Sample records for structural characterization magnetochemistry

  1. Introduction to magnetochemistry

    CERN Document Server

    Earnshaw, Alan


    Introduction to Magnetochemistry provides an introduction to the more important aspects of magnetochemistry. The measurement of magnetic moment has been one of the most consistently useful to coordination chemists. For teaching purposes it provides a simple method of illustrating the ideas of electronic structure, and in research it can provide fundamental information about the bonding and stereochemistry of complexes. The book contains six chapters covering topics such as free atoms and ions, transition metal complexes, crystal field theory, second and third row transition metal complexes, a

  2. On-surface magnetochemistry


    Wäckerlin, Christian


    This thesis reports on the on-surface magnetochemistry of square-planar transition-metal complexes adsorbed on ferromagnetic substrates. Specifically, the magnetochemistry of the transition-metal ions (Mn / Fe / Co / Ni) coordinated in square-planar porphyrin / phthalocyanine ligands arranged on native and oxygen-reconstructed ferromagnetic Ni(001) / Co(001) thin-films is studied. The metal-centers in the surface-adsorbed complexes are five-fold coordinated: four coordination-bonds with the s...

  3. Magnetochemistry: Compounds and Concepts (United States)

    Lueken, Heiko; Schilder, Helmut; Eifert, Thomas; Handrick, Klaus; Huening, Felix

    New materials in today's magnetochemistry are reviewed, among them spin-crossover compounds, single-molecule magnets, supramolecular magnetic materials, ferrofluids, and ferromagnetic nanocrystal superlattices, each with its specific application potential. Advanced computer programs are available which consider all relevant perturbations on the 'magnetic electrons' and allow, on the basis of precise measurement results, the evaluation of magnetic parameters, above all the exchange parameter J. By means of molecular, ionic, and metallic compounds the J values are discussed with respect to sign and magnitude on the basis of concepts which take into consideration overlap of magnetic orbitals (direct exchange, superexchange) and the conduction electron concentration. Finally, further developments in the field of magnetochemistry are prospected.

  4. A new tetraiminodiphenol macrocyclic ligand and its two dicopper(II) complexes: Syntheses, crystal structures, electrochemistry and magnetochemistry (United States)

    Majumder, Samit; Fleck, Michel; Lucas, C. Robert; Mohanta, Sasankasekhar


    This paper deals with the diprotonated salt, [H4L](ClO4)2 (1), of the tetraiminodiphenolate macrocyclic ligand, H2L which is the [2 + 2] condensation product of 4-ethyl-2,6-diformylphenol and 2,2'-dimethyl-1,3-diaminopropane, and two diphenoxo-bridged dicopper(II) complexes [Cu2L(ClO4)2] (2) and [Cu2L(ClO4)](ClO4) (3). The syntheses, characterization and crystal structures of 1-3 and the magnetic and electrochemical properties of the metal complexes 2 and 3 are presented. The cationic macrocycle [H4L]2+ is stabilized by four intramolecular and symmetric Nsbnd H…O…Hsbnd N hydrogen bonds involving phenoxo oxygen and imino nitrogen atoms. One metal center in 3 is tetracoordinated and in a square planar geometry. The second metal ion of 3 and both the metal ions in 2 are pentacoordinated and in a square pyramidal geometry; one perchlorate oxygen atom occupies the apical position in each case. Both 2 and 3 exhibit quasireversible two-step one-electron couples in the reduction window. The E½ (ΔEp) values (in mV) for the CuIICuII/CuIICuI couple is -0.466 V (0.067 V) for 2 and -0.490 V (0.076 V) for 3, while the E½ (ΔEp) values (in mV) for the CuIICuI/CuICuI couple is -0.953 V (0.060 V) for 2 and -0.985 V (0.069 V) for 3. Variable-temperature (2-300 K) magnetic susceptibility measurements of the two compounds reveal that the metal centers in both of the complexes are coupled by strong antiferromagnetic interactions with 2J values (H = -JS1·S2) of -780 and -820 cm-1 for 2 and 3, respectively.

  5. Magnetochemistry at low temperatures: Crystal structure and magnetic susceptibility of [CoCl 2(3,5-lutidine) 2 (United States)

    Carlin, Richard L.; Vaziri, M.; Sinn, Ekk


    The crystal structure of [CoCl 2(3,5-lutidine) 2] along with magnetic susceptibility measurements over the temperature interval 50 mK-4.2 K are reported. The space group is P2 1/c, with a = 13.075(2), b = 15.903(4), and c = 8.035(1) Å; the angle β = 101.00(2)°. There are four molecules in the unit cell. The molecules are distorted tetrahedra (the Cl-Co-Cl angle is 120.29°) and well-isolated from each other. The magnetic anisotropy of single crystals is large and due to the zero-field splitting. The data may be fit by the spin-Hamiltonian parameters g‖ = 2.1±0.1, g⊥ = 2.1±0.1 and 2D/ kB = (10.5± 1) K. Measurements of the susceptibility of a polycrystalline powder sample show that magnetic ordering does not occur down to 50 mK. This is consistent with the crystal structure.

  6. Database of magnetochemistry in solutions (abstract) (United States)

    Tarasov, O. Ju.; Vinogradov, A. G.


    The database (DB) of magnetochemistry in solutions was created to systematize and to critically review data of the magnetic susceptibility of liquids, solutions, and substances in solutions. The database ``MagChemSol 1.0'' was made on a mfoxplus base and may be supported by dbaseiii plus or higher. Search fields include substances, solvent, condition and method of investigation, critical magnetochemistry characteristics, and references to literature. All material is printable and the database can change and expand itself. System requirements include IBM PC or compatible with 640 Kb of RAM, 5 in. and 3 in. diskette drive or hard-disk, and dos 3.30 or higher; printers are Epson or compatible. The DB ``MagChemSol 1.0'' version includes about 1000 data entries according to the magnetochemical properties, the majority solvents in general use some diamagnetic and paramagnetic salts, and also the complex compounds of d and f elements in the solutions.

  7. Emergence of On-Surface Magnetochemistry


    Ballav, Nirmalya; Waeckerlin, Christian; Siewert, Dorota; Oppeneer, Peter M.; Jung, Thomas A.


    The control of exchange coupling across the molecule–substrate interface is a key feature in molecular spintronics. This Perspective reviews the emerging field of on-surface magnetochemistry, where coordination chemistry is applied to surface-supported metal porphyrins and metal phthalocyanines to control their magnetic properties. The particularities of the surface as a multiatomic ligand or “surface ligand” are introduced. The asymmetry involved in the action of a chemical ligand and a surf...

  8. Theoretical magnetochemistry of dinuclear manganese complexes: broken symmetry density functional theory investigation on the influence of bridging motifs on structure and magnetism. (United States)

    Pantazis, Dimitrios A; Krewald, Vera; Orio, Maylis; Neese, Frank


    A systematic study of the magnetic coupling in homovalent (III-III and IV-IV) and heterovalent (III-IV) manganese dimers as a function of the chemical identity and coordination mode of the bridging ligands is carried out with the aim of establishing a reference library of magnetostructural correlations. Emphasis is placed on rationalising the results through analysis of the superexchange pathways in terms of corresponding orbitals. Additionally, the influence of specific structural distortions on magnetic properties is explored. Consistent with chemical intuition and decades of experience, oxo bridges are shown to be efficient mediators of superexchange, primarily through pi-type pathways, whereas the introduction of bridging carboxylates inhibits the magnetic coupling of the metal centres by introducing structural distortions in the core and by reducing the antiferromagnetic contribution to the exchange. Protonation of oxo bridges is shown to induce a predictably systematic reduction in the magnitude of antiferromagnetic coupling by switching off the dominant antiferromagnetic exchange pathways. In the case of weakly coupled dimers, this can even induce a reversal of the coupling from antiferromagnetic to ferromagnetic.

  9. Magnetochemistry of the tetrahaloferrate (III) ions. 7. Crystal structure and magnetic ordering in (pyridinium){sub 3}Fe{sub 2}Br{sub 9}

    Energy Technology Data Exchange (ETDEWEB)

    Lowe, C.B.; Shaviv, R.; Carlin, R.L. [Univ. of Illinois, Chicago, IL (United States)] [and others


    A monoclinic crystal structure was found by X-ray diffraction for bis [pyridinium tetrabromferrate(III)]-pyridinium bromide. The double salt contains two slightly distorted [FeBr{sub 4}]{sup -} tetrahedra, three pyridinium rings, and an uncoordinated halide in each asymmetric unit, as is characteristic of the A{sub 3}Fe{sub 2}X{sub 9} series of compounds. Unit cell parameters, monoclinic space group P2{sub 1}, are a = 7.656(3) {angstrom}, b = 14.237(5) {angstrom}, c = 13.725(5) {angstrom}, {beta} = 93.42(3){degrees}, and V = 1493(1) {angstrom}{sup 3}, using Mo K{alpha} radiation {lambda} = 0.710 69 {angstrom}, {rho}{sub calc} = 2.38 g cm{sup -3}, and Z = 2. The tetrahedra are aligned with their 3-fold axes parallel to the crystallographic c axis. Bond lengths (Fe-Br) range from 2.271(9) {angstrom} to 2.379(9) {angstrom} for the two different slightly distorted tetrahedral units. Magnetic susceptibility studies show that the material orders three-dimensionally at 7.4 {+-} 0.2 K. The data are compared to a HTS expansion of 1/{sub {chi}} for the S = 5/2 three-dimensional Heisenberg model antiferromagnet for a sc lattice with g = 1.98 and J/k{sub B} = -0.43 K. The specific heat measurements indicate two odd-shaped {lambda} features, at 7.3 and 8 K.

  10. Magnetochemistry of the tetrahaloferrate (III) ions: Crystal structure and magnetic ordering in [(4-chloropyridinium)FeCl4]2ṡ4-chloropyridinium chloride and related salts (abstract) (United States)

    Lowe, C. B.; Shum, D. P.; Carlin, Richard L.


    The yellow compound of stoichiometry (4-chloropyridinium)3Fe2Cl9 belongs to the space group P21/n with four formula units in the unit cell. Structural analysis shows that the iron is present as the FeX4- ion. Magnetic measurements on single crystals show that the material orders as a canted antiferromagnet at 2.725 K. Replacement of the 4-chloro cation by the 4-bromo analog yields an isomorphous material and shifts the transition temperature to 2.34 K. The phase diagrams of both salts have also been determined. For [(4-chloropyridinium)FeCl4]2ṡ4-chloropyridinium chloride, the bicritical point is at 2.40 K and 7 kOe, and HSF(0)=5.5 kOe. With Hc(0)=56 kOe, α=HA/HE=1.9×10-2. In the case of [(4-bromopyridinium)FeCl4]2ṡ4-bromopyridinium chloride, HSF(0)=3 kOe, Hc(0)=42 kOe, α=1.0×10-2, and the bicritical point is at 2.24 K and 4.2 kOe. Crystallographic investigations at 25 K are reported on the isomorphous (4-chloropyridinium)3Fe2Br9 and on (4-bromopyridinium)3Fe2Cl1.3Br7.7. Magnetic measurements on single crystals show that (4-bromopyridinium)3Fe2Cl1.3Br7.7 orders as a canted antiferromagnet at 5.67 K, while (4-chloropyridinium)3Fe2Br9 orders similarly at 7.96 K. These compounds behave approximately as S=5/2, three-dimensional Heisenberg antiferromagnets.

  11. Competing Magnetic Exchange Interactions in Tetranuclear d(1) Systems: Synthesis, Structure, and Magnetochemistry of a Neutral Vanadium(IV) Complex with a {(VO)(4)(&mgr;(3)-OR)(2)(&mgr;(2)-OR)(4)}(2+) Core. (United States)

    Plass, Winfried


    The complex [{VO(L)}(2){VO(acac)}(2)(&mgr;(2)-OMe)(2)] 1 can be synthesized by reaction of the Schiff base ligand N,N-bis(2-hydroxyethyl)-N'-(2-pyrrolylmethylidene)ethylenediamine (H(2)L) with [VO(acac)(2)] (Hacac = 2,4-pentanedione). The compound 1.MeOH has been characterized by IR, UV/vis, and ESR spectroscopy as well as magnetic susceptibility measurements. A single-crystal diffraction study performed on 1. MeOH gives the following crystal data: triclinic, P&onemacr;, a = 7.352(2) Å, b = 12.584(4) Å, c = 12.826(4) Å, alpha = 107.61(2) degrees, beta = 102.96(2) degrees, gamma = 95.25(2) degrees, Z = 1. The tetranuclear {(VO)(4)(&mgr;(3)-OR)(2)(&mgr;(2)-OR)(4)}(2+) core of 1 is composed of three different types of edge-shared binuclear units, an anti-coplanar, two syn-coplanar, and two twist configurations. Consistent with this connectivity pattern, analysis of the magnetic data reveals competing ferromagnetic and antiferromagnetic exchange interactions within the tetranuclear core structure. Both ESR and magnetic data indicate a singlet ground state for 1. In addition, the general magnetic behavior of oxovanadium(IV) clusters is discussed on the basis of classification schemes derived from simple binuclear fragmentation patterns. Consistent with the superexchange mechanism expected to be operative for binuclear oxovanadium(IV) units with syn-coplanar configuration, the corresponding magnetic exchange parameter J(sc) of 1 (V.V = 3.410(2) Å) is determined to be antiferromagnetic at -153 cm(-)(1).

  12. Heterobridged dinuclear, tetranuclear, dinuclear-based 1-d, and heptanuclear-based 1-D complexes of copper(II) derived from a dinucleating ligand: syntheses, structures, magnetochemistry, spectroscopy, and catecholase activity. (United States)

    Majumder, Samit; Sarkar, Sohini; Sasmal, Sujit; Sañudo, E Carolina; Mohanta, Sasankasekhar


    The work in this paper presents syntheses, characterization, crystal structures, variable-temperature/field magnetic properties, catecholase activity, and electrospray ionization mass spectroscopic (ESI-MS positive) study of five copper(II) complexes of composition [Cu(II)(2)L(μ(1,1)-NO(3))(H(2)O)(NO(3))](NO(3)) (1), [{Cu(II)(2)L(μ-OH)(H(2)O)}(μ-ClO(4))](n)(ClO(4))(n) (2), [{Cu(II)(2)L(NCS)(2)}(μ(1,3)-NCS)](n) (3), [{Cu(II)(2)L(μ(1,1)-N(3))(ClO(4))}(2)(μ(1,3)-N(3))(2)] (4), and [{Cu(II)(2)L(μ-OH)}{Cu(II)(2)L(μ(1,1)-N(3))}{Cu(II)(μ(1,1)-N(3))(4)(dmf)}{Cu(II)(2)(μ(1,1)-N(3))(2)(N(3))(4)}](n)·ndmf (5), derived from a new compartmental ligand 2,6-bis[N-(2-pyridylethyl)formidoyl]-4-ethylphenol, which is the 1:2 condensation product of 4-ethyl-2,6-diformylphenol and 2-(2-aminoethyl)pyridine. The title compounds are either of the following nuclearities/topologies: dinuclear (1), dinuclear-based one-dimensional (2 and 3), tetranuclear (4), and heptanuclear-based one-dimensional (5). The bridging moieties in 1-5 are as follows: μ-phenoxo-μ(1,1)-nitrate (1), μ-phenoxo-μ-hydroxo and μ-perchlorate (2), μ-phenoxo and μ(1,3)-thiocyanate (3), μ-phenoxo-μ(1,1)-azide and μ(1,3)-azide (4), μ-phenoxo-μ-hydroxo, μ-phenoxo-μ(1,1)-azide, and μ(1,1)-azide (5). All the five compounds exhibit overall antiferromagnetic interaction. The J values in 1-4 have been determined (-135 cm(-1) for 1, -298 cm(-1) for 2, -105 cm(-1) for 3, -119.5 cm(-1) for 4). The pairwise interactions in 5 have been evaluated qualitatively to result in S(T) = 3/2 spin ground state, which has been verified by magnetization experiment. Utilizing 3,5-di-tert-butyl catechol (3,5-DTBCH(2)) as the substrate, catecholase activity of all the five complexes have been checked. While 1 and 3 are inactive, complexes 2, 4, and 5 show catecholase activity with turn over numbers 39 h(-1) (for 2), 40 h(-1) (for 4), and 48 h(-1) (for 5) in dmf and 167 h(-1) (for 2) and 215 h(-1) (for 4) in acetonitrile

  13. Structures, magnetochemistry, spectroscopy, theoretical study, and catechol oxidase activity of dinuclear and dimer-of-dinuclear mixed-valence Mn(III)Mn(II) complexes derived from a macrocyclic ligand. (United States)

    Jana, Arpita; Aliaga-Alcalde, Núria; Ruiz, Eliseo; Mohanta, Sasankasekhar


    The work in this paper presents syntheses, characterization, magnetic properties (experimental and density functional theoretical), catecholase activity, and electrospray ionization mass spectroscopic (ESI-MS positive) studies of two mixed-valence dinuclear Mn(III)Mn(II) complexes, [Mn(III)Mn(II)L(μ-O2CMe)(H2O)2](ClO4)2·H2O·MeCN (1) and [Mn(III)Mn(II)L(μ-O2CPh)(MeOH)(ClO4)](ClO4) (2), and a Mn(III)Mn(II)Mn(II)Mn(III) complex, [{Mn(III)Mn(II)L(μ-O2CEt)(EtOH)}2(μ-O2CEt)](ClO4)3 (3), derived from the Robson-type macrocycle H2L, which is the [2 + 2] condensation product of 2,6-diformyl-4-methylphenol and 2,2-dimethyl-1,3-diaminopropane. In 1 and 2 and in two Mn(III)Mn(II) units in 3, the two metal centers are bridged by a bis(μ-phenoxo)-μ-carboxylate moiety. The two Mn(II) centers of the two Mn(III)Mn(II) units in 3 are bridged by a propionate moiety, and therefore this compound is a dimer of two dinuclear units. The coordination geometry of the Mn(III) and Mn(II) centers are Jahn-Teller distorted octahedral and distorted trigonal prism, respectively. Magnetic studies reveal weak ferro- or antiferromagnetic interactions between the Mn(III) and Mn(II) centers in 1 (J = +0.08 cm(-1)), 2 (J = -0.095 cm(-1)), and 3 (J1 = +0.015 cm(-1)). A weak antiferromagnetic interaction (J2 = -0.20 cm(-1)) also exists between the Mn(II) centers in 3. DFT methods properly reproduce the nature of the exchange interactions present in such systems. A magneto-structural correlation based on Mn-O bridging distances has been proposed to explain the different sign of the exchange coupling constants. Utilizing 3,5-di-tert-butyl catechol (3,5-DTBCH2) as the substrate, catecholase activity of all the three complexes has been checked in MeCN and MeOH, revealing that all three are active catalysts with Kcat values lying in the range 7.5-64.7 h(-1). Electrospray ionization mass (ESI-MS positive) spectra of the complexes 1-3 have been recorded in MeCN solutions, and the positive ions have been

  14. Crystal and molecular structure and magnetic exchange properties of bis(di-micro-ethoxo-bis(3,5-di-tert-butylsemiquinonato)dicopper(II)) complex. A synergy between DFT and experimental magnetochemistry. (United States)

    Bencini, Alessandro; Dei, Andrea; Sangregorio, Claudio; Totti, Federico; Vaz, Maria G F


    The compound bis(di-micro-ethoxo-bis(3,5-di-tert-butylsemiquinonato)dicopper(II)) has been synthesized and its structure was determined by single-crystal X-ray diffraction. The compound crystallizes in the monoclinic system, space group C2/c, with a = 37.736(8) A, b = 9.173(2) A, c = 23.270(5) A, beta = 122.24(3) degrees. The structure can be described as a Lewis adduct between two dinuclear [Cu(DBSQ)(C(2)H(5)O)](2) units (DBSQ = 3,5-di-tert-butyl-semiquinonato). The temperature dependence of the magnetic susceptibility was efficiently analyzed by a combined DFT/experimental approach, showing that a rather strong ferromagnetic interaction exists between the DBSQ(-) and the copper(II) ions modulated by an antiferromagnetic interaction between the two copper(II) ions of the dinuclear units. Weak antiferromagnetism between the two units in the unit cell was measured.

  15. Characterization of Injection Molded Structures

    DEFF Research Database (Denmark)

    Sun, Ling; Søgaard, Emil; Andersen, Nis Korsgaard

    and limitations. Therefore, it would be difficult to characterize complex, especially hierarchical structures by using only one method. Here we present a combined optical microscopy, scanning electron microscopy (SEM), and scanning probe microscopy study on injection molded structures. These structures are used......-properties relationship of the injection molded polymer samples. These results are very important in optimizing injection molding parameters....

  16. Characterization of DPOAE fine structure

    DEFF Research Database (Denmark)

    Reuter, Karen; Hammershøi, Dorte


    The distortion product otoacoustic emission (DPOAE) fine structure is revealed, when measuring DPOAE with a very fine frequency resolution. It is characterized by consistent maxima and minima with notches of up to 20 dB depth. The fine structure is known also from absolute hearing thresholds...

  17. Transition metal complexes with thiosemicarbazide-based ligands. Part 60. Reactions of copper(II bromide with pyridoxal S-methylisothiosemicarbazone (PLITSC. Crystal structure of [Cu(PLITSC−HH2O]Br•H2O

    Directory of Open Access Journals (Sweden)

    Leovac Vukadin M.


    Full Text Available The synthesis and structural characterization of a square-planar copper(II complex with pyridoxal S-methylisothiosemicarbazone (PLITSC of the formula [Cu(PLITSC−HH2O]Br•H2O (1 as the first Cu(II complex with monoanionic form of this ligand were described. Complex 1 together with two previously synthesized complexes [Cu(PLITSCBr2] (2 and [Cu(PLITSCBr(MeOH]Br (3 were characterized by elemental analysis, IR and electronic spectra and also by the methods of thermal analysis, conductometry and magnetochemistry. [Projekat Pokrajisnkog sekretarijata za nauku i tehnoloski razvoj Vojvodine i Ministarstva nauke Republike Srbije, br. 172014

  18. Structural characterization of electrodeposited boron

    Indian Academy of Sciences (India)

    Structural characterization of electrodeposited boron was carried out by using transmission electron microscopy and Raman spectroscopy. Electron diffraction and phase contrast imaging were carried out by using transmission electron microscopy. Phase identification was done based on the analysis of electron diffraction ...


    African Journals Online (AJOL)


    *Corresponding author. E-mail: CHEMICAL AND STRUCTURAL CHARACTERIZATION OF NATURAL. PHOSPHATE OF HAHOTOE (TOGO). Gado Tchangbeddji1*, Gnande Djeteli1, Koffi Ani Kili1, Jean Michel Savariault2 and. Jean Louis Lacout3. 1Laboratoire de Physico-Chimie des Matériaux, ...

  20. Structural characterization of electrodeposited boron

    Indian Academy of Sciences (India)

    Abstract. Structural characterization of electrodeposited boron was carried out by using transmission electron microscopy and Raman spectroscopy. Electron diffraction and phase contrast imaging were carried out by using transmission electron microscopy. Phase identification was done based on the analysis of electron ...

  1. Applications of magnetochemistry to the characterization of calcium-nickel-potassium oxide catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Perry, D.L.; Berdahl, P.H.; Perrino, C. [Lawrence Berkely Laboratory, CA (United States)


    Magnetochemical studies, using SQUID magnetometry, have been conducted on calcium-nickel-potassium oxide phases that have been shown to be active in the catalyzed gasification of carbonaceous materials. The research has focused on the chemical state of the paramagnetic nickel(II) oxide system and the paramagnetic oxygen binary compounds with potassium. Studies were performed on various samples of the quaternary metal oxide system that has been synthesized by a variety of routes, including dehydration of hydroxides, thermal decomposition of the parent metal salts (such as nitrates), and the calcining of their parent metal oxides. The magetochemistry is discussed in relationship to the different particles sizes of NiO{sub 3}, the temperature and periods of time of annealing the oxide system, and the synthetic routes used to prepare the compounds. Data are compared to those obtained for the compounds using x-ray photoelectron spectroscopy.

  2. Magnetochemistry of the tetrahaloferrate(III) ions. 2. Crystal structure and magnetic ordering in (4-Br(py)H) sub 3 Fe sub 2 Cl sub 1. 3 Br sub 7. 7 and (4-Cl(py)H) sub 3 Fe sub 2 Br sub 9. The superexchange paths in the A sub 3 Fe sub 2 X sub 9 salts

    Energy Technology Data Exchange (ETDEWEB)

    Lowe, C.B.; Carlin, R.L.; Schultz, A.J.; Loong, C.K. (Univ. of Illinois, Chicago (USA) Argonne National Lab., IL (USA))


    A series of neutron diffraction investigations at 25 K are reported on single crystals of stoichiometry (4-chloropyridinium){sub 3}Fe{sub 2}Br{sub 9} and on (4-bromopyridinium){sub 3}Fe{sub 2}Cl{sub 1.3}Br{sub 7.7}. The compound of stoichiometry (4-bromopyridinium){sub 3}Fe{sub 2}Cl{sub 1.3}Br{sub 7.7} is found to belong to the space group P2{sub 1}/n with four formula units in the unit cell, and the related compound (4-chloropyridinium){sub 3}Fe{sub 2}Bn{sub 9} was found to belong to the same space groups. Structural analysis shows that the iron is present as the (FeX{sub 4}){sup {minus}} ion (X = Cl, Br). The results of the determination of the crystal structure of the compounds are reported. Both materials are isomorphous with the previously reported bis(4-chloropyridinium tetrachloroferrate(III))-4-chloropyridinium chloride. Magnetic measurements on single crystals show that the S = 5/2 material (4-bromopyridinium){sub 3}Fe{sub 2}Cl{sub 1.3}Br{sub 7.7} orders as a canted antiferromagnet at 5.67 K, while (4-chloropyridinium){sub 3}Fe{sub 2}Br{sub 9} orders in a similar fashion at 7.96 K. Magnetic susceptibility data are compared with the theoretical predictions for the simple cubic (sc) Heisenberg high-temperature series expansion model, and superexchange pathways for the isostructural series of monoclinic A{sub 3}Fe{sub 2}X{sub 9} salts are examined. 19 refs., 6 figs., 6 tabs.


    monocarboxylic acids and organosulfur compounds; solid state mass spectrometric studies; and the characterization of polyurethane elastomers with special reference to those used as binders for solid propellants.


    African Journals Online (AJOL)

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    The Mo atom in the complex is in octahedral coordination. Thermal stability of the complex has also been studied. KEY WORDS: Molybdenum complex, Hydrazone ligand, Crystal structure, X-ray diffraction, Thermal property. INTRODUCTION. Coordination chemistry of molybdenum(VI) has attracted considerable attention ...

  5. Synthesis, spectroscopic and structural characterization of new ...

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 125; Issue 3. Synthesis, spectroscopic and structural characterization of new linear mononuclear silver(I) complexes containing -keto phosphorus ylides as ambidentate ligands. Seyed Javad Sabounchei Mohsen Ahmadi Fatemeh Akhlaghi Hamid Reza Khavasi.

  6. Characterizing Asteroid Internal Structure Through Tectonic Analyses (United States)

    Wyrick, D. Y.; Buczkowski, D. L.; Durda, D. D.


    Critical data gaps remain in characterizing the mechanical strength and internal structure of asteroids. Understanding asteroid internal coherency is required to develop effective mitigation, diversion, or destruction strategies against impact threat.

  7. On characterization of anisotropic plant protein structures

    NARCIS (Netherlands)

    Krintiras, G.A.; Göbel, J.; Bouwman, W.G.; Goot, van der A.J.; Stefanidis, G.D.


    In this paper, a set of complementary techniques was used to characterize surface and bulk structures of an anisotropic Soy Protein Isolate (SPI)–vital wheat gluten blend after it was subjected to heat and simple shear flow in a Couette Cell. The structured biopolymer blend can form a basis for a

  8. Fabrication and characterization of woodpile structures

    DEFF Research Database (Denmark)

    Zalkovskij, Maksim; Malureanu, Radu; Andryieuski, Andrei


    In this paper we present the whole fabrication and characterization cycle for obtaining 3D metal-dielectric woodpile structures. The optical properties of these structures have been measured using different setups showing the need of considering e.g. border effects when planning their use in real...

  9. Health Monitoring for Airframe Structural Characterization (United States)

    Munns, Thomas E.; Kent, Renee M.; Bartolini, Antony; Gause, Charles B.; Borinski, Jason W.; Dietz, Jason; Elster, Jennifer L.; Boyd, Clark; Vicari, Larry; Ray, Asok; hide


    This study established requirements for structural health monitoring systems, identified and characterized a prototype structural sensor system, developed sensor interpretation algorithms, and demonstrated the sensor systems on operationally realistic test articles. Fiber-optic corrosion sensors (i.e., moisture and metal ion sensors) and low-cycle fatigue sensors (i.e., strain and acoustic emission sensors) were evaluated to validate their suitability for monitoring aging degradation; characterize the sensor performance in aircraft environments; and demonstrate placement processes and multiplexing schemes. In addition, a unique micromachined multimeasure and sensor concept was developed and demonstrated. The results show that structural degradation of aircraft materials could be effectively detected and characterized using available and emerging sensors. A key component of the structural health monitoring capability is the ability to interpret the information provided by sensor system in order to characterize the structural condition. Novel deterministic and stochastic fatigue damage development and growth models were developed for this program. These models enable real time characterization and assessment of structural fatigue damage.

  10. Advanced Structural Characterization of Organic Thin Films

    DEFF Research Database (Denmark)

    Gu, Yun

    In this thesis, the structural characterizations of three organic film systems are described. Several X-ray based techniques have been utilized for the characterizations for different research goals. The structures of N,N',N-trioctyltriazatriangulenium (Oct3-TATA+) salts have been investigated...... of small molecule and polymer layers is indicated by Flory- Huggins theory for the triisopropylsilylethynl pentacene (TIPS-PEN) and polystyrene blend films. In order to investigate the phase separated layers in the ink-jet printed films, we propose a method to measure diraction Bragg peaks by X...

  11. Vortex structure and characterization of quasiperiodic functions

    CERN Document Server

    Dana, I


    Quasiperiodic functions (QPFs) are characterized by their full vortex structure in one unit cell. This characterization is much finer and more sensitive than the topological one given by the total vorticity per unit cell (the 'Chern index'). It is shown that QPFs with an arbitrarily prescribed vortex structure exist by constructing explicitly such a 'standard' QPF. Two QPFs with the same vortex structure are equivalent, in the sense that their ratio is a function which is strictly periodic, nonvanishing and at least continuous. A general QPF can then be approximately reconstructed from its vortex structure on the basis of the standard QPF and the equivalence concept. As another application of this concept, a simple method is proposed for calculating the quasiperiodic eigenvectors of periodic matrices. Possible applications to the quantum-chaos problem on a phase-space torus are briefly discussed.

  12. Preparation, Structure Characterization and Thermal Decomposition ...

    African Journals Online (AJOL)

    The complex was structurally characterized by single crystal X-ray diffraction, elemental analysis,UVand IR spectroscopy, molar conductance and TG-DTG techniques. ... Each Dy(III) ion is eight-coordinated to one 1,10-phenanthroline molecule, one bidentate carboxylate group and four bridging carboxylate groups.

  13. Synthesis, structural characterization and biological activities of ...

    Indian Academy of Sciences (India)

    The School of Chemical Sciences, Universiti Sains Malaysia, 11800 USM, Penang, Malaysia e-mail:; ... complexes have been characterized by elemental analyses, UV-Vis, FT-IR, 1H, 13C and 119Sn NMR spectral studies. The molecular structure of complex 5 has been confirmed ...

  14. Structural characterization of proteins using residue environments. (United States)

    Mooney, Sean D; Liang, Mike Hsin-Ping; DeConde, Rob; Altman, Russ B


    A primary challenge for structural genomics is the automated functional characterization of protein structures. We have developed a sequence-independent method called S-BLEST (Structure-Based Local Environment Search Tool) for the annotation of previously uncharacterized protein structures. S-BLEST encodes the local environment of an amino acid as a vector of structural property values. It has been applied to all amino acids in a nonredundant database of protein structures to generate a searchable structural resource. Given a query amino acid from an experimentally determined or modeled structure, S-BLEST quickly identifies similar amino acid environments using a K-nearest neighbor search. In addition, the method gives an estimation of the statistical significance of each result. We validated S-BLEST on X-ray crystal structures from the ASTRAL 40 nonredundant dataset. We then applied it to 86 crystallographically determined proteins in the protein data bank (PDB) with unknown function and with no significant sequence neighbors in the PDB. S-BLEST was able to associate 20 proteins with at least one local structural neighbor and identify the amino acid environments that are most similar between those neighbors. Proteins 2005. 2005 Wiley-Liss, Inc.

  15. Instrumentation for the Characterization of Inflatable Structures (United States)

    Swanson, Gregory T.; Cassell, Alan M.; Johnson, R. Keith


    Current entry, descent, and landing technologies are not practical for heavy payloads due to mass and volume constraints dictated by limitations imposed by launch vehicle fairings. Therefore, new technologies are now being explored to provide a mass- and volume-efficient solution for heavy payload capabilities, including Inflatable Aerodynamic Decelerators (IAD) [1]. Consideration of IADs for space applications has prompted the development of instrumentation systems for integration with flexible structures to characterize system response to flight-like environment testing. This development opportunity faces many challenges specific to inflatable structures in extreme environments, including but not limited to physical flexibility, packaging, temperature, structural integration and data acquisition [2]. In the spring of 2012, two large scale Hypersonic Inflatable Aerodynamic Decelerators (HIAD) will be tested in the National Full-Scale Aerodynamics Complex s 40 by 80 wind tunnel at NASA Ames Research Center. The test series will characterize the performance of a 3.0 m and 6.0 m HIAD at various angles of attack and levels of inflation during flight-like loading. To analyze the performance of these inflatable test articles as they undergo aerodynamic loading, many instrumentation systems have been researched and developed. These systems will utilize new experimental sensing systems developed by the HIAD ground test campaign instrumentation team, in addition to traditional wind tunnel sensing techniques in an effort to improve test article characterization and model validation. During the 2012 test series the instrumentation systems will target inflatable aeroshell static and dynamic deformation, structural strap loading, surface pressure distribution, localized skin deflection, and torus inflation pressure. This paper will offer an overview of inflatable structure instrumentation, and provide detail into the design and implementation of the sensors systems that will

  16. Synthesis, structural characterization and thermal properties of a new copper(II) one-dimensional coordination polymer based on bridging N,N'-bis(2-hydroxybenzylidene)-2,2-dimethylpropane-1,3-diamine and dicyanamide ligands. (United States)

    Hopa, Cigdem; Cokay, Ismail


    The design and synthesis of polymeric coordination compounds of 3d transition metals are of great interest in the search for functional materials. The coordination chemistry of the copper(II) ion is of interest currently due to potential applications in the areas of molecular biology and magnetochemistry. A novel coordination polymer of Cu(II) with bridging N,N'-bis(2-hydroxyphenyl)-2,2-dimethylpropane-1,3-diamine (H2L-DM) and dicyanamide (dca) ligands, catena-poly[[[μ2-2,2-dimethyl-N,N'-bis(2-oxidobenzylidene)propane-1,3-diamine-1:2κ(6)O,N,N',O':O,O']dicopper(II)]-di-μ-dicyanamido-1:2'κ(2)N(1):N(5);2:1'κ(2)N(1):N(5)], [Cu2(C19H20N2O2)(C2N3)2]n, has been synthesized and characterized by CHN elemental analysis, IR spectroscopy, thermal analysis and X-ray single-crystal diffraction analysis. Structural studies show that the Cu(II) centres in the dimeric asymmetric unit adopt distorted square-pyramidal geometries, as confirmed by the Addison parameter (τ) values. The chelating characteristics of the L-DM(2-) ligand results in the formation of a Cu(II) dimer with a double phenolate bridge in the asymmetric unit. In the crystal, the dimeric units are further linked to adjacent dimeric units through μ1,5-dca bridges to produce one-dimensional polymeric chains.

  17. Structural Characterization of supramolecule/nanoparticle nanocomposites (United States)

    Xiao, Yihan; Xu, Ting

    Supramolecular nanocomposites offer great opportunities toward functional materials. However, these systems also challenge our basic understanding in self-assembly in multiple component systems. The multicomponent nature of the supramolecular system introduces significant complexity in mapping out the hierarchical spatial distribution of each building block. To this end, various techniques have been adopted to decouple the convoluted structures. Transmission electron microscopy (TEM), scanning transmission electron microscopy tomography (STEMT) and small-angle X-ray scattering (SAXS) collaboratively determined the hexagonal structure of nanoparticle superlattice. Resonant X-ray scattering (RSoXS) provides a novel opportunity to selectively characterize the lamellar arrangement of supramolecular matrix. Finally, a model is proposed for the nanocomposite morphology based on these results that is critical toward delineation of energetic contribution from individual component. The work was supported by the U.S. Department of Energy, Office of Science, Materials Sciences and Engineering Division.

  18. Structure and bonding in three-coordinate N-heterocyclic carbene adducts of iron(II) bis(trimethylsilyl)amide. (United States)

    Layfield, Richard A; McDouall, Joseph J W; Scheer, Manfred; Schwarzmaier, Christoph; Tuna, Floriana


    The molecular structures, chemical bonding and magnetochemistry of the three-coordinate iron(II) NHC complexes [(NHC)Fe{N(SiMe(3))(2)}(2)] (NHC = IPr, 2; NHC = IMes, 3) are reported. This journal is © The Royal Society of Chemistry 2011

  19. Structural characterization of MAPLE deposited lipase biofilm

    Energy Technology Data Exchange (ETDEWEB)

    Aronne, Antonio [Department of Chemical Engineering, Materials and Industrial Production, Università degli Studi di Napoli Federico II, Piazzale V. Tecchio 80, 80125 Napoli (Italy); Ausanio, Giovanni; Bloisi, Francesco [CNR-SPIN and Department of Physics, Università degli Studi di Napoli Federico II, Piazzale V. Tecchio 80, 80125 Napoli (Italy); Calabria, Raffaela [Istituto Motori-CNR, via G. Marconi 8, 80125 Napoli (Italy); Califano, Valeria, E-mail: [Istituto Motori-CNR, via G. Marconi 8, 80125 Napoli (Italy); Fanelli, Esther [Department of Chemical Engineering, Materials and Industrial Production, Università degli Studi di Napoli Federico II, Piazzale V. Tecchio 80, 80125 Napoli (Italy); Massoli, Patrizio [Istituto Motori-CNR, via G. Marconi 8, 80125 Napoli (Italy); Vicari, Luciano R.M. [CNR-SPIN and Department of Physics, Università degli Studi di Napoli Federico II, Piazzale V. Tecchio 80, 80125 Napoli (Italy)


    Highlights: • Lipase from Candida Rugosa was deposited by Matrix Assisted Pulsed Laser Evaporation (MAPLE) on KBr pellets, mica and glass substrate. • The deposited film was characterized morphologically and structurally by optical microscopy, SEM and FTIR analysis. • Results of characterization underlined a phenomenon of aggregation taking place. • The aggregation phenomenon was reversible since lipase showed activity in the transesterification reaction between soybean oil and isopropyl alcohol once detached from the substrate. - Abstract: Lipases (triacylglycerol ester hydrolases) are enzymes used in several industrial applications. Enzymes immobilization can be used to address key issues limiting widespread application at industrial level. Immobilization efficiency is related to the ability to preserve the native conformation of the enzyme. MAPLE (Matrix Assisted Pulsed Laser Evaporation) technique, a laser deposition procedure for treating organic/polymeric/biomaterials, was applied for the deposition of lipase enzyme in an ice matrix, using near infrared laser radiation. Microscopy analysis showed that the deposition occurred in micrometric and submicrometric clusters with a wide size distribution. AFM imaging showed that inter-cluster regions are uniformly covered with smaller aggregates of nanometric size. Fourier transform infrared spectroscopy was used for both recognizing the deposited material and analyzing its secondary structure. Results showed that the protein underwent reversible self-association during the deposition process. Actually, preliminary tests of MAPLE deposited lipase used for soybean oil transesterification with isopropyl alcohol followed by gas chromatography–mass spectrometry gave results consistent with undamaged deposition of lipase.

  20. The magnetochemistry of supramolecular particles: The transition from the molecular to the solid-state (United States)

    Papaefthymiou, Georgia C.


    The magnetic properties of nanometer-sized molecular complexes or clusters that contain an increasing number n of superexchange-coupled iron ions participating in 3-D or lower-dimensional magnetic interactions were examined. The experimental criteria that establish the onset of incipient solid-state magnetic correlation effects in these molecules were emphasized. These chemical structures are beyond the molecular realm but convergence to the bulk has not yet been attained. Thus, they afforded appropriate experimental systems to test theoretical predictions that the onset of incipient solid-state phenomena - such as the emergence of a conduction band in metallic clusters and collective magnetic interactions responsible for magnetic ordering in solids - occurs at the vicinity of n greater than 10, where n is the number of atoms or interacting spins in the cluster. The study provided, by means of Mossbauer spectroscopy with a characteristic measuring time tau(sub m) approx. 10(exp -8) sec the first experimental observation of the onset of intramolecular magnetic ordering in 10 A diameter clusters whose magnetic exchange interaction network among iron ions was three-dimensional. Owing to the extremely small size of the magnetic domain transitional magnetic behavior and superparamagnetic relaxation phenomena dominated the Mossbauer spectra.

  1. Structural Characterization of Chitosan-Clay Nanocomposite (United States)

    Paluszkiewicz, C.; Weselucha-Birczynska, A.; Stodolak, E.


    Novel materials originating from renowable sources mainly consist of biopolymers and their composites or nanocomposites. A typical material belonging to this group is chitosane (CS), which is a cationic natural polysaccharide that can be produced by alkaline N-deacetylation of chitine. Chitosane has a variety of applications in biomedical products, cosmetics, and food processing [1, 2].Organic-inorganic hybrid materials basing on chitosane and nanoclay (montmoryllonite, MMT) were characterized by the vibrational spectrocopy methods (Micro-Raman spectroscopy and FT-Raman spectroscopy) and the thermal analysis methods (TG, DSC). It was shown, that small amount on a nanofiller (MMT, 3 wt.%) used to modify the polymer matrix influences the structure of its polymeric chains.

  2. Structural Characterization of Bimetallic Nanocrystal Electrocatalysts

    Energy Technology Data Exchange (ETDEWEB)

    Cullen, David A [ORNL


    Late transition metal nanocrystals find applications in heterogeneous catalysis such as plasmon-enhanced catalysis and as electrode materials for fuel cells, a zero-emission and sustainable energy technology. Their commercial viability for automotive transportation has steadily increased in recent years, almost exclusively due to the discovery of more efficient bimetallic nanocatalysts for the oxygen reduction reaction (ORR) at the cathode. Despite improvements to catalyst design, achieving high activity while maintaining durability is essential to further enhance their performance for this and other important applications in catalysis. Electronic effects arising from the generation of metal-metal interfaces, from plasmonic metals, and from lattice distortions, can vastly improve sorption properties at catalytic surfaces, while increasing durability.[1] Multimetallic lattice-strained nanoparticles are thus an interesting opportunity for fundamental research.[2,3] A colloidal synthesis approach is demonstrated to produce AuPd alloy and Pd@Au core-shell nanoicosahedra as catalysts for electro-oxidations. The nanoparticles are characterized using aberration-corrected scanning transmission electron microscopy (ac-STEM) and large solid angle energy dispersive X-ray spectroscopy (EDS) on an FEI Talos 4-detector STEM/EDS system. Figure 1 shows bright-field (BF) and high-angle annular dark-field (HAADF) ac-STEM images of the alloy and core-shell nanoicosahedra together with EDS line-scans and elemental maps. These structures are unique in that the presence of twin boundaries, alloying, and core-shell morphology could create highly strained surfaces and interfaces. The shell thickness of the core-shell structures observed in HAADF-STEM images is tuned by adjusting the ratio between metal precursors (Figure 2a-f) to produce shells ranging from a few to several monolayers. Specific activity was measured in ethanol electro-oxidation to examine the effect of shell thickness on

  3. Structural characterization of SiC nanoparticles (United States)

    Sun, Baoxing; Xie, Ruobing; Yu, Cun; Li, Cheng; Xu, Hongjie


    The structure and size of SiC nanoparticles were studied by different characterization methods including small angle X-ray scattering (SAXS), transmission electron microscope (TEM), and X-ray diffraction (XRD). The results showed that particle size distributions determined respectively from SAXS and TEM are comparable and follow the log-normal function. The size distribution of the particles is between 10 to 100 nm with most of them being in the range of 20–50 nm. The average particle size is around 42 nm. XRD identifies the phase of the SiC nanoparticles and suggests the average size of the single crystalline domain to be around 21 nm. The combined results from XRD and SAXS suggest the existence of many polycrystals, which is confirmed by the HRTEM observation of particles with twins and stacking faults. The material synthesis methods leading to various particle sizes are also discussed. Project supported by the National Natural Science Foundation of China (No. 11505273) and the Strategic Priority Research Program of the Chinese Academy of Sciences (No. XDA02000000).

  4. Characterization of Forest Structure and an Assessment of Litter ...

    African Journals Online (AJOL)

    Characterization of Forest Structure and an Assessment of Litter Production, Accumulation and Litter-asscociated Invertebrates in Two Naturally Occuring Rhizophora mucronata Stands in Mauritius (Indian Ocean)

  5. Structural characterization of copolymer embedded magnetic nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Nedelcu, G.G., E-mail: [Faculty of Physics, University “Alexandru Ioan Cuza”, Carol I Bulevard, Nr.11, 700506 Iasi (Romania); Nastro, A.; Filippelli, L. [Department of Chemistry and Chemical Technology, University of Calabria, Via P. Bucci, 87036 Arcavacata di Rende, Cosenza (Italy); Cazacu, M.; Iacob, M. [Institute of Macromolecular Chemistry “Petru Poni”, Aleea Grigore Ghica Voda, nr. 41A, 700487 Iasi (Romania); Rossi, C. Oliviero [Department of Chemistry and Chemical Technology, University of Calabria, Via P. Bucci, 87036 Arcavacata di Rende, Cosenza (Italy); Popa, A.; Toloman, D. [National Institute for Research and Development of Isotopic and Molecular Technologies, 65-103 Donath Str., 400293 Cluj-Napoca 5 (Romania); Dobromir, M.; Iacomi, F. [Faculty of Physics, University “Alexandru Ioan Cuza”, Carol I Bulevard, Nr.11, 700506 Iasi (Romania)


    Highlights: • The emulsion polymerization method was used to synthesize three samples of poly(methyl methacrylate-co-acrylic acid) coated magnetite obtained before through co-precipitation technique. • Poly(methyl methacrylate-co-acrylic acid) coated magnetite nanoparticles were prepared having spherical shape and dimensions between 13 and 16 nm without agglomerations. • Fourier transform infrared spectra have found that the magnetite was pure and spectral characteristics of PMMA-co-AAc were present. • The electron spin resonance spectra revealed that interactions between nanoparticles are very weak due to the fact that the nanoparticles have been individually embedded in polymer. • The resonance field values as function of temperature demonstrate that the presence of polymer has not modified essentially its magnetic properties, except that at temperatures below 140 K there was a change due to decreasing of the magnetic anisotropy. - Abstract: Small magnetic nanoparticles (Fe{sub 3}O{sub 4}) were synthesized by co-precipitation and coated by emulsion polymerization with poly(methyl methacrylate-co-acrylic acid) (PMMA-co-AAc) to create surface functional groups that can attach drug molecules and other biomolecules. The coated and uncoated magnetite nanoparticles were stored for two years in normal closed ships and than characterized by Fourier transform infrared spectroscopy, X-ray diffraction, transmission electron microscopy, vibrating sample magnetometry, and electron paramagnetic resonance spectroscopy. The solid phase transformation of magnetite to maghemite, as well as an increase in particle size were evidenced for the uncoated nanoparticles. The coated nanoparticles preserved their magnetite structure and magnetic properties. The influences of monomers and surfactant layers on interactions between the magnetic nanoparticles evidenced that the thickness of the polymer has a significant effect on magnetic properties.

  6. Structure-based characterization of multiprotein complexes. (United States)

    Wiederstein, Markus; Gruber, Markus; Frank, Karl; Melo, Francisco; Sippl, Manfred J


    Multiprotein complexes govern virtually all cellular processes. Their 3D structures provide important clues to their biological roles, especially through structural correlations among protein molecules and complexes. The detection of such correlations generally requires comprehensive searches in databases of known protein structures by means of appropriate structure-matching techniques. Here, we present a high-speed structure search engine capable of instantly matching large protein oligomers against the complete and up-to-date database of biologically functional assemblies of protein molecules. We use this tool to reveal unseen structural correlations on the level of protein quaternary structure and demonstrate its general usefulness for efficiently exploring complex structural relationships among known protein assemblies. Copyright © 2014 The Authors. Published by Elsevier Inc. All rights reserved.

  7. Structural characterization of human Uch37

    Energy Technology Data Exchange (ETDEWEB)

    Burgie, E. Sethe; Bingman, Craig A.; Soni, Ameet B.; Phillips, Jr., George N. (UW)


    Uch37 is a deubiquitylating enzyme (DUB) that is functionally linked with multiple protein complexes and signal transduction pathways. Uch37 associates with the 26S proteasome through Rpn13 where it serves to remove distal ubiquitin moeities from polyubiquitylated proteins. Uch37's proteasome associated activity was shown to liberate proteins from destruction. However, Uch37 may also specifically facilitate the destruction of inducible nitric oxide synthase and I{kappa}B-{alpha} at the proteasome. Wicks et al. established Uch37's potential to modulate the transforming growth factor-{beta}(TGF-{beta}) signaling cascade, through tis interaction with SMAD7. Yao et al. demonstrated that Uch37 also associates with the Ino80 chromatin-remodeling complex (Ino80 complex), which is involved in DNA repair and transcriptional regulation. Uch37's importance in metazoan development was underscored recently as Uch37 knockouts in mice result in prenatal lethality, where mutant embryos had severe defects in brain development. Protein ubiquitylation is an ATP-dependent post-translational modification that serves to signal a wide variety of cellular processes in eukaryotes. A protein cascade, generally comprising three enzymes, functions to activate, transport and specifically transfer ubiquitin to the targeted protein, culminating in an isopeptide linkage between the {epsilon}-amino group of a target protein's lysysl residue and the ubiquitin's terminal carboxylate. Monoubiquitination plays an important role in histone regulation, endocytosis, and viral budding. Further processing of the target protein may be accomplished by ubiquitylation of the protein on a different lysine, or through the formation of polyubiquitin chains, where the best-characterized outcome is destruction of the polyubiquitin-labeled protein in the proteasome. DUBs catalyze the removal of ubiquitin from proteins. This activity serves to reverse the effects of ubiquitination, permit

  8. Magnetochemistry of Model Complexes for the Water Oxidation Center of Photosystem II and High Nuclearity Manganese Complexes. (United States)

    Tsai, Hui-Lien


    Several polynuclear oxo-bridged manganese compounds have been synthesized, and their structural, magnetic, and spectroscopic properties have been characterized. The tetranuclear complexes have been investigated as models of the manganese cluster in the water oxidation center of photosystem II. As the nuclearity increases, manganese complexes are no longer good model complexes. However, they exhibit interesting magnetic properties. Some have high spin ground states as a result of the spin frustration mechanism, or they show some quite unusual properties, such as relaxation behavior shown in superparamagnetic materials. The work described in this thesis focuses on characterizing the electronic structure of polynuclear manganese complexes that have from three to twelve manganese atoms. Of the complexes synthesized, (Mn_3 O(O_2C_2Cl _3)(HO_2CMe) _2(H_2O)) crystallizes in triclinic space group P1 and possesses asymmetric Mn_3 units and is a valence trapped Mn^{II}Mn^ {III}_2 complex. Variable temperature magnetic susceptibility studies have been performed for four trinuclear Mn complexes. The ground state is calculated to have S = 3/2 or S = 1/2 for rm Mn^ {II}Mn^{III}_2 complexes. The Mn^{III} _3 complexes have S = 0 ground state. By changing the ratio of the exchange interaction constant in a Mn_3O complex, it is possible to stabilize ground states with different total spin S _{T} for a rm Mn^{II}Mn^{III} _2 complex. The Mn_4 cubane complexes have been characterized to have an S = 9/2 ground state. Changing the mu_3-bridging ligand or the terminal ligand does not change the ground state of the cubane complexes. The cubane complexes show appreciable zero-field splitting thus have a large anisotropy energy. Because of this relaxation process be seen in theses molecules and shows an out-of-phase component in the AC susceptibility. Mn _8 and Mn_9 clusters show S = 11 and S = 3 ground state respectively. Neutral an reduced Mn_{12} complexes were also synthesized. All of

  9. Soil structure characterized using computed tomographic images (United States)

    Zhanqi Cheng; Stephen H. Anderson; Clark J. Gantzer; J. W. Van Sambeek


    Fractal analysis of soil structure is a relatively new method for quantifying the effects of management systems on soil properties and quality. The objective of this work was to explore several methods of studying images to describe and quantify structure of soils under forest management. This research uses computed tomography and a topological method called Multiple...

  10. Hydrothermal synthesis, structure and characterization of new ...

    Indian Academy of Sciences (India)


    The structure has tunnel-type cavities and are congenial for ion transportation through them. The compound exhibits moderate thermal stability. Keywords. Hydrothermal; crystal structure; solid electrolyte; iron (III) pyrophosphate. 1. Introduction. NASICON and related compounds belong to the well known family of solid ...

  11. Predicting and characterizing data sequences from structure-variable systems

    CERN Document Server

    Fangi, H P


    Abstract: In principle, all the natural systems such as biological, ecological and economical systems are structure-variable systems (in which some environment parameters are not fixed). In this Letter we show that data sequences from many structure-variable systems are short-term predictable. We also argue how to characterize the data sequences from structure-variable systems.

  12. AFM Structural Characterization of Drinking Water Biofilm ... (United States)

    Due to the complexity of mixed culture drinking water biofilm, direct visual observation under in situ conditions has been challenging. In this study, atomic force microscopy (AFM) revealed the three dimensional morphology and arrangement of drinking water relevant biofilm in air and aqueous solution. Operating parameters were optimized to improve imaging of structural details for a mature biofilm in liquid. By using a soft cantilever (0.03 N/m) and slow scan rate (0.5 Hz), biofilm and individual bacterial cell’s structural topography were resolved and continuously imaged in liquid without loss of spatial resolution or sample damage. The developed methodology will allow future in situ investigations to temporally monitor mixed culture drinking water biofilm structural changes during disinfection treatments. Due to the complexity of mixed culture drinking water biofilm, direct visual observation under in situ conditions has been challenging. In this study, atomic force microscopy (AFM) revealed the three dimensional morphology and arrangement of drinking water relevant biofilm in air and aqueous solution. Operating parameters were optimized to improve imaging of structural details for a mature biofilm in liquid. By using a soft cantilever (0.03 N/m) and slow scan rate (0.5 Hz), biofilm and individual bacterial cell’s structural topography were resolved and continuously imaged in liquid without loss of spatial resolution or sample damage. The developed methodo

  13. Carbon nanotubes: synthesis, structure, functionalization, and characterization. (United States)

    Zamolo, Valeria Anna; Vazquez, Ester; Prato, Maurizio


    Carbon nanotubes have generated great expectations in the scientific arena, mainly due to their spectacular properties, which include a high aspect ratio, high strain resistance, and high strength, along with high conductivities. Nowadays, carbon nanotubes are produced by a variety of methods, each of them with advantages and disadvantages. Once produced, carbon nanotubes can be chemically modified, using a wide range of chemical reactions. Functionalization makes these long wires much easier to manipulate and dispersible in several solvents. In addition, the properties of carbon nanotubes can be combined with those of organic appendages. Finally, carbon nanotubes need to be carefully characterized, either as pristine or modified materials.

  14. Structural and ethnobotanical characterization of velvet tamarind ...

    African Journals Online (AJOL)

    In order to help the sustainable management and conservation of this species, its structural characteristics and ethnobotanical traits were studied in the 4 vegetation types (typical dense forest, degraded dense forest, young fallow and old fallow) of the Lama forest reserve. A forest inventory was carried out in 100 randomly ...

  15. Synthesis, structural and surface morphological characterizations of ...

    African Journals Online (AJOL)

    Sulfated zirconia (SZ) nanoparticles (NPs) were successfully synthesized and deposited via chemical route called sol-gel technique. The structural, morphological, and optical properties the samples were investigated by X-ray diffraction (XRD), Energy Dispersive X-ray Spectrometry (EDX), Scanning Electron Microscopy ...

  16. Synthesis, structural characterization and biological activities of ...

    Indian Academy of Sciences (India)

    , 1H, 13C and 119Sn NMR spectral studies. The molecular structure of complex 5 has been confirmed by single ... Rosenani A Haque1 M A Salam1. The School of Chemical Sciences, Universiti Sains Malaysia, 11800 USM, Penang, Malaysia ...

  17. Hydrothermal synthesis, structure and characterization of new ...

    Indian Academy of Sciences (India)

    The structure has tunnel-type cavities and are congenial for ion transportation through them. The compound exhibits moderate ... Prasad2 K G Ashamanjari1. Department of Studies in Geology, University of Mysore, Mysore 570 006, India; Department of Studies in Physics, University of Mysore, Mysore 570 006, India ...

  18. Structural characterization of vegetation in the fynbos biome

    CSIR Research Space (South Africa)

    Campbell, BM


    Full Text Available A proposed system for the standardization of descriptive terminology for structural characterization of vegetation in the Fynbos Biome is presented in tabular form. Specific applications of the system are described and illustrations of some...

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

    African Journals Online (AJOL)

    Purpose: To synthesize thiosemicarbazide and determine its antimicrobial properties. Methods: Pyridine-based thiosemicarbazide was synthesized, characterized and evaluated for antimicrobial activity. The structure of the synthesized compound was established by spectral analysis, namely, Fourier transform infrared ...

  20. Synthesis and structural characterization of lithium ...

    Indian Academy of Sciences (India)

    of metal ions spans over s, p, d blocks and recently a few lanthanide complexes were also reported.17–32 .... version 2.1d was used to generate graphics for the X-ray structures. 2.3 General synthetic method for ligands (1 ...... Takolpuckdee P, Tomov A K, White A J P, Williams. D J, Elsegood M R J and Dale S H 2007 Inorg.

  1. Structural characterization of bacterioferritin from Blastochloris viridis.

    Directory of Open Access Journals (Sweden)

    Weixiao Y Wahlgren

    Full Text Available Iron storage and elimination of toxic ferrous iron are the responsibility of bacterioferritins in bacterial species. Bacterioferritins are capable of oxidizing iron using molecular oxygen and import iron ions into the large central cavity of the protein, where they are stored in a mineralized form. We isolated, crystallized bacterioferritin from the microaerophilic/anaerobic, purple non-sulfur bacterium Blastochloris viridis and determined its amino acid sequence and X-ray structure. The structure and sequence revealed similarity to other purple bacterial species with substantial differences in the pore regions. Static 3- and 4-fold pores do not allow the passage of iron ions even though structural dynamics may assist the iron gating. On the other hand the B-pore is open to water and larger ions in its native state. In order to study the mechanism of iron import, multiple soaking experiments were performed. Upon Fe(II and urea treatment the ferroxidase site undergoes reorganization as seen in bacterioferritin from Escherichia coli and Pseudomonas aeruginosa. When soaking with Fe(II only, a closely bound small molecular ligand is observed close to Fe(1 and the coordination of Glu94 to Fe(2 changes from bidentate to monodentate. DFT calculations indicate that the bound ligand is most likely a water or a hydroxide molecule representing a product complex. On the other hand the different soaking treatments did not modify the conformation of other pore regions.

  2. Structural characterization of Heusler compounds using NMR

    Energy Technology Data Exchange (ETDEWEB)

    Wurmehl, Sabine; Fecher, Gerhard; Balke, Benjamin; Ksenofontov, Vadim; Jung, Verena; Felser, Claudia [Johannes Gutenberg - Universitaet, 55099 Mainz (Germany); Wojcik, Marek [Institute of Physics, Polish Academy of Sciences, 02-668 Warszawa (Poland)


    The L2{sub 1} ordered Heusler alloys Co{sub 2}Mn{sub 1-x}Fe{sub x}Si with 0{<=}x{<=}1 attracted much scientific interest, as they are predicted to show high spin polarisation at the Fermi-energy. Therefore Co{sub 2}Mn{sub 1-x}Fe{sub x}Si samples were investigated using spin echo nuclear magnetic resonance (NMR) measurements. This method provides a tool to measure the hyperfine fields. The hyperfine fields represent a very sensitive local probe to order-disorder phenomena. The NMR measurements of polycrystalline Co{sub 2}FeSi samples exhibit a two-peak spectrum with an additional shoulder. This additional signals are attributed to second-order quadrupole splitting, a so called asymmetric line broadening and might be caused by tension within the structure (strain). This effect occurs even in highly ordered systems. Thus previous structural results are corroborated, demonstrating even locally a very high degree of order in Co{sub 2}FeSi. The NMR spectra of the series Co{sub 2}Mn{sub 1-x}Fe{sub x}Si (0.1{<=}x{<=}0.9) exhibit multiplet structures. These might be explained by quadrupole splitting and statistical distribution of Mn and Fe atoms on the Mn site. In summary, the high degree of order in Co{sub 2}Mn{sub 1-x}Fe{sub x}Si is shown.

  3. Continuous Dimensionality Characterization of Image Structures

    DEFF Research Database (Denmark)

    Felsberg, Michael; Kalkan, Sinan; Krüger, Norbert


    Intrinsic dimensionality is a concept introduced by statistics and later used in image processing to measure the dimensionality of a data set. In this paper, we introduce a continuous representation of the intrinsic dimension of an image patch in terms of its local spectrum or, equivalently, its...... is the representation of confidences as prior probabilities which can be used within a probabilistic framework. To show the potential of our continuous representation, we highlight applications in various contexts such as image structure classification, feature detection and localisation, visual scene statistics...... and optic flow evaluation....

  4. Native Cellulose: Structure, Characterization and Thermal Properties

    Directory of Open Access Journals (Sweden)

    Matheus Poletto


    Full Text Available In this work, the relationship between cellulose crystallinity, the influence of extractive content on lignocellulosic fiber degradation, the correlation between chemical composition and the physical properties of ten types of natural fibers were investigated by FTIR spectroscopy, X-ray diffraction and thermogravimetry techniques. The results showed that higher extractive contents associated with lower crystallinity and lower cellulose crystallite size can accelerate the degradation process and reduce the thermal stability of the lignocellulosic fibers studied. On the other hand, the thermal decomposition of natural fibers is shifted to higher temperatures with increasing the cellulose crystallinity and crystallite size. These results indicated that the cellulose crystallite size affects the thermal degradation temperature of natural fibers. This study showed that through the methods used, previous information about the structure and properties of lignocellulosic fibers can be obtained before use in composite formulations.

  5. Mechanical strength characterization of three-component composite structural components (United States)

    Chumaevskii, A. V.; Tarasov, S. Yu.; Kolubaev, E. A.; Rubtsov, V. E.; Eliseev, A. A.


    Mechanical strength characterization of structural components made of three-component composite material using additive manufacturing has been carried out. The deformation and fracture behaviour of two types was revealed. Mechanical strength characteristics of structural components have been determined in connection with the material properties.

  6. Dielectrical and structural characterization of iron oxide added to ...

    Indian Academy of Sciences (India)


    Dielectrical and structural characterization of iron oxide added to hydroxyapatite. C C SILVA*, F P FILHO, M F P GRAÇA, M A VALENTE and A S B SOMBRA. Physics Department, Aveiro University, Aveiro, Portugal. MS received 10 July 2007; revised 19 May 2008. Abstract. In this work we report preparation, structural ...

  7. Structural characterization of iodinated bovine growth hormone. (United States)

    Mattera, R; Turyn, D; Fernandez, H N; Dellacha, J M


    Bovine growth hormone (bGH) was submitted to iodination using limited amounts of oxidizing reagent, yielding a derivative with no more than 1-g-atom of iodine per mole of hormone. Analysis of the hydrolysis products indicated that monoiodotyrosine was almost the only product of substitution. Isolation and identification of the tryptic fragments showed that half of the 125I-labeled bGH molecules were iodinated in Tyr 174, followed by Tyr 158 (16%) and Tyr 42 (14%). Frontal gel chromatography indicated that the preparation did not contain significant amounts of unreacted bGH. Circular dichroism evidenced structural similarity between the native and the iodinated bGH. The iodinated hormone, like the native protein, undergoes self-association. The dissociation constant of the iodo-labeled bGH self-association equilibrium showed a two-fold increase when compared to that corresponding to the unlabeled hormone. At pH 8.5, where the equilibrium constant was estimated, one tenth of the molecules bear a charged iodotyrosyl residue (average pKapp = 9.3), which could account for part, if not all, of the observed difference regarding self-association. By this criterion, the presence of the iodine atom does not disturb the area engaged in dimer formation.

  8. Structural characterization of MAPLE deposited lipase biofilm (United States)

    Aronne, Antonio; Ausanio, Giovanni; Bloisi, Francesco; Calabria, Raffaela; Califano, Valeria; Fanelli, Esther; Massoli, Patrizio; Vicari, Luciano R. M.


    Lipases (triacylglycerol ester hydrolases) are enzymes used in several industrial applications. Enzymes immobilization can be used to address key issues limiting widespread application at industrial level. Immobilization efficiency is related to the ability to preserve the native conformation of the enzyme. MAPLE (Matrix Assisted Pulsed Laser Evaporation) technique, a laser deposition procedure for treating organic/polymeric/biomaterials, was applied for the deposition of lipase enzyme in an ice matrix, using near infrared laser radiation. Microscopy analysis showed that the deposition occurred in micrometric and submicrometric clusters with a wide size distribution. AFM imaging showed that inter-cluster regions are uniformly covered with smaller aggregates of nanometric size. Fourier transform infrared spectroscopy was used for both recognizing the deposited material and analyzing its secondary structure. Results showed that the protein underwent reversible self-association during the deposition process. Actually, preliminary tests of MAPLE deposited lipase used for soybean oil transesterification with isopropyl alcohol followed by gas chromatography-mass spectrometry gave results consistent with undamaged deposition of lipase.

  9. Structural Characterization of Polypropylene (PP) Mesomorphic Phases (United States)

    Hristov, Hristo; Werpetinski, Katrina; Taylor, Denise


    Rapid quenching and mechanical deformation of PP can generate structures (commonly known as ``mesomorphic'' phases), exhibiting specific WAXS patterns. The mesophase, presently studied, was prepared by grinding PP in a freezer mill, using liquid nitrogen as cryogenic agent. The analysis of the WAXS curve from the mesophase indicates that the extent of the interatomic correlation is in the range of 2-3 nm. The SAXS curve can be interpreted as resulting from particles with diameters close to 12 nm. To elucidate the source of this discrepancy, the WAXS curve was modeled by using the atomic coordinates of the monoclinic alfa-crystal. We found that satisfactory match is obtained by introducing an aggregation of small crystals ( ˜ 3X4X3 nm), having different types of mismatches at their boundaries. These results are a key to understand the peculiarities of the PP mesophase. Large mosaic crystals made of small blocks will show different coherence lengths depending on the experimental method. WAXS measurements will give the average size of the small block, EM and SAXS will measure the large dimensions. It is proposed that the PP mesomorphic phase is composed of highly defective mosaic PP crystals.

  10. Characterization of fluid transport in microscale structures

    Energy Technology Data Exchange (ETDEWEB)

    Paul, P.H.


    A new tool for imaging both scalar transport and velocity fields in liquid flows through microscale structures is described. The technique employs an ultraviolet laser pulse to write a pattern into the flow by uncaging a fluorescent dye. This is followed, at selected time delays, by flood illumination with a pulse of visible light which excites the uncaged dye. The resulting fluorescence image collected onto a sensitive CCD camera. The instrument is designed as an oil immersion microscope to minimize the beam steering effects. The caged fluorescent dye is seeded in trace quantities throughout the active fluid, thus images with high contrast and minimal distortion due to any molecular diffusion history can be obtained at any point within the microchannel by selectivity activating the dye in the immediate region of interest. The author reports images of pressure- and electrokinetically-driven steady flow within round cross section capillaries having micron scale inner diameters. The author also demonstrates the ability to recover the velocity profile from a time sequence of these scalar images by direct inversion of the conserved scalar advection-convection equation.

  11. Carbon nano structures: Production and characterization (United States)

    Beig Agha, Rosa

    L'objectif de ce memoire est de preparer et de caracteriser des nanostructures de carbone (CNS -- Carbon Nanostructures, en licence a l'Institut de recherche sur l'hydrogene, Quebec, Canada), un carbone avec un plus grand degre de graphitisation et une meilleure porosite. Le Chapitre 1 est une description generale des PEMFCs (PEMFC -- Polymer Electrolyte Membrane Fuel Cell) et plus particulierement des CNS comme support de catalyseurs, leur synthese et purification. Le Chapitre 2 decrit plus en details la methode de synthese et la purification des CNS, la theorie de formation des nanostructures et les differentes techniques de caracterisation que nous avons utilises telles que la diffraction aux rayons-X (XRD -- X-ray diffraction), la microscopie electronique a transmission (TEM -- transmission electron microscope ), la spectroscopie Raman, les isothermes d'adsorption d'azote a 77 K (analyse BET, t-plot, DFT), l'intrusion au mercure, et l'analyse thermogravimetrique (TGA -- thermogravimetric analysis). Le Chapitre 3 presente les resultats obtenus a chaque etape de la synthese des CNS et avec des echantillons produits a l'aide d'un broyeur de type SPEXRTM (SPEX/CertiPrep 8000D) et d'un broyeur de type planetaire (Fritsch Pulverisette 5). La difference essentielle entre ces deux types de broyeur est la facon avec laquelle les materiaux sont broyes. Le broyeur de type SPEX secoue le creuset contenant les materiaux et des billes d'acier selon 3 axes produisant ainsi des impacts de tres grande energie. Le broyeur planetaire quant a lui fait tourner et deplace le creuset contenant les materiaux et des billes d'acier selon 2 axes (plan). Les materiaux sont donc broyes differemment et l'objectif est de voir si les CNS produits ont les memes structures et proprietes. Lors de nos travaux nous avons ete confrontes a un probleme majeur. Nous n'arrivions pas a reproduire les CNS dont la methode de synthese a originellement ete developpee dans les laboratoires de l'Institut de

  12. Three-dimensional structural characterization of nonwoven fabrics. (United States)

    Venu, Lalith B Suragani; Shim, Eunkyoung; Anantharamaiah, Nagendra; Pourdeyhimi, Behnam


    Nonwoven materials are found in a gamut of critical applications. This is partly due to the fact that these structures can be produced at high speed and engineered to deliver unique functionality at low cost. The behavior of these materials is highly dependent on alignment of fibers within the structure. The ability to characterize and also to control the structure is important, but very challenging due to the complex nature of the structures. Thus, to date, focus has been placed mainly on two-dimensional analysis techniques for describing the behavior of nonwovens. This article demonstrates the utility of three-dimensional (3D) digital volumetric imaging technique for visualizing and characterizing a complex 3D class of nonwoven structures produced by hydroentanglement.

  13. Mathematical model for characterizing noise transmission into finite cylindrical structures (United States)

    Li, Deyu; Vipperman, Jeffrey S.


    This work presents a theoretical study of the sound transmission into a finite cylinder under coupled structural and acoustic vibration. Particular attention of this study is focused on evaluating a dimensionless quantity, ``noise reduction,'' for characterizing noise transmission into a small cylindrical enclosure. An analytical expression of the exterior sound pressure resulting from an oblique plane wave impinging upon the cylindrical shell is first presented, which is approximated from the exterior sound pressure for an infinite cylindrical structure. Next, the analytical solution of the interior sound pressure is computed using modal-interaction theory for the coupled structural acoustic system. These results are then used to derive the analytical formula for the noise reduction. Finally, the model is used to predict and characterize the sound transmission into a ChamberCore cylindrical structure, and the results are compared with experimental data. The effects of incidence angle and internal acoustic damping on the sound transmission into the cylinder are also parametrically studied. .

  14. Characterization of Structure and Damage in Materials in Four Dimensions

    Energy Technology Data Exchange (ETDEWEB)

    Robertson, I. M. [Univ. of Illinois, Urbana, IL (United States); Schuh, C. A. [Massachusetts Inst. of Technology (MIT), Cambridge, MA (United States); Vetrano, J. S. [U.S. Department of Energy, Washington, DC (United States); Browning, N. D. [Univ. of California, Davis, CA (United States); Field, D. P. [Washington State Univ., Pullman, WA (United States); Jensen, D. J. [Technical Univ. of Denmark, Roskilde (Denmark); Miller, M. K. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Baker, I. [Darmouth College, Hanover, NH (United States); Dunand, D. C. [Northwestern Univ., Evanston, IL (United States); Dunin-Borkowski, R. [Technical Univ. of Denmark, Lyngby (Denmark); Kabius, B. [Argonne National Lab. (ANL), Argonne, IL (United States); Kelly, T. [Cameca Instruments Corp., Madison, WI (United States); Lozano-Perez, S. [Univ. of Oxford (United Kingdom); Misra, A. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Rohrer, G. S. [Carnegie Mellon Univ., Pittsburgh, PA (United States); Rollett, A. D. [Carnegie Mellon Univ., Pittsburgh, PA (United States); Taheri, M. [Drexel Univ., Philadelphia, PA (United States); Thompson, G. B. [Univ. of Alabama, Tuscaloosa, AL (United States); Uchic, M. [Air Force Research Lab. (AFRL), Wright-Patterson AFB, OH (United States); Wang, X. L. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Was, G. [Univ. of Michigan, Ann Arbor, MI (United States)


    The materials characterization toolbox has recently experienced a number of parallel revolutionary advances, foreshadowing a time in the near future when materials scientists can quantify material structure across orders of magnitude in length and time scales (i.e., in four dimensions) completely. This paper presents a viewpoint on the materials characterization field, reviewing its recent past, evaluating its present capabilities, and proposing directions for its future development. Electron microscopy; atom-probe tomography; X-ray, neutron and electron tomography; serial sectioning tomography; and diffraction-based analysis methods are reviewed, and opportunities for their future development are highlighted. Particular attention is paid to studies that have pioneered the synergetic use of multiple techniques to provide complementary views of a single structure or process; several of these studies represent the state-of-the-art in characterization, and suggest a trajectory for the continued development of the field. Based on this review, a set of grand challenges for characterization science is identified, including suggestions for instrumentation advances, scientific problems in microstructure analysis, and complex structure evolution problems involving materials damage. The future of microstructural characterization is proposed to be one not only where individual techniques are pushed to their limits, but where the community devises strategies of technique synergy to address complex multiscale problems in materials science and engineering.

  15. Characterization of Forest Structure and an Assessment of Litter ...

    African Journals Online (AJOL)


    Many studies have cited mangroves as being among the most productive ecosystems of the world in terms of gross primary productivity and litter turnover, which forms a major food source for most estuarine animals. The present study aimed at characterizing the forest structure and assessing litter production, accumulation ...

  16. Structural and biochemical characterization of 3-hydroxybenzoate 6-hydroxylase

    NARCIS (Netherlands)

    Montersino, S.


