to examine pressure compartmentalization in the Mowry Formation. The carbon aromaticity of the kerogen increased with depth of burial, and at depths greater that approximately 10,000 ft the kerogen showed little capacity to generate additional oil because of the small fraction of residual aliphatic carbon. By combining NMR and Rock-Eval measurements, an estimate of the hydrogen budget was obtained. The calculations indicated that approximately 20% of the kerogen was converted to hydrocarbons, and that sufficient hydrogen was liberated from aromatization and condensation reactions to stabilize the generated products. The [sup 29]Si NMR spectra were characterized by a relatively sharp quartz resonance and a broad resonance from the clay minerals. With increasing depth of burial, the clay resonance became broader and shifted slightly downfield. These changes qualitatively support X-ray analysis that shows progressive alteration of illite to smectite with depth of burial.

  1. The T1 ρ13C spin-lattice relaxation time of helical polyguanidines

    NASA Astrophysics Data System (ADS)

    Lim, A. R.; Stewart, J. R.; Novak, B. M.

    1999-03-01

    The solid state dynamics of three helical polyguanidines differing only in their stereochemistry was investigated by 13C CP/MAS NMR. From these studies, the structures of the polyguanidines were confirmed, and the 13C spin-lattice relaxation times in the rotating frame were measured. The relaxation times of all the polyguanidines indicated that they undergo fast motions, i.e. motions on the fast side of the T1 ρ minimum. The main chain carbon of polyguanidine I-( R/ S), with equal amounts of ( R) and ( S) chiral side chains, has higher activation energy, 10.7 kJ/mol, than the analogous polymers with enantiomerically pure side chains ( I-( R) and I-( S)), 5.1 kJ/mol.

  2. Hard and elastic amorphous carbon nitride thin films studied by 13C nuclear magnetic resonance spectroscopy

    NASA Astrophysics Data System (ADS)

    Gammon, W. J.; Malyarenko, D. I.; Kraft, O.; Hoatson, G. L.; Reilly, A. C.; Holloway, B. C.

    2002-10-01

    The chemical bonding of hard and elastic amorphous carbon nitride (a-CNx) thin films was examined using solid-state 13C NMR spectroscopy. The films were deposited by DC magnetron sputtering in a pure nitrogen discharge on Si(001) substrates at 300 °C. Nanoindentation tests reveal a recovery of 80%, a hardness of 5 GPa, and an elastic modulus of 47 GPa. This combination of low modulus and high strength means the material can be regarded as hard and elastic; the material gives when pressed on and recovers its shape when the load is released. The 13C NMR results conclusively demonstrate that hard and elastic a-CNx has an sp2 carbon bonded structure and that sp3 hybridized carbons are absent. Our results stand in contrast with earlier work that proposed that the interesting mechanical properties of hard and elastic a-CNx were due, in part, to sp3 bonded carbon.

  3. Evolution of a solid state laser

    NASA Astrophysics Data System (ADS)

    Yamamoto, R. M.; Parker, J. M.; Allen, K. L.; Allmon, R. W.; Alviso, K. F.; Barty, C. P. J.; Bhachu, B. S.; Boley, C. D.; Burnham, A. K.; Combs, R. L.; Cutter, K. P.; Fochs, S. N.; Gonzales, S. A.; Hurd, R. L.; LaFortune, K. N.; Manning, W. J.; McClelland, M. A.; Merrill, R. D.; Molina, L.; Parks, C. W.; Pax, P. H.; Posey, A. S.; Rotter, M. D.; Roy, B. M.; Rubenchik, A. M.; Soules, T. F.; Webb, D. E.

    2007-04-01

    Lawrence Livermore National Laboratory (LLNL) has been developing compact solid state lasers since the 1990's. One of the first lasers to be developed utilized flashlamp pumped architecture and neodymium glass as the laser gain media. In the early 2000's, a diode pumped version of the original flashlamp pumped laser was designed and built, responding to the requirements that a laser system for the military be compact in both size and weight while creating significant power (~100 kW) for the missions envisioned. This paper will discuss the evolution of solid state lasers at LLNL and provide a glimpse into the types of capabilities that could be achieved in the near future.

  4. Solid state mechanochemical processes for better electroceramics.

    PubMed

    Mamoru, Senna

    2014-01-01

    The present short overview focuses on the renovation of solid state processes toward phase pure and well-crystallized complex oxides centered on the electroceramic materials. Elevation of the reactivity and preservation of stoichiometry of the starting mixture or precursor are of universal importance. Mechanical activation, being considered as versatile, may also need reconsideration in view of contamination and process rationalization. After briefly reviewing mechanochemical processes for direct synthesis of complex oxides, solid state processes toward well crystallized fine particles of complex oxides are discussed by starting from mechanochemically derived precursors with subsequent optimized calcination. Case studies were cited from literatures for complex oxides, including author's own experimental studies mainly with BaBi(2)Ta(2)O(9) (BBT), Ba(Mg(1/3)Ta(2/3))O(3) (BMT) and KNbO(3) (KN). The substances discussed are mostly associated with ferroelectric materials, with a few exceptions of iron-containing magnetic materials. PMID:25286196

  5. Unique beam delivery and processing tools for high power solid state laser processing

    NASA Astrophysics Data System (ADS)

    Ryba, Tracey; Havrilla, David; Holzer, Marco; Bea, Martin

    2012-03-01

    The continued advances in high power, high brightness solid state laser has necessitated new tools for use with laser material processing. Some of the challenges of higher power lasers have been met with Reflective Focusing Optic to combat Thermal focus shift and new fiber optic cables to more efficiently deliver the higher power. Conversely the improved brightness has led to new opportunities with patented dual core fibers, advances in remote scanner welding devices and calibration devices for them. This paper will explain recent advances in beam delivery and processing optics for high power, high brightness solid state lasers.

  6. Solid state lithium-iodine primary battery

    SciTech Connect

    Sekido, S.; Ninomiya, Y.; Sotomura, T.

    1984-01-10

    A solid-state primary cell comprising a lithium anode, an iodine cathode containing a charge transfer complex and a solid lithium iodide electrolyte doped with a 1-normal-alkyl-pyridinium iodide. The anode surface can be coated with LiOH or Li/sub 3/N. The iodine cathode comprises a complex of iodine and 1-normal-alkyl-pyridinium iodide and preferably contains titanium dioxide powder, alumina gel powder or silica gel powder admixed with the complex.

  7. High energy efficient solid state laser sources

    NASA Technical Reports Server (NTRS)

    Byer, Robert L.

    1987-01-01

    Diode-laser-pumped solid-state laser oscillators and nonlinear processes were investigated. A new generation on nonplanar oscillator was fabricated, and it is anticipated that passive linewidths will be pushed to the kilohertz regime. A number of diode-pumped laser transitions were demonstrated in the rod configuration. Second-harmonic conversion efficiencies as high as 15% are routinely obtained in a servo-locked external resonant doubling crystal at 15 mW cw input power levels at 1064 nm.

  8. Pulsed solid state lasers for medicine

    NASA Astrophysics Data System (ADS)

    Kertesz, Ivan; Danileiko, A. Y.; Denker, Boris I.; Kroo, Norbert; Osiko, Vyacheslav V.; Prokhorov, Alexander M.

    1994-02-01

    The effect on living tissues of different pulsed solid state lasers: Nd:YAG ((lambda) equals 1.06 micrometers ) Er:glass (1.54 micrometers ), Ho:YAG (2.1 micrometers ) and Er:YAG (2.94 micrometers ) is compared with the continuous wave Nd:YAG- and CO2-lasers used in operating theaters. Portable Er:glass- and Er:YAG-lasers are developed for surgery/cosmetics and HIV-safe blood testing.

  9. Solid-state-laser-rod holder

    DOEpatents

    Gettemy, D.J.; Barnes, N.P.; Griggs, J.E.

    1981-08-11

    The disclosure relates to a solid state laser rod holder comprising Invar, copper tubing, and epoxy joints. Materials and coefficients of expansion of the components of the holder combine with the rod to produce a joint which will give before the rod itself will. The rod may be lased at about 70 to 80/sup 0/K and returned from such a temperature to room temperature repeatedly without its or the holder's destruction.

  10. Solid state synthesis of poly(dichlorophosphazene)

    DOEpatents

    Allen, Christopher W.; Hneihen, Azzam S.; Peterson, Eric S.

    2001-01-01

    A method for making poly(dichlorophosphazene) using solid state reactants is disclosed and described. The present invention improves upon previous methods by removing the need for chlorinated hydrocarbon solvents, eliminating complicated equipment and simplifying the overall process by providing a "single pot" two step reaction sequence. This may be accomplished by the condensation reaction of raw materials in the melt phase of the reactants and in the absence of an environmentally damaging solvent.

  11. Analysis of Technology for Solid State Coherent Lidar

    NASA Technical Reports Server (NTRS)

    Amzajerdian, Farzin

    1997-01-01

    Over the past few years, considerable advances have been made in the areas of the diode-pumped, eye-safe, solid state lasers, wide bandwidth, semiconductor detectors operating in the near-infrared region. These advances have created new possibilities for the development of low-cost, reliable, and compact coherent lidar systems for measurements of atmospheric winds and aerosol backscattering from a space-based platform. The work performed by the UAH personnel concentrated on design and analyses of solid state pulsed coherent lidar systems capable of measuring atmospheric winds from space, and design and perform laboratory experiments and measurements in support of solid state laser radar remote sensing systems which are to be designed, deployed, and used by NASA to measure atmospheric processes and constituents. A lidar testbed system was designed and analyzed by considering the major space operational and environmental requirements, and its associated physical constraints. The lidar optical system includes a wedge scanner and the compact telescope designed by the UAH personnel. The other major optical components included in the design and analyses were: polarizing beam splitter, routing mirrors, wave plates, signal beam derotator, and lag angle compensator. The testbed lidar optical train was designed and analyzed, and different design options for mounting and packaging the lidar subsystems and components and support structure were investigated. All the optical components are to be mounted in a stress-free and stable manner to allow easy integration and alignment, and long term stability. This lidar system is also intended to be used for evaluating the performance of various lidar subsystems and components that are to be integrated into a flight unit and for demonstrating the integrity of the signal processing algorithms by performing actual atmospheric measurements from a ground station.

  12. SPS solid state antenna power combiner

    NASA Technical Reports Server (NTRS)

    Fitzsimmons, G. W.

    1980-01-01

    A concept for a solar power satellite antenna power combiner which utilizes solid state dc-rf converters is described. To avoid the power combining losses associated with circuit hybrids it is proposed that the power from multiple solid state amplifiers be combined by direct coupling of each amplifier's output to the radiating antenna structure. The selected power-combining antenna consists of a printed (metalized) microstrip circuit on a ceramic type dielectric substrate which is backed by a shallow lightweight aluminum cavity which sums the power of four microwave sources. The antenna behaves like two one-half wavelength slot-line antennas coupled together via their common cavity structure. A significant feature of the antenna configuration selected is that the radiated energy is summed to yield a single radiated output phase which represents the average insertion phase of the four power amplifiers. This energy may be sampled and, by comparison with the input signal, one can phase error correct to maintain the insertion phase of all solid state power combining modules at exactly the same value. This insures that the insertion phase of each SPS power combining antenna module is identical. An experiment verification program is described.

  13. Protein structure by solid-state NMR of oriented systems

    SciTech Connect

    Stewart, P.L.

    1987-01-01

    A method for determining protein backbone structure from angular information obtainable by solid state NMR spectroscopy is presented. Various spin interactions including quadrupole, dipole, and chemical shift interactions and nuclei including /sup 14/N, /sup 15/N, /sup 13/C, and /sup 2/H may be observed. Angularly dependent measurements can be made when the sample has at least one direction of order along the externally applied magnetic field. Several NMR parameters are used to determine the orientation of each peptide plane with respect to the magnetic field vector, B/sub O/, to within a few symmetry related possibilities. The computer program Totlink can then be used to perform the necessary coordinate transformations and to evaluate the possible backbone structures and select for the most chemically reasonable. Experimental /sup 14/N NMR structural studies of the model peptides n-acetyl-d,l-valine, n-acetyl-l-valyl-l-leucine, and l-alanyl-glycyl-glycine and preliminary /sup 14/N NMR results on a large single crystal of orthorhombic lysozyme are presented.

  14. Chemical shift changes and line narrowing in 13C NMR spectra of hydrocarbon clathrate hydrates.

    PubMed

    Kida, Masato; Sakagami, Hirotoshi; Takahashi, Nobuo; Nagao, Jiro

    2013-05-23

    The solid-state (13)C NMR spectra of various guest hydrocarbons (methane, ethane, propane, adamantane) in clathrate hydrates were measured to elucidate the local structural environments around hydrocarbon molecules isolated in guest-host frameworks of clathrate hydrates. The results show that, depending on the cage environment, the trends in the (13)C chemical shift and line width change as a function of temperature. Shielding around the carbons of the guest normal alkanes in looser cage environments tends to decrease with increasing temperature, whereas shielding in tighter cage environments tends to increase continuously with increasing temperature. Furthermore, the (13)C NMR line widths suggest, because of the reorientation of the guest alkanes, that the local structures in structure II are more averaged than those in structure I. The differences between structures I and II tend to be very large in the lower temperature range examined in this study. The (13)C NMR spectra of adamantane guest molecules in structure H hydrate show that the local structures around adamantane guests trapped in structure H hydrate cages are averaged at the same level as in the α phase of solid adamantane. PMID:23607335

  15. High-resolution magic-angle spinning (13)C spectroscopy of brain tissue at natural abundance.

    PubMed

    Yang, Yongxia; Chen, Lei; Gao, Hongchang; Zeng, Danlin; Yue, Yong; Liu, Maili; Lei, Hao; Deng, Feng; Ye, Chaohui

    2006-03-01

    High-resolution magic-angle spinning (MAS) (1)H and (13)C magnetic resonance spectroscopy (MRS) has recently been applied to study the metabolism in intact biological tissue samples. Because of the low natural abundance and the low gyromagnetic ratio of the (13)C nuclei, signal enhancement techniques such as cross-polarization (CP) and distortionless enhancement by polarization transfer (DEPT) are often employed in MAS (13)C MRS to improve the detection sensitivity. In this study, several sensitivity enhancement techniques commonly used in liquid- and solid-state NMR, including CP, DEPT and nuclear Overhauser enhancement (NOE), were combined with MAS to acquire high-resolution (13)C spectra on intact rat brain tissue at natural abundance, and were compared for their performances. The results showed that different signal enhancement techniques are sensitive to different classes of molecules/metabolites, depending on their molecular weights and mobility. DEPT was found to enhance the signals of low-molecular weight metabolites exclusively, while the signals of lipids, which often are associated with membranes and have relatively lower mobility, were highly sensitive to CP enhancement. PMID:16477685

  16. (13)C NMR Studies, Molecular Order, and Mesophase Properties of Thiophene Mesogens.

    PubMed

    Veeraprakash, B; Lobo, Nitin P; Narasimhaswamy, T

    2015-12-01

    Three-ring mesogens with a core comprising thiophene linked to one phenyl ring directly and to the other via flexible ester are synthesized with terminal alkoxy chains to probe the mesophase properties and find the molecular order. The phenyl thiophene link in the core offers a comparison of the mesophase features with the molecular shape of the mesogen. The synthesized mesogens display enantiotropic polymesomorphism and accordingly nematic, smectic A, smectic C and smectic B mesophases are perceived depending upon the terminal chain length. For some of the homologues, monotropic higher order smectic phases such as smectic F and crystal E are also witnessed. The existence of polymesomorphism are originally observed by HOPM and DSC and further confirmed by powder X-ray diffraction studies. For the C8 homologue, high resolution solid state (13)C NMR spectroscopy is employed to find the molecular structure in the liquid crystalline phase and using the 2D SLF technique, the (13)C-(1)H dipolar couplings are extracted to calculate the order parameter. By comparing the ratio of local order of thiophene as well as phenyl rings, we establish the bent-core shape of the mesogen. Importantly, for assigning the carbon chemical shifts of the core unit of aligned C8 mesogen, the (13)C NMR measured in mesophase of the synthetic intermediate is employed. Thus, the proposed approach addresses the key step in the spectral assignment of target mesogens with the use of (13)C NMR data of mesomorphic intermediate. PMID:26551439

  17. Optoacoustic 13C-breath test analyzer

    NASA Astrophysics Data System (ADS)

    Harde, Hermann; Helmrich, Günther; Wolff, Marcus

    2010-02-01

    The composition and concentration of exhaled volatile gases reflects the physical ability of a patient. Therefore, a breath analysis allows to recognize an infectious disease in an organ or even to identify a tumor. One of the most prominent breath tests is the 13C-urea-breath test, applied to ascertain the presence of the bacterium helicobacter pylori in the stomach wall as an indication of a gastric ulcer. In this contribution we present a new optical analyzer that employs a compact and simple set-up based on photoacoustic spectroscopy. It consists of two identical photoacoustic cells containing two breath samples, one taken before and one after capturing an isotope-marked substrate, where the most common isotope 12C is replaced to a large extent by 13C. The analyzer measures simultaneously the relative CO2 isotopologue concentrations in both samples by exciting the molecules on specially selected absorption lines with a semiconductor laser operating at a wavelength of 2.744 μm. For a reliable diagnosis changes of the 13CO2 concentration of 1% in the exhaled breath have to be detected at a concentration level of this isotope in the breath of about 500 ppm.

  18. Impact of Ho(3+)-doping on (13)C dynamic nuclear polarization using trityl OX063 free radical.

    PubMed

    Kiswandhi, Andhika; Niedbalski, Peter; Parish, Christopher; Kaur, Pavanjeet; Martins, André; Fidelino, Leila; Khemtong, Chalermchai; Song, Likai; Sherry, A Dean; Lumata, Lloyd

    2016-08-21

    We have investigated the effects of Ho-DOTA doping on the dynamic nuclear polarization (DNP) of [1-(13)C] sodium acetate using trityl OX063 free radical at 3.35 T and 1.2 K. Our results indicate that addition of 2 mM Ho-DOTA on 3 M [1-(13)C] sodium acetate sample in 1 : 1 v/v glycerol : water with 15 mM trityl OX063 improves the DNP-enhanced (13)C solid-state nuclear polarization by a factor of around 2.7-fold. Similar to the Gd(3+) doping effect on (13)C DNP, the locations of the positive and negative (13)C maximum polarization peaks in the (13)C microwave DNP sweep are shifted towards each other with the addition of Ho-DOTA on the DNP sample. W-band electron spin resonance (ESR) studies have revealed that while the shape and linewidth of the trityl OX063 ESR spectrum was not affected by Ho(3+)-doping, the electron spin-lattice relaxation time T1 of trityl OX063 was prominently reduced at cryogenic temperatures. The reduction of trityl OX063 electron T1 by Ho-doping is linked to the (13)C DNP improvement in light of the thermodynamic picture of DNP. Moreover, the presence of Ho-DOTA in the dissolution liquid at room temperature has negligible reduction effect on liquid-state (13)C T1, in contrast to Gd(3+)-doping which drastically reduces the (13)C T1. The results here suggest that Ho(3+)-doping is advantageous over Gd(3+) in terms of preservation of hyperpolarized state-an important aspect to consider for in vitro and in vivo NMR or imaging (MRI) experiments where a considerable preparation time is needed to administer the hyperpolarized (13)C liquid. PMID:27424954

  19. Solid state structural and theoretical investigations of a biologically active chalcone

    NASA Astrophysics Data System (ADS)

    Abbas, Asghar; Gökce, Halil; Bahceli, Semiha; Bolte, Michael; Naseer, Muhammad Moazzam

    2016-05-01

    The computational methods are presently emerging as an efficient and reliable tool for predicting structural properties of biologically important compounds. In the present manuscript, the solid state structural and theoretical investigations of a biologically active chalcone i-e (E)-3-(4-(hexyloxy)phenyl)-1-phenylprop-2-en-1-one (6c) have been reported. The solid state structure of 6c was measured by X-ray crystallographic technique whereas the optimized molecular geometry, vibrational frequencies, the simulated UV-vis spectra (in gas and in methanol solvent), 1H and 13C NMR chemical shift (in gas and in chloroform solvent) values, HOMO-LUMO analysis, the molecular electrostatic potential (MEP) surface and thermodynamic parameters were calculated by using DFT/B3LYP method with 6-311++G(d,p) basis set in ground state. The results of the theoretical investigations were found to be in good agreement with experimental data.

  20. Application and Reliability of Solid-State NMR in Environmental Sciences

    NASA Astrophysics Data System (ADS)

    Knicker, Heike

    2010-05-01

    For the characterization of soil organic matter, a suite of analytical approaches are available. Chemical degradative methods involve an extraction scheme with which the soluble part of the mixture is isolated and analyzed by colorimetrical or chromatographic means. Macromolecular structures can be subjected to thermolytic or combined thermochemolytic degradation. Because secondary reactions (rearrangement, cracking, hydrogenation and polymerization) in a heterogeneous mixture cannot be excluded, it is obvious that conclusions regarding the original structure in the macromolecular phase have to be drawn with caution. A powerful alternative represents solid-state nuclear magnetic resonance (NMR) spectroscopy, allowing the examination of the bulk sample without major pre-treatment In environmental sciences, this technique mostly involves the isotope 13C to study the chemical composition of organic matter in soils, sediments or compost to study the temporal development of humic material or chemical alterations due to variation in environmental parameters. Due to its low sensibility solid-state 15N NMR studies on such samples are only found occasionally. The emphasis of solid-state NMR spectroscopy is not only to determine the gross chemical composition of the material under study via a chemical shift assignment but also a quantitative correlation between the different signal intensities and the relative contribution of the respective C or N types to the total organic C or N content. However, despite increasing popularity, this approach is still viewed as mysterious techniques, in particular with respect to quantification. Accordingly, the purpose of this review is to give a short overview on the possibilities and limitations of this technique in environmental science and in particular for the study of soil organic matter. In general, solid-state 13C NMR spectra of soil organic matter are obtained with the cross polarization magic angle spinning (CPMAS) technique. This

  1. Solid state and aqueous behavior of uranyl peroxide cage clusters

    NASA Astrophysics Data System (ADS)

    Pellegrini, Kristi Lynn

    Uranyl peroxide cage clusters include a large family of more than 50 published clusters of a variety of sizes, which can incorporate various ligands including pyrophosphate and oxalate. Previous studies have reported that uranyl clusters can be used as a method to separate uranium from a solid matrix, with potential applications in reprocessing of irradiated nuclear fuel. Because of the potential applications of these novel structures in an advanced nuclear fuel cycle and their likely presence in areas of contamination, it is important to understand their behavior in both solid state and aqueous systems, including complex environments where other ions are present. In this thesis, I examine the aqueous behavior of U24Pp 12, as well as aqueous cluster systems with added mono-, di-, and trivalent cations. The resulting solutions were analyzed using dynamic light scattering and ultra-small angle X-ray scattering to evaluate the species in solution. Precipitates of these systems were analyzed using powder X-ray diffraction, X-ray fluorescence spectrometry, and Raman spectroscopy. The results of these analyses demonstrate the importance of cation size, charge, and concentration of added cations on the aqueous behavior of uranium macroions. Specifically, aggregates of various sizes and shapes form rapidly upon addition of cations, and in some cases these aggregates appear to precipitate into an X-ray amorphous material that still contains U24Pp12 clusters. In addition, I probe aggregation of U24Pp12 and U60, another uranyl peroxide cage cluster, in mixed solvent water-alcohol systems. The aggregation of uranyl clusters in water-alcohol systems is a result of hydrogen bonding with polar organic molecules and the reduction of the dielectric constant of the system. Studies of aggregation of uranyl clusters also allow for comparison between the newer uranyl polyoxometalate family and century-old transition metal polyoxometalates. To complement the solution studies of uranyl

  2. High Extraction Phosphors for Solid State Lighting

    SciTech Connect

    Summers, Chris; Menkara, Hisham; Wagner, Brent

    2011-09-01

    We have developed high-index, high efficiency bulk luminescent materials and novel nano-sized phosphors for improved solid-state white LED lamps. These advances can potentially contribute to reducing the loss in luminous efficiencies due to scattering, re-absorption, and thermal quenching. The bulk and nanostructured luminescent materials investigated are index matched to GaN and have broad and size-tunable absorption bands, size and impurity tuned emission bands, size-driven elimination of scattering effects, and a separation between absorption and emission bands. These innovations were accomplished through the use of novel synthesis techniques suitable for high volume production for LED lamp applications. The program produced a full-color set of high quantum yield phosphors with high chemical stability. In the bulk phosphor study, the ZnSeS:Cu,Ag phosphor was optimized to achieve >91% efficiency using erbium (Er) and other activators as sensitizers. Detailed analysis of temperature quenching effects on a large number of ZnSeS:Cu,Ag,X and strontium- and calcium-thiogallate phosphors lead to a breakthrough in the understanding of the anti-quenching behavior and a physical bandgap model was developed of this phenomena. In a follow up to this study, optimized phosphor blends for high efficiency and color performance were developed and demonstrated a 2-component phosphor system with good white chromaticity, color temperature, and high color rendering. By extending the protocols of quantum dot synthesis, large nanocrystals, greater than 20 nm in diameter were synthesized and exhibited bulk-like behavior and blue light absorption. The optimization of ZnSe:Mn nanophosphors achieved ~85% QE The limitations of core-shell nanocrystal systems were addressed by investigating alternative deltadoped structures. To address the manufacturability of these systems, a one-pot manufacturing protocol was developed for ZnSe:Mn nanophosphors. To enhance the stability of these material

  3. BOOK REVIEW: Solid State Physics: An Introduction

    NASA Astrophysics Data System (ADS)

    Jakoby, Bernhard

    2009-07-01

    There's a wealth of excellent textbooks on solid state physics. The author of the present book is well aware of this fact and does not attempt to write just another one. Rather, he has provided a very compact introduction to solid state physics for third-year students. As we are faced with the continuous appearance interdisciplinary fields and associated study curricula in natural and engineering sciences (biophysics, mechatronics, etc), a compact text in solid state physics would be appreciated by students of these disciplines as well. The book features 11 chapters where each is provided with supplementary discussion questions and problems. The first chapters deal with a review of chemical bonding mechanisms, crystal structures and mechanical properties of solids, which are brief but by no means superficial. The following, somewhat more detailed chapter on thermal properties of lattices includes a nice introduction to phonons. The foundations of solid state electronics are treated in the next three chapters. Here the author first discusses the classical treatment of electronic behaviour in metals (Drude model) and continues with a quantum-theoretical approach starting with the free-electron model and leading to the band structures in conductive solids. The next chapter is devoted to semiconductors and ends with a brief but, with respect to the topical scope, adequate discussion of semiconductor devices. The classical topics of magnetic and dielectric behaviour are treated in the sequel. The book closes with a chapter on superconductivity and a brief chapter covering the modern topics of quantum confinement and aspects of nanoscale physics. In my opinion, the author has succeeded in creating a very concise yet not superficial textbook. The account presented often probes subjects deep enough to lay the basis for a thorough understanding, preparing the reader for more specialized textbooks. For instance, I think that this book may serve as an excellent first

  4. Solid State Laser Technology Development for Atmospheric Sensing Applications

    NASA Technical Reports Server (NTRS)

    Barnes, James C.

    1998-01-01

    NASA atmospheric scientists are currently planning active remote sensing missions that will enable global monitoring of atmospheric ozone, water vapor, aerosols and clouds as well as global wind velocity. The measurements of these elements and parameters are important because of the effects they have on climate change, atmospheric chemistry and dynamics, atmospheric transport and, in general, the health of the planet. NASA will make use of Differential Absorption Lidar (DIAL) and backscatter lidar techniques for active remote sensing of molecular constituents and atmospheric phenomena from advanced high-altitude aircraft and space platforms. This paper provides an overview of NASA Langley Research Center's (LaRC's) development of advanced solid state lasers, harmonic generators, and wave mixing techniques aimed at providing the broad range of wavelengths necessary to meet measurement goals of NASA's Earth Science Enterprise.

  5. Towards hyperpolarized 13C-succinate imaging of brain cancer

    NASA Astrophysics Data System (ADS)

    Bhattacharya, Pratip; Chekmenev, Eduard Y.; Perman, William H.; Harris, Kent C.; Lin, Alexander P.; Norton, Valerie A.; Tan, Chou T.; Ross, Brian D.; Weitekamp, Daniel P.

    2007-05-01

    We describe a novel 13C enriched precursor molecule, sodium 1- 13C acetylenedicarboxylate, which after hydrogenation by PASADENA (Parahydrogen and Synthesis Allows Dramatically Enhanced Nuclear Alignment) under controlled experimental conditions, becomes hyperpolarized 13C sodium succinate. Fast in vivo 3D FIESTA MR imaging demonstrated that, following carotid arterial injection, the hyperpolarized 13C-succinate appeared in the head and cerebral circulation of normal and tumor-bearing rats. At this time, no in vivo hyperpolarized signal has been localized to normal brain or brain tumor. On the other hand, ex vivo samples of brain harvested from rats bearing a 9L brain tumor, 1 h or more following in vivo carotid injection of hyperpolarized 13C sodium succinate, contained significant concentrations of the injected substrate, 13C sodium succinate, together with 13C maleate and succinate metabolites 1- 13C-glutamate, 5- 13C-glutamate, 1- 13C-glutamine and 5- 13C-glutamine. The 13C substrates and products were below the limits of NMR detection in ex vivo samples of normal brain consistent with an intact blood-brain barrier. These ex vivo results indicate that hyperpolarized 13C sodium succinate may become a useful tool for rapid in vivo identification of brain tumors, providing novel biomarkers in 13C MR spectral-spatial images.

  6. Interference of homonuclear decoupling and exchange in the solid-state NMR of perfluorocyclohexane

    NASA Astrophysics Data System (ADS)

    McMillan, Deborah E.; Hazendonk, Paul; Hodgkinson, Paul

    2003-04-01

    We observe an interference between RF irradiation used for homonuclear decoupling of 19F and conformational exchange in the 13C spectrum of perfluorocyclohexane. We show that these effects can be readily reproduced in simulation, and characterise their dependence on the various NMR and experimental parameters. Their application to observing exchange rates on the kHz timescale is evaluated with respect to T1 ρ measurements and the connections between the two approaches established. The implications for experiments that use homonuclear decoupling of 1H to resolve 1J CH couplings in the solid-state are also evaluated in detail.

  7. Passivation-free solid state battery

    DOEpatents

    Abraham, K.M.; Peramunage, D.

    1998-06-16

    This invention pertains to passivation-free solid-state rechargeable batteries composed of Li{sub 4}Ti{sub 5}O{sub 12} anode, a solid polymer electrolyte and a high voltage cathode. The solid polymer electrolyte comprises a polymer host, such as polyacrylonitrile, poly(vinyl chloride), poly(vinyl sulfone), and poly(vinylidene fluoride), plasticized by a solution of a Li salt in an organic solvent. The high voltage cathode includes LiMn{sub 2}O{sub 4}, LiCoO{sub 2}, LiNiO{sub 2} and LiV{sub 2}O{sub 5} and their derivatives. 5 figs.

  8. Pulsed Power for Solid-State Lasers

    SciTech Connect

    Gagnon, W; Albrecht, G; Trenholme, J; Newton, M

    2007-04-19

    Beginning in the early 1970s, a number of research and development efforts were undertaken at U.S. National Laboratories with a goal of developing high power lasers whose characteristics were suitable for investigating the feasibility of laser-driven fusion. A number of different laser systems were developed and tested at ever larger scale in pursuit of the optimum driver for laser fusion experiments. Each of these systems had associated with it a unique pulsed power option. A considerable amount of original and innovative engineering was carried out in support of these options. Ultimately, the Solid-state Laser approach was selected as the optimum driver for the application. Following this, the Laser Program at the Lawrence Livermore National Laboratory and the University of Rochester undertook aggressive efforts directed at developing the technology. In particular, at Lawrence Livermore National Laboratory, a series of laser systems beginning with the Cyclops laser and culminating in the present with the National Ignition Facility were developed and tested. As a result, a large amount of design information for solid-state laser pulsed power systems has been documented. Some of it is in the form of published papers, but most of it is buried in internal memoranda, engineering reports and LLNL annual reports. One of the goals of this book is to gather this information into a single useable format, such that it is easily accessed and understood by other engineers and physicists for use with future designs. It can also serve as a primer, which when seriously studied, makes the subsequent reading of original work and follow-up references considerably easier. While this book deals only with the solid-state laser pulsed power systems, in the bibliography we have included a representative cross section of papers and references from much of the very fine work carried out at other institutions in support of different laser approaches. Finally, in recent years, there has

  9. Solid-state turn coordinator display

    NASA Technical Reports Server (NTRS)

    Meredith, B. D.; Crouch, R. K.; Kelly, W. L., IV

    1975-01-01

    A solid state turn coordinator display which employs light emitting diodes (LED's) as the display medium was developed to demonstrate the feasibility of such displays for aircraft applications. The input to the display is supplied by a fluidic inertial rate sensor used in an aircraft wing leveler system. The display is composed of the LED radial display face and the electronics necessary to address and drive the individual lines of LED's. Three levels of brightness are provided to compensate for the different amounts of ambient light present in the cockpit.

  10. Entanglement and Squeezing in Solid State Circuits

    SciTech Connect

    Wen Yihuo; Gui Lulong

    2008-11-07

    We investigate the dynamics of a system consisting of a Cooper-pair box and two superconducting transmission line resonators. There exist both linear and nonlinear interactions in such a system. We show that single-photon entanglement state can be generated in a simple way in the linear interaction regime. In nonlinear interaction regime, we derive the Hamiltonian of degenerate three-wave mixing and propose a scheme for generating squeezed state of microwave using the three-wave mixing in solid state circuits. In the following, we design a system for generating squeezed states of nanamechanical resonator.

  11. High temperature solid state storage cell

    SciTech Connect

    Rea, Jesse R.; Kallianidis, Milton; Kelsey, G. Stephen

    1983-01-01

    A completely solid state high temperature storage cell comprised of a solid rechargeable cathode such as TiS.sub.2, a solid electrolyte which remains solid at the high temperature operating conditions of the cell and which exhibits high ionic conductivity at such elevated temperatures such as an electrolyte comprised of lithium iodide, and a solid lithium or other alkali metal alloy anode (such as a lithium-silicon alloy) with 5-50% by weight of said anode being comprised of said solid electrolyte.

  12. Solid state transport-based thermoelectric converter

    DOEpatents

    Hu, Zhiyu

    2010-04-13

    A solid state thermoelectric converter includes a thermally insulating separator layer, a semiconducting collector and an electron emitter. The electron emitter comprises a metal nanoparticle layer or plurality of metal nanocatalyst particles disposed on one side of said separator layer. A first electrically conductive lead is electrically coupled to the electron emitter. The collector layer is disposed on the other side of the separator layer, wherein the thickness of the separator layer is less than 1 .mu.m. A second conductive lead is electrically coupled to the collector layer.

  13. Energy compensated solid state gamma dosimeter

    SciTech Connect

    Sinclair, F.; Clapp, A.; Entine, G.; Kronenberg, S.

    1988-02-01

    Solid state semiconductor detectors using pulse mode detection are attractive candidates for real time dosimetry systems. Their high atomic number relative to that of tissue gives a nonlinear response as a function of the photon energy over the range from 30 keV to 10 MeV. An analytical model of a silicon PIN diode has been developed, including the photoelectric and Compton interactions as well as the ejection of the secondary electrons from the sensitive volume. The authors tested a nonlinear pulse height compensation algorithm using calibrated gamma and x-ray fluxes, and find that this approach improves the dose accuracy.

  14. Fast-neutron solid-state dosimeter

    DOEpatents

    Kecker, K.H.; Haywood, F.F.; Perdue, P.T.; Thorngate, J.H.

    1975-07-22

    This patent relates to an improved fast-neutron solid-state dosimeter that does not require separation of materials before it can be read out, that utilizes materials that do not melt or otherwise degrade at about 300$sup 0$C readout temperature, that provides a more efficient dosimeter, and that can be reused. The dosimeters are fabricated by intimately mixing a TL material, such as CaSO$sub 4$:Dy, with a powdered polyphenyl, such as p-sexiphenyl, and hot- pressing the mixture to form pellets, followed by out-gassing in a vacuum furnace at 150$sup 0$C prior to first use dosimeters. (auth)

  15. Programmable solid state atom sources for nanofabrication

    NASA Astrophysics Data System (ADS)

    Han, Han; Imboden, Matthias; Stark, Thomas; Del Corro, Pablo G.; Pardo, Flavio; Bolle, Cristian A.; Lally, Richard W.; Bishop, David J.

    2015-06-01

    In this paper we discuss the development of a MEMS-based solid state atom source that can provide controllable atom deposition ranging over eight orders of magnitude, from ten atoms per square micron up to hundreds of atomic layers, on a target ~1 mm away. Using a micron-scale silicon plate as a thermal evaporation source we demonstrate the deposition of indium, silver, gold, copper, iron, aluminum, lead and tin. Because of their small sizes and rapid thermal response times, pulse width modulation techniques are a powerful way to control the atomic flux. Pulsing the source with precise voltages and timing provides control in terms of when and how many atoms get deposited. By arranging many of these devices into an array, one has a multi-material, programmable solid state evaporation source. These micro atom sources are a complementary technology that can enhance the capability of a variety of nano-fabrication techniques.In this paper we discuss the development of a MEMS-based solid state atom source that can provide controllable atom deposition ranging over eight orders of magnitude, from ten atoms per square micron up to hundreds of atomic layers, on a target ~1 mm away. Using a micron-scale silicon plate as a thermal evaporation source we demonstrate the deposition of indium, silver, gold, copper, iron, aluminum, lead and tin. Because of their small sizes and rapid thermal response times, pulse width modulation techniques are a powerful way to control the atomic flux. Pulsing the source with precise voltages and timing provides control in terms of when and how many atoms get deposited. By arranging many of these devices into an array, one has a multi-material, programmable solid state evaporation source. These micro atom sources are a complementary technology that can enhance the capability of a variety of nano-fabrication techniques. Electronic supplementary information (ESI) available: A document containing further information about device characterization

  16. Solid State Marx Modulators for Emerging Applications

    SciTech Connect

    Kemp, M.A.; /SLAC

    2012-09-14

    Emerging linear accelerator applications increasingly push the boundaries of RF system performance and economics. The power modulator is an integral part of RF systems whose characteristics play a key role in the determining parameters such as efficiency, footprint, cost, stability, and availability. Particularly within the past decade, solid-state switch based modulators have become the standard in high-performance, high power modulators. One topology, the Marx modulator, has characteristics which make it particularly attractive for several emerging applications. This paper is an overview of the Marx topology, some recent developments, and a case study of how this architecture can be applied to a few proposed linear accelerators.

  17. The 60 GHz solid state power amplifier

    NASA Technical Reports Server (NTRS)

    Mcclymonds, J.

    1991-01-01

    A new amplifier architecture was developed during this contract that is superior to any other solid state approach. The amplifier produced 6 watts with 4 percent efficiency over a 2 GHz band at 61.5 GHz. The unit was 7 x 9 x 3 inches in size, 5.5 pounds in weight, and the conduction cooling through the baseplate is suitable for use in space. The amplifier used high efficiency GaAs IMPATT diodes which were mounted in 1-diode circuits, called modules. Eighteen modules were used in the design, and power combining was accomplished with a proprietary passive component called a combiner plate.

  18. Passivation-free solid state battery

    DOEpatents

    Abraham, Kuzhikalail M.; Peramunage, Dharmasena

    1998-01-01

    This invention pertains to passivation-free solid-state rechargeable batteries composed of Li.sub.4 Ti.sub.5 O.sub.12 anode, a solid polymer electrolyte and a high voltage cathode. The solid polymer electrolyte comprises a polymer host, such as polyacrylonitrile, poly(vinyl chloride), poly(vinyl sulfone), and poly(vinylidene fluoride), plasticized by a solution of a Li salt in an organic solvent. The high voltage cathode includes LiMn.sub.2 O.sub.4, LiCoO.sub.2, LiNiO.sub.2 and LiV.sub.2 O.sub.5 and their derivatives.

  19. Biosynthesis of highly enriched 13C-lycopene for human metabolic studies using repeated batch tomato cell culturing with 13C-glucose

    PubMed Central

    Moran, Nancy E.; Rogers, Randy B.; Lu, Chi-Hua; Conlon, Lauren E.; Lila, Mary Ann; Clinton, Steven K.; Erdman, John W.

    2013-01-01

    While putative disease-preventing lycopene metabolites are found in both tomato (Solanum lycopersicum) products and in their consumers, mammalian lycopene metabolism is poorly understood. Advances in tomato cell culturing techniques offer an economical tool for generation of highly-enriched 13C-lycopene for human bioavailability and metabolism studies. To enhance the 13C-enrichment and yields of labeled lycopene from the hp-1 tomato cell line, cultures were first grown in 13C-glucose media for three serial batches and produced increasing proportions of uniformly labeled lycopene (14.3 +/− 1.2 %, 39.6 +/− 0.5 %, and 48.9 +/− 1.5% with consistent yields (from 5.8 to 9 mg/L). An optimized 9-day-long 13C-loading and 18-day-long labeling strategy developed based on glucose utilization and lycopene yields, yielded 13C-lycopene with 93% 13C isotopic purity, and 55% of isotopomers were uniformly labeled. Furthermore, an optimized acetone and hexane extraction led to a four-fold increase in lycopene recovery from cultures compared to a standard extraction. PMID:23561155

  20. Solid-state NMR Reveals the Carbon-based Molecular Architecture of Cryptococcus neoformans Fungal Eumelanins in the Cell Wall*

    PubMed Central

    Chatterjee, Subhasish; Prados-Rosales, Rafael; Itin, Boris; Casadevall, Arturo; Stark, Ruth E.

    2015-01-01

    Melanin pigments protect against both ionizing radiation and free radicals and have potential soil remediation capabilities. Eumelanins produced by pathogenic Cryptococcus neoformans fungi are virulence factors that render the fungal cells resistant to host defenses and certain antifungal drugs. Because of their insoluble and amorphous characteristics, neither the pigment bonding framework nor the cellular interactions underlying melanization of C. neoformans have yielded to comprehensive molecular-scale investigation. This study used the C. neoformans requirement of exogenous obligatory catecholamine precursors for melanization to produce isotopically enriched pigment “ghosts” and applied 2D 13C-13C correlation solid-state NMR to reveal the carbon-based architecture of intact natural eumelanin assemblies in fungal cells. We demonstrated that the aliphatic moieties of solid C. neoformans melanin ghosts include cell-wall components derived from polysaccharides and/or chitin that are associated proximally with lipid membrane constituents. Prior to development of the mature aromatic fungal pigment, these aliphatic moieties form a chemically resistant framework that could serve as the scaffold for melanin synthesis. The indole-based core aromatic moieties show interconnections that are consistent with proposed melanin structures consisting of stacked planar assemblies, which are associated spatially with the aliphatic scaffold. The pyrrole aromatic carbons of the pigments bind covalently to the aliphatic framework via glycoside or glyceride functional groups. These findings establish that the structure of the pigment assembly changes with time and provide the first biophysical information on the mechanism by which melanin is assembled in the fungal cell wall, offering vital insights that can advance the design of bioinspired conductive nanomaterials and novel therapeutics. PMID:25825492

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

    PubMed

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

    2011-12-01

    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. PMID:21953355

  2. Synthesis Of 2h- And 13c-Substituted Dithanes

    DOEpatents

    Martinez, Rodolfo A.; Alvarez, Marc A.; Silks, III, Louis A.; Unkefer, Clifford J.

    2004-05-04

    The present invention is directed to labeled compounds, [2-.sup.13 C]dithane wherein the .sup.13 C atom is directly bonded to one or two deuterium atoms. The present invention is also directed to processes of preparing [2-.sup.13 C]dithane wherein the .sup.13 C atom is directly bonded to one or two deuterium atoms. The present invention is also directed to labeled compounds, e.g., [.sup.2 H.sub.1-2, .sup.13 C]methanol (arylthio)-, acetates wherein the .sup.13 C atom is directly bonded to exactly one or two deuterium atoms.

  3. Synthesis of 2H- and 13C-substituted dithanes

    DOEpatents

    Martinez, Rodolfo A.; Alvarez, Marc A.; Silks, III, Louis A.; Unkefer, Clifford J.

    2003-01-01

    The present invention is directed to labeled compounds, [2-.sup.13 C]dithiane wherein the .sup.13 C atom is directly bonded to one or two deuterium atoms. The present invention is also directed to processes of preparing [2-.sup.13 C]dithiane wherein the .sup.13 C atom is directly bonded to one or two deuterium atoms. The present invention is also directed to labeled compounds, e.g., [.sup.2 H.sub.1-2, .sup.13 C]methanol (arylthio)-, acetates wherein the .sup.13 C atom is directly bonded to exactly one or two deuterium atoms.