    The thesis deals with the characterization of a new flavoprotein hydroxylase 3 hydroxybenzoate 6-hydroxylase (3HB6H) from Rhodococcus jostii RHA1. 3HB6H is able to insert exclusively oxygen in para-position and the enzyme has been chosen to study the structural basis of such regioselectivity. As

  17. Synthesis, characterization, X-ray crystal structure, electrochemical ...

    Indian Academy of Sciences (India)

    DOI 10.1007/s12039-015-0978-8. Synthesis, characterization, X-ray crystal structure, electrochemical evaluation and anti-cancer studies of a mixed ligand Cu(II) complex of (E)-N -((2-hydroxynaphthalen-1-yl)methylene)acetohydrazide. IRAN SHEIKHSHOAIEa, S YOUSEF EBRAHIMIPOURa,∗, MAHDIEH SHEIKHSHOAIEa,.

  18. Synthesis and structural characterization of a calcium coordination ...

    Indian Academy of Sciences (India)

    has been isolated from the calcium chloride–glycine–water system and structurally characterized. Each Ca(II) in 1 is eight-coordinated and is bonded to .... cal absorption correction was applied. All non- hydrogen atoms were refined ..... is available for coordination in the glycinate anion. Of the several metal, halogenide ...

  19. Characterization of structural and free energy properties of ...

    Indian Academy of Sciences (India)


    Jun 25, 2012 ... Characterization of structural and free energy properties of promoters associated with Primary and Operon TSS in Helicobacter pylori genome and their orthologs. ADITYA KUMAR and MANJU BANSAL*. Molecular Biophysics Unit, Indian Institute of Science, Bangalore 560 012, India. *Corresponding ...

  20. Characterization and global analysis of a family of Poisson structures

    Energy Technology Data Exchange (ETDEWEB)

    Hernandez-Bermejo, Benito [Escuela Superior de Ciencias Experimentales y Tecnologia, Edificio Departamental II, Universidad Rey Juan Carlos, Calle Tulipan S/N, 28933 (Mostoles), Madrid (Spain)]. E-mail:


    A three-dimensional family of solutions of the Jacobi equations for Poisson systems is characterized. In spite of its general form it is possible the explicit and global determination of its main features, such as the symplectic structure and the construction of the Darboux canonical form. Examples are given.

  1. Synthesis, structural characterization and biological activity of a ...

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 125; Issue 6. Synthesis, structural characterization and biological activity of a trinuclear zinc(II) complex: DNA interaction study and antimicrobial activity. Bhaskar Biswas Niranjan Kole Moumita Patra Shampa Dutta Mousumi Ganguly. Regular Articles Volume 125 ...

  2. Structural, magnetic and photocatalytic characterization of Bi1 ...

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 40; Issue 1. Structural, magnetic and photocatalytic characterization of Bi 1 − x La x FeO 3 nanoparticles synthesized by thermal decomposition method. S M MASOUDPANAH S M MIRKAZEMI R BAGHERIYEH F JABBARI F BAYAT. Volume 40 Issue 1 February 2017 pp ...

  3. Characterizing Thematized Derivative Schema by the Underlying Emergent Structures (United States)

    Garcia, Mercedes; Llinares, Salvador; Sanchez-Matamoros, Gloria


    This paper reports on different underlying structures of the derivative schema of three undergraduate students that were considered to be at the trans level of development of the derivative schema (action-process-object-schema). The derivative schema is characterized in terms of the students' ability to explicitly transfer the relationship between…

  4. Crystal structure, characterization and magnetic properties of a 1D ...

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 128; Issue 6. Crystal structure, characterization and magnetic properties of a 1D copper(II) polymer incorporating a Schiff base with carboxylate side arm. SHYAMAPADA SHIT MADHUSUDAN NANDY CORRADO RIZZOLI CÉDRIC DESPLANCHES SAMIRAN MITRA.

  5. Synthesis, characterization and crystal structure of new nickel ...

    Indian Academy of Sciences (India)

    Abstract. A novel nickel molybdenum complex with the 2,6-pyridine dicarboxylic acid ligand was successfully synthesized and characterized by thermogravimetric analysis and single crystal X-ray crystallography. The single-crystal X-ray data revealed that the structure is a hydrated 1-D polymer with two different Ni sites.

  6. Syntheses, characterization and crystal structures of potassium and ...

    Indian Academy of Sciences (India)

    Syntheses, characterization and crystal structures of potassium and barium complexes of a Schiff base ligand with different anions. Bhavesh Parmar Kamal Kumar Bisht Pratyush Maiti Parimal Paul Eringathodi Suresh. Special issue on Chemical Crystallography Volume 126 Issue 5 September 2014 pp 1373-1384 ...

  7. Syntheses, characterization and crystal structures of potassium and ...

    Indian Academy of Sciences (India)

    Syntheses, characterization and crystal structures of potassium and barium complexes of a Schiff base ligand with different anions. BHAVESH PARMARa, KAMAL KUMAR BISHTa,b, PRATYUSH MAITIc, PARIMAL PAULa,b, and ERINGATHODI SURESHa,b,∗. aAnalytical Discipline and Centralized Instrument Facility, ...

  8. Fluorescence microscopy for the characterization of structural integrity (United States)

    Street, Kenneth W.; Leonhardt, Todd A.


    The absorption characteristics of light and the optical technique of fluorescence microscopy for enhancing metallographic interpretation are presented. Characterization of thermally sprayed coatings by optical microscopy suffers because of the tendency for misidentification of the microstructure produced by metallographic preparation. Gray scale, in bright field microscopy, is frequently the only means of differentiating the actual structural details of porosity, cracking, and debonding of coatings. Fluorescence microscopy is a technique that helps to distinguish the artifacts of metallographic preparation (pullout, cracking, debonding) from the microstructure of the specimen by color contrasting structural differences. Alternative instrumentation and the use of other dye systems are also discussed. The combination of epoxy vacuum infiltration with fluorescence microscopy to verify microstructural defects is an effective means to characterize advanced materials and to assess structural integrity.

  9. Structural and electrical characterization of zinc oxide doped with antimony

    Directory of Open Access Journals (Sweden)

    G. Juárez Díaz


    Full Text Available In this work we report the results of structural and electrical characterization realized on zinc oxide single crystal samples with (001 orientation, which were doped with antimony. Doping was carried out by antimony thermal diffusion at 1000 °C for periods of 1 and 2 hours under nitrogen environment from a solid source formed by antimony oxide. Electrical characterization by I-V curves and Hall effect shown an increase in acceptor concentration which demonstrates that doping is effective and create holes in zinc oxide samples.

  10. Characterization of Quadruplex DNA Structure by Circular Dichroism. (United States)

    Del Villar-Guerra, Rafael; Gray, Robert D; Chaires, Jonathan B


    Circular dichroism (CD) is a phenomenon that arises from the differential absorption of left- and right-handed circularly polarized light, and may be seen with optically active molecules. CD spectroscopy provides useful spectral signatures for biological macromolecules in solution, and provides low-resolution structural information about macromolecular conformation. CD spectroscopy is particularly useful for monitoring conformational changes in macromolecules upon environmental perturbations. G-quadruplex structures show unique CD spectral signatures, and CD is an important tool for characterizing their formation and global structure. This protocol offers step-by-step methods for determining reliable and reproducible CD spectra of quadruplex structures and normalizing the spectra for presentation. CD spectra properly normalized with respect to quadruplex concentration and path length are required to facilitate accurate comparison of results among laboratories. The standard operating procedures proposed are recommended to make such comparison accurate and informative. © 2017 by John Wiley & Sons, Inc. Copyright © 2017 John Wiley & Sons, Inc.

  11. Structural and mechanical characterization of hybrid metallic-inorganic nanosprings (United States)

    Habtoun, Sabrina; Houmadi, Said; Reig, Benjamin; Pouget, Emilie; Dedovets, Dmytro; Delville, Marie-Hélène; Oda, Reiko; Cristiano, Fuccio; Bergaud, Christian


    Silica nanosprings (NS) are fabricated by a sol–gel deposition of silica precursors onto a template made of self-assembled organic chiral nanostructures. They are deposited and assembled on microstructured silicon substrates, and then metallized and clamped in a single lithography-free step using a focused ion beam (FIB). The resulting suspended hybrid metallic/inorganic NS are then characterized with high-resolution transmission electron microscopy (HRTEM) and scanning TEM/energy-dispersive X-ray spectroscopy (STEM/EDX), showing the atomic structure of the metallic layer. Three-point bending tests are also carried out using an atomic force microscope (AFM) and supported by finite element method (FEM) simulation with COMSOL Multiphysics allowing the characterization of the mechanical behavior and the estimation of the stiffness of the resulting NS. The information obtained on the structural and mechanical properties of the NS is discussed for future nano-electro-mechanical system (NEMS) applications.

  12. Characterization of Multiferroic Domain Structures in Multiferroic Oxides

    Directory of Open Access Journals (Sweden)

    Lizhi Liang


    Full Text Available Multiferroic oxides have been received much attention due to that these materials exhibit multiple ferroic order parameters (e.g., electric polarization in ferroelectrics, magnetization in ferromagnetics, or spontaneous strain in ferroelastics simultaneously in the same phase in a certain temperature range, which offer an exciting way of coupling between the ferroic order parameters. Thus, this provides a possibility for constructing new type of multifunctional devices. The multiferroic domain structures in these materials are considered to be an important factor to improve the efficiency and performance of future multiferroic devices. Therefore, the domain structures in multiferroic oxides are widely investigated. Recent developments in domain characterization techniques, particularly the aberration-corrected transmission electron microscopy (TEM, have enabled us to determine the domain structures at subangstrom scale, and the recent development of in situ TEM techniques allows ones to study the dynamic behaviors of multiferroic domains under applied fields or stress while the atomic structure is imaged directly. This paper provides a review of recent advances on the characterization of multiferroic domain structures in multiferroic oxides, which have been achieved by the notable advancement of aberration-corrected TEM.

  13. Characterizing the Relative Spatial Structure of Point Patterns

    Directory of Open Access Journals (Sweden)

    Eric Marcon


    Full Text Available We generalize Ripley’s K function to get a new function, M, to characterize the spatial structure of a point pattern relatively to another one. We show that this new approach is pertinent in ecology when space is not homogenous and the size of objects matters. We present how to use the function and test the data against the null hypothesis of independence between points. In a tropical tree data set we detect intraspecific aggregation and interspecific competition.

  14. In situ characterization of structural dynamics in swelling hydrogels. (United States)

    Guzman-Sepulveda, J R; Deng, J; Fang, J Y; Dogariu, A


    Characterizing the structural morphology and the local viscoelastic properties of soft complex systems raises significant challenges. Here we introduce a dynamic light scattering method capable of in situ, continuous monitoring of structural changes in evolving systems such as swelling gels. We show that the inherently non-stationary dynamics of embedded probes can be followed using partially coherent radiation, which effectively isolates only single scattering contributions even during the dramatic changes in the scattering regime. Using a simple and robust experimental setup, we demonstrate the ability to continuously monitor the structural dynamics of chitosan hydrogels formed by the Ag(+) ion-triggered gelation during their long-term swelling process. We demonstrate that both the local viscoelastic properties of the suspending medium and an effective cage size experienced by diffusing probe particles loaded into the hydrogel can be recovered and used to describe the structural dynamics of hydrogels with different levels of cross-linking. This characterization capability is critical for defining and controlling the hydrogel performance in different biomedical applications.

  15. Characterization of electronic structure of periodically strained graphene

    Energy Technology Data Exchange (ETDEWEB)

    Aslani, Marjan; Garner, C. Michael, E-mail:; Nishi, Yoshio [Department of Electrical Engineering, Stanford University, Stanford, California 94305 (United States); Kumar, Suhas [Department of Electrical Engineering, Stanford University, Stanford, California 94305 (United States); Hewlett-Packard Laboratories, 1501 Page Mill Road, Palo Alto, California 94304 (United States); Nordlund, Dennis [Stanford Synchrotron Radiation Lightsource, SLAC National Accelerator Laboratory, 2575 Sand Hill Road, Menlo Park, California 94025 (United States); Pianetta, Piero [Department of Electrical Engineering, Stanford University, Stanford, California 94305 (United States); Stanford Synchrotron Radiation Lightsource, SLAC National Accelerator Laboratory, 2575 Sand Hill Road, Menlo Park, California 94025 (United States)


    We induced periodic biaxial tensile strain in polycrystalline graphene by wrapping it over a substrate with repeating pillar-like structures with a periodicity of 600 nm. Using Raman spectroscopy, we determined to have introduced biaxial strains in graphene in the range of 0.4% to 0.7%. Its band structure was characterized using photoemission from valance bands, shifts in the secondary electron emission, and x-ray absorption from the carbon 1s levels to the unoccupied graphene conduction bands. It was observed that relative to unstrained graphene, strained graphene had a higher work function and higher density of states in the valence and conduction bands. We measured the conductivity of the strained and unstrained graphene in response to a gate voltage and correlated the changes in their behavior to the changes in the electronic structure. From these sets of data, we propose a simple band diagram representing graphene with periodic biaxial strain.

  16. Dimensional characterization of biperiodic imprinted structures using optical scatterometry

    KAUST Repository

    Gereige, Issam


    In this paper, we report on the characterization of biperiodic imprinted structures using a non-destructive optical technique commonly called scatterometry. The nanostructures consist of periodic arrays of square and circular dots which were imprinted in a thermoplastic polymer by thermal nanoimprint lithography. Optical measurements were performed using spectroscopic ellipsometry in the spectral region of 1.5-4 eV. The geometrical profiles of the imprinted structures were reconstructed using the Rigorous Coupled-Wave Analysis (RCWA) to model the diffraction phenomena by periodic gratings. The technique was also adapted for large scale evaluation of the imprint process. Uniqueness of the solution was examined by analyzing the diffraction of the structure at different experimental conditions, for instance at various angles of incidence. © 2013 Elsevier B.V. All rights reserved.

  17. Synthesis and electronic structure of bis(imino)pyridine iron metallacyclic intermediates in iron-catalyzed cyclization reactions. (United States)

    Hoyt, Jordan M; Sylvester, Kevin T; Semproni, Scott P; Chirik, Paul J


    The bis(imino)pyridine iron dinitrogen compound, ((iPr(TB))PDI)Fe(N2)2 ((iPr(TB))PDI = 2,6-(2,6-(i)Pr2-C6H3-N═C-(CH2)3)2(C5H1N)) is an effective precatalyst for the [2π + 2π] cycloaddition of diallyl amines as well as the hydrogenative cyclization of N-tosylated enynes and diynes. Addition of stoichiometric quantities of amino-substituted enyne and diyne substrates to ((iPr(TB))PDI)Fe(N2)2 resulted in isolation of catalytically competent bis(imino)pyridine iron metallacycle intermediates. A combination of magnetochemistry, X-ray diffraction, and Mössbauer spectroscopic and computational studies established S = 1 iron compounds that are best described as intermediate-spin iron(III) (SFe = 3/2) antiferromagnetically coupled to a chelate radical anion (SPDI = 1/2). Catalytically competent bis(imino)pyridine iron diene and metallacycles relevant to the [2π + 2π] cycloaddition were also isolated and structurally characterized. The combined magnetic, structural, spectroscopic, and computational data support an Fe(I)-Fe(III) catalytic cycle where the bis(imino)pyridine chelate remains in its one-electron reduced radical anion form. These studies revise a previous mechanistic proposal involving exclusively ferrous intermediates and highlight the importance of the redox-active bis(imino)pyridine chelate for enabling catalytic cyclization chemistry with iron.

  18. Magnetochemistry of chromium (III) (abstract) (United States)

    Merabet, K. E.; Burriel, R.; Carlin, Richard L.


    There are relatively few superexchange-coupled antiferromagnets of chromium (III), largely because the exchange interactions are so weak. We have begun a program to study these materials and present magnetic susceptibility measurements on several new systems. We find that a polycrystalline sample of [Cr(NH3)5Cl]Cl2 behaves as a magnetic linear chain, and orders antiferromagnetically at about 600 mK, and that single crystals of [Cr(en)3]X3ṡ3H2O order at 130 mK when X is chloride. The analogous bromide orders at 112 mK. The chloride exhibits an easy axis, parallel to the longitudinal axis, while the bromide exhibits an easy plane. The data have been successfully fitted by several different procedures which result in much the same parameters. In addition to the exchange, it is necessary to include in the analysis the zero-field splitting of the chromium ions. The zero-field splitting in paramagnetic NaMg[Cr(oxalate)3]ṡ9H2O has also been measured.

  19. Porous Structure Characterization in Titanium Coating for Surgical Implants

    Directory of Open Access Journals (Sweden)

    M.V. Oliveira


    Full Text Available Powder metallurgy techniques have been used to produce controlled porous structures, such as the porous coatings applied for dental and orthopedic surgical implants, which allow bony tissue ingrowth within the implant surface improving fixation. This work presents the processing and characterization of titanium porous coatings of different porosity levels, processed through powder metallurgy techniques. Pure titanium sponge powders were used for coating and Ti-6Al7Nb powder metallurgy rods were used as substrates. Characterization was made through quantitative metallographic image analysis using optical light microscope for coating porosity data and SEM analysis for evaluation of the coating/substrate interface integrity. The results allowed optimization of the processing parameters in order to obtain porous coatings that meet the requirements for use as implants.

  20. Structural and functional characterization of two alpha-synuclein strains (United States)

    Bousset, Luc; Pieri, Laura; Ruiz-Arlandis, Gemma; Gath, Julia; Jensen, Poul Henning; Habenstein, Birgit; Madiona, Karine; Olieric, Vincent; Böckmann, Anja; Meier, Beat H.; Melki, Ronald


    α-synuclein aggregation is implicated in a variety of diseases including Parkinson’s disease, dementia with Lewy bodies, pure autonomic failure and multiple system atrophy. The association of protein aggregates made of a single protein with a variety of clinical phenotypes has been explained for prion diseases by the existence of different strains that propagate through the infection pathway. Here we structurally and functionally characterize two polymorphs of α-synuclein. We present evidence that the two forms indeed fulfil the molecular criteria to be identified as two strains of α-synuclein. Specifically, we show that the two strains have different structures, levels of toxicity, and in vitro and in vivo seeding and propagation properties. Such strain differences may account for differences in disease progression in different individuals/cell types and/or types of synucleinopathies.

  1. Structural and optical characterization of the propolis films (United States)

    Drapak, S. I.; Bakhtinov, A. P.; Gavrylyuk, S. V.; Drapak, I. T.; Kovalyuk, Z. D.


    We have performed structural and optical characterizations of the propolis (an organic entity of biological nature) films grown on various non-organic substrates. The films were grown from a propolis melt or a propolis alcohol solution. The crystal structure has been observed in the films precipitated from the solution onto substrates such as an amorphous glass and sapphire or semiconductor indium monoselenide. For any growth method, the propolis film is a semiconductor with the bandgap of 3.07 eV at 300 K that is confirmed by a maximum in photoluminescence spectra at 2.86 eV. We argue that propolis films might be used in various optoelectronic device applications.

  2. Structural and optical characterization of the propolis films

    Energy Technology Data Exchange (ETDEWEB)

    Drapak, S.I. [Frantsevich Institute of Materials Science Problems, National Academy of Sciences of Ukraine, Chernivtsi Department, 5 Iryna Vilde Str., 58001 Chernivtsi (Ukraine)]. E-mail:; Bakhtinov, A.P. [Frantsevich Institute of Materials Science Problems, National Academy of Sciences of Ukraine, Chernivtsi Department, 5 Iryna Vilde Str., 58001 Chernivtsi (Ukraine); Gavrylyuk, S.V. [Frantsevich Institute of Materials Science Problems, National Academy of Sciences of Ukraine, Chernivtsi Department, 5 Iryna Vilde Str., 58001 Chernivtsi (Ukraine); Drapak, I.T. [Chernivtsi National University, 2 Kotsyubynskii Str., 58012 Chernivtsi (Ukraine); Kovalyuk, Z.D. [Frantsevich Institute of Materials Science Problems, National Academy of Sciences of Ukraine, Chernivtsi Department, 5 Iryna Vilde Str., 58001 Chernivtsi (Ukraine)


    We have performed structural and optical characterizations of the propolis (an organic entity of biological nature) films grown on various non-organic substrates. The films were grown from a propolis melt or a propolis alcohol solution. The crystal structure has been observed in the films precipitated from the solution onto substrates such as an amorphous glass and sapphire or semiconductor indium monoselenide. For any growth method, the propolis film is a semiconductor with the bandgap of 3.07 eV at 300 K that is confirmed by a maximum in photoluminescence spectra at 2.86 eV. We argue that propolis films might be used in various optoelectronic device applications.

  3. Structural and Energetic Characterization of the Ankyrin Repeat Protein Family.

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    R Gonzalo Parra


    Full Text Available Ankyrin repeat containing proteins are one of the most abundant solenoid folds. Usually implicated in specific protein-protein interactions, these proteins are readily amenable for design, with promising biotechnological and biomedical applications. Studying repeat protein families presents technical challenges due to the high sequence divergence among the repeating units. We developed and applied a systematic method to consistently identify and annotate the structural repetitions over the members of the complete Ankyrin Repeat Protein Family, with increased sensitivity over previous studies. We statistically characterized the number of repeats, the folding of the repeat-arrays, their structural variations, insertions and deletions. An energetic analysis of the local frustration patterns reveal the basic features underlying fold stability and its relation to the functional binding regions. We found a strong linear correlation between the conservation of the energetic features in the repeat arrays and their sequence variations, and discuss new insights into the organization and function of these ubiquitous proteins.

  4. Thermodynamic and structural characterization of amphiphilic melamine-type monolayers. (United States)

    Vollhardt, D; Fainerman, V B; Liu, F


    Monolayers of amphiphilic melamine derivatives are good candidates for the formation of supramolecular structures by hydrogen-bonding of nonsurface active species dissolved in the aqueous subphase by molecular recognition. In the present work, the thermodynamic and structural properties of the Langmuir monolayers of a homologous series of a selected amphiphilic melamine-type are characterized. Good candidates for such studies are the decyl, undecyl, and dodecyl homologues of the 2,4-di(n-alkylamino)-6-amino-1,3,5-triazine (2CnH(2n+1)-melamine) monolayers because of their two-phase coexistence region in the accessible temperature range. The characterization of the structural and phase behavior is performed by a combination of surface pressure studies with Brewster angle microscopy (BAM) imaging and Grazing incidence X-ray diffraction (GIXD) measurements. A comprehensive thermodynamic analysis provides good agreement between the experimental surface pressure - area (Pi-A) isotherms and the theoretical curves that were calculated on the basis of equations of state for a large region of monolayer stages developed by us in J. Phys. Chem. 1999, 103, 145. Theoretical curves calculated by application of equations of state only for the fluid monolayer state proposed recently by Rusanov (J. Chem Phys. 2004, 120, 10736) are in good agreement with the experiments in a limited temperature range. A rigorous equation is derived and applied to the experimental results for the calculation of the enthalpy of two-dimensional phase transition. The combination of BAM and GIXD illustrates that the microscopic long range ordering of the condensed monolayer phases is related to the lattice structure of the condensed monolayer.

  5. Characterization of monomeric intermediates during VSV glycoprotein structural transition.

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    Aurélie A Albertini


    Full Text Available Entry of enveloped viruses requires fusion of viral and cellular membranes, driven by conformational changes of viral glycoproteins. Crystal structures provide static pictures of pre- and post-fusion conformations of these proteins but the transition pathway remains elusive. Here, using several biophysical techniques, including analytical ultracentrifugation, circular dichroïsm, electron microscopy and small angle X-ray scattering, we have characterized the low-pH-induced fusogenic structural transition of a soluble form of vesicular stomatitis virus (VSV glycoprotein G ectodomain (G(th, aa residues 1-422, the fragment that was previously crystallized. While the post-fusion trimer is the major species detected at low pH, the pre-fusion trimer is not detected in solution. Rather, at high pH, G(th is a flexible monomer that explores a large conformational space. The monomeric population exhibits a marked pH-dependence and adopts more elongated conformations when pH decreases. Furthermore, large relative movements of domains are detected in absence of significant secondary structure modification. Solution studies are complemented by electron micrographs of negatively stained viral particles in which monomeric ectodomains of G are observed at the viral surface at both pH 7.5 and pH 6.7. We propose that the monomers are intermediates during the conformational change and thus that VSV G trimers dissociate at the viral surface during the structural transition.

  6. Characterization of monomeric intermediates during VSV glycoprotein structural transition. (United States)

    Albertini, Aurélie A; Mérigoux, Cécile; Libersou, Sonia; Madiona, Karine; Bressanelli, Stéphane; Roche, Stéphane; Lepault, Jean; Melki, Ronald; Vachette, Patrice; Gaudin, Yves


    Entry of enveloped viruses requires fusion of viral and cellular membranes, driven by conformational changes of viral glycoproteins. Crystal structures provide static pictures of pre- and post-fusion conformations of these proteins but the transition pathway remains elusive. Here, using several biophysical techniques, including analytical ultracentrifugation, circular dichroïsm, electron microscopy and small angle X-ray scattering, we have characterized the low-pH-induced fusogenic structural transition of a soluble form of vesicular stomatitis virus (VSV) glycoprotein G ectodomain (G(th), aa residues 1-422, the fragment that was previously crystallized). While the post-fusion trimer is the major species detected at low pH, the pre-fusion trimer is not detected in solution. Rather, at high pH, G(th) is a flexible monomer that explores a large conformational space. The monomeric population exhibits a marked pH-dependence and adopts more elongated conformations when pH decreases. Furthermore, large relative movements of domains are detected in absence of significant secondary structure modification. Solution studies are complemented by electron micrographs of negatively stained viral particles in which monomeric ectodomains of G are observed at the viral surface at both pH 7.5 and pH 6.7. We propose that the monomers are intermediates during the conformational change and thus that VSV G trimers dissociate at the viral surface during the structural transition.

  7. Ambazone-lipoic acid salt: Structural and thermal characterization

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    Kacso, Irina [National Institute for Research and Development of Isotopic and Molecular Technologies, 65-103 Donath street, 400293 Cluj-Napoca (Romania); Racz, Csaba-Pal; Santa, Szabolcs [Babes-Bolyai' University, Faculty of Chemistry, 11 Arany Janos street, Cluj-Napoca (Romania); Rus, Lucia [' Iuliu Hatieganu' University of Medicine and Pharmacy, Faculty of Pharmacy, 6 Louis Pasteur street, 400349 Cluj-Napoca (Romania); Dadarlat, Dorin; Borodi, Gheorghe [National Institute for Research and Development of Isotopic and Molecular Technologies, 65-103 Donath street, 400293 Cluj-Napoca (Romania); Bratu, Ioan, E-mail: [National Institute for Research and Development of Isotopic and Molecular Technologies, 65-103 Donath street, 400293 Cluj-Napoca (Romania)


    Highlights: Black-Right-Pointing-Pointer Salt of Ambazone with lipoic acid obtained by solvent-drop grinding. Black-Right-Pointing-Pointer Ambazone lipoate salt crystallizes in monoclinic system. Black-Right-Pointing-Pointer FTIR data suggest the deprotonation of the lipoic acid. Black-Right-Pointing-Pointer Thermal behaviour different of ambazone salt as compared to the starting compounds. - Abstract: A suitable method for increasing the solubility, dissolution rate and consequently the bioavailability of poor soluble acidic or basic drugs is their salt formation. The aim of this study is to investigate the structural and thermal properties of the compound obtained by solvent drop grinding (SDG) method at room temperature, starting from the 1:1 molar ratios of ambazone (AMB) and {alpha}-lipoic acid (LA). The structural characterization was performed with X-ray powder diffraction (XRPD) and infrared spectroscopy (FTIR). The thermal behaviour of the obtained compound (AMB{center_dot}LA) was investigated by differential scanning calorimetry (DSC) and thermogravimetry (TG). The photopyroelectric calorimetry, in front detection configuration (FPPE), was applied to measure and compare the room temperature values of one dynamic thermal parameter (thermal effusivity) for starting and resulting compounds. Both structural and supporting calorimetric techniques pointed out a salt structure for AMB{center_dot}LA compound as compared to those of the starting materials.

  8. Mid foot kinetics characterize structural polymorphism in diabetic foot disease. (United States)

    Sinacore, David R; Bohnert, Kathryn L; Hastings, Mary K; Johnson, Jeffrey E


    Diabetic foot disease is characterized by progressive foot deformities that lead to amputation and disabling morbidity. The purpose is to investigate the classification of two distinct phenotypes of mid foot structural polymorphism in individuals using plantar kinetic and pressure distribution and tarsal bone density assessments. Twenty-two individuals (26 ft) with diabetes mellitus, peripheral neuropathy and at least one mid foot deformity were compared to 29 age-, gender- and race-matched healthy controls (58 ft). Eleven subjects with diabetes mellitus and peripheral neuropathy (11 ft) had lateral deformity; 11 subjects (15 ft) had medial deformity. Each subject had calcaneal bone mineral density and plantar force and pressure assessments walking barefoot over an EMED-ST P-2 platform. Control subjects had lower mid foot vertical forces and pressures despite significantly higher preferred walking speed. In subjects with diabetes and neuropathy, maximum vertical force was 6-fold greater, force-time integral 9.5-fold greater, peak pressure 6.7-fold higher, pressure-time integral was 9.7-fold greater, contact area 2-fold greater and contact time 1.9-fold higher than controls. Pressure values were larger in involved vs uninvolved (P0.05). During stance in the mid foot, subjects with medial column phenotype showed greater pressure in the medial mask; subjects with lateral column phenotype had greater pressures in the lateral mask (Pfoot vs the non-deformity foot; bone mineral density was lower in medial column phenotype vs lateral column phenotype (P=0.02). Diabetic foot disease can be classified as stereotypical, structurally-distinct phenotypes of deformities of the medial and lateral columns of the mid foot. Assessments of pedal bone density and plantar mid foot force and pressure during barefoot walking can characterize the structural polymorphic phenotypes and may assist the foot care specialist in clinical decision making.

  9. Function Discovery and Structural Characterization of a Methylphosphonate Esterase

    Energy Technology Data Exchange (ETDEWEB)

    Xiang, Dao Feng [Texas A & M Univ., College Station, TX (United States); Patskovsky, Yury [Einstein College of Medicine, Bronx, NY (United States); Nemmara, Venkatesh V. [Texas A & M Univ., College Station, TX (United States); Toro, Rafael [Einstein College of Medicine, Bronx, NY (United States); Almo, Steven C. [Einstein College of Medicine, Bronx, NY (United States); Raushel, Frank M. [Texas A & M Univ., College Station, TX (United States)


    Pmi1525, an enzyme of unknown function from Proteus mirabilis HI4320 and the amidohydrolase superfamily, was cloned, purified to homogeneity, and functionally characterized. The three-dimensional structure of Pmi1525 was determined with zinc and cacodylate bound in the active site (PDB id: 3RHG). We also determined the structure with manganese and butyrate in the active site (PDB id: 4QSF). Pmi1525 folds as a distorted (β/α)8-barrel that is typical for members of the amidohydrolase superfamily and cog1735. Moreover, the substrate profile for Pmi1525 was determined via a strategy that marshaled the utilization of bioinformatics, structural characterization, and focused library screening. The protein was found to efficiently catalyze the hydrolysis of organophosphonate and carboxylate esters. The best substrates identified for Pmi1525 are ethyl 4-nitrophenylmethyl phosphonate (kcat and kcat /Km values of 580 s–1 and 1.2 × 105 M–1 s–1, respectively) and 4-nitrophenyl butyrate (kcat and kcat /Km values of 140 s–1 and 1.4 × 105 M–1 s–1, respectively). Pmi1525 is stereoselective for the hydrolysis of chiral methylphosphonate esters. The enzyme hydrolyzes the (SP)-enantiomer of isobutyl 4-nitrophenyl methylphosphonate 14 times faster than the corresponding (RP)-enantiomer. The catalytic properties of this enzyme make it an attractive template for the evolution of novel enzymes for the detection, destruction, and detoxification of organophosphonate nerve agents.

  10. Molecular and electronic structure of [Mn(V)N(cyclam-acetato)]PF6. A combined experimental and DFT study. (United States)

    Grapperhaus, C A; Bill, E; Weyhermüller, T; Neese, F; Wieghardt, K


    From the reaction of Li(cyclam-acetate), MnCl(2).4H(2)O, and KPF(6) in methanol brown microcrystals of [Mn(III)Cl(cyclam-acetato)]PF(6) (1) were obtained in the presence of air (cyclam-acetic acid = 1,4,8,11-tetraazacyclotetradecane-1-acetic acid). The reaction of 1 in aqueous NH(3) solution with NaOCl produced blue crystals of [Mn(V)N(cyclam-acetato)]PF(6) (2). Complexes 1 and 2 were characterized by single-crystal X-ray crystallography, IR and Raman, electronic absorption, and (1)H, (13)C, and (15)N NMR spectroscopies. Their magnetochemistry as well as their electrochemistry have been investigated. The complexes [MnN(cyclam-acetato)](+/2+) were studied by theoretical calculations at the DFT and semiempirical levels in order to obtain more insight into the ground and excited states of the Mn(V)(triple bond)N unit. Structural and spectroscopic parameters were successfully calculated and compared to experiment. A pictorial description of the bonding has been developed.

  11. Solid state synthesis and structural characterization of zinc titanates

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    Ayed, Sarra, E-mail: [Laboratory of Composite Ceramic and Polymer Materials, Scientific Faculty of Sfax (Tunisia); Abdelkefi, Helmi; Khemakhem, Hamadi [Laboratory of Ferroelectric Materials, Scientific Faculty of Sfax (Tunisia); Matoussi, Adel [Laboratory of Composite Ceramic and Polymer Materials, Scientific Faculty of Sfax (Tunisia)


    Zinc titanate composite materials were synthesized via solid state sintering process using high-purity metal oxide powders (purity ∼99.99%). The titanium incorporation into ZnO matrix was investigated by X-ray diffraction which revealed the coexistence of spinel Zn{sub 2}TiO{sub 4} and hexagonal ZnTiO{sub 3} with the ZnO wurtzite structures. No reflection peaks of rutile TiO{sub 2} phase were detected. The IR spectroscopy and Raman scattering spectroscopy were used to characterize the structural and chemical properties of the ZnO/TiO{sub 2} composites. The IR bands and vibrational modes of all crystalline phases were detected. The effect of TiO{sub 2} doping rates (x = 3, 5 and 7 wt%) on bands shifting, Raman intensity and structural quality was discussed. - Highlights: • Zinc titanates materials were synthesized via solid state sintering process. • XRD measurements reveal the formation of Zn{sub 2}TiO{sub 4}, hexagonal ZnTiO{sub 3} and ZnO phases. • IR analysis provokes the presence of Ti−O stretching vibration bands. • Raman study provokes the appearance of new zinc titanates vibrational peaks. • The TiO{sub 2} effect into ZnO is sensed by the shift and intensity changes of peaks.

  12. Fabrication, characterization, and application of microresonators and resonant structures (United States)

    Cohoon, Gregory A.

    Optical resonators are structures that allow light to circulate and store energy for a duration of time. This work primarily looks at the fabrication, characterization, and application of whispering gallery mode microresonators and the analysis of organic photonic crystal-like structures and simulation of their resonant effects. Whispering gallery mode (WGM) microresonators are a class of cylindrically symmetric optical resonator which light circulates around the equator of the structure. These resonators are named after acoustic whispering galleries, where a whisper can be heard anywhere along the perimeter of a circular room. These optical structures are known for their ultra high Q-factor and their low mode volume. Q-factor describes the photon lifetime in the cavity and is responsible for the energy buildup within the cavity and sharp spectral characteristics of WGM resonators. The energy buildup is ideal for non-linear optics and the sharp spectral features are beneficial for sensing applications. Characterization of microbubble resonators is done by coupling light from a tunable laser source via tapered optical fiber into the cavity. The fabrication of quality tapered optical fiber on the order of 1--2 microm is critical to working on WGM resonators. The measurement of Q-factors up to 2x10 8 and mode spectra are possible with these resonators and experimental techniques. This work focuses on microdisk and microbubble WGM resonators. The microdisk resonators are fabricated by femtosecond laser micromachining. The micromachined resonators are fabricated by ablating rotating optical fiber to generate the disk shape and then heated to reflow the surface to improve optical quality. These resonators have a spares mode spectrum and display a Q factor as high a 2x106. The microbubble resonators are hollow microresonators fabricated by heating a pressurized capillary tube which forms a bubble in the area exposed to heat. These have a wall thickness of 2--5 microm and

  13. Structural Characterization of Core Region in Erwinia amylovora Lipopolysaccharide

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    Angela Casillo


    Full Text Available Erwinia amylovora (E. amylovora is the first bacterial plant pathogen described and demonstrated to cause fire blight, a devastating plant disease affecting a wide range of species including a wide variety of Rosaceae. In this study, we reported the lipopolysaccharide (LPS core structure from E. amylovora strain CFBP1430, the first one for an E. amylovora highly pathogenic strain. The chemical characterization was performed on the mutants waaL (lacking only the O-antigen LPS with a complete LPS-core, wabH and wabG (outer-LPS core mutants. The LPSs were isolated from dry cells and analyzed by means of chemical and spectroscopic methods. In particular, they were subjected to a mild acid hydrolysis and/or a hydrazinolysis and investigated in detail by one and two dimensional Nuclear Magnetic Resonance (NMR spectroscopy and ElectroSpray Ionization Fourier Transform-Ion Cyclotron Resonance (ESI FT-ICR mass spectrometry.


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    Diana Dragancea, Vladimir B. Arion, Sergiu Shova


    Full Text Available The new ligand, bis(2-hydroxybenzaldehydediaminoguanizone (1 has been synthesized and characterized by elemental analysis, IR and 1H NMR spectroscopies. The crystal structure of the compound was determined by X-ray diffraction. The ligand C15H15N5O2·C2H5OH crystallizes in the monoclinic space group P21/c with unit cell parameters a = 8.9102(3, b = 10.0357(3, c = 19.7618(6 Å, β = 98.385(2°, Z = 4, V = 1748.21(9 Å3, R1 = 0.040. The amino form of the ligand adopts a planar conformation stabilized by two intramolecular hydrogen bonds of the type O–H···N, in which the H atoms of the central amino group are directed to the lone-pair regions of the azomethine nitrogen atoms.

  15. [Structural characterization and spectroscopic analysis of the aloin]. (United States)

    Xie, Yun-Fei; Huan, Nan; Cao, Yuan-Yuan; Wang, He-Ya; Zhong, Ying; Yao, Wei-Rong; Qian, He


    Aloe is widely used in various fields for its rich polysaccharides, proteins, amino acids, vitamins, active enzymes and trace beneficial elements to human body. However, the main active ingredient aloin is also an allergenic ingredient, which even may cause a severe allergic reaction In this study, infrared spectroscopy, Raman spectroscopy applied to the structural characterization of the aloin Density functional theory (DFT) is applied to the theoretical calculations using the B3LYP/6-31G (d) basis set vibration, which was helpful to understand the aloin molecular vibrational frequency. By comparing we choose the optimal experimental condition for water as solvent under alkaline conditions, the detection limit of the Aloin can reach a level of 5 ppm, which can be considered the theoretical basis for rapid detection of aloin content.

  16. Isolation and structural characterization of chondroitin sulfate from bony fishes. (United States)

    Maccari, Francesca; Galeotti, Fabio; Volpi, Nicola


    Chondroitin sulfate (CS) was purified from the bones of common fishes, monkfish, cod, spiny dogfish, salmon and tuna, and characterized in an effort to find alternative sources and new peculiar structures of this complex biomacromolecule utilized in the pharmaceutical and nutraceutical industry. Quantitative analyses yielded a CS content ranging from 0.011% for cod up to 0.34% for monkfish. The disaccharide pattern showed the presence of nonsulfated disaccharide, monosulfated species ΔDi6s and ΔDi4s, and disulfated disaccharides in different percentages. The disulfated species ΔDi2,6dis was present in all CS extracts in a range of 1.3-10.5%. The presence of these disulfated disaccharides may be a useful marker for the marine origin of CS. The newly identified sources would certainly enable the production of CS with unique disaccharide composition and properties. Copyright © 2015 Elsevier Ltd. All rights reserved.

  17. Characterization of photonic structures using visible and infrared polarimetry

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    Kral Z.


    Full Text Available Photonic Crystals are materials with a spatial periodic variation of the refractive index on the wavelength scale. This confers these materials interesting photonic properties such as the existence of photonic bands and forbidden photon frequency ranges, the photonic band gaps. Among their applications it is worth mentioning the achievement of low-threshold lasers and high-Q resonant cavities. A particular case of the Photonic Crystals is well-known and widely studied since a long time: the periodic thin film coatings. The characterization of thin film coatings is a classical field of study with a very well established knowledge. However, characterization of 2D and 3D photonic crystals needs to be studied in detail as it poses new problems that have to be solved. In this sense, Polarimetry is a specially suited tool given their inherent anisotropy: photonic bands depend strongly on the propagation direction and on polarization. In this work we show how photonic crystal structures can be characterized using polarimetry equipment. We compare the numerical modeling of the interaction of the light polarization with the photonic crystal with the polarimetry measurements. With the S-Matrix formalism, the Mueller matrix of a Photonic Crystal for a given wavelength, angle of incidence and propagation direction can be obtained. We will show that useful information from polarimetry (and also from spectrometry can be obtained when multivariate spectra are considered. We will also compare the simulation results with Polarimetry measurements on different kinds of samples: macroporous silicon photonic crystals in the near-IR range and Laser-Interference-Lithography nanostructured photoresist.

  18. Structural Characterization of Myotoxic Ecarpholin S From Echis carinatus Venom

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, X.; Tan, T; Valiyaveettil, S; Go, M; Kini, R; Velazquez-Campoy, A; Sivaraman, J


    Phospholipase A2 (PLA2), a common toxic component of snake venom, has been implicated in various pharmacological effects. Ecarpholin S, isolated from the venom of the snake Echis carinatus sochureki, is a phospholipase A2 (PLA2) belonging to the Ser49-PLA2 subgroup. It has been characterized as having low enzymatic but potent myotoxic activities. The crystal structures of native ecarpholin S and its complexes with lauric acid, and its inhibitor suramin, were elucidated. This is the first report of the structure of a member of the Ser49-PLA2 subgroup. We also examined interactions of ecarpholin S with phosphatidylglycerol and lauric acid, using surface plasmon resonance, and of suramin with isothermal titration calorimetry. Most Ca2+-dependent PLA2 enzymes have Asp in position 49, which plays a crucial role in Ca2+ binding. The three-dimensional structure of ecarpholin S reveals a unique conformation of the Ca2+-binding loop that is not favorable for Ca2+ coordination. Furthermore, the endogenously bound fatty acid (lauric acid) in the hydrophobic channel may also interrupt the catalytic cycle. These two observations may account for the low enzymatic activity of ecarpholin S, despite full retention of the catalytic machinery. These observations may also be applicable to other non-Asp49-PLA2 enzymes. The interaction of suramin in its complex with ecarpholin S is quite different from that reported for the Lys49-PLA2/suramin complex, where the interfacial recognition face (i-face), C-terminal region, and N-terminal region of ecarpholin S play important roles. This study provides significant structural and functional insights into the myotoxic activity of ecarpholin S and, in general, of non-Asp49-PLA2 enzymes.

  19. Structural characterization of the interaction of human lactoferrin with calmodulin.

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    Jessica L Gifford

    Full Text Available Lactoferrin (Lf is an 80 kDa, iron (Fe(3+-binding immunoregulatory glycoprotein secreted into most exocrine fluids, found in high concentrations in colostrum and milk, and released from neutrophil secondary granules at sites of infection and inflammation. In a number of cell types, Lf is internalized through receptor-mediated endocytosis and targeted to the nucleus where it has been demonstrated to act as a transcriptional trans-activator. Here we characterize human Lf's interaction with calmodulin (CaM, a ubiquitous, 17 kDa regulatory calcium (Ca(2+-binding protein localized in the cytoplasm and nucleus of activated cells. Due to the size of this intermolecular complex (∼100 kDa, TROSY-based NMR techniques were employed to structurally characterize Ca(2+-CaM when bound to intact apo-Lf. Both CaM's backbone amides and the ε-methyl group of key methionine residues were used as probes in chemical shift perturbation and cross-saturation experiments to define the binding interface of apo-Lf on Ca(2+-CaM. Unlike the collapsed conformation through which Ca(2+-CaM binds the CaM-binding domains of its classical targets, Ca(2+-CaM assumes an extended structure when bound to apo-Lf. Apo-Lf appears to interact predominantly with the C-terminal lobe of Ca(2+-CaM, enabling the N-terminal lobe to potentially bind another target. Our use of intact apo-Lf has made possible the identification of a secondary interaction interface, removed from CaM's primary binding domain. Secondary interfaces play a key role in the target's response to CaM binding, highlighting the importance of studying intact complexes. This solution-based approach can be applied to study other regulatory calcium-binding EF-hand proteins in intact intermolecular complexes.

  20. Structural characterization of genomes by large scale sequence-structure threading

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    Cherkasov Artem


    Full Text Available Abstract Background Using sequence-structure threading we have conducted structural characterization of complete proteomes of 37 archaeal, bacterial and eukaryotic organisms (including worm, fly, mouse and human totaling 167,888 genes. Results The reported data represent first rather general evaluation of performance of full sequence-structure threading on multiple genomes providing opportunity to evaluate its general applicability for large scale studies. According to the estimated results the sequence-structure threading has assigned protein folds to more then 60% of eukaryotic, 68% of archaeal and 70% of bacterial proteomes. The repertoires of protein classes, architectures, topologies and homologous superfamilies (according to the CATH 2.4 classification have been established for distant organisms and superkingdoms. It has been found that the average abundance of CATH classes decreases from "alpha and beta" to "mainly beta", followed by "mainly alpha" and "few secondary structures". 3-Layer (aba Sandwich has been characterized as the most abundant protein architecture and Rossman fold as the most common topology. Conclusion The analysis of genomic occurrences of CATH 2.4 protein homologous superfamilies and topologies has revealed the power-law character of their distributions. The corresponding double logarithmic "frequency – genomic occurrence" dependences characteristic of scale-free systems have been established for individual organisms and for three superkingdoms. Supplementary materials to this works are available at 1.

  1. Characterizing 3D Vegetation Structure from Space: Mission Requirements (United States)

    Hall, Forrest G.; Bergen, Kathleen; Blair, James B.; Dubayah, Ralph; Houghton, Richard; Hurtt, George; Kellndorfer, Josef; Lefsky, Michael; Ranson, Jon; Saatchi, Sasan; hide


    Human and natural forces are rapidly modifying the global distribution and structure of terrestrial ecosystems on which all of life depends, altering the global carbon cycle, affecting our climate now and for the foreseeable future, causing steep reductions in species diversity, and endangering Earth s sustainability. To understand changes and trends in terrestrial ecosystems and their functioning as carbon sources and sinks, and to characterize the impact of their changes on climate, habitat and biodiversity, new space assets are urgently needed to produce high spatial resolution global maps of the three-dimensional (3D) structure of vegetation, its biomass above ground, the carbon stored within and the implications for atmospheric green house gas concentrations and climate. These needs were articulated in a 2007 National Research Council (NRC) report (NRC, 2007) recommending a new satellite mission, DESDynI, carrying an L-band Polarized Synthetic Aperture Radar (Pol-SAR) and a multi-beam lidar (Light RAnging And Detection) operating at 1064 nm. The objectives of this paper are to articulate the importance of these new, multi-year, 3D vegetation structure and biomass measurements, to briefly review the feasibility of radar and lidar remote sensing technology to meet these requirements, to define the data products and measurement requirements, and to consider implications of mission durations. The paper addresses these objectives by synthesizing research results and other input from a broad community of terrestrial ecology, carbon cycle, and remote sensing scientists and working groups. We conclude that: (1) current global biomass and 3-D vegetation structure information is unsuitable for both science and management and policy. The only existing global datasets of biomass are approximations based on combining land cover type and representative carbon values, instead of measurements of actual biomass. Current measurement attempts based on radar and multispectral

  2. Production and Structural Characterization of Lactobacillus helveticus Derived Biosurfactant

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    Deepansh Sharma


    Full Text Available A probiotic strain of lactobacilli was isolated from traditional soft Churpi cheese of Yak milk and found positive for biosurfactant production. Lactobacilli reduced the surface tension of phosphate buffer saline (PBS from 72.0 to 39.5 mNm−1 pH 7.2 and its critical micelle concentration (CMC was found to be 2.5 mg mL−1. Low cost production of Lactobacilli derived biosurfactant was carried out at lab scale fermenter which yields 0.8 mg mL−1 biosurfactant. The biosurfactant was found least phytotoxic and cytotoxic as compared to the rhamnolipid and sodium dodecyl sulphate (SDS at different concentration. Structural attributes of biosurfactant were determined by FTIR, NMR (1H and 13C, UPLC-MS, and fatty acid analysis by GCMS which confirmed the presence of glycolipid type of biosurfactant closely similar to xylolipids. Biosurfactant is mainly constituted by lipid and sugar fractions. The present study outcomes provide valuable information on structural characterization of the biosurfactant produced by L. helveticus MRTL91. These findings are encouraging for the application of Lactobacilli derived biosurfactant as nontoxic surface active agents in the emerging field of biomedical applications.

  3. Synthesis, structure characterization, and enzyme screening of clenbuterol glucuronides. (United States)

    Alonen, Anna; Gartman, Minna; Aitio, Olli; Finel, Moshe; Yli-Kauhaluoma, Jari; Kostiainen, Risto


    Two clenbuterol O-glucuronide diastereomers were synthesized by the Koenigs-Knorr reaction. Structures and glucuronidation sites of the glucuronides were characterized by tandem mass spectrometry and nuclear magnetic resonance spectroscopy. The two diastereomers were used as standard compounds in studies of stereoselective glucuronidation of clenbuterol with liver microsomes from different species and with 15 human recombinant UDP-glucuronosyltransferases. In this study, chemical and enzymatic reactions produced only O-glucuronides of clenbuterol, although on the basis of the chemical structure of the aglycone, both O- and N-glucuronides of clenbuterol could be formed. Differences in the production of diastereomers of clenbuterol glucuronides were observed among liver microsomes from the various animals. Dog and bovine liver microsomes were significantly active, and also stereoselective, each producing only one but a different diastereomer. Liver microsomes from rabbit and rat were also rather actively glucuronidating clenbuterol, but human, pig, and moose liver microsomes produced only minor amounts of glucuronides. Human liver microsomes produced only one clenbuterol glucuronide diastereomer, and the same was true of the human UDP-glucuronosyltransferases that were active (formation of glucuronide: 1A9 > 1A10 > 1A7). The marked differences in the stereoselective glucuronidation of clenbuterol show that UDP-glucuronosyltransferases in the livers of different animals do not have the same functions, activities, or distribution. This needs to be taken into account, particularly in toxicology testing.

  4. Characterization and Degradation of Masonry Mortar in Historic Brick Structures

    Directory of Open Access Journals (Sweden)

    Denis A. Brosnan


    Full Text Available This study characterized mortars from a masonry fortification in Charleston, South Carolina (USA, harbor where construction was during the period 1839–1860. This location for analysis was interesting because of the sea water impingement on the structure. The study was included as part of an overall structural assessment with restoration as an objective. The mortars were found to be cement, lime, and sand mixtures in proportions similar to ones expected from the historic literature, that is, one part binder to two parts of sand. The binder was found to be American natural cement, a substance analogous to the European Roman cement. The results suggest that the thermal history of the cement during manufacturing affected setting rate explaining why the cements were considered as variable during the mid-to-late 1800s. Fine pores were found in mortars exposed to sea water resulting from corrosion. Contemporary natural cement was shown to release calcium in aqueous solution. While this release of calcium is necessary for setting in natural and Portland cements, excessive calcium solution, as exacerbated by sea water contact and repointing with Portland cement mortars, was shown to result in brick scaling or decay through cryptoflorescence.

  5. Nanostructured Polypyrrole Powder: A Structural and Morphological Characterization

    Directory of Open Access Journals (Sweden)

    Edgar A. Sanches


    Full Text Available Polypyrrole (PPY powder was chemically synthesized using ferric chloride (FeCl3 and characterized by X-ray diffraction (XRD, Le Bail Method, Fourier Transform Infrared Spectrometry (FTIR, and Scanning Electron Microscopy (SEM. XRD pattern showed a broad scattering of a semicrystalline structure composed of main broad peaks centered at 2θ = 11.4°, 22.1°, and 43.3°. Crystallinity percentage was estimated by the ratio between the sums of the peak areas to the area of amorphous broad halo due to the amorphous phase and showed that PPY has around 20 (1%. FTIR analysis allowed assigning characteristic absorption bands in the structure of PPY. SEM showed micrometric particles of varying sizes with morphologies similar to cauliflower. Crystal data (monoclinic, space group P 21/c, a=7.1499 (2 Å, b=13.9470 (2 Å, c=17.3316 (2 Å, α=90 Å, β=61.5640 (2 Å and γ=90 Å were obtained using the FullProf package program under the conditions of the method proposed by Le Bail. Molecular relaxation was performed using the density functional theory (DFT and suggests that tetramer polymer chains are arranged along the “c” direction. Average crystallite size was found in the range of 20 (1 Å. A value of 9.33 × 10−9 S/cm was found for PPY conductivity.

  6. Mechanochemically synthesized cobalt monoselenide: structural characterization and optical properties (United States)

    Achimovičová, Marcela; Daneu, Nina; Dutková, Erika; Zorkovská, Anna


    Chalcogenide semiconductor cobalt monoselenide, CoSe, was prepared from metallic cobalt and selenium powders in stoichiometric ratio by simple and fast mechanochemical synthesis after 120 min of milling in a planetary ball mill Pulverisette 6 (Fritsch, Germany) in an argon atmosphere. Crystal structure and morphology of the product were characterized by X-ray diffraction, specific surface area measurements, and transmission electron microscopy. X-ray diffraction analysis confirmed the hexagonal crystal structure of the product-CoSe (freboldite) with the average size of the crystallites 26 nm. Transmission electron microscopy analysis has revealed that CoSe nanostructures are composed of agglomerated and randomly oriented nanoparticles. The optical properties were studied using UV-Vis and photoluminescence spectroscopy. Mechanochemically synthesized CoSe nanostructures showed higher absorption in whole UV-Vis optical region and the determined band-gap energy 1.70 eV is blue-shifted relative to the bulk CoSe. Both UV-Vis and photoluminescence spectra indicate quantum size effect of CoSe nanocrystals.

  7. Characterization of strained semiconductor structures using transmission electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Oezdoel, Vasfi Burak


    Today's state-of-the-art semiconductor electronic devices utilize the charge transport within very small volumes of the active device regions. The structural, chemical and optical material properties in these small dimensions can critically affect the performance of these devices. The present thesis is focused on the nanometer scale characterization of the strain state in semiconductor structures using transmission electron microscopy (TEM). Although high-resolution TEM has shown to provide the required accuracy at the nanometer scale, optimization of imaging conditions is necessary for accurate strain measurements. An alternative HRTEM method based on strain mapping on complex-valued exit face wave functions is developed to reduce the artifacts arising from objective lens aberrations. However, a much larger field of view is crucial for mapping strain in the active regions of complex structures like latest generation metal-oxide-semiconductor field-effect transistors (MOSFETs). To overcome this, a complementary approach based on electron holography is proposed. The technique relies on the reconstruction of the phase shifts in the diffracted electron beams from a focal series of dark-field images using recently developed exit-face wave function reconstruction algorithm. Combining high spatial resolution, better than 1 nm, with a field of view of about 1 {mu}m in each dimension, simultaneous strain measurements on the array of MOSFETs are possible. Owing to the much lower electron doses used in holography experiments when compared to conventional quantitative methods, the proposed approach allows to map compositional distribution in electron beam sensitive materials such as InGaN heterostructures without alteration of the original morphology and chemical composition. Moreover, dark-field holography experiments can be performed on thicker specimens than the ones required for high-resolution TEM, which in turn reduces the thin foil relaxation. (orig.)

  8. Characterization of Polyimide Foams for Ultra-Lightweight Space Structures (United States)

    Meador, Michael (Technical Monitor); Hillman, Keithan; Veazie, David R.


    Ultra-lightweight materials have played a significant role in nearly every area of human activity ranging from magnetic tapes and artificial organs to atmospheric balloons and space inflatables. The application range of ultra-lightweight materials in past decades has expanded dramatically due to their unsurpassed efficiency in terms of low weight and high compliance properties. A new generation of ultra-lightweight materials involving advanced polymeric materials, such as TEEK (TM) polyimide foams, is beginning to emerge to produce novel performance from ultra-lightweight systems for space applications. As a result, they require that special conditions be fulfilled to ensure adequate structural performance, shape retention, and thermal stability. It is therefore important and essential to develop methodologies for predicting the complex properties of ultra-lightweight foams. To support NASA programs such as the Reusable Launch Vehicle (RLV), Clark Atlanta University, along with SORDAL, Inc., has initiated projects for commercial process development of polyimide foams for the proposed cryogenic tank integrated structure (see figure 1). Fabrication and characterization of high temperature, advanced aerospace-grade polyimide foams and filled foam sandwich composites for specified lifetimes in NASA space applications, as well as quantifying the lifetime of components, are immensely attractive goals. In order to improve the development, durability, safety, and life cycle performance of ultra-lightweight polymeric foams, test methods for the properties are constant concerns in terms of timeliness, reliability, and cost. A major challenge is to identify the mechanisms of failures (i.e., core failure, interfacial debonding, and crack development) that are reflected in the measured properties. The long-term goal of the this research is to develop the tools and capabilities necessary to successfully engineer ultra-lightweight polymeric foams. The desire is to reduce density

  9. Structural characterization of self-assembled multifunctional binary nanoparticle superlattices. (United States)

    Shevchenko, Elena V; Talapin, Dmitri V; Murray, Christopher B; O'Brien, Stephen


    Nanocrystals of different size and functionality (e.g., noble metals, semiconductors, oxides, magnetic alloys) can be induced to self-assemble into ordered binary superlattices (also known as opals or colloidal crystals), retaining the size tunable properties of their constituents. We have built a variety of binary superlattices from monodisperse PbS, PbSe, CoPt3, Fe2O3, Au, Ag, and Pd nanocrystals, mixing and matching these nanoscale building blocks to yield multifunctional nanocomposites (metamaterials). Superlattices with AB, AB2, AB3, AB4, AB5, AB6, and AB13 stoichiometry with cubic, hexagonal, tetragonal, and orthorhombic symmetries have been identified. Assemblies with the same stoichiometry can be produced in several polymorphous forms by tailoring the particle size and deposition conditions. We have identified arrays isostructural with NaCl, CuAu, AlB2, MgZn2, MgNi2, Cu3Au, Fe4C, CaCu5, CaB6, NaZn13, and cub-AB13 compounds emphasizing the parallels between nanoparticle assembly and atomic scale crystal growth and providing confidence that many more structures will follow. Recently, we have demonstrated that electrical charges on sterically stabilized nanoparticles in addition to such parameters as particle size ratio and their concentrations can provide the formation of a much broader pallet of binary nanoparticle superlattices as compared with the limited number of possible superlattices formed by hard noninteracting spheres. In this contribution, we demonstrate a large variety of different binary superlattices, provide their detailed structural characterization, and discuss the role of energetic and kinetic factors in the cocrystallization process. We found that Coulomb, van der Waals, charge-dipole, dipole-dipole, and other interactions can contribute equally to cocrystallization, allowing superlattice formation to be dependent on a number of tunable parameters. We present binary superlattices as a new class of materials with a potentially unlimited

  10. [Separation and purification and structural characterization of baicalein]. (United States)

    Li, Yun-xia; Suo, Quan-ling; He, Wen-zhi; Li, Chun-ping; Huang, Yan-chun


    The root of scutellaria baicalensis georgi that contains a variety of flavonoids is a very old and well-known drug in traditional Chinese medicine, which is widely used for treatment of bronchitis, tumors and inflammatory diseases. The baicalein is the main active component from traditional Chinese medicine-scutellaria baicalensis georgi. It is a very significance research work that the baicalein was separated and purified, and its composition and molecular structure are analyzed and determined for the pharmacology study of Chinese medicine-scutellaria baicalensis georgi. The main works in this paper are as follows. Powdered roots (100 g) were extracted with methanol by three times, each time for 48 hours. The crude extracts were purified by polyamide column chromatography and CH3Cl-C2H5OH gradient desorption. A short yellow prismatic crystal was acquired by recrystallizing technique and its composition and molecular structure were characterized by color reactions and spectral analysis methods as FTIR, UV-Vis, MS and 1H NMR, 13C-NMR. The FTIR spectrum appears the absorption bands for hydroxyls, pyrone carbonyl, aromatic C=C bond and singly substituted phenyl. The characteristic absorption peaks and the vibration modes in FTIR spectrum were identified as corresponding groups. The UV-Vis spectrum in methanol solution and the mix solution of methanol with 5 diagnostic reagents, NaOMe, NaOAc, NaOAc/H3BO3, AlCl3, AlCl3/HCl, respectively indicate that the yellow prismatic crystal is flavone with 5-hydroxyl, 4-carbonyl and 5,6,7- or 5,7,8-trihydroxyls on ring A. The structure of the crystal was characterized by three different MS. The results of FAB-, ESI- and EI-MS show that it is not a flavone glocuside but the flavone with three phenyl hydroxyls on ring A, and no OH group and other substituted groups on ring B. The molecular ion and fragment ions are identified by MS, which include such as m/z 270 M+, m/z 242 [M-CO]+, m/z 168 A, m/z 140 [A1-CO]+, m/z 105 B, m/z 102 B

  11. Molecular and electronic structures of the members of the electron transfer series [Mn(bpy)3]n (n = 2+, 1+, 0, 1-) and [Mn(tpy)2]m (m = 4+, 3+, 2+, 1+, 0). An experimental and density functional theory study. (United States)

    Wang, Mei; England, Jason; Weyhermüller, Thomas; Wieghardt, Karl


    The members of the electron transfer series [Mn(bpy)3](n) (n = 2+, 1+, 0, 1-) and [Mn(tpy)2](m) (m = 2+, 1+, 0) have been investigated using a combination of magnetochemistry, electrochemistry, and UV-vis-NIR spectroscopy; and X-ray crystal structures of [Mn(II)((Me)bpy(•))2((Me)bpy(0))](0), [Li(THF)4][Mn(II)(bpy(•))3], and [Mn(II)(tpy(•))2](0) have been obtained (bpy = 2,2'-bipyridine; (Me)bpy = 4,4'-dimethyl-2,2'-bipyridine; tpy = 2,2':6,2″-terpyridine; THF = tetrahydrofuran). It is the first time that the latter complex has been isolated and characterized. Through these studies, the electronic structures of each member of both series of complexes have been elucidated, and their molecular and electronic structures further corroborated by broken symmetry (BS) density functional theoretical (DFT) calculations. It is shown that all one-electron reductions that comprise the aforementioned redox series are ligand-based. Hence, all species contain a central high-spin Mn(II) ion (SMn = 5/2). In contrast, the analogous series of Tc(II) and Re(II) complexes possess low-spin electron configurations.

  12. Characterization of structural relaxation in inorganic glasses using length dilatometry (United States)

    Koontz, Erick

    The processes that govern how a glass relaxes towards its thermodynamic quasi-equilibrium state are major factors in understanding glass behavior near the glass transition region, as characterized by the glass transition temperature (Tg). Intrinsic glass properties such as specific volume, enthalpy, entropy, density, etc. are used to map the behavior of the glass network below in and near the transition region. The question of whether a true thermodynamic second order phase transition takes place in the glass transition region is another pending question. Linking viscosity behavior to entropy, or viewing the glass configuration as an energy landscape are just a couple of the most prevalent methods used for attempting to understand the glass transition. The structural relaxation behavior of inorganic glasses is important for more than scientific reasons, many commercial glass processing operations including glass melting and certain forms of optical fabrication include significant time spent in the glass transition region. For this reason knowledge of structural relaxation processes can, at a minimum, provide information for annealing duration of melt-quenched glasses. The development of a predictive model for annealing time prescription has the potential to save glass manufacturers significant time and money as well as increasing volume throughput. In optical hot forming processes such as precision glass molding, molded optical components can significantly change in shape upon cooling through the glass transition. This change in shape is not scientifically predictable as of yet though manufacturers typically use empirical rules developed in house. The classification of glass behavior in the glass transition region would allow molds to be accurately designed and save money for the producers. The work discussed in this dissertation is comprised of the development of a dilatometric measurement and characterization method of structural relaxation. The measurement and

  13. Structural characterization of chondroitin sulfate from sturgeon bone. (United States)

    Maccari, Francesca; Ferrarini, Fabrizio; Volpi, Nicola


    Chondroitin sulfate (CS) was purified for the first time from the bones of sturgeon and analyzed to evaluate its structure and properties. A single polysaccharide was extracted from sturgeon bone in a concentration of 0.28-0.34% for dry tissue and characterized as CS. By means of specific chondroitinases and HPLC separation of generated unsaturated repeating disaccharides, this polymer was found to be composed of approximately 55% of disaccharide monosulfated in position 6 of the GalNAc, approximately 38% of disaccharide monosulfated in position 4 of the GalNAc, and approximately 7% of nonsulfated disaccharide. The charge density was 0.93 and the ratio of 4:6 sulfated residues was equal to 0.69, a value confirmed by (13)C NMR experiments. Chondroitinase B confirmed that the purified sturgeon CS contained mainly GlcA (>99.5%) as uronic acid. PAGE analysis showed a CS having a high molecular mass with an average value of 39,880 according to HPSEC values producing a weight average molecular weight (Mw) of 37,500. On the basis of the data collected, it is reasonable to assume that CS isolated from sturgeon bone might be potentially useful for scientific and pharmacological applications, making this bony fish, which is generally discarded after ovary collection, a useful source of this polymer. Finally, this newly identified source of CS would enable the production of this macromolecule having a particular repeating disaccharide composition, structure, and biological properties. Copyright (c) 2010 Elsevier Ltd. All rights reserved.

  14. Magnetic structures synthesized by controlled oxidative etching: Structural characterization and magnetic behavior

    Directory of Open Access Journals (Sweden)

    Álvaro de Jesús Ruíz-Baltazar

    Full Text Available A facile strategy for the fabrication Fe3O4 nanostructures at room temperature and with well-defined morphology is proposed. In this methodology, the iron precursors were reduced by sodium borohydride. Subsequently an oxidative etching process promotes the formation of Fe2O3 nanostructures. Magnetic measurements revealed a well-defined superparamagnetic behavior for the material. The Zero-Field-Cooled (ZFC and Field-Cooled (FC magnetization curves reveals that critical and blocking temperature were 24 and 350 °C respectively. The Fe3O4 nanostructures were characterized using aberration-corrected (Cs scanning transmission electron microscopy (STEM and energy dispersive spectroscopy (EDS. Additionally, Raman spectra support the Fe3O4 presence and corroborate the efficiency of the synthesis process to obtain magnetite. Keywords: Chemical synthesis, Fe3O4 nanoparticles, Structural characterization, Magnetic properties

  15. Structural characterization and mechanical properties of polypropylene reinforced natural fibers (United States)

    Karim, M. A. A.; Zaman, I.; Rozlan, S. A. M.; Berhanuddin, N. I. C.; Manshoor, B.; Mustapha, M. S.; Khalid, A.; Chan, S. W.


    Recently the development of natural fiber composite instead of synthetics fiber has lead to eco-friendly product manufacturing to meet various applications in the field of automotive, construction and manufacturing. The use of natural fibers offer an alternative to the reinforcing fibers because of their good mechanical properties, low density, renewability, and biodegradability. In this present research, the effects of maleic anhydride polypropylene (MAPP) on the mechanical properties and material characterization behaviour of kenaf fiber and coir fiber reinforced polypropylene were investigated. Different fractions of composites with 10wt%, 20wt% and 30wt% fiber content were prepared by using brabender mixer at 190°C. The 3wt% MAPP was added during the mixing. The composites were subsequently molded with injection molding to prepare the test specimens. The mechanical properties of the samples were investigated according to ISO 527 to determine the tensile strength and modulus. These results were also confirmed by the SEM machine observations of fracture surface of composites and FTIR analysis of the chemical structure. As the results, the presence of MAPP helps increasing the mechanical properties of both fibers and 30wt% kenaf fiber with 3wt% MAPP gives the best result compare to others.

  16. Structural and functional characterization of the zebrafish lamin B receptor. (United States)

    Schild-Prüfert, Kristina; Giegerich, Marieke; Schäfer, Matthias; Winkler, Christoph; Krohne, Georg


    The lamin B receptor (LBR) is an integral membrane protein of the inner nuclear membrane that is interacting with B-type lamins, chromatin and DNA. The complete loss of the protein in mouse mutants causes a reduced viability of embryos, and viable animals develop abnormalities of the skeleton. Here, we present the molecular characterization of the zebrafish LBR (zLBR) gene and the functional analysis of LBR during zebrafish embryogenesis. We found that the coding region of the LBR mRNA of zebrafish as well as of mammals is contained in 13 exons. At the protein level, human and zebrafish LBR exhibit a high sequence identity (57% and higher) in 8 of the 13 exons. Knockdown of zLBR by microinjection of 0.5-1.0 mM morpholino antisense oligonucleotides (MO) into 1- to 2-cell stage embryos reduced the amount of endogenous zLBR protein to approximately 10-20%. The viability of MO-injected embryos within 24 h was reduced to 70-77%. Surviving 1-day-old embryos exhibited morphological alterations including reduced growth of head structures, retardation of tail growth and a bent backbone and tail. Expression analysis of the transcription factors no tail (ntl) and goosecoid (gsc) by in situ hybridization suggests that these malformations are caused by altered cell migration during gastrulation. Our data indicate that the LBR of zebrafish and mammals are both required for correct development.

  17. Biochemical and Structural Characterization of Enolase from Chloroflexus aurantiacus: Evidence for a Thermophilic Origin

    National Research Council Canada - National Science Library

    Zadvornyy, Oleg A; Boyd, Eric S; Posewitz, Matthew C; Zorin, Nikolay A; Peters, John W


    .... Here, we report the purification and biochemical and structural characterization of enolase from Chloroflexus aurantiacus, a thermophilic anoxygenic phototroph affiliated with the green non-sulfur bacteria...

  18. Characterization of the passivation processes for PIN structures

    Energy Technology Data Exchange (ETDEWEB)

    Avila Garcia, Alejandro; Reyes Barranca, Mario Alfredo [Instituto Politecnico Nacional, Mexico, D.F (Mexico); Zarate Corona, Oscar [Universidad Autonoma de Puebla, Puebla (Mexico)


    Result on the evaluation of PIN structures made on crystalline silicon, processed in our laboratory, which underwent several gettering treatments are reported. Structures were evaluated through the measurement of lifetime {tau} and I-V characteristic. Also, deep levels due to defects were characterized; the activation energy (E{sub c} -E{sub t}), capture cross section {sigma} and relative concentration (N{sub t} / N{sub d}) were obtained. Techniques used in the characterization were Output Circuit Voltage Decay (OCVD), Current-Voltage measurements (I-V) and Deep Level Transient Spectroscopy (DLTS), respectively. These measurements show variations in the parameters, as a result of the gettering techniques applied. The best results were achieved for two types of samples: the first having high phosphorus concentration, no backside damage and annealed at 850 Celsius degrees without HCI atmosphere; the second having low phosphorus concentration, no backside damage and annealed at 850 Celsius degrees without HCI atmosphere. For these samples, the minority carrier lifetime was near 3{upsilon}s, the I-V characteristics imply that conductivity modulation takes place within the intrinsic region even for low voltages, as in commercial diodes. Two defects were observed to remain after the gettering processes: one is related to the phosphorus-vacant pair and the other to the divacancy. Concentrations could be decreased from {approx}4 x 10{sup 1}1cm{sup -3} down to 3 x 10{sup -9} cm{sup -3} for the first and down to 2 x 10{sup 1}0 cm{sup -3} for the second one. [Spanish] Se reportan resultados de la evaluacion de estructuras PIN en silicio procesadas en nuestro laboratorio, las cuales fueron sometidas a diversos tratamientos de gettering. Las estructuras fueron evaluadas a traves de la medicion de tiempo de vida {tau} y la caracteristica I-V. Se caracterizaron tambien los defectos que introducen niveles profundos en la region activa del dispositivo, obteniendo energia de

  19. Structural level characterization of base oils using advanced analytical techniques

    KAUST Repository

    Hourani, Nadim


    Base oils, blended for finished lubricant formulations, are classified by the American Petroleum Institute into five groups, viz., groups I-V. Groups I-III consist of petroleum based hydrocarbons whereas groups IV and V are made of synthetic polymers. In the present study, five base oil samples belonging to groups I and III were extensively characterized using high performance liquid chromatography (HPLC), comprehensive two-dimensional gas chromatography (GC×GC), and Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) equipped with atmospheric pressure chemical ionization (APCI) and atmospheric pressure photoionization (APPI) sources. First, the capabilities and limitations of each analytical technique were evaluated, and then the availed information was combined to reveal compositional details on the base oil samples studied. HPLC showed the overwhelming presence of saturated over aromatic compounds in all five base oils. A similar trend was further corroborated using GC×GC, which yielded semiquantitative information on the compound classes present in the samples and provided further details on the carbon number distributions within these classes. In addition to chromatography methods, FT-ICR MS supplemented the compositional information on the base oil samples by resolving the aromatics compounds into alkyl- and naphtheno-subtituted families. APCI proved more effective for the ionization of the highly saturated base oil components compared to APPI. Furthermore, for the detailed information on hydrocarbon molecules FT-ICR MS revealed the presence of saturated and aromatic sulfur species in all base oil samples. The results presented herein offer a unique perspective into the detailed molecular structure of base oils typically used to formulate lubricants. © 2015 American Chemical Society.

  20. Synthesis, structure, and spectroscopic characterization of three uranyl phosphates with unique structural units (United States)

    Wylie, Ernest M.; Dawes, Colleen M.; Burns, Peter C.


    Single crystals of Zn4(OH)2[(UO2)(PO4)2(OH)2(H2O)] (UZnP), Cs[(UO2)(HPO4)NO3] (UCsP), and In3[(UO2)2(PO4)4OH(H2O)6].2H2O (UInP) were obtained from hydrothermal reactions and have been structurally and chemically characterized. UZnP crystallizes in space group Pbcn, a=8.8817(7), b=6.6109(5), c=19.569(1) Å; UCsP crystallizes in P-1, a=7.015(2), b=7.441(1), c=9.393(2) Å, α=72.974(2), β=74.261(2), γ=79.498(2); and UInP crystallizes in P-1, a=7.9856(5), b=9.159(1), c=9.2398(6) Å α=101.289(1), β=114.642(1), γ=99.203(2). The U6+ cations are present as (UO2)2+ uranyl ions coordinated by five O atoms to give pentagonal bipyramids. The structural unit in UZnP is a finite cluster containing a uranyl pentagonal bipyramid that shares corners with two phosphate tetrahedra. The structural unit in UCsP is composed of uranyl pentagonal bipyramids with one chelating nitrate group that are linked into chains by three bridging hydrogen phosphate tetrahedra. In UInP, the structural unit contains pairs of edge-sharing uranyl pentagonal bipyramids with two chelating phosphate tetrahedra that are linked into chains through two bridging phosphate tetrahedra. Indium octahedra link these uranyl phosphate chains into a 3-dimensional framework. All three compounds exhibit unique structural units that deviate from the typical layered structures observed in uranyl phosphate solid-state chemistry.