  4. Dynamic Nuclear Polarization (DNP) solid-state NMR spectroscopy, a new approach to study humic material?

    NASA Astrophysics Data System (ADS)

    Knicker, Heike; Lange, Sascha; van Rossum, Barth; Oschkinat, Hartmut

    2016-04-01

    Compared to solution NMR spectroscopy, solid-state NMR spectra suffer from broad resonance lines and low resolution. This could be overcome by the use of 2-dimenstional solid-state NMR pulse sequences. Until recently, this approach has been unfeasible as a routine tool in soil chemistry, mainly because of the low NMR sensitivity of the respective samples. A possibility to circumvent those sensitivity problems represents high-field Dynamic Nuclear Polarization (DNP) solid-state NMR spectroscopy (Barnes et al., 2008), allowing considerable signal enhancements (Akbey et al., 2010). This is achieved by a microwave-driven transfer of polarization from a paramagnetic center to nuclear spins. Application of DNP to MAS spectra of biological systems (frozen solutions) showed enhancements of the factor 40 to 50 (Hall et al., 1997). Enhancements of this magnitude, thus may enable the use of at least some of the 2D solid-state NMR techniques that are presently already applied for pure proteins but are difficult to apply to soil peptides in their complex matrix. After adjusting the required acquisition parameters to the system "soil organic matter", lower but still promising enhancement factors were achieved. Additional optimization was performed and allowed the acquisition of 2D 13C and 15N solid-state NMR spectra of humified 13C and 15N enriched plant residues. Within the present contribution, the first solid-state DNP NMR spectra of humic material are presented. Those data demonstrate the great potential of this approach which certainly opens new doors for a better understanding of biochemical processes in soils, sediments and water. Akbey, Ü., Franks, W.T., Linden, A., Lange, S., Griffin, R.G., van Rossum, B.-J., Oschkinat, H., 2010. Dynamic nuclear polarization of deuterated proteins. Angewandte Chemie International Edition 49, 7803-7806. Barnes, A.B., De Paëpe, G., van der Wel, P.C.A., Hu, K.N., Joo, C.G., Bajaj, V.S., Mak-Jurkauskas, M.L., Sirigiri, J.R., Herzfeld, J

  5. In vivo dynamic turnover of cerebral 13C isotopomers from [U- 13C]glucose

    NASA Astrophysics Data System (ADS)

    Xu, Su; Shen, Jun

    2006-10-01

    An INEPT-based 13C MRS method and a cost-effective and widely available 11.7 Tesla 89-mm bore vertical magnet were used to detect dynamic 13C isotopomer turnover from intravenously infused [U- 13C]glucose in a 211 μL voxel located in the adult rat brain. The INEPT-based 1H → 13C polarization transfer method is mostly adiabatic and therefore minimizes signal loss due to B 1 inhomogeneity of the surface coils used. High quality and reproducible data were acquired as a result of combined use of outer volume suppression, ISIS, and the single-shot three-dimensional localization scheme built in the INEPT pulse sequence. Isotopomer patterns of both glutamate C4 at 34.00 ppm and glutamine C4 at 31.38 ppm are dominated first by a doublet originated from labeling at C4 and C5 but not at C3 (with 1JC4C5 = 51 Hz) and then by a quartet originated from labeling at C3, C4, and C5 (with 1JC3C4 = 35 Hz). A lag in the transition of glutamine C4 pattern from doublet-dominance to quartet dominance as compared to glutamate C4 was observed, which provides an independent verification of the precursor-product relationship between neuronal glutamate and glial glutamine and a significant intercompartmental cerebral glutamate-glutamine cycle between neurons and glial cells.

  6. Calculation of total meal d13C from individual food d13C.

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Variations in the isotopic signature of carbon in biological samples can be used to distinguish dietary patterns and monitor shifts in metabolism. But for these variations to have meaning, the isotopic signature of the diet must be known. We sought to determine if knowledge of the 13C isotopic abund...

  7. Nanocrystal-enabled solid state bonding.

    SciTech Connect

    San Diego State University, San Diego, CA; Puskar, Joseph David; Tikare, Veena; Garcia Cardona, Cristina; Reece, Mark; Brewer, Luke N.; Holm, Elizabeth Ann

    2010-10-01

    In this project, we performed a preliminary set of sintering experiments to examine nanocrystal-enabled diffusion bonding (NEDB) in Ag-on-Ag and Cu-on-Cu using Ag nanoparticles. The experimental test matrix included the effects of material system, temperature, pressure, and particle size. The nanoparticle compacts were bonded between plates using a customized hot press, tested in shear, and examined post mortem using microscopy techniques. NEDB was found to be a feasible mechanism for low-temperature, low-pressure, solid-state bonding of like materials, creating bonded interfaces that were able to support substantial loads. The maximum supported shear strength varied substantially within sample cohorts due to variation in bonded area; however, systematic variation with fabrication conditions was also observed. Mesoscale sintering simulations were performed in order to understand whether sintering models can aid in understanding the NEDB process. A pressure-assisted sintering model was incorporated into the SPPARKS kinetic Monte Carlo sintering code. Results reproduce most of the qualitative behavior observed in experiments, indicating that simulation can augment experiments during the development of the NEDB process. Because NEDB offers a promising route to low-temperature, low-pressure, solid-state bonding, we recommend further research and development with a goal of devising new NEDB bonding processes to support Sandia's customers.

  8. Solid-state power conversion handbook

    SciTech Connect

    Tarter, R.E.

    1993-01-01

    This new handbook is the first to be devoted to the field of solid-state power conversion. The material in this book is to be used in engineering practice and is oriented toward application rather than theory. The purpose of the book is to assemble in a single volume all the pertinent and comprehensive information necessary to meet the growing demands placed upon solid-state power conversion equipment. These demands include increased efficiency, improved reliability, higher packaging density, improved performance, and meeting safety and electromagnetic compatibility (EMC) requirements. The material presented includes a thorough analysis of fundamental electrical and magnetic aspects of power conversion plus thermal, protection, and reliability considerations. Attention is focused on semi-conductor and magnetic components and on analysis of various topologies. The handbook is organized into four sections. (1) Chapters 1-3 present the relations of various waveforms, transient components with emphasis on power semiconductors and magnetic components. (2) Chapters 4-12 deal with single-level conversion of rectifier circuits, filters, inverters and converters, feedback and stability analysis, and modulators and pulse-forming networks. (3) Chapters 13-16 discuss ancillary topics related to safety, EMC, thermal management, and reliability. (4) Chapters 17-19 cover design and operation of power supplies and systems from a detailed building block standpoint.

  9. A Model of Solid State Gas Sensors

    NASA Astrophysics Data System (ADS)

    Woestman, J. T.; Brailsford, A. D.; Shane, M.; Logothetis, E. M.

    1997-03-01

    Solid state gas sensors are widely used to measure the concentrations of gases such as CO, CH_4, C_3H_6, H_2, C_3H8 and O2 The applications of these sensors range from air-to-fuel ratio control in combustion processes including those in automotive engines and industrial furnaces to leakage detection of inflammable and toxic gases in domestic and industrial environments. As the need increases to accurately measure smaller and smaller concentrations, problems such as poor selectivity, stability and response time limit the use of these sensors. In an effort to overcome some of these limitations, a theoretical model of the transient behavior of solid state gas sensors has been developed. In this presentation, a model for the transient response of an electrochemical gas sensor to gas mixtures containing O2 and one reducing species, such as CO, is discussed. This model accounts for the transport of the reactive species to the sampling electrode, the catalyzed oxidation/reduction reaction of these species and the generation of the resulting electrical signal. The model will be shown to reproduce the results of published steady state models and to agree with experimental steady state and transient data.

  10. The 20 GHz spacecraft IMPATT solid state transmitter

    NASA Technical Reports Server (NTRS)

    Best, T.; Ngan, Y. C.

    1986-01-01

    The engineering development of a solid-state transmitter amplifier operating in the 20-GHz frequency range is described. This effort involved a multitude of disciplines including IMPATT device development, circulator design, multiple-diode circuit design, and amplifier integration and test. The objective was to develop a transmitter amplifier demonstrating the feasibility of providing an efficient, reliable, lightweight solid-state transmitter to be flown on a 30 to 20 GHz communication demonstration satellite. The work was done under contract from NASA/Lewis Research Center for a period of three years. The result was the development of a GaAs IMPACT diode amplifier capable of an 11-W CW output power and a 2-dB bandwidth of 300 MHz. GaAs IMPATT diodes incorporating diamond heatsink and double-Read doping profile capable of 5.3-W CW oscillator output power and 15.5% efficiency were developed. Up to 19% efficiency was also observed for an output power level of 4.4 W. High performance circulators with a 0.2 dB inserting loss and bandwidth of 5 GHz have also been developed. These represent a significant advance in both device and power combiner circuit technologies in K-band frequencies.

  11. In-Situ Creation of Solid State Nanopores

    NASA Astrophysics Data System (ADS)

    Briggs, Kyle; Kwok, Harold; Tabard-Cossa, Vincent

    2013-03-01

    Recent advances in nanopore technology have demonstrated that they are a powerful tool for single biomolecule analysis, and great progress has been made toward the promise of nanopore-based DNA sequencing devices. A limiting factor in solid-state nanopore science is the complexity, throughput and cost of current fabrication methods, based on focused ion or election beam drilling, which require sophisticated equipment and highly trained personnel. Our laboratory at the University of Ottawa has demonstrated a simple and extremely low cost method to fabricate individual nanopores on thin solid-state membranes. By controlling an applied voltage across the membrane in aqueous salt solution, we are able to routinely create sub-5nm pores in dielectric membranes. In addition, the method can easily be extended to tune nanopore size with sub-nm precision. We will describe the fabrication method in detail, and present the effects of electric field strength, membrane material, solution salt composition, concentration and pH on the pore creation time and size distribution. These results allow us to elucidate the physical mechanisms responsible for nanopore formation.

  12. Analyses of Technology for Solid State Coherent Lidar

    NASA Technical Reports Server (NTRS)

    Amzajerdian, Farzin

    1997-01-01

    Over past few years, considerable advances have been made in the areas of the diode-pumped, eye-safe, solid state lasers and room temperature, wide bandwidth, semiconductor detectors operating in the near-infrared region. These advances have created new possibilities for the development of reliable and compact coherent lidar systems for a wide range of applications. This research effort is aimed at further developing solid state coherent lidar technology for remote sensing of atmospheric processes such as wind, turbulence and aerosol concentration. The work performed by the UAH personnel under this Delivery Order concentrated on design and analyses of laboratory experiments and measurements, and development of advanced lidar optical subsystems in support of solid state laser radar remote sensing systems which are to be designed, deployed, and used to measure atmospheric processes and constituents. Under this delivery order, a lidar breadboard system was designed and analyzed by considering the major aircraft and space operational requirements. The lidar optical system was analyzed in detail using SYNOPSIS and Code V optical design packages. The lidar optical system include a wedge scanner and the compact telescope designed by the UAH personnel. The other major optical components included in the design and analyses were: polarizing beam splitter, routing mirrors, wave plates, signal beam derotator, and lag angle compensator. This lidar system is to be used for demonstrating all the critical technologies for the development of a reliable and low-cost space-based instrument capable of measuring global wind fields. A number of laboratory experiments and measurements were performed at the NASA/MSFC Detector Characterization Facility, previously developed by the UAH personnel. These laboratory measurements include the characterization of a 2-micron InGaAs detectors suitable for use in coherent lidars and characterization of Holographic Optical Element Scanners. UAH

  13. Zero-quantum stochastic dipolar recoupling in solid state nuclear magnetic resonance

    NASA Astrophysics Data System (ADS)

    Qiang, Wei; Tycko, Robert

    2012-09-01

    We present the theoretical description and experimental demonstration of a zero-quantum stochastic dipolar recoupling (ZQ-SDR) technique for solid state nuclear magnetic resonance (NMR) studies of 13C-labeled molecules, including proteins, under magic-angle spinning (MAS). The ZQ-SDR technique combines zero-quantum recoupling pulse sequence blocks with randomly varying chemical shift precession periods to create randomly amplitude- and phase-modulated effective homonuclear magnetic dipole-dipole couplings. To a good approximation, couplings between different 13C spin pairs become uncorrelated under ZQ-SDR, leading to spin dynamics (averaged over many repetitions of the ZQ-SDR sequence) that are fully described by an orientation-dependent N × N polarization transfer rate matrix for an N-spin system, with rates that are inversely proportional to the sixth power of internuclear distances. Suppression of polarization transfers due to non-commutivity of pairwise couplings (i.e., dipolar truncation) does not occur under ZQ-SDR, as we show both analytically and numerically. Experimental demonstrations are reported for uniformly 13C-labeled L-valine powder (at 14.1 T and 28.00 kHz MAS), uniformly 13C-labeled protein GB1 in microcrystalline form (at 17.6 T and 40.00 kHz MAS), and partially labeled 13C-labeled protein GB1 (at 14.1 T and 40.00 kHz MAS). The experimental results verify that spin dynamics under ZQ-SDR are described accurately by rate matrices and suggest the utility of ZQ-SDR in structural studies of 13C-labeled solids.

  14. Simultaneous imaging of 13C metabolism and 1H structure: technical considerations and potential applications.

    PubMed

    Gordon, Jeremy W; Fain, Sean B; Niles, David J; Ludwig, Kai D; Johnson, Kevin M; Peterson, Eric T

    2015-05-01

    Real-time imaging of (13)C metabolism in vivo has been enabled by recent advances in hyperpolarization. As a result of the inherently low natural abundance of endogenous (13)C nuclei, hyperpolarized (13)C images lack structural information that could be used to aid in motion detection and anatomical registration. Motion before or during the (13)C acquisition can therefore result in artifacts and misregistration that may obscure measures of metabolism. In this work, we demonstrate a method to simultaneously image both (1)H and (13)C nuclei using a dual-nucleus spectral-spatial radiofrequency excitation and a fully coincident readout for rapid multinuclear spectroscopic imaging. With the appropriate multinuclear hardware, and the means to simultaneously excite and receive on both channels, this technique is straightforward to implement requiring little to no increase in scan time. Phantom and in vivo experiments were performed with both Cartesian and spiral trajectories to validate and illustrate the utility of simultaneous acquisitions. Motion compensation of dynamic metabolic measurements acquired during free breathing was demonstrated using motion tracking derived from (1)H data. Simultaneous multinuclear imaging provides structural (1)H and metabolic (13)C images that are correlated both spatially and temporally, and are therefore amenable to joint (1)H and (13)C analysis and correction of structure-function images. PMID:25810146

  15. Solid-state curved focal plane arrays

    NASA Technical Reports Server (NTRS)

    Nikzad, Shouleh (Inventor); Hoenk, Michael (Inventor); Jones, Todd (Inventor)

    2010-01-01

    The present invention relates to curved focal plane arrays. More specifically, the present invention relates to a system and method for making solid-state curved focal plane arrays from standard and high-purity devices that may be matched to a given optical system. There are two ways to make a curved focal plane arrays starting with the fully fabricated device. One way, is to thin the device and conform it to a curvature. A second way, is to back-illuminate a thick device without making a thinned membrane. The thick device is a special class of devices; for example devices fabricated with high purity silicon. One surface of the device (the non VLSI fabricated surface, also referred to as the back surface) can be polished to form a curved surface.

  16. Solid-state lighting technology perspective.

    SciTech Connect

    Tsao, Jeffrey Yeenien; Coltrin, Michael Elliott

    2006-08-01

    Solid-State Lighting (SSL) uses inorganic light-emitting diodes (LEDs) and organic light-emitting diodes (OLEDs) to convert electricity into light for illumination. SSL has the potential for enormous energy savings and accompanying environmental benefits if its promise of 50% (or greater) energy efficiencies can be achieved. This report provides a broad summary of the technologies that underlie SSL. The applications for SSL and potential impact on U.S. and world-wide energy consumption, and impact on the human visual experience are discussed. The properties of visible light and different technical metrics to characterize its properties are summarized. The many factors contributing to the capital and operating costs for SSL and traditional lighting sources (incandescent, fluorescent, and high-intensity discharge lamps) are discussed, with extrapolations for future SSL goals. The technologies underlying LEDs and OLEDs are also described, including current and possible alternative future technologies and some of the present limitations.

  17. Solid-state ring laser gyroscope

    NASA Astrophysics Data System (ADS)

    Schwartz, S.

    The ring laser gyroscope is a rotation sensor used in most kinds of inertial navigation units. It usually consists in a ring cavity filled with a mixture of helium and neon, together with high-voltage pumping electrodes. The use of a gaseous gain medium, while resulting naturally in a stable bidirectional regime enabling rotation sensing, is however the main industrially limiting factor for the ring laser gyroscopes in terms of cost, reliability and lifetime. We study in this book the possibility of substituting for the gaseous gain medium a solid-state medium (diode-pumped Nd-YAG). For this, a theoretical and experimental overview of the lasing regimes of the solid-state ring laser is reported. We show that the bidirectional emission can be obtained thanks to a feedback loop acting on the states of polarization and inducing differential losses proportional to the difference of intensity between the counterpropagating modes. This leads to the achievement of a solid-state ring laser gyroscope, whose frequency response is modified by mode coupling effects. Several configurations, either mechanically or optically based, are then successively studied, with a view to improving the quality of this frequency response. In particular, vibration of the gain crystal along the longitudinal axis appears to be a very promising technique for reaching high inertial performances with a solid-state ring laser gyroscope. Gyrolaser à état solide. Le gyrolaser est un capteur de rotation utilisé dans la plupart des centrales de navigation inertielle. Dans sa forme usuelle, il est constitué d'une cavité laser en anneau remplie d'un mélange d'hélium et de néon pompé par des électrodes à haute tension. L'utilisation d'un milieu amplificateur gazeux, si elle permet de garantir naturellement le fonctionnement bidirectionnel stable nécessaire à la mesure des rotations, constitue en revanche la principale limitation industrielle des gyrolasers actuels en termes de coût, fiabilit

  18. Enhanced electrodes for solid state gas sensors

    DOEpatents

    Garzon, Fernando H.; Brosha, Eric L.

    2001-01-01

    A solid state gas sensor generates an electrical potential between an equilibrium electrode and a second electrode indicative of a gas to be sensed. A solid electrolyte substrate has the second electrode mounted on a first portion of the electrolyte substrate and a composite equilibrium electrode including conterminous transition metal oxide and Pt components mounted on a second portion of the electrolyte substrate. The composite equilibrium electrode and the second electrode are electrically connected to generate an electrical potential indicative of the gas that is being sensed. In a particular embodiment of the present invention, the second electrode is a reference electrode that is exposed to a reference oxygen gas mixture so that the electrical potential is indicative of the oxygen in a gas stream.

  19. Solid state synthesis of calcium borohydroxyapatite

    NASA Astrophysics Data System (ADS)

    Güler, H.; Gündoğmaz, G.; Kurtuluş, F.; Çelik, G.; Gacanoğlu, Ş. S.

    2011-11-01

    Calcium borohydroxyapatite was synthesized by the solid-state reaction of colemanite (Ca 2B 6O 11·5H 2O) and diamonium hydrogenphosphate ((NH 4) 2HPO 4) at 1200 °C for 12 h. X-ray diffraction pattern showed only the formation of calcium borohydroxyapatite. The experimental analysis assigned the chemical formula as Ca 10[(PO 4) 5.80(BO 3) 0.20](OH) 2. It was indexed in the hexagonal system with the refined unit cell parameters of a = 9.557(3) Å, c = 6.926(8) Å and space group P6 3/ m. The experimental results verified that if colemanite was used as a primary reactant for both calcium and boron source, the calcium borohydroxyapatite could be obtained.

  20. Experimental aspects of solid-state voltammetry

    SciTech Connect

    Wooster, T.T.; Longmire, M.L.; Zhang, H.

    1992-05-15

    This paper describes the properties of poly(ether) polymer electrolytes as solvent media for solid-state voltammetry. Experimental requirements for microelectrode voltammetry and results for the dependency of diffusive transport of electroactive solutes on polymer solvent molecular weight, structure, and temperature (and related phase state) are described for eight poly(ether)s: linear poly(ethylene oxides) MW = 400, 1000, 2000, and 600 000 (Me{sub 2}PEG-400, Me{sub 2}PEG-1000, Me{sub 2}PEG-2000, PEO-600 000), linear poly(propylene oxide) MW = 4000 (PPO-4000), the comb polymer poly(bis[(methoxyethoxy)ethoxy]phosphazine) (MEEP), the block copolymer poly(ether)-poly(urethane urea)(PEUU), and the cross-linked poly(ether) network PEO. 28 refs., 10 figs., 1 tab.

  1. Radioactive isotopes in solid state physics

    NASA Astrophysics Data System (ADS)

    Forkel-Wirth, D.

    1996-04-01

    A wide range of solid state physics techniques is using radioactive ion beams, both from on-line and off-line separators. The different techniques can be roughly subdivided into two classes: one, including the hyperfine techniques like Mößbauer spectroscopy (MS), Perturbed Angular Correlation (PAC) spectroscopy, β-NMR and the ion-beam technique of Emission Channeling (EC). They all crucially depend on the availability of radioactive isotopes with very specific decay properties. The second group comprises radio-tracer techniques which combine radioactive probe atoms with conventional semiconductor physics methods like Deep Level Transient Spectroscopy (DLTS), Capacitance Voltage measurements (CV), Hall-effect measurements or Photoluminescence Spectroscopy (PL). They are perfectly feasible without any radioactive probe atom, however, using such isotopes enables the unambiguous chemical identification of impurities. The present paper gives an overview on the potential of nuclear techniques by describing some typical experiments.

  2. Compact high voltage solid state switch

    DOEpatents

    Glidden, Steven C.

    2003-09-23

    A compact, solid state, high voltage switch capable of high conduction current with a high rate of current risetime (high di/dt) that can be used to replace thyratrons in existing and new applications. The switch has multiple thyristors packaged in a single enclosure. Each thyristor has its own gate drive circuit that circuit obtains its energy from the energy that is being switched in the main circuit. The gate drives are triggered with a low voltage, low current pulse isolated by a small inexpensive transformer. The gate circuits can also be triggered with an optical signal, eliminating the trigger transformer altogether. This approach makes it easier to connect many thyristors in series to obtain the hold off voltages of greater than 80 kV.

  3. Solid state dye laser for medical applications

    NASA Astrophysics Data System (ADS)

    Aldag, Henry R.

    1994-06-01

    The development of solid state dye lasers could lead to a major breakthrough in the cost and compactness of a medical device. Advantages include: elimination of the flow system for the gain medium; ease with which to implement wavelength agility or the replacement of a degraded rod or sheet; and toxicity and flammability become a non-issue. Dye lasers have played a role in cardiology, dermatology, and urology. Of these cardiology is of interest to Palomar. The Palomar Model 3010 flashlamp-pumped dye laser medical device was used during phase 1 FDA clinical trials to break-up blood clots that cause heart attacks, a process known as coronary laser thrombolysis. It is the objective of this research and development effort to produce solid matrix lasers that will replace liquid dye lasers in these medical specialties.

  4. Efficient scalable solid-state neutron detector

    SciTech Connect

    Moses, Daniel

    2015-06-15

    We report on scalable solid-state neutron detector system that is specifically designed to yield high thermal neutron detection sensitivity. The basic detector unit in this system is made of a {sup 6}Li foil coupled to two crystalline silicon diodes. The theoretical intrinsic efficiency of a detector-unit is 23.8% and that of detector element comprising a stack of five detector-units is 60%. Based on the measured performance of this detector-unit, the performance of a detector system comprising a planar array of detector elements, scaled to encompass effective area of 0.43 m{sup 2}, is estimated to yield the minimum absolute efficiency required of radiological portal monitors used in homeland security.

  5. Solid-state spectral transmissometer and radiometer

    NASA Technical Reports Server (NTRS)

    Carder, K. L.; Steward, R. G.; Payne, P. R.

    1985-01-01

    An in situ instrument designed to measure the spectral attenuation coefficient of seawater and the ocean remote-sensing reflectance from 400 to 750 nm is in the test and development stage. It employs a 256 channel, charge-coupled type of linear array measuring the spectral intensities diffracted by a grating. Examples of the types of data delivered by this instrument have been simulated using a breadboard laboratory instrument and an above-water, solid-state radiometer. Algorithms developed using data from these instruments provide measures of chlorophyll a plus phaeophytin a concentrations from less than 0.1 to 77.0 mg/cu m, gelbstoff spectral absorption coefficients, and detrital spectral backscattering coefficients for waters of the west Florida shelf.

  6. Electronically shielded solid state charged particle detector

    DOEpatents

    Balmer, D.K.; Haverty, T.W.; Nordin, C.W.; Tyree, W.H.

    1996-08-20

    An electronically shielded solid state charged particle detector system having enhanced radio frequency interference immunity includes a detector housing with a detector entrance opening for receiving the charged particles. A charged particle detector having an active surface is disposed within the housing. The active surface faces toward the detector entrance opening for providing electrical signals representative of the received charged particles when the received charged particles are applied to the active surface. A conductive layer is disposed upon the active surface. In a preferred embodiment, a nonconductive layer is disposed between the conductive layer and the active surface. The conductive layer is electrically coupled to the detector housing to provide a substantially continuous conductive electrical shield surrounding the active surface. The inner surface of the detector housing is supplemented with a radio frequency absorbing material such as ferrite. 1 fig.

  7. Supramolecular interactions in the solid state

    PubMed Central

    Resnati, Giuseppe; Boldyreva, Elena; Bombicz, Petra; Kawano, Masaki

    2015-01-01

    In the last few decades, supramolecular chemistry has been at the forefront of chemical research, with the aim of understanding chemistry beyond the covalent bond. Since the long-range periodicity in crystals is a product of the directionally specific short-range intermolecular interactions that are responsible for molecular assembly, analysis of crystalline solids provides a primary means to investigate intermolecular interactions and recognition phenomena. This article discusses some areas of contemporary research involving supramolecular interactions in the solid state. The topics covered are: (1) an overview and historical review of halogen bonding; (2) exploring non-ambient conditions to investigate intermolecular interactions in crystals; (3) the role of intermolecular interactions in morphotropy, being the link between isostructurality and polymorphism; (4) strategic realisation of kinetic coordination polymers by exploiting multi-interactive linker molecules. The discussion touches upon many of the prerequisites for controlled preparation and characterization of crystalline materials. PMID:26594375

  8. Solid state potentiometric gaseous oxide sensor

    NASA Technical Reports Server (NTRS)

    Wachsman, Eric D. (Inventor); Azad, Abdul Majeed (Inventor)

    2003-01-01

    A solid state electrochemical cell (10a) for measuring the concentration of a component of a gas mixture (12) includes first semiconductor electrode (14) and second semiconductor electrode (16) formed from first and second semiconductor materials, respectively. The materials are selected so as to undergo a change in resistivity upon contacting a gas component, such as CO or NO. An electrolyte (18) is provided in contact with the first and second semiconductor electrodes. A reference cell can be included in contact with the electrolyte. Preferably, a voltage response of the first semiconductor electrode is opposite in slope direction to that of the second semiconductor electrode to produce a voltage response equal to the sum of the absolute values of the control system uses measured pollutant concentrations to direct adjustment of engine combustion conditions.

  9. Electronically shielded solid state charged particle detector

    SciTech Connect

    Balmer, D.K.; Haverty, T.W.; Nordin, C.W.; Tyree, W.H.

    1995-12-31

    An electronically shielded solid state charged particle detector system having enhanced radio frequency interference immunity includes a detector housing with a detector entrance opening for receiving the charged particles. A charged particle detector having an active surface is disposed within the housing. The active surface faces toward the detector entrance opening for providing electrical signals representative of the received charged particles when the received charged particles are applied to the active surface. A conductive layer is disposed upon the active surface. In a preferred embodiment, a nonconductive layer is disposed between the conductive layer and the active surface. The conductive layer is electrically coupled to the detector housing to provide a substantially continuous conductive electrical shield surrounding the active surface. The inner surface of the detector housing is supplemented with a radio frequency absorbing material such as ferrite.

  10. Efficient scalable solid-state neutron detector

    NASA Astrophysics Data System (ADS)

    Moses, Daniel

    2015-06-01

    We report on scalable solid-state neutron detector system that is specifically designed to yield high thermal neutron detection sensitivity. The basic detector unit in this system is made of a 6Li foil coupled to two crystalline silicon diodes. The theoretical intrinsic efficiency of a detector-unit is 23.8% and that of detector element comprising a stack of five detector-units is 60%. Based on the measured performance of this detector-unit, the performance of a detector system comprising a planar array of detector elements, scaled to encompass effective area of 0.43 m2, is estimated to yield the minimum absolute efficiency required of radiological portal monitors used in homeland security.

  11. Efficient scalable solid-state neutron detector.

    PubMed

    Moses, Daniel

    2015-06-01

    We report on scalable solid-state neutron detector system that is specifically designed to yield high thermal neutron detection sensitivity. The basic detector unit in this system is made of a (6)Li foil coupled to two crystalline silicon diodes. The theoretical intrinsic efficiency of a detector-unit is 23.8% and that of detector element comprising a stack of five detector-units is 60%. Based on the measured performance of this detector-unit, the performance of a detector system comprising a planar array of detector elements, scaled to encompass effective area of 0.43 m(2), is estimated to yield the minimum absolute efficiency required of radiological portal monitors used in homeland security. PMID:26133869

  12. Principles of solid-state power conversion

    NASA Astrophysics Data System (ADS)

    Tarter, R. E.

    1985-12-01

    The purpose of this book is to assemble, in one place, the comprehensive tools necessary to meet the growing demands placed upon solid-state power conversion equipment. Aspects of transient analysis, circuit analysis, and waveforms are discussed, taking into account waveform relations, magnetic fields, dielectric fields, the RL circuit, the RC circuit, the RLC circuit, the RLCR circuit with a DC input, AC circuit analysis, and components scaling. Semiconductors and resistors are considered along with capacitors, transformers, inductors, conductors, rectifiers and filters, phase-control circuits, transistor inverters, thyristor inverters, switching regulators, DC-DC converters, protection and safety, electromagnetic compatibility and grounding, semiconductor and equipment cooling, reliability and quality, regulated power supplies, and uninterruptible power systems. Attention is given to magnetic materials, toroid tape core transformers, permalloy powder cores, a six-phase dual bridge, thermal conduction and resistance, heat pipes, and thermoelectric coolers.

  13. Solid state neutron dosimeter for space applications

    SciTech Connect

    Nagarkar, V.; Entine, G.; Stoppel, P.; Cirignano, L. ); Swinehart, P. )

    1992-08-01

    One of the most important contributions to the radiation exposure of astronauts engaged in space flight is the significant flux of high energy neutrons arising from both primary and secondary sources of ionizing radiation. Under NASA sponsorship, the authors are developing a solid state neutron sensor capable of being incorporated into a very compact, flight instrument to provide high quality real time measurement of this important radiation flux. The dosimeter uses a special, high neutron sensitivity, PIN diode that is insensitive t the other forms of ionizing radiation. The dosimeter will have the ability to measure and record neutron dose over a range of 50 microgray to tens of milligrays (5 millirads to several rads) over a flight of up to 30 days. the performance characteristics of the PIN diode with a detailed description of the overall dosimeter is presented. in this paper.

  14. High-efficiency solid state power amplifier

    NASA Technical Reports Server (NTRS)

    Wallis, Robert E. (Inventor); Cheng, Sheng (Inventor)

    2005-01-01

    A high-efficiency solid state power amplifier (SSPA) for specific use in a spacecraft is provided. The SSPA has a mass of less than 850 g and includes two different X-band power amplifier sections, i.e., a lumped power amplifier with a single 11-W output and a distributed power amplifier with eight 2.75-W outputs. These two amplifier sections provide output power that is scalable from 11 to 15 watts without major design changes. Five different hybrid microcircuits, including high-efficiency Heterostructure Field Effect Transistor (HFET) amplifiers and Monolithic Microwave Integrated Circuit (MMIC) phase shifters have been developed for use within the SSPA. A highly efficient packaging approach enables the integration of a large number of hybrid circuits into the SSPA.

  15. Electronically shielded solid state charged particle detector

    DOEpatents

    Balmer, David K.; Haverty, Thomas W.; Nordin, Carl W.; Tyree, William H.

    1996-08-20

    An electronically shielded solid state charged particle detector system having enhanced radio frequency interference immunity includes a detector housing with a detector entrance opening for receiving the charged particles. A charged particle detector having an active surface is disposed within the housing. The active surface faces toward the detector entrance opening for providing electrical signals representative of the received charged particles when the received charged particles are applied to the active surface. A conductive layer is disposed upon the active surface. In a preferred embodiment, a nonconductive layer is disposed between the conductive layer and the active surface. The conductive layer is electrically coupled to the detector housing to provide a substantially continuous conductive electrical shield surrounding the active surface. The inner surface of the detector housing is supplemented with a radio frequency absorbing material such as ferrite.

  16. Solid State Technology Meets Collider Challenge

    SciTech Connect

    Hazi, A

    2005-09-20

    Probing the frontiers of particle physics and delving into the mysteries of the universe and its beginnings require machines that can accelerate beams of fundamental particles to very high energies and then collide those beams together, producing a multitude of exotic subatomic particles. The proposed Next Linear Collider (NLC), being developed by Stanford Linear Accelerator Center (SLAC), Lawrence Livermore and Lawrence Berkeley national laboratories, and Fermi National Accelerator Laboratory (Fermilab), is such a machine. The NLC is expected to produce a variety of subatomic particles by smashing together electrons and their antimatter counterparts (positrons) at nearly the speed of light with energies in the teraelectronvolt (TeV) range. Plans are that the NLC will initially operate at 0.5 TeV and ultimately be scaled up to 1.5 TeV. (See S&TR, April 2000, pp. 12-16.) Work at the facility will complement the research to be conducted at another high-energy particle accelerator, the 14-TeV Large Hadron Collider at the European Laboratory for Particle Physics (commonly known by the acronym CERN from its former name) in Geneva, which is scheduled for completion in 2007. Achieving beam energy levels in the TeV range requires modulator systems that can convert ac line power--the same type of power one gets from the wall plug--into dc pulses. Ultimately, these pulses are transformed into radiofrequency (rf) pulses that ''kick'' the particles up to the required energy levels. Livermore scientists and engineers have designed a solid-state modulator to replace oldstyle modulators based on vacuum-tube technology. These new modulators promise to be far more efficient, reliable, and serviceable than the previous components. Livermore's Laboratory Directed Research and Development Program supported the basic research and development on the solid-state modulator technology, and SLAC supported the systems integration.

  17. Characterization of a 30-GHz IMPATT solid state amplifier

    NASA Technical Reports Server (NTRS)

    Wald, Lawrence W.

    1988-01-01

    Described are the characterization and testing of a 20 W solid state amplifier operating in the Ka band to be used in low cost experimental ground terminals. The amplifier was developed by the TRW Electronic Systems Group under NASA Contract NAS3-23266 as a proof-of-concept (POC) device in support of the Advanced Communications Technology Satellite (ACTS) program. Additional goals were development of high-power IMPATT devices and circulators, and multistage diode circuits, which are an integral part of the amplifier. The amplifier underwent acceptance testing at the NASA Lewis Research Center, Cleveland, Ohio. Characteristics measured include the output power of 42 dB m, gain of 30 dB, an injection-locking RF bandwidth of 260 MHz, and an overall direct current-to-radiofrequency (dc-to-RF) efficiency of 6.7 percent.

  18. Modeling of Material Removal by Solid State Heat Capacity Lasers

    SciTech Connect

    Boley, C D; Rubenchik, A M

    2002-04-17

    Pulsed lasers offer the capability of rapid material removal. Here we present simulations of steel coupon tests by two solid state heat capacity lasers built at LLNL. Operating at 1.05 pm, these deliver pulse energies of about 80 J at 10 Hz, and about 500 J at 20 Hz. Each is flashlamp-pumped. The first laser was tested at LLNL, while the second laser has been delivered to HELSTF, White Sands Missile Range. Liquid ejection appears to be an important removal mechanism. We have modeled these experiments via a time-dependent code called THALES, which describes heat transport, melting, vaporization, and the hydrodynamics of liquid, vapor, and air. It was previously used, in a less advanced form, to model drilling by copper vapor lasers [1] . It was also used to model vaporization in beam dumps for a high-power laser [2]. The basic model is in 1D, while the liquid hydrodynamics is handled in 2D.

  19. NMR doesn't lie or how solid-state NMR spectroscopy contributed to a better understanding of the nature and function of soil organic matter (Philippe Duchaufour Medal Lecture)

    NASA Astrophysics Data System (ADS)

    Knicker, Heike

    2016-04-01

    for organo-mineral interactions. Since decent solid-state NMR spectra cannot be obtained from graphenic components, the successful acquisition of solid-state 13C and 15N NMR spectra of charcoals challenged the well accepted model of their chemical nature. Application of advanced 2D NMR approaches confirmed the new view of charcoal as a heterogeneous material, the composition of which depends upon the feedstock and charring condition. The respective consequences of this alternative for the understanding of C sequestration are still matter of ongoing debates. Although the sensitivity of 15N for NMR spectroscopy is 50 times lower than that of 13C, first solid-state 15N NMR spectra of soils with natural 15N abundance were already published in the 1990's. They clearly identified peptide-like structures as the main organic N form in unburnt soils. However, in spite of their high contribution to SOM, the role of peptides in soils is far from understood. Considering the new technological developments in the field of NMR spectroscopy, this technique will certainly not stop to contribute to unexpected results.

  20. The cluster and single-particle states in 13C (α,α)13C reactions

    NASA Astrophysics Data System (ADS)

    Mynbayev, N. A.; Nurmukhanbetova, A. K.; Goldberg, V. Z.; Rogachev, G. V.; Golovkov, M. S.; Koloberdin, M.; Ivanov, I.; Nauruzbayev, D. K.; Berdibek, Sh S.; Rakhymzhanov, A. M.; Tribble, R. E.

    2016-06-01

    The excitation functions of elastic scattering of 13C on alpha particle have been measured using the thick-target inverse kinematic method at the heavy ion DC-60 cyclotron. The helium gas was used as a target and also as a degrader to stop the beam. New data (including 180°degree) of the resonances close to the threshold in 17O have been obtained.

  1. Arabidopsis thalianafrom Polarization Transfer Solid-State NMR

    SciTech Connect

    White, Paul B; Wang, Tuo; Park, Yong Bum; Cosgrove, Daniel J; Hong, Mei

    2014-07-23

    Polysaccharide-rich plant cell walls are hydrated under functional conditions, but the molecular interactions between water and polysaccharides in the wall have not been investigated. In this work, we employ polarization transfer solid-state NMR techniques to study the hydration of primary-wall polysaccharides of the model plant, Arabidopsis thaliana. By transferring water 1H polarization to polysaccharides through distance- and mobility-dependent 1H–1H dipolar couplings and detecting it through polysaccharide 13C signals, we obtain information about water proximity to cellulose, hemicellulose, and pectins as well as water mobility. Both intact and partially extracted cell wall samples are studied. Our results show that water–pectin polarization transfer is much faster than water–cellulose polarization transfer in all samples, but the extent of extraction has a profound impact on the water–polysaccharide spin diffusion. Removal of calcium ions and the consequent extraction of homogalacturonan (HG) significantly slowed down spin diffusion, while further extraction of matrix polysaccharides restored the spin diffusion rate. These trends are observed in cell walls with similar water content, thus they reflect inherent differences in the mobility and spatial distribution of water. Combined with quantitative analysis of the polysaccharide contents, our results indicate that calcium ions and HG gelation increase the amount of bound water, which facilitates spin diffusion, while calcium removal disrupts the gel and gives rise to highly dynamic water, which slows down spin diffusion. The recovery of spin diffusion rates after more extensive extraction is attributed to increased water-exposed surface areas of the polysaccharides. Water–pectin spin diffusion precedes water–cellulose spin diffusion, lending support to the single-network model of plant primary walls in which a substantial fraction of the cellulose surface is surrounded by pectins.

  2. High average power diode pumped solid state lasers for CALIOPE

    SciTech Connect

    Comaskey, B.; Halpin, J.; Moran, B.

    1994-07-01

    Diode pumping of solid state media offers the opportunity for very low maintenance, high efficiency, and compact laser systems. For remote sensing, such lasers may be used to pump tunable non-linear sources, or if tunable themselves, act directly or through harmonic crystals as the probe. The needs of long range remote sensing missions require laser performance in the several watts to kilowatts range. At these power performance levels, more advanced thermal management technologies are required for the diode pumps. The solid state laser design must now address a variety of issues arising from the thermal loads, including fracture limits, induced lensing and aberrations, induced birefringence, and laser cavity optical component performance degradation with average power loading. In order to highlight the design trade-offs involved in addressing the above issues, a variety of existing average power laser systems are briefly described. Included are two systems based on Spectra Diode Laboratory`s water impingement cooled diode packages: a two times diffraction limited, 200 watt average power, 200 Hz multi-rod laser/amplifier by Fibertek, and TRW`s 100 watt, 100 Hz, phase conjugated amplifier. The authors also present two laser systems built at Lawrence Livermore National Laboratory (LLNL) based on their more aggressive diode bar cooling package, which uses microchannel cooler technology capable of 100% duty factor operation. They then present the design of LLNL`s first generation OPO pump laser for remote sensing. This system is specified to run at 100 Hz, 20 nsec pulses each with 300 mJ, less than two times diffraction limited, and with a stable single longitudinal mode. The performance of the first testbed version will be presented. The authors conclude with directions their group is pursuing to advance average power lasers. This includes average power electro-optics, low heat load lasing media, and heat capacity lasers.

  3. CARBON-13 NUCLEAR MAGNETIC RESONANCE. 13C CHEMICAL SHIFTS AND 13C-199HG COUPLING CONSTANTS FOR SOME ORGANOMERCURY COMPOUNDS

    EPA Science Inventory

    The (13)C shieldings and (13)C-(199)Hg coupling constants of fourteen phenyl- and seven alkyl- and alkenyl-mercury compounds have been obtained. Substituent effects on the (13)C shieldings are similar to those in nonmercurated phenyl compounds, with a similar relationship between...

  4. Solid-state NMR analysis of the {beta}-strand orientation of the protofibrils of amyloid {beta}-protein

    SciTech Connect

    Doi, Takashi; Masuda, Yuichi; Irie, Kazuhiro; Akagi, Ken-ichi; Monobe, Youko; Imazawa, Takayoshi; Takegoshi, K.

    2012-11-30

    Highlights: Black-Right-Pointing-Pointer The supramolecular structure of A{beta}42 protofibrils was analyzed by solid-state NMR. Black-Right-Pointing-Pointer The Ala-21 residue in the A{beta}42 protofibrils is included in a slightly disordered {beta}-strand. Black-Right-Pointing-Pointer The A{beta}42 protofibrils do not form intermolecular in-register parallel {beta}-sheets. -- Abstract: Alzheimer's disease (AD) is caused by abnormal deposition (fibrillation) of a 42-residue amyloid {beta}-protein (A{beta}42) in the brain. During the process of fibrillation, the A{beta}42 takes the form of protofibrils with strong neurotoxicity, and is thus believed to play a crucial role in the pathogenesis of AD. To elucidate the supramolecular structure of the A{beta}42 protofibrils, the intermolecular proximity of the Ala-21 residues in the A{beta}42 protofibrils was analyzed by {sup 13}C-{sup 13}C rotational resonance experiments in the solid state. Unlike the A{beta}42 fibrils, an intermolecular {sup 13}C-{sup 13}C correlation was not found in the A{beta}42 protofibrils. This result suggests that the {beta}-strands of the A{beta}42 protofibrils are not in an in-register parallel orientation. A{beta}42 monomers would assemble to form protofibrils with the {beta}-strand conformation, then transform into fibrils by forming intermolecular parallel {beta}-sheets.

  5. Standardized Testing Program for Solid-State Hydrogen Storage Technologies

    SciTech Connect

    Miller, Michael A.; Page, Richard A.