  1. Synthesis, crystal structure and characterization of new biologically ...

    Indian Academy of Sciences (India)

    characterized by FT-IR, electronic, EPR spectroscopic and magnetic methods. ... complexes.15–17. In this paper we report the synthesis, the physico- chemical characterization of two new Cu(II) complexes with N-substituted sulfonamides and we demonstrate .... agent of copper(I), neocuproine (36 μM), along with the.

  2. Structural characterization by Nuclear Magnetic Resonance of ozonized triolein

    Directory of Open Access Journals (Sweden)

    F. Díaz, Maritza


    Full Text Available In the present study ozonized triolein with 739 mmolequiv/ kg peroxide index is characterized by NMR.The triolein and ozonized triolein show very similar 1H NMR spectra except for the resonances at δ 9.74 ppm, which correspond to aldehydic protons and δ 5.14 ppm (ozonides methylic protons. Other new signal assignments are based on the connectivities provided by the proton scalar coupling constants δ 2.41 ppm (methylenic group allylic to aldehydic protons and ozonides methynic protons and δ 1.67 ppm (methylenic protons in position with respect to ozonides methylic protons. From the 13C and 1H-13C spectrum of the ozonized triolein, the presence of ozonides was confirmed by the signals δ 104.2 and 104.3 ppm, respectively. Other new signals in δ 43.9 ppm confirm the presence of methylenic carbon ozonides. From the structural elucidation of ozonated triglycerides, relevant chemical information about ozonated vegetable oil can be found .En el presente estudio ha sido caracterizada por RMN la trioleina ozonizada con índice de peróxidos de 739 mmolequiv/ kg. La trioleina y la trioleina ozonizada muestran espectros muy similares exceptuando los valores de las resonancias δ 9,74 ppm de los protones aldehídicos, y δ 5,14 ppm (protones metínicos de los ozónidos. Otras nuevas asignaciones fueron basadas en las conectividades obtenidas por las constantes de acoplamiento escalar como δ 2,41 ppm (grupo metilénico alilico a los protones aldehídicos y protones metínicos de los ozónidos y δ 1,67 ppm (protones metilénicos en posición βcon respecto a los protones metínicos de los ozónidos. En los espectros 13C y 1H-13C de la trioleina ozonizada la presencia de ozónidos fue atribuida, respectivamente, por las señales δ 104,2 y δ 104,3 ppm. Una nueva señal en δ 43,9 ppm confirma la presencia de carbono metilénico de ozónidos. Estos resultados indican que la elucidación estructural de triglicéridos ozonizados, ofrece información qu

  3. Structural and morphological characterization of CdSe:Mn thin films

    Indian Academy of Sciences (India)

    Sarika Singh


    Jun 24, 2017 ... C. The annealed samples were subjected to morphological and structural characterization using scanning electron microscope and XRD. XRD was used for structural characterization whereas scanning electron microscope shows the surface morphology of the films. XRD spectra reveal that the grown ...

  4. Growth and structural characterization of III-V semiconductor nanowires


    Rieger, Torsten


    In this thesis, the growth and structural properties of III-V semiconductor nanowires and nanowire heterostructures are studied. These nanowires represent structures suitable for both fundamental physics and applications in electronic devices such as (tunnel) field effect transistors. The III-V nanowires are grown with molecular beam epitaxy, high κ dielectric layers are deposited conformally around the nanowires by atomic layer deposition. The morphological and structural characteristics of ...

  5. Structural characterization of bacteriophage M13 solubilization by amphiphiles

    NARCIS (Netherlands)

    Stopar, D.; Spruijt, R.B.; Wolfs, C.J.A.M.; Hemminga, M.A.


    The structural properties of bacteriophage M13 during disassembly were studied in different membrane model systems, composed of a homologue series of the detergents sodium octyl sulfate, sodium decyl sulfate, and sodium dodecyl sulfate. The structural changes during phage disruption were monitored

  6. Structural and optical characterization of thick and thin ...

    Indian Academy of Sciences (India)

    The grown polycrystalline films were characterized by micro-Raman, transmission electron microscope (TEM), spectrophotometer and atomic force microscope (AFM). The results were compared with that of a thicker diamond film grown elsewhere in a same make MWPACVD system at relatively higher power densities.

  7. Structural and surface compositional characterization of silver thin ...

    African Journals Online (AJOL)

    Silver thin films were deposited on microscope glass slides by the electroless Solution Growth Technique (SGT). The films were characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM), and x-ray photoelectron spectroscopy (XPS). The films were found to exhibit a random orientation with peak positions ...

  8. Extraction, structural and physical characterization of type I collagen ...

    African Journals Online (AJOL)

    The acid soluble collagen (ASC) and pepsin soluble collagen (PSC) were extracted from the outer skin of Sepiella inermis and further characterized partially. The yield of ASC was low (0.58% on dry weight basis); whereas the yield of PSC was comparatively more (16.23% on dry weight basis). The protein content in ASC ...

  9. Detection and characterization of near surface structures using ...

    African Journals Online (AJOL)

    A geophysical investigation was carried out at Shika, using seismic refraction method. The aim was to delineate, map and characterize the different strata of the subsurface within the flanks of a dam. In order to achieve this aim, varying geometric spreads were used with geophone spacings of 5m, 4m, 3m and 2m ...

  10. Characterization of crystalline structures in Opuntia ficus-indica


    Contreras-Padilla, Margarita; Eric M. Rivera-Muñoz; Gutiérrez-Cortez, Elsa; del López, Alicia Real; Rodríguez-García, Mario Enrique


    This research studies the crystalline compounds present in nopal (Opuntia ficus-indica) cladodes. The identification of the crystalline structures was performed using X-ray diffraction, scanning electron microscopy, mass spectrometry, and Fourier transform infrared spectroscopy. The crystalline structures identified were calcium carbonate (calcite) [CaCO3], calcium-magnesium bicarbonate [CaMg(CO3)2], magnesium oxide [MgO], calcium oxalate monohydrate [Ca(C2O4)•(H2O)], potassium peroxydiphosph...

  11. Synthesis and structural characterization of polyaniline/cobalt chloride composites

    Energy Technology Data Exchange (ETDEWEB)

    Asha, E-mail: [Department of Basic and Applied Sciences, Bhagat Phool Singh Mahilla Vishwavidyalaya, Khanpur Kalan, Sonipat-131305 (India); Goyal, Sneh Lata; Kishore, Nawal [Department of Applied Physics, Guru Jambheshwar University of Science and Technology, Hisar-125001 (India)


    Polyaniline (PANI) and PANI /cobalt chloride composites were synthesized by in situ chemical oxidative polymerization of aniline with CoCl{sub 2}.6H{sub 2}O using ammonium peroxidisulphate as an oxidant. These composites were characterized by X-ray diffraction (XRD) and Scanning electron microscopy (SEM). The XRD study reveals that both PANI and composites are amorphous. The XRD and SEM results confirm the presence of cobalt chloride in the composites.

  12. Structural and magnetic characterization of Pd nanoparticles encapsulated in apoferritin

    Energy Technology Data Exchange (ETDEWEB)

    Galvez, Natividad; Valero, Elsa; DomInguez-Vera, Jose M [Departamento Quimica Inorganica, Facultad de Ciencias, Universidad de Granada, 18071, Granada (Spain); Masciocchi, Norberto [Dipartimento di Scienze Chimiche e Ambientali and CNISM, Universita dell' Insubria, via Valleggio 11, 22100 Como (Italy); Guagliardi, Antonietta [Istituto di Cristallografia del CNR, via Amendola 122/O, 70126 Bari (Italy); Clemente-Leon, Miguel; Coronado, Eugenio, E-mail:, E-mail: [ICMol Instituto de Ciencia Molecular, Universidad de Valencia, calle catedratico Jose Beltran 2, 46980, Paterna (Spain)


    Pd nanoparticles exhibiting permanent magnetism at room temperature have been prepared within the apoferritin cavity. Pd nanoparticles in air and under an inert atmosphere were synthesized to study the influence of the aerobic and anaerobic conditions in the final magnetic properties. The surface of nanoparticles as well as the type of crystalline phase could determine the magnetic properties. X-ray powder diffraction, including Debye-function analysis, transmission electronic microscopy, and magnetization measurements have been used for characterizing the nanoparticles.

  13. Q+: characterizing the structure of young star clusters (United States)

    Jaffa, S. E.; Whitworth, A. P.; Lomax, O.


    Many young star clusters appear to be fractal, I.e. they appear to be concentrated in a nested hierarchy of clusters within clusters. We present a new algorithm for statistically analysing the distribution of stars to quantify the level of substructure. We suggest that, even at the simplest level, the internal structure of a fractal cluster requires the specification of three parameters. (I) The 3D fractal dimension, D, measures the extent to which the clusters on one level of the nested hierarchy fill the volume of their parent cluster. (II) The number of levels, L, reflects the finite ratio between the linear size of the large root-cluster at the top of the hierarchy, and the smallest leaf-clusters at the bottom of the hierarchy. (III) The volume-density scaling exponent, C = -d ln [δ n]/d ln [L] measures the factor by which the excess density, δn, in a structure of scale L, exceeds that of the background formed by larger structures; it is similar, but not exactly equivalent, to the exponent in Larson's scaling relation between density and size for molecular clouds. We describe an algorithm that can be used to constrain the values of (D,L,C) and apply this method to artificial and observed clusters. We show that this algorithm is able to reliably describe the three-dimensional structure of an artificial star cluster from the two-dimensional projection, and quantify the varied structures observed in real and simulated clusters.

  14. Characterization of crystalline structures in Opuntia ficus-indica. (United States)

    Contreras-Padilla, Margarita; Rivera-Muñoz, Eric M; Gutiérrez-Cortez, Elsa; del López, Alicia Real; Rodríguez-García, Mario Enrique


    This research studies the crystalline compounds present in nopal (Opuntia ficus-indica) cladodes. The identification of the crystalline structures was performed using X-ray diffraction, scanning electron microscopy, mass spectrometry, and Fourier transform infrared spectroscopy. The crystalline structures identified were calcium carbonate (calcite) [CaCO3], calcium-magnesium bicarbonate [CaMg(CO3)2], magnesium oxide [MgO], calcium oxalate monohydrate [Ca(C2O4)•(H2O)], potassium peroxydiphosphate [K4P2O8] and potassium chloride [KCl]. The SEM images indicate that calcite crystals grow to dipyramidal, octahedral-like, prismatic, and flower-like structures; meanwhile, calcium-magnesium bicarbonate structures show rhombohedral exfoliation and calcium oxalate monohydrate is present in a drusenoid morphology. These calcium carbonate compounds have a great importance for humans because their bioavailability. This is the first report about the identification and structural analysis of calcium carbonate and calcium-magnesium bicarbonate in nopal cladodes, as well as the presence of magnesium oxide, potassium peroxydiphosphate and potassium chloride in these plants. The significance of the study of the inorganic components of these cactus plants is related with the increasing interest in the potential use of Opuntia as a raw material of products for the food, pharmaceutical, and cosmetic industries.

  15. The Structural Characterization of Tumor Fusion Genes and Proteins. (United States)

    Wang, Dandan; Li, Daixi; Qin, Guangrong; Zhang, Wen; Ouyang, Jian; Zhang, Menghuan; Xie, Lu


    Chromosomal translocation, which generates fusion proteins in blood tumor or solid tumor, is considered as one of the major causes leading to cancer. Recent studies suggested that the disordered fragments in a fusion protein might contribute to its carcinogenicity. Here, we investigated the sequence feature near the breakpoints in the fusion partner genes, the structure features of breakpoints in fusion proteins, and the posttranslational modification preference in the fusion proteins. Results show that the breakpoints in the fusion partner genes have both sequence preference and structural preference. At the sequence level, nucleotide combination AG is preferred before the breakpoint and GG is preferred at the breakpoint. At the structural level, the breakpoints in the fusion proteins prefer to be located in the disordered regions. Further analysis suggests the phosphorylation sites at serine, threonine, and the methylation sites at arginine are enriched in disordered regions of the fusion proteins. Using EML4-ALK as an example, we further explained how the fusion protein leads to the protein disorder and contributes to its carcinogenicity. The sequence and structural features of the fusion proteins may help the scientific community to predict novel breakpoints in fusion genes and better understand the structure and function of fusion proteins.

  16. Raman scattering characterization of space solar cell structures (United States)

    Mintairov, Alexander M.; Khvostikov, V. P.; Paleeva, E. V.; Sorokina, S. V.


    A contactless method for the determination of the free-carrier density and the composition distribution across the thickness of 3-5 multi-layer solar cell structures, using the Raman scattering method, is developed. The method includes a step analysis of Raman spectra from optical phonons and phonon-plasmon modes of different layers. The method provides simultaneous measurements of the element composition and the thickness of the structure's layers together with the free-carrier density. The results of measurements of the free-carrier density composition distributions of the liquid phase epitaxy grown AlGaAs/GaAs and GaSb solar cell structures are presented and discussed.

  17. Structural characterization of coatomer in its cytosolic state

    Directory of Open Access Journals (Sweden)

    Shengliu Wang


    Full Text Available Abstract Studies on coat protein I (COPI have contributed to a basic understanding of how coat proteins generate vesicles to initiate intracellular transport. The core component of the COPI complex is coatomer, which is a multimeric complex that needs to be recruited from the cytosol to membrane in order to function in membrane bending and cargo sorting. Previous structural studies on the clathrin adaptors have found that membrane recruitment induces a large conformational change in promoting their role in cargo sorting. Here, pursuing negative-stain electron microscopy coupled with single-particle analyses, and also performing CXMS (chemical cross-linking coupled with mass spectrometry for validation, we have reconstructed the structure of coatomer in its soluble form. When compared to the previously elucidated structure of coatomer in its membrane-bound form we do not observe a large conformational change. Thus, the result uncovers a key difference between how COPI versus clathrin coats are regulated by membrane recruitment.

  18. Synthesis and characterization of one-dimensional titanate structure

    Directory of Open Access Journals (Sweden)

    Ljubica M. Nikolić


    Full Text Available One-dimensional titania structures were synthesized trough a simple hydrothermal process in a highly alkaline conditions. The aim of this work was to elucidate the effect of time on the formation of 1D titanates as well on its structural characteristics (morphology, phase composition, surface area. Apart from that, the effect of heat treatment conditions on the stability of titanate based 1D samples has been investigated. The results have revealed that it is possible to form one-dimensional titanates already after 1 hour of hydrothermal synthesis. Although the composition of titanates is still under debate, the results probably correspond to the layered sodium titanates. The 1D prepared structures show a remarkable stability during heating, remaining the basic morphology and composition even up to 700°C.

  19. A structurally characterized organometallic plutonium(IV) complex

    Energy Technology Data Exchange (ETDEWEB)

    Apostolidis, Christos; Walter, Olaf [European Commission, Joint Research Centre, Directorate G - Nuclear Safety and Security, Karlsruhe (Germany); Vogt, Jochen; Liebing, Phil; Edelmann, Frank T. [Chemisches Institut, Otto-von-Guericke-Universitaet Magdeburg (Germany); Maron, Laurent [Laboratoire de Physique et Chimie des Nanoobjets (LPCNO), Universite de Toulouse/INSA/CNRS (UMR5215), Toulouse (France)


    The blood-red plutonocene complex Pu(1,3-COT'')(1,4-COT'') (4; COT''=η{sup 8}-bis(trimethylsilyl)cyclooctatetraenyl) has been synthesized by oxidation of the anionic sandwich complex Li[Pu(1,4-COT''){sub 2}] (3) with anhydrous cobalt(II) chloride. The first crystal structure determination of an organoplutonium(IV) complex revealed an asymmetric sandwich structure for 4 where one COT'' ring is 1,3-substituted while the other retains the original 1,4-substitution pattern. The electronic structure of 4 has been elucidated by a computational study, revealing a probable cause for the unexpected silyl group migration. (copyright 2017 Wiley-VCH Verlag GmbH and Co. KGaA, Weinheim)

  20. Structural characterization of lipidic systems under nonequilibrium conditions

    DEFF Research Database (Denmark)

    Yaghmur, Anan; Rappolt, Michael


    manipulation techniques including, for instance, stop-flow mixing or rapid temperature-jump perturbation is given. Second, our recent synchrotron SAXS findings on the dynamic structural response of gold nanoparticle-loaded vesicles upon exposure to an ultraviolet light source, the impact of rapidly mixing...... negatively charged vesicles with calcium ions, and in situ hydration-induced formation of inverted-type liquid-crystalline phases loaded with the local anesthetic bupivacaine are summarized. These in situ time-resolved experiments allow real-time monitoring of the dynamics of the structural changes...

  1. Synthesis and structural characterization of boron nitride thin films

    Energy Technology Data Exchange (ETDEWEB)

    Elena, M. (CMBM, 38050 Povo (Trento) (Italy)); Guzman, L. (CMBM, 38050 Povo (Trento) (Italy)); Calliari, L. (CMBM, 38050 Povo (Trento) (Italy)); Moro, L. (CMBM, 38050 Povo (Trento) (Italy)); Steiner, A. (Institute for Advanced Materials, Joint Research Centre, Commission of the European Communities, 21020 Ispra (Vatican City State, Holy See) (Italy)); Miotello, A. (Department of Physics, Trento Univ. (Italy)); Bonelli, M. (Department of Physics, Trento Univ. (Italy)); Capelletti, R. (Department of Physics, Parma Univ. (Italy)); Ossi, P.M. (Dipartimento di Ingegneria Nucleare del Politecnico, Milano (Italy))


    The purpose of this paper is to present first results of an investigation on the properties of boron-nitrogen thin films obtained by different deposition techniques. Films of different stoichiometries were produced on silicon substrates using r.f. magnetron sputtering and ion-beam-assisted deposition.In order to study the influence of the deposition process parameters on the film properties, the films were characterized by scanning electron microscopy. Auger electron spectroscopy, secondary neutral mass spectrometry, IR spectroscopy and nanoindentation.With the chosen experimental conditions, only hexagonal BN is formed. A considerable dependence of hardness of film microstructure has been evidenced. ((orig.))

  2. Structural, dielectric and ferroelectric characterization of PZT thin films

    Directory of Open Access Journals (Sweden)

    Araújo E.B.


    Full Text Available In this work ferroelectric thin films of PZT were prepared by the oxide precursor method, deposited on Pt/Si substrate. Films of 0.5 mm average thickness were obtained. Electrical and ferroelectric characterization were carried out in these films. The measured value of the dielectric constant for films was 455. Ferroelectricity was confirmed by Capacitance-Voltage (C-V characteristics and P-E hysteresis loops. Remanent polarization for films presented value around 5.0 µC/cm2 and a coercive field of 88.8 kV/cm.

  3. Synthesis and structural characterization of CsNiP crystal

    Indian Academy of Sciences (India)


    Fluck and Issleib 1965). However, studies of these alka- line metal phosphides gained momentum since last three decades (Johnson and Jeitschlo 1972; Barz et al 1983;. Muller et al 1983; Schnering et al 1999). In recent years, structural data of phosphides also were reported (Shan- non 1976; Jeitschlo and Braun 1977; ...

  4. Characterization of genetic structure of alfalfa (Medicago sp.) from ...

    African Journals Online (AJOL)



    Aug 8, 2011 ... Slatkin M (1987). Gene flow and the geographic structure of natural populations. Science, 236: 787-792. Small E Jomphe M (1989). A synopsis of the genus Medicago. (Leguminosae). Can. J. Bot. 67: 3260-3294. Soltis DE, Soltis PS, Tate JA (2003). Advances in the study of polyploidy since plant speciation ...

  5. Directed Evolution and Structural Characterization of a Simvastatin Synthase

    Energy Technology Data Exchange (ETDEWEB)

    Gao, Xue; Xie, Xinkai; Pashkov, Inna; Sawaya, Michael R.; Laidman, Janel; Zhang, Wenjun; Cacho, Ralph; Yeates, Todd O.; Tang, Yi; UCLA


    Enzymes from natural product biosynthetic pathways are attractive candidates for creating tailored biocatalysts to produce semisynthetic pharmaceutical compounds. LovD is an acyltransferase that converts the inactive monacolin J acid (MJA) into the cholesterol-lowering lovastatin. LovD can also synthesize the blockbuster drug simvastatin using MJA and a synthetic {alpha}-dimethylbutyryl thioester, albeit with suboptimal properties as a biocatalyst. Here we used directed evolution to improve the properties of LovD toward semisynthesis of simvastatin. Mutants with improved catalytic efficiency, solubility, and thermal stability were obtained, with the best mutant displaying an {approx}11-fold increase in an Escherichia coli-based biocatalytic platform. To understand the structural basis of LovD enzymology, seven X-ray crystal structures were determined, including the parent LovD, an improved mutant G5, and G5 cocrystallized with ligands. Comparisons between the structures reveal that beneficial mutations stabilize the structure of G5 in a more compact conformation that is favorable for catalysis.

  6. Crystal structure, characterization and magnetic properties of a 1D ...

    Indian Academy of Sciences (India)

    A new 1D polymeric copper(II) complex [{Cu(L)(CF3COO)}2]n has been synthesized using a potentially tetradentate Schiff base ... 1D copper(II) polymer; Schiff base; crystal structure; electrochemistry; EPR; magnetic properties. 1. Introduction ... number of copper(II) poly-clusters/assemblies may be mentioned in this regard ...

  7. Structural characterization of polymorphs and molecular complexes of finasteride (United States)

    Wawrzycka, Irena; Stȩpniak, Krystyna; Matyjaszczyk, Sławomir; Kozioł, Anna E.; Lis, Tadeusz; Abboud, Khalil A.


    The molecular structure of finasteride, 17 β-( N-tert-butylcarbamoyl)-4-aza-5 α-androst-1-en-3-one, and structures of three related crystalline forms have been determined by X-ray analysis. The rigid steroid skeleton of the molecule adopts a half-chair/chair/chair/half-chair conformation. Two peptide groups, one cyclic (lactam) in the ring A and a second being a part of the substituent at C17, are the main factors influencing intermolecular contacts. Different hydrogen-bond interactions of these hydrophilic groups are observed in the crystal structures. An infinite ribbon of finasteride molecules is formed between lactam groups in the orthorhombic homomolecular crystal ( 1) obtained from an ethanol solution. The linear molecular complex finasteride-acetic acid ( 1a) is connected by hydrogen bonds between the lactam of finasteride and the carboxyl group of acetic acid. The crystallization from an ethyl acetate solution gives a complex structure of bis-finasteride monohydrate ethyl acetate clathrate ( 1b) with guest molecule disordered in channels. Crystals of a second (monoclinic) finasteride polymorph ( 2) were obtained during thermal decomposition of 1a, and sublimation of 1, 1a and 1b. Two polymorphic forms show different IR spectra.

  8. Structural characterization of thyroglobulin type-1 domains of equistatin

    NARCIS (Netherlands)

    Galesa, K.; Pain, R.; Jongsma, M.A.; Turk, V.; Lenarci, B.


    Equistatin is a protein composed of three thyroglobulin type-1 domains. It inhibits papain-like cysteine proteinases and the aspartic proteinase, cathepsin D. To determine the structural basis for this inhibition we cloned and expressed the separated domains (eq d-1, eq d-2, eq d-3) in Pichia

  9. Structural characterization of vacuum evaporated ZnSe thin films

    Indian Academy of Sciences (India)

    ... polycrystalline nature having f.c.c. zincblende structure. The most preferential orientation is along [111] direction for all deposited films together with other abundant planes [220] and [311]. The lattice parameter, grain size, average internal stress, microstrain, dislocation density and degree of preferred orientation in the film ...

  10. Structural and optical characterization of thick and thin ...

    Indian Academy of Sciences (India)

    Typical twin bands and also a quintuplet twinned crystal were observed in TEM, further it was found that the twinned region in thin sample composed of very fine platelet like structure. Keywords. Diamond film; plasma CVD; defects; optical properties. 1. Introduction. Diamond is one of the most sought after material not only.

  11. Towards the structural characterization of proteins involved in peptidoglycan biosynthesis

    NARCIS (Netherlands)

    Nikolaidis, I.|info:eu-repo/dai/nl/330830260


    The cell wall is an essential structure for bacterial survival and unique to bacteria. It is responsible for maintenance of cellular shape and allows the bacterium to withstand high differences in osmotic pressure between the inner and outer leaflet of the cell. Consequently, the bacterial cell wall

  12. Reliability characterization of MEMS switch using MIM test structures

    Directory of Open Access Journals (Sweden)

    Vaibhav Dubey


    Full Text Available Silicon nitride thin film dielectrics are used in capacitive radio frequency micro-electromechanical systems (MEMS switches since they provide a low insertion loss, good isolation, and low return loss. The lifetime of these switches is believed to be adversely affected by charge trapping in the silicon nitride. The goal of this research was to characterize Si3N4-based MIM (Metal–Insulator–Metal capacitors to describe the mechanisms responsible for the conduction and trapping behaviour in MEMS switches. The silicon nitride films were deposited by ICP chemical vapour deposition at room temperatures. The upper Si3N4 layer was removed by the reactive ion etching process (RIE in order to provide contact paths to the bottom electrode. In the near-stoichiometric films, different electrical characterizations were performed to study dependence of the leakage current on different electrical parameters. It was concluded that the Poole–Frenkel mechanism dominated the conduction in the silicon nitride films at high fields.

  13. Structural and Kinetic Characterization of Thymidine Kinase from Leishmania major.

    Directory of Open Access Journals (Sweden)

    Jennifer Timm


    Full Text Available Leishmania spp. is a protozoan parasite and the causative agent of leishmaniasis. Thymidine kinase (TK catalyses the transfer of the γ-phosphate of ATP to 2'-deoxythymidine (dThd forming thymidine monophosphate (dTMP. L. major Type II TK (LmTK has been previously shown to be important for infectivity of the parasite and therefore has potential as a drug target for anti-leishmanial therapy. In this study, we determined the enzymatic properties and the 3D structures of holo forms of the enzyme. LmTK efficiently phosphorylates dThd and dUrd and has high structural homology to TKs from other species. However, it significantly differs in its kinetic properties from Trypanosoma brucei TK since purines are not substrates of the enzyme and dNTPs such as dUTP inhibit LmTK. The enzyme had Km and kcat values for dThd of 1.1 μM and 2.62 s(-1 and exhibits cooperative binding for ATP. Additionally, we show that the anti-retroviral prodrug zidovudine (3-azido-3-deoxythymidine, AZT and 5'-modified dUrd can be readily phosphorylated by LmTK. The production of recombinant enzyme at a level suitable for structural studies was achieved by the construction of C-terminal truncated versions of the enzyme and the use of a baculoviral expression system. The structures of the catalytic core of LmTK in complex with dThd, the negative feedback regulator dTTP and the bi-substrate analogue AP5dT, were determined to 2.74, 3.00 and 2.40 Å, respectively, and provide the structural basis for exclusion of purines and dNTP inhibition. The results will aid the process of rational drug design with LmTK as a potential target for anti-leishmanial drugs.

  14. Fabrication and characterization of micro- /nano structures for nanophotonic applications (United States)

    Jee, Hongsub

    The objective of this thesis is finding and developing fabrication methods to provide background techniques for potential applications with nanomaterials. The inclined UV lithography has announced to make three-dimensional fabrication process. With a movable stage, complex structures were achieved but difference of the refractive index, design of the final structures were limited. Refractive index matching medium between the substrate and the light source could reduce the refractive indices between the polymer and the substrate successfully. Nanoporous structures fabricated by multibeam interference lithography shows limitation of the usage since its periodicity. By insertion of the lift off resist layer between the patterned layer and the substrate, final photonic crystal structures could be partially removed for its own purpose and it provide potential application in the future. Two-step processing, combining with reactive ion etching system, nanoporous structures were on various substrates such as silicon and Polydimethylsiloxane. Photonic crystal template anodic aluminum oxide process has been described too. Large optical activity at visible wavelengths are of great attention in photonics. Dramatic enhancement of the optical activity of chiral poly(fluorene-alt-benzothiadiazole) with photoresist was demonstrated and successive photo patterning of chiral polymer shows the potential usage of this material for the photonics applications. Two photon lithography also used to pattern a photoresist-chiral polymer mixture into planar shapes and enhanced chirality can be realized by tuning the wavelength-dependent chiral response at both the molecular and geometric level. Near infrared light induced photopolymerization in-situ was demonstrated which can be applied everywhere where ultraviolet-polymerization is employed such as dentistry, coating industry. Use of the ultraviolet upconverting nanoparticles doped into the polymer, we show that expensive femtosecond pulsed

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

    DEFF Research Database (Denmark)

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


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

  16. Morphology Characterization of PP/Clay Nanocomposites Across the Length Scales of the Structural Architecture

    NARCIS (Netherlands)

    Szazdi, Laszlo; Abranyi, Agnes; Pukansky Jr, Bela; Vancso, Gyula J.; Pukanszky, B.; Pukanszky, Bela


    The structure and rheological properties of a large number of layered silicate poly(propylene) nanocomposites were studied with widely varying compositions. Morphology characterization at different length scales was achieved by SEM, TEM, and XRD. Rheological measurements supplied additional

  17. Fabrication and characterization of nanometric SiOx/SiOy multilayer structures obtained by LPCVD

    Energy Technology Data Exchange (ETDEWEB)

    Román-López, S.; Aceves-Mijares, M.; Pedraza-Chávez, J. [National Institute for Astrophysics, Optics and Electronics, L. Erro 1, Tonatzintla Puebla (Mexico); Carrillo-López, J. [Center of Res. on Semiconductors Dev. BUAP, Av. San Claudio y 14 Sur CU, Puebla Puebla (Mexico)


    This work presents the fabrication of nanometric multilayer structures and their characterization by Atomic Force Microscopy, Photoluminescence and Fourier Transform Infra Red spectroscopy. The structures were deposited by Low Pressure Chemical Vapor Deposition (LPCVD). Three types of multilayer structure were fabricated. After the deposition some samples were annealed in N{sub 2} ambient for three hours. It was found that the structures keep the characteristics of each layer.

  18. Structural and functional characterization of annexin 1 from Medicago truncatula. (United States)

    Kodavali, Praveen Kumar; Skowronek, Krzysztof; Koszela-Piotrowska, Izabela; Strzelecka-Kiliszek, Agnieszka; Pawlowski, Krzysztof; Pikula, Slawomir


    Annexins are calcium- and membrane-binding proteins that have been shown to have diverse properties such as actin, integrin and GTP binding, both in animals and plants. Recently, Medicago truncatula annexin 1 (AnnMt1) has been suggested to participate in nodulation (Nod factor signaling) and mycorrhization in legume plants. In this report we demonstrate for the first time that recombinant AnnMt1 (rec-AnnMt1) mediates membrane permeabilization to cations with conductance ranging from 16 pS to 329 pS. In agreement with other structurally determined annexins, homology modeling of AnnMt1 suggests that most of the functional determinants are found on the convex surface of the modeled structure. In conclusion, we propose a potential constitutive role of AnnMt1 in Nod factor signaling as a non-specific ion channel. Copyright © 2013 Elsevier Masson SAS. All rights reserved.

  19. Structural and functional characterization of barium zirconium titanate / epoxy composites

    Directory of Open Access Journals (Sweden)

    Filiberto González Garcia


    Full Text Available The dielectric behavior of composite materials (barium zirconium titanate / epoxy system was analyzed as a function of ceramic concentration. Structure and morphologic behavior of the composites was investigated by X-ray Diffraction (XRD, Fourier transformed infrared spectroscopy (FT-IR, Raman spectroscopy, field emission scanning electron microscopy (FE-SEM and transmission electron microscopy (TEM analyses. Composites were prepared by mixing the components and pouring them into suitable moulds. It was demonstrated that the amount of inorganic phase affects the morphology of the presented composites. XRD revealed the presence of a single phase while Raman scattering confirmed structural transitions as a function of ceramic concentration. Changes in the ceramic concentration affected Raman modes and the distribution of particles along into in epoxy matrix. Dielectric permittivity and dielectric losses were influenced by filler concentration.

  20. Structural Characterization of a Eukaryotic Cyanase from Tetranychus urticae. (United States)

    Schlachter, Caleb R; Klapper, Vincent; Wybouw, Nicky; Radford, Taylor; Van Leeuwen, Thomas; Grbic, Miodrag; Chruszcz, Maksymilian


    The two-spotted spider mite Tetranychus urticae is a polyphagous agricultural pest and poses a high risk to global crop production as it is rapidly developing pesticide resistance. Genomic and transcriptomic analysis has revealed the presence of a remarkable cyanase gene in T. urticae and related mite species within the Acariformes lineage. Cyanase catalyzes the detoxification of cyanate and is potentially an attractive protein target for the development of new acaricides. Phylogenetic analysis indicates that within the Acariformes, the cyanase gene originates from a single horizontal gene transfer event, which precedes subsequent speciation. Our structural studies presented here compare and contrast prokaryotic cyanases to T. urticae cyanase, which all form homodecamers and have conserved active site residues, but display different surface areas between homodimers in the overall decameric structure.

  1. Structural behaviour characterization of existing adobe constructions in Aveiro


    H. Varum; Costa, A; Martins, T.(); Pereira, H; Almeida, J; Rodrigues, H.; D. Silveira


    Adobe was a widely used construction material in Aveiro, Portugal, till the middle of the 20th century. Nowadays, adobe can still be found in varied types of constructions, many of which are of cultural, historical, and also architectural recognized value. The existing adobe buildings present an important level of structural damage and, in many cases, are even near to ruin, having the majority a high vulnerability to seismic actions. To face the lack of information concerning the mechanica...

  2. The Structural Characterization of Tumor Fusion Genes and Proteins


    Wang, Dandan; Li, Daixi; Qin, Guangrong; Zhang, Wen; Ouyang, Jian; Zhang, Menghuan; Xie, Lu


    Chromosomal translocation, which generates fusion proteins in blood tumor or solid tumor, is considered as one of the major causes leading to cancer. Recent studies suggested that the disordered fragments in a fusion protein might contribute to its carcinogenicity. Here, we investigated the sequence feature near the breakpoints in the fusion partner genes, the structure features of breakpoints in fusion proteins, and the posttranslational modification preference in the fusion proteins. Result...

  3. Structural Characterization of Novel Pseudomonas aeruginosa Type IV Pilins

    Energy Technology Data Exchange (ETDEWEB)

    Nguyen, Y.; Jackson, S; Aidoo, F; Junop, M; Burrows, L


    Pseudomonas aeruginosa type IV pili, composed of PilA subunits, are used for attachment and twitching motility on surfaces. P. aeruginosa strains express one of five phylogenetically distinct PilA proteins, four of which are associated with accessory proteins that are involved either in pilin posttranslational modification or in modulation of pilus retraction dynamics. Full understanding of pilin diversity is crucial for the development of a broadly protective pilus-based vaccine. Here, we report the 1.6-{angstrom} X-ray crystal structure of an N-terminally truncated form of the novel PilA from strain Pa110594 (group V), which represents the first non-group II pilin structure solved. Although it maintains the typical T4a pilin fold, with a long N-terminal {alpha}-helix and four-stranded antiparallel {beta}-sheet connected to the C-terminus by a disulfide-bonded loop, the presence of an extra helix in the {alpha}{beta}-loop and a disulfide-bonded loop with helical character gives the structure T4b pilin characteristics. Despite the presence of T4b features, the structure of PilA from strain Pa110594 is most similar to the Neisseria gonorrhoeae pilin and is also predicted to assemble into a fiber similar to the GC pilus, based on our comparative pilus modeling. Interactions between surface-exposed areas of the pilin are suggested to contribute to pilus fiber stability. The non-synonymous sequence changes between group III and V pilins are clustered in the same surface-exposed areas, possibly having an effect on accessory protein interactions. However, based on our high-confidence model of group III PilA{sub PA14}, compensatory changes allow for maintenance of a similar shape.

  4. Structural and compositional characterization of cilverFil amalgam


    Ramasindarum, C.; Abu Kasim, N.H.


    SilverFil (Silverfildental Products, Malaysia) is another commercially available dental amalgam; however it is based on silver and mercury only. It is claimed that upon amalgamation, there is no excess mercury in SilverFil. Objectives: The objectives of this study were to determine the structural state and chemical composition of the starting materials and presence of mercury in the resulting amalgam. Methods: All the starting materials of SilverFil and the SilverFil amalgam specimens were ch...

  5. Material characterization of structural adhesives in the lap shear mode (United States)

    Sancaktar, E.; Schenck, S. C.


    A general method for characterizing structual adhesives in the bonded lap shear mode is proposed. Two approaches in the form of semiempirical and theoretical approaches are used. The semiempirical approach includes Ludwik's and Zhurkov's equations to describe respectively, the failure stresses in the constant strain rate and constant stress loading modes with the inclusion of the temperature effects. The theoretical approach is used to describe adhesive shear stress-strain behavior with the use of viscoelastic or nonlinear elastic constitutive equations. Two different model adhesives are used in the single lap shear mode with titanium adherends. These adhesives (one of which was developed at NASA Langley Research Center) are currently considered by NASA for possible aerospace applications. Use of different model adhesives helps in assessment of the generality of the method.

  6. Structural characterization of chemically deposited PbS thin films

    Energy Technology Data Exchange (ETDEWEB)

    Fernandez-Lima, F.A. [Instituto Superior de Tecnologias y Ciencias Aplicadas Ave Salvador Allende esq. Luaces, s/n, AP 6163, CP 10600, Ciudad de La Habana (Cuba); Departamento de Fisica, Pontificia Universidade Catolica do Rio do Janeiro, 22453-900 Rio de Janeiro, RJ (Brazil); Gonzalez-Alfaro, Y. [Facultad de Fisica-IMRE, Universidad de La Habana (Cuba); Larramendi, E.M. [Facultad de Fisica-IMRE, Universidad de La Habana (Cuba); Fonseca Filho, H.D. [Departamento de Fisica, Pontificia Universidade Catolica do Rio do Janeiro, 22453-900 Rio de Janeiro, RJ (Brazil); Maia da Costa, M.E.H. [Departamento de Fisica, Pontificia Universidade Catolica do Rio do Janeiro, 22453-900 Rio de Janeiro, RJ (Brazil); Freire, F.L. [Departamento de Fisica, Pontificia Universidade Catolica do Rio do Janeiro, 22453-900 Rio de Janeiro, RJ (Brazil)]. E-mail:; Prioli, R. [Departamento de Fisica, Pontificia Universidade Catolica do Rio do Janeiro, 22453-900 Rio de Janeiro, RJ (Brazil); Avillez, R.R. de [Departamento de Ciencia dos Materiais e Metalurgia, Pontificia Universidade Catolica do Rio do Janeiro, 22453-900 Rio de Janeiro, RJ (Brazil); Silveira, E.F. da [Facultad de Fisica-IMRE, Universidad de La Habana (Cuba); Calzadilla, O. [Facultad de Fisica-IMRE, Universidad de La Habana (Cuba); Melo, O. de [Facultad de Fisica-IMRE, Universidad de La Habana (Cuba); Pedrero, E. [Facultad de Fisica-IMRE, Universidad de La Habana (Cuba); Hernandez, E. [Facultad de Fisica-IMRE, Universidad de La Habana (Cuba)


    Polycrystalline thin films of lead sulfide (PbS) grown using substrate colloidal coating chemical bath depositions were characterized by RBS, XPS, AFM and GIXRD techniques. The films were grown on glass substrates previously coated with PbS colloidal particles in a polyvinyl alcohol solution. The PbS films obtained with the inclusion of the polymer showed non-oxygen-containing organic contamination. All samples maintained the Pb:S 1:1 stoichiometry throughout the film. The amount of effective nucleation centers and the mean grain size have being controlled by the substrate colloidal coating. The analysis of the polycrystalline PbS films showed that a preferable (1 0 0) lattice plane orientation parallel to the substrate surface can be obtained using a substrate colloidal coating chemical bath deposition, and the orientation increases when a layer of colloid is initially dried on the substrate.

  7. Assembly and microscopic characterization of DNA origami structures. (United States)

    Scheible, Max; Jungmann, Ralf; Simmel, Friedrich C


    DNA origami is a revolutionary method for the assembly of molecular nanostructures from DNA with precisely defined dimensions and with an unprecedented yield. This can be utilized to arrange nanoscale components such as proteins or nanoparticles into pre-defined patterns. For applications it will now be of interest to arrange such components into functional complexes and study their geometry-dependent interactions. While commonly DNA nanostructures are characterized by atomic force microscopy or electron microscopy, these techniques often lack the time-resolution to study dynamic processes. It is therefore of considerable interest to also apply fluorescence microscopic techniques to DNA nanostructures. Of particular importance here is the utilization of novel super-resolved microscopy methods that enable imaging beyond the classical diffraction limit.

  8. Characterization of a structural intermediate of flavivirus membrane fusion.

    Directory of Open Access Journals (Sweden)

    Karin Stiasny


    Full Text Available Viral membrane fusion proceeds through a sequence of steps that are driven by triggered conformational changes of viral envelope glycoproteins, so-called fusion proteins. Although high-resolution structural snapshots of viral fusion proteins in their prefusion and postfusion conformations are available, it has been difficult to define intermediate structures of the fusion pathway because of their transient nature. Flaviviruses possess a class II viral fusion protein (E mediating fusion at acidic pH that is converted from a dimer to a trimer with a hairpin-like structure during the fusion process. Here we show for tick-borne encephalitis virus that exposure of virions to alkaline instead of acidic pH traps the particles in an intermediate conformation in which the E dimers dissociate and interact with target membranes via the fusion peptide without proceeding to the merger of the membranes. Further treatment to low pH, however, leads to fusion, suggesting that these monomers correspond to an as-yet-elusive intermediate required to convert the prefusion dimer into the postfusion trimer. Thus, the use of nonphysiological conditions allows a dissection of the flavivirus fusion process and the identification of two separate steps, in which membrane insertion of multiple copies of E monomers precedes the formation of hairpin-like trimers. This sequence of events provides important new insights for understanding the dynamic process of viral membrane fusion.

  9. The synthesis and structural characterization of novel transition metal fluorides

    Energy Technology Data Exchange (ETDEWEB)

    Casteel, W.J. Jr.


    High purity KMF[sub 6] and K[sub 2]MF[sub 6] salts (M = Mo,Re, Ru, Os, Ir, Pt) are obtained from reduction hexafluorides. A rhombohedral unit cell is observed for KReF[sub 6]. Fluoride ion capture by Lewis acids from the hexafluorometallate (IV) salts affords high purity tetrafluorides for M = Mo, Re, Ru, Os, and Pd. The structure of RuF[sub 4] is determined from X-ray synchrotron and neutron powder data. Unit cells based on theorthorhombic PdF[sub 4] type cell are derived from X-ray powder data for ReF[sub 4] and OsF[sub 4]. Fluoride ion capture from KAgF[sub 4] provides the thermally unstable trifluoride as a bright, red, diamagnetic solid. The structure solution of AgF[sub 3] and redetermination of the AuF[sub 3] structure from X-ray synchrotron and neutron powder data demonstrate that the two are isostnictural. Thermal decomposition product of AgF[sub 3] is the mixed valence compound Ag[sup II]Ag[sub 2][sup III]F[sub 8]. Several new salts containing the (Ag - F)[sub n][sup n+] chain cation are prepared. The first linear (Ag - F)[sub n][sup n+] chain is observed in AgF[sup +]BF[sub 4 [sup [minus

  10. Cryo-Electron Tomography for Structural Characterization of Macromolecular Complexes (United States)

    Cope, Julia; Heumann, John; Hoenger, Andreas


    Cryo-electron tomography (cryo-ET) is an emerging 3-D reconstruction technology that combines the principles of tomographic 3-D reconstruction with the unmatched structural preservation of biological material embedded in vitreous ice. Cryo-ET is particularly suited to investigating cell-biological samples and large macromolecular structures that are too polymorphic to be reconstructed by classical averaging-based 3-D reconstruction procedures. This unit aims to make cryo-ET accessible to newcomers and discusses the specialized equipment required, as well as the relevant advantages and hurdles associated with sample preparation by vitrification and cryo-ET. Protocols describe specimen preparation, data recording and 3-D data reconstruction for cryo-ET, with a special focus on macromolecular complexes. A step-by-step procedure for specimen vitrification by plunge freezing is provided, followed by the general practicalities of tilt-series acquisition for cryo-ET, including advice on how to select an area appropriate for acquiring a tilt series. A brief introduction to the underlying computational reconstruction principles applied in tomography is described, along with instructions for reconstructing a tomogram from cryo-tilt series data. Finally, a method is detailed for extracting small subvolumes containing identical macromolecular structures from tomograms for alignment and averaging as a means to increase the signal-to-noise ratio and eliminate missing wedge effects inherent in tomographic reconstructions. PMID:21842467

  11. Isolation, characterization, and aggregation of a structured bacterial matrix precursor. (United States)

    Chai, Liraz; Romero, Diego; Kayatekin, Can; Akabayov, Barak; Vlamakis, Hera; Losick, Richard; Kolter, Roberto


    Biofilms are surface-associated groups of microbial cells that are embedded in an extracellular matrix (ECM). The ECM is a network of biopolymers, mainly polysaccharides, proteins, and nucleic acids. ECM proteins serve a variety of structural roles and often form amyloid-like fibers. Despite the extensive study of the formation of amyloid fibers from their constituent subunits in humans, much less is known about the assembly of bacterial functional amyloid-like precursors into fibers. Using dynamic light scattering, atomic force microscopy, circular dichroism, and infrared spectroscopy, we show that our unique purification method of a Bacillus subtilis major matrix protein component results in stable oligomers that retain their native α-helical structure. The stability of these oligomers enabled us to control the external conditions that triggered their aggregation. In particular, we show that stretched fibers are formed on a hydrophobic surface, whereas plaque-like aggregates are formed in solution under acidic pH conditions. TasA is also shown to change conformation upon aggregation and gain some β-sheet structure. Our studies of the aggregation of a bacterial matrix protein from its subunits shed new light on assembly processes of the ECM within bacterial biofilms.

  12. Characterization of the structure and composition of gecko adhesive setae. (United States)

    Rizzo, N W; Gardner, K H; Walls, D J; Keiper-Hrynko, N M; Ganzke, T S; Hallahan, D L


    The ability of certain reptiles to adhere to vertical (and hang from horizontal) surfaces has been attributed to the presence of specialized adhesive setae on their feet. Structural and compositional studies of such adhesive setae will contribute significantly towards the design of biomimetic fibrillar adhesive materials. The results of electron microscopy analyses of the structure of such setae are presented, indicating their formation from aggregates of proteinaceous fibrils held together by a matrix and potentially surrounded by a limiting proteinaceous sheath. Microbeam X-ray diffraction analysis has shown conclusively that the only ordered protein constituent in these structures exhibits a diffraction pattern characteristic of beta-keratin. Raman microscopy of individual setae, however, clearly shows the presence of additional protein constituents, some of which may be identified as alpha-keratins. Electrophoretic analysis of solubilized setal proteins supports these conclusions, indicating the presence of a group of low-molecular-weight beta-keratins (14-20 kDa), together with alpha-keratins, and this interpretation is supported by immunological analyses.

  13. Sol-Gel Titanium Dioxide Nanoparticles: Preparation and Structural Characterization

    Directory of Open Access Journals (Sweden)

    Oon Lee Kang


    Full Text Available Titanium dioxide (TiO2 nanoparticle was achieved in an alternative sol-gel route, as involved in 1 M acidic solution: HCl-tetrahydrofuran (HCl-THF, HNO3-tetrahydrofuran (HNO3-THF, and ClHNO2-tetrahydrofuran (ClHNO2-THF solution. Resultant TiO2 nanoparticle was further investigated in a systematic analytical approach. Nanoscale TiO2 structure was observed at a moderate hydrolysis ratio (8≤RH≤16. Particle size range was much narrower in an aprotic HNO3-THF medium, as compared to a differential HCl-THF medium. Biphasic TiO2 structure was detected at a certain hydrolysis ratio (RH≥16. Even so, relative anatase content was rather insignificant in an aprotic HCl-THF medium, as compared to a differential HNO3-THF medium. Tetragonal TiO2 structure was observed in the entire hydrolysis ratio (4≤RH≤32. Interstitial lattice defect was evident in an aprotic HNO3-THF medium but absent in a differential ClHNO2-THF medium.

  14. Characterization of power absorption response of periodic three-dimensional structures to partially coherent fields. (United States)

    Tihon, Denis; Withington, Stafford; Thomas, Christopher N; Craeye, Christophe


    In many applications of absorbing structures it is important to understand their spatial response to incident fields, for example in thermal solar panels, bolometric imaging, and controlling radiative heat transfer. In practice, the illuminating field often originates from thermal sources and is only partially spatially coherent when it reaches the absorbing device. In this paper, we present a method to fully characterize the way a structure can absorb such partially coherent fields. The method is presented for any three-dimensional material and accounts for the partial coherence and partial polarization of the incident light. This characterization can be achieved numerically using simulation results or experimentally using the energy absorption interferometry that has been described previously in the literature. The absorbing structure is characterized through a set of absorbing functions onto which any partially coherent field can be projected. This set is compact for any structure of finite extent, and the absorbing function is discrete for periodic structures.

  15. Characterization of breakpoint regions of large structural autosomal mosaic events. (United States)

    Machiela, Mitchell J; Jessop, Lea; Zhou, Weiyin; Yeager, Meredith; Chanock, Stephen J


    Recent studies have reported a higher than anticipated frequency of large clonal autosomal mosaic events >2 Mb in size in the aging population. Mosaic events are detected from analyses of intensity parameters of linear stretches with deviations in heterozygous probes of single nucleotide polymorphism microarrays. The non-random distribution of detected mosaic events throughout the genome suggests common mechanisms could influence the formation of mosaic events. Here we use publicly available data tracks from the University of California Santa Cruz Genome Browser to investigate the genomic characteristics of the regions at the terminal ends of two frequent types of large structural mosaic events: telomeric neutral events and interstitial losses. We observed breakpoints are more likely to occur in regions enriched for open chromatin, increased gene density, elevated meiotic recombination rates and in the proximity of repetitive elements. These observations suggest that detected mosaic event breakpoints are preferentially recovered in genomic regions that are observed to be active and thus more accessible to environmental exposures and events related to gene transcription. We propose that errors in DNA repair pathways, such as non-homologous end joining and homologous recombination, may be important cellular mechanisms that lead to the formation of large structural mosaic events such as interstitial losses and copy neutral events that include telomeres. Further studies using next generation sequencing technologies should be instrumental in mapping the specific junctions of mosaic events to the nucleotide and provide insights into the molecular mechanisms responsible for clonal somatic structural events. Published by Oxford University Press 2017. This work is written by US Government employees and is in the public domain in the US.

  16. Structural and Biophysical Characterization of Cajanus cajan Protease Inhibitor (United States)

    Shamsi, Tooba Naz; Parveen, Romana; Ahamad, Shahzaib; Fatima, Sadaf


    Context: A large number of studies have proven that Protease inhibitors (PIs), specifically serine protease inhibitors, show immense divergence in regulation of proteolysis by targeting their specific proteases and hence, they play a key role in healthcare. Objective: We aimed to access in-vitro anticancer potential of PI from Cajanus cajan (CCPI). Also, crystallization of CCPI was targetted alongwith structure determination and its structure-function relationship. Materials and Methods: CCPI was purified from Cajanus cajan seeds by chromatographic techniques. The purity and molecular mass was determined by SDS-PAGE. Anticancer potential of CCPI was determined by MTT assay in normal HEK and cancerous A549 cells. The crystallization screening of CCPI was performed by commercially available screens. CCPI sequence was subject to BLASTp with homologous PIs. Progressive multiple alignment was performed using clustalw2 and was modelled using ab initio protocol of I-TASSER. Results: The results showed ~14kDa CCPI was purified in homogeneity. Also, CCPI showed low cytotoxic effects of in HEK i.e., 27% as compared with 51% cytotoxicity in A549 cells. CCPI crystallized at 16°C using 15% PEG 6000 in 0.1M potassium phosphate buffer (pH 6.0) in 2-3weeks as rod or needles visualized as clusters under the microscope. The molecular modelling revealed that it contains 3 beta sheets, 3 beta hairpins, 2 β-bulges, 6 strands, 3 helices, 1helix-helix interaction, 41 β-turns and 27 γ-turns. Discussion and Conclusion: The results indicate that CCPI may help to treat cancer in vivo aswell. Also, this is the first report on preliminary crystallization and structural studies of CCPI. PMID:28781485

  17. Characterization, Microstructure, and Dielectric properties of cubic pyrochlore structural ceramics

    KAUST Repository

    Li, Yangyang


    The (BMN) bulk materials were sintered at 1050°C, 1100°C, 1150°C, 1200°C by the conventional ceramic process, and their microstructure and dielectric properties were investigated by Scanning electron microscopy (SEM), X-ray diffraction (XRD), Raman spectroscopy, Transmission electron microscopy (TEM) (including the X-ray energy dispersive spectrometry EDS and high resolution transmission electron microscopy HRTEM) and dielectric impedance analyzer. We systematically investigated the structure, dielectric properties and voltage tunable property of the ceramics prepared at different sintering temperatures. The XRD patterns demonstrated that the synthesized BMN solid solutions had cubic phase pyrochlore-type structure when sintered at 1050°C or higher, and the lattice parameter (a) of the unit cell in BMN solid solution was calculated to be about 10.56Å. The vibrational peaks observed in the Raman spectra of BMN solid solutions also confirmed the cubic phase pyrochlore-type structure of the synthesized BMN. According to the Scanning Electron Microscope (SEM) images, the grain size increased with increasing sintering temperature. Additionally, it was shown that the densities of the BMN ceramic tablets vary with sintering temperature. The calculated theoretical density for the BMN ceramic tablets sintered at different temperatures is about 6.7521 . The density of the respective measured tablets is usually amounting more than 91% and 5 approaching a maximum value of 96.5% for sintering temperature of 1150°C. The microstructure was investigated by using Scanning Transmission Electron Microscope (STEM), X-ray diffraction (XRD). Combined with the results obtained from the STEM and XRD, the impact of sintering temperature on the macroscopic and microscopic structure was discussed. The relative dielectric constant ( ) and dielectric loss ( ) of the BMN solid solutions were measured to be 161-200 and (at room temperature and 100Hz-1MHz), respectively. The BMN solid

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

    DEFF Research Database (Denmark)

    Pantleon, Wolfgang; Wejdemann, Christian; Jakobsen, Bo


    With high-angular resolution three-dimensional X-ray diffraction (3DXRD), quantitative information is gained about dislocation structures in individual grains in the bulk of a macroscopic specimen by acquiring reciprocal space maps. In high-resolution 3D reciprocal space maps of tensile...... dynamics is followed in situ during varying loading conditions by reciprocal space mapping: during uninterrupted tensile deformation, formation of subgrains is observed concurrently with broadening of Bragg reflections shortly after the onset of plastic deformation. When the traction is terminated, stress...

  19. Structural and functional characterization of human complement factor P

    DEFF Research Database (Denmark)

    Pedersen, Dennis

    The complement system is of great importance for the innate immune response, which can lead to opsonization and removal of invading pathogens, as well as immune complexes and damaged self-cells. Factor P (FP), also known as properdin, acts as a positive regulator of the alternative pathway...... of complement by stabilizing the C3 convertase complex (C3bBb). FP has also been suggested to serve as a pattern recognition molecule for the initiation of the alternative pathway. However, the molecular mechanisms of FP remain unclear due to its oligomeric nature and hence the atomic structure of FP has...

  20. Graphite materials prepared from an anthracite: a structural characterization

    Energy Technology Data Exchange (ETDEWEB)

    David Gonzalez; Miguel A. Montes-Moran; Ana B. Garcia [CSIC, Instituto Nacional del Carbon, Oviedo (Spain)


    The purpose of this research was to study the influence of the temperature, treatment time, and initial coal particle size on the evolution of the structural order of graphite materials that have been prepared from an anthracite at temperatures {gt} 2273 K. Crystalline parameters such as the interlayer spacing and crystallite sizes were calculated from X-ray diffractometry measurements. The analysis of the first- and second-order Raman spectra allowed the assessment of the degree of orientation at the outermost layers of these materials. The graphitization of the anthracite happened in two different stages. The temperature of 2673 K seems to be the inflection point for the change in the graphitization rate of the anthracite. Highly crystalline materials were obtained at 2673 K. Temperatures of treatment {gt}2673 K led to minor changes in the degree of structural order of the graphite materials obtained. The initial particle size of the anthracite affected the evolution of the graphitization process with temperature, because of differences in the ratio of particles that contain organic matter and mineral matter associations. The degree of graphitization achieved with this coal was comparable to that of other natural and synthetic graphites. 35 refs., 1 fig., 3 tabs.

  1. Structural and functional characterization of a specific antidote for ticagrelor (United States)

    Newton, Philip; Pehrsson, Susanne; Inghardt, Tord; Antonsson, Thomas; Svensson, Peder; Sjögren, Tove; Öster, Linda; Janefeldt, Annika; Sandinge, Ann-Sofie; Keyes, Feenagh; Austin, Mark; Spooner, Jennifer; Gennemark, Peter; Penney, Mark; Howells, Garnet; Vaughan, Tristan; Nylander, Sven


    Ticagrelor is a direct-acting reversibly binding P2Y12 antagonist and is widely used as an antiplatelet therapy for the prevention of cardiovascular events in acute coronary syndrome patients. However, antiplatelet therapy can be associated with an increased risk of bleeding. Here, we present data on the identification and the in vitro and in vivo pharmacology of an antigen-binding fragment (Fab) antidote for ticagrelor. The Fab has a 20 pM affinity for ticagrelor, which is 100 times stronger than ticagrelor’s affinity for its target, P2Y12. Despite ticagrelor’s structural similarities to adenosine, the Fab is highly specific and does not bind to adenosine, adenosine triphosphate, adenosine 5′-diphosphate, or structurally related drugs. The antidote concentration-dependently neutralized the free fraction of ticagrelor and reversed its antiplatelet activity both in vitro in human platelet-rich plasma and in vivo in mice. Lastly, the antidote proved effective in normalizing ticagrelor-dependent bleeding in a mouse model of acute surgery. This specific antidote for ticagrelor may prove valuable as an agent for patients who require emergency procedures. PMID:25788700

  2. Multiple Approaches to Characterizing Pore Structure in Natural Rock (United States)

    Hu, Q.; Dultz, S.; Hamamoto, S.; Ewing, R. P.


    Microscopic characteristics of porous media - pore shape, pore-size distribution, and pore connectivity - control fluid flow and chemical transport, and are important in hydrogeological studies of rock formations in the context of energy, environmental, and water resources management. This presentation discusses various approaches to investigating pore structure of rock, with a particular focus on the Barnett Shale in north Texas used for natural gas production. Approaches include imbibition, tracer diffusion, porosimetry (MIP, vapor adsorption/desorption isotherms, NMR cyroporometry), and imaging (μ-tomography, Wood's metal impregnation, FIB/SEM). Results show that the Barnett Shale pores are predominantly in the nm size range, with a measured median pore-throat diameter of 6.5 nm. But small pore size is not the major contributor to low gas recovery; rather, the low gas diffusivity appears to be caused by low pore connectivity. Chemical diffusion in sparsely-connected pore spaces is not well described by classical Fickian behavior; anomalous behavior is suggested by percolation theory, and confirmed by results of imbibition tests. Our evolving complementary approaches, with their several advantages and disadvantages, provide a rich toolbox for tackling the pore structure characteristics in the Barnett Shale and other natural rocks.

  3. Facile synthesis and structure characterization of hexagonal tungsten bronzes crystals (United States)

    Lee, Jiann-Shing; Liu, Hao-Chuan; Peng, Gao-De; Tseng, Yawteng


    A facile molten-salt route was used to synthesize hexagonal Cs0.33WO3, Rb0.33WO3 and K0.30WO3 crystals. The three isostructural compounds were successfully prepared from the reaction of MxWO3 powders (M = Cs, Rb, K) in the CsCl/NaCl, RbCl/NaCl and KCl/NaCl fluxes, respectively. The structure determination and refinement, based on single-crystal X-ray diffraction data, are in agreement with previous works, possessing space group P63/mcm. The a and c parameters vary non-linearly with increasing radii of the M+ cations (rM) that is coordinated to twelve oxygen atoms. Both the volumes of unit-cell and WO6 octahedra vary linearly with rM, which become smaller from Cs0.33WO3 to K0.30WO3. The distortion of WO6 octahedra as well as isotropic displacement parameters increases from Cs0.33WO3 to K0.30WO3. The geometry of the WO6 octahedron becomes more regular with increasing rM. These structural trends arise from the effective size of the M+ cation.

  4. Structural characterization of the mitomycin 7-O-methyltransferase. (United States)

    Singh, Shanteri; Chang, Aram; Goff, Randal D; Bingman, Craig A; Grüschow, Sabine; Sherman, David H; Phillips, George N; Thorson, Jon S


    Mitomycins are quinone-containing antibiotics, widely used as antitumor drugs in chemotherapy. Mitomycin-7-O-methyltransferase (MmcR), a key tailoring enzyme involved in the biosynthesis of mitomycin in Streptomyces lavendulae, catalyzes the 7-O-methylation of both C9β- and C9α-configured 7-hydroxymitomycins. We have determined the crystal structures of the MmcR-S-adenosylhomocysteine (SAH) binary complex and MmcR-SAH-mitomycin A (MMA) ternary complex at resolutions of 1.9and 2.3 Å, respectively. The study revealed MmcR to adopt a common S-adenosyl-L-methionine-dependent O-methyltransferase fold and the presence of a structurally conserved active site general acid-base pair is consistent with a proton-assisted methyltransfer common to most methyltransferases. Given the importance of C7 alkylation to modulate mitomycin redox potential, this study may also present a template toward the future engineering of catalysts to generate uniquely bioactive mitomycins. Copyright © 2011 Wiley-Liss, Inc.

  5. Structural characterization of the mitomycin 7-O-methyltransferase

    Energy Technology Data Exchange (ETDEWEB)

    Singh, Shanteri; Chang, Aram; Goff, Randal D.; Bingman, Craig A.; Grüschow, Sabine; Sherman, David H.; Phillips, Jr., George N.; Thorson, Jon S. (Michigan); (UW)


    Mitomycins are quinone-containing antibiotics, widely used as antitumor drugs in chemotherapy. Mitomycin-7-O-methyltransferase (MmcR), a key tailoring enzyme involved in the biosynthesis of mitomycin in Streptomyces lavendulae, catalyzes the 7-O-methylation of both C9{beta}- and C9{alpha}-configured 7-hydroxymitomycins. We have determined the crystal structures of the MmcR-S-adenosylhomocysteine (SAH) binary complex and MmcR-SAH-mitomycin A (MMA) ternary complex at resolutions of 1.9 and 2.3 {angstrom}, respectively. The study revealed MmcR to adopt a common S-adenosyl-L-methionine-dependent O-methyltransferase fold and the presence of a structurally conserved active site general acid-base pair is consistent with a proton-assisted methyltransfer common to most methyltransferases. Given the importance of C7 alkylation to modulate mitomycin redox potential, this study may also present a template toward the future engineering of catalysts to generate uniquely bioactive mitomycins.

  6. Spectroscopic studies of anthracyclines: Structural characterization and in vitro tracking. (United States)

    Szafraniec, Ewelina; Majzner, Katarzyna; Farhane, Zeineb; Byrne, Hugh J; Lukawska, Malgorzata; Oszczapowicz, Irena; Chlopicki, Stefan; Baranska, Malgorzata


    A broad spectroscopic characterization, using ultraviolet-visible (UV-vis) and Fourier transform infrared absorption as well as Raman scattering, of two commonly used anthracyclines antibiotics (DOX) daunorubicin (DNR), their epimers (EDOX, EDNR) and ten selected analogs is presented. The paper serves as a comprehensive spectral library of UV-vis, IR and Raman spectra of anthracyclines in the solid state and in solution. The particular advantage of Raman spectroscopy for the measurement and analysis of individual antibiotics is demonstrated. Raman spectroscopy can be used to monitor the in vitro uptake and distribution of the drug in cells, using both 488nm and 785nm as source wavelengths, with submicrometer spatial resolution, although the cellular accumulation of the drug is different in each case. The high information content of Raman spectra allows studies of the drug-cell interactions, and so the method seems very suitable for monitoring drug uptake and mechanisms of interaction with cellular compartments at the subcellular level. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. Fracture network topology and characterization of structural permeability (United States)

    Hansberry, Rowan; King, Rosalind; Holford, Simon


    There are two fundamental requirements for successful geothermal development: elevated temperatures at accessible depths, and a reservoir from which fluids can be extracted. The Australian geothermal sector has successfully targeted shallow heat, however, due in part to the inherent complexity of targeting permeability, obtaining adequate flow rates for commercial production has been problematic. Deep sedimentary aquifers are unlikely to be viable geothermal resources due to the effects of diagenetic mineral growth on rock permeability. Therefore, it is likely structural permeability targets, exploiting natural or induced fracture networks will provide the primary means for fluid flow in geothermal, as well as unconventional gas, reservoirs. Recent research has focused on the pattern and generation of crustal stresses across Australia, while less is known about the resultant networks of faults, joints, and veins that can constitute interconnected sub-surface permeability pathways. The ability of a fracture to transmit fluid is controlled by the orientation and magnitude of the in-situ stress field that acts on the fracture walls, rock strength, and pore pressure, as well as fracture properties such as aperture, orientation, and roughness. Understanding the distribution, orientation and character of fractures is key to predicting structural permeability. This project focuses on extensive mapping of fractures over various scales in four key Australian basins (Cooper, Otway, Surat and Perth) with the potential to host geothermal resources. Seismic attribute analysis is used in concert with image logs from petroleum wells, and field mapping to identify fracture networks that are usually not resolved in traditional seismic interpretation. We use fracture network topology to provide scale-invariant characterisation of fracture networks from multiple data sources to assess similarity between data sources, and fracture network connectivity. These results are compared with

  8. The synthesis and structural characterization of novel transition metal fluorides

    Energy Technology Data Exchange (ETDEWEB)

    Casteel, Jr., William Jack [Univ. of California, Berkeley, CA (United States)


    High purity KMF6 and K2MF6 salts (M = Mo,Re, Ru, Os, Ir, Pt) are obtained from reduction hexafluorides. A rhombohedral unit cell is observed for KReF6. Fluoride ion capture by Lewis acids from the hexafluorometallate (IV) salts affords high purity tetrafluorides for M = Mo, Re, Ru, Os, and Pd. The structure of RuF4 is determined from X-ray synchrotron and neutron powder data. Unit cells based on theorthorhombic PdF4 type cell are derived from X-ray powder data for ReF4 and OsF4. Fluoride ion capture from KAgF4 provides the thermally unstable trifluoride as a bright, red, diamagnetic solid. The structure solution of AgF3 and redetermination of the AuF3 structure from X-ray synchrotron and neutron powder data demonstrate that the two are isostnictural. Thermal decomposition product of AgF3 is the mixed valence compound AgIIAg2IIIF8. Several new salts containing the (Ag - F)$n+\\atop{n}$ chain cation are prepared. The first linear (Ag - F)$n+\\atop{n}$ chain is observed in AgF+BF4- which crystallizes in a tetragonal unit. AgFAuF4 has a triclinic unit cell and is isostructural with CuFAuF4. AgFAuF6 has an orthorhombic unit cell and appears to be isostructural with AgFAsF6. A second mixed valence silver fluoride, AgIIAgIIIF5, is prepared, which magnetic measurements indicate is probably an AgF+ salt. Magnetic data for all of the AgF+ salts exhibit low magnitude, temperature independent paramagnetism characteristic of metallic systems. Cationic AG(II) in acidic AHF solutions is a powerful oxidizer, capable of oxidizing Xe to Xe(II) and O2 to O2+. Reactions with C6F6 and C3F6 suggest an electron capture

  9. Chemical and structural characterization of copper adsorbed on mosses (Bryophyta)

    Energy Technology Data Exchange (ETDEWEB)

    González, Aridane G., E-mail: [GET (Géosciences Environnement Toulouse) UMR 5563CNRS, 14 Avenue Edouard Belin, F-31400 Toulouse (France); Jimenez-Villacorta, Felix [Instituto de Ciencia de Materiales Madrid, CSIC, Cantoblanco, E-28049 Madrid (Spain); Beike, Anna K. [Plant Biotechnology, Faculty of Biology, University of Freiburg, Schaenzlestrasse 1, 79104 Freiburg (Germany); State Museum of Natural History Stuttgart, Rosenstein 1, 70191 Stuttgart (Germany); Reski, Ralf [Plant Biotechnology, Faculty of Biology, University of Freiburg, Schaenzlestrasse 1, 79104 Freiburg (Germany); BIOSS—Centre for Biological Signalling Studies, 79104 Freiburg (Germany); FRIAS—Freiburg Institute for Advanced Studies, 79104 Freiburg (Germany); Adamo, Paola [Department of Agricultural Sciences, University of Naples Federico II, Via Università 100, 80055 Naples (Italy); Pokrovsky, Oleg S. [GET (Géosciences Environnement Toulouse) UMR 5563CNRS, 14 Avenue Edouard Belin, F-31400 Toulouse (France); BIO-GEO-CLIM Laboratory, Tomsk State University, Tomsk (Russian Federation); Institute of Ecological Problems of the North, Russian Academy of Science, Arkhangelsk (Russian Federation)


    Highlights: • Cu{sup 2+} was adsorbed on four mosses used in moss-bag pollution monitoring technique. • Thermodynamic approach was used to model Cu speciation based on XAS results. • All studied mosses have ∼4.5 O/N atoms at ∼1.95 Å around Cu likely in a pseudo-square geometry. • Cu(II)-carboxylates and Cu(II)-phosphoryls are the main moss surface binding groups. • Moss growing in batch reactor yielded ∼20% of Cu(I) in the form of Cu–S(CN) complexes. - Abstract: The adsorption of copper on passive biomonitors (devitalized mosses Hypnum sp., Sphagnum denticulatum, Pseudoscleropodium purum and Brachythecium rutabulum) was studied under different experimental conditions such as a function of pH and Cu concentration in solution. Cu assimilation by living Physcomitrella patents was also investigated. Molecular structure of surface adsorbed and incorporated Cu was studied by X-ray Absorption Spectroscopy (XAS). Devitalized mosses exhibited the universal adsorption pattern of Cu as a function of pH, with a total binding sites number 0.05–0.06 mmolg{sub dry}{sup −1} and a maximal adsorption capacity of 0.93–1.25 mmolg{sub dry}{sup −1} for these devitalized species. The Extended X-ray Absorption Fine Structure (EXAFS) fit of the first neighbor demonstrated that for all studied mosses there are ∼4.5 O/N atoms around Cu at ∼1.95 Å likely in a pseudo-square geometry. The X-ray Absorption Near Edge Structure (XANES) analysis demonstrated that Cu(II)-cellulose (representing carboxylate groups) and Cu(II)-phosphate are the main moss surface binding moieties, and the percentage of these sites varies as a function of solution pH. P. patens exposed during one month to Cu{sup 2+} yielded ∼20% of Cu(I) in the form of Cu–S(CN) complexes, suggesting metabolically-controlled reduction of adsorbed and assimilated Cu{sup 2+}.

  10. Mechanosynthesis, crystal structure and magnetic characterization of neodymium orthoferrite

    Energy Technology Data Exchange (ETDEWEB)

    Serna, Pedro Vera; Campos, Cecilio Garcia [Division de Ingenierias, Universidad Politecnica de Tecamac (UPTECAMAC), Tecamac de Felipe Villanueva, Estado de Mexico (Mexico); De Jesus, Felix Sanchez; Miro, Ana Maria Bolarin [Area Academica de Ciencias de la Tierra y Materiales, Universidad Autonoma del Estado de Hidalgo (UAEH), Mineral de la Reforma, Hidalgo (Mexico); Loran, Jose Antonio Juanico [Division de Ingenieria Industrial Nanotecnologia, Universidad Politecnica del Valle de Mexico (UPVM), Tultitlan, Estado de Mexico (Mexico); Longwell, Jeffrey, E-mail: [Department of Languages and Linguistics, New Mexico State University (NMSU), Las Cruces, NM (United States)


    Neodymium orthoferrite NdFeO{sub 3} was obtained at room temperature by mechanosynthesis with a stoichiometric ratio of Nd2O{sub 3} and Fe{sub 2}O{sub 3} powders, whereas the traditional synthesis requires a temperature of approximately 1000 °C. The crystal structure was analyzed by X-ray diffraction analysis using Cu radiation and a LynxEye XE detector, whose strong fluorescence filtering enabled a high signal intensity. The analysis indicated that the obtained crystallites were nano-sized. The particle morphology was observed by scanning electron microscopy, and the magnetic saturation was tested by vibrating sample magnetometry. The synthesis of NdFeO{sub 3} was detected after a few hours of milling, indicating that the milling imparted mechanical energy to the system. (author)

  11. Au-Based Catalysts: Electrochemical Characterization for Structural Insights

    Directory of Open Access Journals (Sweden)

    Valentina Pifferi


    Full Text Available Au-based catalysts are widely used in important processes because of their peculiar characteristics. The catalyst performance depends strongly on the nature and structure of the metal nanoparticles, especially in the case of bimetallic catalysts where synergistic effects between the two metals can be occasionally seen. In this paper, it is shown that electrochemical characterisation (cyclovoltammetry CV and electrochemical impedance spectroscopy EIS of AuPd systems can be used to determine the presence of an electronic interaction between the two metals, thus providing a strong support in the determination of the nature of the synergy between Au and Pd in the liquid phase oxidation of alcohols. However, it seems likely that the strong difference in the catalytic behavior between the single metals and the bimetallic system is connected not only to the redox behaviour, but also to the energetic balance between the different elementary steps of the reaction.

  12. Genetic structure characterization of Chileans reflects historical immigration patterns (United States)

    Eyheramendy, Susana; Martinez, Felipe I.; Manevy, Federico; Vial, Cecilia; Repetto, Gabriela M.


    Identifying the ancestral components of genomes of admixed individuals helps uncovering the genetic basis of diseases and understanding the demographic history of populations. We estimate local ancestry on 313 Chileans and assess the contribution from three continental populations. The distribution of ancestry block-length suggests an average admixing time around 10 generations ago. Sex-chromosome analyses confirm imbalanced contribution of European men and Native-American women. Previously known genes under selection contain SNPs showing large difference in allele frequencies. Furthermore, we show that assessing ancestry is harder at SNPs with higher recombination rates and easier at SNPs with large difference in allele frequencies at the ancestral populations. Two observations, that African ancestry proportions systematically decrease from North to South, and that European ancestry proportions are highest in central regions, show that the genetic structure of Chileans is under the influence of a diffusion process leading to an ancestry gradient related to geography. PMID:25778948

  13. Low Dimensional Semiconductor Structures Characterization, Modeling and Applications

    CERN Document Server

    Horing, Norman


    Starting with the first transistor in 1949, the world has experienced a technological revolution which has permeated most aspects of modern life, particularly over the last generation. Yet another such revolution looms up before us with the newly developed capability to control matter on the nanometer scale. A truly extraordinary research effort, by scientists, engineers, technologists of all disciplines, in nations large and small throughout the world, is directed and vigorously pressed to develop a full understanding of the properties of matter at the nanoscale and its possible applications, to bring to fruition the promise of nanostructures to introduce a new generation of electronic and optical devices. The physics of low dimensional semiconductor structures, including heterostructures, superlattices, quantum wells, wires and dots is reviewed and their modeling is discussed in detail. The truly exceptional material, Graphene, is reviewed; its functionalization and Van der Waals interactions are included h...