    2012-07-30

    In the US and abroad, major research and development initiatives toward establishing a hydrogen-based transportation infrastructure have been undertaken, encompassing key technological challenges in hydrogen production and delivery, fuel cells, and hydrogen storage. However, the principal obstacle to the implementation of a safe, low-pressure hydrogen fueling system for fuel-cell powered vehicles remains storage under conditions of near-ambient temperature and moderate pressure. The choices for viable hydrogen storage systems at the present time are limited to compressed gas storage tanks, cryogenic liquid hydrogen storage tanks, chemical hydrogen storage, and hydrogen absorbed or adsorbed in a solid-state material (a.k.a. solid-state storage). Solid-state hydrogen storage may offer overriding benefits in terms of storage capacity, kinetics and, most importantly, safety.The fervor among the research community to develop novel storage materials had, in many instances, the unfortunate consequence of making erroneous, if not wild, claims on the reported storage capacities achievable in such materials, to the extent that the potential viability of emerging materials was difficult to assess. This problem led to a widespread need to establish a capability to accurately and independently assess the storage behavior of a wide array of different classes of solid-state storage materials, employing qualified methods, thus allowing development efforts to focus on those materials that showed the most promise. However, standard guidelines, dedicated facilities, or certification programs specifically aimed at testing and assessing the performance, safety, and life cycle of these emergent materials had not been established. To address the stated need, the Testing Laboratory for Solid-State Hydrogen Storage Technologies was commissioned as a national-level focal point for evaluating new materials emerging from the designated Materials Centers of Excellence (MCoE) according to

  6. Spectroscopy of composite solid-state spin environments for improved metrology with spin ensembles

    NASA Astrophysics Data System (ADS)

    Bar-Gill, Nir; Pham, Linh; Belthangady, Chinmay; Lesage, David; Cappellaro, Paola; Maze, Jeronimo; Lukin, Mikhail; Yacoby, Amir; Walsworth, Ronald

    2012-02-01

    For precision coherent measurements with ensembles of quantum spins the relevant Figure-of-Merit (FOM) is the product of spin density and coherence lifetime, which is generally limited by the dynamics of spin coupling to the environment. Significant effort has been invested in understanding the causes of decoherence in a diverse range of spin systems in order to increase the FOM and improve measurement sensitivity. Here, we apply a coherent spectroscopic technique to characterize the dynamics of a composite solid-state spin environment consisting of Nitrogen-Vacancy (NV) color centers in room temperature diamond coupled to baths of electronic spin (N) and nuclear spin (13C) impurities. For diamond samples with a wide range of NV densities and impurity spin concentrations we employ a dynamical decoupling technique to minimize coupling to the environment, and find similar values for the FOM, which is three orders of magnitude larger than previously achieved in any room-temperature solid-state spin system, and thus should enable greatly improved precision spin metrology. We also identify a suppression of electronic spin bath dynamics in the presence of a nuclear spin bath of sufficient nuclear spin concentration. This suppression could inform efforts to engineer samples with even larger FOM for solid-state spin ensemble metrology and collective quantum information processing.

  7. The Rotational Spectrum of Singly and Doubly 13C-SUBSTITUTED Dimethylether

    NASA Astrophysics Data System (ADS)

    Koerber, Monika; Endres, Christian P.; Lewen, Frank; Giesen, Thomas F.; Schlemmer, Stephan; Pohl, Roland; Klein, Axel

    2010-06-01

    Dimethylether (DME) is a nearly prolate asymmetric top with two internal rotors (methyl groups) which undergo periodic large amplitude motions and show a complicated torsional splitting of each rotational energy level. Due to its complex spectrum and its high abundance in hot cores such as Orion KL or Sagittarius B2 at temperatures exceeding 100 K, DME is very prominent in astronomical line surveys and contributes to spectral line confusion of such sources. The interpretation of astronomical observations therefore depends on the knowledge of accurate rest frequencies and reliable intensities. Precise predictions for the ground state of DME's main isotopologue are now available up to 2.1 THz In contrast, very little is known about 13C-substituted DME. Only a few data are available on singly 13C-substituted DME, 12CH_3O13CH_3. However, no data are available on doubly 13C-substituted DME, (13CH_3)_2O, yet. While in (13CH_3)_2O the two internal rotating methyl groups are equivalent and the splitting of rotational energy levels into four substates is comparable to the main isotopologue, singly 13C-substituted DME has two non-equivalent internal rotors resulting in torsional splitting of rotational energy levels into five substates. The purpose of our new laboratory measurements is to extend the knowledge on the astrophysically relevant species 12CH_3O13CH_3. To analyze the complicated spectrum resulting from a 13C-enriched sample of DME, containing all different 13C-substituted species as well as the main isotopologue, also precise data on doubly 13C-substituted DME are inevitable. We performed measurements in the frequency region 35-120 GHz using an all solid state spectrometer. Rotational as well as torsional parameters have been obtained for (13CH_3)_2O as well as 12CH_3O13CH_3 by fitting the assigned transitions to an effective rotational Hamiltonian introduced by Peter Groner. C. Comito et al., Astrophys. J. Suppl. Ser. 156, 127-167 (2005) C. P. Endres et al

  8. New synthetic discoveries via high-pressure solid-state chemistry.

    PubMed

    Huppertz, Hubert

    2011-01-01

    Most of the syntheses in solid-state chemistry are performed at constant pressure of ∼1 atm (about 10(5) Pa) by the manipulation of the thermodynamic parameters temperature and composition, leading to a rich variety of compounds. In contrast, the additional variation of pressure has remained virtually unexplored, due to the relatively large costs of maintaining high-pressure conditions and the inevitably tiny sample volumes. In the last two decades, technical advances, developed for studying the properties of minerals, have found access into the preparative solid-state chemistry, opening up tremendously large areas to synthesize new materials. PMID:20859577

  9. Realization of Reliable Solid-State Quantum Memory for Photonic Polarization Qubit

    NASA Astrophysics Data System (ADS)

    Zhou, Zong-Quan; Lin, Wei-Bin; Yang, Ming; Li, Chuan-Feng; Guo, Guang-Can

    2012-05-01

    Faithfully storing an unknown quantum light state is essential to advanced quantum communication and distributed quantum computation applications. The required quantum memory must have high fidelity to improve the performance of a quantum network. Here we report the reversible transfer of photonic polarization states into collective atomic excitation in a compact solid-state device. The quantum memory is based on an atomic frequency comb (AFC) in rare-earth ion-doped crystals. We obtain up to 0.999 process fidelity for the storage and retrieval process of single-photon-level coherent pulse. This reliable quantum memory is a crucial step toward quantum networks based on solid-state devices.

  10. Instrumentation for solid-state dynamic nuclear polarization with magic angle spinning NMR

    NASA Astrophysics Data System (ADS)

    Rosay, Melanie; Blank, Monica; Engelke, Frank

    2016-03-01

    Advances in dynamic nuclear polarization (DNP) instrumentation and methodology have been key factors in the recent growth of solid-state DNP NMR applications. We review the current state of the art of solid-state DNP NMR instrumentation primarily based on available commercial platforms. We start with a general system overview, including options for microwave sources and DNP NMR probes, and then focus on specific developments for DNP at 100 K with magic angle spinning (MAS). Gyrotron microwave sources, passive components to transmit microwaves, the DNP MAS probe, a cooling device for low-temperature MAS, and sample preparation procedures including radicals for DNP are considered.

  11. The Use of Large Transparent Ceramics in a High Powered, Diode Pumped Solid State Laser

    SciTech Connect

    Yamamoto, R; Bhachu, B; Cutter, K; Fochs, S; Letts, S; Parks, C; Rotter, M; Soules, T

    2007-09-24

    The advent of large transparent ceramics is one of the key enabling technological advances that have shown that the development of very high average power compact solid state lasers is achievable. Large ceramic neodymium doped yttrium aluminum garnet (Nd:YAG) amplifier slabs are used in Lawrence Livermore National Laboratory's (LLNL) Solid State Heat Capacity Laser (SSHCL), which has achieved world record average output powers in excess of 67 kilowatts. We will describe the attributes of using large transparent ceramics, our present system architecture and corresponding performance; as well as describe our near term future plans.

  12. Instrumentation for solid-state dynamic nuclear polarization with magic angle spinning NMR.

    PubMed

    Rosay, Melanie; Blank, Monica; Engelke, Frank

    2016-03-01

    Advances in dynamic nuclear polarization (DNP) instrumentation and methodology have been key factors in the recent growth of solid-state DNP NMR applications. We review the current state of the art of solid-state DNP NMR instrumentation primarily based on available commercial platforms. We start with a general system overview, including options for microwave sources and DNP NMR probes, and then focus on specific developments for DNP at 100K with magic angle spinning (MAS). Gyrotron microwave sources, passive components to transmit microwaves, the DNP MAS probe, a cooling device for low-temperature MAS, and sample preparation procedures including radicals for DNP are considered. PMID:26920834

  13. Solid-state Raman image amplification

    NASA Astrophysics Data System (ADS)

    Calmes, Lonnie Kirkland

    Amplification of low-light-level optical images is important for extending the range of lidar systems that image and detect objects in the atmosphere and underwater. The use of range-gating to produce images of particular range bins is also important in minimizing the image degradation due to light that is scattered backward from aerosols, smoke, or water along the imaging path. For practical lidar systems that must be operated within sight of unprotected observers, eye safety is of the utmost importance. This dissertation describes a new type of eye-safe, range-gated lidar sensing element based on Solid-state Raman Image Amplification (SSRIA) in a solid- state optical crystal. SSRIA can amplify low-level images in the eye-safe infrared at 1.556 μm with gains up to 106 with the addition of only quantum- limited noise. The high gains from SSRIA can compensate for low quantum efficiency detectors and can reduce the need for detector cooling. The range-gate of SSRIA is controlled by the pulsewidth of the pump laser and can be as short as 30-100 cm, using pump pulses of 2-6.7 nsec FWHM. A rate equation theoretical model is derived to help in the design of short pulsed Raman lasers. A theoretical model for the quantum noise properties of SSRIA is presented. SSRIA results in higher SNR images throughout a broad range of incident light levels, in contrast to the increasing noise factor with reduced gain in image intensified CCD's. A theoretical framework for the optical resolution of SSRIA is presented and it is shown that SSRIA can produce higher resolution than ICCD's. SSRIA is also superior in rejecting unwanted sunlight background, further increasing image SNR. Lastly, SSRIA can be combined with optical pre-filtering to perform optical image processing functions such as high-pass filtering and automatic target detection/recognition. The application of this technology to underwater imaging, called Marine Raman Image Amplification (MARIA) is also discussed. MARIA

  14. Improving Reliability of High Power Quasi-CW Laser Diode Arrays for Pumping Solid State Lasers

    NASA Technical Reports Server (NTRS)

    Amzajerdian, Farzin; Meadows, Byron L.; Baker, Nathaniel R.; Barnes, Bruce W.; Baggott, Renee S.; Lockard, George E.; Singh, Upendra N.; Kavaya, Michael J.

    2005-01-01

    Most Lidar applications rely on moderate to high power solid state lasers to generate the required transmitted pulses. However, the reliability of solid state lasers, which can operate autonomously over long periods, is constrained by their laser diode pump arrays. Thermal cycling of the active regions is considered the primary reason for rapid degradation of the quasi-CW high power laser diode arrays, and the excessive temperature rise is the leading suspect in premature failure. The thermal issues of laser diode arrays are even more drastic for 2-micron solid state lasers which require considerably longer pump pulses compared to the more commonly used pump arrays for 1-micron lasers. This paper describes several advanced packaging techniques being employed for more efficient heat removal from the active regions of the laser diode bars. Experimental results for several high power laser diode array devices will be reported and their performance when operated at long pulsewidths of about 1msec will be described.

  15. DEVELOPMENT OF SOLID-STATE DRIVERS FOR THE NIF PLASMA ELECTRODE POCKELS CELL

    SciTech Connect

    Barbosa, F; Arnold, P A; McHale, G B; James, G; Brown, G; Cook, E G; Hickman, B C

    2008-05-14

    Large aperture Plasma Electrode Pockels Cells (PEPC) are an enabling technology in the National Ignition Facility (NIF) at the Lawrence Livermore National Laboratory. The Pockels cell allows the NIF laser to take advantage of multipass amplifier architecture, thus reducing costs and physical size of the facility. Each Pockels cell comprises four 40-cm x 40-cm apertures arranged in a 4 x 1 array. The combination of the Pockels cell and a thin-film polarizer, configured in a 4 x 1 array, form an optical switch that is key to achieving multi-pass operation. Solid-state Plasma Pulse Generators (PPGs) and high current high voltage solid-state Switch Pulse Generators (SPGs) have been developed for use in the PEPC. The solid-state plasma pulse generators initiate and maintain plasma within the cells; each pulser is capable of delivering 60J of energy to each plasma channel. Deployment of the solid-state PPGs has been completed in NIF. The MOSFET-switched SPG is capable of delivering a requisite fast rise time, 17kV flattop pulse to the cells nonlinear crystals. A complete software and hardware control system has been developed and is currently being tested for use on the solid-state SPGs. Also a transmission line modeling, development, and testing effort is in process, in support of NIFs Advanced Radiographic Capabilities (ARC). Work is scheduled for completion by the end of the calendar year.

  16. Quantitative Determination of Site-Specific Conformational Distributions in an Unfolded Protein by Solid State Nuclear Magnetic Resonance

    PubMed Central

    Hu, Kan-Nian; Havlin, Robert H.; Yau, Wai-Ming; Tycko, Robert

    2009-01-01

    Summary Solid state nuclear magnetic resonance (NMR) techniques are used to investigate the structure of the 35-residue villin headpiece subdomain (HP35) in folded, partially denatured, and fully denatured states. Experiments are carried out in frozen glycerol/water solutions, with chemical denaturation by guanidine hydrochloride (GdnHCl). Without GdnHCl, two-dimensional solid state 13C NMR spectra of samples prepared with uniform 13C labeling of selected residues show relatively sharp crosspeaks at chemical shifts that are consistent with the known three-helix bundle structure of folded HP35. At high GdnHCl concentrations, most crosspeaks broaden and shift, qualitatively indicating disruption of the folded structure and development of static conformational disorder in the frozen denatured state. Conformational distributions at one residue in each helical segment are probed quantitatively with three solid state NMR techniques that provide independent constraints on backbone ϕ and ψ torsion angles in samples with sequential pairs of carbonyl 13C labels. Without GdnHCl, the combined data are well fit by α-helical conformations. At [GdnHCl] = 4.5 M, corresponding to the approximate denaturation midpoint, the combined data are well fit by a combination of α-helical and partially extended conformations at each site, but with a site-dependent population ratio. At [GdnHCl] = 7.0 M, corresponding to the fully denatured state, the combined data are well fit by a combination of partially extended and polyproline II conformations, again with a site-dependent population ratio. Two entirely different models for conformational distributions lead to nearly the same best-fit distributions, demonstrating the robustness of these conclusions. This work represents the first quantitative investigation of site-specific conformational distributions in partially folded and unfolded states of a protein by solid state NMR. PMID:19647001

  17. Modified Reference SPS with Solid State Transmitting Antenna

    NASA Technical Reports Server (NTRS)

    Woodcock, G. R.; Sperber, B. R.

    1980-01-01

    The development of solid state microwave power amplifiers for a solar power satellite transmitting antenna is discussed. State-of-the-art power-added efficiency, gain, and single device power of various microwave solid state devices are compared. The GaAs field effect transistors and the Si-bipolar transistors appear potentially feasible for solar power satellite use. The integration of solid state devices into antenna array elements is examined and issues concerning antenna integration and consequent satellite configurations are examined.

  18. Synthesis Of [2h, 13c]M [2h2m 13c], And [2h3,, 13c] Methyl Aryl Sulfones And Sulfoxides

    DOEpatents

    Martinez, Rodolfo A.; Alvarez, Marc A.; Silks, III, Louis A.; Unkefer, Clifford J.; Schmidt, Jurgen G.

    2004-07-20

    The present invention is directed to labeled compounds, [.sup.2 H.sub.1, .sup.13 C], [.sup.2 H.sub.2, .sup.13 C] and [.sup.2 H.sub.3, .sup.13 C]methyl aryl sulfones and [.sup.2 H.sub.1, .sup.13 C], [.sup.2 H.sub.2, .sup.13 C] and [.sup.2 H.sub.3, .sup.13 C]methyl aryl sulfoxides, wherein the .sup.13 C methyl group attached to the sulfur of the sulfone or sulfoxide includes exactly one, two or three deuterium atoms and the aryl group is selected from the group consisting of 1-naphthyl, substituted 1-naphthyl, 2-naphthyl, substituted 2-naphthyl, and phenyl groups with the structure: ##STR1## wherein R.sub.1, R.sub.2, R.sub.3, R.sub.4 and R.sub.5 are each independently, hydrogen, a C.sub.1 -C.sub.4 lower alkyl, a halogen, an amino group from the group consisting of NH.sub.2, NHR and NRR' where R and R' are each a C.sub.1 -C.sub.4 lower alkyl, a phenyl, or an alkoxy group. The present invention is also directed to processes of preparing methyl aryl sulfones and methyl aryl sulfoxides.

  19. Polarization transfer solid-state NMR for studying surfactant phase behavior.

    PubMed

    Nowacka, Agnieszka; Mohr, Parveen Choudhary; Norrman, Jens; Martin, Rachel W; Topgaard, Daniel

    2010-11-16

    The phase behavior of amphiphiles, e.g., lipids and surfactants, at low water content is of great interest for many technical and pharmaceutical applications. When put in contact with air having a moderate relative humidity, amphiphiles often exhibit coexistence between solid and liquid crystalline phases, making their complete characterization difficult. This study describes a (13)C solid-state NMR technique for the investigation of amphiphile phase behavior in the water-poor regime. While the (13)C chemical shift is an indicator of molecular conformation, the (13)C signal intensities obtained with the CP and INEPT polarization transfer schemes yield information on molecular dynamics. A theoretical analysis incorporating the effect of molecular segment reorientation, with the correlation time τ(c) and order parameter S, shows that INEPT is most efficient for mobile segments with τ(c) < 0.01 μs and S < 0.05, while CP yields maximal signal for rigid segments with τ(c) > 10 μs and/or S > 0.5 under typical solid-state NMR experimental conditions. For liquid crystalline phases, where τ(c) < 0.01 μs and 0 < S < 0.3, the observed CP and INEPT intensities serve as a gauge of S. The combination of information on molecular conformation and dynamics permits facile phase diagram determination for systems with solid crystalline, solid amorphous, anisotropic liquid crystalline, and isotropic liquid (crystalline) phases as demonstrated by experiments on a series of reference systems with known phase structure. Three solid phases (anhydrous crystal, dihydrate, gel), two anisotropic liquid crystalline phases (normal hexagonal, lamellar), and two isotropic liquid crystalline phases (micellar cubic, bicontinuous cubic) are identified in the temperature-composition phase diagram of the cetyltrimethylammonium succinate/water system. Replacing the succinate counterion with DNA prevents the formation of phases other than hexagonal and leads to a general increase of τ(c). PMID

  20. Characterization of the Vibrio cholerae Extracellular Matrix: A Top-Down Solid-State NMR Approach

    PubMed Central

    Reichhardt, Courtney; Fong, Jiunn C.N.; Yildiz, Fitnat; Cegelski, Lynette

    2015-01-01

    Bacterial biofilms are communities of bacterial cells surrounded by a self-secreted extracellular matrix. Biofilm formation by Vibrio cholerae, the human pathogen responsible for cholera, contributes to its environmental survival and infectivity. Important genetic and molecular requirements have been identified for V. cholerae biofilm formation, yet a compositional accounting of these parts in the intact biofilm or extracellular matrix has not been described. As insoluble and non-crystalline assemblies, determinations of biofilm composition pose a challenge to conventional biochemical and biophysical analysis. The V. cholerae extracellular matrix composition is particularly complex with several proteins, complex polysaccharides, and other biomolecules having been identified as matrix parts. We developed a new top-down solid-state NMR approach to spectroscopically assign and quantify the carbon pools of the intact V. cholerae extracellular matrix using 13C CPMAS and 13C{15N}, 15N{31P}, and 13C{31P}REDOR. General sugar, lipid, and amino acid pools were first profiled and then further annotated and quantified as specific carbon types, including carbonyls, amides, glycyl carbons, and anomerics. In addition, 15N profiling revealed a large amine pool relative to amide contributions, reflecting the prevalence of molecular modifications with free amine groups. Our top-down approach could be implemented immediately to examine the extracellular matrix from mutant strains that might alter polysaccharide production or lipid release beyond the cell surface; or to monitor changes that may accompany environmental variations and stressors such as altered nutrient composition, oxidative stress or antibiotics. More generally, our analysis has demonstrated that solid-state NMR is a valuable tool to characterize complex biofilm systems. PMID:24911407

  1. Radiation-Hardened Solid-State Drive

    NASA Technical Reports Server (NTRS)

    Sheldon, Douglas J.

    2010-01-01

    A method is provided for a radiationhardened (rad-hard) solid-state drive for space mission memory applications by combining rad-hard and commercial off-the-shelf (COTS) non-volatile memories (NVMs) into a hybrid architecture. The architecture is controlled by a rad-hard ASIC (application specific integrated circuit) or a FPGA (field programmable gate array). Specific error handling and data management protocols are developed for use in a rad-hard environment. The rad-hard memories are smaller in overall memory density, but are used to control and manage radiation-induced errors in the main, and much larger density, non-rad-hard COTS memory devices. Small amounts of rad-hard memory are used as error buffers and temporary caches for radiation-induced errors in the large COTS memories. The rad-hard ASIC/FPGA implements a variety of error-handling protocols to manage these radiation-induced errors. The large COTS memory is triplicated for protection, and CRC-based counters are calculated for sub-areas in each COTS NVM array. These counters are stored in the rad-hard non-volatile memory. Through monitoring, rewriting, regeneration, triplication, and long-term storage, radiation-induced errors in the large NV memory are managed. The rad-hard ASIC/FPGA also interfaces with the external computer buses.

  2. Introduction to cryogenic solid state cooling

    NASA Astrophysics Data System (ADS)

    Heremans, Joseph P.

    2016-05-01

    Thermoelectric (Peltier) coolers have historically not been used for cooling to temperatures much below 200 K, because of limitations with existing thermoelectric materials. There are many advantages to solid-state coolers: they have no moving parts, are compact, vibration-free, inherently durable, and scalable to low power levels. A significant drawback is their low coefficient of performance. The figure of merit, zT, is the materials characteristic that sets this efficiency in Peltier coolers. The zT decreases rapidly with temperature, roughly following a T7/2 law. However, new material developments have taken place in the last decade that have made it possible to reach zT>0.5 down to 50 K. Many new ideas have also been put forward that enable better ZT's and lower temperatures. This article reviews the difficulties associated with Peltier cooling at cryogenic temperatures, as an introduction to the following presentations and proceeding entries that will present solutions that have been developed since 2010.

  3. Solid state replacement of rotating mirror cameras

    NASA Astrophysics Data System (ADS)

    Frank, Alan M.; Bartolick, Joseph M.

    2007-01-01

    Rotating mirror cameras have been the mainstay of mega-frame per second imaging for decades. There is still no electronic camera that can match a film based rotary mirror camera for the combination of frame count, speed, resolution and dynamic range. The rotary mirror cameras are predominantly used in the range of 0.1 to 100 micro-seconds per frame, for 25 to more than a hundred frames. Electron tube gated cameras dominate the sub microsecond regime but are frame count limited. Video cameras are pushing into the microsecond regime but are resolution limited by the high data rates. An all solid state architecture, dubbed 'In-situ Storage Image Sensor' or 'ISIS', by Prof. Goji Etoh has made its first appearance into the market and its evaluation is discussed. Recent work at Lawrence Livermore National Laboratory has concentrated both on evaluation of the presently available technologies and exploring the capabilities of the ISIS architecture. It is clear though there is presently no single chip camera that can simultaneously match the rotary mirror cameras, the ISIS architecture has the potential to approach their performance.