  14. Microstructure characterization and magnetic properties of nano structured materials

    Energy Technology Data Exchange (ETDEWEB)

    Sun, X.C


    The present thesis deals with the unique microstructural properties and their novel magnetic properties of core-shell Ni-Ce nano composite particles, carbon encapsulated Fe, Co, and Ni nanoparticles and the nano crystallization behavior of typical ferromagnetic Fe{sub 78}Si{sub 9}B{sub 13} ribbons. These properties have intensively been investigated by high resolution transmission electron microscopy (HREM), X-ray diffraction (XRD), scanning electron microscopy (Sem), X-ray energy dispersive spectroscopy [eds.]; selected area electron diffraction pattern (SAED), Ft-IR, differential scanning calorimeter (DSC). In addition, magnetic moments measurements at different temperatures and applied fields have been performed by transmission Moessbauer spectroscopy, superconducting quantum interference device magnetometer (SQUID), and vibrating sample magnetometer (VSM). The present studies may provide the insights for the better understanding of the correlation between the unique microstructure and novel magnetic properties for several magnetic nano structured materials. (Author)

  15. Structural characterization of core-bradavidin in complex with biotin (United States)

    Agrawal, Nitin; Määttä, Juha A. E.; Kulomaa, Markku S.; Hytönen, Vesa P.; Johnson, Mark S.; Airenne, Tomi T.


    Bradavidin is a tetrameric biotin-binding protein similar to chicken avidin and bacterial streptavidin, and was originally cloned from the nitrogen-fixing bacteria Bradyrhizobium diazoefficiens. We have previously reported the crystal structure of the full-length, wild-type (wt) bradavidin with 138 amino acids, where the C-terminal residues Gly129-Lys138 (“Brad-tag”) act as an intrinsic ligand (i.e. Gly129-Lys138 bind into the biotin-binding site of an adjacent subunit within the same tetramer) and has potential as an affinity tag for biotechnological purposes. Here, the X-ray structure of core-bradavidin lacking the C-terminal residues Gly114-Lys138, and hence missing the Brad-tag, was crystallized in complex with biotin at 1.60 Å resolution [PDB:4BBO]. We also report a homology model of rhodavidin, an avidin-like protein from Rhodopseudomonas palustris, and of an avidin-like protein from Bradyrhizobium sp. Ai1a-2, both of which have the Brad-tag sequence at their C-terminus. Moreover, core-bradavidin V1, an engineered variant of the original core-bradavidin, was also expressed at high levels in E. coli, as well as a double mutant (Cys39Ala and Cys69Ala) of core-bradavidin (CC mutant). Our data help us to further engineer the core-bradavidin–Brad-tag pair for biotechnological assays and chemical biology applications, and provide deeper insight into the biotin-binding mode of bradavidin. PMID:28426764

  16. Structural characterization of core-bradavidin in complex with biotin.

    Directory of Open Access Journals (Sweden)

    Nitin Agrawal

    Full Text Available Bradavidin is a tetrameric biotin-binding protein similar to chicken avidin and bacterial streptavidin, and was originally cloned from the nitrogen-fixing bacteria Bradyrhizobium diazoefficiens. We have previously reported the crystal structure of the full-length, wild-type (wt bradavidin with 138 amino acids, where the C-terminal residues Gly129-Lys138 ("Brad-tag" act as an intrinsic ligand (i.e. Gly129-Lys138 bind into the biotin-binding site of an adjacent subunit within the same tetramer and has potential as an affinity tag for biotechnological purposes. Here, the X-ray structure of core-bradavidin lacking the C-terminal residues Gly114-Lys138, and hence missing the Brad-tag, was crystallized in complex with biotin at 1.60 Å resolution [PDB:4BBO]. We also report a homology model of rhodavidin, an avidin-like protein from Rhodopseudomonas palustris, and of an avidin-like protein from Bradyrhizobium sp. Ai1a-2, both of which have the Brad-tag sequence at their C-terminus. Moreover, core-bradavidin V1, an engineered variant of the original core-bradavidin, was also expressed at high levels in E. coli, as well as a double mutant (Cys39Ala and Cys69Ala of core-bradavidin (CC mutant. Our data help us to further engineer the core-bradavidin-Brad-tag pair for biotechnological assays and chemical biology applications, and provide deeper insight into the biotin-binding mode of bradavidin.

  17. Production and characterization of carbon structures derived from wood (United States)

    Xie, Xinfeng

    The objective of this research was to produce structural carbon materials from wood, a renewable biomaterial, for advanced material application. A broad range of materials were produced for study including carbonized wood, resin infused carbon composites made from carbonized wood, and carbon nanotubes from wood fibers. The effect of slow heating on the properties of carbonized wood was studied and important carbonized wood properties were found to be produced over a range of heating rates and peak temperatures. Slow heating rates promoted the formation and growth of graphene sheets in turbostratic crystallites, which had a significant influence on the electrical resistivity and Young's modulus of the carbonized wood. A reduction in the rate of heating may be beneficial with respect to carbon properties and the prevention of crack production during the manufacture of large monolithic carbon specimens from wood and wood-based materials. Investigation of selected physical and mechanical properties of resin-infused porous carbon composites made from medium density fiberboard demonstrated that the infused material can be used in specific applications, where high mechanical strength is not required but high dimensional stability at elevated-use temperatures, fire safety, or static dissipation and shielding is required. A unique cyclic heating process has been developed to produce carbon nanotubes directly from wood fibers. Study on the oxidative behavior of carbons derived from cellulose and lignin showed that cellulose carbon ablates faster at a lower temperature in air than lignin carbon when they were prepared at temperatures lower than 500°C due to cellulose carbon's lower content of aromatic structures. It is hypothesized that the formation of carbon nanotubes during the cyclic heating process occurred via template synthesis, with the nanochannels formed from the ablation of cellulose fibrils functioning as a template. Evidence of formation of nanochannels has been

  18. Structural characterization of core-bradavidin in complex with biotin. (United States)

    Agrawal, Nitin; Määttä, Juha A E; Kulomaa, Markku S; Hytönen, Vesa P; Johnson, Mark S; Airenne, Tomi T


    Bradavidin is a tetrameric biotin-binding protein similar to chicken avidin and bacterial streptavidin, and was originally cloned from the nitrogen-fixing bacteria Bradyrhizobium diazoefficiens. We have previously reported the crystal structure of the full-length, wild-type (wt) bradavidin with 138 amino acids, where the C-terminal residues Gly129-Lys138 ("Brad-tag") act as an intrinsic ligand (i.e. Gly129-Lys138 bind into the biotin-binding site of an adjacent subunit within the same tetramer) and has potential as an affinity tag for biotechnological purposes. Here, the X-ray structure of core-bradavidin lacking the C-terminal residues Gly114-Lys138, and hence missing the Brad-tag, was crystallized in complex with biotin at 1.60 Å resolution [PDB:4BBO]. We also report a homology model of rhodavidin, an avidin-like protein from Rhodopseudomonas palustris, and of an avidin-like protein from Bradyrhizobium sp. Ai1a-2, both of which have the Brad-tag sequence at their C-terminus. Moreover, core-bradavidin V1, an engineered variant of the original core-bradavidin, was also expressed at high levels in E. coli, as well as a double mutant (Cys39Ala and Cys69Ala) of core-bradavidin (CC mutant). Our data help us to further engineer the core-bradavidin-Brad-tag pair for biotechnological assays and chemical biology applications, and provide deeper insight into the biotin-binding mode of bradavidin.

  19. Biosynthesis and structural characterization of silver nanoparticles from bacterial isolates

    Energy Technology Data Exchange (ETDEWEB)

    Zaki, Sahar, E-mail: [Environmental Biotechnology Department, Genetic Engineering and Biotechnology Research Institute, Mubarak City for Scientific Research and Technology Applications, Alexandria, 21934 New Burgelarab City (Egypt); El Kady, M.F. [Fabrication Technology Department, Advanced Technology and New Materials Research Institute (ATNMRI), Mubarak City for Scientific Research and Technology Applications, Alexandria (Egypt); Abd-El-Haleem, Desouky [Environmental Biotechnology Department, Genetic Engineering and Biotechnology Research Institute, Mubarak City for Scientific Research and Technology Applications, Alexandria, 21934 New Burgelarab City (Egypt)


    Graphical abstract: In this study five bacterial isolates belong to different genera were found to be able to biosynthesize silver nanoparticles. Biosynthesis and spectral characterization are reported here. Highlights: {yields} About 300 bacterial isolates were screened for their ability to produce nanosilvers {yields} Five of them were potential candidates for synthesis of silver nanoparticles {yields} Production of silver nanoparticles was examined using UV-Vis, XRD, SEM and EDS. {yields} The presence of nanoparticles with all five bacterial isolates was confirmed. -- Abstract: This study aimed to develop a green process for biosynthesis of silver nanomaterials by some Egyptian bacterial isolates. This target was achieved by screening an in-house culture collection consists of 300 bacterial isolates for silver nanoparticle formation. Through screening process, it was observed that strains belonging to Escherichia coli (S30, S78), Bacillus megaterium (S52), Acinetobacter sp. (S7) and Stenotrophomonas maltophilia (S54) were potential candidates for synthesis of silver nanoparticles. The extracellular production of silver nanoparticles by positive isolates was investigated by UV-Vis spectroscopy, X-ray diffraction (XRD), transmission electron microscope (TEM), scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS). The results demonstrated that UV-visible spectrum of the aqueous medium containing silver ion showed a peak at 420 nm corresponding to the plasmon absorbance of silver nanoparticles. Scanning electron microscopy micrograph showed formation of silver nanoparticles in the range of 15-50 nm. XRD-spectrum of the silver nanoparticles exhibited 2{theta} values corresponding to the silver nanocrystal that produce in hexagonal and cubic crystal configurations with different plane of orientation. In addition, the signals of the silver atoms were observed by EDS-spectrum analysis that confirms the presence of silver nanoparticles (Ag

  20. Structural properties and hyperfine characterization of Sn-substituted goethites

    Energy Technology Data Exchange (ETDEWEB)

    Larralde, A.L. [INQUIMAE, Departamento de Quimica Inorganica, Analitica y Quimica Fisica, Facultad de Ciencias Exactas y Naturales, Universidad de Buenos Aires (Argentina); Ramos, C.P. [Departamento de Fisica de la Materia Condensada, GIyA - CAC - CNEA, Av. Gral. Paz 1499 (1650), San Martin, Bs. As. (Argentina); Arcondo, B. [Departamento de Fisica, Facultad de Ingenieria, Universidad de Buenos Aires, Av. Paseo Colon 850 (C1063ACV), Bs. As. (Argentina); Tufo, A.E. [INQUIMAE, Departamento de Quimica Inorganica, Analitica y Quimica Fisica, Facultad de Ciencias Exactas y Naturales, Universidad de Buenos Aires (Argentina); Saragovi, C. [Departamento de Fisica de la Materia Condensada, GIyA - CAC - CNEA, Av. Gral. Paz 1499 (1650), San Martin, Bs. As. (Argentina); Sileo, E.E., E-mail: [INQUIMAE, Departamento de Quimica Inorganica, Analitica y Quimica Fisica, Facultad de Ciencias Exactas y Naturales, Universidad de Buenos Aires (Argentina)


    Highlights: Black-Right-Pointing-Pointer Pure and tin-doped goethites were synthesized from Sn(II) solutions at ambient pressure and 70 Degree-Sign C. Black-Right-Pointing-Pointer The Rietveld refinement of PXRD data indicated that Sn partially substituted the Fe(III) ions. Black-Right-Pointing-Pointer The substitution provoked unit cell expansion, and a distortion of the coordination polyhedron. Black-Right-Pointing-Pointer {sup 119}Sn Moessbauer spectroscopy revealed that Sn(II) is incorporated as Sn(IV). Black-Right-Pointing-Pointer {sup 57}Fe Moessbauer spectroscopy showed a lower magnetic coupling as tin concentration increased. - Abstract: Tin-doped goethites obtained by a simple method at ambient pressure and 70 Degree-Sign C were characterized by inductively coupled plasma atomic emission spectrometry, scanning electron microscopy, Rietveld refinement of powder X-ray diffraction data, and {sup 57}Fe and {sup 119}Sn Moessbauer spectroscopy. The particles size and the length to width ratios decreased with tin-doping. Sn partially substituted the Fe(III) ions provoking unit cell expansion and increasing the crystallinity of the particles with enlarged domains that grow in the perpendicular and parallel directions to the anisotropic broadening (1 1 1) axis. Intermetallic E, E Prime and DC distances also change although the variations are not monotonous, indicating different variations in the coordination polyhedron. In general, the Sn-substituted samples present larger intermetallic distances than pure goethite, and the greatest change is shown in the E Prime distance which coincides with the c-parameter. {sup 119}Sn Moessbauer spectroscopy revealed that Sn(II) is incorporated as Sn(IV) in the samples. On the other hand, Fe(II) presence was not detected by {sup 57}Fe Moessbauer spectroscopy, suggesting the existence of vacancies in the Sn-doped samples. A lower magnetic coupling is also evidenced from the average magnetic hyperfine field values obtained as tin

  1. Structural and morphological characterization of CdSe: Mn thin films

    Indian Academy of Sciences (India)


    Jun 24, 2017 ... XRD was used for structural characterization whereas scanning electron microscope shows the surface morphology of the films. XRD spectra reveal that the grown CdSe films are polycrystalline in nature and have cubic structure. The average particle size decreases on doping CdSe with Mn ions.

  2. Mechanical characterization and structural assessment of biocomposites for construction (United States)

    Christian, Sarah Jane

    The objective of this dissertation is to assess whether or not two particular biocomposite materials, made from hemp fabric and cellulose acetate or polyhydroxybutyrate matrices, are capable of being used for structural and/or construction purposes within in the construction and building industry. The objective of this dissertation was addressed by conducting research to meet the following three goals: (1) to measure the basic mechanical properties of hemp/cellulose acetate and hemp/PHB biocomposites and evaluate if they suitable for use in construction applications, (2) to determine how quickly moisture diffuses into the biocomposite materials and how the moisture affects the mechanical behavior, and (3) to determine how well simple models can predict behavior of structural scale laminates in tension and flexure using biocomposite ply behavior. Compression molding was used to manufacturing the biocomposites from hemp fabric and the themoplastic matrices: cellulose acetate and polyhydroxybutyrate. Four methods for determining the fiber volume fraction were evaluated, and the dissolution method, using different solvents for each matrix type, was used to determine the fiber volume fraction for each composite plate manufactured. Both types of biocomposite were tested in tension, compression, shear, and flexure and the measured properties were compared to wood and engineered wood products to assess whether the biocomposite properties are suitable for use in the construction industry. The biocomposites were conditioned in a humid environment to determine the rate of moisture diffusion into the materials. Then saturated specimens and specimens that were saturated and then dried were tested in tension to evaluate how moisture absorption affects the mechanical behavior of the biocomposites. Finally, simple models of laminate behavior based on laminate plate theory were evaluated to determine if ply level behavior could be used to predict structural scale laminate behavior

  3. Characterization and estimation of permeability correlation structure from performance data

    Energy Technology Data Exchange (ETDEWEB)

    Ershaghi, I.; Al-Qahtani, M. [Univ. of Southern California, Los Angeles, CA (United States)


    In this study, the influence of permeability structure and correlation length on the system effective permeability and recovery factors of 2-D cross-sectional reservoir models, under waterflood, is investigated. Reservoirs with identical statistical representation of permeability attributes are shown to exhibit different system effective permeability and production characteristics which can be expressed by a mean and variance. The mean and variance are shown to be significantly influenced by the correlation length. Detailed quantification of the influence of horizontal and vertical correlation lengths for different permeability distributions is presented. The effect of capillary pressure, P{sub c1} on the production characteristics and saturation profiles at different correlation lengths is also investigated. It is observed that neglecting P{sub c} causes considerable error at large horizontal and short vertical correlation lengths. The effect of using constant as opposed to variable relative permeability attributes is also investigated at different correlation lengths. Next we studied the influence of correlation anisotropy in 2-D reservoir models. For a reservoir under five-spot waterflood pattern, it is shown that the ratios of breakthrough times and recovery factors of the wells in each direction of correlation are greatly influenced by the degree of anisotropy. In fully developed fields, performance data can aid in the recognition of reservoir anisotropy. Finally, a procedure for estimating the spatial correlation length from performance data is presented. Both the production performance data and the system`s effective permeability are required in estimating the correlation length.

  4. Structural characterization and immunomodulating activity of polysaccharide from Dendrobium officinale. (United States)

    He, Tao-Bin; Huang, Yan-Ping; Yang, Liu; Liu, Ti-Ti; Gong, Wan-Ying; Wang, Xuan-Jun; Sheng, Jun; Hu, Jiang-Miao


    A neutral heteropolysaccharide (DOP-1-1) consisted by mannose and glucose (5.9:1) with an average molecular weight at about 1.78×10(5) Da was purified from Dendrobium officinale. Based on Fourier transform infrared spectrum (FT-IR) and nuclear magnetic resonance (NMR) spectra, it suggested that partial structure of DOP-1-1 is an O-acetylated glucomannan with β-d configuration in pyranose sugar forms. The immunomodulatory activity of DOP-1-1 was evaluated by secretion level of cytokine (interleukin (IL)-1β and IL-10) and tumor necrosis factor (TNF)-α in vitro. Our results suggested that DOP-1-1 could stimulate cytokine production (TNF-α, IL-1β) in cells. These findings demonstrated that the purified polysaccharide from D. officinale presented significant immune-modulating activities. Furthermore, by Western-blot we can found that the signaling pathways of DOP-1-1 induced immune activities involving ERK1/2 and NF-кB. As to antioxidant activity, DOP-1-1 hadn't showed remarkable scavenging capacity of 1,1-diphenyl-2-picrylhydrazyl radical (DPPH) in contrast with other studies of polysaccharides from D. officinale. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Structural versatility of Metal-organic frameworks: Synthesis and Characterization

    KAUST Repository

    Alsadun, Norah S.


    Metal-Organic Frameworks (MOFs), an emerging class of porous crystalline materials, have shown promising properties for diverse applications such as catalysis, gas storage and separation. The high degree of tunability of MOFs vs other solid materials enable the assembly of advanced materials with fascinating properties for specific applications. Nevertheless, the precise control in the construction of MOFs at the molecular level remains challenging. Particularly, the formation of pre-targeted multi-nuclear Molecular Building Block (MBB) precursors to unveil materials with targeted structural characteristics is captivating. The aim of my master project in the continuous quest of the group of Prof. Eddaoudi in exploring different synthetic pathways to control the assembly of Rare Earth (RE) based MOF. After giving a general overview about MOFs, I will discuss in this thesis the results of my work on the use of tri-topic oriented organic carboxylate building units with the aim to explore the assembly/construction of new porous RE based MOFs. In chapter 2 will discuss the assembly of 3-c linkers with RE metals was then evaluated based on symmetry and angularity of the three connected linkers. The focus of chapter 3 is cerium based MOFs and heterometallic system, based on 3-c ligands with different length and symmetry. Overall, the incompatibility of 3-c ligands with the 12-c cuo MBB did not allow to any formation of higher neuclearity (˃6), but it has resulted in affecting the connectivity of the cluster.

  6. Structural characterization of mammalian bHLH-PAS transcription factors. (United States)

    Wu, Dalei; Rastinejad, Fraydoon


    The mammalian basic helix-loop-helix-PER-ARNT-SIM (bHLH-PAS) transcription factors share common architectural features that include a bHLH DNA-binding domain and tandemly positioned PAS domains. The sixteen members of this family include the hypoxia-inducible factors (HIF-1α and HIF-2α), ARNT (also known as HIF-1β), CLOCK and BMAL1. Most bHLH-PAS proteins have been genetically linked to variety of diseases in humans, including cancers, metabolic syndromes and psychiatric conditions. To function as transcription factors, the bHLH-PAS proteins must form heterodimeric complexes. Recent crystallographic studies of HIF-α-ARNT and CLOCK-BMAL1 complexes have unveiled the organization of their multi-domain bHLH-PAS-A-PAS-B segments, revealing how these architectures can give rise to unique patterns of heterodimerization. As our structural understanding becomes better integrated with ligand-discovery and target gene identification, a more comprehensive picture of their architectural and functional properties will emerge. Copyright © 2016 Elsevier Ltd. All rights reserved.

  7. Crystal structure and characterization of pyrroloquinoline quinone disodium trihydrate

    Directory of Open Access Journals (Sweden)

    Ikemoto Kazuto


    Full Text Available Abstract Background Pyrroloquinoline quinone (PQQ, a tricarboxylic acid, has attracted attention as a growth factor, and its application to supplements and cosmetics is underway. The product used for these purposes is a water-soluble salt of PQQ disodium. Although in the past, PQQ disodiumpentahydrates with a high water concentration were used, currently, low hydration crystals of PQQ disodiumpentahydrates are preferred. Results We prepared a crystal of PQQ disodium trihydrate in a solution of ethanol and water, studied its structure, and analyzed its properties. In the prepared crystal, the sodium atom interacted with the oxygen atom of two carboxylic acids as well as two quinones of the PQQ disodium trihydrate. In addition, the hydration water of the prepared crystal was less than that of the conventional PQQ disodium crystal. From the results of this study, it was found that the color and the near-infrared (NIR spectrum of the prepared crystal changed depending on the water content in the dried samples. Conclusions The water content in the dried samples was restored to that in the trihydrate crystal by placing the samples in a humid environment. In addition, the results of X-ray diffraction (XRD and X-ray diffraction-differential calorimetry (XRD-DSC analyses show that the phase of the trihydrate crystal changed when the crystallization water was eliminated. The dried crystal has two crystalline forms that are restored to the original trihydrate crystals in 20% relative humidity (RH. This crystalline (PQQ disodium trihydrate is stable under normal environment.

  8. Two new bismuth thiourea bromides: crystal structure, growth, and characterization. (United States)

    Li, Ming; Li, R K


    Crystals of two new bismuth thiourea bromides, bismuth trithiourea bromide (Bi[CS(NH2)2]3Br3, BTB) and bismuth protonated-hexathiourea bromide (Bi[CS(NH2)2H]6Br9, BHB), have been successfully grown from hydrobromic acid solution with different pH values by slow evaporation. Single crystal X-ray diffraction reveals that BTB is isostructural to its Cl-analog crystallizing in a monoclinic space group Cc with unit cell dimensions of a = 8.6238(7) Å, b = 12.2506(11) Å, c = 15.5040(13) Å, β = 90.7810(10)° and Z = 4. In contrast, BHB crystallizes in a trigonal space group R3[combining macron]c with unit cell dimensions of a = b = 12.748(17) Å, c = 40.45(11) Å, and Z = 6. The protonation of the thiourea in BHB is confirmed by the structure solution, IR and Raman spectroscopy. The UV diffuse reflection spectra clearly indicate that both of the two crystals have good optical transparency in the range below 2000 nm. Both compounds decompose above 190 °C, and BHB melts at around 140 °C while BTB possesses a phase transition at 145 °C as indicated by thermogravimetric (TG) and differential thermal analysis (DTA).

  9. Towards the Structural Characterization of Intrinsically Disordered Proteins by SAXS and MD Simulation (United States)

    Oroguchi, Tomotaka; Ikeguchi, Mitsunori; Sato, Mamoru


    Dynamical structures of intrinsically disordered proteins (IDPs) and multi-domain proteins that include large ID regions between the domains are unable to be determined by such conventional methods as X-ray crystallography and electron microscopy. Small-angle X-ray scattering (SAXS) is suitable to determine low-resolution structures of proteins and protein complexes in solution, but the structural data on protein dynamics are averaged over the structural ensemble in protein solution. To overcome this problem, we have developed a novel method, named MD-SAXS, of the combined use of SAXS and molecular dynamics (MD) simulation to analyze protein dynamics in solution of multi-subunit protein complexes and multi-domain proteins toward the structural characterization of IDPs. Here we show validity of the method through the structural characterization of restriction Endonuclease EcoO109I.

  10. Synthesis and magnetochemistry of heterometallic triangular FeLn(III) (Ln = La, Gd, Tb, Dy, and Ho) and FeY(III) complexes. (United States)

    Singh, Namrata; Das Gupta, Sayak; Butcher, Raymond J; Christou, George


    A series of Fe2Ln (Ln = La, Gd, Tb, Dy and Ho) and Fe2Y complexes have been synthesized via metal substitution and characterized by single crystal X-ray diffraction. All the molecules are isostructural and have a Fe2LnO triangular core with the oxygen atom existing as an μ3-oxo(2-) anion. DC and AC magnetic susceptibility studies were performed on all the molecules. For Fe2Ln (Ln = Gd, La) and Fe2Y, the data were fitted to Van Vleck equations and the magnetic coupling constants were obtained. In all cases, the two Fe(iii) spins were found to be antiparallel to each other in the ground state leaving the heterometal to remain essentially uncoupled.

  11. Characterization of Power Absorption Response of Periodic 3D Structures to Partially Coherent Fields

    CERN Document Server

    Tihon, Denis; Thomas, Christopher N; Craeye, Christophe


    In many applications of absorbing structures it is important to understand their spatial response to incident fields, for example in thermal solar panels, bolometric imaging and controlling radiative heat transfer. In practice, the illuminating field often originates from thermal sources and is only spatially partially coherent when reaching the absorbing device. In this paper, we present a method to fully characterize the way a structure can absorb such partially coherent fields. The method is presented for any 3D material and accounts for the partial coherence and partial polarization of the incident light. This characterization can be achieved numerically using simulation results or experimentally using the Energy Absorption Interferometry (EAI) that has been described previously in the literature. The absorbing structure is characterized through a set of absorbing functions, onto which any partially coherent field can be projected. This set is compact for any structure of finite extent and the absorbing f...

  12. Low dimensional semiconductor structures. Characterization, modeling and applications

    Energy Technology Data Exchange (ETDEWEB)

    Uenlue, Hilmi [Istanbul Technical Univ. (Turkey). Dept. of Physics Engineering; Horing, Norman J.M. (eds.) [Stevens Institute of Technology, Hoboken, NJ (United States). Dept. of Physics and Engineering Physics


    Gives a state of the art report of important topics in nanoscience. Includes a broad spectrum of areas developing rapidly in nanostructures science and technology. Delivers a tutorial- and review-like presentation. Starting with the first transistor in 1949, the world has experienced a technological revolution which has permeated most aspects of modern life, particularly over the last generation. Yet another such revolution looms up before us with the newly developed capability to control matter on the nanometer scale. A truly extraordinary research effort, by scientists, engineers, technologists of all disciplines, in nations large and small throughout the world, is directed and vigorously pressed to develop a full understanding of the properties of matter at the nanoscale and its possible applications, to bring to fruition the promise of nanostructures to introduce a new generation of electronic and optical devices. The physics of low dimensional semiconductor structures, including heterostructures, superlattices, quantum wells, wires and dots is reviewed and their modeling is discussed in detail. The truly exceptional material, Graphene, is reviewed; its functionalization and Van der Waals interactions are included here. Recent research on optical studies of quantum dots and on the physical properties of one-dimensional quantum wires is also reported. Chapters on fabrication of nanowire - based nanogap devices by the dielectrophoretic assembly approach. The broad spectrum of research reported here incorporates chapters on nanoengineering and nanophysics. In its presentation of tutorial chapters as well as advanced research on nanostructures, this book is ideally suited to meet the needs of newcomers to the field as well as experienced researchers interested in viewing colleagues' recent advances.

  13. Synthesis and structural characterization of scandium SALEN complexes. (United States)

    Meermann, Christian; Sirsch, Peter; Törnroos, Karl W; Anwander, Reiner


    A series of heteroleptic scandium SALEN complexes, [(SALEN)Sc(mu-Cl)]2 and (SALEN)Sc[N(SiHMe2)2] is obtained via amine elimination reactions using [Sc(N(i)Pr2)2(mu-Cl)(THF)]2 and Sc[N(SiHMe2)2]3(THF) as metal precursors, respectively. H(2)SALEN ligand precursors comprising H2Salen [(1,2-ethandiyl)bis(nitrilomethylidyne)bis(2,4-di-tert-butyl)phenol], H2Salpren [(2,2-dimethylpropanediyl)bis(nitrilomethylidyne)bis(2,4-di-tert-butyl)phenol], H2Salcyc [(1R,2R)-(-)-1,2-cyclohexanediyl)bis(nitrilomethylidyne)bis(2,4-di-tert-butyl)phenol] and H2Salphen [((1S,2S)-(-)-1,2-diphenylethandiyl)bis(nitrilomethylidyne)bis(2,4-di-tert-butyl)phenol] are selected according to solubility and ligand backbone variation ("=N-(R)-N=" bite angle) criteria. Consideration is given to the feasibility of [Cl --> NR2] and [N(SiHMe2)2--> OSiR3] secondary ligand exchange reactions. X-ray crystal structure analyses of donor-free (Salpren)Sc(N(i)Pr2), (R,R)-(Salcyc)Sc[N(SiHMe2)2], (Salen)Sc(OSi(t)BuPh2) and (Salphen)Sc(OSiH(t)Bu2) reveal (i) a very short Sc-N bond distance of 2.000(3) A, (ii) weak beta(Si-H)(amido)-Sc agostic interactions and (iii) an exclusive intramolecularly tetradentate and intrinsically bent coordination mode of the SALEN ligands with angle(Ph,Ph) dihedral angles and Sc-[N(2)O(2)] distances in the 124.27(9)-127.7(3) degrees and 0.638(1)-0.688(1) A range, respectively.

  14. Morphological, Mechanical and Structural Characterization of Damselfly Wing (United States)

    Talucdher, ABSM Rupan Ali

    The damselfly belongs to the same insect family as the dragonfly that inspired the development of Micro Air Vehicles (MAVs). Understanding the morphological, mechanical and structural properties of wings, veins and membranes of fly would provide guidelines to develop efficient MAVs. Lack of test methodologies inhibited the progress. The objective of this research was to develop the above methodologies and then measure the properties of veins, membranes and wings of damselflies. The research yielded four test methodologies: fluorescence spectroscopic analysis to map the morphology of vein; axial nanoindentation test to measure indentation properties; micro tension test to measure tensile properties of microscopic components; and a unique vibration test of wings to measure natural frequency, stiffness and air damping factor. Axial indentation test contrasts the transverse indentation used in the past, whose results were corrupted by surface roughness and flexibility of veins. Veins were found to be made of two layered, elliptical tubular members. The thickness of inner and outer layers was about 8 and 5 microm, respectively and corresponding indentation moduli were 8.42 and 16.00 GPa. The modulus of veins agreed with those of human bones. The tensile modulus and strength of veins ranged from 14 to 17 GPa and 232 to 285 MPa, respectively. The damselfly wing was found to vibrate under bending and torsional deformations, the natural frequency (in air) ranged from 130 to 178 Hz, the wing stiffness ranged from 0.18 to 0.30 N/m with the air damping ratio from 0.67 to 0.79. Pathway to develop a material of matching properties is also presented.

  15. Advances in ion mobility-mass spectrometry instrumentation and techniques for characterizing structural heterogeneity. (United States)

    Maurer, Megan M; Donohoe, Gregory C; Valentine, Stephen J


    Over the last decade, the field of ion mobility-mass spectrometry (IM-MS) has experienced dramatic growth in its application toward ion structure characterization. Enabling advances in instrumentation during this time period include improved conformation resolution and ion sensitivity. Such advances have rendered IM-MS a powerful approach for characterizing samples presenting a diverse array of ion structures. The structural heterogeneity that can be interrogated by IM-MS techniques now ranges from samples containing mixtures of small molecules exhibiting a variety of structural types to those containing very large protein complexes and subcomplexes. In addition to this diversity, IM-MS techniques have been used to probe spontaneous and induced structural transformations occurring in solution or the gas phase. To support these measurement efforts, significant advances have been made in theoretical methods aimed at translating IM-MS data into structural information. These efforts have ranged from providing more reliable trial structures for comparison to the experimental measurements to dramatically reducing the time required to calculate collision cross sections for such structures. In this short review, recent advances in developments in IM-MS instrumentation, techniques, and theory are discussed with regard to their implications for characterization of gas- and solution-phase structural heterogeneity.

  16. Identification and Structural Characterization of Unidentified Impurity in Bisoprolol Film-Coated Tablets

    Directory of Open Access Journals (Sweden)

    Ivana Mitrevska


    Full Text Available The aim of this study is the identification, structural characterization, and qualification of a degradation impurity of bisoprolol labeled as Impurity RRT 0.95. This degradation product is considered as a principal thermal degradation impurity identified in bisoprolol film-coated tablets. The impurity has been observed in the stress thermal degradation study of the drug product. Using HPLC/DAD/ESI-MS method, a tentative structure was assigned and afterwards confirmed by detailed structural characterization using NMR spectroscopy. The structure of the target Impurity RRT 0.95 was elucidated as phosphomonoester of bisoprolol, having relative molecular mass of 406 (positive ionization mode. The structural characterization was followed by qualification of Impurity RRT 0.95 using several different in silico methodologies. From the results obtained, it can be concluded that no new structural alerts have been generated for Impurity RRT 0.95 relative to the parent compound bisoprolol. The current study presents an in-depth analysis of the full characterization and qualification of an unidentified impurity in a drug product with the purpose of properly defining the quality specification of the product.

  17. Structural and morphological characterization of CdSe:Mn thin films (United States)

    Singh, Sarika; Shrivastava, A. K.


    CdSe:Mn thin films were grown by chemical bath deposition. The pH of the solution was maintained at 11. Dry films so obtained were annealed in vacuum (10^{-1} Torr) for about 2 h at 400°C. The annealed samples were subjected to morphological and structural characterization using scanning electron microscope and XRD. XRD was used for structural characterization whereas scanning electron microscope shows the surface morphology of the films. XRD spectra reveal that the grown CdSe films are polycrystalline in nature and have cubic structure. The average particle size decreases on doping CdSe with Mn ions. The FE-SEM images show spherical particles having uniform distribution. Optical characterization was done using PL studies and UV-Visible spectrophotometer. PL spectra show an increase in PL intensity on doping. Optical band gap also decreases on doping.

  18. Comprehensive structural and functional characterization of the human kinome by protein structure modeling and ligand virtual screening. (United States)

    Brylinski, Michal; Skolnick, Jeffrey


    The growing interest in the identification of kinase inhibitors, promising therapeutics in the treatment of many diseases, has created a demand for the structural characterization of the entire human kinome. At the outset of the drug development process, the lead-finding stage, approaches that enrich the screening library with bioactive compounds are needed. Here, protein structure based methods can play an important role, but despite structural genomics efforts, it is unlikely that the three-dimensional structures of the entire kinome will be available soon. Therefore, at the proteome level, structure-based approaches must rely on predicted models, with a key issue being their utility in virtual ligand screening. In this study, we employ the recently developed FINDSITE/Q-Dock ligand homology modeling approach, which is well-suited for proteome-scale applications using predicted structures, to provide extensive structural and functional characterization of the human kinome. Specifically, we construct structure models for the human kinome; these are subsequently subject to virtual screening against a library of more than 2 million compounds. To rank the compounds, we employ a hierarchical approach that combines ligand- and structure-based filters. Modeling accuracy is carefully validated using available experimental data with particularly encouraging results found for the ability to identify, without prior knowledge, specific kinase inhibitors. More generally, the modeling procedure results in a large number of predicted molecular interactions between kinases and small ligands that should be of practical use in the development of novel inhibitors. The data set is freely available to the academic community via a user-friendly Web interface at as well as at the ZINC Web site ( ).

  19. Characterizing the geometric and electronic structure of defects in the "29" copper surface oxide (United States)

    Therrien, Andrew J.; Hensley, Alyssa J. R.; Zhang, Renqin; Pronschinske, Alex; Marcinkowski, Matthew D.; McEwen, Jean-Sabin; Sykes, E. Charles H.


    The geometric and electronic structural characterization of thin film metal oxides is of fundamental importance to many fields such as catalysis, photovoltaics, and electrochemistry. Surface defects are also well known to impact a material's performance in any such applications. Here, we focus on the "29" oxide Cu2O/Cu(111) surface and we observe two common structural defects which we characterize using scanning tunneling microscopy/spectroscopy and density functional theory. The defects are proposed to be O vacancies and Cu adatoms, which both show unique topographic and spectroscopic signatures. The spatially resolved electronic and charge state effects of the defects are investigated, and implications for their reactivity are given.

  20. Optical and micro-structural characterizations of MBE grown indium gallium nitride polar quantum dots

    KAUST Repository

    Elafandy, Rami T.


    Comparison between indium rich (27%) InGaN/GaN quantum dots (QDs) and their underlying wetting layer (WL) is performed by means of optical and structural characterizations. With increasing temperature, micro-photoluminescence (μPL) study reveals the superior ability of QDs to prevent carrier thermalization to nearby traps compared to the two dimensional WL. Thus, explaining the higher internal quantum efficiency of the QD nanostructure compared to the higher dimensional WL. Structural characterization (X-ray diffraction (XRD)) and transmission electron microscopy (TEM)) reveal an increase in the QD indium content over the WL indium content which is due to strain induced drifts. © 2011 IEEE.

  1. Simultaneous characterization of cellular RNA structure and function with in-cell SHAPE-Seq. (United States)

    Watters, Kyle E; Abbott, Timothy R; Lucks, Julius B


    Many non-coding RNAs form structures that interact with cellular machinery to control gene expression. A central goal of molecular and synthetic biology is to uncover design principles linking RNA structure to function to understand and engineer this relationship. Here we report a simple, high-throughput method called in-cell SHAPE-Seq that combines in-cell probing of RNA structure with a measurement of gene expression to simultaneously characterize RNA structure and function in bacterial cells. We use in-cell SHAPE-Seq to study the structure-function relationship of two RNA mechanisms that regulate translation in Escherichia coli. We find that nucleotides that participate in RNA-RNA interactions are highly accessible when their binding partner is absent and that changes in RNA structure due to RNA-RNA interactions can be quantitatively correlated to changes in gene expression. We also characterize the cellular structures of three endogenously expressed non-coding RNAs: 5S rRNA, RNase P and the btuB riboswitch. Finally, a comparison between in-cell and in vitro folded RNA structures revealed remarkable similarities for synthetic RNAs, but significant differences for RNAs that participate in complex cellular interactions. Thus, in-cell SHAPE-Seq represents an easily approachable tool for biologists and engineers to uncover relationships between sequence, structure and function of RNAs in the cell. © The Author(s) 2015. Published by Oxford University Press on behalf of Nucleic Acids Research.

  2. Electrical and structural characterization of InAs/InGaAs quantum dot structures on GaAs

    Energy Technology Data Exchange (ETDEWEB)

    Rimada, J.C., E-mail: jcrimada@imem.cnr.i [CNR-IMEM, Parco delle Scienze 37a, I-43100 Parma (Italy); Laboratorio de Celdas Solares, IMRE, Universidad de La Habana, 10400 La Habana (Cuba); Prezioso, M.; Nasi, L.; Gombia, E.; Mosca, R.; Trevisi, G.; Seravalli, L.; Frigeri, P.; Bocchi, C.; Franchi, S. [CNR-IMEM, Parco delle Scienze 37a, I-43100 Parma (Italy)


    In this work we present the results of an electrical and structural characterization of molecular beam epitaxy (MBE) grown InAs/In{sub 0.15}Ga{sub 0.85}As quantum dot (QD) structures having InAs coverages of 2.0 and 3.0 ML that are, respectively, below and above the expected critical value for QD ripening in the InAs/GaAs system. The samples have been investigated by atomic force microscopy (AFM), transmission electron microscope (TEM), capacitance-voltage (C-V), and deep level transient spectroscopy (DLTS) techniques. The results obtained by the above techniques are compared and discussed.

  3. Structural Characterization of the Low-Molecular-Weight Heparin Dalteparin by Combining Different Analytical Strategies

    Directory of Open Access Journals (Sweden)

    Antonella Bisio


    Full Text Available A number of low molecular weight heparin (LMWH products are available for clinical use and although all share a similar mechanism of action, they are classified as distinct drugs because of the different depolymerisation processes of the native heparin resulting in substantial pharmacokinetic and pharmacodynamics differences. While enoxaparin has been extensively investigated, little information is available regarding the LMWH dalteparin. The present study is focused on the detailed structural characterization of Fragmin® by LC-MS and NMR applied both to the whole drug and to its enzymatic products. For a more in-depth approach, size homogeneous octasaccharide and decasaccharide components together with their fractions endowed with high or no affinity toward antithrombin were also isolated and their structural profiles characterized. The combination of different analytical strategies here described represents a useful tool for the assessment of batch-to-batch structural variability and for comparative evaluation of structural features of biosimilar products.

  4. Form and function in hillslope hydrology : In situ imaging and characterization of flow-relevant structures


    Jackisch, Conrad; Angermann, Lisa; Allroggen, Niklas; Sprenger, Matthias; Blume, Theresa; Tronicke, Jens; Zehe, Erwin


    The study deals with the identification and characterization of rapid subsurface flow structures through pedo- and geo-physical measurements and irrigation experiments at the point, plot and hillslope scale. Our investigation of flow-relevant structures and hydrological responses refers to the general interplay of form and function, respectively. To obtain a holistic picture of the subsurface, a large set of different laboratory, exploratory and experimental methods was used...

  5. Synthesis and structural characterization of (Bi2O3)(Y2O3) x and ...

    Indian Academy of Sciences (India)

    Keywords. Fast ion conductors; fluorite structure; fuel cell materials. Abstract. Solid solution series, (Bi2O3)1– (Y2O$_3) and (Bi2O$_3)1– (Gd2O$_3), for = 0.10, 0.20, 0.30 and 0.40 were synthesized by standard ceramic technique. The structural phase characterization was carried out using X-ray powder diffraction ...

  6. Synthesis and structural characterization of some Pb (B $^{'} _ {1/3 ...

    Indian Academy of Sciences (India)

    Two-stage columbite solid state reaction route has been used for the preparation of Pb (B 1 / 3 ′ Nb2/3)O3 materials (B′ = Mg, Ni and Cd). The columbite precursor phase was structurally characterized using diffraction data. MgNb2O6, NiNb2O6 and CdNb2O6 show orthorhombic structures i.e. pure columbite phase.

  7. First structurally characterized mixed-halogen nickel(III) NCN-pincer complex. (United States)

    Kozhanov, Konstantin A; Bubnov, Michael P; Cherkasov, Vladimir K; Fukin, Georgy K; Vavilina, Nina N; Efremova, Larisa Yu; Abakumov, Gleb A


    A square-pyramidal mixed-halogen nickel(III) NCN-pincer complex (PipeNCN)NiClBr (where PipeNCN=2,6-bis(piperidinomethyl)phenyl) was structurally characterized. Bromine occupies apical position; pincer ligand and chlorine atom are in the basal plane. EPR detects that complex in solution exists as a mixture of two structural isomers with bromine or chlorine atoms in the top of pyramid.

  8. X-ray diffraction characterization of suspended structures forMEMS applications

    Energy Technology Data Exchange (ETDEWEB)

    Goudeau, P.; Tamura, N.; Lavelle, B.; Rigo, S.; Masri, T.; Bosseboeuf, A.; Sarnet, T.; Petit, J.-A.; Desmarres, J.-M.


    Mechanical stress control is becoming one of the major challenges for the future of micro and nanotechnologies. Micro scanning X-ray diffraction is one of the promising techniques that allows stress characterization in such complex structures at sub micron scales. Two types of MEMS structure have been studied: a bilayer cantilever composed of a gold film deposited on poly-silicon and a boron doped silicon bridge. X-ray diffraction results are discussed in view of numerical simulation experiments.

  9. Mass Spectrometry Combinations for Structural Characterization of Sulfated-Steroid Metabolites (United States)

    Yan, Yuetian; Rempel, Don L.; Holy, Timothy E.; Gross, Michael L.


    Steroid conjugates, which often occur as metabolites, are challenging to characterize. One application is female-mouse urine, where steroid conjugates serve as important ligands for the pheromone-sensing neurons. Although the two with the highest abundance in mouse urine were previously characterized with mass spectrometry (MS) and NMR to be sulfated steroids, many more exist but remain structurally unresolved. Given that their physical and chemical properties are similar, they are likely to have a sulfated steroid ring structure. Because these compounds occur in trace amounts in mouse urine and elsewhere, their characterization by NMR will be difficult. Thus, MS methods become the primary approach for determining structure. Here, we show that a combination of MS tools is effective for determining the structures of sulfated steroids. Using 4-pregnene analogs, we explored high-resolving power MS (HR-MS) to determine chemical formulae; HD exchange MS (HDX-MS) to determine number of active, exchangeable hydrogens (e.g., OH groups); methoxyamine hydrochloride (MOX) derivatization MS, or reactive desorption electrospray ionization with hydroxylamine to determine the number of carbonyl groups; and tandem MS (MSn), high-resolution tandem MS (HRMS/MS), and GC-MS to obtain structural details of the steroid ring. From the fragmentation studies, we deduced three major fragmentation rules for this class of sulfated steroids. We also show that a combined MS approach is effective for determining structure of steroid metabolites, with important implications for targeted metabolomics in general and for the study of mouse social communication in particular.

  10. Magnetic properties of Cu(phen)(H2O)2SO4 - S= {1}/{2} zigzag ladder with spatially anisotropic exchange coupling (United States)

    Kajňaková, M.; Orendáčová, A.; Orendáč, M.; Park, J.-H.; Kravchyna, O. V.; Anders, A. G.; Černák, J.; Feher, A.; Meisel, M. W.


    Low-temperature specific heat, susceptibility, magnetization, and electron paramagnetic resonance studies of Cu(phen)(H 2O) 2SO 4 have been performed to characterize the magnetic interactions. In contrast to expectations based on structural considerations, the investigations revealed surprisingly weak magnetic correlations which can be ascribed to the non-trivial magnetochemistry of the hydrogen bonds present in the structure.

  11. Characterization of Boroaluminosilicate Glass Surface Structures by B k-edge NEXAFS

    Energy Technology Data Exchange (ETDEWEB)

    R Schaut; R Lobello; K Mueller; C Pantano


    Techniques traditionally used to characterize bulk glass structure (NMR, IR, etc.) have improved significantly, but none provide direct measurement of local atomic coordination of glass surface species. Here, we used Near-Edge X-ray Absorption Fine Structure (NEXAFS) as a direct measure of atomic structure at multicomponent glass surfaces. Focusing on the local chemical structure of boron, we address technique-related issues of calibration, quantification, and interactions of the beam with the material. We demonstrate that beam-induced adsorption and structural damage can occur within the timeframe of typical measurements. The technique is then applied to the study of various fracture surfaces where it is shown that adsorption and reaction of water with boroaluminosilicate glass surfaces induces structural changes in the local coordination of boron, favoring B{sup IV} species after reaction.

  12. Detection, Characterization and Evolution of Internal Repeats in Chitinases of Known 3-D Structure (United States)

    Sivaji, Manigandan; Sadasivam, Vinoth; Narayanasamy, Jayabalan; Samuel, Selvaraj; Fan, Chuanzhu


    Chitinase proteins have evolved and diversified almost in all organisms ranging from prokaryotes to eukaryotes. During evolution, internal repeats may appear in amino acid sequences of proteins which alter the structural and functional features. Here we deciphered the internal repeats from Chitinase and characterized the structural similarities between them. Out of 24 diverse Chitinase sequences selected, six sequences (2CJL, 2DSK, 2XVP, 2Z37, 3EBV and 3HBE) did not contain any internal repeats of amino acid sequences. Ten sequences contained repeats of length Chitinase sequences, 1ITX and 3SIM, were found to be structurally similar when analyzed using secondary structure of Chitinase from secondary and 3-Dimensional structure database of Protein Data Bank. Internal repeats of 3N17 and 1O6I were also involved in the ligand-binding site of those Chitinase proteins, respectively. Our analyses enhance our understanding towards the identification of structural characteristics of internal repeats in Chitinase proteins. PMID:24637574

  13. Electrical network method for the thermal or structural characterization of a conducting material sample or structure (United States)

    Ortiz, Marco G.


    A method for modeling a conducting material sample or structure system, as an electrical network of resistances in which each resistance of the network is representative of a specific physical region of the system. The method encompasses measuring a resistance between two external leads and using this measurement in a series of equations describing the network to solve for the network resistances for a specified region and temperature. A calibration system is then developed using the calculated resistances at specified temperatures. This allows for the translation of the calculated resistances to a region temperature. The method can also be used to detect and quantify structural defects in the system.

  14. Structural Characterization of Lignin in Fruits and Stalks of Chinese Quince

    Directory of Open Access Journals (Sweden)

    Hui-Shuang Yin


    Full Text Available Chinese quince (Chaenomeles sinensis is used in food and pharmaceutical products, but it is seldom eaten as a raw fruit due to its astringent, woody flesh. The structural characterization of lignin fractions from Chinese quince was very important to investigate the structure-activity relationships of lignin. In this investigation, to characterize the structure of lignin in Chinese quince fruits, the milled wood lignin sample was isolated from the fruits (FMWL and the chemical structure of FMWL was investigated by sugar analysis, FT-IR, GPC, pyrolysis-GC/MS analysis, UV spectra analysis, thermogravimetric analysis (TGA, and advanced NMR spectroscopic techniques. In addition, the lignin fraction from the stalk of Chinese quince (SMWL was also prepared for comparison to obtained more information of lignin structure in the fruits. The results showed that the two lignin fractions isolated from fruit and stalk of Chinese quince exhibited different structural features. The two MWL samples were mainly composed of β-O-4 ether bonds, β-5 and β-β′ carbon-carbon linkages in the lignin structural units. Compared to the SMWL, the FMWL fraction had the higher S/G ratio and more carbohydrates linkages. The predominant carbohydrates associated with FMWL and SMWL fractions were glucans-type hemicelluloses and xylan-type hemicelluloses, respectively. Understanding the structure of lignin could give insight into the properties of the lignin and enable the food processing industry to separate lignin more efficiently.

  15. Characterizing Stand Structure and Growth of Natural Beech Forests for the Development of Sustainable Forest Practices

    DEFF Research Database (Denmark)

    Ghalandarayeshi, Shaaban

    forests in northern Iran lack such scientific foundation. The objective of the present study is to assist in this process by characterizing growth and stand structure of oriental beech for a range of growing conditions in northern Iran and to provide useful insight for application in sustainable...

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

    Digital Repository Service at National Institute of Oceanography (India)

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

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

  17. Structural characterization of lead sulfide thin films by means of X ...

    Indian Academy of Sciences (India)


    Structural characterization of lead sulfide thin films by means of X-ray line profile analysis. N CHOUDHURY* and B K SARMA. Department of Physics, Gauhati University, Guwahati 781 014, India. MS received 25 May 2008; revised 25 January 2009. Abstract. X-ray diffraction patterns of chemically deposited lead sulphide ...

  18. DNA binding and cleavage activity of a structurally characterized Ni(II)

    Indian Academy of Sciences (India)

    1375–1381. c Indian Academy of Sciences. DOI 10.1007/s12039-015-0900-4. DNA binding and cleavage activity of a structurally characterized Ni(II). Schiff base complex. SARAT CHANDRA KUMARa, ABHIJIT PALa, MERRY MITRAa,. V M MANIKANDAMATHAVANb, CHIA -HER LINc, BALACHANDRAN UNNI NAIRb,∗.

  19. An integrated approach using orthogonal analytical techniques to characterize heparan sulfate structure. (United States)

    Beccati, Daniela; Lech, Miroslaw; Ozug, Jennifer; Gunay, Nur Sibel; Wang, Jing; Sun, Elaine Y; Pradines, Joël R; Farutin, Victor; Shriver, Zachary; Kaundinya, Ganesh V; Capila, Ishan


    Heparan sulfate (HS), a glycosaminoglycan present on the surface of cells, has been postulated to have important roles in driving both normal and pathological physiologies. The chemical structure and sulfation pattern (domain structure) of HS is believed to determine its biological function, to vary across tissue types, and to be modified in the context of disease. Characterization of HS requires isolation and purification of cell surface HS as a complex mixture. This process may introduce additional chemical modification of the native residues. In this study, we describe an approach towards thorough characterization of bovine kidney heparan sulfate (BKHS) that utilizes a variety of orthogonal analytical techniques (e.g. NMR, IP-RPHPLC, LC-MS). These techniques are applied to characterize this mixture at various levels including composition, fragment level, and overall chain properties. The combination of these techniques in many instances provides orthogonal views into the fine structure of HS, and in other instances provides overlapping / confirmatory information from different perspectives. Specifically, this approach enables quantitative determination of natural and modified saccharide residues in the HS chains, and identifies unusual structures. Analysis of partially digested HS chains allows for a better understanding of the domain structures within this mixture, and yields specific insights into the non-reducing end and reducing end structures of the chains. This approach outlines a useful framework that can be applied to elucidate HS structure and thereby provides means to advance understanding of its biological role and potential involvement in disease progression. In addition, the techniques described here can be applied to characterization of heparin from different sources.

  20. Structure-based phylogeny as a diagnostic for functional characterization of proteins with a cupin fold. (United States)

    Agarwal, Garima; Rajavel, Malligarjunan; Gopal, Balasubramanian; Srinivasan, Narayanaswamy


    The members of cupin superfamily exhibit large variations in their sequences, functions, organization of domains, quaternary associations and the nature of bound metal ion, despite having a conserved beta-barrel structural scaffold. Here, an attempt has been made to understand structure-function relationships among the members of this diverse superfamily and identify the principles governing functional diversity. The cupin superfamily also contains proteins for which the structures are available through world-wide structural genomics initiatives but characterized as "hypothetical". We have explored the feasibility of obtaining clues to functions of such proteins by means of comparative analysis with cupins of known structure and function. A 3-D structure-based phylogenetic approach was undertaken. Interestingly, a dendrogram generated solely on the basis of structural dissimilarity measure at the level of domain folds was found to cluster functionally similar members. This clustering also reflects an independent evolution of the two domains in bicupins. Close examination of structural superposition of members across various functional clusters reveals structural variations in regions that not only form the active site pocket but are also involved in interaction with another domain in the same polypeptide or in the oligomer. Structure-based phylogeny of cupins can influence identification of functions of proteins of yet unknown function with cupin fold. This approach can be extended to other proteins with a common fold that show high evolutionary divergence. This approach is expected to have an influence on the function annotation in structural genomics initiatives.

  1. Structure-based phylogeny as a diagnostic for functional characterization of proteins with a cupin fold.

    Directory of Open Access Journals (Sweden)

    Garima Agarwal


    Full Text Available The members of cupin superfamily exhibit large variations in their sequences, functions, organization of domains, quaternary associations and the nature of bound metal ion, despite having a conserved beta-barrel structural scaffold. Here, an attempt has been made to understand structure-function relationships among the members of this diverse superfamily and identify the principles governing functional diversity. The cupin superfamily also contains proteins for which the structures are available through world-wide structural genomics initiatives but characterized as "hypothetical". We have explored the feasibility of obtaining clues to functions of such proteins by means of comparative analysis with cupins of known structure and function.A 3-D structure-based phylogenetic approach was undertaken. Interestingly, a dendrogram generated solely on the basis of structural dissimilarity measure at the level of domain folds was found to cluster functionally similar members. This clustering also reflects an independent evolution of the two domains in bicupins. Close examination of structural superposition of members across various functional clusters reveals structural variations in regions that not only form the active site pocket but are also involved in interaction with another domain in the same polypeptide or in the oligomer.Structure-based phylogeny of cupins can influence identification of functions of proteins of yet unknown function with cupin fold. This approach can be extended to other proteins with a common fold that show high evolutionary divergence. This approach is expected to have an influence on the function annotation in structural genomics initiatives.

  2. Fabrication and Structure Characterization of Alumina-Aluminum Interpenetrating Phase Composites (United States)

    Dolata, Anna J.


    Alumina-Aluminum composites with interpenetrating networks structure belong to advanced materials with potentially better properties when compared with composites reinforced by particles or fibers. The paper presents the experimental results of fabrication and structure characterization of Al matrix composites locally reinforced via Al2O3 ceramic foam. The composites were obtained using centrifugal infiltration of porous ceramics by liquid aluminum alloy. Both scanning electron microscopy (SEM + EDS) and x-ray tomography were used to determine the structure of foams and composites especially in reinforced areas. The quality of castings, degree of pore filling in ceramic foams by Al alloy, and microstructure in area of interface were assessed.

  3. Magnetochemistry of the Apollo landing sites (United States)

    Wasilewski, P. J.; Fuller, M. D.


    A coherent magnetochemical picture of lunar samples is presented which was determined from a synthesis of available magnetic-property data and corresponding chemical and petrographic data for soils and rock samples collected at the Apollo landing sites. The magnetic properties of the samples are correlated with Al/Si ratio as well as with telescope spectral reflectivity curves, and magnetochemical diagrams based on composition-sensitive magnetic parameters describing the Fe metal and Fe(2+) contents are used to classify the samples. It is shown that the relative metal-fraction size distribution and magnetic stability for different rock types and soils of varying Al/Si values are reflected in a plot of the ratio of saturation isothermal remanence to saturation magnetization vs the ratio of remanent coercive force to coercive force. It is concluded that all the Apollo landing sites have distinct telescope curves correlated with petrology, chemistry, Al/Si values, and magnetic properties. The established correlations suggest the possibility of estimating the magnetic properties of the regolith from remote-sensing observations.

  4. Structural characterization of a recombinant fusion protein by instrumental analysis and molecular modeling.

    Directory of Open Access Journals (Sweden)

    Zhigang Wu

    Full Text Available Conbercept is a genetically engineered homodimeric protein for the treatment of wet age-related macular degeneration (wet AMD that functions by blocking VEGF-family proteins. Its huge, highly variable architecture makes characterization and development of a functional assay difficult. In this study, the primary structure, number of disulfide linkages and glycosylation state of conbercept were characterized by high-performance liquid chromatography, mass spectrometry, and capillary electrophoresis. Molecular modeling was then applied to obtain the spatial structural model of the conbercept-VEGF-A complex, and to study its inter-atomic interactions and dynamic behavior. This work was incorporated into a platform useful for studying the structure of conbercept and its ligand binding functions.

  5. Characterization of oil nano-structures with monochromatic x-ray micro-tomography (United States)

    Asadchikov, Victor E.; Buzmakov, Alexey V.; Osadchaya, Anna S.; Zolotov, Denis A.; Rafailov, Michael K.


    Here we report work done toward detection and characterization of micro-and nano-structures in bitumen, including mineral particles-clay and sand as well as metal-organic micro-and nano-structures containing porphyrines. X-ray micro-tomograph with monochromatic radiation has been used for detection of the structures. In order to detect and characterize nano-and micro-structures tomograph's operational wavelength has been tuned to absorption wavelength of "chemical element of interest" X-ray spectrum: whatever it is Si or porphyrine-forming metals like V, Ni, Co. Contrast between X-ray absorption of micro-structures containing specific element and average bitumen's environment absorption provides a tool for measurement of element mass concentration as well as size and mass density distributions of micro-and nano structures not only on surface but in bitumen volume. Specifically the most interest is in measurement of vanadyl porphyrines and other metal containing chemicals in asphaltene micro-structures changing per asphalten concentration due to bitumen processing.

  6. Structural and vibrational characterization of sugar arabinitol structures employing micro-Raman spectra and DFT calculations (United States)

    Hédoux, Alain; Guinet, Yannick; Carpentier, Laurent; Paccou, Laurent; Derollez, Patrick; Brandán, Silvia Antonia


    In this work, three monomeric forms of arabinitol, usually named arabitol, and their dimeric species have been structural and vibrationally studied by using the micro-Raman spectra in the solid phase accomplished with theoretical calculations based on the theory of the functional of the density (DFT). The hybrid B3LYP method was used for all the calculations together with the 6-31G* and 6-311++g** basis sets. Two different L structures with minima energies were predicted in accordance to the two polymorphic structures revealed by recent X-ray diffraction experiments. The studies by natural bond orbital (NBO) calculations reveals high stabilities of the L form as compared with the D one but the topological properties by using the atoms in molecules (AIM) suggest a higher stability of the D form due to a strong H bond interactions. The scaled mechanical force fields (SQMFF) procedure was used to perform the complete vibrational assignments for the monomeric forms and their dimer. On the other hand, the similarity in the gap values computed for the three forms of arabitol with those observed for sucrose, trehalose, maltose and lactose in gas phase at the same level of theory could partially explain the sweetening property of this alcohol. In addition, the influences of the size of the basis set on some properties were evidenced.

  7. A novel structure of gel grown strontium cyanurate crystal and its structural, optical, electrical characterization (United States)

    Divya, R.; Nair, Lekshmi P.; Bijini, B. R.; Nair, C. M. K.; Gopakumar, N.; Babu, K. Rajendra


    Strontium cyanurate crystals with novel structure and unique optical property like mechanoluminescence have been grown by conventional gel method. Transparent crystals were obtained. The single crystal X-ray diffraction analysis reveals the exquisite structure of the grown crystal. The crystal is centrosymmetric and has a three dimensional polymeric structure. The powder X ray diffraction analysis confirms its crystalline nature. The functional groups present in the crystal were identified by Fourier transform infrared spectroscopy. Elemental analysis confirmed the composition of the complex. A study of thermal properties was done by thermo gravimetric analysis and differential thermal analysis. The optical properties like band gap, refractive index and extinction coefficient were evaluated from the UV visible spectral analysis. The etching study was done to reveal the dislocations in the crystal which in turn explains mechanoluminescence emission. The mechanoluminescence property exhibited by the crystal makes it suitable for stress sensing applications. Besides being a centrosymmetric crystal, it also exhibits NLO behavior. Dielectric properties were studied and theoretical calculations of Fermi energy, valence electron plasma energy, penn gap and polarisability have been done.

  8. Characterization of Slosh Damping for Ortho-Grid and Iso-Grid Internal Tank Structures (United States)

    Westra, Douglas G.; Sansone, Marco D.; Eberhart, Chad J.; West, Jeffrey S.


    Grid stiffened tank structures such as Ortho-Grid and Iso-Grid are widely used in cryogenic tanks for providing stiffening to the tank while reducing mass, compared to tank walls of constant cross-section. If the structure is internal to the tank, it will positively affect the fluid dynamic behavior of the liquid propellant, in regard to fluid slosh damping. As NASA and commercial companies endeavor to explore the solar system, vehicles will by necessity become more mass efficient, and design margin will be reduced where possible. Therefore, if the damping characteristics of the Ortho-Grid and Iso-Grid structure is understood, their positive damping effect can be taken into account in the systems design process. Historically, damping by internal structures has been characterized by rules of thumb and for Ortho-Grid, empirical design tools intended for slosh baffles of much larger cross-section have been used. There is little or no information available to characterize the slosh behavior of Iso-Grid internal structure. Therefore, to take advantage of these structures for their positive damping effects, there is much need for obtaining additional data and tools to characterize them. Recently, the NASA Marshall Space Flight Center conducted both sub-scale testing and computational fluid dynamics (CFD) simulations of slosh damping for Ortho-Grid and Iso-Grid tanks for cylindrical tanks containing water. Enhanced grid meshing techniques were applied to the geometrically detailed and complex Ortho-Grid and Iso-Grid structures. The Loci-STREAM CFD program with the Volume of Fluid Method module for tracking and locating the water-air fluid interface was used to conduct the simulations. The CFD simulations were validated with the test data and new empirical models for predicting damping and frequency of Ortho-Grid and Iso-Grid structures were generated.

  9. Structure and magnetism in Fe-Gd based dinuclear and chain systems. The interplay of weak exchange coupling and zero field splitting effects. (United States)

    Ferbinteanu, Marilena; Cimpoesu, Fanica; Gîrţu, Mihai A; Enachescu, Cristian; Tanase, Stefania


    The synthesis and characterization of two Fe-Gd systems based on bpca(-) (Hbpca = bis(2-pyridilcarbonyl)amine) as bridging ligand is presented, taking the systems as a case study for structure-property correlations. Compound 1, [Fe(LS)(II)(μ-bpca)(2)Gd(NO(3))(2)(H(2)O)]NO(3)·2CH(3)NO(2), is a zigzag polymer, incorporating the diamagnetic low spin Fe(LS)(II) ion. The magnetism of 1 is entirely determined by the weak zero field splitting (ZFS) effect on the Gd(III) ion. Compound 2 is a Fe(III)-Gd(III) dinuclear compound, [Fe(LS)(III)(bpca)(μ-bpca)Gd(NO(3))(4)]·4CH(3)NO(2)·CH(3)OH, its magnetism being interpreted as due to the antiferromagnetic coupling between the S(Fe) = ½ and S(Gd) = 7/2 spins, interplayed with the local ZFS on the lanthanide center. In both systems, the d-f assembly is determined by the bridging capabilities of the ambidentate bpca(-) ligand, which binds the d ion by a tridentate moiety with nitrogen donors and the f center by the diketonate side. We propose a spin delocalization and polarization mechanism that rationalizes the factors leading to the antiferromagnetic d-f coupling. Although conceived for compound 2, the scheme can be proposed as a general mechanism. The rationalization of the weak ZFS effects on Gd(III) by multiconfiguration and spin-orbit ab initio calculations allowed us to determine the details of the small but still significant anisotropy of Gd(III) ion in the coordination sites of compounds 1 and 2. The outlined methodologies and generalized conclusions shed new light on the field of gadolinium coordination magnetochemistry.

  10. Characterizing the Structure and Porosity of Organic Molecules of Intrinsic Microporosity by Molecular Simulations and Experiment (United States)

    Abbott, Lauren J.; McDermott, Amanda G.; Del Regno, Annalaura; Msayib, Kadhum J.; Carta, Mariolino; Taylor, Rupert; McKeown, Neil B.; Siperstein, Flor R.; Runt, James; Colina, Coray M.


    Organic molecules of intrinsic microporosity (OMIMs) are amorphous, glassy solids that contain interconnected pores of sizes smaller than 2 nm. The philosophy behind OMIMs is similar to that of polymers of intrinsic microporosity (PIMs); rigid, awkwardly shaped molecules frustrate packing and form low density materials with intrinsically porous structures. Atomistic simulations were performed on OMIMs using our recently developed packing and compression procedure to study the effect of structure on packing behavior. The structure and porosity of the simulated samples were characterized, such as by surface areas and structure factors, and compared to experimental results. The presented computational procedure will further understanding of structure-property relationships and aid in the design of novel materials with high surface areas. Supported by NSF/Materials World Network/EPSRC.

  11. Revised domain structure of ulvan lyase and characterization of the first ulvan binding domain. (United States)

    Melcher, Rebecca L J; Neumann, Marten; Fuenzalida Werner, Juan Pablo; Gröhn, Franziska; Moerschbacher, Bruno M


    Biomass waste products from green algae have recently been given new life, as these polysaccharides have potential applications in industry, agriculture, and medicine. One such polysaccharide group called ulvans displays many different, potentially useful properties that arise from their structural versatility. Hence, performing structural analyses on ulvan is crucial for future applications. However, chemical reaction-based analysis methods cannot fully characterize ulvan and tend to alter its structure. Thus, better methods require well-characterized ulvan-degrading enzymes. Therefore, we analysed a previously sequenced ulvan lyase (Genebank TM reference number JN104480) and characterized its domains. We suggest that the enzyme consists of a shorter than previously described catalytic domain, a newly identified substrate binding domain, and a C-terminal type 9 secretion system signal peptide. By separately expressing the two domains in E. coli, we confirmed that the binding domain is ulvan specific, having higher affinity for ulvan than most lectins for their ligands (affinity constant: 10 5  M -1 ). To our knowledge, this is the first description of an ulvan-binding domain. Overall, identifying this new binding domain is one step towards engineering ulvan enzymes that can be used to characterize ulvan, e.g. through enzymatic/mass spectrometric fingerprinting analyses, and help unlock its full potential.

  12. Structural and biophysical characterization of human EXTL3: domain organisation, glycosylation and solution structure. (United States)

    Awad, Wael; Kjellstrom, Sven; Svensson Birkedal, Gabriel; Mani, Katrin; Logan, Derek Thomas


    Heparan sulfate proteoglycans are proteins substituted with one or more heparan sulfate (HS) polysaccharides, found in abundance at cell surfaces. HS chains influence the activity of many biologically important molecules involved in cellular communication and signaling. The exostosin (EXT) proteins are glycosyltransferases in the Golgi apparatus that assemble HS chains on HSPGs. The EXTL3 enzyme mainly works as an initiator in HS biosynthesis. In this work, human lumenal N-glycosylated EXTL3 (EXTL3ΔN) was cloned, expressed in human embryonic kidney cells and purified. Various biophysical and biochemical approaches were then employed to elucidate the N-glycosylation sites and the function of their attached N-glycans. Furthermore, the stability and conformation of the purified EXTL3ΔN protein in solution have been analyzed. Our data show that EXTL3ΔN has N-glycans at least at two positions, Asn290 and Asn592, which seem to be critical for proper protein folding and/or release. EXTL3ΔN is quite stable, as high temperature (~59 °C) was required for denaturation. Deconvolution of the EXTL3ΔN far-UV CD spectrum revealed a substantial fraction of β sheets (25%) with a minor proportion of α-helices (14%) in the secondary structure. Solution small angle X-ray scattering and dynamic light scattering revealed an extended structure suggestive of a dimeric arrangement and consisting of two distinct regions, narrow and broad respectively. This is consistent with bioinformatics analyses suggesting a 3-domain structure with two glycosyltransferase domains and a coiled-coil domain.

  13. Test method development for structural characterization of fiber composites at high temperatures (United States)

    Mandell, J. F.; Grande, D. H.; Edwards, B.


    Test methods used for structural characterization of polymer matrix composites can be applied to glass and ceramic matrix composites only at low temperatures. New test methods are required for tensile, compressive, and shear properties of fiber composites at high temperatures. A tensile test which should be useful to at least 1000 C has been developed and used to characterize the properties of a Nicalon/glass composite up to the matrix limiting temperature of 600 C. Longitudinal and transverse unidirectional composite data are presented and discussed.

  14. Synthesis, structural characterization and crystal structure of some dimethyltin complexes containing substituted 1,10-phenanthroline (United States)

    Momeni, Badri Z.; Haghshenas, Fahimeh; Hadi, Saba


    The reaction of dimethyltin dichloride with four substituted 1, 10- phenanthroline has been studied. The reactions of dimethyltin dichloride with 5-methyl-1,10-phenanthroline (Mephen); 5,6-dimethyl-1,10-phenanthroline (Me2phen); 5-nitro-1,10-phenanthroline (NO2phen); 5-chloro-1,10-phenanthroline (Clphen) resulted in the formation of the hexa-coordinated complexes of [SnMe2Cl2(NN)] {Mephen (1), Me2phen (2), NO2phen (3), Clphen (4)}. The resulting products have been fully characterized by elemental analysis, multinuclear (1H, 13C, 119Sn) NMR, DEPT-135, HHCOSY and HSQC NMR spectroscopy. The solid state X-ray determination of complexes [SnMe2Cl2(Mephen)] (1) and [SnMe2Cl2(Me2phen)] (2) revealed that the complexes 1 and 2 contain the hexa-coordinated tin(IV) atom in an octahedral geometry with the trans-[SnMe2] configuration. The Snsbnd N bond distances in 1-2 are 2.47-2.48 Å which are almost among the largest values.

  15. Structural characterization of nonactive site, TrkA-selective kinase inhibitors

    Energy Technology Data Exchange (ETDEWEB)

    Su, Hua-Poo; Rickert, Keith; Burlein, Christine; Narayan, Kartik; Bukhtiyarova, Marina; Hurzy, Danielle M.; Stump, Craig A.; Zhang, Xufang; Reid, John; Krasowska-Zoladek, Alicja; Tummala, Srivanya; Shipman, Jennifer M.; Kornienko, Maria; Lemaire, Peter A.; Krosky, Daniel; Heller, Amanda; Achab, Abdelghani; Chamberlin, Chad; Saradjian, Peter; Sauvagnat, Berengere; Yang, Xianshu; Ziebell, Michael R.; Nickbarg, Elliott; Sanders, John M.; Bilodeau, Mark T.; Carroll, Steven S.; Lumb, Kevin J.; Soisson, Stephen M.; Henze, Darrell A.; Cooke, Andrew J. (Merck)


    Current therapies for chronic pain can have insufficient efficacy and lead to side effects, necessitating research of novel targets against pain. Although originally identified as an oncogene, Tropomyosin-related kinase A (TrkA) is linked to pain and elevated levels of NGF (the ligand for TrkA) are associated with chronic pain. Antibodies that block TrkA interaction with its ligand, NGF, are in clinical trials for pain relief. Here, we describe the identification of TrkA-specific inhibitors and the structural basis for their selectivity over other Trk family kinases. The X-ray structures reveal a binding site outside the kinase active site that uses residues from the kinase domain and the juxtamembrane region. Three modes of binding with the juxtamembrane region are characterized through a series of ligand-bound complexes. The structures indicate a critical pharmacophore on the compounds that leads to the distinct binding modes. The mode of interaction can allow TrkA selectivity over TrkB and TrkC or promiscuous, pan-Trk inhibition. This finding highlights the difficulty in characterizing the structure-activity relationship of a chemical series in the absence of structural information because of substantial differences in the interacting residues. These structures illustrate the flexibility of binding to sequences outside of—but adjacent to—the kinase domain of TrkA. This knowledge allows development of compounds with specificity for TrkA or the family of Trk proteins.

  16. Characterization of carbohydrate structures of bovine MUC15 and distribution of the mucin in bovine milk

    DEFF Research Database (Denmark)

    Pallesen, Lone Tjener; Pedersen, Lise Refstrup Linnebjerg; Petersen, Torben Ellebæk


    The present work reports the characterization of carbohydrate structures and the distribution of the newly identified mucin MUC15, a highly glycosylated protein associated with the bovine milk fat globule membrane (MFGM). Distribution of MUC15 was investigated in various fractions of bovine milk......-containing fractions as well, such as skim milk and whey. Compositional and structural studies of the carbohydrates of bovine milk MUC15 showed that the glycans are composed of fucose, galactose, mannose, N-acetylgalactosamine, N-acetylglycosamine, and sialic acid. The carbohydrate was shown to constitute 65......-linked glycans were shown to contain mainly hybrid-type N-glycans. In addition, the N-glycans were shown to be sialylated and contain terminal poly-lactosamine structures. The O-linked glycans were found to constitute some unsubstituted Core-1 structures and a substantial number of sialylated Core-1 O...