  4. Flexible solid-state photoelectrochromic windows

    SciTech Connect

    Pichot, F.; Ferrere, S.; Pitts, R.J.; Gregg, B.A.

    1999-11-01

    Photoelectrochromic smart window technology is extended to include the use of flexible substrates and solid-state electrolytes. This should facilitate their application as retrofit modifications of office windows, where, by blocking incoming solar irradiation, they could substantially lower air-conditioning costs. These devices are based on a dye-sensitized TiO{sub 2} electrode coupled with a 500 nm thick WO{sub 3} electrochromic counter electrode, separated by a cross-linked polymer electrolyte containing LiI. A novel method for preparing conducting nanoporous TiO{sub 2} films is described that allows for the construction of these devices on flexible organic substrates. Colloidal solutions of TiO{sub 2} free of surfactants were spin-coated onto indium-tin oxide coated polyester substrates, resulting in highly transparent films ranging from 100 nm to 1 {micro}m in thickness. Upon annealing at 100 C, these films were strongly adherent and displayed excellent photoconductivity as shown by their current-voltage characteristics. The devices typically transmit 75% of visible light in the bleached state. After a few minutes of exposure to white light (75 mW/cm{sup 2}), the windows turn dark blue, transmitting only 30% of visible light. They spontaneously bleach back to their initial noncolored state upon removal of the light source.

  5. Solid state photomultiplier for astronomy, phase 2

    NASA Technical Reports Server (NTRS)

    Besser, P. J.; Hays, K. M.; Laviolette, R. A.

    1989-01-01

    Epitaxial layers with varying donor concentration profiles were grown on silicon substrate wafers using chemical vapor deposition (CVD) techniques, and solid state photomultiplier (SSPM) devices were fabricated from the wafers. Representative detectors were tested in a low background photon flux, low temperature environment to determine the device characteristics for comparison to NASA goals for astronomical applications. The SSPM temperatures varied between 6 and 11 K with background fluxes in the range from less than 5 x 10 to the 6th power to 10 to the 13th power photons/square cm per second at wavelengths of 3.2 and 20 cm. Measured parameters included quantum efficiency, dark count rate and bias current. Temperature for optimal performance is 10 K, the highest ever obtained for SSPMs. The devices exhibit a combination of the lowest dark current and highest quantum efficiency yet achieved. Experimental data were reduced, analyzed and used to generate recommendations for future studies. The background and present status of the microscopic theory of SSPM operation were reviewed and summarized. Present emphasis is on modeling of the avalanche process which is the basis for SSPM operation. Approaches to the solution of the Boltzmann transport equation are described and the treatment of electron scattering mechanisms is presented. The microscopic single-electron transport theory is ready to be implemented for large-scale computations.

  6. A novel solid state general illumination source

    NASA Astrophysics Data System (ADS)

    Nicol, David B.

    A novel solid state illumination source has been developed. A two terminal dual LED has been created with the ability to control the relative intensities of the two emission peaks by varying drive current. Doping profiles have been used to extend the dynamic range of the dual LED over other reported devices. Operation of the dual LEDs is explained as a function of drive current. In addition, novel use of phosphor mixtures allows the creation of a broadband spectral power distribution that can be varied using a dual LED as an excitation source. Combinations of phosphors that have varied excitation spectra provide the ability to selectively excite different phosphors with the different LED emission peaks. First and second generations of the two terminal dual LED and the phosphor combination are discussed. The final source has the ability to mimic the light of a blackbody radiator over a range of 3200 K - 5300 K. The development of a three terminal dual LED as a pump source was prohibited by the need for a III-nitride tunnel junction, that proved unattainable in the scope of this work. However, several novel doping schemes were investigated toward this end. Finally, a circadian light source has also been developed that can affect physiological changes in humans, and a light box for entrainment of circadian rhythms in rats has been built.

  7. Solid State Replacement of Rotating Mirror Cameras

    SciTech Connect

    Frank, A M; Bartolick, J M

    2006-08-25

    Rotating mirror cameras have been the mainstay of mega-frame per second imaging for decades. There is still no electronic camera that can match a film based rotary mirror camera for the combination of frame count, speed, resolution and dynamic range. The rotary mirror cameras are predominantly used in the range of 0.1 to 100 micro-seconds per frame, for 25 to more than a hundred frames. Electron tube gated cameras dominate the sub microsecond regime but are frame count limited. Video cameras are pushing into the microsecond regime but are resolution limited by the high data rates. An all solid state architecture, dubbed ''In-situ Storage Image Sensor'' or ''ISIS'', by Prof. Goji Etoh, has made its first appearance into the market and its evaluation is discussed. Recent work at Lawrence Livermore National Laboratory has concentrated both on evaluation of the presently available technologies and exploring the capabilities of the ISIS architecture. It is clear though there is presently no single chip camera that can simultaneously match the rotary mirror cameras, the ISIS architecture has the potential to approach their performance.

  8. Testing the limits of sensitivity in a solid-state structural investigation by combined X-ray powder diffraction, solid-state NMR, and molecular modelling.

    PubMed

    Filip, Xenia; Borodi, Gheorghe; Filip, Claudiu

    2011-10-28

    A solid state structural investigation of ethoxzolamide is performed on microcrystalline powder by using a multi-technique approach that combines X-ray powder diffraction (XRPD) data analysis based on direct space methods with information from (13)C((15)N) solid-state Nuclear Magnetic Resonance (SS-NMR) and molecular modeling. Quantum chemical computations of the crystal were employed for geometry optimization and chemical shift calculations based on the Gauge Including Projector Augmented-Wave (GIPAW) method, whereas a systematic search in the conformational space was performed on the isolated molecule using a molecular mechanics (MM) approach. The applied methodology proved useful for: (i) removing ambiguities in the XRPD crystal structure determination process and further refining the derived structure solutions, and (ii) getting important insights into the relationship between the complex network of non-covalent interactions and the induced supra-molecular architectures/crystal packing patterns. It was found that ethoxzolamide provides an ideal case study for testing the accuracy with which this methodology allows to distinguish between various structural features emerging from the analysis of the powder diffraction data. PMID:21931906

  9. X-Band, 17-Watt Solid-State Power Amplifier

    NASA Technical Reports Server (NTRS)

    Mittskus, Anthony; Stone, Ernest; Boger, William; Burgess, David; Honda, Richard; Nuckolls, Carl

    2005-01-01

    An advanced solid-state power amplifier that can generate an output power of as much as 17 W at a design operating frequency of 8.4 GHz has been designed and constructed as a smaller, lighter, less expensive alternative to traveling-wave-tube X-band amplifiers and to prior solid-state X-band power amplifiers of equivalent output power. This amplifier comprises a monolithic microwave integrated circuit (MMIC) amplifier module and a power-converter module integrated into a compact package (see Figure 1). The amplifier module contains an input variable-gain amplifier (VGA), an intermediate driver stage, a final power stage, and input and output power monitors (see Figure 2). The VGA and the driver amplifier are 0.5-m GaAs-based metal semiconductor field-effect transistors (MESFETs). The final power stage contains four parallel high-efficiency, GaAs-based pseudomorphic high-electron-mobility transistors (PHEMTs). The gain of the VGA is voltage-variable over a range of 10 to 24 dB. To provide for temperature compensation of the overall amplifier gain, the gain-control voltage is generated by an operational-amplifier circuit that includes a resistor/thermistor temperature-sensing network. The driver amplifier provides a gain of 14 dB to an output power of 27 dBm to drive the four parallel output PHEMTs, each of which is nominally capable of putting out as much as 5 W. The driver output is sent to the input terminals of the four parallel PHEMTs through microstrip power dividers; the outputs of these PHEMTs are combined by microstrip power combiners (which are similar to the microstrip power dividers) to obtain the final output power of 17 W.

  10. /sup 13/C nuclear magnetic resonance studies of cardiac metabolism

    SciTech Connect

    Seeholzer, S.H.

    1985-01-01

    The last decade has witnessed the increasing use of Nuclear Magnetic Resonance (NMR) techniques for following the metabolic fate of compounds specifically labeled with /sup 13/C. The goals of the present study are: (1) to develop reliable quantitative procedures for measuring the /sup 13/C enrichment of specific carbon sites in compounds enriched by the metabolism of /sup 13/C-labeled substrates in rat heart, and (2) to use these quantitative measurements of fractional /sup 13/C enrichment within the context of a mathematical flux model describing the carbon flow through the TCA cycle and ancillary pathways, as a means for obtaining unknown flux parameters. Rat hearts have been perfused in vitro with various combinations of glucose, acetate, pyruvate, and propionate to achieve steady state flux conditions, followed by perfusion with the same substrates labeled with /sup 13/C in specific carbon sites. The hearts were frozen at different times after addition of /sup 13/C-labeled substrates and neutralized perchloric acid extracts were used to obtain high resolution proton-decoupled /sup 13/C NMR spectra at 90.55 MHz. The fractional /sup 13/C enrichment (F.E.) of individual carbon sites in different metabolites was calculated from the area of the resolved resonances after correction for saturation and nuclear Overhauser effects. These F.E. measurements by /sup 13/C NMR were validated by the analysis of /sup 13/C-/sup 1/H scalar coupling patterns observed in /sup 1/H NMR spectra of the extracted metabolites. The results obtained from perfusion of hearts glucose plus either (2-/sup 13/C) acetate or (3-/sup 13/C) pyruvate are similar to those obtained by previous investigators using /sup 14/C-labeled substrates.

  11. Photo-CIDNP 13C magic angle spinning NMR on bacterial reaction centres: exploring the electronic structure of the special pair and its surroundings.

    PubMed

    Matysik, J; Schulten, E; Alia; Gast, P; Raap, J; Lugtenburg, J; Hoff, A J; de Groot, H J

    2001-08-01

    Photochemically induced dynamic nuclear polarisation (photo-CIDNP) in intact bacterial reaction centres has been observed by 13C-solid state NMR under continuous illumination with white light. Strong intensity enhancement of 13C NMR signals of the aromatic rings allows probing the electronic ground state of the two BChl cofactors of the special pair at the molecular scale with atomic selectivity. Differences between the two BChl cofactors are discussed. Several aliphatic 13C atoms of cofactors, as well as 13C atoms of the imidazole ring of histidine residue(s), show nuclear-spin polarisation to the same extent as the aromatic nuclei of the cofactors. Mechanisms and applications of polarisation transfer are discussed. PMID:11592409

  12. /sup 15/N and /sup 13/C NMR determination of methionine metabolism in developing soybean cotyledons

    SciTech Connect

    Coker, G.T. III; Garbow, J.R.; Schaefer, J.

    1987-03-01

    The metabolism of D- and L-methionine by immature cotyledons of soybean (Glycine max, L. cv Elf) grown in culture has been investigated using solid-state /sup 13/C and /sup 15/N nuclear magnetic resonance. D-Methionine is taken up by the cotyledons and converted to an amide, most likely by N-malonylation. About 16% of the L-methionine taken up is incorporated intact into protein, and 25% remains as soluble methionine. Almost two-thirds of the L-methionine that enters the cotyledons is degraded. The largest percentage of this is used in transmethylation of the carboxyl groups of pectin. Methionine is not extensively converted to polyamines. The authors attribute the stimulation of growth of the cotyledons by exogenous methionine to the bypassing of a rate-limiting methyl-transfer step in the synthesis of methionine itself, and subsequently of pectins and proteins.

  13. The effect of sample hydration on 13C CPMAS NMR spectra of fulvic acids

    USGS Publications Warehouse

    Hatcher, P.G.; Wilson, M.A.

    1991-01-01

    Three fulvic acids, two of which have been well studied by a number of other groups (Armadale and Suwannee river fulvic acids) have been examined by high resolution solid-state 13C-NMR techniques to delineate the effect of absorbed water. Two main effects of absorbed water were observed: (1) changes in spin lattice relaxation times in the rotating frame and cross polarization times and (2) total loss of signal so that some fulvic acid is effectively in solution. These results suggest that discrepancies in the literature concerning observed relative signal intensities from different structural groups are due to absorbed water and emphasize the necessity for proper precautionary drying before spectroscopic analysis. ?? 1991.

  14. Interactions between Nafion resin and protonated dodecylamine modified montmorillonite: a solid state NMR study.

    PubMed

    Zhang, Limin; Xu, Jun; Hou, Guangjin; Tang, Huiru; Deng, Feng

    2007-07-01

    A series of nanocomposites have been prepared from perfluorosulfonylfluoride copolymer resin (Nafion) and layered montmorillonite (MMT) modified with protonated dodecylamine by conventional sol-gel intercalation. The structure of these nanocomposite materials have been characterized using FT-IR, elemental analysis, XRD and solid state NMR techniques, including 19F magic-angle spinning (MAS) NMR, 19F NMR relaxation time measurements, 29Si MAS, 1H MAS, 1H-13C cross-polarization magic-angle spinning (CPMAS), and 1H-13C heteronuclear correlation (HETCOR) 2D NMR. The results showed that thermal stability of Nafion was improved moderately by the addition of dodecylamine modified MMT without intercalation. FT-IR and 29Si MAS NMR results indicated that dodecylamine modification did not result in obvious changes in the MMT lattice structure. The XRD results showed that the protonated dodecylamine has been embedded and intercalated into the MMT interlayers, whereas Nafion was not. Elemental analysis results also suggested that some dodecylamine was adsorbed on the surface of MMT. 1H-13C HETCOR 2D NMR experiment clearly indicated that strong electrostatic interactions were present between the NH+3 group of dodecylamine and the fluorine-containing groups (CF3, OCF2, and SCF2) of Nafion resin. Such electrostatic interactions are probably the major contributors for the improved thermal stability of the resultant composite materials. PMID:17382953

  15. Investigation of a naphthalene pitch by high-resolution solid-state dynamic nuclear polarization.

    PubMed

    Zhou, J; Yang, B; Hu, J; Hu, H; Li, L; Qiu, J; Zeng, F; Ye, C

    1996-04-01

    The possibility of applying the dynamic nuclear polarization (DNP) technique to a study of char is explored with a naphthalene-derived pitch. It is shown that a 13C DNP enhancement factor of about 10(2) is obtained when the polarization is directly transferred from the unpaired electrons to the 13C nuclei. An undistorted spectrum with an enhancement factor of 8 is obtained by the DNP cross-polarization magic-angle spinning nuclear magnetic resonance (DNP-CP-MAS NMR) method. With such a high increase in S/N, it is possible to measure the 13C polarization time (Tp) and the spin-lattice relaxation time (T1) of the system in a reasonable experimental time. The resultant values are Tp = 19 s and T1 = 38 s, respectively. Based on the DNP enhancement as a function of the microwave frequency, it is found that the predominant DNP mechanism in the pitch is the solid-state effect. PMID:8784951

  16. Structure determination of individual electron-nuclear spin complexes in a solid-state matrix

    NASA Astrophysics Data System (ADS)

    Laraoui, Abdelghani; Pagliero, Daniela; Meriles, Carlos

    2015-03-01

    A spin-based quantum computer will store and process information via ``spin complexes'' formed by a small number of interacting electronic and nuclear spins within a solid-state host. Unlike present electronic circuits, differences in the atomic composition and local geometry make each of these spin clusters distinct from the rest. Integration of these units into a working network thus builds on our ability to determine the cluster atomic structure, a problem we tackle herein with the aid of a magnetic resonance protocol. Using the nitrogen-vacancy (NV) center in diamond as a model system, we show analytically and numerically that the spatial coordinates of weakly coupled 13C spins can be determined by selectively transferring and retrieving spin polarization. The technique's spatial resolution can reach up to 0.1 nm, limited by the NV spin coherence lifetime. No external magnetic field gradient is required, which makes this imaging scheme applicable to NV-13C complexes buried deep inside the crystal host. Further, this approach can be adapted to nuclear spins other than 13C, and thus applied to the characterization of individual molecules anchored to the diamond surface.

  17. Electron correlations in solid state physics

    SciTech Connect

    Freericks, J.K.

    1991-04-01

    Exactly solvable models of electron correlations in solid state physics are presented. These models include the spinless Falicov- Kimball model, the t-t{prime}-J model, and the Hubbard model. The spinless Falicov-Kimball model is analyzed in one-dimension. Perturbation theory and numerical techniques are employed to determine the phase diagram at zero temperature. A fractal structure is found where the ground-state changes (discontinuously) at each rational electron filling. The t-t{prime}-J model (strongly interacting limit of a Hubbard model) is studied on eight-site small clusters in the simple-cubic, body-centered-cubic, face-centered-cubic, and square lattices. Symmetry is used to simplify the problem and determine the exact many-body wavefunctions. Ground states are found that exhibit magnetic order or heavy-fermionic character. Attempts to extrapolate to the thermodynamic limit are also made. The Hubbard model is examined on an eight-site square-lattice cluster in the presence of and in the absence of a magnetic field'' that couples only to orbital motion. A new magnetic phase is discovered for the ordinary Hubbard model at half-filling. In the magnetic field'' case, it is found that the strongly frustrated Heisenberg model may be studied from adiabatic continuation of a tight-binding model (from weak to strong coupling) at one point. The full symmetries of the Hamiltonian are utilized to make the exact diagonalization feasibile. Finally, the presence of hidden'' extra symmetry for finite size clusters with periodic boundary conditions is analyzed for a variety of clusters. Moderately sized systems allow nonrigid transformations that map a lattice onto itself preserving its neighbor structure; similar operations are not present in smaller or larger systems. The additional symmetry requires particular representations of the space group to stick together explaining many puzzling degeneracies found in exact diagonalization studies.

  18. Nanoprobes, nanostructured materials and solid state materials

    NASA Astrophysics Data System (ADS)

    Yin, Houping

    2005-07-01

    Novel templates have been developed to prepare nanostructured porous materials through nonsurfactant templated pathway. And new applications of these materials, such as drug delivery and molecular imprinting, have been explored. The relationship between template content and pore structure has been investigated. The composition and pore structures were studied in detail using IR, TGA, SEM, TEM, BET and XRD. The obtained mesoporous materials have tunable diameters in the range of 2--12 nm. Due to the many advantages of this nonsurfactant templated pathway, such as environment friendly and biocompatibility, controlled release of antibiotics in the nanoporous materials were studied. The in vitro release properties were found to depend on the silica structures which were well tuned by varying the template content. A controlled long-term release pattern of vancomycin was achieved when the template content was 30 wt% or lower. Nanoscale electrochemical probes with dimensions as small as 50 nm in diameter and 1--2 mum in length were fabricated using electron beam deposition on the apex of conventional micron size electrodes. The electroactive region was limited to the extreme tip of the nanoprobe by coating with an insulating polymer and re-opening of the coating at the extreme tip. The novel nanoelectrodes thus prepared were employed to probe neurons in mouse brain slice and the results suggest that the nanoprobes were capable of recording neuronal excitatory postsynaptic potential signals. Interesting solid state chemistry was found in oxygenated iron phthalocyanine. Their Mossbauer spectra show the formation of four oxygenated species apart from the unoxygenated parent compound. The oxygen-bridged compounds formed in the solid matrix bear no resemblance to the one formed by solution chemistry. Tentative assignment of species has been made with the help of Mossbauer and IR spectroscopy. An effort to modify aniline trimer for potential nanoelectronics applications and to

  19. SOLID-STATE CERAMIC LIGHTING PROJECT

    SciTech Connect

    Wayne D. Brown

    2003-06-01

    Meadow River Enterprises, Inc. (MRE) and the New York State College of Ceramics at Alfred University (NYSCC) received a DOE cooperative agreement award in September 1999 to develop an energy-efficient Solid-State Ceramic Lamp (SSCL). The program spanned a nominal two(2) year period ending in February of 2002. The federal contribution to the program totaled $1.6 million supporting approximately 78% of the program costs. The SSCL is a rugged electroluminescent lamp designed for outdoor applications. MRE has filed a provisional patent for this ''second generation'' technology and currently produces and markets blue-green phosphor SSCL devices. White phosphor SSCL devices are also available in prototype quantities. In addition to reducing energy consumption, the ceramic EL lamp offers several economic and societal advantages including lower lifecycle costs and reduced ''light pollution''. Significant further performance improvements are possible but will require a dramatic change in device physical construction related to the use of micro-powder materials and processes. The subject ''second-generation'' program spans a 27 month period and combines the materials and processing expertise of NYSCC, the manufacturing expertise of Meadow River Enterprises, and the phosphor development expertise of OSRAM Sylvania to develop an improved SSCL system. The development plan also includes important contributions by Marshall University (a part of the West Virginia University system). All primary development objectives have been achieved with the exception of improved phosphor powders. The performance characteristics of the first generation SSCL devices were carefully analyzed in year 1 and a second generation lamp was defined and optimized in year 2. The provisional patent was ''perfected'' through a comprehensive patent application filed in November 2002. Lamp efficiency was improved more than 2:1.

  20. Solid State Molecular Reactors in Space

    NASA Astrophysics Data System (ADS)

    Maurette, M.

    2011-03-01

    Lunar minerals and impact glasses, convert the polyatomic beam of solar wind (SW) ions into a flux of small molecules (e.g., H2, N2, H2O, CO, CO2, CH4, C2H4, C2H6, HCN, metal carbides and deuterides, etc.). They thus behave as "Solid State Molecular Reactors". Moreover, ~100-200 μm size micrometeoroids (μMs) have also been exposed to the SW in the zodiacal cloud, before being captured by the Earth and recovered as Antarctic micrometeorites. They are mostly composed of a PAH-rich hydrous-carbonaceous material, which amplifies their power as molecular reactors. In particular, during the first ~200 Myr of the post-lunar period, about 75% of the μMs have been melted and/or volatilized upon atmospheric entry. The release of their volatile species triggered a cosmic volcanism around the mesopause that ruled the formation of the early Earth's atmosphere and climate. Furthermore, a fraction of the μMs that survive unmelted upon atmospheric entry did settle on the proto-oceans floors. Upon further burial in sediments their constituent PAH-rich kerogen was cracked into abiotic oil, which generated giant oil slicks that fed prebiotic chemistry. Many stars, of all ages and types, are embedded into a secondary debris-disk loaded with ion implanted μMs. Some of them are expelled to the interstellar medium (ISM) where they behave first as "dormant-invisible" molecular reactors, until they became reactivated by various processes to synthesize interstellar molecules. This short paper only focus on some highlights of this research dealing with the synthesis of important interstellar molecules, including the most abundant ones (H2 and CO) and H2O, HCN and PAHs, all involved in prebiotic chemistry.

  1. General purpose solid state camera for SERTS

    NASA Astrophysics Data System (ADS)

    Payne, Leslie J.; Haas, J. Patrick

    1996-11-01

    The Laboratory for Astronomy and Solar Physics at Goddard Space Flight Center uses a variety of CCD's and other solid state imaging sensors for its instrumentation programs. Traditionally, custom camera systems are built around the imaging device to optimize the circuitry for the particular sensor. This usually produces a camera that is small, uses little power and is elegant. Although these are desirable characteristics, this approach is also expensive and time consuming. An alternative approach is to design a `universal' camera that is easily customized to meet specific mission requirements. This is the approach our team used for SERTS. The camera design used to support the SERTS mission is a general purpose camera design that is derived from an existing camera on the SOHO spacecraft. This camera is designed to be rugged, modest in power requirements and flexible. The base design of the camera supports quadrant CCD devices with up to 4 phases. Imaging devices with simpler architectures are in general supportable. The basic camera is comprised of a main electronics box which performs all timing generation, voltage level control, data processing and compression. A second unit, placed close to the detector head, is responsible for driving the image device control electrodes and amplifying the multichannel detector video. Programmable high voltage units are used for the single stage MCP type intensifier. The detector head is customized for each sensor type supported. Auxiliary equipment includes a frame buffer that works either as a multi-frame storage unit or as a photon counting accumulation unit. This unit also performs interface buffering so that the camera may appear as a piece of GPIB instrumentation.

  2. Solid state device technology for Solar Power Satellite

    NASA Technical Reports Server (NTRS)

    Weir, D. G.

    1980-01-01

    The feasibility of using solid state elements in the solar power satellite transmitter system is addressed. Recommendations are given concerning device types, the antenna modules, and the overall antenna system. The development of a solid state amplifier based on GaAs field effect transistor devices is also described.

  3. Metal speciation of phosphorus derived from solid state spectroscopic analysis

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Significant improvements have been made in the last decade towards understanding metal species associated with manure P using XANES and solid-state 31P NMR techniques. Both solid-state techniques are particularly sensitive to inorganic forms of P associated with metals in manure samples. In unamen...

  4. Relaxation-Compensated Difference Spin Diffusion NMR for Detecting 13C-13C Long-Range Correlations in Proteins and Polysaccharides

    PubMed Central

    Wang, Tuo; Williams, Jonathan K.; Schmidt-Rohr, Klaus; Hong, Mei

    2015-01-01

    The measurement of long-range distances remains a challenge in solid-state NMR structure determination of biological macromolecules. In 2D and 3D correlation spectra of uniformly 13C-labeled biomolecules, inter-residue, inter-segmental, and intermolecular 13C-13C cross peaks that provide important long-range distance constraints for three-dimensional structures often overlap with short-range cross peaks that only reflect the covalent structure of the molecule. It is therefore desirable to develop new approaches to obtain spectra containing only long-range cross peaks. Here we show that a relaxation-compensated modification of the commonly used 2D 1H-driven spin diffusion (PDSD) experiment allows the clean detection of such long-range cross peaks. By adding a z-filter to keep the total z-period of the experiment constant, we compensate for 13C T1 relaxation. As a result, the difference spectrum between a long- and a scaled short-mixing time spectrum show only long-range correlation signals. We show that one- and two-bond cross peaks equalize within a few tens of milliseconds. Within ~200 ms, the intensity equilibrates within an amino acid residue and a monosaccharide to a value that reflects the number of spins in the local network. With T1 relaxation compensation, at longer mixing times, inter-residue and inter-segmental cross peaks increase in intensity whereas intra-segmental cross-peak intensities remain unchanged relative to each other and can all be subtracted out. Without relaxation compensation, the difference 2D spectra exhibit both negative and positive intensities due to heterogeneous T1 relaxation in most biomolecules, which can cause peak cancellation. We demonstrate this relaxation-compensated difference PDSD approach on amino acids, monosaccharides, a crystalline model peptide, a membrane-bound peptide and a plant cell wall sample. The resulting difference spectra yield clean multi-bond, inter-residue and intermolecular correlation peaks, which are

  5. 2010 Ceramics, Solid State Studies in Gordon Research Conference

    SciTech Connect

    John Halloran

    2010-08-20

    The 2010 Gordon Conference on Solid State Studies in Ceramics will present forefront research on ceramic materials in energy conversion, storage, and environmental sustainability. Oxide materials in advanced Li-ion batteries will be featured, including first principles computational methods, new experimental methods, novel synthesis, and the design of batteries that exploit nanoscale cathode materials. Several speakers address advances in oxides for solar applications, including photo-catalysts for solar hydrogen production and dye sensitized solar cells, along with thin film photovoltaics. Fast ionic conducting ceramics in electrochemical energy conversion and storage will be addressed for fuel cells and electrochemical storage. New concepts for electrochemical capacitor materials will be addressed, as will thermoelectric, geopolymers, and ceramics in nuclear energy. The Conference will bring together investigators at the forefront of their field as well as junior scientists in a collegial atmosphere, with programmed discussion sessions and informal gatherings in the afternoons and evenings. Poster presentations provide opportunities for junior scientists and graduate students to present their work and exchange ideas with leaders in the field. This Conference provides an avenue for scientists from different disciplines to explore new ideas and promotes cross-disciplinary collaborations in the various research areas represented.

  6. Nitride and Oxynitride Based Phosphors for Solid State Lighting

    SciTech Connect

    Tian, Yongchi

    2011-10-15

    The objective of the project is to advance the technology of the Lightscape Materials Inc. (Lightscape) proprietary nitride and oxynitride phosphors for solid state lighting (SSL) from the current level of maturity of applied research to advanced engineering development. This objective will be accomplished by optimizing the novel nitride and oxynitride phosphors, whose formulations are listed in Table 1, and establishing cost-effective preparation processes for the phosphors. The target performances of the phosphors are: • High luminescence efficiency: Quantum Yield = 90%. • Superior thermal stability of luminescence: Thermal Quenching Loss <10% at 150 °C. • Superior environmental stability: Luminescence Maintenance >90% after 5,000 hours at 85 °C and 85% relative humidity. • Scattering loss <10%. • Cost-effective preparation processes. The resulting phosphor materials and their preparation processes are anticipated to be a drop-in component for product development paths undertaken by LED lamp makers in the SSL industry. Upon program completion, Lightscape will target market insertion that enables high efficacy, high color rendering index (CRI), high thermal stability and long lifetime LED-based lighting products for general illumination that realizes substantial energy savings.

  7. Non-stationary (13)C-metabolic flux ratio analysis.

    PubMed

    Hörl, Manuel; Schnidder, Julian; Sauer, Uwe; Zamboni, Nicola

    2013-12-01

    (13)C-metabolic flux analysis ((13)C-MFA) has become a key method for metabolic engineering and systems biology. In the most common methodology, fluxes are calculated by global isotopomer balancing and iterative fitting to stationary (13)C-labeling data. This approach requires a closed carbon balance, long-lasting metabolic steady state, and the detection of (13)C-patterns in a large number of metabolites. These restrictions mostly reduced the application of (13)C-MFA to the central carbon metabolism of well-studied model organisms grown in minimal media with a single carbon source. Here we introduce non-stationary (13)C-metabolic flux ratio analysis as a novel method for (13)C-MFA to allow estimating local, relative fluxes from ultra-short (13)C-labeling experiments and without the need for global isotopomer balancing. The approach relies on the acquisition of non-stationary (13)C-labeling data exclusively for metabolites in the proximity of a node of converging fluxes and a local parameter estimation with a system of ordinary differential equations. We developed a generalized workflow that takes into account reaction types and the availability of mass spectrometric data on molecular ions or fragments for data processing, modeling, parameter and error estimation. We demonstrated the approach by analyzing three key nodes of converging fluxes in central metabolism of Bacillus subtilis. We obtained flux estimates that are in agreement with published results obtained from steady state experiments, but reduced the duration of the necessary (13)C-labeling experiment to less than a minute. These results show that our strategy enables to formally estimate relative pathway fluxes on extremely short time scale, neglecting cellular carbon balancing. Hence this approach paves the road to targeted (13)C-MFA in dynamic systems with multiple carbon sources and towards rich media. PMID:23860906

  8. 13C CPMAS NMR studies and DFT calculations of triterpene xylosides isolated from Actaea racemosa

    NASA Astrophysics Data System (ADS)

    Jamróz, Marta K.; Paradowska, Katarzyna; Gliński, Jan A.; Wawer, Iwona

    2011-05-01

    13C CPMAS NMR spectra of four triterpene glycosides: cimigenol xyloside ( 1), 26-deoxyactein ( 2), cimicifugoside H-1 ( 3) and 24-acethylhydroshengmanol xyloside ( 4) were recorded and analyzed to characterize their solid-state structure. Experimental data were supported by theoretical calculations of NMR shielding constants with the GIAO/6-31G**-su1 approach. A number of methods for the conformational search and a number of functionals for the DFT calculations were applied to ( 1). The best method was proven to be MMFF or MMFFAQ for the conformational search and the PBE1PBE functional for the DFT calculations. Extra calculations simulating C16 dbnd O⋯HOH hydrogen bond yield the isotropic shielding closer to the experimental solid-state value. For all the compounds CP kinetics parameters were calculated using either the I-S or the I-I*-S model. The analysis of CP kinetics data for methyl groups revealed differences in the T2 time constant for two methyl groups (C29 and C30) linked at C4.

  9. Preliminary field evaluation of solid state cameras for security applications

    SciTech Connect

    Murray, D.W.

    1987-07-01

    Recent developments in solid state imager technology have resulted in a series of compact, lightweight, all-solid-state closed circuit television (CCTV) cameras. Although it is widely known that the various solid state cameras have less light sensitivity and lower resolution than their vacuum tube counterparts, the potential for having a much longer Mean Time Between Failure (MTBF) for the all-solid-state cameras is generating considerable interest within the security community. Questions have been raised as to whether the newest and best of the solid state cameras are a viable alternative to the high maintenance vacuum tube cameras in exterior security applications. To help answer these questions, a series of tests were performed by Sandia National Laboratories at various test sites and under several lighting conditions. The results of these tests as well as a description of the test equipment, test sites, and procedures are presented in this report.

  10. Sample preparation for actinide solid state research

    NASA Astrophysics Data System (ADS)

    Spirlet, J. C.

    1982-09-01

    The actinide elements (5f elements) and their compounds constitute a very interesting group for solid state research. The electronic properties of the 5f elements show intermediate behavior between the well-understood, completely localized 4f system (lanthanides) and the 3d system (transition elements). The possibility of understanding some unexplained properties of the 3d elements through a systematic investigation of the electronic structures of the actinides considerably increased interest in samples with well-defined composition and structure and with well-known purity. In some cases, single crystals of low defect densities and high purity levels are needed to allow sophisticated investigations of physical properties. Actinide compounds are easily obtained at a high purity level by direct synthesis from pure elements using noncontaminating techniques. Examples of these techniques are the reaction of the actinide metal powder with the vapor of an oxidant in a sealed quartz ampoule, leviation melting on a water-cooled pedestal or melting in a Huking crucible. Actinide metals are produced by metallothermic reduction of commercially available oxides or carbides or by the van Arkel purification process. The metals are refined to the desired purity level by evaporation in vacuum for the more volatile elements (Ac, Pu, Am, Cm, Bk) and by the van Arkel process for the metals with low vapor pressure. Single crystals of actinide compounds have been grown by chemical vapor transport methods (oxides, chalcogenides), high temperature solution growth techniques (oxides), and pulling from the melt by the Czochralski method (oxides, intermetallics). Thin solid films have been prepared by vacuum evaporation or by focused ion-beam sputtering. The materials are analyzed for trace-level impurity content by inductively-coupled plasma spectroscopy, by spark source mass spectroscopy and by secondary-ion mass spectroscopy. The chemical composition of the compounds is determined by

  11. Solid-state impact-ionization multiplier

    NASA Astrophysics Data System (ADS)

    Lee, Hong-Wei

    This dissertation presents an innovative solid-state current amplifier based on impact-ionization. Unlike avalanche photodetectors which use the same amplification principle, this device can be integrated with any external current source. A discrete amplifier was built on a silicon surface using standard CMOS fabrication processes including lithography, oxidation, ion implantation, diffusion, chemical wet etching, metal deposition, annealing, and rapid thermal processing. Testing was performed by connecting the device to a silicon photodiode, indium-gallium-arsenide photodiodes, and a function generator to demonstrate its compatibility with arbitrary current sources. Current gains above 100 along with pre-amplified leakage currents of less than 10 nA were measured. This amplifier can also be cascaded to achieve very high gains similar to the photomultiplier tube but with much smaller size and no vacuum environment required. Testing was done by amplifying the output signal from an external silicon photodiode. Current gains over 600 were measured when two amplifying devices were cascaded. Additionally, the gain saturation phenomenon of the amplifier due to the space-charge effect is investigated. The measured gain saturation is observed to match very well with the theoretical based predictions. We also present a design rule for obtaining high current gain from the cascaded structure without experiencing gain saturation. Initial bandwidth of the SIM when connected to a silicon photodiode was measured to be about 300 kHz. As we replace the photodiode by a function generator, the bandwidth improved to 450 kHz which is the frequency limit of the system. These results were made on the first generation of SIM devices. We discovered that the space-charge resistance Rsc plays a significant role in determining frequency response. In future generations of the device, we can begin with optimizing the device geometry to reduce this resistance. Also, we can reduce the size of the

  12. ADVANCED SOLID STATE SENSORS FOR VISION 21 SYSTEMS

    SciTech Connect

    C.D. Stinespring

    2005-04-28

    Silicon carbide (SiC) is a high temperature semiconductor with the potential to meet the gas and temperature sensor needs in both present and future power generation systems. These devices have been and are currently being investigated for a variety of high temperature sensing applications. These include leak detection, fire detection, environmental control, and emissions monitoring. Electronically these sensors can be very simple Schottky diode structures that rely on gas-induced changes in electrical characteristics at the metal-semiconductor interface. In these devices, thermal stability of the interfaces has been shown to be an essential requirement for improving and maintaining sensor sensitivity and lifetime. In this report, we describe device fabrication and characterization studies relevant to the development of SiC based gas and temperature sensors. Specifically, we have investigated the use of periodically stepped surfaces to improve the thermal stability of the metal semiconductor interface for simple Pd-SiC Schottky diodes. These periodically stepped surfaces have atomically flat terraces on the order of 200 nm wide separated by steps of 1.5 nm height. It should be noted that 1.5 nm is the unit cell height for the 6H-SiC (0001) substrates used in these studies. These surfaces contrast markedly with the ''standard'' SiC surfaces normally used in device fabrication. Obvious scratches and pots as well as subsurface defects characterize these standard surfaces. This research involved ultrahigh vacuum deposition and characterization studies to investigate the thermal stability of Pd-SiC Schottky diodes on both the stepped and standard surfaces, high temperature electrical characterization of these device structures, and high temperature electrical characterization of diodes under wet and dry oxidizing conditions. To our knowledge, these studies have yielded the first electrical characterization of actual sensor device structures fabricated under ultrahigh vacuum conditions. The results demonstrate that the Pd-SiC interfaces formed on the stepped surface are remarkably stable at temperatures up to 670 C and that there is a definite improvement in the electrical characteristics. This temperature, though lower than DOE target temperatures is still 100 C higher than that used in reported field studies. The Pd films studied here ranged in thickness from the monolayer level ({approx}0.4 nm) to actual device dimensions ({approx}46.5 nm) and are deposited under ultrahigh vacuum conditions at {approx}50 C. The films were characterized in-situ using Auger electron spectroscopy both before and after annealing at 670 C. The Auger lineshapes were used to provide quantitative information on the chemistry of the reaction products. Ex-situ atomic force microscopy was used to characterize changes in surface morphology. Current-voltage (I-V) measurements were made as a function of temperature to further characterize the devices. Additional studies were performed to gain an understanding of the effects of wet and dry oxidizing environments on device performance. These measurements were performed for temperatures up to 325 C, the highest temperature attainable with our current apparatus. Our results clearly show a significant benefit in thermal stability and electrical characteristics associated with the stepped surface. These results are quite promising but much development and testing work remains to be done.

  13. Recent Advances in Solid-State Electronic Terahertz Systems

    NASA Astrophysics Data System (ADS)

    Rieh, Jae-Sung; Kim, Dong-Hyun; Kim, Kyungmin; Kim, Hyunchul

    The terahertz (THz) band generally indicates the spectrum range that falls on roughly between the traditional electrical and optical frequency bands. Its definition varies over different sources, but one widely accepted definition is the frequency range of 0.1-10 THz. In terms of the wavelength in free space, it corresponds to the range of 3-0.03 mm. In terms of the more readily accepted band definition in the scientific community, the THz band partly include the millimeter-wave band (1 mm-1 cm, or 30-300 GHz) for the lower side and the infrared band (0.3 mm-750 nm, or 1-400 THz) for the upper boundary, while it covers the entire range of sub-millimeter band (0.1-1 mm, or 300 GHz-3 THz). It is notable that the range includes some scientifically significant points, one example being the frequency that corresponds to a photon energy equal to kT at room temperature (~6.2 THz).

  14. Distinct fungal and bacterial δ13C signatures can drive the increase in soil δ13C with depth

    NASA Astrophysics Data System (ADS)

    Kohl, Lukas; Laganièrea, Jérôme; Edwards, Kate A.; Billings, Sharon A.; Morrill, Penny L.; Van Biesen, Geert; Ziegler, Susan E.

    2015-04-01

    Soil microbial biomass is a key precursor of soil organic carbon (SOC), and the enrichment in 13C during SOC diagenesis has been purported to be driven by increasing proportions of microbially derived SOC. Yet, little is known about how the δ13C of soil microbial biomass - and by extension the δ13C of microbial inputs to SOC - vary in space, time, or with the composition of the microbial community. Phospholipid fatty acids (PLFA) can be analyzed to measure the variation of the natural abundance δ13C values of both individual groups of microorganisms and the microbial community as a whole. Here, we show how variations of δ13CPLFA within the soil profile provides insight into C fluxes in undisturbed soils and demonstrate that distinct δ13C of fungal and bacterial biomass and their relative abundance can drive the increase of bulk δ13CSOC with depth. We studied the variation in natural abundance δ13C signatures of PLFA in podzolic soil profiles from mesic boreal forests in Atlantic Canada. Samples from the organic horizons (L,F,H) and the mineral (B; top 10 cm) horizons were analyzed for δ13C values of PLFA specific to fungi, G+ bacteria, or G- bacteria as proxies for the δ13C of the biomass of these groups, and for δ13C values of PLFA produced by a wide range of microorganisms (e.g. 16:0) as a proxy for the δ13C value of microbial biomass as a whole. Results were compared to fungi:bacteria ratios (F:B) and bulk δ13CSOC values. The δ13C values of group-specific PLFA were driven by differences among source organisms, with fungal PLFA consistently depleted (2.1 to 6.4‰) relative to and G+ and G- bacterial PLFA in the same sample. All group-specific PLFA, however, exhibited nearly constant δ13C values throughout the soil profile, apparently unaffected by the over 2.8‰ increase in δ13CSOC with depth from the L to B horizons. This indicates that bulk SOC poorly represents the substrates actually consumed by soil microorganisms in situ. Instead, our

  15. Synthesis of D-[U-{sup 13}C]Glucal, D-[U-{sup 13}C] Galactal, and L-[U-{sup 13}C]Fucose for NMR structure studies of oligosaccharides

    SciTech Connect

    Wu, R.; Unkefer, C.J.; Silks, L.A. III

    1996-12-31

    The role of carbohydrates is well recognized in a variety of important biological phenomena such as cell surface recognition. Recent advances in carbohydrate chemistry, including the development of solid phase synthesis methods, have helped to provide significant quantities of material by offering general protocols for synthesis of well-defined, pure material. However, the study of the solution structure of oligosaccharides by nuclear magnetic resonance techniques have been hampered by the lack of enriched {sup 13}C material. In an effort to help alleviate this situation, we have been interested in the construction of the title compounds from a single economical carbon source, D-[U-{sup 13}C]glucose. Details of the syntheses will be provided.

  16. Area per Lipid and Cholesterol Interactions in Membranes from Separated Local-Field 13C NMR Spectroscopy

    PubMed Central

    Leftin, Avigdor; Molugu, Trivikram R.; Job, Constantin; Beyer, Klaus; Brown, Michael F.

    2014-01-01

    Investigations of lipid membranes using NMR spectroscopy generally require isotopic labeling, often precluding structural studies of complex lipid systems. Solid-state 13C magic-angle spinning NMR spectroscopy at natural isotopic abundance gives site-specific structural information that can aid in the characterization of complex biomembranes. Using the separated local-field experiment DROSS, we resolved 13C-1H residual dipolar couplings that were interpreted with a statistical mean-torque model. Liquid-disordered and liquid-ordered phases were characterized according to membrane thickness and average cross-sectional area per lipid. Knowledge of such structural parameters is vital for molecular dynamics simulations, and provides information about the balance of forces in membrane lipid bilayers. Experiments were conducted with both phosphatidylcholine (dimyristoylphosphatidylcholine (DMPC) and palmitoyloleoylphosphatidylcholine (POPC)) and egg-yolk sphingomyelin (EYSM) lipids, and allowed us to extract segmental order parameters from the 13C-1H residual dipolar couplings. Order parameters were used to calculate membrane structural quantities, including the area per lipid and bilayer thickness. Relative to POPC, EYSM is more ordered in the ld phase and experiences less structural perturbation upon adding 50% cholesterol to form the lo phase. The loss of configurational entropy is smaller for EYSM than for POPC, thus favoring its interaction with cholesterol in raftlike lipid systems. Our studies show that solid-state 13C NMR spectroscopy is applicable to investigations of complex lipids and makes it possible to obtain structural parameters for biomembrane systems where isotope labeling may be prohibitive. PMID:25418296

  17. Whole-core analysis by sup 13 C NMR

    SciTech Connect

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

    1991-06-01

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

  18. Accurate quantitative 13C NMR spectroscopy: repeatability over time of site-specific 13C isotope ratio determination.