  17. Synthesis, structure characterizations, and theoretical studies of novel tricyclic multiple(urea) molecules (United States)

    Zhang, Junlin; Liu, Yingzhe; Bi, Fuqiang; Zhou, Jing; Wang, Bozhou


    Three novel Bn-protected tricyclic multiple(urea) molecules were synthesized and characterized by 1H NMR, 13C NMR, FT-IR and elementary analysis. Structures of the Bn-protected tricyclic tris(urea) and bis(urea) molecules were further characterized by X-ray single-crystal diffraction analysis, indicating the urea carbonyl group has great influence on the molecular conformation and chemical reactivity. The electrostatic potentials on isosurfaces of electron density of the crystal structures obtained were studied by B3LYP/6-311G(d,p) method and Hirshfeld surface analysis were carried out to identify and quantify the interaction nature and proportion in crystals.

  18. Foam injection molding of thermoplastic elastomers: Blowing agents, foaming process and characterization of structural foams (United States)

    Ries, S.; Spoerrer, A.; Altstaedt, V.


    Polymer foams play an important role caused by the steadily increasing demand to light weight design. In case of soft polymers, like thermoplastic elastomers (TPE), the haptic feeling of the surface is affected by the inner foam structure. Foam injection molding of TPEs leads to so called structural foam, consisting of two compact skin layers and a cellular core. The properties of soft structural foams like soft-touch, elastic and plastic behavior are affected by the resulting foam structure, e.g. thickness of the compact skins and the foam core or density. This inner structure can considerably be influenced by different processing parameters and the chosen blowing agent. This paper is focused on the selection and characterization of suitable blowing agents for foam injection molding of a TPE-blend. The aim was a high density reduction and a decent inner structure. Therefore DSC and TGA measurements were performed on different blowing agents to find out which one is appropriate for the used TPE. Moreover a new analyzing method for the description of processing characteristics by temperature dependent expansion measurements was developed. After choosing suitable blowing agents structural foams were molded with different types of blowing agents and combinations and with the breathing mold technology in order to get lower densities. The foam structure was analyzed to show the influence of the different blowing agents and combinations. Finally compression tests were performed to estimate the influence of the used blowing agent and the density reduction on the compression modulus.

  19. Quantitative Acoustic Emission Fatigue Crack Characterization in Structural Steel and Weld

    Directory of Open Access Journals (Sweden)

    Adutwum Marfo


    Full Text Available The fatigue crack growth characteristics of structural steel and weld connections are analyzed using quantitative acoustic emission (AE technique. This was experimentally investigated by three-point bending testing of specimens under low cycle constant amplitude loading using the wavelet packet analysis. The crack growth sequence, that is, initiation, crack propagation, and fracture, is extracted from their corresponding frequency feature bands, respectively. The results obtained proved to be superior to qualitative AE analysis and the traditional linear elastic fracture mechanics for fatigue crack characterization in structural steel and welds.

  20. Characterization of nano structured metallic materials; Caracterizacion de materiales metalicos nanoestructurados

    Energy Technology Data Exchange (ETDEWEB)

    Marin A, M.; Gutierrez W, C.; Cruz C, R.; Angeles C, C. [Instituto Nacional de Investigaciones Nucleares, A.P. 18-1027, 11801 Mexico D.F. (Mexico)


    Nowadays the search of new materials with specific optical properties has carried out to realize a series of experiments through the polymer synthesis [(C{sub 3}N{sub 3}){sub 2} (NH){sub 3}]{sub n} doped with gold metallic nanoparticles. The thermal stability of a polymer is due to the presence of tyazine rings contained in the structure. The samples were characterized by High Resolution Transmission Electron Microscopy, X-ray diffraction by the Powder method, Ft-infrared and its thermal properties by Differential Scanning Calorimetry (DSC) and Thermogravimetry (TGA). One of the purposes of this work is to obtain nano structured materials over a polymeric matrix. (Author)

  1. Structural characterization of the nickel thin film deposited by glad technique

    Directory of Open Access Journals (Sweden)

    Potočnik J.


    Full Text Available In this work, a columnar structure of nickel thin film has been obtained using an advanced deposition technique known as Glancing Angle Deposition. Nickel thin film was deposited on glass sample at the constant emission current of 100 mA. Glass sample was positioned 15 degrees with respect to the nickel vapor flux. The obtained nickel thin film was characterized by Force Modulation Atomic Force Microscopy and by Scanning Electron Microscopy. Analysis indicated that the formation of the columnar structure occurred at the film thickness of 1 μm, which was achieved for the deposition time of 3 hours. [Projekat Ministarstva nauke Republike Srbije, br. III45005


    Directory of Open Access Journals (Sweden)

    Birgit Neitzel


    Full Text Available Polymers have various interesting properties, which depend largely on their inner structure. One way to influence the macroscopic behaviour is the deformation of the polymer chains, which effects the change in microstructure. For analyzing the microstructure of non-deformed and deformed polymer materials, Raman spectroscopy as well as differential scanning calorimetry (DSC were used. In the present study we compare the results for crystallinity measurements of deformed polymers using both methods in order to characterize the differences in micro-structure due to deformation. The study is ongoing, and we present the results of the first tests.

  3. Fabrication and characterization of 3D pn junction structure for radiation detection (United States)

    Liu, Tingting; Liu, Tao; Li, Jinlong; Lin, Jilei; Chen, Xiaoming; Guo, Xinglong; Xin, Peisheng; Xu, Shaohui; Xue, Weijia; Wang, Lianwei


    In this report, p-type macroporous silicon has been prepared by anodization. A phosphorus diffusion step is employed for the formation of three dimensional pn junction structures on this macroporous silicon. I-V and C-V measurement were employed to characterize the electrical properties. The results were compared with numeric simulation with T-SUPREM4 and MEDICI. It has been demonstrated that three-dimensional structure can increase the effective junction area and the collective efficiency remarkably, and hence improve the performance of semiconductor radiation detector.

  4. Computational Methods for Protein Structure Prediction and Modeling Volume 1: Basic Characterization

    CERN Document Server

    Xu, Ying; Liang, Jie


    Volume one of this two volume sequence focuses on the basic characterization of known protein structures as well as structure prediction from protein sequence information. The 11 chapters provide an overview of the field, covering key topics in modeling, force fields, classification, computational methods, and struture prediction. Each chapter is a self contained review designed to cover (1) definition of the problem and an historical perspective, (2) mathematical or computational formulation of the problem, (3) computational methods and algorithms, (4) performance results, (5) existing software packages, and (6) strengths, pitfalls, challenges, and future research directions.

  5. Characterization and structural analysis of an active particulate methane monooxygenase trimer from Methylococcus capsulatus (Bath). (United States)

    Kitmitto, Ashraf; Myronova, Natalia; Basu, Piku; Dalton, Howard


    The oxidation of methane to methanol in methanotrophs is catalyzed by the enzyme methane monooxygenase (MMO). Two distinct forms of this enzyme exist, a soluble cytoplasmic MMO (sMMO) and a membrane-bound particulate form (pMMO). We describe here the biochemical characterization of a stable and active purified pMMO hydroxylase (pMMO-H) and report a three-dimensional (3D) structure, determined by electron microscopy and single-particle analysis at 23 A resolution. Both biochemical and structural data indicate that pMMO hydroxylase is trimeric, with each monomer unit comprised of three polypeptides of 47, 26, and 23 kDa. Comparison of the recent crystal structure [Lieberman, R. L., and Rosenzweig, A. C. (2005) Nature 434, 177] of an uncharacterized pMMO-H complex with the three-dimensional (3D) structure determined here yielded a good match between the principal features and the organization of the enzyme monomers into trimers. The data presented here advance our current understanding of particulate methane monooxygenase function by the characterization of an active form of the enzyme and the corresponding 3D structure.

  6. Biophysical characterization of recombinant proteins: a key to higher structural genomics success. (United States)

    Vedadi, Masoud; Arrowsmith, Cheryl H; Allali-Hassani, Abdellah; Senisterra, Guillermo; Wasney, Gregory A


    Hundreds of genomes have been successfully sequenced to date, and the data are publicly available. At the same time, the advances in large-scale expression and purification of recombinant proteins have paved the way for structural genomics efforts. Frequently, however, little is known about newly expressed proteins calling for large-scale protein characterization to better understand their biochemical roles and to enable structure-function relationship studies. In the Structural Genomics Consortium (SGC), we have established a platform to characterize large numbers of purified proteins. This includes screening for ligands, enzyme assays, peptide arrays and peptide displacement in a 384-well format. In this review, we describe this platform in more detail and report on how our approach significantly increases the success rate for structure determination. Coupled with high-resolution X-ray crystallography and structure-guided methods, this platform can also be used toward the development of chemical probes through screening families of proteins against a variety of chemical series and focused chemical libraries.

  7. Unexpected structural complexity of supernumerary marker chromosomes characterized by microarray comparative genomic hybridization

    Directory of Open Access Journals (Sweden)

    Hing Anne V


    Full Text Available Abstract Background Supernumerary marker chromosomes (SMCs are structurally abnormal extra chromosomes that cannot be unambiguously identified by conventional banding techniques. In the past, SMCs have been characterized using a variety of different molecular cytogenetic techniques. Although these techniques can sometimes identify the chromosome of origin of SMCs, they are cumbersome to perform and are not available in many clinical cytogenetic laboratories. Furthermore, they cannot precisely determine the region or breakpoints of the chromosome(s involved. In this study, we describe four patients who possess one or more SMCs (a total of eight SMCs in all four patients that were characterized by microarray comparative genomic hybridization (array CGH. Results In at least one SMC from all four patients, array CGH uncovered unexpected complexity, in the form of complex rearrangements, that could have gone undetected using other molecular cytogenetic techniques. Although array CGH accurately defined the chromosome content of all but two minute SMCs, fluorescence in situ hybridization was necessary to determine the structure of the markers. Conclusion The increasing use of array CGH in clinical cytogenetic laboratories will provide an efficient method for more comprehensive characterization of SMCs. Improved SMC characterization, facilitated by array CGH, will allow for more accurate SMC/phenotype correlation.

  8. Partial structural characterization of pectin cell wall from Argania spinosa leaves


    Hachem, Kadda; Benabdesslem, Yasmina; Ghomari, Samia; Hasnaoui, Okkacha; Kaid-Harche, Meriem


    The pectin polysaccharides from leaves of Argania spinosa (L.) Skeels, collected from Stidia area in the west coast of northern Algeria, were investigated by using sequential extractions and the resulting fractions were analysed for monosaccharide composition and chemical structure. Water-soluble pectic (ALS-WSP) and chelating-soluble pectic (ALS-CSP) fractions were obtained, de-esterified and fractionated by anion-exchange chromatography and characterized by sugar analysis combined with meth...

  9. Structural characterization of the lipid A component of pathogenic Neisseria meningitidis.


    Kulshin, V A; Zähringer, U; Lindner, B; Frasch, C E; Tsai, C M; Dmitriev, B A; Rietschel, E T


    The lipid A component of meningococcal lipopolysaccharide was structurally characterized by using chemical modification methods, methylation analysis, 31P nuclear magnetic resonance, and laser desorption mass spectroscopy. It was shown that Neisseria meningitidis lipid A consists of a 1,4'-bisphosphorylated beta(1'----6)-linked D-glucosamine disaccharide (lipid A backbone), both phosphate groups being largely replaced by O-phosphorylethanolamine. This disaccharide harbors two nonsubstituted h...

  10. IR and UV Photodissociation as Analytical Tools for Characterizing Lipid A Structures


    Madsen, James A.; Cullen, Thomas W.; Trent, M. Stephen; Brodbelt, Jennifer S.


    The utility of 193 nm ultraviolet photodissociation (UVPD) and 10.6 μm infrared multiphoton dissociation (IRMPD) for characterization of lipid A structures was assessed in an ion trap mass spectrometer. The fragmentation behavior of lipid A species was also evaluated by activated – electron photodetachment (a-EPD), which uses 193 nm photons to create charge reduced radicals that are subsequently dissociated by collisional activation. In contrast to collision induced dissociation (CID), IRMPD ...

  11. Dispersed metal cluster catalysts by design. Synthesis, characterization, structure, and performance

    Energy Technology Data Exchange (ETDEWEB)

    Arslan, Ilke [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Dixon, David A. [Univ. of Alabama, Tuscaloosa, AL (United States); Gates, Bruce C. [Univ. of California, Davis, CA (United States); Katz, Alexander [Univ. of California, Berkeley, CA (United States)


    To understand the class of metal cluster catalysts better and to lay a foundation for the prediction of properties leading to improved catalysts, we have synthesized metal catalysts with well-defined structures and varied the cluster structures and compositions systematically—including the ligands bonded to the metals. These ligands include supports and bulky organics that are being tuned to control both the electron transfer to or from the metal and the accessibility of reactants to influence catalytic properties. We have developed novel syntheses to prepare these well-defined catalysts with atomic-scale control the environment by choice and placement of ligands and applied state-of-the art spectroscopic, microscopic, and computational methods to determine their structures, reactivities, and catalytic properties. The ligands range from nearly flat MgO surfaces to enveloping zeolites to bulky calixarenes to provide controlled coverages of the metal clusters, while also enforcing unprecedented degrees of coordinative unsaturation at the metal site—thereby facilitating bonding and catalysis events at exposed metal atoms. With this wide range of ligand properties and our arsenal of characterization tools, we worked to achieve a deep, fundamental understanding of how to synthesize robust supported and ligand-modified metal clusters with controlled catalytic properties, thereby bridging the gap between active site structure and function in unsupported and supported metal catalysts. We used methods of organometallic and inorganic chemistry combined with surface chemistry for the precise synthesis of metal clusters and nanoparticles, characterizing them at various stages of preparation and under various conditions (including catalytic reaction conditions) and determining their structures and reactivities and how their catalytic properties depend on their compositions and structures. Key characterization methods included IR, NMR, and EXAFS spectroscopies to identify

  12. Structural characterization of genomes by large scale sequence-structure threading: application of reliability analysis in structural genomics

    Directory of Open Access Journals (Sweden)

    Brunham Robert C


    Full Text Available Abstract Background We establish that the occurrence of protein folds among genomes can be accurately described with a Weibull function. Systems which exhibit Weibull character can be interpreted with reliability theory commonly used in engineering analysis. For instance, Weibull distributions are widely used in reliability, maintainability and safety work to model time-to-failure of mechanical devices, mechanisms, building constructions and equipment. Results We have found that the Weibull function describes protein fold distribution within and among genomes more accurately than conventional power functions which have been used in a number of structural genomic studies reported to date. It has also been found that the Weibull reliability parameter β for protein fold distributions varies between genomes and may reflect differences in rates of gene duplication in evolutionary history of organisms. Conclusions The results of this work demonstrate that reliability analysis can provide useful insights and testable predictions in the fields of comparative and structural genomics.

  13. Structure of dehaloperoxidase B at 1.58 Å resolution and structural characterization of the AB dimer from Amphitrite ornata

    Energy Technology Data Exchange (ETDEWEB)

    de Serrano, Vesna; D; Antonio, Jennifer; Franzen, Stefan; Ghiladi, Reza A. (NCSU)


    As members of the globin superfamily, dehaloperoxidase (DHP) isoenzymes A and B from the marine annelid Amphitrite ornata possess hemoglobin function, but they also exhibit a biologically relevant peroxidase activity that is capable of converting 2,4,6-trihalophenols to the corresponding 2,6-dihaloquinones in the presence of hydrogen peroxide. Here, a comprehensive structural study of recombinant DHP B, both by itself and cocrystallized with isoenzyme A, using X-ray diffraction is presented. The structure of DHP B refined to 1.58 {angstrom} resolution exhibits the same distal histidine (His55) conformational flexibility as that observed in isoenzyme A, as well as additional changes to the distal and proximal hydrogen-bonding networks. Furthermore, preliminary characterization of the DHP AB heterodimer is presented, which exhibits differences in the AB interface that are not observed in the A-only or B-only homodimers. These structural investigations of DHP B provide insights that may relate to the mechanistic details of the H{sub 2}O{sub 2}-dependent oxidative dehalogenation reaction catalyzed by dehaloperoxidase, present a clearer description of the function of specific residues in DHP at the molecular level and lead to a better understanding of the paradigms of globin structure-function relationships.

  14. Characterization of a Novel Water Pocket Inside the Human Cx26 Hemichannel Structure (United States)

    Araya-Secchi, Raul; Perez-Acle, Tomas; Kang, Seung-gu; Huynh, Tien; Bernardin, Alejandro; Escalona, Yerko; Garate, Jose-Antonio; Martínez, Agustin D.; García, Isaac E.; Sáez, Juan C.; Zhou, Ruhong


    Connexins (Cxs) are a family of vertebrate proteins constituents of gap junction channels (GJCs) that connect the cytoplasm of adjacent cells by the end-to-end docking of two Cx hemichannels. The intercellular transfer through GJCs occurs by passive diffusion allowing the exchange of water, ions, and small molecules. Despite the broad interest to understand, at the molecular level, the functional state of Cx-based channels, there are still many unanswered questions regarding structure-function relationships, perm-selectivity, and gating mechanisms. In particular, the ordering, structure, and dynamics of water inside Cx GJCs and hemichannels remains largely unexplored. In this work, we describe the identification and characterization of a believed novel water pocket—termed the IC pocket—located in-between the four transmembrane helices of each human Cx26 (hCx26) monomer at the intracellular (IC) side. Using molecular dynamics (MD) simulations to characterize hCx26 internal water structure and dynamics, six IC pockets were identified per hemichannel. A detailed characterization of the dynamics and ordering of water including conformational variability of residues forming the IC pockets, together with multiple sequence alignments, allowed us to propose a functional role for this cavity. An in vitro assessment of tracer uptake suggests that the IC pocket residue Arg-143 plays an essential role on the modulation of the hCx26 hemichannel permeability. PMID:25099799

  15. A model based bayesian solution for characterization of complex damage scenarios in aerospace composite structures. (United States)

    Reed, H; Leckey, Cara A C; Dick, A; Harvey, G; Dobson, J


    Ultrasonic damage detection and characterization is commonly used in nondestructive evaluation (NDE) of aerospace composite components. In recent years there has been an increased development of guided wave based methods. In real materials and structures, these dispersive waves result in complicated behavior in the presence of complex damage scenarios. Model-based characterization methods utilize accurate three dimensional finite element models (FEMs) of guided wave interaction with realistic damage scenarios to aid in defect identification and classification. This work describes an inverse solution for realistic composite damage characterization by comparing the wavenumber-frequency spectra of experimental and simulated ultrasonic inspections. The composite laminate material properties are first verified through a Bayesian solution (Markov chain Monte Carlo), enabling uncertainty quantification surrounding the characterization. A study is undertaken to assess the efficacy of the proposed damage model and comparative metrics between the experimental and simulated output. The FEM is then parameterized with a damage model capable of describing the typical complex damage created by impact events in composites. The damage is characterized through a transdimensional Markov chain Monte Carlo solution, enabling a flexible damage model capable of adapting to the complex damage geometry investigated here. The posterior probability distributions of the individual delamination petals as well as the overall envelope of the damage site are determined. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. PREFACE: Symposium 1: Advanced Structure Analysis and Characterization of Ceramic Materials (United States)

    Yashima, Masatomo


    Preface to Symposium 1 (Advanced Structure Analysis and Characterization of Ceramic Materials) of the International Congress of Ceramics III, held 14-18 November 2010 in Osaka, Japan Remarkable developments have been made recently in the structural analysis and characterization of inorganic crystalline and amorphous materials, such as x-ray, neutron, synchrotron and electron diffraction, x-ray/neutron scattering, IR/Raman scattering, NMR, XAFS, first-principle calculations, computer simulations, Rietveld analysis, the maximum-entropy method, in situ measurements at high temperatures/pressures and electron/nuclear density analysis. These techniques enable scientists to study not only static and long-range periodic structures but also dynamic and short-/intermediate-range structures. Multi-scale characterization from the electron to micrometer levels is becoming increasingly important as a means of understanding phenomena at the interfaces, grain boundaries and surfaces of ceramic materials. This symposium has discussed the structures and structure/property relationships of various ceramic materials (electro, magnetic and optical ceramics; energy and environment related ceramics; bio-ceramics; ceramics for reliability secure society; traditional ceramics) through 38 oral presentations including 8 invited lectures and 49 posters. Best poster awards were given to six excellent poster presentations (Y-C Chen, Tokyo Institute of Technology; C-Y Chung, Tohoku University; T Stawski, University of Twente; Y Hirano, Nagoya Institute of Technology; B Bittova, Charles University Prague; Y Onodera, Kyoto University). I have enjoyed working with my friends in the ICC3 conference. I would like to express special thanks to other organizers: Professor Scott T Misture, Alfred University, USA, Professor Xiaolong Chen, Institute of Physics, CAS, China, Professor Takashi Ida, Nagoya Institute of Technology, Japan, Professor Isao Tanaka, Kyoto University, Japan. I also acknowledge the

  17. Structural characterization of ether lipids from the archaeon Sulfolobus islandicus by high-resolution shotgun lipidomics. (United States)

    Jensen, Sara Munk; Brandl, Martin; Treusch, Alexander H; Ejsing, Christer S


    The molecular structures, biosynthetic pathways and physiological functions of membrane lipids produced by organisms in the domain Archaea are poorly characterized as compared with that of counterparts in Bacteria and Eukaryota. Here we report on the use of high-resolution shotgun lipidomics to characterize, for the first time, the lipid complement of the archaeon Sulfolobus islandicus. To support the identification of lipids in S. islandicus, we first compiled a database of ether lipid species previously ascribed to Archaea. Next, we analyzed the lipid complement of S. islandicus by high-resolution Fourier transform mass spectrometry using an ion trap-orbitrap mass spectrometer. This analysis identified five clusters of molecular ions that matched ether lipids in the database with sub-ppm mass accuracy. To structurally characterize and validate the identities of the potential lipid species, we performed structural analysis using multistage activation on the ion trap-orbitrap instrument as well as tandem mass analysis using a quadrupole time-of-flight machine. Our analysis identified four ether lipid species previously reported in Archaea, and one ether lipid species that had not been described before. This uncharacterized lipid species features two head group structures composed of a trisaccharide residue carrying an uncommon sulfono group (-SO3) and an inositol phosphate group. Both head groups are linked to a glycerol dialkyl glycerol tetraether core structure having isoprenoid chains with a total of 80 carbon atoms and 4 cyclopentane moieties. The shotgun lipidomics approach deployed here defines a novel workflow for exploratory lipid profiling of Archaea. Copyright © 2015 John Wiley & Sons, Ltd.

  18. Characterization of Novel Thin-Films and Structures for Integrated Circuit and Photovoltaic Applications (United States)

    Zhao, Zhao

    Thin films have been widely used in various applications. This research focuses on the characterization of novel thin films in the integrated circuits and photovoltaic techniques. The ion implanted layer in silicon can be treated as ion implanted thin film, which plays an essential role in the integrated circuits fabrication. Novel rapid annealing methods, i.e. microwave annealing and laser annealing, are conducted to activate ion dopants and repair the damages, and then are compared with the conventional rapid thermal annealing (RTA). In terms of As+ and P+ implanted Si, the electrical and structural characterization confirms that the microwave and laser annealing can achieve more efficient dopant activation and recrystallization than conventional RTA. The efficient dopant activation in microwave annealing is attributed to ion hopping under microwave field, while the liquid phase growth in laser annealing provides its efficient dopant activation. The characterization of dopants diffusion shows no visible diffusion after microwave annealing, some extent of end range of diffusion after RTA, and significant dopant diffusion after laser annealing. For photovoltaic applications, an indium-free novel three-layer thin-film structure (transparent composited electrode (TCE)) is demonstrated as a promising transparent conductive electrode for solar cells. The characterization of TCE mainly focuses on its optical and electrical properties. Transfer matrix method for optical transmittance calculation is validated and proved to be a desirable method for predicting transmittance of TCE containing continuous metal layer, and can estimate the trend of transmittance as the layer thickness changes. TiO2/Ag/TiO2 (TAgT) electrode for organic solar cells (OSCs) is then designed using numerical simulation and shows much higher Haacke figure of merit than indium tin oxide (ITO). In addition, TAgT based OSC shows better performance than ITO based OSC when compatible hole transfer layer

  19. Synthesis, structure, and physicochemical properties of dinuclear NiII complexes as highly efficient functional models of phosphohydrolases. (United States)

    Greatti, Alessandra; Scarpellini, Marciela; Peralta, Rosely A; Casellato, Annelise; Bortoluzzi, Adailton J; Xavier, Fernanado R; Jovito, Rafael; de Brito, Marcos Aires; Szpoganicz, Bruno; Tomkowicz, Zbigniew; Rams, Michal; Haase, Wolfgang; Neves, Ademir


    As metal ions are present in the catalytic sites of several enzymes, attention has been focused on the synthesis and characterization of metal complexes able to act as biomimetic functional and structural models for these systems. In this study, a novel dinuclear NiII complex was synthesized, [Ni2(L2)(OAc)2(CH3CN)]BPh4 (2) (HL2=2-[N-(2-(pyridyl-2-yl)ethyl)(1-methylimidazol-2-yl)amin omethyl]-4-methyl-6-[N-(2-(imidazol-4-yl)ethyl)amino methyl]phenol), employing a new unsymmetrical dinucleating ligand containing N,O-donor groups as a model for hydrolases. Complex 2 was characterized by a variety of techniques including: elemental analysis, infrared and UV-vis spectroscopies, molar conductivity, electrochemistry, potentiometric titration, magnetochemistry, and single-crystal X-ray diffractometry. The structural and magnetochemical data of 2 allow us to consider this complex as a structural model for the active site of the ureases, as previously reported for [Ni2(L1)(OAc)2(H2O)]ClO4.H2O (1) (HL1=2-[N-bis-(2-pyridylmethyl)aminomethyl]-4-methyl-6-[N-(2-pyridylmethyl)aminomethyl] phenol). The characterization of complexes 1 and 2 (mainly by X-ray diffraction and potentiometric titration) led us to study their reactivities toward the hydrolysis of the substrate bis(2,4-dinitrophenyl)phosphate (2,4-BDNPP). These studies revealed that complexes 1 and 2 show the best catalytic activity reported so far, with acceleration rates 8.8x10(4) and 9.95x10(5) times faster, respectively, than the uncatalyzed hydrolysis of 2,4-BDNPP. Catalytic activity of 2 on 2,4-DNPP showed that the monoester is hydrolyzed 27 times slower than the 2,4-BDNPP diester under identical experimental conditions. Therefore, 1 and 2 can undoubtedly be considered highly efficient functional models of the phosphohydrolases.

  20. Structural characterization of neutral and acidic glycolipids from Thermus thermophilus HB8.

    Directory of Open Access Journals (Sweden)

    Yasuo Suda

    Full Text Available The structural characterization of glycolipids from Thermus thermophilus HB8 was performed in this study. Two neutral and one acidic glycolipids were extracted and purified by the modified TLC-blotting method, after which their chemical structures were determined by chemical composition analysis, mass spectrometry (MS and nuclear magnetic resonance (NMR spectroscopy. The structure of one of the neutral glycolipids, NGL-A, was Galp(α1-6GlcpNacyl(β1-2Glcp(α1-acyl(2Gro, and the other, NGL-C, was Galf(β1-2Galp(α1-6GlcpNacyl(β1-2Glcp(α1-acyl(2Gro. The structure of NGL-C was identical to that reported previously [Oshima, M. and Ariga, T. (1976 FEBS Lett. 64, 440]. Both neutral glycolipids shared a common structural unit found in the Thermus species. The acyl groups found in NGL-A and NGL-C, iso-type pentadecanoxy and heptadecanoxy fatty acid, were also the same as those found in this species. In contrast, the acidic glycolipid, AGL-B, possessed the structure of N-(((GlcpNAc(α1-acyl(2GroP-2GroAalkylamine. The alkyl group in AGL-B was an iso-type heptadecanyl, suggesting that the iso-type structure of the long alkyl chain is responsible for the thermal stability of the bacteria.

  1. Characterization of piezoelectric paint and its refinement for structural health monitoring applications (United States)

    Yang, Cheng; Fritzen, Claus-Peter


    Piezoelectric paint is a composite piezoelectric material, due to its outstanding properties consisting of flexibility and conformability, it has been a great interest in structural health monitoring applications recently. The normal piezoelectric ceramics offer high piezoelectric properties, but are difficult to adhere on curly structural surfaces. For normal polymers, it offers high flexibility but missing the ability to transform the mechanical energy into the electrical energy, and vice versa. The piezoelectric paint combines the features of both, so it could be distributed on both even and uneven structural surface, as a sensor or actuator. This work starts with the development of the piezoelectric paint, followed by a systematic characterization of its mechanical and piezoelectric properties, which includes microstructure, Young's modulus, sensitivity and piezoelectric charge constant da1. The characterization results helps to understand the performance of the piezoelectric paint more deeply. Finally, a refinement method is demonstrated to improve the piezoelectricity of the paint. The results showed that the piezoelectricity was greatly improved and therefore its applications in structural health monitoring is widely expanded.

  2. Tree Root System Characterization and Volume Estimation by Terrestrial Laser Scanning and Quantitative Structure Modeling

    Directory of Open Access Journals (Sweden)

    Aaron Smith


    Full Text Available The accurate characterization of three-dimensional (3D root architecture, volume, and biomass is important for a wide variety of applications in forest ecology and to better understand tree and soil stability. Technological advancements have led to increasingly more digitized and automated procedures, which have been used to more accurately and quickly describe the 3D structure of root systems. Terrestrial laser scanners (TLS have successfully been used to describe aboveground structures of individual trees and stand structure, but have only recently been applied to the 3D characterization of whole root systems. In this study, 13 recently harvested Norway spruce root systems were mechanically pulled from the soil, cleaned, and their volumes were measured by displacement. The root systems were suspended, scanned with TLS from three different angles, and the root surfaces from the co-registered point clouds were modeled with the 3D Quantitative Structure Model to determine root architecture and volume. The modeling procedure facilitated the rapid derivation of root volume, diameters, break point diameters, linear root length, cumulative percentages, and root fraction counts. The modeled root systems underestimated root system volume by 4.4%. The modeling procedure is widely applicable and easily adapted to derive other important topological and volumetric root variables.

  3. Structural and biochemical characterization of engineered tissue using FTIR spectroscopic imaging: melanoma progression as an example (United States)

    Bhargava, Rohit; Kong, Rong


    Engineered tissue represents a convenient path to providing models for imaging and disease progression. The use of these models or phantoms is becoming increasingly prevalent. While structural characterization of these systems is well-documented, a combination of biochemical and structural knowledge is often helpful. Fourier transform infrared (FTIR) spectroscopic imaging is a rapidly emerging technique that combines the molecular selectivity of spectroscopy with the spatial specificity of optical microscopy. Here, we report on the application of FTIR spectroscopic for analysis of a melanoma model in engineered skin. We first characterize the biochemical properties, consistency and spectral changes in different layers of growing skin. Results provide simple indices for monitoring tissue consistency and reproducibility as a function of time. Second, we introduce malignant melanocytes to simulate tumor formation and growth. Both cellular changes associated with tumor formation and growth can be observed. FTIR images indicate holistic chemical changes during the tumor growth, allowing for the development of automated pathology protocols. FTIR imaging being non-destructive, further, samples remain entirely compatible with downstream tissue processing or staining. We specifically examined the correlation of structural changes, molecular content and reproducibility of the model systems. The development of analysis, integrating spectroscopy, imaging and computation will allow for quality control and standardization of both the structural and biochemical properties of tissue phantoms.

  4. Biophysical characterization of recombinant proteins: A key to higher structural genomics success (United States)

    Vedadi, Masoud; Arrowsmith, Cheryl H.; Allali-Hassani, Abdellah; Senisterra, Guillermo; Wasney, Gregory A.


    Hundreds of genomes have been successfully sequenced to date, and the data are publicly available. At the same time, the advances in large-scale expression and purification of recombinant proteins have paved the way for structural genomics efforts. Frequently, however, little is known about newly expressed proteins calling for large-scale protein characterization to better understand their biochemical roles and to enable structure–function relationship studies. In the Structural Genomics Consortium (SGC), we have established a platform to characterize large numbers of purified proteins. This includes screening for ligands, enzyme assays, peptide arrays and peptide displacement in a 384-well format. In this review, we describe this platform in more detail and report on how our approach significantly increases the success rate for structure determination. Coupled with high-resolution X-ray crystallography and structure-guided methods, this platform can also be used toward the development of chemical probes through screening families of proteins against a variety of chemical series and focused chemical libraries. PMID:20466062

  5. Novel aldehyde and thiosemicarbazone derivatives: Synthesis, spectroscopic characterization, structural studies and molecular docking studies (United States)

    Karakurt, Tuncay; Tahtaci, Hakan; Subasi, Nuriye Tuna; Er, Mustafa; Ağar, Erbil


    In this study our purpose is that, synthesis and characterization of compounds containing the aldehyde and thiosemicarbazone groups and comparison of the theoretical results with the experimental results. The structures of all synthesized compounds were elucidated by IR, 1H NMR, 13C NMR, elemental analyses techniques. The structure of compound (4) (C9H8N4O2S) was also elucidated by X-ray diffraction analysis. In addition, the theoretical IR spectrum, 1H NMR and 13C NMR chemical shift values, frontier molecular orbital values (FMO) of these molecules were analyzed by using Becke-3- Lee-Yang-Parr (B3LYP) method with LanL2DZ basis set. Finally, molecular docking studies were performed on synthesized compounds using the 4DKI beta-lactam protein structure to determine the potential binding mode of inhibitors.

  6. Structure and mechanical characterization of DNA i-motif nanowires by molecular dynamics simulation

    CERN Document Server

    Singh, Raghvendra Pratap; Cleri, Fabrizio


    We studied the structure and mechanical properties of DNA i-motif nanowires by means of molecular dynamics computer simulations. We built up to 230 nm long nanowires, based on a repeated TC5 sequence from crystallographic data, fully relaxed and equilibrated in water. The unusual stacked C*C+ stacked structure, formed by four ssDNA strands arranged in an intercalated tetramer, is here fully characterized both statically and dynamically. By applying stretching, compression and bending deformation with the steered molecular dynamics and umbrella sampling methods, we extract the apparent Young's and bending moduli of the nanowire, as wel as estimates for the tensile strength and persistence length. According to our results, the i-motif nanowire shares similarities with structural proteins, as far as its tensile stiffness, but is closer to nucleic acids and flexible proteins, as far as its bending rigidity is concerned. Furthermore, thanks to its very thin cross section, the apparent tensile toughness is close to...

  7. Characterization and crystal structure of lysine insensitive Corynebacterium glutamicum dihydrodipicolinate synthase (cDHDPS) protein

    Energy Technology Data Exchange (ETDEWEB)

    Rice, E.A.; Bannon, G.A.; Glenn, K.C.; Jeong, S.S.; Sturman, E.J.; Rydel, T.J. (Monsanto)


    The lysine insensitive Corynebacterium glutamicum dihydrodipicolinate synthase enzyme (cDHDPS) was recently successfully introduced into maize plants to enhance the level of lysine in the grain. To better understand lysine insensitivity of the cDHDPS, we expressed, purified, kinetically characterized the protein, and solved its X-ray crystal structure. The cDHDPS enzyme has a fold and overall structure that is highly similar to other DHDPS proteins. A noteworthy feature of the active site is the evidence that the catalytic lysine residue forms a Schiff base adduct with pyruvate. Analyses of the cDHDPS structure in the vicinity of the putative binding site for S-lysine revealed that the allosteric binding site in the Escherichia coli DHDPS protein does not exist in cDHDPS due to three non-conservative amino acids substitutions, and this is likely why cDHDPS is not feedback inhibited by lysine.

  8. Metal-organic frameworks: structure, properties, methods of synthesis and characterization (United States)

    Butova, V. V.; Soldatov, M. A.; Guda, A. A.; Lomachenko, K. A.; Lamberti, C.


    This review deals with key methods of synthesis and characterization of metal-organic frameworks (MOFs). The modular structure affords a wide variety of MOFs with different active metal sites and organic linkers. These compounds represent a new stage of development of porous materials in which the pore size and the active site structure can be modified within wide limits. The set of experimental methods considered in this review is sufficient for studying the short-range and long-range order of the MOF crystal structure, determining the morphology of samples and elucidating the processes that occur at the active metal site in the course of chemical reactions. The interest in metal-organic frameworks results, first of all, from their numerous possible applications, ranging from gas separation and storage to chemical reactions within the pores. The bibliography includes 362 references.

  9. Fine structural characterization of chondroitin sulfate in urine of bladder pain syndrome subjects. (United States)

    Maccari, Francesca; Buzzega, Dania; Galeotti, Fabio; Volpi, Nicola


    Urothelial glycosaminoglycans (GAGs) are decreased in bladder pain syndrome (BPS), and urinary GAGs are thought to reflect this deficiency. In previous researches, urine GAG levels were found increased, decreased, or similar between BPS and controls. Additionally, no study is available on the structure characterization of urinary chondroitin sulfate (CS) in BPS patients. CS in the urine of BPS-affected patients and controls has been determined by specific electrophoresis, along with total GAGs and heparan sulfate (HS) percentage, and CS disaccharides have been quantified by high-performance liquid chromatography. No significant differences were obtained for total amount of GAGs, absolute content of CS and HS, and their relative percentages. Moreover, no differences were observed for CS structure confirming similar urine CS composition in BPS subjects and controls. This study found no significant differences of BPS and control urine GAG levels and CS structure to allow use of these parameters as diagnostic markers for BPS diagnosis.

  10. Stand structure and dead wood characterization in cork forest of Calabria region (southern Italy

    Directory of Open Access Journals (Sweden)

    Barreca L


    Full Text Available The cork forests are one the most interesting forest ecosystems in the Mediterranean area. Their distribution and ecological characteristics have undergone a significant transformation after the significant changes following the development and establishment of agricultural crops. Currently, only a few stands, which survive in hard to reach places, prove the wide spread distribution of this species was also in the recent past. This study describes the stand structure of some cork forests in Calabria region (southern Italy. In order, to characterize the vertical structure Latham index has been applied, while for the description of the horizontal distribution NBSI group indices has been used. Detailed surveys on dead wood were also conducted determining the occurring volume and its decay stage according to the decay classes system proposed by Hunter. The aim of this study is to provide guidelines for sustainable management of cork forests, improving and promoting the structural complexity and functional efficiency of these forest stands.

  11. Synthesis, structural characterization and myorelaxant activity of 4-naphthylhexahydroquinoline derivatives containing different ester groups

    Directory of Open Access Journals (Sweden)

    Gündüz Miyase Gözde


    Full Text Available The present study reports the synthesis, structural characterization and myorelaxant activity evaluation of a series of 16 novel 4-naphthyl-hexahydroquinoline derivatives. The compounds were achieved by one-pot microwave-assisted method via a modified Hantzsch reaction. The structures of the compounds were confirmed by various spectral methods like IR, 1D-2D NMR techniques and mass analysis. X-ray studies of compound 10 provided further evidence for the proposed structure. To evaluate their myorelaxant activities, the Emax and pD2 values of the compounds and nifedipine were determined on isolated rabbit gastric fundus smooth muscle strips. The obtained results indicated that introduction of long chain alkyl groups such as 2-methoxyethyl or 2-(methacryloyloxyethyl moiety to the ester group led to the most active compounds.

  12. Structural characterization of the N-linked oligosaccharides from tomato fruit. (United States)

    Zeleny, R; Altmann, F; Praznik, W


    The primary structures of the N-linked oligosaccharides from tomato fruit (Lycopersicon esculentum) have been elucidated. For the isolation of the protein fraction, two procedures were employed alternatively: a low temperature acetone powder method and ammonium sulfate precipitation of the tomato extract. After peptic digestion, the glycopeptides were purified by cation-exchange chromatography; the oligosaccharides were released by N-glycosidase A and fluorescently labelled with 2-aminopyridine. Structural characterization was accomplished by means of two-dimensional HPLC in combination with exoglycosidase digestions and MALDI-TOF mass spectrometry. Two varieties as well as two stages of ripening were investigated. In all the samples, the same sixteen N-glycosidic structures were detected; the two most abundant glycans showed identical properties to those of the major N-linked oligosaccharides of horseradish peroxidase and pineapple stem bromelain, respectively and accounted for about 65-78% of the total glycan amount; oligomannosidic glycans occurred only in small quantities (3-9%). The majority of the N-glycans were beta 1,2-xylosylated and carried an alpha 1,3-fucose residue linked to the terminal N-acetylglucosamine. This structural element contributes to cross-reactions among non-related glycoproteins and has been shown to be an IgE-reactive determinant (Tretter, Altmann, Kubelka, März, & Becker, 1993). The presented study gives a possible structural explanation for reported immunological cross-reactivities between tomato and grass pollen extracts due to carbohydrate IgE epitopes (Petersen, Vieths, Aulepp, Schlaak, & Becker, 1996), thereby demonstrating the importance of the structural characterization of plant N-glycans for a more reliable interpretation of immunological data.

  13. Impedance measures in analysis and characterization of multistable structures subjected to harmonic excitation (United States)

    Harne, Ryan L.; Goodpaster, Benjamin A.


    Structural components susceptible to adverse, post-buckled dynamic behaviors have long challenged the success of applications requiring lightweight, slender curved structures, while researchers have begun to leverage such bistable systems in emerging applications for novel energy attenuation and shape-changing properties. To expedite development and deployment of these built-up platforms containing post-buckled constituents, efficient approaches are required to complement time-consuming full-field models in the prediction of the near- and far-from-equilibrium dynamics. This research meets the need by introducing a semi-analytical model framework to enable the characterization of steady-state responses in multi degree-of-freedom (DOF) and multistable structural systems subjected to harmonic excitation. In so doing, the pathway for assessing impedance measures is created here so as to identify how energy travels and returns within built-up multistable structures. Verified by simulations and qualitatively validated by experiments, the analysis is shown to accurately reproduce both near- and far-from-equilibrium responses including different classes of energetic snap-through dynamics that only exist in such multistable structures. A first look at the impedance measures of different dynamic regimes reveals a connection between damping in multistable structures and the sustainability of far-from-equilibrium oscillations.

  14. Design, Fabrication and Characterization of Thin Film Structures through Oxidation Kinetics (United States)

    Diaz Leon, Juan Jose

    Materials science and engineering is devoted to the understanding of the physics and chemistry of materials at the mesoscale and to applying that knowledge into real-life applications. In this work, different oxide materials and different oxidation methods are studied from a materials science point of view and for specific applications. First, the deposition of complex metal oxides is explored for solar energy concentration. This requires a number of multi-cation oxide structures such as thin-film dielectric barriers, low loss waveguides or the use of continuously graded composition oxides for antireflection coatings and light concentration. Then, oxidation via Joule heating is used for the self-alignment of a selector on top of a memristor structure on a nanovia. Simulations are used to explore the necessary voltage for the insulator-to-metal transition temperature of NbO2 using finite element analysis, followed by the fabrication and the characterization of such a device. Finally, long-term copper oxidation at room temperature and pressure is studied using optical techniques. Alternative characterization techniques are used to confirm the growth rate and phase change, and an application of copper oxide as a volatile conductive bridge is shown. All these examples show how the combination of novel simulation, fabrication and characterization techniques can be used to understand physical mechanisms and enable disruptive technologies in fields such as solar cells, light emitting diodes, photodetectors or memory devices.

  15. Comparison of nitrogen adsorption and transmission electron microscopy analyses for structural characterization of carbon nanotubes (United States)

    Abbaslou, Reza Malek; Vosoughi, Vahid; Dalai, Ajay K.


    Carbon nanotubes (CNTs) are different from other porous substrates such as activated carbon due to their high external surfaces. This structural feature can lead in some uncertainties in the results of nitrogen adsorption analysis for characterization of CNTs. In this paper, the results of microscopic analyses and nitrogen adsorption method for characterization of carbon nanotubes were compared. Five different types of CNTs with different structures were either synthesized or purchased. The CNT samples were characterized by high resolution transmission electron microscopy (HRTEM), scanning electron microscopy (SEM) and N2 adsorption analysis. The comparisons between the results from the microscopic analyses and N2 adsorption showed that the total pore volume and BET surface measurements include the internal and external porosity of CNTs. Therefore, the interpretation of N2 adsorption data required accurate TEM analysis. In addition, the evaluation of pore size distribution curves from all CNT samples in this study and several instances in the literature revealed the presence of a common peak in the range of 2-5 nm. This peak does not explain the inner pore size distribution. The presence of this common peak can be attributed to the strong adsorption of N2 on the junction of touched and crossed nanotubes.

  16. Optical Fourier transform based in-plane vibration characterization for MEMS comb structure. (United States)

    Gao, Yongfeng; Cao, Liangcai; You, Zheng; Zhao, Jiahao; Zhang, Zichen; Yang, Jianzhong


    On-line and on-wafer characterizations of mechanical properties of Micro-Electro-Mechanical-System (MEMS) with efficiency are very important to the mass production of MEMS foundry in the near future. However, challenges still remain. In this paper, we present an in-plane vibration characterizing method for MEMS comb using optical Fourier transform (OFT). In the experiment, the intensity distribution at the focal plane was captured to characterize the displacement of the vibrator in the MEMS comb structure. A typical MEMS comb was tested to verify the principle. The shape and the movement of MEMS comb was imitated and tested to calibrate the measurement by using a spatial light modulator (SLM). The relative standard deviations (RSD) of the measured displacements were better than 5%, where the RSD is defined as the ratio of the standard deviation to the mean. It is convinced that the presented method is feasible for on-line and on-wafer characterizations for MEMS with great convenience, high efficiency and low cost.

  17. An FFT-accelerated fdtd scheme with exact absorbing conditions for characterizing axially symmetric resonant structures

    KAUST Repository

    Sirenko, Kostyantyn


    An accurate and efficient finite-difference time-domain (FDTD) method for characterizing transient waves interactions on axially symmetric structures is presented. The method achieves its accuracy and efficiency by employing localized and/or fast Fourier transform (FFT) accelerated exact absorbing conditions (EACs). The paper details the derivation of the EACs, discusses their implementation and discretization in an FDTD method, and proposes utilization of a blocked-FFT based algorithm for accelerating the computation of temporal convolutions present in nonlocal EACs. The proposed method allows transient analyses to be carried for long time intervals without any loss of accuracy and provides reliable numerical data pertinent to physical processes under resonant conditions. This renders the method highly useful in characterization of high-Q microwave radiators and energy compressors. Numerical results that demonstrate the accuracy and efficiency of the method are presented.

  18. Complex of hexamethylenetetramine with magnesium-tetraphenylporphyrin: Synthesis, structure, spectroscopic characterizations and electrochemical properties (United States)

    Ezzayani, Khaireddine; Ben Khelifa, Arbia; Saint-Aman, Eric; Loiseau, Frederique; Nasri, Habib


    A new crystalline material of a magnesium (II)-porphyrin complex was prepared and characterized by single crystal X-ray diffraction. The molecular structure is made by (5,10,15,20-tetraphenylporphyrinato-κ4N)bis(hexamethylenetetramine) magnesium dichloromethane disolvate. The title compound crystallizes in the orthorhombic system, space group Pbcn, with a = 19.2932 (6) Å, b = 10.4878 (4) Å, c = 26.0025 (14) Å, V = 5261.4 (4) Å3 and Z = 4. The supramolecular architecture includes weak C__H⋯N hydrogen bond. This magnesium-porphyrin species was also characterized by UV-visible, IR and fluorescence spectroscopy and a cyclic voltammetry investigation was also carried out on this species.

  19. Image-based characterization of cement pore structure using Wood`s metal intrusion

    Energy Technology Data Exchange (ETDEWEB)

    Willis, K.L.; Abell, A.B.; Lange, D.A. [Univ. of Illinois, Urbana, IL (United States). Dept. of Civil Engineering


    Mercury intrusion porosimetry is a widely used technique for characterization of the pore size distribution of cement-based materials. However, the technique has several limitations, among which are the ink bottle effect and a cylindrical pore geometry assumption that lead to inaccurate pore size distribution curves. By substituting Wood`s metal for mercury as the intruding liquid, scanning electron microscopy and imaging techniques can be applied to the sample after intrusion. The molten Wood`s metal solidifies within the pore structure of the sample, which allows it to be sectioned and observed in the scanning electron microscopy. From here, the sample can be analyzed both qualitatively, by observing the changes in the appearance of the sample as the intrusion process progresses, and quantitatively, by applying image analysis techniques. This study provides insight for better interpretation of mercury intrusion porosimetry results and the possibility for quantitative characterization of the spatial geometry of pores in cement-based materials.

  20. Mechanical characterization of auxetic stainless steel thin sheets with reentrant structure (United States)

    Lekesiz, H.; Bhullar, S. K.; Karaca, A. A.; Jun, M. B. G.


    Smart materials in auxetic form present a great potential for various medical applications due to their unique deformation mechanisms along with durable infrastructure. Both analytical and finite element (FE) models are extensively used in literature to characterize mechanical response of auxetic structures but these structures are mostly thick enough to be considered as bulk material and 3D inherently. Auxetic plates in very thin form, a.e. foil, may bring numerous advantages such as very light design and better biodegradability when needed. However, there is a gap in literature on mechanical characterization of auxetic thin plates. In this study, structural analysis of very thin auxetic plates under uniaxial loading is investigated using both FE method and experimental method. 25 μm thick stainless steel (316L) plates are fabricated with reentrant texture for three different unit cell dimensions and tested under uniaxial loading using universal testing machine. 25 and 50 μm thick sheets with same cell dimensions were analyzed using implicit transient FE model including strain hardening and failure behaviors. FE results cover all the deformation schemes seen in actual tests and total deformation level matches with test results. Effect of plate thickness and cell geometry on auxetic behavior is discussed in detail using FE results. Finally, based on FE analysis results, an optimum geometry for prolonged auxetic behavior, high flexibility and high durability is suggested for future potential applications.

  1. Nonlinear characterization of a bolted, industrial structure using a modal framework (United States)

    Roettgen, Daniel R.; Allen, Matthew S.


    This article presents measurements from a sub assembly of an off-the-shelf automotive exhaust system containing a bolted-flange connection and uses a recently proposed modal framework to develop a nonlinear dynamic model for the structure. The nonlinear identification and characterization methods used are reviewed to highlight the strengths of the current approach and the areas where further development is needed. This marks the first use of these new testing and nonlinear identification tools, and the associated modal framework, on production hardware with a realistic joint and realistic torque levels. To screen the measurements for nonlinearities, we make use of a time frequency analysis routine designed for transient responses called the zeroed early-time fast Fourier transform (ZEFFT). This tool typically reveals the small frequency shifts and distortions that tend to occur near each mode that is affected by the nonlinearity. The damping in this structure is found to be significantly nonlinear and a Hilbert transform is used to characterize the damping versus amplitude behavior. A model is presented that captures these effects for each mode individually (e.g. assuming negligible nonlinear coupling between modes), treating each mode as a single degree-of-freedom oscillator with a spring and viscous damping element in parallel with a four parameter Iwan model. The parameters of this model are identified for each of the structure's modes that exhibited nonlinearity and the resulting nonlinear model is shown to capture the stiffness and damping accurately over a large range of response amplitudes.

  2. Novel polymeric potassium complex: Its synthesis, structural characterization, photoluminescence and electrochemical properties

    Energy Technology Data Exchange (ETDEWEB)

    Ceyhan, Goekhan [Chemistry Department, K.Maras Suetcue Imam University, 46100 K.Maras (Turkey); Tuemer, Mehmet, E-mail: [Chemistry Department, K.Maras Suetcue Imam University, 46100 K.Maras (Turkey); Koese, Muhammet; McKee, Vickie [Chemistry Department, Loughborough University, LE11 3TU Leicestershire (United Kingdom)


    In this paper, we obtained a novel poly(vanillinato potassium) complex (PVP) as a single crystal and characterized by analytical and spectroscopic methods. A single crystal of the PVP was obtained from the acetone solution. X-ray structural data show that crystals contain polymeric K{sup +} complex of vanillin. Each potassium ion in the polymeric structure is identical and seven-coordinate, bonded to two methoxy, two phenoxy and three aldehyde oxygen atoms from four vaniline molecules. Two aldehyde oxygen atoms are bridging between potassium ions. It crystallizes in the monoclinic system, space group P2{sub 1}/c, with lattice parameters a=9.6215(10) A, b=17.4139(19) A, c=9.6119(10) A, {beta}=100.457(2) Degree-Sign and Z=4. Thermal properties of the PVP were investigated by TGA, DTA and DSC methods. The electrochemical properties of the complex were studied in different solvents and at various scan rates. The luminescence properties of the complex in different solvents and at different pH values have been investigated. The results show that the complex exhibits more efficient luminescence property in CH{sub 3}CN and n-butanol. - Highlights: Black-Right-Pointing-Pointer Novel polymeric potassium complex was prepared and fully characterized. Black-Right-Pointing-Pointer X-ray crystal structure of complex was reported. Black-Right-Pointing-Pointer Electrochemical properties of compound were investigated. Black-Right-Pointing-Pointer Thermal and DSC measurements of complex were examined.

  3. Structural defects in cubic semiconductors characterized by aberration-corrected scanning transmission electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Arroyo Rojas Dasilva, Yadira; Kozak, Roksolana; Erni, Rolf; Rossell, Marta D., E-mail:


    The development of new electro-optical devices and the realization of novel types of transistors require a profound understanding of the structural characteristics of new semiconductor heterostructures. This article provides a concise review about structural defects which occur in semiconductor heterostructures on the basis of micro-patterned Si substrates. In particular, one- and two-dimensional crystal defects are being discussed which are due to the plastic relaxation of epitaxial strain caused by the misfit of crystal lattices. Besides a few selected examples from literature, we treat in particular crystal defects occurring in GaAs/Si, Ge/Si and β-SiC/Si structures which are studied by high-resolution annular dark-field scanning transmission electron microscopy. The relevance of this article is twofold; firstly, it should provide a collection of data which are of help for the identification and characterization of defects in cubic semiconductors by means of atomic-resolution imaging, and secondly, the experimental data shall provide a basis for advancing the understanding of device characteristics with the aid of theoretical modelling by considering the defective nature of strained semiconductor heterostructures. - Highlights: • The heterogeneous integration of high-quality compound semiconductors remains a challenge. • Lattice defects cause severe degradation of the semiconductor device performances. • Aberration-corrected HAADF-STEM allows atomic-scale characterization of defects. • An overview of lattice defects found in cubic semiconductors is presented. • Theoretical modelling and calculations are needed to determine the defect properties.

  4. Form and function in hillslope hydrology: in situ imaging and characterization of flow-relevant structures

    Directory of Open Access Journals (Sweden)

    C. Jackisch


    Full Text Available The study deals with the identification and characterization of rapid subsurface flow structures through pedo- and geo-physical measurements and irrigation experiments at the point, plot and hillslope scale. Our investigation of flow-relevant structures and hydrological responses refers to the general interplay of form and function, respectively. To obtain a holistic picture of the subsurface, a large set of different laboratory, exploratory and experimental methods was used at the different scales. For exploration these methods included drilled soil core profiles, in situ measurements of infiltration capacity and saturated hydraulic conductivity, and laboratory analyses of soil water retention and saturated hydraulic conductivity. The irrigation experiments at the plot scale were monitored through a combination of dye tracer, salt tracer, soil moisture dynamics, and 3-D time-lapse ground penetrating radar (GPR methods. At the hillslope scale the subsurface was explored by a 3-D GPR survey. A natural storm event and an irrigation experiment were monitored by a dense network of soil moisture observations and a cascade of 2-D time-lapse GPR trenches. We show that the shift between activated and non-activated state of the flow paths is needed to distinguish structures from overall heterogeneity. Pedo-physical analyses of point-scale samples are the basis for sub-scale structure inference. At the plot and hillslope scale 3-D and 2-D time-lapse GPR applications are successfully employed as non-invasive means to image subsurface response patterns and to identify flow-relevant paths. Tracer recovery and soil water responses from irrigation experiments deliver a consistent estimate of response velocities. The combined observation of form and function under active conditions provides the means to localize and characterize the structures (this study and the hydrological processes (companion study Angermann et al., 2017, this issue.

  5. Form and function in hillslope hydrology: in situ imaging and characterization of flow-relevant structures (United States)

    Jackisch, Conrad; Angermann, Lisa; Allroggen, Niklas; Sprenger, Matthias; Blume, Theresa; Tronicke, Jens; Zehe, Erwin


    The study deals with the identification and characterization of rapid subsurface flow structures through pedo- and geo-physical measurements and irrigation experiments at the point, plot and hillslope scale. Our investigation of flow-relevant structures and hydrological responses refers to the general interplay of form and function, respectively. To obtain a holistic picture of the subsurface, a large set of different laboratory, exploratory and experimental methods was used at the different scales. For exploration these methods included drilled soil core profiles, in situ measurements of infiltration capacity and saturated hydraulic conductivity, and laboratory analyses of soil water retention and saturated hydraulic conductivity. The irrigation experiments at the plot scale were monitored through a combination of dye tracer, salt tracer, soil moisture dynamics, and 3-D time-lapse ground penetrating radar (GPR) methods. At the hillslope scale the subsurface was explored by a 3-D GPR survey. A natural storm event and an irrigation experiment were monitored by a dense network of soil moisture observations and a cascade of 2-D time-lapse GPR trenches. We show that the shift between activated and non-activated state of the flow paths is needed to distinguish structures from overall heterogeneity. Pedo-physical analyses of point-scale samples are the basis for sub-scale structure inference. At the plot and hillslope scale 3-D and 2-D time-lapse GPR applications are successfully employed as non-invasive means to image subsurface response patterns and to identify flow-relevant paths. Tracer recovery and soil water responses from irrigation experiments deliver a consistent estimate of response velocities. The combined observation of form and function under active conditions provides the means to localize and characterize the structures (this study) and the hydrological processes (companion study Angermann et al., 2017, this issue).

  6. Using LiDAR Metrics to Characterize Forest Structural Complexity at Multiple Scales (United States)

    Kane, V. R.; McGaughey, R. J.; Gersonde, R.; Franklin, J. F.


    Forest structure - the size and arrangement of trees and foliage - reflects a stand's history of initiation, growth, disturbance, and mortality. Because of this, studying the structure of forests can provide key insights into ecological processes, guides to silvicultural prescriptions to improve habitat, and assessments of forested landscapes. This study tested LiDAR metrics to characterize stands based on canopy structure. The study site was the 34,591 ha of forests in the Cedar River Watershed in western Washington State, USA. Stands ranged in age from 350 years old (including old-growth). Study sites spanned the western hemlock- Douglas fir (Tsuga heterophylla-Pseudotsuga menziesii), Pacific silver fir (Abies amabilis), and mountain hemlock (Tsuga mertansiana) forest zones. Eighty sample plots were used to ground truth the LiDAR data. A variety of structural indices were used to study canopy structural variations at the plot, stand, and landscape scales. The two most successful indices used the exposed geometry of the canopy surface: (1) the ratio of the canopy surface area to ground surface area (rumple index), and (2) the ratio of the volume beneath the canopy surface to maximum volume beneath the 95th percentile height (modified canopy volume method). These two indices integrated the spatial effects of tree heights, foliage distribution, and tree arrangement within 15m pixels. Variation between pixels revealed structural complexity at larger scales. Results: At the plot scale (~4 pixels), correlations with standard plot metrics (e.g., diameter at breast height) were similar to those reported by other studies. Comparison of structural complexity with age and height revealed a diversity of development pathways. The relationship between height and complexity allowed stands to be classified by the degree to which they have achieved their potential structural complexity, a new way to examine forest development. At the stand scale, the indices allowed spatial

  7. Structural, magnetic and hyperfine characterizations of nanocrystalline Zn-Cd doped nickel ferrites (United States)

    Aakash; Nordblad, Per; Rajendra Mohan; Mukherjee, Samrat


    In our present work, we have synthesized a series of Cd-Zn doped nickel ferrite ((Cd0.5-xZnx)Ni0.5Fe2O4; x = 0, 0.1, 0.2, 0.3, 0.4 and 0.5) through standard chemical co-precipitation method to study the influence of diamagnetic ions (Cd, Zn) on the magnetic properties of ferrites. XRD and Raman spectroscopy were employed for the structural characterizations. The refinement of the X-ray diffractogram data augmented by the Williamson-Hall plots showed the presence of Cd2+ vacancies and a strained crystal structure. The vibrational spectroscopy indicated the presence of lower space-group symmetry and a distorted crystal structure. Magnetic measurements showed the samples possessed low magnetic anisotropy along with a canted spin structure. The Mössbauer measurements confirmed the cation distribution and gave evidence of super transferred hyperfine interactions arising due to canted spin structure of the system.

  8. Crystal Structure and Characterization of Particulate Methane Monooxygenase from Methylocystis species Strain M

    Energy Technology Data Exchange (ETDEWEB)

    Smith, Stephen M.; Rawat, Swati; Telser, Joshua; Hoffman, Brian M.; Stemmler, Timothy L.; Rosenzweig, Amy C. (WSU-MED); (NWU)


    Particulate methane monooxygenase (pMMO) is an integral membrane metalloenzyme that oxidizes methane to methanol in methanotrophic bacteria. Previous biochemical and structural studies of pMMO have focused on preparations from Methylococcus capsulatus (Bath) and Methylosinus trichosporium OB3b. A pMMO from a third organism, Methylocystis species strain M, has been isolated and characterized. Both membrane-bound and solubilized Methylocystis sp. strain M pMMO contain {approx}2 copper ions per 100 kDa protomer and exhibit copper-dependent propylene epoxidation activity. Spectroscopic data indicate that Methylocystis sp. strain M pMMO contains a mixture of Cu{sup I} and Cu{sup II}, of which the latter exhibits two distinct type 2 Cu{sup II} electron paramagnetic resonance (EPR) signals. Extended X-ray absorption fine structure (EXAFS) data are best fit with a mixture of Cu-O/N and Cu-Cu ligand environments with a Cu-Cu interaction at 2.52-2.64 {angstrom}. The crystal structure of Methylocystis sp. strain M pMMO was determined to 2.68 {angstrom} resolution and is the best quality pMMO structure obtained to date. It provides a revised model for the pmoA and pmoC subunits and has led to an improved model of M. capsulatus (Bath) pMMO. In these new structures, the intramembrane zinc/copper binding site has a different coordination environment from that in previous models.

  9. Crystal structure and characterization of particulate methane monooxygenase from Methylocystis species strain M. (United States)

    Smith, Stephen M; Rawat, Swati; Telser, Joshua; Hoffman, Brian M; Stemmler, Timothy L; Rosenzweig, Amy C


    Particulate methane monooxygenase (pMMO) is an integral membrane metalloenzyme that oxidizes methane to methanol in methanotrophic bacteria. Previous biochemical and structural studies of pMMO have focused on preparations from Methylococcus capsulatus (Bath) and Methylosinus trichosporium OB3b. A pMMO from a third organism, Methylocystis species strain M, has been isolated and characterized. Both membrane-bound and solubilized Methylocystis sp. strain M pMMO contain ~2 copper ions per 100 kDa protomer and exhibit copper-dependent propylene epoxidation activity. Spectroscopic data indicate that Methylocystis sp. strain M pMMO contains a mixture of Cu(I) and Cu(II), of which the latter exhibits two distinct type 2 Cu(II) electron paramagnetic resonance (EPR) signals. Extended X-ray absorption fine structure (EXAFS) data are best fit with a mixture of Cu-O/N and Cu-Cu ligand environments with a Cu-Cu interaction at 2.52-2.64 Å. The crystal structure of Methylocystis sp. strain M pMMO was determined to 2.68 Å resolution and is the best quality pMMO structure obtained to date. It provides a revised model for the pmoA and pmoC subunits and has led to an improved model of M. capsulatus (Bath) pMMO. In these new structures, the intramembrane zinc/copper binding site has a different coordination environment from that in previous models.

  10. Comprehensive comparison of the chemical and structural characterization of landfill leachate and leonardite humic fractions. (United States)

    Tahiri, Abdelghani; Richel, Aurore; Destain, Jacqueline; Druart, Philippe; Thonart, Philippe; Ongena, Marc


    Humic substances (HS) are complex and heterogeneous mixtures of organic compounds that occur everywhere in the environment. They represent most of the dissolved organic matter in soils, sediments (fossil), water, and landfills. The exact structure of HS macromolecules has not yet been determined because of their complexity and heterogeneity. Various descriptions of HS are used depending on specific environments of origin and research interests. In order to improve the understanding of the structure of HS extracted from landfill leachate (LHS) and commercial HS from leonardite (HHS), this study sought to compare the composition and characterization of the structure of LHS and HHS using elemental composition, chromatographic (high-performance liquid chromatography (HPLC)), and spectroscopic techniques (UV-vis, FTIR, NMR, and MALDI-TOF). The results showed that LHS molecules have a lower molecular weight and less aromatic structure than HHS molecules. The characteristics of functional groups of both LHS and HHS, however, were basically similar, but there was some differences in absorbance intensity. There were also less aliphatic and acidic functional groups and more aromatic and polyphenolic compounds in the humic acid (HA) fraction than in the fulvic acid (FA) and other molecules (OM) fractions of both origins. The differences between LHS and HHS might be due to the time course of humification. Combining the results obtained from these analytical techniques cold improve our understanding of the structure of HS of different origins and thus enhance their potential use.

  11. Preparation and structural characterization of a needle like carbon from the refined coal tar pitch

    Energy Technology Data Exchange (ETDEWEB)

    Xue fei Zhao; Shi quan Lai; Ya ru Zhang; Shu lin Liu; Li juan Gao; Hong u Yu [University of Science and Technology Liaoning, Anshan (China)


    A refined coal tar pitch with softening point of 33{sup o}C was obtained by a mixed solvent extraction method. The pitch was carbonized at 500{sup o}C to get micrometer carbon material with needle like structure. The carbonized produce was further calcined at 1500{sup o}C for 30h. The resultant product was characterized by SEM, OM, EDS and XRD. Experimental results indicated that a mixed solvent extraction method could effectively get rid of primary quinoline insoluble (QI). SEM and OM examinations showed that there were more than 70% fibrous structures and a small amount mosaic structures. The size of the fibrous structure was greater than 150 {mu}m in length and less than 30{mu}m in width. The result of EDS exhibited that the material mainly consisted of carbon. XRD analysis revealed that there was a sharp diffraction peaks at 26.5{sup o}C, which was corresponded to the (002) plane of graphite structure.

  12. Electromagnetic studies in the Parnaiba Basin: Structural characterization by magnetotelluric imaging (United States)

    Solon, F. F.; Fontes, S. L.; La Terra, E. F.


    A magnetotelluric profile (MT) of approximately 1430 km long, EW direction,crossing the Parnaíba Basin was conducted in order to characterize the main structural featuresthat can be enhanced through the electromagnetic imaging. This profile is coincident with aseismic reflection profile acquired by BP Energy do Brasil, and it is included in amultidisciplinary study which is being conducted in the Parnaíba Basin between ObservatórioNacional/MCTI, University of Oxford and BP Energy. The study aims to review the evolutionmodels of the Parnaiba basin and to provide an exploratory context. The MT study comprises220 broadband MT stations and 57 long-period MT stations along the profile. The investigationdepth varies from a couple of hundred meters to approximately 40 km, allowing thecharacterization of deep structures of the crust. Some attributes, such as phase tensor andinduction vectors were also analyzed in order to characterize preferential geoelectric strikedirections (directions of electric currents) and dimensionality of the MT data. Induction vectors,are often used to infer the presence or absence of lateral variations in conductivity. The phasetensor provides information about both the dimensionality and directionality of the structures inthe subsurface. The analysis of these two attributes pointed to the presence of a conductivebody at the lower crust. This body has been interpreted as a mid-crustal reflector in the seismicreflection section. It is characterized by a high amplitude seismic reflector at the lower crust andlocated in the central region of the Parnaíba basin. Modeling and inversion routines are beingapplied to better understand the relation between conductor bodies in the crust and the mid-crustal reflector. The modelling and the analysis of the induction vectors suggests the presenceof anomalous conductivity concentrations in the crust region, while the phase sensor confirmsthe hypothesis of a conductive body with three

  13. Uranyl Sequestration: Synthesis and Structural Characterization of Uranyl Complexes with a Tetradentate Methylterephthalamide Ligand

    Energy Technology Data Exchange (ETDEWEB)

    Ni, Chengbao; Shuh, David; Raymond, Kenneth


    Uranyl complexes of a bis(methylterephthalamide) ligand (LH{sub 4}) have been synthesized and characterized by X-ray crystallography. The structure is an unexpected [Me{sub 4}N]{sub 8}[L(UO{sub 2})]{sub 4} tetramer, formed via coordination of the two MeTAM units of L to two uranyl moieties. Addition of KOH to the tetramer gave the corresponding monomeric uranyl methoxide species [Me{sub 4}N]K{sub 2}[LUO{sub 2}(OMe)].

  14. Flexible and Asymmetric Ligand in Constructing Coordinated Complexes: Synthesis, Crystal Structures and Fluorescent Characterization

    Directory of Open Access Journals (Sweden)

    Jianhua Lin


    Full Text Available Flexible and asymmetric ligand L [L = 1-((pyridin-3-ylmethyl-1H-benzotriazole], is used as a basic backbone to construct complicated metal-organic frameworks. Two new polymers, namely, [Ag2(L2(NO32]n (1 and [Ag(L(ClO4]n (2, were synthesized and characterized by X-ray structure analysis and fluorescent spectroscopy. The complex 1 gives an “S” type double helical conformation, whereas complex 2 exhibits a 1D zigzag configuration. Different anions affect the silver coordination geometry and crystal packing topology.

  15. Characterization of structurally defined epitopes recognized by monoclonal antibodies produced by chronic lymphocytic leukemia B cells


    Seiler, Till; Woelfle, Manuela; Yancopoulos, Sophia; Catera, Rosa; Li, Wentian; Hatzi, Katerina; Moreno, Carol; Torres, Marcela; Paul, Santanu; Dohner, Hartmut; Stilgenbauer, Stephan; Kaufman, Matthew S.; Kolitz, Jonathan E.; Allen, Steven L.; Rai, Kanti R


    Despite a wealth of information about the structure of surface membrane immunoglobulin (smIg) on chronic lymphocytic leukemia (CLL) cells, little is known about epitopes reacting with their binding sites. Probing phage-displayed peptide libraries, we identified and characterized mimetopes for Igs of 4 patients with IGHV mutated CLL (M-CLL) and 4 with IGHV unmutated CLL (U-CLL). Six of these mAbs were representatives of stereotyped B-cell receptors characteristic of CLL. We found that mimetic ...

  16. Molecular characterization of pouched amphistome parasites (Trematoda: Gastrothylacidae) using ribosomal ITS2 sequence and secondary structures. (United States)

    Ghatani, S; Shylla, J A; Tandon, V; Chatterjee, A; Roy, B


    Members of the family Gastrothylacidae (Trematoda: Digenea: Paramphistomata) are parasitic in ruminants throughout Africa and Asia. In north-east India, five species of pouched amphistomes, namely Fischoederius cobboldi, F. elongatus, Gastrothylax crumenifer, Carmyerius spatiosus and Velasquezotrema tripurensis, belonging to this family have been reported so far. In the present study, the molecular phylogeny of these five gastrothylacid species is derived using the second internal transcribed spacer (ITS2) sequence and secondary structure analyses. ITS2 sequence analysis was carried out to see the occurrence of interspecific variations among the species. Phylogenetic analyses were performed for primary sequence data alone as well as the combined sequence-structure information using neighbour-joining and Bayesian approaches. The sequence analysis revealed that there exist considerable interspecific variations among the various gastrothylacid fluke species. In contrast, the inferred secondary structures for the five species using minimum free energy modelling showed structural identities, in conformity with the core four-helix domain structure that has been recently identified as common to almost all eukaryotic taxa. The phylogenetic tree reconstructed using combined sequence-structure data showed a better resolution, as compared to the one using sequence data alone, with the gastrothylacid species forming a monophyletic group that is well separated from members of the other family, Paramphistomidae, of the amphistomid flukes group. The study provides the molecular characterization based on primary sequence data of the rDNA ITS2 region of the gastrothylacid amphistome flukes. Results also demonstrate the phylogenetic utility of the ITS2 sequence-secondary structure data for inferences at higher taxonomic levels.

  17. Stochastic model reduction for robust dynamical characterization of structures with random parameters (United States)

    Ghienne, Martin; Blanzé, Claude; Laurent, Luc


    In this paper, we characterize random eigenspaces with a non-intrusive method based on the decoupling of random eigenvalues from their corresponding random eigenvectors. This method allows us to estimate the first statistical moments of the random eigenvalues of the system with a reduced number of deterministic finite element computations. The originality of this work is to adapt the method used to estimate each random eigenvalue depending on a global accuracy requirement. This allows us to ensure a minimal computational cost. The stochastic model of the structure is thus reduced by exploiting specific properties of random eigenvectors associated with the random eigenfrequencies being sought. An indicator with no additional computation cost is proposed to identify when the method needs to be enhanced. Finally, a simple three-beam frame and an industrial structure illustrate the proposed approach.

  18. Synthesis and characterization of Al-TON zeolite using a dialkylimizadolium as structure-directing agent

    Energy Technology Data Exchange (ETDEWEB)

    Lopes, Christian Wittee; Pergher, Sibele Berenice Castella, E-mail: [Universidade Federal do Rio Grande do Norte (UFRN), Natal, RN (Brazil); Villarroel-Rocha, Jhonny [Laboratorio de Solidos Porosos, Instituto de Fisica Aplicada, Universidad Nacional de San Luis, Chacabuco, San Luis (Argentina); Silva, Bernardo Araldi Da; Mignoni, Marcelo Luis [Universidade Regional Integrada, Erechim, RS (Brazil)


    In this work, the synthesis of zeolites using 1-butyl-3-methylimidazolium chloride [C{sub 4}MI]Cl as a structure-directing agent was investigated. The organic cation shows effectiveness and selectivity for the syntheses of TON zeolites under different reaction conditions compared to the traditional structure directing agent, 1,8-diaminooctane. The 1-butyl-3-methylimidazolium cation lead to highly crystalline materials and its role as OSDA in our synthesis conditions has been confirmed by characterization techniques. ICP-OES confirms the presence of Al in the samples and {sup 27}Al MAS NMR analysis indicated that aluminum atoms were incorporated in tetrahedral coordination. Scanning electron microscopy indicated that changing the crystallization condition (static or stirring), zeolites with different crystal size were obtained, which consequently affects the textural properties of the zeolites. Moreover, varying some synthesis parameters MFI zeolite can also be obtained. (author)

  19. Exchanging conformations of a hydroformylation catalyst structurally characterized using two-dimensional vibrational spectroscopy. (United States)

    Panman, Matthijs R; Vos, Jannie; Bocokić, Vladica; Bellini, Rosalba; de Bruin, Bas; Reek, Joost H N; Woutersen, Sander


    Catalytic transition-metal complexes often occur in several conformations that exchange rapidly (structures are difficult to characterize with conventional methods. Here, we determine specific bond angles in the two rapidly exchanging solution conformations of the hydroformylation catalyst (xantphos)Rh(CO)2H using two-dimensional vibrational spectroscopy, a method that can be applied to any catalyst provided that the exchange between its conformers occurs on a time scale of a few picoseconds or slower. We find that, in one of the conformations, the OC-Rh-CO angle deviates significantly from the canonical value in a trigonal-bipyramidal structure. On the basis of complementary density functional calculations, we ascribe this effect to attractive van der Waals interaction between the CO and the xantphos ligand.

  20. Structural characterization and ytterbium spectroscopy in Sc{sub 2}O{sub 3} nanocrystals

    Energy Technology Data Exchange (ETDEWEB)

    Galceran, M. [Fisica i Cristal.lografia de Materials i Nanomaterials (FiCMA-FiCNA), Universitat Rovira i Virgili (URV), Campus Sescelades, c/ Marcel. li Domingo, s/n, E-43007 Tarragona (Spain); Pujol, M.C., E-mail: [Fisica i Cristal.lografia de Materials i Nanomaterials (FiCMA-FiCNA), Universitat Rovira i Virgili (URV), Campus Sescelades, c/ Marcel. li Domingo, s/n, E-43007 Tarragona (Spain); Carvajal, J.J.; Mateos, X. [Fisica i Cristal.lografia de Materials i Nanomaterials (FiCMA-FiCNA), Universitat Rovira i Virgili (URV), Campus Sescelades, c/ Marcel. li Domingo, s/n, E-43007 Tarragona (Spain); Zaldo, C. [Instituto de Ciencia de Materiales de Madrid (ICMM), Consejo Superior de Investigaciones Cientificas (CSIC), c/ Sor Juana Ines de la Cruz 3, E-28049 Madrid (Spain); Aguilo, M.; Diaz, F. [Fisica i Cristal.lografia de Materials i Nanomaterials (FiCMA-FiCNA), Universitat Rovira i Virgili (URV), Campus Sescelades, c/ Marcel. li Domingo, s/n, E-43007 Tarragona (Spain)


    Ytterbium-doped scandium oxide nanocrystals measuring less than 25 nm with compositions of Sc{sub 2-x}Yb{sub x}O{sub 3} (x=0.001-1) were prepared using the modified Pechini method. The Yb:Sc{sub 2}O{sub 3} nanocrystals were obtained by calcination at low temperature such as 1073 K for 2 h. X-ray powder diffraction (XRD) and transmission electronic microscopy (TEM) were used to perform the structural characterization of nanocrystals; these studies indicated that the nanocrystals have high crystalline quality with cubic structure and Ia3-bar space group. The morphology and particle size were studied using electron microscopy. A detailed study of the effect of the nanodimension and the ytterbium concentration on the spectroscopic characteristics of Yb{sup 3+} as an active ion was carried out in terms of optical absorption, optical emission and fluorescence decay time at room and low temperature.

  1. Structural Characterization of Bimetallic Nanomaterials with Overlapping X-ray Absorption Edges

    Energy Technology Data Exchange (ETDEWEB)

    Menard, L.; Wang, Q; Kang, J; Sealey, A; Girolami, G; Teng, X; Frenkel, A; Nuzzo, R


    We describe a data analysis method for extended x-ray absorption fine structure spectroscopy suitable for use with compounds of diverse form that contain overlapping absorption edges. This method employs direct concurrent analysis of the data-demonstrated here for cases involving two interfering metal edges-and does not utilize subtractive or data filtering strategies that have been previously used to address this challenge. Its generality and precision are demonstrated in analyses made on two model nanoscale samples: (1) a Ir-Pt nanoparticle system supported on ?-Al2O3 and (2) a hybrid system of Pt nanowires on which Au nanoparticles have been nucleated and grown at the nanowire tips, stacking faults, and twinning boundaries. The results obtained demonstrate the unique compositional and structural qualities of these two systems as well as the broader utility of the new x-ray absorption spectroscopy based protocol used to characterize them.

  2. Characterization, Microbial Community Structure, and Pathogen Occurrence in Urban Faucet Biofilms in South China. (United States)

    Lin, Huirong; Zhang, Shuting; Gong, Song; Zhang, Shenghua; Yu, Xin


    The composition and microbial community structure of the drinking water system biofilms were investigated using microstructure analysis and 454 pyrosequencing technique in Xiamen city, southeast of China. SEM (scanning electron microscope) results showed different features of biofilm morphology in different fields of PVC pipe. Extracellular matrix material and sparse populations of bacteria (mainly rod-shaped and coccoid) were observed. CLSM (confocal laser scanning microscope) revealed different distributions of attached cells, extracellular proteins, α-polysaccharides, and β-polysaccharides. The biofilms had complex bacterial compositions. Differences in bacteria diversity and composition from different tap materials and ages were observed. Proteobacteria was the common and predominant group in all biofilms samples. Some potential pathogens (Legionellales, Enterobacteriales, Chromatiales, and Pseudomonadales) and corrosive microorganisms were also found in the biofilms. This study provides the information of characterization and visualization of the drinking water biofilms matrix, as well as the microbial community structure and opportunistic pathogens occurrence.

  3. Characterization and modeling of fiber reinforced concrete for structural applications in beams and plates

    DEFF Research Database (Denmark)

    Paegle, Ieva

    properties in direct tension and compression or from flexural beam tests. The model considers the balance between work done on the deformed structure and the energy required to induce the corresponding rotational deformations in the RFS. The flexural response in terms of load-deflection of a structural...... through flexural testing is generally easier to perform than direct tension tests in conventional testing laboratories. Various standardized test methods, based on beams and plates in flexure, are typically used to characterize FRC. However, the suitability of these methods for FRC materials with tension...... element can be accurately predicted for a FRC with either softening or hardening post cracking behavior in direct tension or bending. The model is verified through experimental results of four-point bending beams and round determinate panels. Additionally, potential applications of SFRC representing...

  4. Identification of inks and structural characterization of contemporary artistic prints by laser-induced breakdown spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Oujja, M. [Instituto de Quimica Fisica Rocasolano, CSIC, Serrano 119, 28006 Madrid (Spain); Vila, A. [Departament de Pintura, Conservacio-Restauracio, Facultat de Belles Arts, Universitat de Barcelona, Pau Gargallo 4, 08028 Barcelona (Spain); Rebollar, E. [Instituto de Quimica Fisica Rocasolano, CSIC, Serrano 119, 28006 Madrid (Spain); Garcia, J.F. [Departament de Pintura, Conservacio-Restauracio, Facultat de Belles Arts, Universitat de Barcelona, Pau Gargallo 4, 08028 Barcelona (Spain); Castillejo, M. [Instituto de Quimica Fisica Rocasolano, CSIC, Serrano 119, 28006 Madrid (Spain)]. E-mail:


    Identification of the inks used in artistic prints and the order in which different ink layers have been applied on a paper substrate are important factors to complement the classical stylistic aspects for the authentication of this type of objects. Laser-induced breakdown spectroscopy (LIBS) is investigated to determine the chemical composition and structural distribution of the constituent materials of model prints made by applying one or two layers of several blue and black inks on an Arches paper substrate. By using suitable laser excitation conditions, identification of the inks was possible by virtue of emissions from key elements present in their composition. Analysis of successive spectra on the same spot allowed the identification of the order in which the inks were applied on the paper. The results show the potential of laser-induced breakdown spectroscopy for the chemical and structural characterization of artistic prints.

  5. Synthesis, characterization and crystal structures of oxovanadium(V complexes derived from similar aroylhydrazone ligands

    Directory of Open Access Journals (Sweden)

    X-Z Zhang


    Full Text Available Reaction of [VO(acac2] (acac = acetylacetonate with N’-(5-chloro-2-hydroxybenzylidene-3-methoxybenzohydrazide (H2L1 and N’-(2-hydroxy-4-methoxybenzylidene-4-nitrobenzohydrazide (H2L2 in methanol affords methanol-coordinated mononuclear oxovanadium(V complexes, [VOL1(OMe(MeOH] (1 and [VOL2(OMe(MeOH] (2, respectively. The complexes were characterized by elemental analysis, FT-IR, 1H NMR and 13C NMR spectra. Crystal and molecular structures of the complexes were determined by single crystal X-ray diffraction method. Single crystal X-ray structural studies indicate that the hydrazone ligands coordinate to the VO core through enolate oxygen, phenolate oxygen and azomethine nitrogen. The V atoms in the complexes are in octahedral coordination. Thermal stabilities of the complexes have also been studied. DOI:

  6. Structure and biochemical characterization of proliferating cellular nuclear antigen from a parasitic protozoon

    Energy Technology Data Exchange (ETDEWEB)

    Cardona-Felix, Cesar S.; Lara-Gonzalez, Samuel; Brieba, Luis G. (LNLS)


    Proliferating cellular nuclear antigen (PCNA) is a toroidal-shaped protein that is involved in cell-cycle control, DNA replication and DNA repair. Parasitic protozoa are early-diverged eukaryotes that are responsible for neglected diseases. In this work, a PCNA from a parasitic protozoon was identified, cloned and biochemically characterized and its crystal structure was determined. Structural and biochemical studies demonstrate that PCNA from Entamoeba histolytica assembles as a homotrimer that is able to interact with and stimulate the activity of a PCNA-interacting peptide-motif protein from E. histolytica, EhDNAligI. The data indicate a conservation of the biochemical mechanisms of PCNA-mediated interactions between metazoa, yeast and parasitic protozoa.

  7. Ni(OH){sub 2} and NiO nano structures: Synthesis, characterization and electrochemical performance

    Energy Technology Data Exchange (ETDEWEB)

    Saghatforoush, Lotf Ali; Sanati, Soheila; Mehdizadeh, Robabeh [Payam Noor Univ., Tehran (Iran, Islamic Republic of); Hasanzadeh, Mohammad [Tabriz Univ. of Medical Sciences, Tabriz (Iran, Islamic Republic of)


    Hydrothermal route have been used in different conditions for preparation of Ni(OH){sub 2} nano structures. The NiO nanoparticles were obtained by calcining the Ni(OH){sub 2} precursor at 450 .deg. C for 2 h. The effect of sodium dodecyl sulfonate (SDS) as surfactant on the morphology and size of Ni(OH){sub 2} nanoparticles were discussed in detail. X-ray diffraction (XRD), Scanning electron microscopy (SEM), Transmission electron microscopy (TEM) and Fourier transform infrared (FT-IR) spectroscopy were used to characterize the products. The growth mechanism of the as-synthesized nano structures was also discussed in detail based on the experimental results. Coming up, the NiO nanoparticle modified carbon paste electrode was applied to the determination of captopril in aqueous solution.

  8. Characterization, Microbial Community Structure, and Pathogen Occurrence in Urban Faucet Biofilms in South China

    Directory of Open Access Journals (Sweden)

    Huirong Lin


    Full Text Available The composition and microbial community structure of the drinking water system biofilms were investigated using microstructure analysis and 454 pyrosequencing technique in Xiamen city, southeast of China. SEM (scanning electron microscope results showed different features of biofilm morphology in different fields of PVC pipe. Extracellular matrix material and sparse populations of bacteria (mainly rod-shaped and coccoid were observed. CLSM (confocal laser scanning microscope revealed different distributions of attached cells, extracellular proteins, α-polysaccharides, and β-polysaccharides. The biofilms had complex bacterial compositions. Differences in bacteria diversity and composition from different tap materials and ages were observed. Proteobacteria was the common and predominant group in all biofilms samples. Some potential pathogens (Legionellales, Enterobacteriales, Chromatiales, and Pseudomonadales and corrosive microorganisms were also found in the biofilms. This study provides the information of characterization and visualization of the drinking water biofilms matrix, as well as the microbial community structure and opportunistic pathogens occurrence.

  9. Cryo-FIB SEM for Characterization of the Structure of Fish Oil Emulsions

    DEFF Research Database (Denmark)

    Jensen, Louise Helene Søgaard; Horn, Anna Frisenfeldt; Jacobsen, Charlotte


    such strategy is to add the oil as an emulsion rather than as neat oil. Studies so far have indicated that emulsification of the fish oil changes the oxidative stability of the product but whether emulsification is an advantage seems to be dependent on the food matrix to which the emulsion is added [1, 2......]. It is therefore of interest to look at the emulsions to assess what determines the oxidation. It has been proposed that oxidation is to some extent dependent on the structure of the emulsion; including oil droplet sizes, size distribution and the thickness of the interface between oil and water. This interface...... can be stabilized by food grade emulsifiers such as proteins and phospholipids from milk. The main objective of this study is to characterize fish oil in water emulsions with respect to oil droplet size, size distribution, and ultimately to view the thickness, structure and morphology of the interface...

  10. Microstructural Characterization of a Prototype Titanium Alloy Structure Processed via Direct Laser Deposition (DLD) (United States)

    Clark, Daniel; Whittaker, Mark T.; Bache, Martin R.


    Processing trials have produced a three-dimensional, thin-walled structure of representative aerospace component geometry, fabricated directly by laser melting of Ti 6Al4V powder. This additive-built form has been subjected to metallographic characterization. The fabrication technique is evaluated as an economic, commercial process that can add features such as bosses or flanges as a hybrid-manufacturing route for existing forms of gas turbine components. The samples were extracted from six locations with different wall thickness, varying forms, and intersecting ligament geometries. A fine-scale Widmanstätten colony microstructure was consistent throughout the structure within grains elongated parallel to the axis of epitaxy. Evidence of limited grain boundary α was detected; however, this was never continuous around individual grains. A moderate Burgers texture was measured employing electron backscatter diffraction (EBSD), which is consistent with the melt/cast titanium alloy forms cooling through the β transus.

  11. Platinum acetate blue: synthesis and characterization. (United States)

    Cherkashina, Natalia V; Kochubey, Dmitry I; Kanazhevskiy, Vladislav V; Zaikovskii, Vladimir I; Ivanov, Vladimir K; Markov, Alexander A; Klyagina, Alla P; Dobrokhotova, Zhanna V; Kozitsyna, Natalia Yu; Baranovsky, Igor B; Ellert, Olga G; Efimov, Nikolai N; Nefedov, Sergei E; Novotortsev, Vladimir M; Vargaftik, Michael N; Moiseev, Ilya I


    Platinum acetate blue (PAB) of the empirical formula Pt(OOCMe)2.5±0.25, a byproduct in the synthesis of crystalline platinum(II) acetate Pt4(OOCMe)8, is an X-ray amorphous substance containing platinum in the oxidation state between (II) and (III). Typical PAB samples were studied with X-ray diffraction, differential thermal analysis-thermogravimetric, extended X-ray absorption fine structure, scanning electron microscopy, transmission electron microscopy, magnetochemistry, and combined quantum chemical density functional theory-molecular mechanics modeling to reveal the main structural features of the PAB molecular building blocks. The applicability of PAB to the synthesis of platinum complexes was demonstrated by the preparation of the new homo- and heteronuclear complexes Pt(II)(dipy)(OOCMe)2 (1), Pt(II)(μ-OOCMe)4Co(II)(OH2) (2), and Pt(III)2(OOCMe)4(O3SPhMe)2 (3) with the use of PAB as starting material.

  12. Design, construction and characterization of fiber extensometer with heart shape structure for detection of displacement (United States)

    Bayuwati, D.; Waluyo, T. B.


    This paper discusses the design, construction and characterization of an optical fiber extensometer with heart shape structure. The extensometer was made from a communication grade fiber loop arranged in a housing and pulling mechanism. As the light source, we used 1310 nm LED and a 1325 nm laser diode/LD. To characterize our extensometer, we used a motorized pulling system controlled by a personal computer. From the bending loss characterization using Fujikura fiber as the sensor, we obtained sensitivity of 0.04 dB/mm and measurement range of 28 mm when using the 1310 nm LED, whereas using the 1325 nm LD allowed us to obtain 0.06 dB/mm of sensitivity and 23 mm of measurement range. Using Thorlabs fiber as the sensor, we obtained sensitivity and measurement range of 0.09 dB/mm and 23 mm, respectively, when using the 1310 nm LED. When we used the 1325 nm LD, we obtained sensitivity of 0.03 dB/mm and 31 mm measurement range but with a noted whispering gallery mode/WGM effect. Compromise has to be considered amongst the high sensitivity, measurement range, WGM existence and noise properties to get best data reading for real application.

  13. Fabrication, polarization, and characterization of PVDF matrix composites for integrated structural load sensing (United States)

    Haghiashtiani, Ghazaleh; Greminger, Michael A.


    The focus of this work is to evaluate a new carbon fiber reinforced composite structure with integrated sensing capabilities. In this composite structure, the typical matrix material used for carbon fiber reinforced composites is replaced with the thermoplastic polyvinylidene difluoride (PVDF). Since PVDF has piezoelectric properties, it enables the structure to be used for integrated load sensing. In addition, the electrical conductivity property of the carbon fabric is harnessed to form the electrodes of the integrated sensor. In order to prevent the carbon fiber electrodes from shorting to each other, a thin Kevlar fabric layer is placed between the two carbon fiber electrode layers as a dielectric. The optimal polarization parameters were determined using a design of experiments approach. Once polarized, the samples were then used in compression and tensile tests to determine the effective d33 and d31 piezoelectric coefficients. The degree of polarization of the PVDF material was determined by relating the effective d33 coefficient of the composite to the achieved d33 of the PVDF component of the composite using a closed form expression. Using this approach, it was shown that optimal polarization of the composite material results in a PVDF component d33 of 3.2 pC N-1. Moreover, the Young’s modulus of the composite structure has been characterized.

  14. Experimental Investigation on Pore Structure Characterization of Concrete Exposed to Water and Chlorides

    Directory of Open Access Journals (Sweden)

    Jun Liu


    Full Text Available In this paper, the pore structure characterization of concrete exposed to deionised water and 5% NaCl solution was evaluated using mercury intrusion porosity (MIP, scanning electron microscopy (SEM and X-ray diffraction (XRD. The effects of calcium leaching, fly ash incorporation, and chloride ions on the evolution of pore structure characteristics were investigated. The results demonstrate that: (i in ordinary concrete without any fly ash, the leaching effect of the cement products is more evident than the cement hydration effect. From the experimental data, Ca(OH2 is leached considerably with the increase in immersion time. The pore structure of concrete can also be affected by the formation of an oriented structure of water in concrete materials; (ii incorporation of fly ash makes a difference for the performance of concrete submersed in solutions as the total porosity and the pore connectivity can be lower. Especially when the dosage of fly ash is up to 30%, the pores with the diameter of larger than 100 nm show significant decrease. It demonstrates that the pore properties are improved by fly ash, which enhances the resistance against the calcium leaching; (iii chlorides have a significant impact on microstructure of concrete materials because of the chemical interactions between the chlorides and cement hydrates.

  15. Structural characterization of Spinacia oleracea trypsin inhibitor III (SOTI-III). (United States)

    Glotzbach, Bernhard; Schmelz, Stefan; Reinwarth, Michael; Christmann, Andreas; Heinz, Dirk W; Kolmar, Harald


    In recent decades, several canonical serine protease inhibitor families have been classified and characterized. In contrast to most trypsin inhibitors, those from garden four o'clock (Mirabilis jalapa) and spinach (Spinacia oleracea) do not share sequence similarity and have been proposed to form the new Mirabilis serine protease inhibitor family. These 30-40-amino-acid inhibitors possess a defined disulfide-bridge topology and belong to the cystine-knot miniproteins (knottins). To date, no atomic structure of this inhibitor family has been solved. Here, the first structure of S. oleracea trypsin inhibitor III (SOTI-III), in complex with bovine pancreatic trypsin, is reported. The inhibitor was synthesized by solid-phase peptide synthesis on a multi-milligram scale and was assayed to test its inhibitory activity and binding properties. The structure confirmed the proposed cystine-bridge topology. The structural features of SOTI-III suggest that it belongs to a new canonical serine protease inhibitor family with promising properties for use in protein-engineering and medical applications.

  16. Characterization of carbonized polydopamine nanoparticles suggests ordered supramolecular structure of polydopamine. (United States)

    Yu, Xiang; Fan, Hailong; Liu, Yang; Shi, Zujin; Jin, Zhaoxia


    Polydopamine is not only a multifunctional biopolymer with promising optoelectronic properties but it is also a versatile coating platform for different surfaces. The structure and formation of polydopamine is an active area of research. Some studies have supposed that polydopamine is composed of covalently bonded dihydroxyindole, indoledione, and dopamine units, but others proposed that noncovalent self-assembly contributes to polydopamine formation as well. However, it is difficult to directly find the details of supramolecular structure of polydopamine via self-assembly. In this study, we first report the graphite-like nanostructure observed in the carbonized polydopamine nanoparticles in nitrogen (or argon) environment at 800 °C. Raman characterization, which presents the typical D band and G band, confirmed the existence of graphite-like nanostructures. Our observation provides clear evidence for a layered-stacking supramolecular structure of polydopamine. Particularly, the size of graphite-like domains is similar to that of disk-shaped aggregates hypothesized in previous study about the polymerization of 5,6-dihydroxyindole [ Biomacromolecules 2012 , 13 , 2379 ]. Analysis of the hierarchical structure of polydopamine helps us understand its formation.

  17. Biochemical and structural characterization of a novel bacterial manganese-dependent hydroxynitrile lyase. (United States)

    Hajnal, Ivan; Lyskowski, Andrzej; Hanefeld, Ulf; Gruber, Karl; Schwab, Helmut; Steiner, Kerstin


    Hydroxynitrile lyases (HNLs), which catalyse the decomposition of cyanohydrins, are found mainly in plants. In vitro, they are able to catalyse the synthesis of enantiopure cyanohydrins, which are versatile building blocks in the chemical industry. Recently, HNLs have also been discovered in bacteria. Here, we report on the detailed biochemical and structural characterization of a hydroxynitrile lyase from Granulicella tundricola (GtHNL), which was successfully heterologously expressed in Escherichia coli. The crystal structure was solved at a crystallographic resolution of 2.5 Å and exhibits a cupin fold. As GtHNL does not show any sequence or structural similarity to any other HNL and does not contain conserved motifs typical of HNLs, cupins represent a new class of HNLs. GtHNL is metal-dependent, as confirmed by inductively coupled plasma/optical emission spectroscopy, and in the crystal structure, manganese is bound to three histidine and one glutamine residue. GtHNL displayed a specific activity of 1.74 U·mg(-1) at pH 6 with (R)-mandelonitrile, and synthesized (R)-mandelonitrile with 90% enantiomeric excess at 80% conversion using 0.5 m benzaldehyde in a biphasic reaction system with methyl tertiary butyl ether. © 2013 FEBS.

  18. Structural, Nanomechanical and Nanotribological Characterization of Human Hair Using Atomic Force Microscopy and Nanoindentation (United States)

    Bhushan, Bharat; Latorre, Carmen; Wei, Guohua

    Human hair is a nanocomposite biological fiber. Healthy, soft hair with good feel, shine, color and overall aesthetics is generally highly desirable. It is important to study hair care products such as shampoos and conditioners as well as damaging processes such as chemical dyeing and permanent wave treatments because they affect the maintenance and grooming process and therefore alter many hair properties. Nanoscale characterization of the cellular structure, the mechanical properties, as well as the morphological, frictional and adhesive properties (tribological properties) of hair is essential if we wish to evaluate and develop better cosmetic products, and crucial to advancing the understanding of biological and cosmetic science. The atomic/friction force microscope (AFM/FFM) and nanoindenter have recently become important tools for studying the micro/nanoscale properties of human hair. In this chapter, we present a comprehensive review of structural, mechanical, and tribological properties of various hair and skin as a function of ethnicity, damage, conditioning treatment, and various environments. Various cellular structures of human hair and fine sublamellar structures of the cuticle are identified and studied. Nanomechanical properties such as hardness, elastic modulus, creep and scratch resistance are discussed. Nanotribological properties such as roughness, friction, and adhesion are presented, as well as investigations of conditioner distribution, thickness and binding interactions.

  19. Characterizing changes in soil bacterial community structure in response to short-term warming

    Energy Technology Data Exchange (ETDEWEB)

    Xiong, Jinbo [State Key Laboratory of Soil and Sustainable Agriculture, Institute of Soil Science, Chinese Academy of Sciences, Nanjing China; School of Marine Sciences, Ningbo University, Ningbo China; Sun, Huaibo [State Key Laboratory of Soil and Sustainable Agriculture, Institute of Soil Science, Chinese Academy of Sciences, Nanjing China; Peng, Fei [Key Laboratory of Desert and Desertification, Cold and Arid Regions Environmental and Engineering Research Institute, Chinese Academy of Sciences, Lanzhou China; Zhang, Huayong [State Key Laboratory of Soil and Sustainable Agriculture, Institute of Soil Science, Chinese Academy of Sciences, Nanjing China; Xue, Xian [Key Laboratory of Desert and Desertification, Cold and Arid Regions Environmental and Engineering Research Institute, Chinese Academy of Sciences, Lanzhou China; Gibbons, Sean M. [Argonne National Laboratory Biosciences Division, Argonne IL USA; Graduate Program in Biophysical Sciences, University of Chicago, Chicago IL USA; Gilbert, Jack A. [Argonne National Laboratory Biosciences Division, Argonne IL USA; Department of Ecology and Evolution, University of Chicago, Chicago IL USA; Chu, Haiyan [State Key Laboratory of Soil and Sustainable Agriculture, Institute of Soil Science, Chinese Academy of Sciences, Nanjing China


    High altitude alpine meadows are experiencing considerably greater than average increases in soil surface temperature, potentially as a result of ongoing climate change. The effects of warming on plant productivity and soil edaphic variables have been established previously, but the influence of warming on soil microbial community structure has not been well characterized. Here, the impact of 15 months of soil warming (both + 1 and + 2 degrees C) on bacterial community structure was examined in a field experiment on a Tibetan plateau alpine meadow using bar-coded pyrosequencing. Warming significantly changed (P < 0.05) the structure of the soil bacterial community, but the alpha diversity was not dramatically affected. Changes in the abundance of the Actinobacteria and Alphaproteobacteria were found to contribute the most to differences between ambient (AT) and artificially warmed conditions. A variance partitioning analysis (VPA) showed that warming directly explained 7.15% variation in bacterial community structure, while warming-induced changes in soil edaphic and plant phenotypic properties indirectly accounted for 28.3% and 20.6% of the community variance, respectively. Interestingly, certain taxa showed an inconsistent response to the two warming treatments, for example Deltaproteobacteria showed a decreased relative abundance at + 1 degrees C, but a return to AT control relative abundance at + 2 degrees C. This suggests complex microbial dynamics that could result from conditional dependencies between bacterial taxa.

  20. Structural characterization of substituted lanthanum tungstates with X-ray and neutron diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Fantin, Andrea; Scherb, Tobias; Schumacher, Gerhard [Helmholtz-Zentrum Berlin fuer Materialen und Energie (Germany); Seeger, Janka; Meulenberg, Wilhelm A. [Forschungszentrum Juelich (Germany)


    Our work on proton conducting materials deals with structural characterization of two different series of substituted lanthanum tungstates: La5.4W(1-x)MxO12-delta with M=Mo,Re and 0<=x<=0.2. The main methods used to understand their crystal structure are Neutron Diffraction (ND) and High-Resolution X-Ray Diffraction (HRXRD). Experiments were carried at ILL (Grenoble, France) and PSI (Villigen, Switzerland). Different elemental contrast is reached with these complementary diffraction techniques. Our specimens consist of three cations (La, W, Mo or Re) and oxygen anions. In order to distinguish W (Z=74, b=4.86fm) and Re (Z=75, b=9.2fm) neutrons are needed, while for La (Z=57, b=8.2fm), W(Z=74, b=4.86fm) and Mo (Z=42, b=6.7fm) good contrast is also given by X-Rays. Combined refinements to model accurately anti-site disorder, position of the substituted elements and oxygen (Z=8, b=5.8fm) positions in this highly disordered material are mandatory. Measurements in dependence of temperature down to 1.5K confirm the structural model suggested by one of the coauthors without any unmodeled static disorder. Substitution and deuteration/humidification show no relevant structural changes.

  1. Micro- and nano-structural characterization of six marine sponges of the class Demospongiae. (United States)

    Şen, Elif Hilal; Ide, Semra; Bayari, Sevgi Haman; Hill, Malcolm


    The sponges produce their skeletal elements and silicateins are the key enzymes in this process. The mechanism underlying the formation of their silica skeleton and its structural properties are of exceptional interest for applications in technology. Micro- and nano-scale structural analysis of the six marine sponges belonging to Demospongiae [Callyspongia (Cladochalia) plicifera (Lamarck, 1814), Cervicornia cuspidifera (Lamarck, 1815), Cinachyrela sp., Niphates erecta (Duchassaing and Michelotti, 1864), Xestospongia muta (Schmidt, 1870) and Amphimedon compressa (Duchassaing and Michelotti, 1864)] were carried out by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM/EDX) and Small-Angle X-ray Scattering (SAXS) techniques. The nano-structural characterizations give some informative evidence about the manner in which silica/silicatein in spicule skeletons is produced by the sponges. The sponge species were successfully discriminated using cluster analysis (HCA) based on FTIR spectra. This study demonstrates and detection of structural differences among sponges and their spicules using combined techniques.

  2. Structural and dynamic characterization of eukaryotic gene regulatory protein domains in solution

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Andrew Loyd [Univ. of California, Berkeley, CA (United States). Dept. of Chemistry


    Solution NMR was primarily used to characterize structure and dynamics in two different eukaryotic protein systems: the δ-Al-ε activation domain from c-jun and the Drosophila RNA-binding protein Sex-lethal. The second system is the Drosophila Sex-lethal (Sxl) protein, an RNA-binding protein which is the ``master switch`` in sex determination. Sxl contains two adjacent RNA-binding domains (RBDs) of the RNP consensus-type. The NMR spectrum of the second RBD (Sxl-RBD2) was assigned using multidimensional heteronuclear NMR, and an intermediate-resolution family of structures was calculated from primarily NOE distance restraints. The overall fold was determined to be similar to other RBDs: a βαβ-βαβ pattern of secondary structure, with the two helices packed against a 4-stranded anti-parallel β-sheet. In addition 15N T1, T2, and 15N/1H NOE relaxation measurements were carried out to characterize the backbone dynamics of Sxl-RBD2 in solution. RNA corresponding to the polypyrimidine tract of transformer pre-mRNA was generated and titrated into 3 different Sxl-RBD protein constructs. Combining Sxl-RBD1+2 (bht RBDs) with this RNA formed a specific, high affinity protein/RNA complex that is amenable to further NMR characterization. The backbone 1H, 13C, and 15N resonances of Sxl-RBD1+2 were assigned using a triple-resonance approach, and 15N relaxation experiments were carried out to characterize the backbone dynamics of this complex. The changes in chemical shift in Sxl-RBD1+2 upon binding RNA are observed using Sxl-RBD2 as a substitute for unbound Sxl-RBD1+2. This allowed the binding interface to be qualitatively mapped for the second domain.

  3. Solvate Structures and Computational/Spectroscopic Characterization of LiBF4 Electrolytes

    Energy Technology Data Exchange (ETDEWEB)

    Seo, D. M.; Boyle, Paul D.; Allen, Joshua L.; Han, Sang D.; Jonsson, Erlendur; Johansson, Patrik; Henderson, Wesley A.


    Crystal structures have been determined for both LiBF4 and HBF4 solvates—(acetonitrile)2:LiBF4, (ethylene glycol diethyl ether)1:LiBF4, (diethylene glycol diethyl ether)1:LiBF4, (tetrahydrofuran)1:LiBF4, (methyl methoxyacetate)1:LiBF4, (suc-cinonitrile)1:LiBF4, (N,N,N',N",N"-pentamethyldiethylenetriamine)1:HBF4, (N,N,N',N'-tetramethylethylenediamine)3/2:HBF4 and (phenanthroline)2:HBF4. These, as well as other known LiBF4 solvate structures, have been characterized by Raman vibrational spectroscopy to unambiguously assign the anion Raman band positions to specific forms of BF4-...Li+ cation coordination. In addition, complementary DFT calculations of BF4-...Li+ cation complexes have provided additional insight into the challenges associated with accurately interpreting the anion interactions from experimental Raman spectra. This information provides a crucial tool for the characterization of the ionic association interactions within electrolytes.

  4. Structural characterization of supported nanocrystalline ZnO thin films prepared by dip-coating

    Energy Technology Data Exchange (ETDEWEB)

    Casanova, J.R. [CITEDEF-CINSO-CONICET Centro de Investigaciones en Solidos, Juan B. de La Salle 4397, B1603ALO, Villa Martelli, Buenos Aires (Argentina); Heredia, E.A., E-mail: [CITEDEF-CINSO-CONICET Centro de Investigaciones en Solidos, Juan B. de La Salle 4397, B1603ALO, Villa Martelli, Buenos Aires (Argentina); Bojorge, C.D.; Canepa, H.R. [CITEDEF-CINSO-CONICET Centro de Investigaciones en Solidos, Juan B. de La Salle 4397, B1603ALO, Villa Martelli, Buenos Aires (Argentina); Kellermann, G. [Departamento de Fisica, Universidade Federal do Parana, Curitiba, PR (Brazil); Craievich, A.F. [Instituto de Fisica, Universidade de Sao Paulo, Cidade Universitaria, Sao Paulo, SP (Brazil)


    Nanocrystalline ZnO thin films prepared by the sol-gel dip-coating technique were characterized by grazing incidence X-ray diffraction (GIXD), atomic force microscopy (AFM), X-ray reflectivity (XR) and grazing incidence small-angle X-ray scattering (GISAXS). The structures of several thin films subjected to (i) isochronous annealing at 350, 450 and 550 deg. C, and (ii) isothermal annealing at 450 deg. C during different time periods, were characterized. The studied thin films are composed of ZnO nanocrystals as revealed by analysing several GIXD patterns, from which their average sizes were determined. Thin film thickness and roughness were determined from quantitative analyses of AFM images and XR patterns. The analysis of XR patterns also yielded the average density of the studied films. Our GISAXS study indicates that the studied ZnO thin films contain nanopores with an ellipsoidal shape, and flattened along the direction normal to the substrate surface. The thin film annealed at the highest temperature, T = 550 deg. C, exhibits higher density and lower thickness and nanoporosity volume fraction, than those annealed at 350 and 450 deg. C. These results indicate that thermal annealing at the highest temperature (550 deg. C) induces a noticeable compaction effect on the structure of the studied thin films.

  5. Isolation and structural characterization of a polysaccharide LRP4-A from Lycium ruthenicum Murr. (United States)

    Lv, Xiaopeng; Wang, Chengjian; Cheng, Yang; Huang, Linjuan; Wang, Zhongfu


    A complex polysaccharide, termed LRP4-A, was isolated from the fruit of Lycium ruthenicum Murr. and its structure was characterized. The crude polysaccharide LRP was obtained from the fruit of L. ruthenicum Murr. using hot water extraction followed by ethanol precipitation. The water-soluble polysaccharide LRP4-A was purified from LRP by anion-exchange chromatography and gel filtration chromatography. Its molecular weight was 1.05×10(5) Da. Monosaccharide composition analysis revealed that LRP4-A mainly consisted of rhamnose, arabinose, glucose, and galactose in the molar ratio of 1:7.6:0.5:8.6, with a trace of xylose. Structure of the polysaccharide LRP4-A was characterized using a series of analytical techniques, including methylation analysis, partial acid hydrolysis, IR, NMR, and ESI-MS. LRP4-A was identified to be a highly branching polysaccharide with a backbone of β-(1→6)-linked galactose partially substituted at O-3 position. The branches were composed of (1→3)-linked-Gal, (1→3)-linked-Ara, (1→5)-linked-Ara, and (1→2,4)-linked-Rha. Arabinose, galactose, and glucose were located at the termini of the branches. Copyright © 2012 Elsevier Ltd. All rights reserved.

  6. Tunable mechanical monolithic sensors for large band low frequency monitoring and characterization of sites and structures (United States)

    Barone, F.; Giordano, G.; Acernese, F.; Romano, R.


    Among the different mechanical architectures present in literature, the Watts linkage is one of the most promising ones for the implementation of a new class of mechanical accelerometers (horizontal, vertical and angular). In this paper, we present monolithic implementations of uniaxial and triaxial mechanical seismometers and accelerometers based on the UNISA Folded Pendulum mechanical configuration, optimized for low frequency characterization of sites (including underground sites) and structures as inertial sensor (seismometer). This mechanical architecture allows the design and implementation of very large band monolithic sensors (10-7Hz 102 Hz), whose sensitivities for the most common applications are defined by the noise introduced by their readouts (e.g. ¡ 10-12 m/sqrt(Hz) with classical LVDT readouts). These unique features, coupled other relevant properties like scalability, compactness, lightness, high directivity, frequency tunability (typical resonance frequencies in the band 10-1 Hz 102 Hz), very high immunity to environmental noises and low cost make this class of sensors very effective for the implementation of uniaxial (horizontal and/or vertical) and triaxial seismometers and accelerometers for ground, space and underwater applications, including UHV and cryogenics ones. Typical applications of this class of monolithic sensors are in the field of earthquake engineering, seismology, geophysics, civil engineering, characterization of sites (including underground sites), structures (e.g. buildings, bridges, historical monuments), and, in general, in all applications requiring large band-low frequency performances coupled with high sensitivities and compactness.

  7. Synthesis, fine structural characterization, and CO2 adsorption capacity of metal organic frameworks-74. (United States)

    Adhikari, Abhijit Krishna; Lin, Kuen-Song


    Two metal organic frameworks of MOF-74 group (zinc and copper-based) were successfully synthesized, characterized, and evaluated for CO2 adsorption. The both samples such as MOF-74(Zn) and MOF-74(Cu) were characterized with FE-SEM for morphology and particle size, XRD patterns for phase structure, FTIR for organic functional groups, nitrogen adsorption for pore textural properties, and X-ray absorption spectroscopy for fine structural parameters and oxidation states of central metal atoms. CO2 adsorption isotherms of MOF-74 samples were measured in a volumetric adsorption unit at 273 K and pressure up to 1.1 bar. The MOF-74(Zn) and MOF-74(Cu) adsorbents have the pore widths of 8.58 and 8.04 angstroms with the BET specific surface areas of 1,474 and 1,345 m2 g(-1), respectively. CO2 adsorption capacities of MOF-74(Zn) and MOF-74(Cu) were 4.10 and 3.38 mmol x g(-1), respectively measured at 273 K and 1.1 bar. The oxidation state of central atoms in MOF-74(Zn) was Zn(II) confirmed by XANES spectra while MOF-74(Cu) was composed of Cu(I) and Cu(II) central atoms. The bond distances of Zn--O and Cu--O were 1.98 and 1.94 angstroms, respectively.

  8. Chemical and structural characterization of char development during lignocellulosic biomass pyrolysis. (United States)

    Mafu, Lihle D; Neomagus, Hein W J P; Everson, Raymond C; Strydom, Christien A; Carrier, Marion; Okolo, Gregory N; Bunt, John R


    The chemical and structural changes of three lignocellulosic biomass samples during pyrolysis were investigated using both conventional and advanced characterization techniques. The use of ATR-FTIR as a characterization tool is extended by the proposal of a method to determine aromaticity, the calculation of both CH2/CH3 ratio and the degree of aromatic ring condensation ((R/C)u). With increasing temperature, the H/C and O/C ratios, XA and CH2/CH3 ratio decreased, while (R/C)u and aromaticity increased. The micropore network developed with increasing temperature, until the coalescence of pores at 1100°C, which can be linked to increasing carbon densification, extent of aromatization and/or graphitization of the biomass chars. WAXRD-CFA measurements indicated the gradual formation of nearly parallel basic structural units with increasing carbonization temperature. The char development can be considered to occur in two steps: elimination of aliphatic compounds at low temperatures, and hydrogen abstraction and aromatic ring condensation at high temperatures. Copyright © 2017 Elsevier Ltd. All rights reserved.

  9. Monodentate Schiff base ligands: their structural characterization, photoluminescence, anticancer, electrochemical and sensor properties. (United States)

    Köse, Muhammet; Ceyhan, Gökhan; Tümer, Mehmet; Demirtaş, Ibrahim; Gönül, İlyas; McKee, Vickie


    Two Schiff base compounds, N,N'-bis(2-methoxy phenylidene)-1,5-diamino naphthalene (L(1)) and N,N'-bis(3,4,5-trimethoxy phenylidene)-1,5-diamino naphthalene (L(2)) were synthesized and characterized by the analytical and spectroscopic methods. The electrochemical and photoluminescence properties of the Schiff bases were investigated in the different conditions. The compounds L(1) and L(2) show the reversible redox processes at some potentials. The sensor properties of the Schiff bases were examined and color changes were observed upon addition of the metal cations, such as Hg(II), Cu(II), Co(II) and Al(III). The Schiff base compounds show the bathochromic shift from 545 to 585 nm. The single crystals of the compounds (L(1)) and (L(2)) were obtained from the methanol solution and characterized structurally by the X-ray crystallography technique. The molecule L(2) is centrosymmetric whereas the L(1) has no crystallographically imposed molecular symmetry. However, the molecular structures for these compounds are quite similar, differing principally in the conformation about methoxy groups and the dihedral angle between the two aromatic rings and diamine naphthalene. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Structural characterization, luminescence and electrochemical properties of the Schiff base ligands

    Energy Technology Data Exchange (ETDEWEB)

    Ceyhan, Goekhan [Chemistry Department, K. Maras Suetcue Imam University, 46100 K. Maras (Turkey); Tuemer, Mehmet, E-mail: [Chemistry Department, K. Maras Suetcue Imam University, 46100 K. Maras (Turkey); Koese, Muhammet; McKee, Vickie [Chemistry Department, Loughborough University, LE11 3TU Leics (United Kingdom); Akar, Seyhan [Chemistry Department, K. Maras Suetcue Imam University, 46100 K. Maras (Turkey)


    In this study, we prepared two Schiff base ligands N-(4-hydroxy phenyl)-2,4-di-methoxy benzaldimine (TS{sup 1}) and N-(4-hydroxy phenyl)-2,5-di-methoxybenzaldimine (TS{sup 2}) which were characterized by structural, spectroscopic and analytical methods. The ligands TS{sup 1} and TS{sup 2} were obtained as single crystals from ethanol solution. X-ray diffraction data for two compounds showed that the bond lengths are within the normal ranges. The electrochemical properties of the Schiff base ligands were studied in different solvents and at various scan rates. The luminescence properties of the ligands TS{sup 1} and TS{sup 2} in different solvents and at different pH values have been investigated. The results show that the ligands exhibit more efficient luminescence properties in CH{sub 3}CN and n-butanol. - Highlights: Black-Right-Pointing-Pointer Schiff base ligands were prepared and fully characterized. Black-Right-Pointing-Pointer X-ray crystal structures of Schiff base ligands were reported. Black-Right-Pointing-Pointer Electrochemical properties of Schiff base ligands were investigated. Black-Right-Pointing-Pointer Absorption and photoluminescence properties of the Schiff bases were examined.

  11. Instrumental methods and techniques for structural and physicochemical characterization of biomaterials and bone tissue: A review. (United States)

    Mitić, Žarko; Stolić, Aleksandra; Stojanović, Sanja; Najman, Stevo; Ignjatović, Nenad; Nikolić, Goran; Trajanović, Miroslav


    A review of recent advances in instrumental methods and techniques for structural and physicochemical characterization of biomaterials and bone tissue is presented in this paper. In recent years, biomaterials attracted great attention primarily because of the wide range of biomedical applications. This paper focuses on the practical aspects of instrumental methods and techniques that were most often applied (X-ray methods, vibrational spectroscopy (IR and Raman), magnetic-resonance spectroscopy (NMR and ESR), mass spectrometry (MS), atomic absorption spectrometry (AAS) and inductively coupled plasma-atomic emission spectrometry (ICP-AES), thermogravimetry (TG), differential thermal analysis (DTA) and differential scanning calorimetry (DSC), scanning electron microscopy (SEM), transmission electron microscopy (TEM)) in the structural investigation and physicochemical characterization of biomaterials and bone tissue. The application of some other physicochemical methods was also discussed. Hands-on information is provided about these valuable research tools, emphasizing practical aspects such as typical measurement conditions, their limitations and advantages, interpretation of results and practical applications. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. Mechanical characterization and structural analysis of recycled fiber-reinforced-polymer resin-transfer-molded beams (United States)

    Tan, Eugene Wie Loon


    The present investigation was focussed on the mechanical characterization and structural analysis of resin-transfer-molded beams containing recycled fiber-reinforced polymers. The beams were structurally reinforced with continuous unidirectional glass fibers. The reinforcing filler materials consisted entirely of recycled fiber-reinforced polymer wastes (trim and overspray). The principal resin was a 100-percent dicyclo-pentadiene unsaturated polyester specially formulated with very low viscosity for resin transfer molding. Variations of the resin transfer molding technique were employed to produce specimens for material characterization. The basic materials that constituted the structural beams, continuous-glass-fiber-reinforced, recycled-trim-filled and recycled-overspray-filled unsaturated polyesters, were fully characterized in axial and transverse compression and tension, and inplane and interlaminar shear, to ascertain their strengths, ultimate strains, elastic moduli and Poisson's ratios. Experimentally determined mechanical properties of the recycled-trim-filled and recycled-overspray-filled materials from the present investigation were superior to those of unsaturated polyester polymer concretes and Portland cement concretes. Mechanical testing and finite element analyses of flexure (1 x 1 x 20 in) and beam (2 x 4 x 40 in) specimens were conducted. These structurally-reinforced specimens were tested and analyzed in four-point, third-point flexure to determine their ultimate loads, maximum fiber stresses and mid-span deflections. The experimentally determined load capacities of these specimens were compared to those of equivalent steel-reinforced Portland cement concrete beams computed using reinforced concrete theory. Mechanics of materials beam theory was utilized to predict the ultimate loads and mid-span deflections of the flexure and beam specimens. However, these predictions proved to be severely inadequate. Finite element (fracture propagation

  13. Structural and morphological TEM characterization of GaAs based nanowires

    Energy Technology Data Exchange (ETDEWEB)

    Soda, Marcello


    The question of a structural and morphological characterization of GaAs based nanowires is the research interest of this thesis. For this purpose standard and analytical transmission electron microscopy techniques were employed. New investigation methodologies are introduced in order to obtain a reliable interpretation of the results. The principal motivation on developing a new investigation method is the necessity to relate the results of crystal structure and morphology characterizations to microscopic and NW-specific parameters and not to macroscopic and general growth parameters. This allows a reliable comparison of NW characteristics and enhances the comprehension of their growth mechanism.The analysis of the results on crystal structure investigations, assuming this new perspective, delivers the fundamental finding that the axial growth of Au-assisted GaAs NWs can change in a pseudo Ga-assisted growth due to a non steady-state regime of the Ga accumulation process in the liquid droplet. The attempt to associate the observed crystal structures to one of these two growth modes reveals that zinc blende segments are most probably generated when a pseudo Ga-assisted growth occurs. This experimental evidence is in accordance with investigations developed by Glas et al. and Spirkoska et al. and with the current understanding of the NW growth mechanism and unifies the interpretation of catalytic growth of GaAs NWs. A Mn doped GaAs shell deposited at low temperature on core GaAs NWs is characterized for the first time. The growth is found to be epitaxial and to confer the quality of the core crystal to the shell crystal. As a consequence a high stacking fault density of the core NW limits the temperature of the shell growth due to the formation of clusters. Cross sections of (Ga,Mn)As shells are investigated. Simple kinetic and thermodynamical considerations lead to the conclusion of morphological instability of the low temperature radial growth. Analytical

  14. Structure activity characterization of Bordetella petrii lipid A, from environment to human isolates. (United States)

    Basheer, Soorej M; Bouchez, Valerie; Novikov, Alexey; Augusto, Luis A; Guiso, Nicole; Caroff, Martine


    Bordetella petrii, a facultative anaerobic species, is the only known member of the Bordetella genus with environmental origin. However it was also recently isolated from humans. The structures of the B. petrii lipid A moieties of the endotoxins were characterized here for the first time for an environmental strain and compared to that of human isolates. Characterization was achieved using chemical analyses, gas chromatography-mass spectrometry, and Matrix Assisted Laser Desorption Ionisation mass spectrometry. The analyses revealed that the different lipid A structures contain a common bisphosphorylated β-(1→6)-linked d-glucosamine disaccharide with hydroxytetradecanoic acid in amide as well at the C-3' in ester linkages. Similar to Bordetella pertussis and Bordetella bronchiseptica lipids A, the hydroxytetradecanoic acid at the C-2' position was substituted by tetradecanoic acid. Unlike B. pertussis, the hydroxytetradecanoic acid at the C-2 position was substituted with either 12:0 or 14:0 and/or their 2-OH forms. Depending on the environmental or human origin the structures differed in the length and degree of fatty acid acylation and impacted the IL-6 and TNF-α inflammatory responses tested. In one isolate we showed the presence at the C-3 position of the short-chain 10:0(3-OH), which according to our previous analyses is more characteristic of the human pathogens in the genus like B. pertussis and Bordetella parapertussis. Copyright © 2015 Elsevier B.V. and Société Française de Biochimie et Biologie Moléculaire (SFBBM). All rights reserved.

  15. Remote Characterization of Forest Structure Using 5 and 10m SPOT-5 Satellite Data (United States)

    Wolter, P. T.; Townsend, P. A.; Sturtevant, B. R.


    Comprehensive understanding of forest dynamics at regional or biome scales is linked to our ability to accurately characterize forest ecosystems over increasingly large areas using remote sensing. LIDAR technology, although promising, is currently not yet viable for repeated regional accounting, necessitating the development of methods which take advantage of existing spaceborne assets. As such, our objective is to estimate a comprehensive set of forest structural attributes at a finer spatial grain size (10 m) over a broader area than is currently available. We employ neighborhood statistics (standard deviation, variance, sill variance, and ratios of these metrics at 5 and 10m) calculated from SPOT-5 data and derivatives to estimate and map forest structural characteristics. A partial least squares (PLS) regression approach was used with the local statistics and field data to produce models for pixel-wise estimation and mapping of mean values, respectively, for deciduous and coniferous forest canopy diameter (R2 = 0.82 and 0.93), tree height (R2 = 0.69 and 0.92), height of live crown (R2 = 0.58 and 0.81), canopy closure (R2 = 0.52 and 0.68), bole diameter at breast height (R2 = 0.82 and 0.90), and basal area (R2 = 0.71 and 0.74) for a 3,660 km2 area in northeast Minnesota. This approach for quantifying forest structure is robust in the sense that a detailed forest cover type map is not required at any step in the process. Hence, we show that multi-resolution SPOT-5 data may be used as a practical alternative to LIDAR for regional characterization of forest biophysical parameters.

  16. Biochemical and structural characterization of the trans-enoyl-CoA reductase from Treponema denticola. (United States)

    Bond-Watts, Brooks B; Weeks, Amy M; Chang, Michelle C Y


    The production of fatty acids is an important cellular pathway for both cellular function and the development of engineered pathways for the synthesis of advanced biofuels. Despite the conserved reaction chemistry of various fatty acid synthase systems, the individual isozymes that catalyze these steps are quite diverse in their structural and biochemical features and are important for controlling differences at the cellular level. One of the key steps in the fatty acid elongation cycle is the enoyl-ACP (CoA) reductase function that drives the equilibrium forward toward chain extension. In this work, we report the structural and biochemical characterization of the trans-enoyl-CoA reductase from Treponema denticola (tdTer), which has been utilized for the engineering of synthetic biofuel pathways with an order of magnitude increase in product titers compared to those of pathways constructed with other enoyl-CoA reductase components. The crystal structure of tdTer was determined to 2.00 Å resolution and shows that the Ter enzymes are distinct from members of the FabI, FabK, and FabL families but are highly similar to members of the FabV family. Further biochemical studies show that tdTer uses an ordered bi-bi mechanism initiated by binding of the NADH redox cofactor, which is consistent with the behavior of other enoyl-ACP (CoA) reductases. Mutagenesis of the substrate binding loop, characterization of enzyme activity with respect to crotonyl-CoA, hexenoyl-CoA, and dodecenoyl-CoA substrates, and product inhibition by lauroyl-CoA suggest that this region is important for controlling chain length specificity, with the major portal playing a more important role for longer chain length substrates.

  17. Silver sulfadoxinate: Synthesis, structural and spectroscopic characterizations, and preliminary antibacterial assays in vitro (United States)

    Zanvettor, Nina T.; Abbehausen, Camilla; Lustri, Wilton R.; Cuin, Alexandre; Masciocchi, Norberto; Corbi, Pedro P.


    The sulfa drug sulfadoxine (SFX) reacted with Ag+ ions in aqueous solution, affording a new silver(I) complex (AgSFX), which was fully characterized by chemical, spectroscopic and structural methods. Elemental, ESI-TOF mass spectrometric and thermal analyses of AgSFX suggested a [Ag(C12H13N4O2S)] empirical formula. Infrared spectroscopic measurements indicated ligand coordination to Ag(I) through the nitrogen atoms of the (deprotonated) sulfonamide group and by the pyrimidine ring, as well as through oxygen atom(s) of the sulfonamide group. These hypotheses were corroborated by 13C and 15N SS-NMR spectroscopy and by an unconventional structural characterization based on X-ray powder diffraction data. The latter showed that AgSFX crystallizes as centrosymmetric dimers with a strong Ag⋯Ag interaction of 2.7435(6) Å, induced by the presence of exo-bidentate N,N‧ bridging ligands and the formation of an eight-membered ring of [AgNCN]2 sequence, nearly planar. Participation of oxygen atoms of the sulfonamide residues generates in the crystal a 1D coordination polymer, likely responsible for its very limited solubility in all common solvents. Besides the analytical, spectroscopic and structural description, the antibacterial properties of AgSFX were assayed using disc diffusion methods against Escherichia coli and Pseudomonas aeruginosa (Gram-negative), and Staphylococcus aureus (Gram-positive) bacterial strains. The AgSFX complex showed to be active against Gram-positive and Gram-negative bacterial strains, being comparable to the activities of silver sulfadiazine.

  18. Characterizing spatial structure of sediment E. coli populations to inform sampling design. (United States)

    Piorkowski, Gregory S; Jamieson, Rob C; Hansen, Lisbeth Truelstrup; Bezanson, Greg S; Yost, Chris K


    Escherichia coli can persist in streambed sediments and influence water quality monitoring programs through their resuspension into overlying waters. This study examined the spatial patterns in E. coli concentration and population structure within streambed morphological features during baseflow and following stormflow to inform sampling strategies for representative characterization of E. coli populations within a stream reach. E. coli concentrations in bed sediments were significantly different (p = 0.002) among monitoring sites during baseflow, and significant interactive effects (p = 0.002) occurred among monitoring sites and morphological features following stormflow. Least absolute shrinkage and selection operator (LASSO) regression revealed that water velocity and effective particle size (D 10) explained E. coli concentration during baseflow, whereas sediment organic carbon, water velocity and median particle diameter (D 50) were important explanatory variables following stormflow. Principle Coordinate Analysis illustrated the site-scale differences in sediment E. coli populations between disconnected stream segments. Also, E. coli populations were similar among depositional features within a reach, but differed in relation to high velocity features (e.g., riffles). Canonical correspondence analysis resolved that E. coli population structure was primarily explained by spatial (26.9–31.7 %) over environmental variables (9.2–13.1 %). Spatial autocorrelation existed among monitoring sites and morphological features for both sampling events, and gradients in mean particle diameter and water velocity influenced E. coli population structure for the baseflow and stormflow sampling events, respectively. Representative characterization of streambed E. coli requires sampling of depositional and high velocity environments to accommodate strain selectivity among these features owing to sediment and water velocity heterogeneity.

  19. Synchrotron radiation based multi-scale structural characterization of CoPt{sub 3} colloidal nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Zargham, Ardalan


    Bimetallic CoPt{sub 3} nanoparticles represent a category of colloidal nanoparticles with high application potentials in, e.g., heterogeneous catalysis, sensor technology, and magnetic storage media. Deposition of this system on functionalized supports delivers opportunities for controlled immobilization of the nanoparticles. In this work, self-assembled monolayers (SAMs) of n-alkanethiol molecules served as functionalizing material for the Au covered Si substrates. Deposition of the ligand-terminated nanoparticles took place by means of spin and dip coating and has been optimized for each of the mentioned methods so that monolayers of nanoparticles on supports were fabricated with a well-controlled coverage The morphology of the nanoparticle film arranged is addressed by grazing-incidence small angle x-ray scattering (GISAXS). This together with x-ray standing waves in total external reflection (TER-XSW) enables a 3D structural characterization of such nanoparticle films, so that the mean particle size, mean distance of the arranged nanoparticle films to the substrate, as well as the mean particle-particle distance in lateral direction have been determined. TER-XSW, being an element-specific position-sensitive method, also reveals the elemental distribution of the particles which complementary provides a fundamental understanding of their internal structure. The CoPt{sub 3} nanoparticles investigated here exhibit a core-shell-like structure with cores of CoPt{sub 3} and shells mainly comprise Co. The results regarding the internal structure of the nanoparticles were then verified by extended X-ray absorption fine structure (EXAFS) measurements. (orig.)

  20. Structural characterization of terrestrial microbial Mn oxides from Pinal Creek, AZ

    Energy Technology Data Exchange (ETDEWEB)

    Bargar, John; Fuller, Christopher; Marcus, Matthew A.; Brearley, Adrian J.; Perez De la Rosa, M.; Webb, Samuel M.; Caldwell, Wendel A.


    The microbial catalysis of Mn(II) oxidation is believed to be a dominant source of abundant sorption- and redox-active Mn oxides in marine, freshwater, and subsurface aquatic environments. In spite of their importance, environmental oxides of known biogenic origin have generally not been characterized in detail from a structural perspective. Hyporheic zone Mn oxide grain coatings at Pinal Creek, Arizona, a metals-contaminated stream, have been identified as being dominantly microbial in origin and are well studied from bulk chemistry and contaminant hydrology perspectives. This site thus presents an excellent opportunity to study the structures of terrestrial microbial Mn oxides in detail. XRD and EXAFS measurements performed in this study indicate that the hydrated Pinal Creek Mn oxide grain coatings are layer-type Mn oxides with dominantly hexagonal or pseudo-hexagonal layer symmetry. XRD and TEM measurements suggest the oxides to be nanoparticulate plates with average dimensions on the order of 11 nm thick x 35 nm diameter, but with individual particles exhibiting thickness as small as a single layer and sheets as wide as 500 nm. The hydrated oxides exhibit a 10-A basal-plane spacing and turbostratic disorder. EXAFS analyses suggest the oxides contain layer Mn(IV) site vacancy defects, and layer Mn(III) is inferred to be present, as deduced from Jahn-Teller distortion of the local structure. The physical geometry and structural details of the coatings suggest formation within microbial biofilms. The biogenic Mnoxides are stable with respect to transformation into thermodynamically more stable phases over a time scale of at least 5 months. The nanoparticulate layered structural motif, also observed in pure culture laboratory studies, appears to be characteristic of biogenic Mn oxides and may explain the common occurrence of this mineral habit in soils and sediments.

  1. Structural characterization of a therapeutic anti-methamphetamine antibody fragment: oligomerization and binding of active metabolites.

    Directory of Open Access Journals (Sweden)

    Eric C Peterson

    Full Text Available Vaccines and monoclonal antibodies (mAb for treatment of (+-methamphetamine (METH abuse are in late stage preclinical and early clinical trial phases, respectively. These immunotherapies work as pharmacokinetic antagonists, sequestering METH and its metabolites away from sites of action in the brain and reduce the rewarding and toxic effects of the drug. A key aspect of these immunotherapy strategies is the understanding of the subtle molecular interactions important for generating antibodies with high affinity and specificity for METH. We previously determined crystal structures of a high affinity anti-METH therapeutic single chain antibody fragment (scFv6H4, K(D = 10 nM in complex with METH and the (+ stereoisomer of 3,4-methylenedioxymethamphetamine (MDMA, or "ecstasy". Here we report the crystal structure of scFv6H4 in homo-trimeric unbound (apo form (2.60Å, as well as monomeric forms in complex with two active metabolites; (+-amphetamine (AMP, 2.38Å and (+-4-hydroxy methamphetamine (p-OH-METH, 2.33Å. The apo structure forms a trimer in the crystal lattice and it results in the formation of an intermolecular composite beta-sheet with a three-fold symmetry. We were also able to structurally characterize the coordination of the His-tags with Ni(2+. Two of the histidine residues of each C-terminal His-tag interact with Ni(2+ in an octahedral geometry. In the apo state the CDR loops of scFv6H4 form an open conformation of the binding pocket. Upon ligand binding, the CDR loops adopt a closed formation, encasing the drug almost completely. The structural information reported here elucidates key molecular interactions important in anti-methamphetamine abuse immunotherapy.

  2. A novel embeddable spherical smart aggregate for structural health monitoring: part I. Fabrication and electrical characterization (United States)

    Kong, Qingzhao; Fan, Shuli; Bai, Xiaolong; Mo, Y. L.; Song, Gangbing


    Recently developed piezoceramic-based transducers, known as smart aggregates (SAs), have shown their applicability and versatility in various applications of structural health monitoring (SHM). The lead zirconate titanate (PZT) patches embedded inside SAs have different modes that are more suitable for generating or receiving different types of stress waves (e.g. P and S waves, each of which has a unique role in SHM). However, due to the geometry of the 2D PZT patch, the embedded SA can only generate or receive the stress wave in a single direction and thus greatly limits its applications. This paper is the first of a series of two companion papers that introduces the authors’ latest work in developing a novel, embeddable spherical smart aggregate (SSA) for the health monitoring of concrete structures. In addition to the 1D guided wave produced by SA, the SSA embedded in concrete structures can generate or receive omni-directional stress waves that can significantly improve the detection aperture and provide additional functionalities in SHM. In the first paper (Part I), the detailed fabrication procedures with the help of 3D printing technology and electrical characterization of the proposed SSA is presented. The natural frequencies of the SSA were experimentally obtained and further compared with the numerical results. In addition, the influence of the components’ thickness (spherical piezoceramic shell and epoxy) and outer radius (spherical piezoceramic shell and protection concrete) on the natural frequencies of the SSA were analytically studied. The results will help elucidate the key parameters that determine the natural frequencies of the SSA. The natural frequencies of the SSA can thus be designed for suitability in the damage detection of concrete structures. In the second paper (Part II), further numerical and experimental verifications on the performance of the proposed SSA in concrete structures will be discussed.

  3. Structural characterization of cellulosic materials using x-ray and neutron scattering

    Energy Technology Data Exchange (ETDEWEB)

    Penttila, P.


    Cellulosic biomass can be used as a feedstock for sustainable production of biofuels and various other products. A complete utilization of the raw material requires understanding on its structural aspects and their role in the various processes. In this thesis, x-ray and neutron scattering methods were applied to study the structure of various cellulosic materials and how they are affected in different processes. The obtained results were reviewed in the context of a model for the cellulose nanostructure. The dimensions of cellulose crystallites and the crystallinity were determined with wide-angle x-ray scattering (WAXS), whereas the nanoscale fibrillar structure of cellulose was characterized with small-angle x-ray and neutron scattering (SAXS and SANS). The properties determined with the small-angle scattering methods included specific surface areas and distances characteristic of the packing of cellulose microfibrils. Also other physical characterization methods, such as x-ray microtomography, infrared spectroscopy, and solid-state NMR were utilized in this work. In the analysis of the results, a comprehensive understanding of the structural changes throughout a range of length scales was aimed at. Pretreatment of birch sawdust by pressurized hot water extraction was observed to increase the crystal width of cellulose, as determined with WAXS, even though the cellulose crystallinity was slightly decreased. A denser packing of microfibrils caused by the removal of hemicelluloses and lignin in the extraction was evidenced by SAXS. This resulted in the opening of new pores between the microfibril bundles and an increase of the specific surface area. Enzymatic hydrolysis of microcrystalline cellulose (MCC) did not lead to differences in the average crystallinity or crystal size of the hydrolysis residues, which was explained to be caused by limitations due to the large size of the enzymes as compared to the pores inside the fibril aggregates. The SAXS intensities

  4. Structural characterization and comparison of three acyl-carrier-protein synthases from pathogenic bacteria

    Energy Technology Data Exchange (ETDEWEB)

    Halavaty, Andrei S. [Center for Structural Genomics of Infectious Diseases, (United States); Northwestern University, Chicago, IL 60611 (United States); Kim, Youngchang [Center for Structural Genomics of Infectious Diseases, (United States); Argonne National Laboratory, Argonne, IL 60439 (United States); University of Chicago, Chicago, IL 60637 (United States); Minasov, George; Shuvalova, Ludmilla; Dubrovska, Ievgeniia; Winsor, James [Center for Structural Genomics of Infectious Diseases, (United States); Northwestern University, Chicago, IL 60611 (United States); Zhou, Min [Center for Structural Genomics of Infectious Diseases, (United States); Argonne National Laboratory, Argonne, IL 60439 (United States); University of Chicago, Chicago, IL 60637 (United States); Onopriyenko, Olena; Skarina, Tatiana [Center for Structural Genomics of Infectious Diseases, (United States); University of Toronto, Toronto, Ontario M5G 1L6 (Canada); Papazisi, Leka; Kwon, Keehwan; Peterson, Scott N. [Center for Structural Genomics of Infectious Diseases, (United States); J. Craig Venter Institute, Rockville, MD 20850 (United States); Joachimiak, Andrzej [Center for Structural Genomics of Infectious Diseases, (United States); Argonne National Laboratory, Argonne, IL 60439 (United States); University of Chicago, Chicago, IL 60637 (United States); Savchenko, Alexei [Center for Structural Genomics of Infectious Diseases, (United States); University of Toronto, Toronto, Ontario M5G 1L6 (Canada); Anderson, Wayne F., E-mail: [Center for Structural Genomics of Infectious Diseases, (United States); Northwestern University, Chicago, IL 60611 (United States)


    The structural characterization of acyl-carrier-protein synthase (AcpS) from three different pathogenic microorganisms is reported. One interesting finding of the present work is a crystal artifact related to the activity of the enzyme, which fortuitously represents an opportunity for a strategy to design a potential inhibitor of a pathogenic AcpS. Some bacterial type II fatty-acid synthesis (FAS II) enzymes have been shown to be important candidates for drug discovery. The scientific and medical quest for new FAS II protein targets continues to stimulate research in this field. One of the possible additional candidates is the acyl-carrier-protein synthase (AcpS) enzyme. Its holo form post-translationally modifies the apo form of an acyl carrier protein (ACP), which assures the constant delivery of thioester intermediates to the discrete enzymes of FAS II. At the Center for Structural Genomics of Infectious Diseases (CSGID), AcpSs from Staphylococcus aureus (AcpS{sub SA}), Vibrio cholerae (AcpS{sub VC}) and Bacillus anthracis (AcpS{sub BA}) have been structurally characterized in their apo, holo and product-bound forms, respectively. The structure of AcpS{sub BA} is emphasized because of the two 3′, 5′-adenosine diphosphate (3′, 5′-ADP) product molecules that are found in each of the three coenzyme A (CoA) binding sites of the trimeric protein. One 3′, 5′-ADP is bound as the 3′, 5′-ADP part of CoA in the known structures of the CoA–AcpS and 3′, 5′-ADP–AcpS binary complexes. The position of the second 3′, 5′-ADP has never been described before. It is in close proximity to the first 3′, 5′-ADP and the ACP-binding site. The coordination of two ADPs in AcpS{sub BA} may possibly be exploited for the design of AcpS inhibitors that can block binding of both CoA and ACP.

  5. Active and passive infrared thermography applied to the detection and characterization of hidden defects in structure (United States)

    Dumoulin, Jean


    Infrared thermography for Non Destructive Testing (NDT) has encountered a wide spreading this last 2 decades, in particular thanks to emergence on the market of low cost uncooled infrared camera. So, infrared thermography is not anymore a measurement technique limited to laboratory application. It has been more and more involved in civil engineering and cultural heritage applications, but also in many other domains, as indicated by numerous papers in the literature. Nevertheless, laboratory, measurements are done as much as possible in quite ideal conditions (good atmosphere conditions, known properties of materials, etc.), while measurement on real site requires to consider the influence of not controlled environmental parameters and additional unknown thermal properties. So, dedicated protocol and additional sensors are required for measurement data correction. Furthermore, thermal excitation is required to enhance the signature of defects in materials. Post-processing of data requires to take into account the protocol used for the thermal excitation and sometimes its nature to avoid false detection. This analysis step is based on signal and image processing tool and allows to carry out the detection. Characterization of anomalies detected at the previous step can be done by additional signal processing in particular for manufactured objects. The use of thermal modelling and inverse method allows to determine properties of the defective area. The present paper will first address a review of some protocols currently in use for field measurement with passive and/or active infrared measurements. Illustrations in various experiments carried out on civil engineering structure will be shown and discussed. In a second part, different post-processing approaches will be presented and discussed. In particular, a review of the most standard processing methods like Fast Fourier Analysis, Principal Components Analysis, Polynomial Decomposition, defect characterization using

  6. Phenylenevinylene oligomers by Mizoroki-Heck cross coupling reaction. Structural and optoelectronic characterization (United States)

    Estrada, Sandra E.; Ochoa-Puentes, Cristian; Sierra, Cesar A.


    In order to study the effect of the molecular structure on the optical properties of totally trans-trans phenylenevinylene oligomers (OPVs), sixteen 1,4-distyrylbenzene derivatives (1a-i and 2a-g) functionalized with different electron-donating (ED) and electron-withdrawing (EW) groups were synthesized by the Mizoroki-Heck cross coupling reaction in moderate to good yields (40-95%). The implemented methodology, with a small modification previously reported by our group, allows obtaining the desired vinyl configuration as well as one novel OPV compound (1h). After structural characterization by several techniques (e.g. FTIR, 1H, 13C and Solid-State NMR), particular emphasis was placed upon the investigation of their optical properties by UV-vis and fluorescence spectroscopies. The results showed that, with only one exception, the ED and EW groups at the ends of OPV systems lead to a bathochromic shift. This effect is intensified with the introduction of methoxy groups on the central ring. Consistent with these, the HOMO-LUMO gaps (ΔE) decreases as the strength of ED and EW substituents increases. The ED and EW substituents also lead to a decrease in the Φf values. This contribution in the area of organic electronics can be used as a reference to better select the most appropriate technological application for each OPV and this can be extrapolated to their respective structurally analogous segmented polymer.

  7. Novel low-dose imaging technique for characterizing atomic structures through scanning transmission electron microscope (United States)

    Su, Chia-Ping; Syu, Wei-Jhe; Hsiao, Chien-Nan; Lai, Ping-Shan; Chen, Chien-Chun


    To investigate dislocations or heterostructures across interfaces is now of great interest to condensed matter and materials scientists. With the advances in aberration-corrected electron optics, the scanning transmission electron microscope has demonstrated its excellent capability of characterizing atomic structures within nanomaterials, and well-resolved atomic-resolution images can be obtained through long-exposure data acquisition. However, the sample drifting, carbon contamination, and radiation damage hinder further analysis, such as deriving three-dimensional (3D) structures from a series of images. In this study, a method for obtaining atomic-resolution images with significantly reduced exposure time was developed, using which an original high-resolution image with approximately one tenth the electron dose can be obtained by combining a fast-scan high-magnification image and a slow-scan low-magnification image. The feasibility of obtaining 3D atomic structures using the proposed approach was demonstrated through multislice simulation. Finally, the feasibility and accuracy of image restoration were experimentally verified. This general method cannot only apply to electron microscopy but also benefit to image radiation-sensitive materials using various light sources.

  8. Recent advances in endophytic exopolysaccharides: Production, structural characterization, physiological role and biological activity. (United States)

    Liu, Jun; Wang, Xingchi; Pu, Huimin; Liu, Shuang; Kan, Juan; Jin, Changhai


    Endophytes are microorganisms that colonize living, internal tissues of plants without causing any immediate, overt negative effects. In recent years, both endophytic bacteria and fungi have been demonstrated to be excellent exopolysaccharides (EPS) producers. This review focuses on the recent advances in EPS produced by endophytes, including its production, isolation and purification, structural characterization, physiological role and biological activity. In general, EPS production is influenced by media components and cultivation conditions. The structures of purified EPS range from linear homopolysaccharides to highly branched heteropolysaccharides. These structurally novel EPS not only play important roles in plant-endophyte interactions; but also exhibit several biological functions, such as antioxidant, antitumor, anti-inflammatory, anti-allergic and prebiotic activities. In order to utilize endophytic EPS on an industrial scale, both yield and productivity enhancement strategies are required at several levels. Besides, the exact mechanisms on the physiological roles and biological functions of EPS should be elucidated in future. Copyright © 2016 Elsevier Ltd. All rights reserved.

  9. Structural Characterization of Inhibitors with Selectivity against Members of a Homologous Enzyme Family

    Energy Technology Data Exchange (ETDEWEB)

    Pavlovsky, Alexander G.; Liu, Xuying; Faehnle, Christopher R.; Potente, Nina; Viola, Ronald E. (Toledo)


    The aspartate biosynthetic pathway provides essential metabolites for many important biological functions, including the production of four essential amino acids. As this critical pathway is only present in plants and microbes, any disruptions will be fatal to these organisms. An early pathway enzyme, L-aspartate-{beta}-semialdehyde dehydrogenase, produces a key intermediate at the first branch point of this pathway. Developing potent and selective inhibitors against several orthologs in the L-aspartate-{beta}-semialdehyde dehydrogenase family can serve as lead compounds for antibiotic development. Kinetic studies of two small molecule fragment libraries have identified inhibitors that show good selectivity against L-aspartate-{beta}-semialdehyde dehydrogenases from two different bacterial species, Streptococcus pneumoniae and Vibrio cholerae, despite the presence of an identical constellation of active site amino acids in this homologous enzyme family. Structural characterization of enzyme-inhibitor complexes have elucidated different modes of binding between these structurally related enzymes. This information provides the basis for a structure-guided approach to the development of more potent and more selective inhibitors.

  10. Structural and Immunological Activity Characterization of a Polysaccharide Isolated from Meretrix meretrix Linnaeus. (United States)

    Li, Li; Li, Heng; Qian, Jianying; He, Yongfeng; Zheng, Jialin; Lu, Zhenming; Xu, Zhenghong; Shi, Jinsong


    Polysaccharides from marine clams perform various biological activities, whereas information on structure is scarce. Here, a water-soluble polysaccharide MMPX-B2 was isolated from Meretrix meretrix Linnaeus. The proposed structure was deduced through characterization and its immunological activity was investigated. MMPX-B2 consisted of d-glucose and d-galctose residues at a molar ratio of 3.51:1.00. The average molecular weight of MMPX-B2 was 510 kDa. This polysaccharide possessed a main chain of (1→4)-linked-α-d-glucopyranosyl residues, partially substituted at the C-6 position by a few terminal β-d-galactose residues or branched chains consisting of (1→3)-linked β-d-galactose residues. Preliminary immunological tests in vitro showed that MMPX-B2 could stimulate the murine macrophages to release various cytokines, and the structure-activity relationship was then established. The present study demonstrated the potential immunological activity of MMPX-B2, and provided references for studying the active ingredients in M. meretrix.