    PubMed

    Caytan, Elsa; Botosoa, Eliot P; Silvestre, Virginie; Robins, Richard J; Akoka, Serge; Remaud, Gérald S

    2007-11-01

    The stability over time (repeatability) for the determination of site-specific 13C/12C ratios at natural abundance by quantitative 13C NMR spectroscopy has been tested on three probes: enriched bilabeled [1,2-13C2]ethanol; ethanol at natural abundance; and vanillin at natural abundance. It is shown in all three cases that the standard deviation for a series of measurements taken every 2-3 months over periods between 9 and 13 months is equal to or smaller than the standard deviation calculated from 5-10 replicate measurements made on a single sample. The precision which can be achieved using the present analytical 13C NMR protocol is higher than the prerequisite value of 1-2 per thousand for the determination of site-specific 13C/12C ratios at natural abundance (13C-SNIF-NMR). Hence, this technique permits the discrimination of very small variations in 13C/12C ratios between carbon positions, as found in biogenic natural products. This observed stability over time in 13C NMR spectroscopy indicates that further improvements in precision will depend primarily on improved signal-to-noise ratio. PMID:17900175

  19. State-of-the-Art Direct 13C and Indirect 1H-[13C] NMR Spectroscopy In Vivo

    PubMed Central

    de Graaf, Robin A.; Rothman, Douglas L.; Behar, Kevin L.

    2013-01-01

    Carbon-13 NMR spectroscopy in combination with 13C-labeled substrate infusion is a powerful technique to measure a large number of metabolic fluxes non-invasively in vivo. It has been used to quantify glycogen synthesis rates, establish quantitative relationships between energy metabolism and neurotransmission and evaluate the importance of different substrates. All measurements can, in principle, be performed through direct 13C NMR detection or via indirect 1H-[13C] NMR detection of the protons attached to 13C nuclei. The choice for detection scheme and pulse sequence depends on the magnetic field strength, whereas substrate selection depends on the metabolic pathways that are studied. 13C NMR spectroscopy remains a challenging technique that requires several non-standard hardware modifications, infusion of 13C-labeled substrates and sophisticated processing and metabolic modeling. Here the various aspects of direct 13C and indirect 1H-[13C] NMR are reviewed with the aim of providing a practical guide. PMID:21919099

  20. Phenylazoindole dyes 3: Determination of azo-hydrazone tautomers of new phenylazoindole dyes in solution and solid state

    NASA Astrophysics Data System (ADS)

    Babür, Banu; Seferoğlu, Nurgül; Aktan, Ebru; Hökelek, Tuncer; Şahin, Ertan; Seferoğlu, Zeynel

    2015-02-01

    A new two series of phenylazo indole dyes was synthesized and the structures of the dyes were confirmed by UV-vis, FT-IR, HRMS and 1H/13C NMR spectroscopic techniques. Five of these dyes (I, I‧, II‧, III and III‧) were also characterized in solid state by using single crystal X-ray diffraction studies besides other spectroscopic techniques. The geometries of the azo and hydrazone tautomeric forms of the dyes were optimized by using Density Functional Theory (DFT). In addition, the effects of the donor and acceptor groups on the azo and hydrazone forms of the dyes were evaluated experimentally and theoretically. The results indicate that the phenylazoindole dyes derived from 2-phenyl indole as coupling component exist as azo form in solution, gas phase and solid state.

  1. The Galileo Solid-State Imaging experiment

    USGS Publications Warehouse

    Belton, M.J.S.; Klaasen, K.P.; Clary, M.C.; Anderson, J.L.; Anger, C.D.; Carr, M.H.; Chapman, C.R.; Davies, M.E.; Greeley, R.; Anderson, D.; Bolef, L.K.; Townsend, T.E.; Greenberg, R.; Head, J. W., III; Neukum, G.; Pilcher, C.B.; Veverka, J.; Gierasch, P.J.; Fanale, F.P.; Ingersoll, A.P.; Masursky, H.; Morrison, D.; Pollack, James B.

    1992-01-01

    The Solid State Imaging (SSI) experiment on the Galileo Orbiter spacecraft utilizes a high-resolution (1500 mm focal length) television camera with an 800 ?? 800 pixel virtual-phase, charge-coupled detector. It is designed to return images of Jupiter and its satellites that are characterized by a combination of sensitivity levels, spatial resolution, geometric fiedelity, and spectral range unmatched by imaging data obtained previously. The spectral range extends from approximately 375 to 1100 nm and only in the near ultra-violet region (??? 350 nm) is the spectral coverage reduced from previous missions. The camera is approximately 100 times more sensitive than those used in the Voyager mission, and, because of the nature of the satellite encounters, will produce images with approximately 100 times the ground resolution (i.e., ??? 50 m lp-1) on the Galilean satellites. We describe aspects of the detector including its sensitivity to energetic particle radiation and how the requirements for a large full-well capacity and long-term stability in operating voltages led to the choice of the virtual phase chip. The F/8.5 camera system can reach point sources of V(mag) ??? 11 with S/N ??? 10 and extended sources with surface brightness as low as 20 kR in its highest gain state and longest exposure mode. We describe the performance of the system as determined by ground calibration and the improvements that have been made to the telescope (same basic catadioptric design that was used in Mariner 10 and the Voyager high-resolution cameras) to reduce the scattered light reaching the detector. The images are linearly digitized 8-bits deep and, after flat-fielding, are cosmetically clean. Information 'preserving' and 'non-preserving' on-board data compression capabilities are outlined. A special "summation" mode, designed for use deep in the Jovian radiation belts, near Io, is also described. The detector is 'preflashed' before each exposure to ensure the photometric linearity

  2. Atomic resolution protein structure determination by three-dimensional transferred echo double resonance solid-state nuclear magnetic resonance spectroscopy

    PubMed Central

    Nieuwkoop, Andrew J.; Wylie, Benjamin J.; Franks, W. Trent; Shah, Gautam J.; Rienstra, Chad M.

    2009-01-01

    We show that quantitative internuclear 15N–13C distances can be obtained in sufficient quantity to determine a complete, high-resolution structure of a moderately sized protein by magic-angle spinning solid-state NMR spectroscopy. The three-dimensional ZF-TEDOR pulse sequence is employed in combination with sparse labeling of 13C sites in the β1 domain of the immunoglobulin binding protein G (GB1), as obtained by bacterial expression with 1,3-13C or 2-13C-glycerol as the 13C source. Quantitative dipolar trajectories are extracted from two-dimensional 15N–13C planes, in which ∼750 cross peaks are resolved. The experimental data are fit to exact theoretical trajectories for spin clusters (consisting of one 13C and several 15N each), yielding quantitative precision as good as 0.1 Å for ∼350 sites, better than 0.3 Å for another 150, and ∼1.0 Å for 150 distances in the range of 5–8 Å. Along with isotropic chemical shift-based (TALOS) dihedral angle restraints, the distance restraints are incorporated into simulated annealing calculations to yield a highly precise structure (backbone RMSD of 0.25±0.09 Å), which also demonstrates excellent agreement with the most closely related crystal structure of GB1 (2QMT, bbRMSD 0.79±0.03 Å). Moreover, side chain heavy atoms are well restrained (0.76±0.06 Å total heavy atom RMSD). These results demonstrate for the first time that quantitative internuclear distances can be measured throughout an entire solid protein to yield an atomic-resolution structure. PMID:19739873

  3. Sensitivity-enhanced IPAP experiments for measuring one-bond 13C '- 13C α and 13C α- 1H α residual dipolar couplings in proteins

    NASA Astrophysics Data System (ADS)

    Ding, Keyang; Gronenborn, Angela M.

    2004-04-01

    Sensitivity-enhanced 2D IPAP experiments using the accordion principle for measuring one-bond 13C '- 13C α and 1H α- 13C α dipolar couplings in proteins are presented. The resolution of the resulting spectra is identical to that of the decoupled HSQC spectra and the sensitivity of the corresponding 1D acquisitions are only slightly lower than those obtained with 3D HNCO and 3D HN(COCA)HA pulse sequences due to an additional delay 2 Δ. For cases of limited resolution in the 2D 15N- 1H N HSQC spectrum the current pulse sequences can easily be modified into 3D versions by introducing a poorly digitized third dimension, if so desired. The experiments described here are a valuable addition to the suites available for determination of residual dipolar couplings in biological systems.

  4. [Characterization of biochar by X-ray photoelectron spectroscopy and 13C nuclear magnetic resonance].

    PubMed

    Xu, Dong-yu; Jin, Jie; Yan, Yu; Han, Lan-fang; Kang, Ming-jie; Wang, Zi-ying; Zhao, Ye; Sun, Ke

    2014-12-01

    The wood (willow branch) and grass (rice straw) materials were pyrolyzed at different temperatures (300, 450 and 600 °C) to obtain the biochars used in the present study. The biochars were characterized using elementary analysis, X-ray photoelectron spectroscopy (XPS) and solid state 13C cross-polarization and magic angle spinning nuclear magnetic resonance spectroscopy (13C NMR) to illuminate the structure and composition of the biochars which were derived from the different thermal temperatures and biomass. The results showed that the H/C, O/C and (O+N)/C ratios of the biochars decreased with the increase in the pyrolysis temperatures. The surface polarity and ash content of the grass-derived biochars were higher than those of the wood-derived biochars. The minerals of the wood-derived biochars were mainly covered by the organic matter; in contrast, parts of the mineral surfaces of the grass-derived biochars were not covered by organic matter? The 13C NMR of the low temperature-derived biochars revealed a large contribution of aromatic carbon, aliphatic carbon, carboxyl and carbonyl carbon, while the high temperature-derived biochars contained a large amount of aromatic carbon. Moreover, the wood-derived biochars produced at low heat treatment temperatures contained more lignin residues than grass-derived ones, probably due to the existence of high lignin content in the feedstock soures of wood-derived biochars. The results of the study would be useful for environmental application of biochars. PMID:25881450

  5. The Influence of Plant Litter on Soil Water Repellency: Insight from 13C NMR Spectroscopy.

    PubMed

    Cesarano, Gaspare; Incerti, Guido; Bonanomi, Giuliano

    2016-01-01

    Soil water repellency (SWR, i.e. reduced affinity for water owing to the presence of organic hydrophobic coatings on soil particles) has relevant hydrological implications because low rates of infiltration enhance water runoff, and untargeted diffusion of fertilizers and pesticides. Previous studies investigated the occurrence of SWR in ecosystems with different vegetation cover but did not clarify its relationships with litter biochemical quality. Here, we investigated the capability of different plant litter types to induce SWR by using fresh and decomposed leaf materials from 12 species, to amend a model sandy soil over a year-long microcosm experiment. Water repellency, measured by the Molarity of an Ethanol Droplet (MED) test, was tested for the effects of litter species and age, and compared with litter quality assessed by 13C-CPMAS NMR in solid state and elemental chemical parameters. All litter types were highly water repellent, with MED values of 18% or higher. In contrast, when litter was incorporated into the soil, only undecomposed materials induced SWR, but with a large variability of onset and peak dynamics among litter types. Surprisingly, SWR induced by litter addition was unrelated to the aliphatic fraction of litter. In contrast, lignin-poor but labile C-rich litter, as defined by O-alkyl C and N-alkyl and methoxyl C of 13C-CPMAS NMR spectral regions, respectively, induced a stronger SWR. This study suggests that biochemical quality of plant litter is a major controlling factor of SWR and, by defining litter quality with 13C-CPMAS NMR, our results provide a significant novel contribution towards a full understanding of the relationships between plant litter biochemistry and SWR. PMID:27022916

  6. The Influence of Plant Litter on Soil Water Repellency: Insight from 13C NMR Spectroscopy

    PubMed Central

    Cesarano, Gaspare; Incerti, Guido; Bonanomi, Giuliano

    2016-01-01

    Soil water repellency (SWR, i.e. reduced affinity for water owing to the presence of organic hydrophobic coatings on soil particles) has relevant hydrological implications because low rates of infiltration enhance water runoff, and untargeted diffusion of fertilizers and pesticides. Previous studies investigated the occurrence of SWR in ecosystems with different vegetation cover but did not clarify its relationships with litter biochemical quality. Here, we investigated the capability of different plant litter types to induce SWR by using fresh and decomposed leaf materials from 12 species, to amend a model sandy soil over a year-long microcosm experiment. Water repellency, measured by the Molarity of an Ethanol Droplet (MED) test, was tested for the effects of litter species and age, and compared with litter quality assessed by 13C-CPMAS NMR in solid state and elemental chemical parameters. All litter types were highly water repellent, with MED values of 18% or higher. In contrast, when litter was incorporated into the soil, only undecomposed materials induced SWR, but with a large variability of onset and peak dynamics among litter types. Surprisingly, SWR induced by litter addition was unrelated to the aliphatic fraction of litter. In contrast, lignin-poor but labile C-rich litter, as defined by O-alkyl C and N-alkyl and methoxyl C of 13C-CPMAS NMR spectral regions, respectively, induced a stronger SWR. This study suggests that biochemical quality of plant litter is a major controlling factor of SWR and, by defining litter quality with 13C-CPMAS NMR, our results provide a significant novel contribution towards a full understanding of the relationships between plant litter biochemistry and SWR. PMID:27022916

  7. Solid-state optical refrigeration to sub-100 Kelvin regime

    NASA Astrophysics Data System (ADS)

    Melgaard, Seth D.; Albrecht, Alexander R.; Hehlen, Markus P.; Sheik-Bahae, Mansoor

    2016-02-01

    Since the first demonstration of net cooling twenty years ago, optical refrigeration of solids has progressed to outperform all other solid-state cooling processes. It has become the first and only solid-state refrigerator capable of reaching cryogenic temperatures, and now the first solid-state cooling below 100 K. Such substantial progress required a multi-disciplinary approach of pump laser absorption enhancement, material characterization and purification, and thermal management. Here we present the culmination of two decades of progress, the record cooling to ≈ 91 K from room temperature.

  8. Fabrication and characterization of solid-state, conducting polymer actuators

    SciTech Connect

    Xie, J.; Sansinena, J. M.; Gao, J.; Wang, H. L.

    2004-01-01

    We report here the fabrication and characterization of solid-state, conducting polymer actuators. The electrochemical activity of polyaniline (PANI) thin film coated with solid-state polyelectrolyte is very similar to the polyaniline thin film in an aqueous solution. The solid-state actuator is adhere to a lever arm of an force transducer and the force generation is measured in real time. The force generated by the actuator is found to be length dependent. However, the overall torques generated by the actuators with different lengths remains essentially the same. The effect of stimulation signals such as voltage, current, on the bending angle and displacement is also studied using square wave potential.

  9. Solar Power Satellite (SPS) solid-state antenna power combiner

    NASA Technical Reports Server (NTRS)

    1980-01-01

    A low loss power-combining microstrip antenna suitable for solid state solar power satellite (SPS) application was developed. A unique approach for performing both the combining and radiating function in a single cavity-type circuit was verified, representing substantial refinements over previous demonstration models in terms of detailed geometry to obtain good matching and adequate bandwidth at the design frequency. The combiner circuit was designed, built, and tested and the overall results support the view that the solid state power-combining antenna approach is a viable candidate for a solid state SPS antenna building block.

  10. Solid-state optical refrigeration to sub-100 Kelvin regime.

    PubMed

    Melgaard, Seth D; Albrecht, Alexander R; Hehlen, Markus P; Sheik-Bahae, Mansoor

    2016-01-01

    Since the first demonstration of net cooling twenty years ago, optical refrigeration of solids has progressed to outperform all other solid-state cooling processes. It has become the first and only solid-state refrigerator capable of reaching cryogenic temperatures, and now the first solid-state cooling below 100 K. Such substantial progress required a multi-disciplinary approach of pump laser absorption enhancement, material characterization and purification, and thermal management. Here we present the culmination of two decades of progress, the record cooling to ≈ 91 K from room temperature. PMID:26847703

  11. Solid-State NMR Studies of Amyloid Fibril Structure

    NASA Astrophysics Data System (ADS)

    Tycko, Robert

    2011-05-01

    Current interest in amyloid fibrils stems from their involvement in neurodegenerative and other diseases and from their role as an alternative structural state for many peptides and proteins. Solid-state nuclear magnetic resonance (NMR) methods have the unique capability of providing detailed structural constraints for amyloid fibrils, sufficient for the development of full molecular models. In this article, recent progress in the application of solid-state NMR to fibrils associated with Alzheimer's disease, prion fibrils, and related systems is reviewed, along with relevant developments in solid-state NMR techniques and technology.

  12. Solid-state optical refrigeration to sub-100 Kelvin regime

    DOE PAGESBeta

    Melgaard, Seth D.; Albrecht, Alexander R.; Hehlen, Markus P.; Sheik-Bahae, Mansoor

    2016-02-05

    We report that since the first demonstration of net cooling twenty years ago, optical refrigeration of solids has progressed to outperform all other solid-state cooling processes. It has become the first and only solid-state refrigerator capable of reaching cryogenic temperatures, and now the first solid-state cooling below 100 K. Such substantial progress required a multi-disciplinary approach of pump laser absorption enhancement, material characterization and purification, and thermal management. Here we present the culmination of two decades of progress, the record cooling to ≈91K from room temperature.

  13. The solid state detector technology for picosecond laser ranging

    NASA Technical Reports Server (NTRS)

    Prochazka, Ivan

    1993-01-01

    We developed an all solid state laser ranging detector technology, which makes the goal of millimeter accuracy achievable. Our design and construction philosophy is to combine the techniques of single photon ranging, ultrashort laser pulses, and fast fixed threshold discrimination while avoiding any analog signal processing within the laser ranging chain. The all solid state laser ranging detector package consists of the START detector and the STOP solid state photon counting module. Both the detectors are working in an optically triggered avalanche switching regime. The optical signal is triggering an avalanche current buildup which results in the generation of a uniform, fast risetime output pulse.

  14. Solid-State Metalloproteins-An Alternative to Immobilisation.

    PubMed

    Rapson, Trevor D

    2016-01-01

    This commentary outlines a protein engineering approach as an alternative to immobilisation developed in our laboratory. We use a recombinant silk protein into which metal active sites can be incorporated to produce solid-state metalloprotein materials. The silk protein directly coordinates to the metal centres providing control over their reactivity akin to that seen in naturally occurring metalloproteins. These solid-state materials are remarkably stable at a range of temperatures and different solvent conditions. I discuss the genesis of this approach and highlight areas where such solid-state materials could find application. PMID:27428936

  15. Solid-state optical refrigeration to sub-100 Kelvin regime

    PubMed Central

    Melgaard, Seth D.; Albrecht, Alexander R.; Hehlen, Markus P.; Sheik-Bahae, Mansoor

    2016-01-01

    Since the first demonstration of net cooling twenty years ago, optical refrigeration of solids has progressed to outperform all other solid-state cooling processes. It has become the first and only solid-state refrigerator capable of reaching cryogenic temperatures, and now the first solid-state cooling below 100 K. Such substantial progress required a multi-disciplinary approach of pump laser absorption enhancement, material characterization and purification, and thermal management. Here we present the culmination of two decades of progress, the record cooling to ≈ 91 K from room temperature. PMID:26847703

  16. Solid State NMR Studies of Amyloid Fibril Structure

    PubMed Central

    Tycko, Robert

    2011-01-01

    Current interest in amyloid fibrils stems from their involvement in neurodegenerative and other diseases and from their role as an alternative structural state for many peptides and proteins. Solid state NMR methods have the unique capability of providing detailed structural constraints for amyloid fibrils, sufficient for the development of full molecular models. In this article, recent progress in the application of solid state NMR to fibrils associated with Alzheimer’s disease, prion fibrils, and related systems is reviewed, along with relevant developments in solid state NMR techniques and technology. PMID:21219138

  17. Diode laser-pumped solid-state lasers

    NASA Technical Reports Server (NTRS)

    Fan, Tso Yee; Byer, Robert L.

    1988-01-01

    Recently, interest in diode laser-pumped solid-state lasers has increased due to their advantages over flashlamp-pumped solid-state lasers. A historical overview is presented of semiconductor diode-pumped solid-state lasers beginning with work in the early 1960s and continuing through recent work on wavelength extension of these devices by laser operation on new transitions. Modeling of these devices by rate equations to obtain expressions for threshold, slope efficiency, and figures of merit is also given.

  18. NMR Determination of Protein pKa Values in the Solid State

    PubMed Central

    Schmidt, Heather L. Frericks; Shah, Gautam J.; Sperling, Lindsay J.; Rienstra, Chad M.

    2010-01-01

    Charged residues play an important role in defining key mechanistic features in many biomolecules. Determining the pKa values of large, membrane or fibrillar proteins can be challenging with traditional methods. In this study we show how solid-state NMR is used to monitor chemical shift changes during a pH titration for the small soluble β1 immunoglobulin binding domain of protein G. The chemical shifts of all the amino acids with charged side-chains throughout the uniformly-13C,15N-labeled protein were monitored over several samples varying in pH; pKa values were determined from these shifts for E27, D36, and E42, and the bounds for the pKa of other acidic side-chain resonances were determined. Additionally, this study shows how the calculated pKa values give insights into the crystal packing of the protein. PMID:20563223

  19. A solid-state NMR investigation of the structure of mesoporous silica nanoparticle supported rhodium catalysts

    SciTech Connect

    Rapp, Jennifer; Huang, Yulin; Natella, Michael; Cai, Yang; Lin, Victor S.-Y.; Pruski, Marek

    2009-01-04

    A detailed study of the chemical structure of mesoporous silica catalysts containing rhodium ligands and nanoparticles (RhP-MSN) was carried out by multi-dimensional solid-state NMR techniques. The degree of functionalization of the rhodium-phosphinosilyl complex to the surface of the RhP-MSN channels was determined by {sup 29}Si NMR experiments. The structural assignments of the rhodium-phosphinosilyl complex were unambiguously determined by employing the novel, indirectly detected heteronuclear correlation ({sup 13}C-{sup 1}H and {sup 31}P-{sup 1}H idHETCOR) techniques, which indicated that oxidation of the attached phosphinosilyl groups and detachment of Rh was enhanced upon syngas conversion.

  20. Rapid and accurate determination of the lignin content of lignocellulosic biomass by solid-state NMR

    PubMed Central

    Fu, Li; McCallum, Scott A.; Miao, Jianjun; Hart, Courtney; Tudryn, Gregory J.; Zhang, Fuming; Linhardt, Robert J.

    2014-01-01

    Biofuels and biomaterials, produced from lignocellulosic feedstock, require facile access to cellulose and hemicellulose to be competitive with petroleum processing and sugar-based fermentation. Physical-chemical barriers resulting from lignin complicates the hydrolysis biomass into fermentable sugars. Thus, the amount of lignin within a substrate is critical in determining biomass processing. The application of 13C cross-polarization, magic-angle spinning, and solid-state nuclear magnetic resonance for the direct quantification of lignin content in biomass is examined. Using a standard curve constructed from pristine lignin and cellulose, the lignin content of a biomass sample is accurately determined through direct measurement without chemical or enzymatic pre-treatment. PMID:25404762