  11. Structure and Mechanical Characterization of DNA i-Motif Nanowires by Molecular Dynamics Simulation (United States)

    Singh, Raghvendra Pratap; Blossey, Ralf; Cleri, Fabrizio


    We studied the structure and mechanical properties of DNA i-motif nanowires by means of molecular dynamics computer simulations. We built up to 230 nm-long nanowires, based on a repeated TC5 sequence from crystallographic data, fully relaxed and equilibrated in water. The unusual C⋅C+ stacked structure, formed by four ssDNA strands arranged in an intercalated tetramer, is here fully characterized both statically and dynamically. By applying stretching, compression, and bending deformations with the steered molecular dynamics and umbrella sampling methods, we extract the apparent Young’s and bending moduli of the nanowire, as well as estimates for the tensile strength and persistence length. According to our results, the i-motif nanowire shares similarities with structural proteins, as far as its tensile stiffness, but is closer to nucleic acids and flexible proteins, as far as its bending rigidity is concerned. Furthermore, thanks to its very thin cross section, the apparent tensile toughness is close to that of a metal. Besides their yet to be clarified biological significance, i-motif nanowires may qualify as interesting candidates for nanotechnology templates, due to such outstanding mechanical properties. PMID:24359754

  12. Stable anilinyl radicals coordinated to nickel: X-ray crystal structure and characterization. (United States)

    Kochem, Amélie; Gellon, Gisèle; Leconte, Nicolas; Baptiste, Benoit; Philouze, Christian; Jarjayes, Olivier; Orio, Maylis; Thomas, Fabrice


    Two anilinosalen and a mixed phenol-anilinosalen ligands involving sterically hindered anilines moieties were synthesized. Their nickel(II) complexes 1, 2, and 3 were prepared and characterized. They could be readily one-electron oxidized (E(1/2)=-0.30, -0.26 and 0.10 V vs. Fc(+)/Fc, respectively) into anilinyl radicals species [1](+), [2](+), and [3](+), respectively. The radical complexes are extremely stable and were isolated as single crystals. X-ray crystallographic structures reveal that the changes in bond length resulting from oxidation do not exceed 0.02 Å within the ligand framework in the symmetrical [1](+) and [2](+). No quinoid bond pattern was present. In contrast, larger structural rearrangements were evidenced for the unsymmetrical [3](+), with shortening of one C(ortho)-C(meta) bond. Radical species [1](+) and [2](+) exhibit a strong absorption band at around 6000 cm(-1) (class III mixed valence compounds). This band is significantly less intense than [3](+), consistent with a rather localized anilinyl radical character, and thus a classification of this species as class II mixed-valence compound. Magnetic and electronic properties, as well as structural parameters, have been computed by DFT methods. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Crystal structure, spectroscopic characterization and antibacterial activities of a silver complex with sulfameter (United States)

    Nakahata, Douglas H.; Lustri, Wilton R.; Cuin, Alexandre; Corbi, Pedro P.


    A silver complex with the sulfonamide sulfameter, also known as sulfamethoxydiazine (SMTR), was prepared and characterized. Chemical analyses were consistent with the [Ag(C11H11N4O3S)] composition (AgSMTR), while conductivity measurements in DMSO indicated a non-electrolyte behavior of the complex in this solvent. High-resolution ESI(+)-QTOF mass spectrometric experiments revealed the presence of the [Ag(C11H11N4O3S)+H]+ and [Ag2(C11H11N4O3S)2+H]+ species in solution. Infrared and NMR spectroscopies indicated coordination of the ligand to the metal by the nitrogen atoms of the sulfonamide group and of the pyrimidine ring. The structure of AgSMTR was solved by powder X-ray diffraction technique using the Rietveld method. The solved structure confirms the formation of a dimer, where each silver ion is coordinated by one of the nitrogen atoms of the pyrimidine ring, the nitrogen of the sulfonamide group and by an oxygen atom from the sulfonyl group. An argentophilic interaction of 2.901(1) Å is present in this dimeric structure. The AgSMTR complex was assayed over Gram-positive (Staphylococcus aureus) and Gram-negative (Pseudomonas aeruginosa and Escherichia coli) bacterial strains, and it was found that the compound is 8 times more active over the Gram-negative bacteria in DMSO solution, with MIC values in the micromolar range.

  14. Structural characterization of amphiphilic homopolymer micelles using light scattering, SANS, and cryo-TEM. (United States)

    Patterson, Joseph P; Kelley, Elizabeth G; Murphy, Ryan P; Moughton, Adam O; Robin, Mathew; Lu, Annhelen; Colombani, Olivier; Chassenieux, Christophe; Cheung, David; Sullivan, Millicent O; Epps, Thomas H; O'Reilly, Rachel K


    We report the aqueous solution self-assembly of a series of poly(N-isopropylacrylamide) (PNIPAM) polymers end-functionalized with a hydrophobic sulfur-carbon-sulfur (SCS) pincer ligand. Although the hydrophobic ligand accounted for structural details were investigated using light scattering, cryogenic transmission electron microscopy (cryo-TEM), and small angle neutron scattering (SANS). Radial density profiles extracted from the cryo-TEM micrographs suggested that the PNIPAM chains formed a diffuse corona with a radially decreasing corona density profile and provided valuable a priori information about the micelle structure for SANS data modeling. SANS analysis indicated a similar profile in which the corona surrounded a small hydrophobic core containing the pincer ligand. The similarity between the SANS and cryo-TEM results demonstrated that detailed information about the micelle density profile can be obtained directly from cryo-TEM and highlighted the complementary use of scattering and cryo-TEM in the structural characterization of solution-assemblies, such as the SCS pincer-functionalized homopolymers described here.

  15. Particle Size and Pore Structure Characterization of Silver Nanoparticles Prepared by Confined Arc Plasma

    Directory of Open Access Journals (Sweden)

    Mingru Zhou


    Full Text Available In the protecting inert gas, silver nanoparticles were successfully prepared by confined arc plasma method. The particle size, microstructure, and morphology of the particles by this process were characterized via X-ray powder diffraction (XRD, transmission electron microscopy (TEM and the corresponding selected area electron diffraction (SAED. The N2 absorption-desorption isotherms of the samples were measured by using the static volumetric absorption analyzer, the pore structure of the sample was calculated by Barrett-Joyner-Halenda (BJH academic model, and the specific surface area was calculated from Brunauer-Emmett-Teller (BET adsorption equation. The experiment results indicate that the crystal structure of the samples is face-centered cubic (FCC structure the same as the bulk materials, the particle size distribution ranging from 5 to 65 nm, with an average particle size about 26 nm obtained by TEM and confirmed by XRD and BET results. The specific surface area is 23.81 m2/g, pore volumes are 0.09 cm3/g, and average pore diameter is 18.7 nm.

  16. Structural and activity characterization of human PHPT1 after oxidative modification. (United States)

    Martin, Daniel R; Dutta, Priyanka; Mahajan, Shikha; Varma, Sameer; Stevens, Stanley M


    Phosphohistidine phosphatase 1 (PHPT1), the only known phosphohistidine phosphatase in mammals, regulates phosphohistidine levels of several proteins including those involved in signaling, lipid metabolism, and potassium ion transport. While the high-resolution structure of human PHPT1 (hPHPT1) is available and residues important for substrate binding and catalytic activity have been reported, little is known about post-translational modifications that modulate hPHPT1 activity. Here we characterize the structural and functional impact of hPHPT1 oxidation upon exposure to a reactive oxygen species, hydrogen peroxide (H2O2). Specifically, liquid chromatography-tandem mass spectrometry was used to quantify site-specific oxidation of redox-sensitive residues of hPHPT1. Results from this study revealed that H2O2 exposure induces selective oxidation of hPHPT1 at Met95, a residue within the substrate binding region. Explicit solvent molecular dynamics simulations, however, predict only a minor effect of Met95 oxidation in the structure and dynamics of the apo-state of the hPHPT1 catalytic site, suggesting that if Met95 oxidation alters hPHPT1 activity, then it will do so by altering the stability of an intermediate state. Employing a novel mass spectrometry-based assay, we determined that H2O2-induced oxidation does not impact hPHPT1 function negatively; a result contrary to the common conception that protein oxidation is typically a loss-of-function modification.

  17. New approach for extraction of cellulose from tucumã's endocarp and its structural characterization (United States)

    Manzato, L.; Rabelo, L. C. A.; de Souza, S. M.; da Silva, C. G.; Sanches, E. A.; Rabelo, D.; Mariuba, L. A. M.; Simonsen, J.


    The recycling of plant wasted materials into useful products represents a green alternative to prevent environmental problems. Tucumã palm fruit (Astrocaryum aculeatum Meyer) is widely used in Amazon region for food and crafts. Due to the large amount of wasted Tucumã's endocarp, this work proposes a new approach for extraction of cellulose and its structural characterization. X-ray Diffraction (XRD), Rietveld Refinement, Scanning Electron Microscopy (SEM), Infrared-transform Fourier Spectroscopy (FTIR) and Thermal Analysis (TG/DSC) have been used for characterization of the extracted cellulose. XRD patterns of the in natura tucumã's endocarp has showed a natural crystalline content embedded in a non-crystalline matrix. Nanocrystals of cellulose have been observed in the XRD pattern of the extracted cellulose, showing a good agreement with type II. Rietveld refinement allowed the cell parameters obtainment (a = 8.43(1) Å, b = 9.50(1) Å, c = 9.39(3) Å and γ = 118.43(4)°). Apparent average crystallite size and microstrain were, respectively, 20.0 Å and 0.1%. Two different methods were applied for estimative of crystallinity percentage. In the first method the height ratio between the intensity of the crystalline peak and the total intensity after the subtraction of the non-crystalline content was applied, leading to 48.5%. The second approach was performed using the amorphous area and the total area of the (1 1 0) peak from the experimental diffractogram, leading to 31.5%. The difference in crystallinity percentage concerning these two used approaches may be explained due to the first method does not consider the broad peaks resulted from nanocrystals diffraction. FTIR spectroscopy has evidenced a cellulose type II structure. SEM images showed micrometric sized fibers with ranged thicknesses. However, a new morphology of spherical nanostructures was observed on the type II matrix fibers. Thermal analysis suggests that the extracted cellulose have low thermal

  18. Characterization and modeling of ionic polymeric smart materials as artificial muscles and robotic swimming structures (United States)

    Mojarrad, Mehran


    In this dissertation document, a thorough review and investigation of works in connection with the ionic polymeric gels as artificial muscles and electrically controllable polymeric network structures were performed. Where possible, comparisons were made with biological muscles and applications in marine propulsion using such polymeric materials were investigated. Furthermore, methods of fabrication of several chemically active ionic polymeric gel muscles such as PolyAcryloNitrile (PAN), Poly(2-Acrylamido-2-Methyl-1-PropaneSulfonic) acid (PAMPS), and PolyAcrylic-acid-bis-AcrylaMide (PAAM) as well as a new class of electrically active composite muscle such as Ion-Exchange-Metal-Composites (IEMC) or Ionic Polymer Metal Composites (IPMC) materials are introduced and investigated that resulted in two US patents regarding their fabrication and application capabilities as actuators and sensors. In this research, various forms of the IPMC fabrication were explored and reported. In addition, characterization of PAN muscles, bundling and encapsulation were investigated. Conversion of chemical to electrical artificial muscles were also investigated using chemical plating techniques as well as physical vapor deposition methods of the pH-activated muscles like PAN fibers. Experimental methods were devised to characterize contraction, expansion, and bending of various actuators using isometric, isoionic, and isotonic characterization methods. Several apparatuses for modeling and testing of the various artificial muscles were built to show the viability of the application of both chemoactive and electroactive muscles. Furthermore PAN fiber muscles in different configurations such as spring-loaded fiber bundles, biceps, triceps, ribbon type muscles, and segmented fiber bundles were fabricated to make a variety of actuators. Additionally, swimming robotic structures and associated hardware were built to incorporate IPMC as biomimetic propulsion fin actuators. In addition, various

  19. Wafer scale imprint uniformity evaluated by LSPR spectroscopy: a high volume characterization method for nanometer scale structures

    DEFF Research Database (Denmark)

    Jeppesen, Claus; Lindstedt, Daniel Nilsson; Vig, Asger Laurberg


    numerical simulations of imprinted structures characterized by atomic force microscopy. There is a fair agreement between the two methods and the simulations enable the translation of optical spectra to critical dimensions of the physical structures, a concept known from scatterometry. The results...

  20. Object-based semi-automatic approach for forest structure characterization using lidar data in heterogeneous Pinus sylvestris stands (United States)

    C. Pascual; A. Garcia-Abril; L.G. Garcia-Montero; S. Martin-Fernandez; W.B. Cohen


    In this paper, we present a two-stage approach for characterizing the structure of Pinus sylvestris L. stands in forests of central Spain. The first stage was to delimit forest stands using eCognition and a digital canopy height model (DCHM) derived from lidar data. The polygons were then clustered into forest structure types based on the DCHM data...

  1. Structural Characterization of 1,1,3,3-Tetramethylguanidinium Chloride Ionic Liquid by Reversible SO2 Gas Absorption

    DEFF Research Database (Denmark)

    Berg, Rolf W.; Harris, Pernille; Riisager, Anders


    A unique new ionic liquid−gas adduct solid state compound formed between 1,1,3,3-tetramethylguanidinium chloride ([tmgH]Cl) and sulfur dioxide has been characterized by X-ray diffraction and Raman spectroscopy. The structure contains SO2 molecules of near normal structure kept at their positions...

  2. Using measurable dosimetric quantities to characterize the inter-structural tradeoff in inverse planning (United States)

    Liu, Hongcheng; Dong, Peng; Xing, Lei


    Traditional inverse planning relies on the use of weighting factors to balance the conflicting requirements of different structures. Manual trial-and-error determination of weighting factors has long been recognized as a time-consuming part of treatment planning. The purpose of this work is to develop an inverse planning framework that parameterizes the dosimetric tradeoff among the structures with physically meaningful quantities to simplify the search for clinically sensible plans. In this formalism, instead of using weighting factors, the permissible variation range of the prescription dose or dose volume histogram (DVH) of the involved structures are used to characterize the ‘importance’ of the structures. The inverse planning is then formulated into a convex feasibility problem, called the dosimetric variation-controlled model (DVCM), whose goal is to generate plans with dosimetric or DVH variations of the structures consistent with the pre-specified values. For simplicity, the dosimetric variation range for a structure is extracted from a library of previous cases which possess similar anatomy and prescription. A two-phase procedure (TPP) is designed to solve the model. The first phase identifies a physically feasible plan to satisfy the prescribed dosimetric variation, and the second phase automatically improves the plan in case there is room for further improvement. The proposed technique is applied to plan two prostate cases and two head-and-neck cases and the results are compared with those obtained using a conventional CVaR approach and with a moment-based optimization scheme. Our results show that the strategy is able to generate clinically sensible plans with little trial and error. In all cases, the TPP generates a very competitive plan as compared to those obtained using the alternative approaches. Particularly, in the planning of one of the head-and-neck cases, the TPP leads to a non-trivial improvement in the resultant dose distribution

  3. Sizing Single Cantilever Beam Specimens for Characterizing Facesheet/Core Peel Debonding in Sandwich Structure (United States)

    Ratcliffe, James G.


    This paper details part of an effort focused on the development of a standardized facesheet/core peel debonding test procedure. The purpose of the test is to characterize facesheet/core peel in sandwich structure, accomplished through the measurement of the critical strain energy release rate associated with the debonding process. The specific test method selected for the standardized test procedure utilizes a single cantilever beam (SCB) specimen configuration. The objective of the current work is to develop a method for establishing SCB specimen dimensions. This is achieved by imposing specific limitations on specimen dimensions, with the objectives of promoting a linear elastic specimen response, and simplifying the data reduction method required for computing the critical strain energy release rate associated with debonding. The sizing method is also designed to be suitable for incorporation into a standardized test protocol. Preliminary application of the resulting sizing method yields practical specimen dimensions.

  4. Defects in ZnO, CdTe, and Si: Optical, structural, and electrical characterization

    CERN Multimedia

    Deicher, M; Kronenberg, J; Johnston, K; Roder, J; Byrne, D J

    Electronic and optical properties of semiconductors are extremely sensitive to defects and impurities that have localized electronic states with energy levels in the band gap of the semiconductor. Spectroscopic techniques like photo-luminescence (PL), deep level transient spectroscopy (DLTS), or Hall effect that are able to detect and characterize band gap states do not reveal direct information about their microscopic origin. To overcome this chemical "blindness" radioactive isotopes are used as a tracer. Moreover, the recoil energies involved in ${\\beta}$- and ${\\gamma}$-decays can be used to create intrinsic, isolated point defects (interstitials, vacancies) in a controlled way. A microscopic insight into the structure and the thermodynamic properties of complexes formed by interacting defects can be gained by detecting the hyperfine interaction between the nuclear moments of radioactive dopants and the electromagnetic fields present at the site of the radioactive nucleus. These techniques will be used to...

  5. Conductance based characterization of structure and hopping site density in 2D molecule-nanoparticle arrays (United States)

    McCold, Cliff E.; Fu, Qiang; Howe, Jane Y.; Hihath, Joshua


    Composite molecule-nanoparticle hybrid systems have recently emerged as important materials for applications ranging from chemical sensing to nanoscale electronics. However, creating reproducible and repeatable composite materials with precise properties has remained one of the primary challenges to the implementation of these technologies. Understanding the sources of variation that dominate the assembly and transport behavior is essential for the advancement of nanoparticle-array based devices. In this work, we use a combination of charge-transport measurements, electron microscopy, and optical characterization techniques to determine the role of morphology and structure on the charge transport properties of 2-dimensional monolayer arrays of molecularly-interlinked Au nanoparticles. Using these techniques we are able to determine the role of both assembly-dependent and particle-dependent defects on the conductivities of the films. These results demonstrate that assembly processes dominate the dispersion of conductance values, while nanoparticle and ligand features dictate the mean value of the conductance. By performing a systematic study of the conductance of these arrays as a function of nanoparticle size we are able to extract the carrier mobility for specific molecular ligands. We show that nanoparticle polydispersity correlates with the void density in the array, and that because of this correlation it is possible to accurately determine the void density within the array directly from conductance measurements. These results demonstrate that conductance-based measurements can be used to accurately and non-destructively determine the morphological and structural properties of these hybrid arrays, and thus provide a characterization platform that helps move 2-dimensional nanoparticle arrays toward robust and reproducible electronic systems.Composite molecule-nanoparticle hybrid systems have recently emerged as important materials for applications ranging from

  6. Characterizing the nano and micro structure of concrete to improve its durability

    KAUST Repository

    Monteiro, P.J.M.


    New and advanced methodologies have been developed to characterize the nano and microstructure of cement paste and concrete exposed to aggressive environments. High resolution full-field soft X-ray imaging in the water window is providing new insight on the nano scale of the cement hydration process, which leads to a nano-optimization of cement-based systems. Hard X-ray microtomography images of ice inside cement paste and cracking caused by the alkali-silica reaction (ASR) enables three-dimensional structural identification. The potential of neutron diffraction to determine reactive aggregates by measuring their residual strains and preferred orientation is studied. Results of experiments using these tools are shown on this paper. © 2009 Elsevier Ltd. All rights reserved.

  7. Desalted Duck Egg White Peptides: Promotion of Calcium Uptake and Structure Characterization. (United States)

    Hou, Tao; Wang, Chi; Ma, Zhili; Shi, Wen; Weiwei, Lui; He, Hui


    The effects of desalted duck egg white peptides (DPs) on calcium absorption were investigated in three models: Caco-2 cell monolayer model, Caco-2 cell population model, and everted intestinal sac model. DPs were found to enhance calcium transport and may do so by acting as calcium carriers and interacting with the cell membrane to open a special Ca(2+) channel, whereas the paracellular pathway may make only a minor contribution. Structure characterization demonstrated the important roles of seven crucial peptides, such as VSEE and LYAEE, in binding calcium and promoting calcium uptake. Three synthetic peptides (VHSS, VSEE, and VHS(p)S(p)) potently induced calcium transport in Caco-2 monolayers, with VHS(p)S(p) being the most effective. This research expands the understanding of the mechanism of cellular calcium uptake by DPs as well as highlights an opportunity for recycling an otherwise discarded processing byproduct.

  8. Material characterization of structural adhesives in the lap shear mode. M.S. Thesis (United States)

    Schenck, S. C.; Sancaktar, E.


    A general method for characterizing structural adhesives in the bonded lap shear mode is proposed. Two approaches in the form of semi-empirical and theoretical approaches are used. The semi-empirical approach includes Ludwik's and Zhurkov's equations to describe respectively, the failure stresses in the constant strain rate and constant stress loading modes with the inclusion of the temperature effects. The theoretical approach is used to describe adhesive shear stress-strain behavior with the use of viscoelastic or nonlinear elastic constitutive equations. Three different model adhesives are used in the simple lap shear mode with titanium adherends. These adhesives (one of which was developed at NASA Langley Research Center) are currently considered by NASA for possible aerospace applications. Use of different model adhesives helps in assessment of the generality of the method.

  9. Optical and Structural Characterization of Nickel Coatings for Solar Collector Receivers

    Directory of Open Access Journals (Sweden)

    Stefano Pratesi


    Full Text Available The development of spectrally selective materials is gaining an increasing role in solar thermal technology. The ideal spectrally selective solar absorber requires high absorbance at the solar spectrum wavelengths and low emittance at the wavelengths of thermal spectrum. Selective coating represents a promising route to improve the receiver efficiency for parabolic trough collectors (PTCs. In this work, we describe an intermediate step in the fabrication of black-chrome based solar absorbers, namely, the fabrication and characterization of nickel coatings on stainless steel substrates. Microstructural characteristics of nickel surfaces are known to favorably affect further black chrome deposition. Moreover, the high reflectivity of nickel in the thermal infrared wavelength region can be advantageously exploited for reducing thermal emission losses. Thus, this report investigates structural features and optical properties of the nickel surfaces, correlating them to coating thickness and deposition process, in the perspective to assess optimal conditions for solar absorber applications.

  10. Functional and structural characterization of plastidic starch phosphorylase during barley endosperm development

    DEFF Research Database (Denmark)

    Cuesta-Seijo, Jose A.; Ruzanski, Christian; Krucewicz, Katarzyna


    The production of starch is essential for human nutrition and represents a major metabolic flux in the biosphere. The biosynthesis of starch in storage organs like barley endosperm operates via two main pathways using different substrates: starch synthases use ADP-glucose to produce amylose...... (HvPho1) for starch biosynthesis in barley endosperm, we analyzed HvPho1 protein production and enzyme activity levels throughout barley endosperm development and characterized structure-function relationships of HvPho1. The molecular mechanisms underlying the initiation of starch granule biosynthesis......, that is, the enzymes and substrates involved in the initial transition from simple sugars to polysaccharides, remain unclear. We found that HvPho1 is present as an active protein at the onset of barley endosperm development. Notably, purified recombinant protein can catalyze the de novo production of α-1...

  11. Tetraphenylphosphonium allyldithiocarbimates derived from Morita-Baylis-Hillman adducts: Synthesis, characterization, crystal structure and antifungal activity (United States)

    Tavares, Eder C.; Rubinger, Mayura M. M.; Filho, Eclair V.; Oliveira, Marcelo R. L.; Piló-Veloso, Dorila; Ellena, Javier; Guilardi, Silvana; Souza, Rafael A. C.; Zambolim, Laércio


    Botrytis blight is a very destructive disease caused by Botrytis spp., infecting flowers, trees, vegetables and fruits. Twelve new compounds were prepared by the reaction of potassium N-aryl-sulfonyldithiocarbimates with Morita-Baylis-Hillman derivatives bearing phenyl and furyl groups. These are the first examples of allyldithiocarbimate anions and were isolated as tetraphenylphosphonium salts. The new compounds were characterized by HRMS, NMR and Infrared spectroscopy. Further, the structures of three allyldithiocarbimates were determined by single crystal X-ray diffraction. The compounds are isostructural and crystallize in the space group P21/c of the monoclinic system, and the allyldithiocarbimate anions present Z configuration. All the compounds were active against Botrytis cinerea. The best results were achieved with the tetraphenylphosphonium (Z)-3-(furan-2-yl)-2-(methoxycarbonyl)allyl-(4-chlorophenylsulfonyl)dithiocarbimate (IC50 38 μM).

  12. Partial structural characterization of pectin cell wall from Argania spinosa leaves. (United States)

    Hachem, Kadda; Benabdesslem, Yasmina; Ghomari, Samia; Hasnaoui, Okkacha; Kaid-Harche, Meriem


    The pectin polysaccharides from leaves of Argania spinosa (L.) Skeels, collected from Stidia area in the west coast of northern Algeria, were investigated by using sequential extractions and the resulting fractions were analysed for monosaccharide composition and chemical structure. Water-soluble pectic (ALS-WSP) and chelating-soluble pectic (ALS-CSP) fractions were obtained, de-esterified and fractionated by anion-exchange chromatography and characterized by sugar analysis combined with methylation analysis and (1)H and (13)C NMR spectroscopy. The data reveal the presence of altering homogalacturonan (HG) and rhamnogalacturonan I (RG-I) in both pectin fraction. The rhamnogalacturonan I (RG-I) are consisted of a disaccharide repeating unit [→ α-D-GalpA-1,2-α-L-Rhap-1,4 →] backbone, with side chains contained highly branched α-(1 → 5)-linked arabinan and short linear β-(1 → 4)-linked galactan, attached to O-4 of the rhamnosyl residues.

  13. Structural Characterization of the Extracellular Polysaccharide from Vibrio cholerae O1 El-Tor (United States)

    Yildiz, Fitnat; Fong, Jiunn; Sadovskaya, Irina; Grard, Thierry; Vinogradov, Evgeny


    The ability to form biofilms is important for environmental survival, transmission, and infectivity of Vibrio cholerae, the causative agent of cholera in humans. To form biofilms, V. cholerae produces an extracellular matrix composed of proteins, nucleic acids and a glycoconjugate, termed Vibrio exopolysaccharide (VPS). Here, we present the data on isolation and characterization of the polysaccharide part of the VPS (VPS-PS), which has the following structure: where α-D-Glc is partially (∼20%) replaced with α-D-GlcNAc. α-GulNAcAGly is an amide between 2-acetamido-2-deoxy-α-guluronic acid and glycine. Apparently, the polysaccharide is bound to a yet unidentified component, which gives it high viscosity and completely suppresses any NMR signals belonging to the sugar chains of the VPS. The only reliable method to remove this component at present is a treatment of the whole glycoconjugate with concentrated hydrochloric acid. PMID:24520310

  14. Structural, Optical, and Electrical Characterization of Spray Pyrolysed Indium Sulfide Thin Films (United States)

    Rahman, F.; Podder, J.; Ichimura, M.


    Indium sulfide (In2S3) thin films were deposited onto the glass substrates by a low cost simple spray pyrolysis technique at 300°C temperature. Aqueous solution of indium chloride and thiourea were used to deposit the binary In-S film. The deposited thin films were annealed at 400° and 500°C temperatures and characterized structurally, optically and electrically using EDX, X-ray diffraction, UV-visible spectroscopy and four probe van der Pauw methods. The optical constants such as refractive index and extinction coefficient are calculated from absorbance and transmittance data from 300 to 1100 nm wavelength. The optical transmittance increased after annealing at 400° and 500°C. The band gap energy was reduced from 2.90 to 2.50 eV after annealing the as deposited films. The electrical conductivity as well as the activation energy was increased after annealing the samples.

  15. Structural characterization of half-metallic Heusler compound NiMnSb

    Energy Technology Data Exchange (ETDEWEB)

    Nowicki, L. E-mail:; Abdul-Kader, A.M.; Bach, P.; Schmidt, G.; Molenkamp, L.W.; Turos, A.; Karczewski, G


    High resolution X-ray diffraction (HRXRD) and Rutherford backscattering/channeling (RBS/c) techniques were used to characterize layers of NiMnSb grown by molecular beam epitaxy (MBE) on InP with a In{sub x}Ga{sub 1-x}As buffer. Angular scans in the channeling mode reveal that the crystal structure of NiMnSb is tetragonally deformed with c/a=1.010{+-}0.002, in agreement with HRXRD data. Although HRXRD demonstrates the good quality of the pseudomorphic NiMnSb layers the channeling studies show that about 20% of atoms in the layers do not occupy lattice sites in the [0 0 1] rows of NiMnSb. The possible mechanisms responsible for the observed disorder are discussed.

  16. Characterizing the nano and micro structure of concrete to improve its durability

    Energy Technology Data Exchange (ETDEWEB)

    Monteiro, P.J.M.; Kirchheim, A.P.; Chae, S.; Fischer, P.; MacDowell, A.A.; Schaible, E.; Wenk, H.R.


    New and advanced methodologies have been developed to characterize the nano and microstructure of cement paste and concrete exposed to aggressive environments. High resolution full-field soft X-ray imaging in the water window is providing new insight on the nano scale of the cement hydration process, which leads to a nano-optimization of cement-based systems. Hard X-ray microtomography images on ice inside cement paste and cracking caused by the alkali-silica reaction (ASR) enables three-dimensional structural identification. The potential of neutron diffraction to determine reactive aggregates by measuring their residual strains and preferred orientation is studied. Results of experiments using these tools will be shown on this paper.

  17. Characterizing the Nano and Micro Structure of Concrete toImprove its Durability

    Energy Technology Data Exchange (ETDEWEB)

    Monteiro, P.J.M.; Kirchheim, A.P.; Chae, S.; Fischer, Peter; MacDowell, Alastair; Schaible, Eirc; Wenk, H.R.; Macdowell, Alastair A.


    New and advanced methodologies have been developed to characterize the nano and microstructure of cement paste and concrete exposed to aggressive environments. High resolution full-field soft X-ray imaging in the water window is providing new insight on the nano scale of the cement hydration process, which leads to a nano-optimization of cement-based systems. Hard X-ray microtomography images of ice inside cement paste and cracking caused by the alkali?silica reaction (ASR) enables three-dimensional structural identification. The potential of neutron diffraction to determine reactive aggregates by measuring their residual strains and preferred orientation is studied. Results of experiments using these tools are shown on this paper.

  18. Structural and spectroscopic ellipsometry characterization for electrodeposited ZnO growth at different hydrogen peroxide concentration

    Energy Technology Data Exchange (ETDEWEB)

    El Hichou, A., E-mail: [Laboratoire de la Matiere Condensee et Nanostructures (LMCN), Faculte des Sciences et Techniques, BP 549, 40000 Marrakech (Morocco); Stein, N.; Boulanger, C. [Institut Jean Lamour, Laboratoire d' Electrochimie des Materiaux, UPV-M, CNRS, 1 bd Arago CP 87811, 57078 Metz cedex 3 (France); Johann, L. [Laboratoire de Physique des Milieux denses, UPV-M, 1 bd Arago CP 87811, 57078 Metz cedex 3 (France)


    This work deals with textural and optical characterization of zinc oxide (ZnO) layers obtained by potentiostatic electroplating at various hydrogen peroxide concentrations (from 0 up to 5 mM). The electrodeposition process was studied by cyclic voltametry and chronoamperometry. The [002] preferred growth orientation of hexagonal phase is obtained for the lowest hydrogen peroxide concentration (1 mM), while additionally X-ray diffraction peaks are observed for hydrogen peroxide concentration ranging from 3 to 5 mM. The optical constants and the thickness of films were determined by spectroscopic ellipsometry measurements. The refractive index of all thin films shows normal dispersion behavior. It was also found that refractive index values decrease with increasing hydrogen peroxide concentration. Further, it was revealed that the changes in the optical properties are correlated to the changes in the surface structure.

  19. Bimetallic octahedral ruthenium-nickel carbido cluster complexes. Synthesis and structural characterization. (United States)

    Saha, Sumit; Zhu, Lei; Captain, Burjor


    The reaction of Ru5(CO)15(μ5-C) with Ni(COD)2 in acetonitrile at 80 °C affords the bimetallic octahedral ruthenium-nickel cluster complex Ru5Ni(NCMe)(CO)15(μ6-C), 3. The acetonitrile ligand in 3 can be replaced by CO and NH3 to yield Ru5Ni(CO)16(μ6-C), 4, and Ru5Ni(NH3)(CO)15(μ6-C), 5, respectively. Photolysis of compound 3 in benzene and toluene solvent yielded the η(6)-coordinated benzene and toluene Ru5Ni carbido cluster complexes Ru5Ni(CO)13(η(6)-C6H6)(μ6-C), 6, and Ru5Ni(CO)13(η(6)-C7H8)(μ6-C), 7, respectively. All five new compounds were structurally characterized by single-crystal X-ray diffraction analyses.

  20. New topologies in pentanuclear nickel/oximato clusters: structural and magnetic characterization. (United States)

    Esteban, Jordi; Font-Bardia, Mercè; Costa, José Sánchez; Teat, Simon J; Escuer, Albert


    In the present work, five new Ni5 clusters employing the versatile 2-pyridylcyanoxime ligand have been synthesized and chemically, structurally, and magnetically characterized. The crystallographic examination of these Ni5 clusters together with those already published in the literature, giving a total number of 14 complexes, exhibiting up to 8 different topologies for which the relationship between topology, reaction conditions and magnetic response has been analyzed. DC magnetic measurements were carried in the 300-2 K range for the new complexes and the analysis of the experimental data revealed an antiferromagnetic response for the oximato mediated interactions with a variety of ground states (S = 0, 1, 3) as function of the cluster topology.

  1. Facile synthesis and structural characterization of amylose-Fatty Acid inclusion complexes. (United States)

    Cao, Zheng; Woortman, Albert J J; Rudolf, Petra; Loos, Katja


    Amylose-fatty acid inclusion complexes can be easily prepared by simple mixing in hot aqueous solutions. Above a critical chain length (C6) of the fatty acid insoluble complexes between amylose and each fatty acid (C8, C10, C12, C14, C16) were precipitated from the solution, and characterized by FT-IR, XRD, DSC, and SEC. The presence of the characteristic (CO) FT-IR absorption peak at 1 710 cm(-1) confirmed the inclusion of the fatty acids inside the amylose helix. XRD showed the same characteristic features of the V amylose single helical structure. Both SEC and DSC revealed that longer fatty acids can form inclusion complexes with amylose fractions having higher degree of polymerization, leading to greater yields, and higher thermal stability (higher melting temperature and enthalpy) of the amylose-complexes. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Machining and Characterizing X-Band RF-Structures for CLIC

    CERN Document Server

    Atieh, S; Arnau-Izquierdo, G; Cherif, A; Deparis, L; Glaude, D; Remandet, L; Riddone, G; Scheubel, M; Gudkov, D; Samoshkin, A; Soldko, A


    The Compact Linear Collider (CLIC) is currently under study at CERN as a potential multi-TeV e+e– collider. The manufacturing and assembling tolerances for making the required RF components are essential for CLIC to perform efficiently. Machining techniques are relevant to the construction of ultra-high-precision parts for the Accelerating Structures (AS). Optical-quality turning and ultra-precision milling using diamond tools are the main manufacturing techniques identified to produce ultra-high shape accuracy parts. A shape error of less than 5 μm and roughness of Ra 0.025 are achieved. Scanning Electron Microscopy (SEM) observation as well as sub-micron precision Coordinate Measuring Machines (CMM), roughness measurements and their crucial environment were implemented at CERN for quality assurance and further development. This paper focuses on the enhancements of precision machining and characterizing the fabrication of AS parts.

  3. Electrical Characterization of Amorphous Silicon MIS-Based Structures for HIT Solar Cell Applications (United States)

    García, Héctor; Castán, Helena; Dueñas, Salvador; Bailón, Luis; García-Hernansanz, Rodrigo; Olea, Javier; del Prado, Álvaro; Mártil, Ignacio


    A complete electrical characterization of hydrogenated amorphous silicon layers (a-Si:H) deposited on crystalline silicon (c-Si) substrates by electron cyclotron resonance chemical vapor deposition (ECR-CVD) was carried out. These structures are of interest for photovoltaic applications. Different growth temperatures between 30 and 200 °C were used. A rapid thermal annealing in forming gas atmosphere at 200 °C during 10 min was applied after the metallization process. The evolution of interfacial state density with the deposition temperature indicates a better interface passivation at higher growth temperatures. However, in these cases, an important contribution of slow states is detected as well. Thus, using intermediate growth temperatures (100-150 °C) might be the best choice.

  4. Characterization of nanostructured TiO2:Ag films: structural and optical properties (United States)

    Ivanova, T.; Harizanova, A.; Koutzarova, T.; Vertruyen, B.


    TiO2:Ag nanocomposites have been prepared by sol-gel method with varying silver concentration. Different technological approaches are employed to study the formation of Ag nanoparticles in titanium dioxide matrix. The obtained thin films are either thermally treated at temperatures from 300 to 600oC or UV irradiated for 15 minutes between layer deposition. XRD and FTIR studies reveal that Ag is incorporated in TiO2 films as nanoparticles and no Ag oxide phases are detected. Optical characterization performed by UV-VIS spectroscopy confirms the formation of silver nanoparticles. The influence of thermal treatment and UV radiation on the optical and structural properties is studied.

  5. NMR and computational methods in the structural and dynamic characterization of ligand-receptor interactions. (United States)

    Ghitti, Michela; Musco, Giovanna; Spitaleri, Andrea


    The recurrent failures in drug discovery campaigns, the asymmetry between the enormous financial investments and the relatively scarce results have fostered the development of strategies based on complementary methods. In this context in recent years the rigid lock-and-key binding concept had to be revisited in favour of a dynamic model of molecular recognition accounting for conformational changes of both the ligand and the receptor. The high level of complexity required by a dynamic description of the processes underlying molecular recognition requires a multidisciplinary investigation approach. In this perspective, the combination of nuclear magnetic resonance spectroscopy with molecular docking, conformational searches along with molecular dynamics simulations has given new insights into the dynamic mechanisms governing ligand receptor interactions, thus giving an enormous contribution to the identification and design of new and effective drugs. Herein a succinct overview on the applications of both NMR and computational methods to the structural and dynamic characterization of ligand-receptor interactions will be presented.

  6. Synthesis and structural characterization of piperazino-modified DNA that favours hybridization towards DNA over RNA

    DEFF Research Database (Denmark)

    Skov, Joan; Bryld, Torsten; Lindegaard, Dorthe


    modifications are tolerated in DNA:RNA hybrids but leave their melting temperatures virtually unaffected. Fluorescence data indicate that the pyrene moiety is residing outside the helix. The available data suggest that the DNA discrimination is due to (i) the positive charge of the piperazino ring having...... a greater impact in the narrow and deep minor groove of a B-type dsDNA duplex than in the wide and shallow minor groove of an A-type DNA:RNA hybrid and (ii) the B-type dsDNA duplex allowing the pyrene to intercalate and bury its apolar surface.......We report the synthesis of two C4'-modified DNA analogues and characterize their structural impact on dsDNA duplexes. The 4'-C-piperazinomethyl modification stabilizes dsDNA by up to 5°C per incorporation. Extension of the modification with a butanoyl-linked pyrene increases the dsDNA stabilization...

  7. Micelles by self-assembling peptide-conjugate amphiphile: synthesis and structural characterization. (United States)

    Accardo, Antonella; Tesauro, Diego; Del Pozzo, Luigi; Mangiapia, Gaetano; Paduano, Luigi; Morelli, Giancarlo


    The chemical synthesis by solid-phase methods of a novel amphiphilic peptide, peptide-conjugate amphiphile (PCA), containing in the same molecule three different functions: (i) the N,N-bis[2-[bis(carboxy-ethyl)amino]ethyl]-L-glutamic acid (DTPAGlu) chelating agent, (ii) the CCK8 bioactive peptide, and (iii) a hydrophobic moiety containing four alkyl chains with 18 carbon atoms each, is reported. In water solution at pH 7.4, PCA self-assembles in very stable micelles at very low concentration [critical micellar concentration (cmc) values of 5 x 10(-7) mol kg(-1)] as confirmed by fluorescence spectroscopy. The structural characterization, obtained with small-angle neutron scattering (SANS) measurements, indicates that the aggregates are substantially represented by ellipsoidal micelles with an aggregation number of 39 +/- 2 and the two micellar axes of about 52 and 26 A. Copyright (c) 2008 European Peptide Society and John Wiley & Sons, Ltd.

  8. Synthesis, characterization, crystal structure and electrochemical studies of ionic iron(III) dipicolinato complex (United States)

    Ghasemi, Fatemeh; Ghasemi, Khaled; Rezvani, Ali Reza; Rosli, Mohd Mustaqim; Razak, Ibrahim Abdul


    The new complex (NH4)[Fe(dipic)2] (1) (dipicH2 = 2,6-pyridinedicarboxylic acid), was synthesized and characterized by elemental analysis, FTIR and UV-Vis spectroscopy and single crystal X-ray method. The crystal system is tetragonal with space group I41/a. The FeIII ion and the N atom of the ammonium cation are located on a crystallographic fourfold rotoinversion axis (4 bar). The Nsbnd H⋯O and Csbnd H⋯O intermolecular hydrogen bonding and π⋯π stacking interactions play an important role in the formation of a 3-dimensional anion-cation network and stabilization of the crystal structure. The redox behavior of the complex was also investigated by cyclic voltammetry.

  9. Partial structural characterization and antioxidant activity of a phenolic-xylan from Castanea sativa hardwood. (United States)

    Renault, Emmanuel; Barbat-Rogeon, Aline; Chaleix, Vincent; Calliste, Claude-Alain; Colas, Cyril; Gloaguen, Vincent


    4-O-Methylglucuronoxylans (MGX) were isolated from chestnut wood sawdust using two different procedures: chlorite delignification followed by the classical alkaline extraction step, and an unusual green chemistry process of delignification using phthalocyanine/H2O2 followed by a simple extraction with hot water. Antioxidant properties of both MGX were evaluated against the stable radical 2,2-diphenyl-1-picrylhydrazyl (DPPH) by electronic spin resonance (ESR). IC50 of water-extracted MGX was found to be less than 225 μg mL(-1), in contrast with alkali-extracted MGX for which no radical scavenging was observed. Characterization of extracts by colorimetric assay, GC, LC-MS and NMR spectroscopy provided some clues to understanding structure-function relationships of MGX in connection with their antioxidant activity. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Characterization of electronic structure and physicochemical properties of antiparasitic nifurtimox analogues: A theoretical study (United States)

    Soriano-Correa, Catalina; Raya, A.; Esquivel, Rodolfo O.

    American trypanosomiasis, also known as Chagas' disease, is caused by Trypanosoma cruzi (T. cruzi). It is well known that trypanosomes, and particularly T. cruzi, are highly sensitive towards oxidative stress, i.e., to compounds than are able to produce free radicals. Generally, nifurtimox (NFX) and benznidazol are most effective in the acute phase of the disease; therefore, nitroheterocycles constitute good models to design other nitrocompounds with specific biological characteristics. Thus, we have performed an ab initio study at the Hartree-Fock and Density Functional Theory levels of theory of several NFX analogues recently synthesized, to characterize them by obtaining their electronic, structural, and physicochemical properties, which might be linked to the observed antichagasic activity. The antitrypanosomal activity scale previously reported for the NFX analogues studied in this work is in good agreement with our theoretical results, from which we can conclude that the activity seems to be related to the reactivity along with the acidity observed for the most active molecules.

  11. Structural, Biochemical, and Biophysical Characterization of Idelalisib Binding to Phosphoinositide 3-Kinase δ* (United States)

    Somoza, John R.; Koditek, David; Villaseñor, Armando G.; Novikov, Nikolai; Wong, Melanie H.; Liclican, Albert; Xing, Weimei; Lagpacan, Leanna; Wang, Ruth; Schultz, Brian E.; Papalia, Giuseppe A.; Samuel, Dharmaraj; Lad, Latesh; McGrath, Mary E.


    Idelalisib (also known as GS-1101, CAL-101, IC489666, and Zydelig) is a PI3Kδ inhibitor that has recently been approved for the treatment of several hematological malignancies. Given its use in human diseases, we needed a clear picture of how idelalisib binds to and inhibits PI3Kδ. Our data show that idelalisib is a potent and selective inhibitor of the kinase activity of PI3Kδ. A kinetic characterization clearly demonstrated ATP-competitive inhibition, and several additional biochemical and biophysical assays showed that the compound binds reversibly and noncovalently to the kinase. A crystal structure of idelalisib bound to the p110δ subunit of PI3Kδ furthers our understanding of the binding interactions that confer the potency and selectivity of idelalisib. PMID:25631052

  12. Characterization of wami tilapia (Oreochromis urolepis hornorum) skin gelatin: microbiological, rheological and structural properties. (United States)

    Alfaro, Alexandre Da Trindade; Fonseca, Gustavo Graciano; Balbinot, Evellin; Prentice, Carlos


    Gelatin was extracted from the skin of tilapia (Oreochromis urolepis hornorum) and its microbiological, rheological and structural properties were characterized. The tilapia skin gelatin presented typical molecular weight distribution of type I collagen with contents of imino acids (proline + hydroxyproline) of 21.67%. Gel strength and viscosity values were 221 ± 5.68 g and 5.98 ± 0.34 cP, respectively, with the maturation time of 18 ± 1 h, and both parameters increased with the maturation time. Melting and gelling points of 25 degrees C and 21 degrees C, respectively, were obtained for tilapia skin gelatin. The gelatin presented microbiological standards in accordance with the Brazilian Legislation.

  13. Accurate and rapid optical characterization of an anisotropic guided structure based on a neural method. (United States)

    Robert, Stéphane; Battie, Yann; Jamon, Damien; Royer, Francois


    Optimal performances of integrated optical devices are obtained by the use of an accurate and reliable characterization method. The parameters of interest, i.e., optical indices and thickness of the waveguide structure, are calculated from effective indices by means of an inversion procedure. We demonstrate how an artificial neural network can achieve such a process. The artificial neural network used is a multilayer perceptron. The first result concerns a simulated anisotropic waveguide. The accuracy in the determination of optical indices and waveguide thickness is 5 x 10(-5) and 4 nm, respectively. Then an experimental application on a silica-titania thin film is performed. In addition, effective indices are measured by m-lines spectroscopy. Finally, a comparison with a classical optimization algorithm demonstrates the robustness of the neural method.

  14. Solid state NMR and IR characterization of wood polymer structure in relation to tree provenance. (United States)

    Santoni, Ilaria; Callone, Emanuela; Sandak, Anna; Sandak, Jakub; Dirè, Sandra


    (13)C nuclear magnetic resonance and mid-infrared spectroscopies were used for characterizing changes in the chemical structure of wood polymers (cellulose, hemicellulose and lignin) in relation to the tree growth location. Samples of three provenances in Europe (Finland, Poland and Italy) were selected for studies. The requirement was to use untreated solid wood samples to minimize any manipulation to the nanostructure of native wood. The results confirm that the chemical and physical properties of samples belonging to the same wood species (Picea abies Karst.) differ due to the origin. Both FT-IR and dynamic NMR spectroscopies were able to correctly discriminate samples originating from three different provenances in Europe. Such methods might be very useful for both, research and understanding of wood microstructure and its variability due to the growth conditions. Copyright © 2014 Elsevier Ltd. All rights reserved.

  15. Biophysical and structural characterization of mono/di-arylated lactosamine derivatives interaction with human galectin-3. (United States)

    Atmanene, Cédric; Ronin, Céline; Téletchéa, Stéphane; Gautier, François-Moana; Djedaïni-Pilard, Florence; Ciesielski, Fabrice; Vivat, Valérie; Grandjean, Cyrille


    Combination of biophysical and structural techniques allowed characterizing and uncovering the mechanisms underlying increased binding affinity of lactosamine derivatives for galectin 3. In particular, complementing information gathered from X-ray crystallography, native mass spectrometry and isothermal microcalorimetry showed favorable enthalpic contribution of cation-π interaction between lactosamine aryl substitutions and arginine residues from the carbohydrate recognition domain, which resulted in two log increase in compound binding affinity. This incrementing strategy allowed individual contribution of galectin inhibitor moieties to be dissected. Altogether, our results suggest that core and substituents of these saccharide-based inhibitors can be optimized separately, providing valuable tools to study the role of galectins in diseases. Copyright © 2017 Elsevier Inc. All rights reserved.

  16. Characterization and radiation studies of diode test structures in LFoundry CMOS technology

    Energy Technology Data Exchange (ETDEWEB)

    Daas, Michael; Gonella, Laura; Hemperek, Tomasz; Huegging, Fabian; Krueger, Hans; Pohl, David-Leon; Wermes, Norbert [Physikalisches Institut der Universitaet Bonn (Germany); Macchiolo, Anna [Max-Planck-Institut fuer Physik, Muenchen (Germany)


    In order to prepare for the High Luminosity upgrade of the LHC, all subdetector systems of the ATLAS experiment will be upgraded. In preparation for this process, different possibilities for new radiation-hard and cost-efficient silicon sensor technologies to be used as part of hybrid pixel detectors in the ATLAS inner tracker are being investigated. One promising way to optimize the cost-efficiency of silicon-based pixel detectors is to use commercially available CMOS technologies such as the 150 nm process by LFoundry. In this talk, several CMOS pixel test structures, such as simple diodes and small pixel arrays, that were manufactured in this technology are characterized regarding general performance and radiation hardness and compared to each other as well as to the current ATLAS pixel detector.

  17. Structural Characterization of Polymers of Intrinsic Microporosity Using X-ray Scattering Methods (United States)

    McDermott, Amanda; Chaukura, Nhamo; Mason, Christopher; Budd, Peter; Msayib, Kadum; Carta, Mariolino; Ghanem, Bader; McKeown, Neil; Runt, James


    Polymers of intrinsic microporosity (PIMs) are a novel class of materials with a large inner surface area and large free volume, which make them suitable for hydrogen adsorption. In addition, they exhibit a combination of high permeability and high selectivity useful for filtration applications. A series of polymers with high glass transition temperatures based on PIM-1, a polybenzodioxane with a ladder-type structure combining stiff segments with sites of contortion, as well as a series of triptycene-based network PIMs, are characterized via small-angle and wide-angle X-ray scattering. Scattering features, including multiple amorphous halos and a characteristic power-law slope, are related to polymer chemistry, hydrogen adsorption performance, and gas permeation parameters.

  18. Development of IR Contrast Data Analysis Application for Characterizing Delaminations in Graphite-Epoxy Structures (United States)

    Havican, Marie


    Objective: Develop infrared (IR) flash thermography application based on use of a calibration standard for inspecting graphite-epoxy laminated/honeycomb structures. Background: Graphite/Epoxy composites (laminated and honeycomb) are widely used on NASA programs. Composite materials are susceptible for impact damage that is not readily detected by visual inspection. IR inspection can provide required sensitivity to detect surface damage in composites during manufacturing and during service. IR contrast analysis can provide characterization of depth, size and gap thickness of impact damage. Benefits/Payoffs: The research provides an empirical method of calibrating the flash thermography response in nondestructive evaluation. A physical calibration standard with artificial flaws such as flat bottom holes with desired diameter and depth values in a desired material is used in calibration. The research devises several probability of detection (POD) analysis approaches to enable cost effective POD study to meet program requirements.

  19. Transparent Window Vibrational Probes for the Characterization of Proteins With High Structural and Temporal Resolution. (United States)

    Adhikary, Ramkrishna; Zimmermann, Jörg; Romesberg, Floyd E


    Vibrational spectroscopy provides a direct route to the physicochemical characterization of molecules. While both IR and Raman spectroscopy have been used for decades to provide detailed characterizations of small molecules, similar studies with proteins are largely precluded due to spectral congestion. However, the vibrational spectra of proteins do include a "transparent window", between ∼1800 and ∼2500 cm-1, and progress is now being made to develop site-specifically incorporated carbon-deuterium (C-D), cyano (CN), thiocyanate (SCN), and azide (N3) "transparent window vibrational probes" that absorb within this window and report on their environment to facilitate the characterization of proteins with small molecule-like detail. This Review opens with a brief discussion of the advantages and limitations of conventional vibrational spectroscopy and then discusses the strengths and weaknesses of the different transparent window vibrational probes, methods by which they may be site-specifically incorporated into peptides and proteins, and the physicochemical properties they may be used to study, including electrostatics, stability and folding, hydrogen bonding, protonation, solvation, dynamics, and interactions with inhibitors. The use of the probes to vibrationally image proteins and other biomolecules within cells is also discussed. We then present four case studies, focused on ketosteroid isomerase, the SH3 domain, dihydrofolate reductase, and cytochrome c, where the transparent window vibrational probes have already been used to elucidate important aspects of protein structure and function. The Review concludes by highlighting the current challenges and future potential of using transparent window vibrational probes to understand the evolution and function of proteins and other biomolecules.

  20. Structural and Functional Characterization of Reston Ebola Virus VP35 Interferon Inhibitory Domain

    Energy Technology Data Exchange (ETDEWEB)

    Leung, Daisy W.; Shabman, Reed S.; Farahbakhsh, Mina; Prins, Kathleen C.; Borek, Dominika M.; Wang, Tianjiao; Mühlberger, Elke; Basler, Christopher F.; Amarasinghe, Gaya K. (Sinai); (BU-M); (Iowa State); (UTSMC)


    Ebolaviruses are causative agents of lethal hemorrhagic fever in humans and nonhuman primates. Among the filoviruses characterized thus far, Reston Ebola virus (REBOV) is the only Ebola virus that is nonpathogenic to humans despite the fact that REBOV can cause lethal disease in nonhuman primates. Previous studies also suggest that REBOV is less effective at inhibiting host innate immune responses than Zaire Ebola virus (ZEBOV) or Marburg virus. Virally encoded VP35 protein is critical for immune suppression, but an understanding of the relative contributions of VP35 proteins from REBOV and other filoviruses is currently lacking. In order to address this question, we characterized the REBOV VP35 interferon inhibitory domain (IID) using structural, biochemical, and virological studies. These studies reveal differences in double-stranded RNA binding and interferon inhibition between the two species. These observed differences are likely due to increased stability and loss of flexibility in REBOV VP35 IID, as demonstrated by thermal shift stability assays. Consistent with this finding, the 1.71-{angstrom} crystal structure of REBOV VP35 IID reveals that it is highly similar to that of ZEBOV VP35 IID, with an overall backbone r.m.s.d. of 0.64 {angstrom}, but contains an additional helical element at the linker between the two subdomains of VP35 IID. Mutations near the linker, including swapping sequences between REBOV and ZEBOV, reveal that the linker sequence has limited tolerance for variability. Together with the previously solved ligand-free and double-stranded-RNA-bound forms of ZEBOV VP35 IID structures, our current studies on REBOV VP35 IID reinforce the importance of VP35 in immune suppression. Functional differences observed between REBOV and ZEBOV VP35 proteins may contribute to observed differences in pathogenicity, but these are unlikely to be the major determinant. However, the high level of similarity in structure and the low tolerance for sequence

  1. Structural characterization of AlN films synthesized by pulsed laser deposition

    Energy Technology Data Exchange (ETDEWEB)

    Szekeres, A. [Institute of Solid State Physics, Bulgarian Academy of Sciences, 72, Tzarigradsko Chaussee blvd., 1784 Sofia (Bulgaria); Fogarassy, Zs.; Petrik, P. [Research Institute for Technical Physics and Materials Science, Hungarian Academy of Sciences, Konkoly Thege Miklos u. 29-33, H-1121 Budapest (Hungary); Vlaikova, E. [Institute of Solid State Physics, Bulgarian Academy of Sciences, 72, Tzarigradsko Chaussee blvd., 1784 Sofia (Bulgaria); Cziraki, A. [Eotvos Lorand University, 1 Pazmany Peter setany, 1117 Budapest (Hungary); Socol, G.; Ristoscu, C.; Grigorescu, S. [National Institute for Lasers, Plasma, and Radiation Physics, PO Box MG-54, RO-77125 Magurele, Ilfov (Romania); Mihailescu, I.N., E-mail: [National Institute for Lasers, Plasma, and Radiation Physics, PO Box MG-54, RO-77125 Magurele, Ilfov (Romania)


    We obtained AlN thin films by pulsed laser deposition (PLD) from a polycrystalline AlN target using a pulsed KrF* excimer laser source (248 nm, 25 ns, intensity of {approx}4 x 10{sup 8} W/cm{sup 2}, repetition rate 3 Hz, 10 J/cm{sup 2} laser fluence). The target-Si substrate distance was 5 cm. Films were grown either in vacuum (10{sup -4} Pa residual pressure) or in nitrogen at a dynamic pressure of 0.1 and 10 Pa, using a total of 20,000 subsequent pulses. The films structure was characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and spectral ellipsometry (SE). Our TEM and XRD studies showed a strong dependence of the film structure on the nitrogen content in the ambient gas. The films deposited in vacuum exhibited a high quality polycrystalline structure with a hexagonal phase. The crystallite growth proceeds along the c-axis, perpendicular to the substrate surface, resulting in a columnar and strongly textured structure. The films grown at low nitrogen pressure (0.1 Pa) were amorphous as seen by TEM and XRD, but SE data analysis revealed {approx}1.7 vol.% crystallites embedded in the amorphous AlN matrix. Increasing the nitrogen pressure to 10 Pa promotes the formation of cubic ({<=}10 nm) crystallites as seen by TEM but their density was still low to be detected by XRD. SE data analysis confirmed the results obtained from the TEM and XRD observations.

  2. Fabrication, characterization, and heuristic trade space exploration of magnetically actuated Miura-Ori origami structures (United States)

    Cowan, Brett; von Lockette, Paris R.


    The authors develop magnetically actuated Miura-Ori structures through observation, experiment, and computation using an initially heuristic strategy followed by trade space visualization and optimization. The work is novel, especially within origami engineering, in that beyond final target shape approximation, Miura-Ori structures in this work are additionally evaluated for the shape approximation while folding and for their efficient use of their embedded actuators. The structures consisted of neodymium magnets placed on the panels of silicone elastomer substrates cast in the Miura-Ori folding pattern. Initially four configurations, arrangements of magnets on the panels, were selected based on heuristic arguments that (1) maximized the amount of magnetic torque applied to the creases and (2) reduced the number of magnets needed to affect all creases in the pattern. The results of experimental and computational performance metrics were used in a weighted sum model to predict the optimum configuration, which was then fabricated and experimentally characterized for comparison to the initial prototypes. As expected, optimization of magnet placement and orientation was effective at increasing the degree of theoretical useful work. Somewhat unexpectedly, however, trade space results showed that even after optimization, the configuration with the most number of magnets was least effective, per magnet, at directing its actuation to the structure’s creases. Overall, though the winning configuration experimentally outperformed its initial, non-optimal counterparts, results showed that the choice of optimum configuration was heavily dependent on the weighting factors. These results highlight both the ability of the Miura-Ori to be actuated with external magnetic stimuli, the effectiveness of a heuristic design approach that focuses on the actuation mechanism, and the need to address path-dependent metrics in assessing performance in origami folding structures.

  3. Assessing Local Structure Motifs Using Order Parameters for Motif Recognition, Interstitial Identification, and Diffusion Path Characterization

    Directory of Open Access Journals (Sweden)

    Nils E. R. Zimmermann


    Full Text Available Structure–property relationships form the basis of many design rules in materials science, including synthesizability and long-term stability of catalysts, control of electrical and optoelectronic behavior in semiconductors, as well as the capacity of and transport properties in cathode materials for rechargeable batteries. The immediate atomic environments (i.e., the first coordination shells of a few atomic sites are often a key factor in achieving a desired property. Some of the most frequently encountered coordination patterns are tetrahedra, octahedra, body and face-centered cubic as well as hexagonal close packed-like environments. Here, we showcase the usefulness of local order parameters to identify these basic structural motifs in inorganic solid materials by developing classification criteria. We introduce a systematic testing framework, the Einstein crystal test rig, that probes the response of order parameters to distortions in perfect motifs to validate our approach. Subsequently, we highlight three important application cases. First, we map basic crystal structure information of a large materials database in an intuitive manner by screening the Materials Project (MP database (61,422 compounds for element-specific motif distributions. Second, we use the structure-motif recognition capabilities to automatically find interstitials in metals, semiconductor, and insulator materials. Our Interstitialcy Finding Tool (InFiT facilitates high-throughput screenings of defect properties. Third, the order parameters are reliable and compact quantitative structure descriptors for characterizing diffusion hops of intercalants as our example of magnesium in MnO2-spinel indicates. Finally, the tools developed in our work are readily and freely available as software implementations in the pymatgen library, and we expect them to be further applied to machine-learning approaches for emerging applications in materials science.

  4. Neuronal accumulation of unrepaired DNA in a novel specific chromatin domain: structural, molecular and transcriptional characterization. (United States)

    Mata-Garrido, Jorge; Casafont, Iñigo; Tapia, Olga; Berciano, Maria T; Lafarga, Miguel


    There is growing evidence that defective DNA repair in neurons with accumulation of DNA lesions and loss of genome integrity underlies aging and many neurodegenerative disorders. An important challenge is to understand how neurons can tolerate the accumulation of persistent DNA lesions without triggering the apoptotic pathway. Here we study the impact of the accumulation of unrepaired DNA on the chromatin architecture, kinetics of the DNA damage response and transcriptional activity in rat sensory ganglion neurons exposed to 1-to-3 doses of ionizing radiation (IR). In particular, we have characterized the structural, molecular and transcriptional compartmentalization of unrepaired DNA in persistent DNA damaged foci (PDDF). IR induced the formation of numerous transient foci, which repaired DNA within the 24 h post-IR, and a 1-to-3 PDDF. The latter concentrate DNA damage signaling and repair factors, including γH2AX, pATM, WRAP53 and 53BP1. The number and size of PDDF was dependent on the doses of IR administered. The proportion of neurons carrying PDDF decreased over time of post-IR, indicating that a slow DNA repair occurs in some foci. The fine structure of PDDF consisted of a loose network of unfolded 30 nm chromatin fiber intermediates, which may provide a structural scaffold accessible for DNA repair factors. Furthermore, the transcription assay demonstrated that PDDF are transcriptionally silent, although transcription occurred in flanking euchromatin. Therefore, the expression of γH2AX can be used as a reliable marker of gene silencing in DNA damaged neurons. Moreover, PDDF were located in repressive nuclear environments, preferentially in the perinucleolar domain where they were frequently associated with Cajal bodies or heterochromatin clumps forming a structural triad. We propose that the sequestration of unrepaired DNA in discrete PDDF and the transcriptional silencing can be essential to preserve genome stability and prevent the synthesis of

  5. Surface Structure Spread Single Crystals (S4C): Preparation and characterization

    Energy Technology Data Exchange (ETDEWEB)

    de Alwis, A.; Holsclaw, B.; Pushkarev, V. V.; Reinicker, A.; Lawton, T. J.; Blecher, M. E.; Sykes, E. C. H.; Gellman, A. J.


    A set of six spherically curved Cu single crystals referred to as Surface Structure Spread Single Crystals (S{sup 4}Cs) has been prepared in such a way that their exposed surfaces collectively span all possible crystallographic surface orientations that can be cleaved from the face centered cubic Cu lattice. The method for preparing these S{sup 4}Cs and for finding the high symmetry pole point are described. Optical profilometry has been used to determine the true shapes of the S{sup 4}Cs and show that over the majority of the surface, the shape is extremely close to that of a perfect sphere. The local orientations of the surfaces lie within ±1{degree} of the orientation expected on the basis of the spherical shape; their orientation is as good as that of many commercially prepared single crystals. STM imaging has been used to characterize the atomic level structure of the Cu(111)±11{degree}-S{sup 4}C. This has shown that the average step densities and the average step orientations match those expected based on the spherical shape. In other words, although there is some distribution of step-step spacing and step orientations, there is no evidence of large scale reconstruction or faceting. The Cu S{sup 4}Cs have local structures based on the ideal termination of the face centered cubic Cu lattice in the direction of termination. The set of Cu S{sup 4}Cs will serve as the basis for high throughput investigations of structure sensitive surface chemistry on Cu.

  6. Synthesis, characterization, and crystal structure of mercury(II) complex containing new phosphine oxide salt (United States)

    Samiee, Sepideh; Kooti, Nadieh; Gable, Robert W.


    The reaction of new phosphonium-phosphine oxide salt [P(O)Ph2(CH2)2PPh2CH2C(O)C6H4NO2]Br (1) with mercury(II) iodide in a methanolic solution yielded [P(O)Ph2(CH2)2PPh2CH2C(O)C6H4NO2]2[Hg2I5Br](2). These two compounds were fully characterized by elemental analysis, IR, 1H, 31P, and 13C NMR spectra. Crystal and molecular structure of 2 has been determined by means of X-ray diffraction. In mercury compound, the phosphine oxide salt is found as a counter ion letting the mercury(II) ion to bound halides to all four coordination sites and to give dimermercurate(II) ions as the structure-constructing species. The neighboring [P(O)Ph2(CH2)2PPh2CH2C(O)C6H4NO2]2+cations are joined together by intramolecular Csbnd H⋯O hydrogen bonds to give a 1-D chain structure along the crystallographic b-axis. The [Hg2I5Br]2-anions act as cross-linkers between neighbouring strands extending the supramolecular structure into 2D layers in (110) planes as well as balances the charge of the complex. The significant effects of Csbnd H⋯X (Xdbnd O, Br and I) and π⋯π aromatic interactions play a major role in the crystal packing of compound 2.

  7. Structural Characterization of the SMRT Corepressor Interacting with Histone Deacetylase 7. (United States)

    Desravines, Danielle C; Serna Martin, Itziar; Schneider, Robert; Mas, Philippe J; Aleksandrova, Nataliia; Jensen, Malene Ringkjøbing; Blackledge, Martin; Hart, Darren J


    The 2525 amino acid SMRT corepressor is an intrinsically disordered hub protein responsible for binding and coordinating the activities of multiple transcription factors and chromatin modifying enzymes. Here we have studied its interaction with HDAC7, a class IIa deacetylase that interacts with the corepressor complex together with the highly active class I deacetylase HDAC3. The binding site of class IIa deacetylases was previously mapped to an approximate 500 amino acid region of SMRT, with recent implication of short glycine-serine-isoleucine (GSI) containing motifs. In order to characterize the interaction in detail, we applied a random library screening approach within this region and obtained a range of stable, soluble SMRT fragments. In agreement with an absence of predicted structural domains, these were characterized as intrinsically disordered by NMR spectroscopy. We identified one of them, comprising residues 1255-1452, as interacting with HDAC7 with micromolar affinity. The binding site was mapped in detail by NMR and confirmed by truncation and alanine mutagenesis. Complementing this with mutational analysis of HDAC7, we show that HDAC7, via its surface zinc ion binding site, binds to a 28 residue stretch in SMRT comprising a GSI motif followed by an alpha helix.

  8. Structural and Chemical Characterization of Silica Spheres before and after Modification by Silanization for Trypsin Immobilization

    Directory of Open Access Journals (Sweden)

    Eduardo F. Barbosa


    Full Text Available In the last decades, silica particles of a variety of sizes and shapes have been characterized and chemically modified for several applications, from chromatographic separation to dental supplies. The present study proposes the use of aminopropyl triethoxysilane (APTS silanized silica particles to immobilize the proteolytic enzyme trypsin for the development of a bioreactor. The major advantage of the process is that it enables the polypeptides hydrolysis interruption simply by removing the silica particles from the reaction bottle. Silanized silica surfaces showed significant morphological changes at micro- and nanoscale level. Chemical characterization showed changes in elemental composition, chemical environment, and thermal degradation. Their application as supports for trypsin immobilization showed high immobilization efficiency at reduced immobilization times, combined with more acidic conditions. Indirect immobilization quantification by reversed-phase ultrafast high performance liquid chromatography proved to be a suitable approach due to its high linearity and sensitivity. Immobilized trypsin activities on nonmodified and silanized silica showed promising features (e.g., selective hydrolysis for applications in proteins/peptides primary structure elucidation for proteomics. Silanized silica system produced some preferential targeting peptides, probably due to the hydrophobicity of the nanoenvironment conditioned by silanization.

  9. Fast characterization of gold nanorods ensemble by correlating its structure with optical extinction spectral features

    Directory of Open Access Journals (Sweden)

    Z. J. Hu


    Full Text Available Owing to unique size- and shape- dependent localized surface plasmon resonance (LSPR of noble metal nanoparticles (NPs, the optical extinction spectroscopy method (OES has received much attention to characterize the geometry of metal NPs by fitting experimental UV-vis-NIR spectra. In this work, we aimed to develop a more convenient and accurate OES method to characterize the structural parameters and concentration of the gold nanorods (GNRs ensemble. The main difference between our approach and previous OES methods is that we solve this inverse spectra problem by establishing the LSPR relation equations of GNRs ensemble so that there is no need of UV-vis-NIR spectra fitting process. The aspect ratio (AR and AR distribution can be directly retrieved from two of UV-vis-NIR spectral parameters (peak position and full width at half maximum using the obtained relation equations. Furthermore, the relation equations are modified for applying to the more general GNRs samples by considering the plasmon shift due to the near distance dielectric sensitivity. Finally, instead of inductively coupled plasma mass spectrometry (ICP-MS measurement, we provide a more facile measure of the mass-volume concentration which can be determined from the extinction value at 400 nm. By comparing with the experimental results, it shows that the retrieved results by the relation equations are reliable.

  10. Structural Characterization of Silica Particles Extracted from Grass Stenotaphrum secundatum: Biotransformation via Annelids

    Directory of Open Access Journals (Sweden)

    A. Espíndola-Gonzalez


    Full Text Available This study shows the structural characterization of silica particles extracted from Stenotaphrum secundatum (St. Augustine grass using an annelid-based biotransformation process. This bioprocess starts when St. Augustine grass is turned into humus by vermicompost, and then goes through calcination and acid treatment to obtain silica particles. To determine the effect of the bioprocess, silica particles without biotransformation were extracted directly from the sample of grass. The characterization of the silica particles was performed using Infrared (FTIR and Raman spectroscopy, Transmission Electron Microscopy (TEM, X-ray Diffraction (XRD, Dynamic Light Scattering (DLS, and Energy Dispersion Spectroscopy (EDS. Both types of particles showed differences in morphology and size. The particles without biotransformation were essentially amorphous while those obtained via annelids showed specific crystalline phases. The biological relationship between the metabolisms of worms and microorganisms and the organic-mineral matter causes changes to the particles' properties. The results of this study are important because they will allow synthesis of silica in cheaper and more ecofriendly ways.

  11. Structural characterization of graphite materials prepared from anthracites of different characteristics: a comparative analysis

    Energy Technology Data Exchange (ETDEWEB)

    David Gonzalez; Miguel A. Montes-Moran; Isabel Suarez-Ruiz; Ana B. Garcia [Instituto Nacional del Carbon, CSIC, Oviedo (Spain)


    Graphite materials were prepared from two Spanish anthracites, AF and ATO, by heating at different temperatures within the range 2000-2800{sup o}C. XRD and Raman spectroscopy were employed to characterize the degrees of crystallinity and crystal orientation of the materials. This work also aimed to evaluate the influence of elemental composition, texture (as measured by optical microscopy), and mineral matter of the raw anthracites on their ability to graphitize. Two temperature segments were discerned during the development of crystallinity. The first segment exhibited major improvements in crystal parameters, which afterward reached a plateau value. Raman parameters indicated that further improvement in crystal orientation could be obtained after heating at the highest temperature (2800{sup o}C). The limiting temperature at which the materials showed their highest degree of structural order, i.e., the temperature at which the plateau was reached, was lower for the most graphitizable anthracite (AF). This anthracite was found to have higher hydrogen and mineral matter (specifically Al, Fe, K, and Si) contents. However, the textural anisotropy of this most graphitizable anthracite was lower than that of the other anthracite under study (ATO). Optical microscopy characterization of the carbonized materials showed that this trend changed after heating the anthracites at 1000{sup o}C, i.e., the anisotropy of the texture in the carbonized AF was higher than that of the corresponding carbonized material prepared from ATO. It was concluded that the structural and textural changes of the anthracites during carbonization, which are related with both their microtexture and hydrogen content, influence the graphitization process. 36 refs., 6 figs., 3 tabs.

  12. Manganese ferrite prepared using reverse micelle process: Structural and magnetic properties characterization

    Energy Technology Data Exchange (ETDEWEB)

    Hashim, Mohd, E-mail: [Department of Physics, Aligarh Muslim University, Aligarh 202002 (India); Shirsath, Sagar E. [Spin Device Technology Centre, Department of Engineering, Shinshu University, Nagano 380-8553 (Japan); Meena, S.S. [Solid State Physics Division, Bhabha Atomic Research Centre, Mumbai 400085 (India); Mane, M.L. [Department of Physics, S.G.R.G. Shinde Mahavidyalaya, Paranda 413502, MS (India); Kumar, Shalendra [School of Materials Science and Engineering, Changwon National University, Changwon, Gyeongnam 641-773 (Korea, Republic of); Bhatt, Pramod [Solid State Physics Division, Bhabha Atomic Research Centre, Mumbai 400085 (India); Kumar, Ravi [Centre for Material Science Engineering, National Institute of Technology, Hamirpur, HP (India); Prasad, N.K.; Alla, S.K. [Deptartment of Metallurgical Engineering, Indian Institute of Technology (Banaras Hindu University), Varanasi 221005 (India); Shah, Jyoti; Kotnala, R.K. [National Physical Laboratory (CSIR), Dr. K.S. Krishnan Road, New Delhi 110012 (India); Mohammed, K.A. [Department of Mathematics & Physics Sciences, College of Arts and Sciences, University of Nizwa, Nizwa (Oman); Şentürk, Erdoğan [Department of Physics, Sakarya University, Esentepe, 54187 Sakarya (Turkey); Alimuddin [Department of Physics, Aligarh Muslim University, Aligarh 202002 (India)


    Highlights: • Preparation of Mn{sup 3+} substituted MnFe{sub 2}O{sub 4} ferrite by Reverse microemulsion process. • Characterization by XRD, SEM, VSM, Mössbauer spectroscopy and dielectric measurements techniques. • Magnetic properties of MnFe{sub 2}O{sub 4} enhanced after Mn{sup 3+} substitution. • The dielectric constant and ac conductivity increased with Mn{sup 3+} substitution. - Abstract: Reverse microemulsion process was employed to prepare of nanocrystalline Mn{sup 3+} substituted MnFe{sub 2−x}Mn{sub x}O{sub 4} ferrites. The structural, magnetic and dielectric properties were studied for different concentrations of Mn{sup 3+}. The structural and microstructural properties were analyzed using X-ray diffraction technique (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and Fourier transform infrared (FT-IR) spectroscopy techniques. The phase identification of the materials was studied by Rietveld refined XRD patterns which reveals single phase with cubic symmetry for the samples. The lattice parameters were ranged in between 8.369 and 8.379 Å and do not show any significant change with the substitution of Mn{sup 3+}. The average particles size was found to be around 11 ± 3 nm. Magnetization results obtained from the vibrating sample magnetometer (VSM) confirm that the substitution of Mn{sup 3+} in MnFe{sub 2}O{sub 4} ferrite caused an increase in the saturation magnetization and coercivity. The dependence of Mössbauer parameters on Mn{sup 3+} substitution has been analyzed. Magnetic behavior of the samples were also studied at field cooled (FC) and zero field cooled (ZFC) mode. The dependence of Mössbauer parameters on Mn{sup 3+} substitution was also analyzed. All the magnetic characterization shows that Mn{sup 3+} substitution enhance the magnetic behavior of MnFe{sub 2}O{sub 4} ferrite nanoparticles.

  13. Synthesis and spectroscopic and structural characterization of two novel photoactivatable Ca2+ compounds. (United States)

    Bacchi, Alessia; Carcelli, Mauro; Pelizzi, Corrado; Pelizzi, Giancarlo; Pelagatti, Paolo; Rogolino, Dominga; Tegoni, Matteo; Viappiani, Cristiano


    Two novel photoactivatable Ca(2+) compounds were synthesized to achieve a fast concentration jump of calcium ions in solution; this is of paramount importance for investigating the physiological cellular response. The light-sensitive ligands 4-(2-nitrophenyl)-3,6-dioxaoctane dioic acid (H2L1) and 4-(4,5-dimethoxy-2-nitrophenyl)-3,6-dioxaoctane dioic acid (H2L2) were generated by multistep syntheses, and the corresponding calcium complexes, Ca1 and Ca2, were isolated and characterized. The solution equilibria of H2L1 and H2L2 with Ca2+ were investigated; for both ligands, the formation of a 1:2 Ca2+/ligand species is detected and the complete characterization is presented. The crystal structures of Ca1 and Ca2 were determined. In Ca1 the solid state assembly is attained by a polymeric association of [(CaL1(H2O))2(mu-OH2)] dimeric units. Each calcium ion coordinates four oxygen atoms of one ligand (two ethereal, one carboxylic, and one bridging carboxylic oxygen atom), one water molecule, one bridging water molecule, and a carboxylate group of the other ligand within the dimer. The octacoordination of the metal is completed by an interaction with the adjacent dimeric unit. The crystal structure of the complex Ca2 does not show a polymeric nature, but it is a centrosymmetric dimer. The coordination number of the metal ion is still 8:4 oxygen atoms of the ligand; 3 water molecules; 1 bridging carboxylate group. A preliminary study of the photochemical features of the complexes Ca1 and Ca2 is reported: photoexcitation by a nanosecond pulsed UV laser induces the cleavage of the ligand. This drastically reduces the affinity of the ligand toward Ca2+, which is then released in solution.

  14. Structural and functional characterization of TRI3 trichothecene 15-O-acetyltransferase from Fusarium sporotrichioides

    Energy Technology Data Exchange (ETDEWEB)

    Garvey, Graeme S.; McCormick, Susan P.; Alexander, Nancy J.; Rayment, Ivan; (US-Agriculture); (UW)


    Fusarium head blight is a devastating disease of cereal crops whose worldwide incidence is increasing and at present there is no satisfactory way of combating this pathogen or its associated toxins. There is a wide variety of trichothecene mycotoxins and they all contain a 12,13-epoxytrichothecene skeleton but differ in their substitutions. Indeed, there is considerable variation in the toxin profile across the numerous Fusarium species that has been ascribed to differences in the presence or absence of biosynthetic enzymes and their relative activity. This article addresses the source of differences in acetylation at the C15 position of the trichothecene molecule. Here, we present the in vitro structural and biochemical characterization of TRI3, a 15-O-trichothecene acetyltransferase isolated from F. sporotrichioides and the 'in vivo' characterization of Deltatri3 mutants of deoxynivalenol (DON) producing F. graminearum strains. A kinetic analysis shows that TRI3 is an efficient enzyme with the native substrate, 15-decalonectrin, but is inactive with either DON or nivalenol. The structure of TRI3 complexed with 15-decalonectrin provides an explanation for this specificity and shows that Tri3 and Tri101 (3-O-trichothecene acetyltransferase) are evolutionarily related. The active site residues are conserved across all sequences for TRI3 orthologs, suggesting that differences in acetylation at C15 are not due to differences in Tri3. The tri3 deletion mutant shows that acetylation at C15 is required for DON biosynthesis even though DON lacks a C15 acetyl group. The enzyme(s) responsible for deacetylation at the 15 position of the trichothecene mycotoxins have not been identified.

  15. An in-situ soil structure characterization methodology for measuring soil compaction (United States)

    Dobos, Endre; Kriston, András; Juhász, András; Sulyok, Dénes


    The agricultural cultivation has several direct and indirect effects on the soil properties, among which the soil structure degradation is the best known and most detectable one. Soil structure degradation leads to several water and nutrient management problems, which reduce the efficiency of agricultural production. There are several innovative technological approaches aiming to reduce these negative impacts on the soil structure. The tests, validation and optimization of these methods require an adequate technology to measure the impacts on the complex soil system. This study aims to develop an in-situ soil structure and root development testing methodology, which can be used in field experiments and which allows one to follow the real time changes in the soil structure - evolution / degradation and its quantitative characterization. The method is adapted from remote sensing image processing technology. A specifically transformed A/4 size scanner is placed into the soil into a safe depth that cannot be reached by the agrotechnical treatments. Only the scanner USB cable comes to the surface to allow the image acquisition without any soil disturbance. Several images from the same place can be taken throughout the vegetation season to follow the soil consolidation and structure development after the last tillage treatment for the seedbed preparation. The scanned image of the soil profile is classified using supervised image classification, namely the maximum likelihood classification algorithm. The resulting image has two principal classes, soil matrix and pore space and other complementary classes to cover the occurring thematic classes, like roots, stones. The calculated data is calibrated with filed sampled porosity data. As the scanner is buried under the soil with no changes in light conditions, the image processing can be automated for better temporal comparison. Besides the total porosity each pore size fractions and their distributions can be calculated for

  16. Characterization of synthetic foam structures used to manufacture artificial vertebral trabecular bone. (United States)

    Fürst, David; Senck, Sascha; Hollensteiner, Marianne; Esterer, Benjamin; Augat, Peter; Eckstein, Felix; Schrempf, Andreas


    Artificial materials reflecting the mechanical properties of human bone are essential for valid and reliable implant testing and design. They also are of great benefit for realistic simulation of surgical procedures. The objective of this study was therefore to characterize two groups of self-developed synthetic foam structures by static compressive testing and by microcomputed tomography. Two mineral fillers and varying amounts of a blowing agent were used to create different expansion behavior of the synthetic open-cell foams. The resulting compressive and morphometric properties thus differed within and also slightly between both groups. Apart from the structural anisotropy, the compressive and morphometric properties of the synthetic foam materials were shown to mirror the respective characteristics of human vertebral trabecular bone in good approximation. In conclusion, the artificial materials created can be used to manufacture valid synthetic bones for surgical training. Further, they provide novel possibilities for studying the relationship between trabecular bone microstructure and biomechanical properties. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Structural characterization and cytotoxicity studies of different forms of a combretastatin A4 analogue (United States)

    de Figueiredo, Laysa P.; Ibiapino, Amanda L.; do Amaral, Daniel N.; Ferraz, Letícia S.; Rodrigues, Tiago; Barreiro, Eliezer J.; Lima, Lídia M.; Ferreira, Fabio F.


    It is well known that combretastatin A4 (CA-4), which is a natural stilbene isolated from Combretum caffrum, is used to inhibit angiogenesis. However, depending on the dose administered to the patient, it can cause some side-effects. Herein, we present the synthesis and structural characterization of a novel N-acylhydrazone derivative - LASSBio-1735 - a CA-4 analogue. LASSBio-1735 has displayed in vitro antiproliferative activity against HL-60 (human leukemia), SF-295 (human glioblastoma), MDA-MB435 (melanoma) and HCT-8 (ileocecal adenocarcinoma) tumor cells. We found different hydration levels in two batches of the as-synthesized compound. As a consequence, we could successfully determine the crystal structures - by using X-ray powder diffraction data and a simulated annealing procedure - of the anhydrous and hydrated forms. The effects on cell viability of anhydrous and hydrated forms of LASSBio-1735 were comparatively evaluated in different tumor cell lines, and the hydrated form exhibited higher cytotoxicity in human leukemia K562 cells. These findings lead us to perform a quantitative phase analysis on one of the samples and may shed some light on the search for possible new solvates and/or hydrates.

  18. Report on maloine, a new alkaloid discovered from G. maloi: Structural characterization and biological activity (United States)

    Çela, Dorisa; Nepravishta, Ridvan; Lazari, Diamanto; Gaziano, Roberta; Moroni, Gabriella; Pica, Francesca; Paci, Maurizio; Abazi, Sokol


    Gymnospermium maloi Kit Tan, & Shuka is a new endemic species of the genus Gymnospermium Spach which has been described recently from the southern part of Albania. The members of this genus are poorly studied for what it concern the secondary metabolites in general and the class of alkaloids in particular. In fact from Gymnospermium genus, there are only few alkaloids characterized, (namely albertramine, albertidine, and albertine) isolated from G. albertii. Until now the chemical composition and the structure elucidation of other possible secondary metabolites, especially alkaloids, remain largely unknown. Here we report, for the first time, the structure of a new alkaloid isolated from G. maloi, designated by us as maloine, and obtained by the use of 2D homonuclear and heteronuclear NMR spectroscopy, FTIR, UV, Fluorescence and HPLC/MS spectra. The biological activity of the crude extract of Gymnospermium maloi and of its alkaloid maloine, was evaluated in vitro on human chronic myeloid leukemia cell line K562 and results herewith reported.

  19. Structural characterization of Fe−Pd nanowires grown by electrodeposition using an acid electrolyte

    Energy Technology Data Exchange (ETDEWEB)

    Domenichini, P. [Instituto Balseiro, Universidad Nacional de Cuyo, Av. Bustillo 9500, 8400 San Carlos de Bariloche (Argentina); Condó, A.M. [Instituto Balseiro, Universidad Nacional de Cuyo, Av. Bustillo 9500, 8400 San Carlos de Bariloche (Argentina); Centro Atómico Bariloche, Comisión Nacional de Energía Atómica, Av. Bustillo 9500, 8400 San Carlos de Bariloche (Argentina); Haberkorn, N., E-mail: [Instituto Balseiro, Universidad Nacional de Cuyo, Av. Bustillo 9500, 8400 San Carlos de Bariloche (Argentina); Centro Atómico Bariloche, Comisión Nacional de Energía Atómica, Av. Bustillo 9500, 8400 San Carlos de Bariloche (Argentina)


    Fe{sub 70}Pd{sub 30} nanostructures have potential application in actuators due to their conventional and magnetic shape memory. Here, we report the microstructure of electrodeposition grown Fe−Pd nanowires in which the process was confined to polycarbonate membranes with a nominal pore diameter of 200 nm. We used an acid electrolyte (pH ≈ 5) in which the solution was stabilized with sulfosalicylic acid. The average chemical concentration of the nanowires can be systematically shifted from rich palladium to rich iron by changing the growth potential. The study of the microstructure by transmission electron microscopy indicates high chemical inhomogeneities due to phase coexistence between rich palladium regions (with FCC structure) and rich iron regions. The latter present a combination of BCC and amorphous phases. The average chemical composition of the nanowires can be better adjusted by using a low frequency square wave voltage excitation (alternating rich Pd and rich Fe regions). However, independently of the growth process, the nanowires morphology collapses after thermal annealing. This could be ascribed to fragile grain boundaries due to the presence of amorphous hydroxides and chemical impurities produced during the electrochemical process. - Highlights: • Synthesis of Fe−Pd nanowires by electrodeposition is reported. • Structural characterization of the nanowires by transmission electron microscopy. • The synthesis of nanowires with austenitic phase is limited by fragile grain boundaries.

  20. Characterization of dipeptidylcarboxypeptidase of Leishmania donovani: a molecular model for structure based design of antileishmanials (United States)

    Baig, Mirza Saqib; Kumar, Ashutosh; Siddiqi, Mohammad Imran; Goyal, Neena


    Leishmania donovani dipeptidylcarboxypeptidsae (LdDCP), an angiotensin converting enzyme (ACE) related metallopeptidase has been identified and characterized as a putative drug target for antileishmanial chemotherapy. The kinetic parameters for LdDCP with substrate, Hip-His-Leu were determined as, Km, 4 mM and Vmax, 1.173 μmole/ml/min. Inhibition studies revealed that known ACE inhibitors (captopril and bradykinin potentiating peptide; BPP1) were weak inhibitors for LdDCP as compared to human testicular ACE (htACE) with Ki values of 35.8 nM and 3.9 μM, respectively. Three dimensional model of LdDCP was generated based on crystal structure of Escherichia coli DCP (EcDCP) by means of comparative modeling and assessed using PROSAII, PROCHECK and WHATIF. Captopril docking with htACE, LdDCP and EcDCP and analysis of molecular electrostatic potentials (MEP) suggested that the active site domain of three enzymes has several minor but potentially important structural differences. These differences could be exploited for designing selective inhibitor of LdDCP thereby antileishmanial compounds either by denovo drug design or virtual screening of small molecule databases.

  1. Synthesize and characterization of graphene nanosheets with high surface area and nano-porous structure

    Energy Technology Data Exchange (ETDEWEB)

    Jabari Seresht, Razieh [Nanotechnology Research Institute, School of Chemical Engineering, Babol University of Technology (Iran, Islamic Republic of); Jahanshahi, Mohsen, E-mail: [Nanotechnology Research Institute, School of Chemical Engineering, Babol University of Technology (Iran, Islamic Republic of); Rashidi, Alimorad [Nanotechnology Research Center, Research Institute of Petroleum Industry, Tehran (Iran, Islamic Republic of); Ghoreyshi, Ali Asghar [Nanotechnology Research Institute, School of Chemical Engineering, Babol University of Technology (Iran, Islamic Republic of)


    A few-layer graphene was obtained by the expansion and exfoliation of water-intercalated graphene oxide via heat treatment in nitrogen environment in the temperature range of 200–1000 °C. Graphene which was synthesized at 800 °C (GT800) had a higher quality than other temperatures. This graphene has a high specific surface area (560.6 m{sup 2} g{sup −1}) and nano-porous structure. However, as for the purpose of comparison, graphene was synthesized with a colloidal suspension of exfoliated graphene oxide sheets in water with hydrazine hydrate in various reaction times (12, 24 and 36 h). This method has obtained a six-layer graphene and graphene that was synthesized during 24 h reaction with hydrazine hydrate (GC24) had a higher quality in comparison with the other products. The GC24 had 195.97 m{sup 2} g{sup −1} specific surface area and nano-porous structure. The as-synthesized graphene were then characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, Raman spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy (SEM) as well as BET measurements. The results demonstrated that this low-cost method for few-layer grapheme, e.g. three-layers, fabrication is reliable and promising.

  2. Structural and Electrical Characterization of Oxidated, Nitridated and Oxi-nitridated (100) GaAs Surfaces (United States)

    Paul, Narayan Chandra; Nakamura, Kazuki; Takebe, Masahide; Takemoto, Akira; Inokuma, Takao; Iiyama, Koichi; Takamiya, Saburo; Higashimine, Koichi; Ohtsuka, Nobuo; Yonezawa, Yasuto


    Oxidation by the UV & ozone process, nitridation by the nitrogen helicon-wave-excited plasma process, and the combination of these processes are applied to (100) GaAs wafers. An atomic force microscope, X-ray photoelectron spectroscopy, a transmission electron microscope, photoluminescence and electrical characteristics (current-voltage and capacitance-voltage) were used to analyze the influences of these processes on the structure and composition of the surfaces and the interfaces. Metal-insulator-semiconductor (MIS) diodes and Schottky diodes were fabricated in order to investigate the electrical influences of these processes. The oxidation slightly disorders GaAs surfaces. Nitridation of a bare surface creates about a 2-nm-thick strongly disordered layer, which strongly deteriorates the electrical and photoluminescence characteristics. Nitridation of oxidated wafers (oxi-nitridation) forms firm amorphous GaON layers, which contain GaN, with very flat and sharp GaON/GaAs interfaces, where crystal disorder is hardly observed. It improves the current-voltage (I-V) and capacitance-voltage (C-V) characteristics and the photoluminescence intensity. Results of the structural and the electrical characterizations qualitatively coincide well with each other.

  3. Structural, vibrational and thermal characterization of phase transformation in L-histidinium bromide monohydrate single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Moura, G.M. [Universidade Federal do Maranhão, CCSST, Imperatriz, MA, 65900-410 (Brazil); Universidade Federal do Sul e Sudeste do Pará, ICEN, Marabá, PA 68505-080 (Brazil); Carvalho, J.O. [Universidade Federal do Maranhão, CCSST, Imperatriz, MA, 65900-410 (Brazil); Instituto Federal do Tocantins, Araguaína, TO, 77.826-170 (Brazil); Silva, M.C.D.; Façanha Filho, P.F. [Universidade Federal do Maranhão, CCSST, Imperatriz, MA, 65900-410 (Brazil); Santos, A.O. dos, E-mail: [Universidade Federal do Maranhão, CCSST, Imperatriz, MA, 65900-410 (Brazil)


    L-Histidinium bromide monohydrate (LHBr) single crystal is a nonlinear optical material. In this work the high temperature phase transformation and the thermal stability of single crystals of LHBr was investigated by X-ray diffraction, thermogravimetric analysis, differential thermal analysis, differential scanning calorimetry and Raman spectroscopy. The results showed the LHBr phase transformation of orthorhombic (P2{sub 1}2{sub 1}2{sub 1}) to monoclinic system (P 1 2 1) at 120 °C, with the lattice parameters a = 12.162(1) Å, b = 16.821(2) Å, c = 19.477(2) Å and β = 108.56(2)°. These techniques are complementary and confirm the structural phase transformation due to loss water of crystallization. - Highlights: • -histidinium bromide single crystal was grown by slow evaporation technique. • X-ray diffraction characterize the high-temperature phase transformation. • The structural phase transformation occur due to loss of water of crystallization. • The LHBr thermal expansion coefficients exhibit an anisotropic behavior.

  4. Structural characterization of the NAP; the major adhesion complex of the human pathogen Mycoplasma genitalium. (United States)

    Scheffer, Margot P; Gonzalez-Gonzalez, Luis; Seybert, Anja; Ratera, Mercè; Kunz, Michael; Valpuesta, José M; Fita, Ignacio; Querol, Enrique; Piñol, Jaume; Martín-Benito, Jaime; Frangakis, Achilleas S


    Mycoplasma genitalium, the causative agent of non-gonococcal urethritis and pelvic inflammatory disease in humans, is a small eubacterium that lacks a peptidoglycan cell wall. On the surface of its plasma membrane is the major surface adhesion complex, known as NAP that is essential for adhesion and gliding motility of the organism. Here, we have performed cryo-electron tomography of intact cells and detergent permeabilized M. genitalium cell aggregates, providing sub-tomogram averages of free and cell-attached NAPs respectively, revealing a tetrameric complex with two-fold rotational (C2) symmetry. Each NAP has two pairs of globular lobes (named α and β lobes), arranged as a dimer of heterodimers with each lobe connected by a stalk to the cell membrane. The β lobes are larger than the α lobes by 20%. Classification of NAPs showed that the complex can tilt with respect to the cell membrane. A protein complex containing exclusively the proteins P140 and P110, was purified from M. genitalium and was structurally characterized by negative-stain single particle EM reconstruction. The close structural similarity found between intact NAPs and the isolated P140/P110 complexes, shows that dimers of P140/P110 heterodimers are the only components of the extracellular region of intact NAPs in M. genitalium. © 2017 John Wiley & Sons Ltd.

  5. Physiochemical Characterization of Iodine (V Oxide Part II: Morphology and Crystal Structure of Particulate Films

    Directory of Open Access Journals (Sweden)

    Brian K. Little


    Full Text Available In this study, the production of particulate films of iodine (V oxides is investigated. The influence that sonication and solvation of suspended particles in various alcohol/ketone/ester solvents have on the physical structure of spin or drop cast films is examined in detail with electron microscopy, powder x-ray diffraction, and UV-visible absorption spectroscopy. Results indicate that sonicating iodine oxides in alcohol mixtures containing trace amounts of water decreases deposited particle sizes and produces a more uniform film morphology. UV-visible spectra of the pre-cast suspensions reveal that for some solvents, the iodine oxide oxidizes the solvent, producing I2 and lowering the pH of the suspension. Characterizing the crystals within the cast films reveal their composition to be primarily HI3O8, their orientations to exhibit a preferential orientation, and their growth to be primarily along the ac-plane of the crystal, enhanced at higher spin rates. Spin-coating at lower spin rates produces laminate-like particulate films versus higher density, one-piece films of stacked particles produced by drop casting. The particle morphology in these films consists of a combination of rods, plates, cubes, and rhombohedra structure.

  6. Distorted tetrahedral nickel-nitrosyl complexes: spectroscopic characterization and electronic structure. (United States)

    Soma, Shoko; Van Stappen, Casey; Kiss, Mercedesz; Szilagyi, Robert K; Lehnert, Nicolai; Fujisawa, Kiyoshi


    The linear nickel-nitrosyl complex [Ni(NO)(L3)] supported by a highly hindered tridentate nitrogen-based ligand, hydrotris(3-tertiary butyl-5-isopropyl-1-pyrazolyl)borate (denoted as L3), was prepared by the reaction of the potassium salt of the ligand with the nickel-nitrosyl precursor [Ni(NO)(Br)(PPh 3 ) 2 ]. The obtained nitrosyl complexes as well as the corresponding chlorido complexes [Ni(NO)(Cl)(PPh 3 ) 2 ] and [Ni(Cl)(L3)] were characterized by X-ray crystallography and different spectroscopic methods including IR/far-IR, UV-Vis, NMR, and multi-edge X-ray absorption spectroscopy at the Ni K-, Ni L-, Cl K-, and P K-edges. For comparative electronic structure analysis we also performed DFT calculations to further elucidate the electronic structure of [Ni(NO)(L3)]. These results provide the nickel oxidation state and the character of the Ni-NO bond. The complex [Ni(NO)(L3)] is best described as [Ni (II) (NO (-) )(L3)], and the spectroscopic results indicate that the phosphane complexes have a similar [Ni (II) (NO (-) )(X)(PPh 3 ) 2 ] ground state.

  7. Characterization of internal structure of hydrated agar and gelatin matrices by cryo-SEM

    KAUST Repository

    Rahbani, Janane


    There has been a considerable interest in recent years in developing polymer gel matrices for many important applications such as 2DE for quantization and separation of a variety of proteins and drug delivery system to control the release of active agents. However, a well-defined knowledge of the ultrastructures of the gels has been elusive. In this study, we report the characterization of two different polymers used in 2DE: Gelatin, a naturally occurring polymer derived from collagen (protein) and agar, a polymer of polysaccharide (sugar) origin. Low-temperature SEM is used to examine the internal structure of these gels in their frozen natural hydrated states. Results of this study show that both polymers have an array of hollow cells that resembles honeycomb structures. While agar pores are almost circular, the corresponding Gaussian curve is very broad exhibiting a range of radii from nearly 370 to 700 nm. Gelatin pores are smaller and more homogeneous reflecting a narrower distribution from nearly 320 to 650 nm. Overall, these ultrastructural findings could be used to correlate with functions of the polymers. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Structural and Functional Characterization of Malate Synthase G from Opportunistic Pathogen Pseudomonas aeruginosa. (United States)

    McVey, Alyssa C; Medarametla, Prasanthi; Chee, Xavier; Bartlett, Sean; Poso, Antti; Spring, David R; Rahman, Taufiq; Welch, Martin


    Pseudomonas aeruginosa is an opportunistic human pathogen recognized as a critical threat by the World Health Organization because of the dwindling number of effective therapies available to treat infections. Over the past decade, it has become apparent that the glyoxylate shunt plays a vital role in sustaining P. aeruginosa during infection scenarios. The glyoxylate shunt comprises two enzymes: isocitrate lyase and malate synthase isoform G. Inactivation of these enzymes has been reported to abolish the ability of P. aeruginosa to establish infection in a mammalian model system, yet we still lack the structural information to support drug design efforts. In this work, we describe the first X-ray crystal structure of P. aeruginosa malate synthase G in the apo form at 1.62 Å resolution. The enzyme is a monomer composed of four domains and is highly conserved with homologues found in other clinically relevant microorganisms. It is also dependent on Mg(2+) for catalysis. Metal ion binding led to a change in the intrinsic fluorescence of the protein, allowing us to quantitate its affinity for Mg(2+). We also identified putative drug binding sites in malate synthase G using computational analysis and, because of the high resolution of the experimental data, were further able to characterize its hydration properties. Our data reveal two promising binding pockets in malate synthase G that may be exploited for drug design.

  9. Structural characterization and evaluation of prebiotic activity of oil palm kernel cake mannanoligosaccharides. (United States)

    Kalidas, Naveena Reddy; Saminathan, Mookiah; Ismail, Intan Safinar; Abas, Faridah; Maity, Prasenjit; Islam, Syed Sirajul; Manshoor, Nurhuda; Shaari, Khozirah


    In this study, mannanoligosaccharides (MOS) were isolated from palm kernel cake by aqueous extraction using high temperature and pressure. Structural characterization of MOS was carried out using acid hydrolysis, methylation analysis, ESI-MS/MS and 1D/2D NMR. The prebiotic activity of MOS was evaluated in vitro using two probiotic Lactobacillus strains. Sugar analysis indicated the presence of mannose in each of the oligomers. Methylation and 1D/2D NMR analysis indicated that the MOS have a linear structure consisting of (1→4)-β-d-mannopyranosyl residues. ESI-MS/MS results showed that the isolated mannan oligomers, MOS-III, MOS-IV, MOS-V and MOS-VI consist of tetra-, penta-, hexa-, and hepta-saccharides with molecular weights of 689, 851, 1013 and 1151Da, respectively. Based on the in vitro growth study, MOS-III and MOS-IV was found to be effective in selectively promoting the growth of Lactobacillus reuteri C1 strain as evidenced by the optical density of the culture broth. Copyright © 2017 Elsevier Ltd. All rights reserved.

  10. Structural Characterization of Whirlin Reveals an Unexpected and Dynamic Supramodule Conformation of Its PDZ Tandem. (United States)

    Delhommel, Florent; Cordier, Florence; Bardiaux, Benjamin; Bouvier, Guillaume; Colcombet-Cazenave, Baptiste; Brier, Sébastien; Raynal, Bertrand; Nouaille, Sylvie; Bahloul, Amel; Chamot-Rooke, Julia; Nilges, Michael; Petit, Christine; Wolff, Nicolas


    Hearing relies on the transduction of sound-evoked vibrations into electric signals, occurring in the stereocilia bundle of hair cells. The bundle is organized in a staircase pattern formed by rows of packed stereocilia. This architecture is pivotal to transduction and involves a network of scaffolding proteins with hitherto uncharacterized features. Key interactions in this network are mediated by PDZ domains. Here, we describe the architecture of the first two PDZ domains of whirlin, a protein involved in these assemblies and associated with congenital deaf-blindness. C-terminal hairpin extensions of the PDZ domains mediate the transient supramodular assembly, which improves the binding capacity of the first domain. We determined a detailed structural model of the closed conformation of the PDZ tandem and characterized its equilibrium with an ensemble of open conformations. The structural and dynamic behavior of this PDZ tandem provides key insights into the regulatory mechanisms involved in the hearing machinery. Copyright © 2017 Elsevier Ltd. All rights reserved.

  11. Biochemical and Structural Characterization of Enolase from Chloroflexus aurantiacus: Evidence for a Thermophilic Origin. (United States)

    Zadvornyy, Oleg A; Boyd, Eric S; Posewitz, Matthew C; Zorin, Nikolay A; Peters, John W


    Enolase catalyzes the conversion of 2-phosphoglycerate to phosphoenolpyruvate during both glycolysis and gluconeogenesis, and is required by all three domains of life. Here, we report the purification and biochemical and structural characterization of enolase from Chloroflexus aurantiacus, a thermophilic anoxygenic phototroph affiliated with the green non-sulfur bacteria. The protein was purified as a homodimer with a subunit molecular weight of 46 kDa. The temperature optimum for enolase catalysis was 80°C, close to the measured thermal stability of the protein which was determined to be 75°C, while the pH optimum for enzyme activity was 6.5. The specific activities of purified enolase determined at 25 and 80°C were 147 and 300 U mg(-1) of protein, respectively. K m values for the 2-phosphoglycerate/phosphoenolpyruvate reaction determined at 25 and 80°C were 0.16 and 0.03 mM, respectively. The K m values for Mg(2+) binding at these temperatures were 2.5 and 1.9 mM, respectively. When compared to enolase from mesophiles, the biochemical and structural properties of enolase from C. aurantiacus are consistent with this being thermally adapted. These data are consistent with the results of our phylogenetic analysis of enolase, which reveal that enolase has a thermophilic origin.

  12. Biochemical and Structural Characterization of Enolase from Chloroflexus aurantiacus: Evidence for a Thermophilic Origin

    Directory of Open Access Journals (Sweden)

    Oleg A Zadvornyy


    Full Text Available Enolase catalyzes the conversion of 2-phosphoglycerate to phosphoenolpyruvate during both glycolysis and gluconeogenesis and is required by all three domains of life. Here, we report the purification and biochemical and structural characterization of enolase from Chloroflexus aurantiacus, a thermophilic andanoxygenic phototroph affiliated with the green non-sulfur bacteria. The protein was purified as a homodimer with a subunit molecular weight of 46 kDa. The temperature optimum for enolase catalysis was 80°C, close to the measured thermal stability of the protein which was determined to be 75°C, while the pH optimum for enzyme activity was 6.5. The specific activities of purified enolase determined at 25°C and 80°C were 147 and 300 units/mg of protein, respectively. Km values for the 2-phosphoglycerate/phosphoenolpyruvate reaction determined at 25°C and 80°C were 0.16 mM and 0.03 mM, respectively. The Km values for Mg2+ binding at these temperatures were 2.5 mM and 1.9 mM, respectively. When compared to enolase from mesophiles, the biochemical and structural properties of enolase from C. aurantiacus are consistent with this being thermally adapted. This data is consistent with the results of our phylogenetic analysis of enolase, which reveal that enolase has a thermophilic origin.

  13. Structural characterization of the entire 1.3S subunit of transcarboxylase from Propionibacterium shermanii. (United States)

    Reddy, D V; Rothemund, S; Shenoy, B C; Carey, P R; Sönnichsen, F D


    Transcarboxylase (TC) from Propionibacterium shermanii, a biotin-dependent enzyme, catalyzes the transfer of a carboxyl group from methylmalonyl-CoA to pyruvate in two partial reactions. Within the multisubunit enzyme complex, the 1.3S subunit functions as the carboxyl group carrier. The 1.3S is a 123-amino acid polypeptide (12.6 kDa), to which biotin is covalently attached at Lys 89. We have expressed 1.3S in Escherichia coli with uniform 15N labeling. The backbone structure and dynamics of the protein have been characterized in aqueous solution by three-dimensional heteronuclear nuclear magnetic resonance (NMR) spectroscopy. The secondary structure elements in the protein were identified based on NOE information, secondary chemical shifts, homonuclear 3J(HNHalpha) coupling constants, and amide proton exchange data. The protein contains a predominantly disordered N-terminal half, while the C-terminal half is folded into a compact domain comprising eight beta-strands connected by short loops and turns. The topology of the C-terminal domain is consistent with the fold found in both carboxyl carrier and lipoyl domains, to which this domain has approximately 26-30% sequence similarity.

  14. Synthesis, growth, structural characterization, Hirshfeld analysis and nonlinear optical studies of a methyl substituted chalcone (United States)

    Prabhu, Shobha R.; Jayarama, A.; Chandrasekharan, K.; Upadhyaya, V.; Ng, Seik Weng


    A new chalcone compound (2E)-3-(3-methylphenyl)-1-(4-nitrophenyl)prop-2-en-1-one (3MPNP) with molecular formula C16H13NO3 has been synthesized and crystallized by slow solvent evaporation technique. The Fourier transform infrared, Fourier transform Raman and nuclear magnetic resonance techniques were used for structural characterization. UV-visible absorption studies were carried out to study the transparency of the crystal in the visible region. Differential scanning calorimetry study shows thermal stability of crystals up to temperature 122 °C. Single crystal X-ray diffraction and powder X-ray diffraction techniques were used to study crystal structure and cell parameters. The Hirshfeld surface and 2-D fingerprint analysis were performed to study the nature of interactions and their quantitative contributions towards the crystal packing. The third order non-linear optical properties have been studied using single beam Z-scan technique and the results show that the material is a potential candidate for optical device applications such as optical limiters and optical switches.

  15. Mechanical characterization of micro/nanoscale structures for MEMS/NEMS applications using nanoindentation techniques. (United States)

    Li, Xiaodong; Bhushan, Bharat; Takashima, Kazuki; Baek, Chang-Wook; Kim, Yong-Kweon


    Mechanical properties of micro/nanoscale structures are needed to design reliable micro/nanoelectromechanical systems (MEMS/NEMS). Micro/nanomechanical characterization of bulk materials of undoped single-crystal silicon and thin films of undoped polysilicon, SiO(2), SiC, Ni-P, and Au have been carried out. Hardness, elastic modulus and scratch resistance of these materials were measured by nanoindentation and microscratching using a nanoindenter. Fracture toughness was measured by indentation using a Vickers indenter. Bending tests were performed on the nanoscale silicon beams, microscale Ni-P and Au beams using a depth-sensing nanoindenter. It is found that the SiC film exhibits higher hardness, elastic modulus and scratch resistance as compared to other materials. In the bending tests, the nanoscale Si beams failed in a brittle manner with a flat fracture surface. The notched Ni-P beam showed linear deformation behavior followed by abrupt failure. The Au beam showed elastic-plastic deformation behavior. FEM simulation can well predict the stress distribution in the beams studied. The nanoindentation, scratch and bending tests used in this study can be satisfactorily used to evaluate the mechanical properties of micro/nanoscale structures for use in MEMS/NEMS.

  16. Physical, Structural, Barrier, and Antifungal Characterization of Chitosan–Zein Edible Films with Added Essential Oils

    Directory of Open Access Journals (Sweden)

    Monserrat Escamilla-García


    Full Text Available Edible films (EFs have gained great interest due to their ability to keep foods safe, maintaining their physical and organoleptic properties for a longer time. The aim of this work was to develop EFs based on a chitosan–zein mixture with three different essential oils (EOs added: anise, orange, and cinnamon, and to characterize them to establish the relationship between their structural and physical properties. The addition of an EO into an EF significantly affected (p < 0.05 the a* (redness/greenness and b* (yellowness/blueness values of the film surface. The EFs presented a refractive index between 1.35 and 1.55, and thus are classified as transparent. The physical properties of EFs with an added EO were improved, and films that incorporated the anise EO showed significantly lower water vapor permeability (1.2 ± 0.1 g mm h−1 m−2 kPa−1 and high hardness (104.3 ± 3.22 MPa. EFs with an added EO were able to inhibit the growth of Penicillium sp. and Rhizopus sp. to a larger extent than without an EO. Films’ structural changes were the result of chemical interactions among amino acid side chains from zein, glucosamine from chitosan, and cinnamaldehyde, anethole, or limonene from the EOs as detected by a Raman analysis. The incorporation of an EO in the EFs’ formulation could represent an alternative use as coatings to enhance the shelf life of food products.

  17. Structural characterization of CAS SH3 domain selectivity and regulation reveals new CAS interaction partners. (United States)

    Gemperle, Jakub; Hexnerová, Rozálie; Lepšík, Martin; Tesina, Petr; Dibus, Michal; Novotný, Marian; Brábek, Jan; Veverka, Václav; Rosel, Daniel


    CAS is a docking protein downstream of the proto-oncogene Src with a role in invasion and metastasis of cancer cells. The CAS SH3 domain is indispensable for CAS-mediated signaling, but structural aspects of CAS SH3 ligand binding and regulation are not well understood. Here, we identified the consensus CAS SH3 binding motif and structurally characterized the CAS SH3 domain in complex with ligand. We revealed the requirement for an uncommon centrally localized lysine residue at position +2 of CAS SH3 ligands and two rather dissimilar optional anchoring residues, leucine and arginine, at position +5. We further expanded the knowledge of CAS SH3 ligand binding regulation by manipulating tyrosine 12 phosphorylation and confirmed the negative role of this phosphorylation on CAS SH3 ligand binding. Finally, by exploiting the newly identified binding requirements of the CAS SH3 domain, we predicted and experimentally verified two novel CAS SH3 binding partners, DOK7 and GLIS2.

  18. Synthesis, structural and magnetic characterization of soft magnetic nanocrystalline ternary FeNiCo particles

    Energy Technology Data Exchange (ETDEWEB)

    Toparli, Cigdem [Department of Metallurgical & Materials Eng., Istanbul Technical University, 34469 Istanbul (Turkey); Max-Planck-Institut für Eisenforschung GmbH, Düsseldorf (Germany); Ebin, Burçak [Department of Metallurgical & Materials Eng., Istanbul Technical University, 34469 Istanbul (Turkey); Nuclear Chemistry and Industrial Material Recycling, Department of Chemistry and Chemical Engineering, Chalmers University of Technology, S-412 96 Gothenburg (Sweden); Gürmen, Sebahattin, E-mail: [Department of Metallurgical & Materials Eng., Istanbul Technical University, 34469 Istanbul (Turkey)


    The present study focuses on the synthesis, microstructural and magnetic properties of ternary FeNiCo nanoparticles. Nanocrystalline ternary FeNiCo particles were synthesized via hydrogen reduction assisted ultrasonic spray pyrolysis method in single step. The effect of precursor concentration on the morphology and the size of particles was investigated. The syntheses were performed at 800 °C. Structure, morphology and magnetic properties of the as-prepared products were characterized through X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM) studies. Scherer calculation revealed that crystallite size of the ternary particles ranged between 36 and 60 nm. SEM and TEM investigations showed that the particle size was strongly influenced by the precursor concentration and Fe, Ni, Co elemental composition of individual particles was homogeneous. Finally, the soft magnetic properties of the particles were observed to be a function of their size. - Highlights: • Ternary FeNiCo alloy nanocrystalline particles were synthesized in a single step. • Cubic crystalline structure and spherical morphology was observed by XRD, SEM and TEM investigations. • The analysis of magnetic properties indicates the soft magnetic features of particles.

  19. Non-Linear Structural Dynamics Characterization using a Scanning Laser Vibrometer (United States)

    Pai, P. F.; Lee, S.-Y.


    This paper presents the use of a scanning laser vibrometer and a signal decomposition method to characterize non-linear dynamics of highly flexible structures. A Polytec PI PSV-200 scanning laser vibrometer is used to measure transverse velocities of points on a structure subjected to a harmonic excitation. Velocity profiles at different times are constructed using the measured velocities, and then each velocity profile is decomposed using the first four linear mode shapes and a least-squares curve-fitting method. From the variations of the obtained modal \\ielocities with time we search for possible non-linear phenomena. A cantilevered titanium alloy beam subjected to harmonic base-excitations around the second. third, and fourth natural frequencies are examined in detail. Influences of the fixture mass. gravity. mass centers of mode shapes. and non-linearities are evaluated. Geometrically exact equations governing the planar, harmonic large-amplitude vibrations of beams are solved for operational deflection shapes using the multiple shooting method. Experimental results show the existence of 1:3 and 1:2:3 external and internal resonances. energy transfer from high-frequency modes to the first mode. and amplitude- and phase- modulation among several modes. Moreover, the existence of non-linear normal modes is found to be questionable.

  20. Physical characterization of icosahedral virus ultra structure, stability, and integrity using electrospray differential mobility analysis. (United States)

    Pease, Leonard F; Tsai, De-Hao; Brorson, Kurt A; Guha, Suvajyoti; Zachariah, Michael R; Tarlov, Michael J


    We present a rapid and quantitative method to physically characterize the structure and stability of viruses. Electrospray differential mobility analysis (ES-DMA) is used to determine the size of capsomers (i.e., hexons) and complete capsids. We demonstrate how to convert the measured mobility size into the icosahedral dimensions of a virus, which for PR772 become 68.4 nm for vertex-to-vertex, 54.4 nm for facet-to-facet, and 58.2 nm for edge-to-edge lengths, in reasonable agreement with dimensions from transmission electron microscopy for other members of the family Tectiviridae (e.g., PRD1). These results indicate ES-DMA's mobility diameter most closely approximates the edge-to-edge length. Using PR772's edge length (36.0 nm) and the size of the major capsid hexon (≈8.4 nm) from ES-DMA with icosahedral geometry, PR772's T = 25 symmetry is confirmed and the number of proteins in the capsid shell is determined. We also demonstrate the use of ES-DMA to monitor the temporal disintegration of PR772, the thermal degradation of PP7, and the appearance of degradation products, essential to viral stability assays. These results lay groundwork essential for the use of ES-DMA for a variety of applications including monitoring of vaccine and gene therapy vector products, confirmation of viral inactivation, and theoretical studies of self-assembling macromolecular structures.

  1. Preparation and structural characterization of corn starch-aroma compound inclusion complexes. (United States)

    Zhang, Shu; Zhou, Yibin; Jin, Shanshan; Meng, Xin; Yang, Liping; Wang, Haisong


    Six corn starch inclusion complexes were synthesized using small nonpolar or weak polar aroma compounds (heptanolide, carvone and menthone) and small polar aroma compounds (linalool, heptanol and menthol). The objectives of this study were to (a) investigate the ability of corn starch to form inclusion complexes with these aroma compounds and (b) characterize the structure of the corn starch inclusion complexes. The resulting inclusion ratios were 75.6, 36.9, 43.8, 91.9, 67.2 and 54.7% for heptanolide, carvone, menthone, linalool, heptanol and menthol respectively. The inclusion complexes had laminated structures with a certain amount of holes or blocky constructions. Compared with gelatinized corn starch, the transition temperatures, peak temperatures and enthalpies of the inclusion complexes were significantly different. The major peak of CO at 1771 cm-1 and significant peak shifts revealed the formation of inclusion complexes. X-ray diffractometry (XRD) analyses revealed that the crystallinity of corn starch-polar aroma compound inclusion complexes increased. Based on cross-polarization magic angle spinning 13 C nuclear magnetic resonance (CP-MAS 13 C NMR) results, novel peaks and chemical shifts were attributed to the presence of small aroma compounds, thereby confirming the formation of corn starch inclusion complexes. Small nonpolar and polar aroma compounds can be complexed to corn starch. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

  2. Controllable synthesis and characterization of novel copper-carbon core-shell structured nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Zhai, Jing [Sin-China Nano Technology Center, Key Lab for Nanomaterials, Ministry of Education, Beijing University of Chemical Technology, Beijing 100029 (China); Research Center of the Ministry of Education for High Gravity Engineering and Technology, Beijing University of Chemical Technology, No. 15 Beisanhuan Dong Lu, Beijing 100029 (China); Tao, Xia; Pu, Yuan; Zeng, Xiao-Fei [Sin-China Nano Technology Center, Key Lab for Nanomaterials, Ministry of Education, Beijing University of Chemical Technology, Beijing 100029 (China); Chen, Jian-Feng, E-mail: [Research Center of the Ministry of Education for High Gravity Engineering and Technology, Beijing University of Chemical Technology, No. 15 Beisanhuan Dong Lu, Beijing 100029 (China)


    Highlights: {yields} We reported a facile, green and cheap hydrothermal method to obtain novel copper-carbon core-shell nanoparticles. {yields} The as-formed particles with controllable size and morphology are antioxidant. {yields} The particles with organic-group-loaded surfaces and protective shells are expected to be applied in fields of medicine, electronics, sensors and lubricant. -- Abstract: A facile hydrothermal method was developed for preparing copper-carbon core-shell structured particles through a reaction at 160 {sup o}C in which glucose, copper sulfate pentahydrate and cetyltrimethylammonium bromide were used as starting materials. The original copper-carbon core-shell structured particles obtained were sized of 100-250 nm. The thickness of carbonaceous shells was controlled ranging from 25 to 100 nm by adjusting the hydrothermal duration time and the concentrations of glucose in the process. Products were characterized with transmission electron microscopy, X-ray diffraction, energy dispersive spectroscopy, Fourier transform infrared spectroscopy. Since no toxic materials were involved in the preparation, particles with stable carbonaceous framework and reactive surface also showed promising applications in medicine, electronics, sensors, lubricant, etc.

  3. Functional and Structural Characterization of a (+)-Limonene Synthase from Citrus sinensis. (United States)

    Morehouse, Benjamin R; Kumar, Ramasamy P; Matos, Jason O; Olsen, Sarah Naomi; Entova, Sonya; Oprian, Daniel D


    Terpenes make up the largest and most diverse class of natural compounds and have important commercial and medical applications. Limonene is a cyclic monoterpene (C 10 ) present in nature as two enantiomers, (+) and (-), which are produced by different enzymes. The mechanism of production of the (-)-enantiomer has been studied in great detail, but to understand how enantiomeric selectivity is achieved in this class of enzymes, it is important to develop a thorough biochemical description of enzymes that generate (+)-limonene, as well. Here we report the first cloning and biochemical characterization of a (+)-limonene synthase from navel orange (Citrus sinensis). The enzyme obeys classical Michaelis-Menten kinetics and produces exclusively the (+)-enantiomer. We have determined the crystal structure of the apoprotein in an "open" conformation at 2.3 Å resolution. Comparison with the structure of (-)-limonene synthase (Mentha spicata), which is representative of a fully closed conformation (Protein Data Bank entry 2ONG ), reveals that the short H-α1 helix moves nearly 5 Å inward upon substrate binding, and a conserved Tyr flips to point its hydroxyl group into the active site.

  4. Characterization of Structural Rebuilding and Shear Migration in Cementitious Materials in Consideration of Thixotropy (United States)

    Qian, Ye

    Characterization of structural rebuilding and shear migration in cementitious materials in consideration of thixotropy Ye Qian From initial contact with water until hardening, and deterioration, cement and concrete materials are subjected to various chemical and physical transformations and environmental impacts. This thesis focuses on the properties during the fresh state, shortly after mixing until the induction period. During this period flow history, including shearing and resting, and hydration both play big roles in determining the rheological properties. The rheological properties of cement and concrete not only affect the casting and pumping process, but also very critical for harden properties and durability properties. Compared with conventional concrete, self-consolidating concrete (SCC) can introduce many advantages in construction application. These include readiness to apply, decreasing labor necessary for casting, and enhancing hardened properties. However, challenges still remain, such as issues relating to formwork pressure and multi-layer casting. Each of these issues is closely related to the property of thixotropy. From the microstructural point of view, thixotropy is described as structural buildup (flocculation) under rest and breakdown (deflocculation) under flow. For SCC, as well as other concrete systems, it is about balancing sufficient flowability during casting and rate of structural buildup after placement for the application at hand. For instance, relating to the issue of SCC formwork, it is ideal for the material to be highly flowable to achieve rapid casting, but then exhibit high rate of structural buildup to reduce formwork pressure. This can reduce the cost of formwork and reduce the risk of formwork failure. It is apparent that accurately quantifying the two aspects of thixotropy, i.e. structuration and destructuration, is key to tackling these challenges in field application. Thus, the overall objective of my doctoral study is

  5. Structural characterization of Pt-Pd core-shell nanoparticles by Cs-corrected STEM

    Energy Technology Data Exchange (ETDEWEB)

    Esparza, R., E-mail: [Universidad Nacional Autonoma de Mexico, Centro de Fisica Aplicada y Tecnologia Avanzada (Mexico); Garcia-Ruiz, Amado F. [UPIICSA-COFAA, Instituto Politecnico Nacional (Mexico); Velazquez Salazar, J. J. [University of Texas at San Antonio, Department of Physics and Astronomy (United States); Perez, R. [Universidad Nacional Autonoma de Mexico, Centro de Fisica Aplicada y Tecnologia Avanzada (Mexico); Jose-Yacaman, M. [The University of Texas at San Antonio, Department of Physics and Astronomy (United States)


    Pt-Pd core-shell nanoparticles were synthesized using a modified polyol method. A thermal method under refluxing, carrying on the reaction up to 285 Degree-Sign C, has been performed to reduce metallic salts using ethylene glycol as reducer and poly(N-vinyl-2-pyrrolidone) as protective reagent of the formed bimetallic nanoparticles. According to other works, this type of structure has been studied and utilized to successfully increase the catalytic properties of monometallic nanoparticles Pt or Pd. Core-shell bimetallic nanoparticles were structurally characterized using aberration-corrected scanning transmission electron microscopy (Cs-STEM) equipped with a high-angle annular dark field detector, energy-dispersive X-ray spectrometry (EDS), and electron energy-loss spectroscopy (EELS). The high-resolution elemental line scan and mappings were carried out using a combination of STEM-EDS and STEM-EELS. The obtained results show the growth of the Pd shell on the Pt core with polyhedral morphology. The average size of the bimetallic nanoparticles was 13.5 nm and the average size of the core was 8.5 nm; consequently, the thickness of the shell was around 2.5 nm. The growth of the Pd shell on the Pt core is layer by layer, suggesting a Frank-van der Merwe growth mechanism.

  6. Physicochemical properties and structural characterization of a galactomannan from Sophora alopecuroides L. seeds. (United States)

    Guo, Rui; Ai, Lianzhong; Cao, Nannan; Ma, Juan; Wu, Yan; Wu, Jinhong; Sun, Xiangjun


    A water-soluble neutral polysaccharide (F25) was fractionated from crude polysaccharides of Sophora alopecuroides L. seeds. Its physicochemical properties and structural characterization were investigated. The I2-KI and Congo red reactions showed F25 possessed many branches without triple-helical conformation, which coincided with methylation and NMR analyses, i.e., F25 was a galactomannan with 1,4-linked β-d-Manp backbone distributed randomly (M/G 1.48-1.84) by major T-α-d-Galp (86.82%) or minor 1,4-linked α-d-Galp (13.18%) at O-6. Compared with [η] of deionized water (2.98dL/g), it was indicated that NaCl (2.89-2.90dL/g) and NaOH (2.27-2.28dL/g) could affect intrinsic interactions and conformation of F25 in solution, leading to molecular non-entanglements and intramolecular associations. This was demonstrated by 3D molecular modeling. Furthermore, the amorphous nature of F25 was revealed with higher crystallinity (25.7%) and crystallite size (7.6nm) compared to other polysaccharides. In this study, the possible relationships between molecular structure and physicochemical properties were obtained for F25, which could be potentially applied in food and pharmaceutical industries. Copyright © 2015 Elsevier Ltd. All rights reserved.

  7. Structural characterization and optical properties of perovskite ZnZrO 3 nanoparticles

    KAUST Repository

    Zhu, Xinhua


    Perovskite ZnZrO3 nanoparticles were synthesized by hydrothermal method, and their microstructures and optical properties were characterized. The crystallinity, phase formation, morphology and composition of the as-synthesized nanoparticles were characterized by X-ray diffraction (XRD), selected area electron diffraction (SAED), high-resolutiontransmission electron microscopy (HRTEM), and energy-dispersive X-ray (EDX) spectroscopy analysis, respectively. TEM images demonstrated that the average particle size of the ZnZrO3 powders was increased with increasing the Zn/Zr molar ratios in the precursors, and more large ZnZrO3 particles with cubic morphology were observed at high Zn/Zr molar ratios. In addition, the phase structures of the ZnZrO3 particles were also evolved from a cubic to tetragonal perovskite phase, as revealed by XRD and SAED patterns. HRTEM images demonstrate that surface structures of the ZnZrO3 powders synthesized at high Zn/Zr molar ratios, are composed of corners bound by the {100} mini-facets, and the surface steps lying on the {100} planes are frequently observed, whereas the (101) facet isoccasionally observed. The formation of such a rough surface structure is understood from the periodic bond chain theory. Quantitative EDX analyses demonstrated that the atomic concentrations (at.%) of Zn:Zr:O in the particles were 20.70:21.07:58.23, as close to the composition of ZnZrO3. In the optical spectra, a significant red shift of the absorption edges (for the ZnZrO3 nanopowders) from UV to visible region (from 394 to 417 nm) was observed as increasing the Zn/Zr molar ratios in the precursors, which corresponds to that the band gap energies of the ZnZrO3 nanopowders can be continuously tuned from 3.15 to 2.97 eV. This opens an easy way to tune the band gap energies of the ZnZrO3 nanopowders. © 2014 The American Ceramic Society.

  8. Characterization and structural analysis of the potent antiparasitic and antiviral agent tizoxanide (United States)

    Bruno, Flavia P.; Caira, Mino R.; Martin, Eliseo Ceballos; Monti, Gustavo A.; Sperandeo, Norma R.


    Tizoxanide [2-(hydroxy)-N-(5-nitro-2-thiazolyl)benzamide, TIZ] is a new potent anti-infective agent which may enhance current therapies for leishmaniasis, Chagas disease and viral hepatitis. The aim of this study was to identify the conformational preferences that may be related to the biological activity of TIZ by resolving its crystal structure and characterizing various physicochemical properties, including its experimental vibrational and 13C nuclear magnetic resonance properties, behavior on heating and solubility in several solvents at 25 °C. TIZ crystallizes from dimethylformamide as the carboxamide tautomer in the triclinic system, space group P(-1) (No. 2) with the following unit cell parameters at 173(2) K: a = 5.4110(3) Å, b = 7.3315(6) Å, c = 13.5293(9) Å, α = 97.528(3), β = 95.390(4), γ = 97.316(5), V = 524.41(6) Å3, Z = 2, Dc = 1.680 g/cm3, R1 = 0.0482 and wR2 = 0.0911 for 2374 reflections. This modification of TIZ has a 'graphitic' structure and is composed of tightly packed layers of extensively hydrogen-bonded molecules. The various spectroscopic data [Diffuse Fourier transform infrared (DRIFT) and FT-Raman, recorded in the range 3600-500 and 4000-200 cm-1 respectively, and solid-state 13C NMR] were consistent with the structure determined by X-ray crystallography. From DSC, TG and thermomicroscopy, it was concluded that TIZ is thermally stable as a solid and that melting is not an isolated event from the one-step thermal decomposition that it undergoes above 270 °C. This modification of TIZ is practically insoluble in water and slightly soluble in polar aprotic solvents such as dimethylsulfoxide, dimethylformamide and dioxane.

  9. Structural characterization of natural diamond shocked to 60 GPa; implications for Earth and planetary systems (United States)

    Jones, Adrian P.; McMillan, Paul F.; Salzmann, Christoph G.; Alvaro, Matteo; Nestola, Fabrizio; Prencipe, Mauro; Dobson, David; Hazael, Rachael; Moore, Moreton


    The possible presence of the high-density carbon polymorph with hexagonal symmetry known as ;lonsdaleite; provides an important marker for shock impact events. It is typically considered to form as a metastable phase produced from graphite or other carbonaceous precursors. However, its existence has recently been called into question. Here we collected high-resolution synchrotron X-ray diffraction data for laboratory-shocked and natural impact diamonds that both show evidence for deviations from cubic symmetry, that would be consistent with the appearance of hexagonal stacking sequences. These results show that hexagonality can be achieved by shocking diamond as well as from graphite precursors. The diffraction results are analyzed in terms of a general model that describes intermediate stacking sequences between pure diamond (fully cubic) and ;lonsdaleite; (fully hexagonal) phases, with provision made for ordered vs disordered stacking arrangements. This approach provides a ;hexagonality index; that can be used to characterize and distinguish among samples that have experienced different degrees of shock or static high pressure-high temperature treatments. We have also examined the relative energetics of diamond and ;lonsdaleite; structures using density functional theoretical (DFT) methods. The results set limits on the conditions under which a transformation between diamond and ;lonsdaleite; structures can be achieved. Calculated Raman spectra provide an indicator for the presence of extended hexagonal stacking sequences within natural and laboratory-prepared samples. Our results show that comparable crystallographic structures may be developed by impact-generated shockwaves starting from ambient conditions using either of the two different allotropes of carbon (diamond, graphite). This broadens the scope for its occurrence in terrestrial and planetary systems.

  10. Characterization of the Interior Density Structure of Near Earth Objects with Muons (United States)

    Prettyman, T. H.; Sykes, M. V.; Miller, R. S.; Pinsky, L. S.; Empl, A.; Nolan, M. C.; Koontz, S. L.; Lawrence, D. J.; Mittlefehldt, D. W.; Reddell, B. D.


    Near Earth Objects (NEOs) are a diverse population of short-lived asteroids originating from the main belt and Jupiter family comets. Some have orbits that are easy to access from Earth, making them attractive as targets for science and exploration as well as a potential resource. Some pose a potential impact threat. NEOs have undergone extensive collisional processing, fragmenting and re-accreting to form rubble piles, which may be compositionally heterogeneous (e.g., like 2008 TC3, the precursor to Almahata Sitta). At present, little is known about their interior structure or how these objects are held together. The wide range of inferred NEO macroporosities hint at complex interiors. Information about their density structure would aid in understanding their formation and collisional histories, the risks they pose to human interactions with their surfaces, the constraints on industrial processing of NEO resources, and the selection of hazard mitigation strategies (e.g., kinetic impactor vs nuclear burst). Several methods have been proposed to characterize asteroid interiors, including radar imaging, seismic tomography, and muon imaging (muon radiography and tomography). Of these, only muon imaging has the potential to determine interior density structure, including the relative density of constituent fragments. Muons are produced by galactic cosmic ray showers within the top meter of asteroid surfaces. High-energy muons can traverse large distances through rock with little deflection. Muons transmitted through an Itokawa-sized asteroid can be imaged using a compact hodoscope placed on or near the surface. Challenges include background rejection and correction for variations in muon production with surface density. The former is being addressed by hodoscope design. Surface density variations can be determined via radar or muon limb imaging. The performance of muon imaging is evaluated for prospective NEO interior-mapping missions.

  11. Structural Characterization of Ferric Hemoglobins from Three Antarctic Fish Species of the Suborder Notothenioidei (United States)

    Vergara, Alessandro; Franzese, Marisa; Merlino, Antonello; Vitagliano, Luigi; Verde, Cinzia; di Prisco, Guido; Lee, H. Caroline; Peisach, Jack; Mazzarella, Lelio


    Spontaneous autoxidation of tetrameric Hbs leads to the formation of Fe (III) forms, whose physiological role is not fully understood. Here we report structural characterization by EPR of the oxidized states of tetrameric Hbs isolated from the Antarctic fish species Trematomus bernacchii, Trematomus newnesi, and Gymnodraco acuticeps, as well as the x-ray crystal structure of oxidized Trematomus bernacchii Hb, redetermined at high resolution. The oxidation of these Hbs leads to formation of states that were not usually detected in previous analyses of tetrameric Hbs. In addition to the commonly found aquo-met and hydroxy-met species, EPR analyses show that two distinct hemichromes coexist at physiological pH, referred to as hemichromes I and II, respectively. Together with the high-resolution crystal structure (1.5 Å) of T. bernacchii and a survey of data available for other heme proteins, hemichrome I was assigned by x-ray crystallography and by EPR as a bis-His complex with a distorted geometry, whereas hemichrome II is a less constrained (cytochrome b5-like) bis-His complex. In four of the five Antartic fish Hbs examined, hemichrome I is the major form. EPR shows that for HbCTn, the amount of hemichrome I is substantially reduced. In addition, the concomitant presence of a penta-coordinated high-spin Fe (III) species, to our knowledge never reported before for a wild-type tetrameric Hb, was detected. A molecular modeling investigation demonstrates that the presence of the bulkier Ile in position 67β in HbCTn in place of Val as in the other four Hbs impairs the formation of hemichrome I, thus favoring the formation of the ferric penta-coordinated species. Altogether the data show that ferric states commonly associated with monomeric and dimeric Hbs are also found in tetrameric Hbs. PMID:17545238

  12. Hydrothermal syntheses and characterization of uranyl tungstates with electro-neutral structural units

    Energy Technology Data Exchange (ETDEWEB)

    Balboni, Enrica; Burns, Peter C. [Univ. of Notre Dame, IN (United States). Dept. of Civil and Enviromental Engineering and Earth Sciences; Univ. of Notre Dame, IN (United States). Dept. of Chemistry and Biochemistry


    Two uranyl tungstates, (UO{sub 2})(W{sub 2}O{sub 7})(H{sub 2}O){sub 3} (1) and (UO{sub 2}){sub 3}(W{sub 2}O{sub 8})F{sub 2}(H{sub 2}O){sub 3} (2), were synthesized under hydrothermal conditions at 220 C and were structurally, chemically, and spectroscopically characterized. 1 Crystallizes in space group Pbcm, a = 6.673(5) Aa, b = 12.601(11) Aa, c = 11.552 Aa; 2 is in C2/m, a = 13.648(1) Aa, b = 16.852(1) Aa, c = 9.832(1) Aa, β = 125.980(1) {sup circle}. In 1 the U(VI) cations are present as (UO{sub 2}){sup 2+} uranyl ions that are coordinated by five oxygen atoms to give pentagonal bipyramids. These share two edges with two tungstate octahedra and single vertices with four additional octahedra, resulting in a sheet with the iriginite-type anion topology. Only water molecules are located in the interlayer. The structural units of 2 consist of (UO{sub 2}){sup 2+} uranyl oxy-fluoride pentagonal bipyramids present as either [UO{sub 2}F{sub 2}O{sub 3}]{sup -6} or [UO{sub 2}FO{sub 4}]{sup -5}, and strongly distorted tungstate octahedra. The linkage of uranyl pentagonal bipyramids and tungstate octahedra gives a unique sheet anion topology consisting of pentagons, squares and triangles. In 2, the uranyl tungstates sheets are connected into a novel electro-neutral three-dimensional framework through dimers of uranyl pentagonal bipyramids. These dimers connecting the sheets share an edge defined by F anions. 2 is the first example of a uranyl tungstate oxy-fluoride, and 1 and 2 are rare examples of uranyl compounds containing electro-neutral structural units.

  13. Structural and biochemical characterization of the broad substrate specificity of Bacteroides thetaiotaomicron commensal sialidase. (United States)

    Park, Kwang-Hyun; Kim, Min-Gyu; Ahn, Hee-Jeong; Lee, Dae-Han; Kim, Jin-Hyo; Kim, Young-Wan; Woo, Eui-Jeon


    Sialidases release the terminal sialic acid residue from a wide range of sialic acid-containing polysaccharides. Bacteroides thetaiotaomicron, a symbiotic commensal microbe, resides in and dominates the human intestinal tract. We characterized the recombinant sialidase from B. thetaiotaomicron (BTSA) and demonstrated that it has broad substrate specificity with a relative activity of 97, 100 and 64 for 2,3-, 2,6- and 2,8-linked sialic substrates, respectively. The hydrolysis activity of BTSA was inhibited by a transition state analogue, 2-deoxy-2,3-dehydro-N-acetyl neuraminic acid, by competitive inhibition with a Ki value of 35μM. The structure of BSTA was determined at a resolution of 2.3Å. This structure exhibited a unique carbohydrate-binding domain (CBM) at its N-terminus (a.a. 23-190) that is adjacent to the catalytic domain (a.a. 191-535). The catalytic domain has a conserved arginine triad with a wide-open entrance for the substrate that exposes the catalytic residue to the surface. Unlike other pathogenic sialidases, the polysaccharide-binding site in the CBM is near the active site and possibly holds and positions the polysaccharide substrate directly at the active site. The structural feature of a wide substrate-binding groove and closer proximity of the polysaccharide-binding site to the active site could be a unique signature of the commensal sialidase BTSA and provide a molecular basis for its pharmaceutical application. Copyright © 2013 Elsevier B.V. All rights reserved.

  14. Structural characterization and pH-induced conformational transition of full-length KcsA. (United States)

    Zimmer, Jochen; Doyle, Declan A; Grossmann, J Günter


    The bacterial K+ channel KcsA from Streptomyces lividans was analyzed by neutron and x-ray small-angle solution scattering. The C-terminally truncated version of KcsA, amenable to crystallographic studies, was compared with the full-length channel. Analyzing the scattering data in terms of radius of gyration reveals differences between both KcsA species of up to 13.2 A. Equally, the real-space distance distribution identifies a 40 to 50 A extension of full-length KcsA compared to its C-terminally truncated counterpart. We show that the x-ray and neutron scattering data are amenable for molecular shape reconstruction of full-length KcsA. The molecular envelopes calculated display an hourglass-shaped structure within the C-terminal intracellular domain. The C-terminus extends the membrane spanning region of KcsA by 54-70 A, with a central constriction 10-30 A wide. Solution scattering techniques were further employed to characterize the KcsA channel under acidic conditions favoring its open conformation. The full-length KcsA at pH 5.0 shows the characteristics of a dumbbell-shaped macromolecular structure, originating from dimerization of the tetrameric K+ channel. Since C-terminally truncated KcsA measured under the same low pH conditions remains tetrameric, oligomerization of full-length KcsA seems to proceed via structurally changed C-terminal domains. The determined maximum dimensions of the newly formed complex increase by 50-60%. Shape reconstruction of the pseudooctameric complex indicates the pH-induced conformational reorganization of the intracellular C-terminal domain.

  15. Functional and structural characterization of neutralizing epitopes of measles virus hemagglutinin protein. (United States)

    Tahara, Maino; Ito, Yuri; Brindley, Melinda A; Ma, Xuemin; He, Jilan; Xu, Songtao; Fukuhara, Hideo; Sakai, Kouji; Komase, Katsuhiro; Rota, Paul A; Plemper, Richard K; Maenaka, Katsumi; Takeda, Makoto


    Effective vaccination programs have dramatically reduced the number of measles-related deaths globally. Although all the available data suggest that measles eradication is biologically feasible, a structural and biochemical basis for the single serotype nature of measles virus (MV) remains to be provided. The hemagglutinin (H) protein, which binds to two discrete proteinaceous receptors, is the major neutralizing target. Monoclonal antibodies (MAbs) recognizing distinct epitopes on the H protein were characterized using recombinant MVs encoding the H gene from different MV genotypes. The effects of various mutations on neutralization by MAbs and virus fitness were also analyzed, identifying the location of five epitopes on the H protein structure. Our data in the present study demonstrated that the H protein of MV possesses at least two conserved effective neutralizing epitopes. One, which is a previously recognized epitope, is located near the receptor-binding site (RBS), and thus MAbs that recognize this epitope blocked the receptor binding of the H protein, whereas the other epitope is located at the position distant from the RBS. Thus, a MAb that recognizes this epitope did not inhibit the receptor binding of the H protein, rather interfered with the hemagglutinin-fusion (H-F) interaction. This epitope was suggested to play a key role for formation of a higher order of an H-F protein oligomeric structure. Our data also identified one nonconserved effective neutralizing epitope. The epitope has been masked by an N-linked sugar modification in some genotype MV strains. These data would contribute to our understanding of the antigenicity of MV and support the global elimination program of measles.

  16. Structural characterization and EXAFS wavelet analysis of Yb doped ZnO by wet chemistry route

    Energy Technology Data Exchange (ETDEWEB)

    Otal, Eugenio H., E-mail: [Division of Porous Materials, UNIDEF, CITEDEF, CONICET, S.J.B de la Salle 4397, Villa Martelli (B1603ALO), Buenos Aires (Argentina); Laboratory for Materials Science and Technology, FRSC-UTN, Av. Inmigrantes 555, Río Gallegos 9400 (Argentina); Sileo, Elsa [INQUIMAE, Departamento de Química Inorgánica, Analítica y Química Física, Facultad de Ciencias Exactas y Naturales, Universidad de Buenos Aires (Argentina); Aguirre, Myriam H. [Dept. of Physics Condensed Matter, University of Zaragoza (Spain); Laboratory of Advanced Microscopy (LMA), Institute of Nanoscience of Aragón (INA), University of Zaragoza (Spain); Fabregas, Ismael O. [Division of Porous Materials, UNIDEF, CITEDEF, CONICET, S.J.B de la Salle 4397, Villa Martelli (B1603ALO), Buenos Aires (Argentina); Kim, Manuela [Division of Porous Materials, UNIDEF, CITEDEF, CONICET, S.J.B de la Salle 4397, Villa Martelli (B1603ALO), Buenos Aires (Argentina); Laboratory for Materials Science and Technology, FRSC-UTN, Av. Inmigrantes 555, Río Gallegos 9400 (Argentina)


    Highlights: • Optical and electrical properties of ZnO are influenced by lanthanide doping. • Optical and electrical properties of ZnO are influenced by lanthanide positioning. • Yb is incorporated in the O{sub h} sites of the wurtzite structure. • There is not Yb{sub 2}O{sub 3} clustering or segregation for treatments below 800 °C. - Abstract: Lanthanide doped ZnO are interesting materials for optical and electrical applications. The wide band gap of this semiconductor makes it transparent in the visible range (E{sub gap} = 3.2 eV), allowing a sharp emission from intra shell transition from the lanthanides. From the electrical side, ZnO is a widely used material in varistors and its electrical properties can be tailored by the inclusion of lanthanides. Both applications are influenced by the location of the lanthanides, grain boundaries or lattice inclusion. Yb doped ZnO samples obtained by wet chemistry route were annealed at different temperatures and characterized by Transmission Electron Microscopy (TEM), X-ray Diffraction (XRD), Rietveld refinement of XRD data, and X-ray Absorption Fine Structure (XAFS). These techniques allowed to follow the changes occurred in the matrix and the Yb environment. The use of the Cauchy continuous wavelet transform allowed identifying a second coordination shell composed of Zn atoms, supporting the observations from XRD Rietveld refinement and XAFS fittings. The information obtained confirmed the incorporation of Yb in O{sub h} sites of the wurtzite structure without Yb{sub 2}O{sub 3} clustering in the lattice.

  17. Structural Characterization of Maize SIRK1 Kinase Domain Reveals an Unusual Architecture of the Activation Segment

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    Bruno Aquino


    Full Text Available Kinases are primary regulators of plant metabolism and excellent targets for plant breeding. However, most kinases, including the abundant receptor-like kinases (RLK, have no assigned role. SIRK1 is a leucine-rich repeat receptor-like kinase (LRR-RLK, the largest family of RLK. In Arabidopsis thaliana, SIRK1 (AtSIRK1 is phosphorylated after sucrose is resupplied to sucrose-starved seedlings and it modulates the sugar response by phosphorylating several substrates. In maize, the ZmSIRK1 expression is altered in response to drought stress. In neither Arabidopsis nor in maize has the function of SIRK1 been completely elucidated. As a first step toward the biochemical characterization of ZmSIRK1, we obtained its recombinant kinase domain, demonstrated that it binds AMP-PNP, a non-hydrolysable ATP-analog, and solved the structure of ZmSIRK1- AMP-PNP co-crystal. The ZmSIRK1 crystal structure revealed a unique conformation for the activation segment. In an attempt to find inhibitors for ZmSIRK1, we screened a focused small molecule library and identified six compounds that stabilized ZmSIRK1 against thermal melt. ITC analysis confirmed that three of these compounds bound to ZmSIRK1 with low micromolar affinity. Solving the 3D structure of ZmSIRK1-AMP-PNP co-crystal provided information on the molecular mechanism of ZmSIRK1 activity. Furthermore, the identification of small molecules that bind this kinase can serve as initial backbone for development of new potent and selective ZmSIRK1 antagonists.

  18. Structural and functional characterization of a multifunctional alanine-rich peptide analogue from Pleuronectes americanus.

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    Ludovico Migliolo

    Full Text Available Recently, defense peptides that are able to act against several targets have been characterized. The present work focuses on structural and functional evaluation of the peptide analogue Pa-MAP, previously isolated as an antifreeze peptide from Pleuronectes americanus. Pa-MAP showed activities against different targets such as tumoral cells in culture (CACO-2, MCF-7 and HCT-116, bacteria (Escherichia coli ATCC 8739 and Staphylococcus aureus ATCC 25923, viruses (HSV-1 and HSV-2 and fungi (Candida parapsilosis ATCC 22019, Trichophyton mentagrophytes (28d&E and T. rubrum (327. This peptide did not show toxicity against mammalian cells such as erythrocytes, Vero and RAW 264.7 cells. Molecular mechanism of action was related to hydrophobic residues, since only the terminal amino group is charged at pH 7 as confirmed by potentiometric titration. In order to shed some light on its structure-function relations, in vitro and in silico assays were carried out using circular dichroism and molecular dynamics. Furthermore, Pa-MAP showed partial unfolding of the peptide changes in a wide pH (3 to 11 and temperature (25 to 95°C ranges, although it might not reach complete unfolding at 95°C, suggesting a high conformational stability. This peptide also showed a conformational transition with a partial α-helical fold in water and a full α-helical core in SDS and TFE environments. These results were corroborated by spectral data measured at 222 nm and by 50 ns dynamic simulation. In conclusion, data reported here show that Pa-MAP is a potential candidate for drug design against pathogenic microorganisms due to its structural stability and wide activity against a range of targets.

  19. Synthesis and structural characterization of raffinosyl-oligofructosides upon transfructosylation by Lactobacillus gasseri DSM 20604 inulosucrase. (United States)

    Díez-Municio, Marina; Herrero, Miguel; de Las Rivas, Blanca; Muñoz, Rosario; Jimeno, M Luisa; Moreno, F Javier


    A new process based on enzymatic synthesis of a series of raffinose-derived oligosaccharides or raffinosyl-oligofructosides (RFOS) with degree of polymerization (DP) from 4 to 8 was developed in the presence of raffinose. This process involves a transfructosylation reaction catalyzed by an inulosucrase from Lactobacillus gasseri DSM 20604 (IS). The main synthesized RFOS were structurally characterized by nuclear magnetic resonance (NMR). According to the elucidated structures, RFOS consist of β-2,1-linked fructose unit(s) to raffinose: α-D-galactopyranosyl-(1 → 6)-α-D-glucopyranosyl-(1↔2)-β-D-fructofuranosyl-((1 ← 2)-β-D-fructofuranoside)n (where n refers to the number of transferred fructose moieties). The maximum yield of RFOS was 33.4 % (in weight respect to the initial amount of raffinose) and was obtained at the time interval of 8-24 h of transfructosylation reaction initiated with 50 % (w/v) of raffinose. Results revealed the high acceptor and donor affinity of IS towards raffinose, being fairly comparable with that of sucrose for the production of fructooligosaccharides (FOS), including when both carbohydrates coexisted (sucrose/raffinose mixture, 250 g L(-1) each). The production of RFOS was also attempted in the presence of sucrose/melibiose mixtures; in this case, the predominant acceptor-product formed was raffinose followed by a minor production of a series of oligosaccharides with varying DP. The easiness of RFOS synthesis and the structural similarities with both raffinose and fructan series of oligosaccharides warrant the further study of the potential bioactive properties of these unexplored oligosaccharides.

  20. Characterization of the chemical structures and physical properties of exopolysaccharides produced by various Streptococcus thermophilus strains. (United States)

    Pachekrepapol, U; Lucey, J A; Gong, Y; Naran, R; Azadi, P


    Exopolysaccharides (EPS) produced by some lactic acid bacteria are often used by the dairy industry to improve the rheological and physical properties of yogurt, but the relationship between their structure and functional effect is still unclear. The EPS from different species, or different strains from the same species, may differ in terms of molar mass, repeating unit structure, and EPS yield during fermentation of milk. This study aimed to characterize the detailed properties of EPS produced from 7 strains of Streptococcus thermophilus, which is one of the key cultures used for yogurt manufacture. Milk was fermented with strains DGCC 7698, DGCC 7710, DGCC 7785, ST-10255y, St-143, STCth-9204, and ST4239. These strains were selected because they have been used in previous studies on yogurt texture, but a complete description of their EPS structural properties has not yet been reported. All strains were fermented under a similar acidification rate by adjusting the level of supplementation with peptone or the inoculation level, which allowed for a comparison of EPS yields under similar growth conditions (reconstituted skim milk at 40°C). The EPS from each strain was isolated and the weight-average molar mass and z-average root mean square radius determined using size-exclusion chromatography multiangle laser light scattering. The monosaccharide composition of EPS was determined using gas chromatography-mass spectrometry, and repeating unit structure was determined using nuclear magnetic resonance spectroscopy. The weight-average molar mass values of EPS ranged from 0.14 to 1.61 × 10(6) g/mol. All 7 EPS samples were uncharged. The strains ST-10255y and ST4239 had EPS with the same repeating unit structure. The monosaccharide compositions of the various EPS were mainly composed of glucose and galactose, with low levels of rhamnose in the EPS isolated from DGCC 7698, and N-acetylgalactosamine in the EPS from DGCC 7785, ST-10255y, and ST4239. The yields of EPS